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Sample records for ultrasonic extraction coupled

  1. Aluminium sensitized spectrofluorimetric determination of fluoroquinolones in milk samples coupled with salting-out assisted liquid-liquid ultrasonic extraction

    Science.gov (United States)

    Xia, Qinghai; Yang, Yaling; Liu, Mousheng

    2012-10-01

    An aluminium sensitized spectrofluorimetric method coupled with salting-out assisted liquid-liquid ultrasonic extraction for the determination of four widely used fluoroquinolones (FQs) namely norfloxacin (NOR), ofloxacin (OFL), ciprofloxacin (CIP) and gatifloxacin (GAT) in bovine raw milk was described. The analytical procedure involves the fluorescence sensitization of aluminium (Al3+) by complexation with FQs, salting-out assisted liquid-liquid ultrasonic extraction (SALLUE), followed by spectrofluorometry. The influence of several parameters on the extraction (the salt species, the amount of salt, pH, temperature and phase volume ratio) was investigated. Under optimized experimental conditions, the detection limits of the method in milk varied from 0.009 μg/mL for NOR to 0.016 μg/mL for GAT (signal-to-noise ratio (S/N) = 3). The relative standard deviations (RSD) values were found to be relatively low (0.54-2.48% for four compounds). The calibration graph was linear from 0.015 to 2.25 μg/mL with coefficient of determinations not less than 0.9974. The methodology developed was applied to the determination of FQs in bovine raw milk samples. The main advantage of this method is simple, accurate and green. The method showed promising applications for analyzing polar analytes especially polar drugs in various sample matrices.

  2. Determination of mercury species in biological samples by inductively coupled plasma mass spectrometry combined with solvent extraction and ultrasonication

    International Nuclear Information System (INIS)

    Sun, J.; Li, Y.F.; Wang, J.X.; Chen, C.Y.; Li, B.; Gao, Y.X.; Chai, Z.F.

    2005-01-01

    Mercury (Hg) is a well-known toxic element. The toxic effects of Hg depend on its chemical forms. The most important chemical forms are elemental Hg (Hg 0 ), inorganic Hg (Hg 2+ ) and methylmercury (CH 3 Hg + ). In the biogeochemical cycle of Hg, these species may interchange in atmospheric, aquatic and terrestrial environments. Among them, methylmercury is considerably higher toxic than elemental mercury and inorganic mercury because it is recognized as one of major health hazards for human due to its teratogenic, immunotoxic, and neurotoxic effects. Therefore, determinations of not only total mercury, but also methylmercury content in biological samples is necessary. In large numbers of analytical methods, inductively coupled plasma mass spectrometry (ICP-MS) using conventional sample introduction with a peristaltic pump is widely used for the determination of trace metals in a wide variety of different sample matrices. ICP-MS can offer high sensitivity, low detection limit, reasonable accuracy and precision, and can easily be automated. However, mercury is considered as an element with analytical problems. One problem is well known in Hg analysis that the memory effect increases the blank counts and worsens the analytical performance of ICP-MS. The possibility of Hg losses during sample decomposition procedure due to its volatility is another important issue. Additionally, its high first ionization potential and numerous isotopes have limited its sensitivity in ICP-MS analysis. In order to solve the above questions, the present work was carried out to develop a method based on ICP-MS coupled with solvent extraction for determination of mercury species in biological samples. At first step, we investigated different solvent extraction methods including acid leaching, CuSO 4 extraction, alkaline-methanol extraction, and surfactant extraction with ultrasonication for methylmercury determination using the certified reference materials GBW07601 (Human Hair). Next, we

  3. Eco-friendly ionic liquid based ultrasonic assisted selective extraction coupled with a simple liquid chromatography for the reliable determination of acrylamide in food samples.

    Science.gov (United States)

    Albishri, Hassan M; El-Hady, Deia Abd

    2014-01-01

    Acrylamide in food has drawn worldwide attention since 2002 due to its neurotoxic and carcinogenic effects. These influences brought out the dual polar and non-polar characters of acrylamide as they enabled it to dissolve in aqueous blood medium or penetrate the non-polar plasma membrane. In the current work, a simple HPLC/UV system was used to reveal that the penetration of acrylamide in non-polar phase was stronger than its dissolution in polar phase. The presence of phosphate salts in the polar phase reduced the acrylamide interaction with the non-polar phase. Furthermore, an eco-friendly and costless coupling of the HPLC/UV with ionic liquid based ultrasonic assisted extraction (ILUAE) was developed to determine the acrylamide content in food samples. ILUAE was proposed for the efficient extraction of acrylamide from bread and potato chips samples. The extracts were obtained by soaking of potato chips and bread samples in 1.5 mol L(-1) 1-butyl-3-methylimmidazolium bromide (BMIMBr) for 30.0 and 60.0 min, respectively and subsequent chromatographic separation within 12.0 min using Luna C18 column and 100% water mobile phase with 0.5 mL min(-1) under 25 °C column temperature at 250 nm. The extraction and analysis of acrylamide could be achieved within 2h. The mean extraction efficiency of acrylamide showed adequate repeatability with relative standard deviation (RSD) of 4.5%. The limit of detection and limit of quantitation were 25.0 and 80.0 ng mL(-1), respectively. The accuracy of the proposed method was tested by recovery in seven food samples giving values ranged between 90.6% and 109.8%. Therefore, the methodology was successfully validated by official guidelines, indicating its reliability to be applied to analysis of real samples, proven to be useful for its intended purpose. Moreover, it served as a simple, eco-friendly and costless alternative method over hitherto reported ones. © 2013 Elsevier B.V. All rights reserved.

  4. Ultrasonic extraction of flavonoids and phenolics from loquat ...

    African Journals Online (AJOL)

    Administrator

    2011-06-08

    Jun 8, 2011 ... ultrasonic pharmaceutical managing machine (Sinobest electronic. Co. Ltd., Jining, Shangdong ... During the ultrasonic treatment, the temperature ..... essential oil extraction by a hydrodistillation process using a 2(4) complete ...

  5. Preconcentration and determination of vanadium and molybdenum in milk, vegetables and foodstuffs by ultrasonic-thermostatic-assisted cloud point extraction coupled to flame atomic absorption spectrometry.

    Science.gov (United States)

    Gürkan, Ramazan; Korkmaz, Sema; Altunay, Nail

    2016-08-01

    A new ultrasonic-thermostatic-assisted cloud point extraction procedure (UTA-CPE) was developed for preconcentration at the trace levels of vanadium (V) and molybdenum (Mo) in milk, vegetables and foodstuffs prior to determination via flame atomic absorption spectrometry (FAAS). The method is based on the ion-association of stable anionic oxalate complexes of V(V) and Mo(VI) with [9-(diethylamino)benzo[a]phenoxazin-5-ylidene]azanium; sulfate (Nile blue A) at pH 4.5, and then extraction of the formed ion-association complexes into micellar phase of polyoxyethylene(7.5)nonylphenyl ether (PONPE 7.5). The UTA-CPE is greatly simplified and accelerated compared to traditional cloud point extraction (CPE). The analytical parameters optimized are solution pH, the concentrations of complexing reagents (oxalate and Nile blue A), the PONPE 7.5 concentration, electrolyte concentration, sample volume, temperature and ultrasonic power. Under the optimum conditions, the calibration curves for Mo(VI) and V(V) are obtained in the concentration range of 3-340µgL(-1) and 5-250µgL(-1) with high sensitivity enhancement factors (EFs) of 145 and 115, respectively. The limits of detection (LODs) for Mo(VI) and V(V) are 0.86 and 1.55µgL(-1), respectively. The proposed method demonstrated good performances such as relative standard deviations (as RSD %) (≤3.5%) and spiked recoveries (95.7-102.3%). The accuracy of the method was assessed by analysis of two standard reference materials (SRMs) and recoveries of spiked solutions. The method was successfully applied into the determination of trace amounts of Mo(VI) and V(V) in milk, vegetables and foodstuffs with satisfactory results. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Selenium speciation in radix puerariae using ultrasonic assisted extraction combined with reversed phase high performance liquid chromatography-inductively coupled plasma-mass spectrometry after magnetic solid-phase extraction with 5-sulfosalicylic acid functionalized magnetic nanoparticles

    Science.gov (United States)

    Cao, Yupin; Yan, Lizhen; Huang, Hongli; Deng, Biyang

    2016-08-01

    A new method for determination of selenium species in radix puerariae was described. The method consists of sample enrichment with 5-sulfosalicylic acid (SSA)-functionalized silica-coated magnetic nanoparticles (SMNPs), high performance liquid chromatography (HPLC) separation, and online detection using inductively coupled plasma mass spectrometry (ICP-MS). The selenium species were extracted using ultrasonic extraction system with a mixture of protease K and lipase. The SSA-SMNPs were used to enrich trace amounts of selenite [Se(IV)], selenate [Se(VI)], selenomethionine (SeMet), and selenocystine (SeCys2) from lower selenium containing samples. Under the optimal conditions, the limits of detection (3σ) for SeCys2, Se(IV), SeMet and Se(VI) were observed as 0.0023, 0.0015, 0.0043, and 0.0016 ng mL- 1, respectively. The RSD values (n = 6) of method for intraday were observed between 0.5% and 0.9%. The RSD values of method for interday were less than 1.3%. The linear concentration ranges for SeCys2, Se(IV), SeMet and Se(VI) were 0.008-1000, 0.005-200, 0.015-500 and 0.006-200 ng mL- 1, respectively. The detection limits of this method were improved by 10 times due to the enrichment with the SSA-SMNP extraction. The contents of SeCys2, Se(IV), SeMet, and Se(VI) in radix puerariae were determined as 0.0140, 0.171, 0.0178, and 0.0344 μg g- 1, respectively. The recoveries were in the range of 95.6%-99.4% and the RSDs (n = 6) of recoveries were less than 1.5%.

  7. A simple one-step ultrasonic-assisted extraction and derivatization method coupling to high-performance liquid chromatographyfor the determination of ε-aminocaproic acid and amino acids in cosmetics.

    Science.gov (United States)

    Du, Yuanqi; Xia, Ling; Xiao, Xiaohua; Li, Gongke; Chen, Xiaoguang

    2018-06-15

    Nowadays, the safety of cosmetics is a widespread concern. Amines are common cosmetic additives. Some of them such as amino acids are beneficial. Another kind of amines, however, ε-aminocaproic acid (EACA) is prohibited to add into cosmetics for its adverse reactions. In this study, a simple, rapid, sensitive and eco-friendly one-step ultrasonic-assisted extraction and derivatization (UAE-D) method was developed for determination of EACA and amino acids in cosmetics by coupling with high-performance liquid chromatography (HPLC). By using this sample preparation method, extraction and derivatization of EACA and amino acids were finished in one step in ultrasound field. During this procedure, 4-fluoro-7-nitrobenzofurazan (NBD-F)was applied as derivatization reagent. The extraction conditions including the amount of NBD-F, extraction and derivatization temperature, the ultrasonic vibration time and pH value of the aqueous phase were evaluated. Meanwhile, the extraction mechanism was investigated. Under optimized conditions, the method detection limits were 0.086-0.15 μg/L, and method quantitation limits were 0.29-0.47 μg/L with RSDs less than 3.7% (n = 3). The recoveries of EACA and amino acids obtained from cosmetic samples were in range from 76.9% to 122.3%. Amino acids were found in all selected samples and quantified in range from 1.9 ± 0.9 to 677.2 ± 17.9 μg/kg. And EACA was found and quantified with the contents of 1284.3 ± 22.1 μg/kg in a toner sample. This UAE-D-HPLC method shortened and simplified the sample pretreatment as well as enhanced the sensitivity of analytical method. In our record, only 10 min was needed for the total sample preparation process. And the method detection limits were two orders of magnitude less than literature reports. Furthermore, we reduced the consumption of solvent and minimized the usage of organic solvents, which made our method moving towards green analytical chemistry. In brief, our UAE

  8. Optimization design of high power ultrasonic circular ring radiator in coupled vibration.

    Science.gov (United States)

    Xu, Long; Lin, Shuyu; Hu, Wenxu

    2011-10-01

    This paper presents a new high power ultrasonic (HPU) radiator, which consists of a transducer, an ultrasonic horn, and a metal circular ring. Both the transducer and horn in longitudinal vibrations are used to drive a metal circular ring in a radial-axial coupled vibration. This coupled vibration cannot only generate ultrasound in both the radial and axial directions, but also focus the ultrasound inside the circular ring. Except for the radial-axial coupled vibration mode, the third longitudinal harmonic vibration mode with relative large vibration amplitude is also detected, which can be used as another operation mode. Overall, the HPU with these two vibration modes should have good potential to be applied in liquid processing, such as sonochemistry, ultrasonic cleaning, and Chinese herbal medicine extraction. Copyright © 2011 Elsevier B.V. All rights reserved.

  9. Ultrasonically enhanced extraction of bioactive principles from Quillaja Saponaria Molina.

    Science.gov (United States)

    Gaete-Garretón, L; Vargas-Hernández, Yolanda; Cares-Pacheco, María G; Sainz, Javier; Alarcón, John

    2011-07-01

    A study of ultrasonic enhancement in the extraction of bioactive principles from Quillaja Saponaria Molina (Quillay) is presented. The effects influencing the extraction process were studied through a two-level factorial design. The effects considered in the experimental design were: granulometry, extraction time, acoustic Power, raw matter/solvent ratio (concentration) and acoustic impedance. It was found that for aqueous extraction the main factors affecting the ultrasonically-assisted process were: granulometry, raw matter/solvent ratio and extraction time. The extraction ratio was increased by Ultrasonics effect and a reduction in extraction time was verified without any influence in the product quality. In addition the process can be carried out at lower temperatures than the conventional method. As the process developed uses chips from the branches of trees, and not only the bark, this research contributes to make the saponin exploitation process a sustainable industry. Copyright © 2010 Elsevier B.V. All rights reserved.

  10. Ultrasonic-Assisted Extraction and Antioxidant Activity of Flavonoids ...

    African Journals Online (AJOL)

    Purpose: To identify the main flavonoid in Adinandra nitida leaf, employ response surface methodology to optimize its ultrasonic-assisted extraction, and determine the antioxidant activity of the obtained extract. Methods: The main flavonoid in Adinandra nitida leaf was obtained by traditional solvent extraction and ...

  11. Ultrasonic extraction of flavonoids and phenolics from loquat ...

    African Journals Online (AJOL)

    Ethanol was used to extract flavonoids and phenolics from loquat (Eriobotrya japonica Lindl. cv. Ruantiaobaisha) flowers with ultrasonic pharmaceutical managing machine. Single-factor and orthogonal experiment were used to investigate the optimum extraction condition. The results showed that, the combination of 30°C, ...

  12. Examination of Sandwich Materials Using Air-Coupled Ultrasonics

    DEFF Research Database (Denmark)

    Borum, K.K.; Berggreen, Carl Christian

    2004-01-01

    The air-coupled ultrasonic techniques have been improved drastically in recent years. Better equipment has made this technique much more useful. This paper focuses on the examination of sandwich materials used in naval ships. It is more convenient to be able to make the measurements directly...

  13. Ultrasonic assisted extraction - an alternative for sample preparation (M4)

    International Nuclear Information System (INIS)

    Santos Junior, P.; Barbosa Junior, F.; Krug, F.J.; Trevizan, L.C.; Nobrega, J.A.

    2002-01-01

    Full text: In the last years the ultrasound assisted metal extraction has been frequency proposed as a simple and inexpensive alternative for sample preparation of biological and inorganic samples. The extraction effect is considered as being caused by acoustic cavitation, that is, bubble formation and subsequent disruptive action. The collapse of bubbles created by sonication of solutions results in the generation of extremely high local temperature and pressure gradients, which may be regarded as localized 'hot spots'. On a timescale of about 10 -10 s, effective local pressures and temperature of about 10 5 atm and about 5000 K, respectively, are generated under sonochemical conditions. Usually, this method uses a diluted acid medium decreasing blank values and reducing both reagents and time consumption compared to traditional wet digestion systems using conductive or microwave-assisted heating. Furthermore, sonication can also allow the preparation of samples directly within the sample container, thereby preventing sample losses and minimizing sample contamination. Although some controversial results concerning metals extraction behavior have been reported, they could be explained by analyte-matrix interaction and the ability of the ultrasonic processor to generate ultrasound (i.e. the use of an ultrasonic bath or an ultrasonic probe at different power, frequency, and amplitude). This contribution presents a review of ultrasound assisted metal extraction and recent performance data obtained in our laboratory for determination of elements in biological materials, soils and sediments by ICP-OES and ETAAS. The effect of extraction parameters, such as type and concentration of the leaching solution, sonication time and performance of ultrasonic processor (bath or probe) will be presented. (author)

  14. Binary Solvent Extraction System and Extraction Time Effects on Phenolic Antioxidants from Kenaf Seeds (Hibiscus cannabinus L.) Extracted by a Pulsed Ultrasonic-Assisted Extraction

    OpenAIRE

    Yu Hua Wong; Hwee Wen Lau; Chin Ping Tan; Kamariah Long; Kar Lin Nyam

    2014-01-01

    The aim of this study was to determine the best parameter for extracting phenolic-enriched kenaf (Hibiscus cannabinus L.) seeds by a pulsed ultrasonic-assisted extraction. The antioxidant activities of ultrasonic-assisted kenaf seed extracts (KSE) were determined by a 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging capacity assay, 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid) (ABTS) radical scavenging assay, β -carotene bleaching inhibition assay, and ferric reducing antioxi...

  15. A short review of headspace extraction and ultrasonic solvent extraction for honey volatiles fingerprinting

    Directory of Open Access Journals (Sweden)

    Z. Marijanović

    2009-01-01

    Full Text Available Honey volatiles exhibit a potential role in distinguishing honeys as a function of botanical origin, but heating of honey generates artefacts such as compounds of Strecker degradation and Maillard reaction products. This short review is focused on the most recently applied methods for honey volatiles fingerprinting (without generation of thermal artefacts: headspace extraction (dynamic headspace extraction (DHE, headspace solid-phase microextraction (HS-SPME and ultrasonic solvent extraction (USE. These methods display a varying degree of selectivity and effectiveness depending upon the compounds involved and the extraction conditions. Recent developments of these methods are discussed, with application examples drawn from the literature as well from our own research. Flavour qualities of the honey are very much dependent on the volatile and semivolatile organic compounds present in both the sample matrix and the headspace aroma. Therefore the use of one single technique is not adequate for reliable honey volatiles profiling, but combined use of headspace extraction and ultrasonic solvent extraction could be a useful tool for the characterization of the honey and identification of its botanical source through typical volatile marker compounds.

  16. Comparison of Enzymatic and Ultrasonic Extraction of Albumin from Defatted Pumpkin (Cucurbita pepo Seed Powder

    Directory of Open Access Journals (Sweden)

    Gia Loi Tu

    2015-01-01

    Full Text Available In this study, ultrasound- and enzyme-assisted extractions of albumin (water-soluble protein group from defatted pumpkin (Cucurbita pepo seed powder were compared. Both advanced extraction techniques strongly increased the albumin yield in comparison with conventional extraction. The extraction rate was two times faster in the ultrasonic extraction than in the enzymatic extraction. However, the maximum albumin yield was 16 % higher when using enzymatic extraction. Functional properties of the pumpkin seed albumin concentrates obtained using the enzymatic, ultrasonic and conventional methods were then evaluated. Use of hydrolase for degradation of cell wall of the plant material did not change the functional properties of the albumin concentrate in comparison with the conventional extraction. The ultrasonic extraction enhanced water-holding, oil-holding and emulsifying capacities of the pumpkin seed albumin concentrate, but slightly reduced the foaming capacity, and emulsion and foam stability.

  17. Air-Coupled Low Frequency Ultrasonic Transducers and Arrays with PMN-32%PT Piezoelectric Crystals

    Directory of Open Access Journals (Sweden)

    Rymantas J. Kazys

    2017-01-01

    Full Text Available Air-coupled ultrasonic techniques are being increasingly used for material characterization, non-destructive evaluation of composite materials using guided waves as well as for distance measurements. Application of those techniques is mainly limited by the big losses of ultrasonic signals due to attenuation and mismatch of the acoustic impedances of ultrasonic transducers and air. One of the ways to solve this problem is by application of novel more efficient piezoelectric materials like lead magnesium niobate-lead titanate (PMN-PT type crystals. The objective of this research was the development and investigation of low frequency (<50 kHz wide band air-coupled ultrasonic transducers and arrays with an improved performance using PMN-32%PT crystals. Results of finite element modelling and experimental investigations of the developed transducers and arrays are presented. For improvement of the performance strip-like matching elements made of low acoustic impedance, materials such as polystyrene foams were applied. It allowed to achieve transduction losses for one single element transducer −11.4 dB, what is better than of commercially available air-coupled ultrasonic transducers. Theoretical and experimental investigations of the acoustic fields radiated by the eight element ultrasonic array demonstrated not only a good performance of the array in a pulse mode, but also very good possibilities to electronically focus and steer the ultrasonic beam in space.

  18. Ultrasonic-assisted extraction and in vitro antioxidant activity of polysaccharides from Agaricus bisporus.

    Science.gov (United States)

    Qiao, De-Liang; Zhao, Feng; Huang, Hai-Zhong; Fan, Chun-Chun; Han, Lei

    2012-08-01

    To optimize ultrasonic-assisted extraction parameters of polysaccharides from Agaricus bisporus and evaluate antioxidant activities of A. bisporus polysaccharides. Polysaccharides from A. bisporus was extracted by using methods of ultrasonic-assisted hot water lixiviation, ethanol precipitation, Sevag's deproteination and ethanol precipitation again. Extraction temperature, extraction time, ratio of water to raw material and ultrasonic power were selected in single-factor tests. Based on the single-factor tests, parameters combination for the ultrasonic-assisted extraction of A. bisporus polysaccharides was optimized by using four-factor-three-level orthogonal test. Antioxidant activities (reductive potential, superoxide anion scavenging activity and H2O2 scavenging activity) of A. bisporus polysaccharides were evaluated in vitro. Optimum conditions for the extracting of A. bisporus polysaccharides were extracting temperature 65 degrees C, extracting time 40 min, ratio of water to raw material 30 mL/g and ultrasonic power 170 w. Practicing this optimal condition, extraction yield of polysaccharides from A. bisporus was 5.6 014%. In crude polysaccharides of A. bisporus, carbohydrates content, determined by applying the phenol-sulfuric acid method, was 75.48%. Polysaccharides of A. bisporus could reduce ferric ion, scavenge superoxide anion and hydrogen peroxide in a dose-dependent manner. Utrasonic-assisted extraction could be used in the extracting of A. bisporus polysaccharides. Polysaccharides of A. bisporus, had direct and potent antioxidant activities, might be developed and utilized as natural antioxidant.

  19. Comparison of two methods of surface profile extraction from multiple ultrasonic range measurements

    NARCIS (Netherlands)

    Barshan, B; Baskent, D

    Two novel methods for surface profile extraction based on multiple ultrasonic range measurements are described and compared. One of the methods employs morphological processing techniques, whereas the other employs a spatial voting scheme followed by simple thresholding. Morphological processing

  20. Study on the extraction of dioscin by the ultrasonic- assisted ethanol

    African Journals Online (AJOL)

    aghomotsegin

    2014-02-19

    Feb 19, 2014 ... 1Shaanxi University of Science and Technology, Key laboratory of Auxiliary ... the effect on extraction yield of dioscin of frequency of ultrasonic, the period of ..... steroidal saponins on Taiwanese yam cultivar (Dioscorea.

  1. Optimization design and application of composite ultrasonic extraction method for effective constituents of green tea

    Directory of Open Access Journals (Sweden)

    Cheng-Chi Wang

    2015-12-01

    Full Text Available A composite ultrasonic process is used to extract five constituent components of green tea, namely caffeine, catechin, epigallocatechin gallate, epicatechin, and chlorogenic acid. The optimal parameters of the extraction process are determined using the robust Taguchi design method. The extracted products are analyzed using gas chromatography and high-performance liquid chromatography. The experimental results confirm the effectiveness of the proposed ultrasonic technique in extracting the components of interest. Moreover, it is shown that the optimal extraction parameters depend on the particular component. In general, the present findings provide a useful reference for further research on the processing of green tea.

  2. New method to enhance the extraction yield of rutin from Sophora japonica using a novel ultrasonic extraction system by determining optimum ultrasonic frequency.

    Science.gov (United States)

    Liao, Jianqing; Qu, Baida; Liu, Da; Zheng, Naiqin

    2015-11-01

    A new method has been proposed for enhancing extraction yield of rutin from Sophora japonica, in which a novel ultrasonic extraction system has been developed to perform the determination of optimum ultrasonic frequency by a two-step procedure. This study has systematically investigated the influence of a continuous frequency range of 20-92 kHz on rutin yields. The effects of different operating conditions on rutin yields have also been studied in detail such as solvent concentration, solvent to solid ratio, ultrasound power, temperature and particle size. A higher extraction yield was obtained at the ultrasonic frequency of 60-62 kHz which was little affected under other extraction conditions. Comparative studies between existing methods and the present method were done to verify the effectiveness of this method. Results indicated that the new extraction method gave a higher extraction yield compared with existing ultrasound-assisted extraction (UAE) and soxhlet extraction (SE). Thus, the potential use of this method may be promising for extraction of natural materials on an industrial scale in the future. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Mapping of an ultrasonic bath for ultrasound assisted extraction of mangiferin from Mangifera indica leaves.

    Science.gov (United States)

    Kulkarni, Vrushali M; Rathod, Virendra K

    2014-03-01

    The present work deals with the mapping of an ultrasonic bath for the maximum extraction of mangiferin from Mangifera indica leaves. I3(-) liberation experiments (chemical transformations) and extraction (physical transformations) were carried out at different locations in an ultrasonic bath and compared. The experimental findings indicated a similar trend in variation in an ultrasonic bath by both these methods. Various parameters such as position and depth of vessel in an ultrasonic bath, diameter and shape of a vessel, frequency and input power which affect the extraction yield have been studied in detail. Maximum yield of mangiferin obtained was approximately 31 mg/g at optimized parameters: distance of 2.54 cm above the bottom of the bath, 7 cm diameter of vessel, flat bottom vessel, 6.35 cm liquid height, 122 W input power and 25 kHz frequency. The present work indicates that the position and depth of vessel in an ultrasonic bath, diameter and shape of a vessel, frequency and input power have significant effect on the extraction yield. This work can be used as a base for all ultrasonic baths to obtain maximum efficiency for ultrasound assisted extraction. Copyright © 2013 Elsevier B.V. All rights reserved.

  4. Response surface optimization of the ultrasonic-assisted extraction of edible brown pigment from Macadamia shells

    Science.gov (United States)

    Liu, Y. Y.; Liu, Y. J.; Gong, X.; Li, J. H.

    2017-09-01

    The ultrasonic extraction of Edible brown pigment from macadamia shells was researched using response surface methodology (RSM) with 3 factors and 3 levels. A Box-Behnken design (BBD) was employed to investigate the effects of Solvent concentration, ratio of water to raw material and extraction time on the extraction yield of brown pigment. By using this new method, the optimum extraction condition was obtained as follows: Ultrasonic treating time 71 min, solvent to sample ratio of 23 mL/g, Alcohol concentrations 62%. Under the optimized condition, the experimental yield of brown pigment was 0.636g.

  5. Optimization of ultrasonic extraction of phenolic antioxidants from green tea using response surface methodology.

    Science.gov (United States)

    Lee, Lan-Sook; Lee, Namhyouck; Kim, Young Ho; Lee, Chang-Ho; Hong, Sang Pil; Jeon, Yeo-Won; Kim, Young-Eon

    2013-10-31

    Response surface methodology (RSM) has been used to optimize the extraction conditions of antioxidants with relatively low caffeine content from green tea by using ultrasonic extraction. The predicted optimal conditions for the highest antioxidant activity and minimum caffeine level were found at 19.7% ethanol, 26.4 min extraction time, and 24.0 ° C extraction temperature. In the predicted optimal conditions, the experimental values were very close to the predicted values. Moreover, the ratio of (EGCg + ECg)/EGC was identified a major factor contributing to the antioxidant activity of green tea extracts. In this study, ultrasonic extraction showed that the ethanol concentration and extraction time used for antioxidant extraction could be remarkably reduced without a decrease in antioxidant activity compared to the conventional extraction conditions.

  6. Optimization of Ultrasonic Extraction of Phenolic Antioxidants from Green Tea Using Response Surface Methodology

    Directory of Open Access Journals (Sweden)

    Lan-Sook Lee

    2013-10-01

    Full Text Available Response surface methodology (RSM has been used to optimize the extraction conditions of antioxidants with relatively low caffeine content from green tea by using ultrasonic extraction. The predicted optimal conditions for the highest antioxidant activity and minimum caffeine level were found at 19.7% ethanol, 26.4 min extraction time, and 24.0 °C extraction temperature. In the predicted optimal conditions, the experimental values were very close to the predicted values. Moreover, the ratio of (EGCg + ECg/EGC was identified a major factor contributing to the antioxidant activity of green tea extracts. In this study, ultrasonic extraction showed that the ethanol concentration and extraction time used for antioxidant extraction could be remarkably reduced without a decrease in antioxidant activity compared to the conventional extraction conditions.

  7. Application of ultrasonic extraction method in the preparation of the directive action beverage from black currant

    Directory of Open Access Journals (Sweden)

    N. S. Rodionova

    2016-01-01

    Full Text Available The article presents the results of experimental determination of physical-and chemical parameters, the amount of anthocyanins, the definition of color and organoleptic characteristics of the beverage prepared with ultrasonic extraction method in comparison with the fruit-drink, obtained according to traditional recipe. Black currant was chosen the main raw material for the development of the beverage production technology. It is characterized by a high content of bioactive components that increase the adaptive abilities of human body. The purpose is to use ultrasonic extraction method in the preparation of functionally directed actions beverages. Extractor with submerged ultrasonic emitter was used as an experimental device. The essence of its operation is as follows: a mixture of the extractant and the plant substrate in different ratios was loaded into a container with the emitter, then the ultrasonic generator was turned on. The vibrations of ultrasonic frequency (22 kHz made high-frequency mechanical vibrations that caused the formation of intense cavitation areas and diffuse dissolution of cell substrates in the extractant in the treated mixture. The ultrasonic extraction technique involves brief contact of berries and extractant (up to 15 minutes upon application of ultrasonic vibrations. With an increase in exposure time, the yield of biologically active substances increases to reach an equilibrium state corresponding to the most complete exhaustion of raw materials. All this leads to a significant acceleration of the transition from the active ingredients from the raw materials into the extractant to obtain a product with improved physical - and chemical, organoleptic characteristics, as well as a higher antioxidant activity.

  8. Influence of Ultrasonic Vibrations on the Static Friction Characteristics of a Rubber/Aluminum Couple

    International Nuclear Information System (INIS)

    Cheng Ting-Hai; Gao Han; Bao Gang

    2011-01-01

    A novel ultrasonic vibration approach is introduced into a chloroprene rubber/aluminum friction couple for improving the static friction properties between rubber and metal. Compared to the test results without vibrations, the static friction force of a chloroprene rubber/aluminum couple decreases observably, leading to the ultimate displacement of rubber. The values of the static friction force and ultimate displacement can be ultimately reduced to 23.1% and 50% of those without ultrasonic vibrations, respectively. (fundamental areas of phenomenology(including applications))

  9. Quality Parameters of Curcuma Longa L. Extracts by Supercritical Fluid Extraction (SFE) and Ultrasonic Assisted Extraction (UAE)

    International Nuclear Information System (INIS)

    Zaibunnisa Abdul Haiyee; Siti Hafsah Mohd Shah; Khudzir Ismail; Nooraain Hashim; Wan Iryani Wan Ismail

    2016-01-01

    Turmeric is one of the prominently use herbal plants due to its diverse beneficial effects especially in Indian medicine. The rhizome part of the turmeric contains valuable compounds which have been said to owe its antimicrobial effects, anti-cancer, anti-inflammatory and enhance wound healing. Due to its short-life span and perishable properties, the conversion of the rhizome into turmeric extract is desirable. Several methods have been used for extraction such as Soxhlet extraction and pressurized liquid extraction (PLE). However, these techniques are tedious, laborious, time consuming and involves the usage of toxic organic solvent, of which safeness of the end product is doubtful. In this study, a rapid, reliable and green extraction method of supercritical fluid extraction (SFE) and ultrasonic assisted extraction (UAE) were used. SFE without modifier has resulted in 0.0006 mg/ 100 g of curcuminoids concentration and 5.62 % of yield (dry weight basis). UAE using ethanol was able to produce significantly the highest yield (6.40 %, dry weight basis) and the highest curcuminoids concentration (0.1020 mg/ 100 g). However, SFE was able to produce extract that contain significantly higher major volatile compounds; tumerone, ar-turmerone and curlone. Therefore, this study proves that both extraction methods were able to produce high quality turmeric extract. (author)

  10. Optimization of Ultrasonic Extraction of Phenolic Antioxidants from Green Tea Using Response Surface Methodology

    OpenAIRE

    Lee, Lan-Sook; Lee, Namhyouck; Kim, Young; Lee, Chang-Ho; Hong, Sang; Jeon, Yeo-Won; Kim, Young-Eon

    2013-01-01

    Response surface methodology (RSM) has been used to optimize the extraction conditions of antioxidants with relatively low caffeine content from green tea by using ultrasonic extraction. The predicted optimal conditions for the highest antioxidant activity and minimum caffeine level were found at 19.7% ethanol, 26.4 min extraction time, and 24.0 °C extraction temperature. In the predicted optimal conditions, the experimental values were very close to the predicted values. Moreover, the ratio ...

  11. Optimization of Ultrasonic-Assisted Extraction of Cordycepin from Cordyceps militaris Using Orthogonal Experimental Design

    Directory of Open Access Journals (Sweden)

    Hsiu-Ju Wang

    2014-12-01

    Full Text Available This study reports on the optimization of the extraction conditions of cordycepin from Cordyceps militaris by using ultrasonication. For this purpose, the orthogonal experimental design was used to investigate the effects of factors on the ultrasonic-assisted extraction (UAE. Four factors: extraction time (min, ethanol concentration (%, extraction temperature (°C and extraction frequency (kHz, were studied. The results showed that the highest cordycepin yield of 7.04 mg/g (86.98% ± 0.23% was obtained with an extraction time of 60 min, ethanol concentration of 50%, extraction temperature of 65 °C and extraction frequency of 56 kHz. It was found that the cordycepin extraction yield increased with the effect of ultrasonication during the extraction process. Therefore, UAE can be used as an alternative to conventional immersion extraction with respect to the recovery of cordycepin from C. militaris, with the advantages of shorter extraction time and reduced solvent consumption.

  12. Optimization of ultrasonic-assisted extraction of pomegranate (Punica granatum L.) seed oil.

    Science.gov (United States)

    Tian, Yuting; Xu, Zhenbo; Zheng, Baodong; Martin Lo, Y

    2013-01-01

    The effectiveness of ultrasonic-assisted extraction (UAE) of pomegranate seed oil (PSO) was evaluated using a variety of solvents. Petroleum ether was the most effective for oil extraction, followed by n-hexane, ethyl acetate, diethyl ether, acetone, and isopropanol. Several variables, such as ultrasonic power, extraction temperature, extraction time, and the ratio of solvent volume and seed weight (S/S ratio) were studied for optimization using response surface methodology (RSM). The highest oil yield, 25.11% (w/w), was obtained using petroleum ether under optimal conditions for ultrasonic power, extraction temperature, extraction time, and S/S ratio at 140 W, 40 °C, 36 min, and 10 ml/g, respectively. The PSO yield extracted by UAE was significantly higher than by using Soxhlet extraction (SE; 20.50%) and supercriti cal fluid extraction (SFE; 15.72%). The fatty acid compositions were significantly different among the PSO extracted by Soxhlet extraction, SFE, and UAE, with punicic acid (>65%) being the most dominant using UAE. Copyright © 2012 Elsevier B.V. All rights reserved.

  13. [Mass Transfer Kinetics Model of Ultrasonic Extraction of Pomegranate Peel Polyphenols].

    Science.gov (United States)

    Wang, Zhan-yi; Zhang, Li-hua; Wang, Yu-hai; Zhang, Yuan-hu; Ma, Li; Zheng, Dan-dan

    2015-05-01

    The dynamic mathematical model of ultrasonic extraction of polyphenols from pomegranate peel was constructed with the Fick's second law as the theoretical basis. The spherical model was selected, with mass concentrations of pomegranate peel polyphenols as the index, 50% ethanol as the extraction solvent and ultrasonic extraction as the extraction method. In different test conditions including the liquid ratio, extraction temperature and extraction time, a series of kinetic parameters were solved, such as the extraction process (k), relative raffinate rate, surface diffusion coefficient(D(S)), half life (t½) and the apparent activation energy (E(a)). With the extraction temperature increasing, k and D(S) were gradually increased with t½ decreasing,which indicated that the elevated temperature was favorable to the extraction of pomegranate peel polyphenols. The exponential equation of relative raffinate rate showed that the established numerical dynamics model fitted the extraction of pomegranate peel polyphenols, and the relationship between the reaction conditions and pomegranate peel polyphenols concentration was well reflected by the model. Based on the experimental results, a feasible and reliable kinetic model for ultrasonic extraction of polyphenols from pomegranate peel is established, which can be used for the optimization control of engineering magnifying production.

  14. ULTRASONIC NEBULIZATION AND ARSENIC VALENCE STATE CONSIDERATIONS PRIOR TO DETERMINATION VIA INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY

    Science.gov (United States)

    An ultrasonic nebulizer (USN) was utilized as a sample introduction device for an inductively coupled plasma mass spectrometer in an attempt to increase the sensitivity for As. The USN produced a valence state response difference for As. The As response was suppressed approximate...

  15. Optimization Extracting Technology of Cynomorium songaricum Rupr. Saponins by Ultrasonic and Determination of Saponins Content in Samples with Different Source

    OpenAIRE

    Xiaoli Wang; Qingwei Wei; Xinqiang Zhu; Chunmei Wang; Yonggang Wang; Peng Lin; Lin Yang

    2015-01-01

    Extraction process was optimized by single factor and orthogonal experiment (L9 (34)). Moreover, the content determination was studied in methodology. The optimum ultrasonic extraction conditions were: ethanol concentration of 75%, ultrasonic power of 420 w, the solid-liquid ratio of 1:15, extraction duration of 45 min, extraction temperature of 90°C and extraction for 2 times. Saponins content in Guazhou samples was significantly higher than those in Xinjiang and Inner Mongolia. Meanwhile, G...

  16. Liquid-phase extraction coupled with metal-organic frameworks-based dispersive solid phase extraction of herbicides in peanuts.

    Science.gov (United States)

    Li, Na; Wang, Zhibing; Zhang, Liyuan; Nian, Li; Lei, Lei; Yang, Xiao; Zhang, Hanqi; Yu, Aimin

    2014-10-01

    Liquid-phase extraction coupled with metal-organic frameworks-based dispersive solid phase extraction was developed and applied to the extraction of pesticides in high fatty matrices. The herbicides were ultrasonically extracted from peanut using ethyl acetate as extraction solvent. The separation of the analytes from a large amount of co-extractive fat was achieved by dispersive solid-phase extraction using MIL-101(Cr) as sorbent. In this step, the analytes were adsorbed on MIL-101(Cr) and the fat remained in bulk. The herbicides were separated and determined by high-performance liquid chromatography. The experimental parameters, including type and volume of extraction solvent, ultrasonication time, volume of hexane and eluting solvent, amount of MIL-101(Cr) and dispersive solid phase extraction time, were optimized. The limits of detection for herbicides range from 0.98 to 1.9 μg/kg. The recoveries of the herbicides are in the range of 89.5-102.7% and relative standard deviations are equal or lower than 7.0%. The proposed method is simple, effective and suitable for treatment of the samples containing high content of fat. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. Optimization of focused ultrasonic extraction of propellant components determined by gas chromatography/mass spectrometry.

    Science.gov (United States)

    Fryš, Ondřej; Česla, Petr; Bajerová, Petra; Adam, Martin; Ventura, Karel

    2012-09-15

    A method for focused ultrasonic extraction of nitroglycerin, triphenyl amine and acetyl tributyl citrate presented in double-base propellant samples following by the gas chromatography/mass spectrometry analysis was developed. A face-centered central composite design of the experiments and response surface modeling was used for optimization of the time, amplitude and sample amount. The dichloromethane was used as the extractant solvent. The optimal extraction conditions with respect to the maximum yield of the lowest abundant compound triphenyl amine were found at the 20 min extraction time, 35% amplitude of ultrasonic waves and 2.5 g of the propellant sample. The results obtained under optimal conditions were compared with the results achieved with validated Soxhlet extraction method, which is typically used for isolation and pre-concentration of compounds from the samples of explosives. The extraction yields for acetyl tributyl citrate using both extraction methods were comparable; however, the yield of ultrasonic extraction of nitroglycerin and triphenyl amine was lower than using Soxhlet extraction. The possible sources of different extraction yields are estimated and discussed. Copyright © 2012 Elsevier B.V. All rights reserved.

  18. The use of ultrasonic instrumentation in liquid/liquid extraction plant

    International Nuclear Information System (INIS)

    Asher, R.C.; Bradshaw, L.; Tolchard, A.C.

    1984-01-01

    Ultrasonic instruments can be used to determine many of the parameters of interest in a liquid/liquid extraction plant, eg liquid levels, the position of interfaces between immiscible liquids and the concentration of solutions. The determinations can often be made non-invasively. A number of instruments developed for a liquid/liquid extraction plant used for nuclear fuel reprocessing is described. These instruments have a wider application in liquid/liquid extraction plant in general. (author)

  19. A transmission and reflection coupled ultrasonic process tomography based on cylindrical miniaturized transducers using PVDF films

    Science.gov (United States)

    Gu, J.; Yang, H.; Fan, F.; Su, M.

    2017-12-01

    A transmission and reflection coupled ultrasonic process tomography has been developed, which is characterized by a proposed dual-mode (DM) reconstruction algorithm, as well as an adaptive search approach to determine an optimal image threshold during the image binarization. In respect of hardware, to improve the accuracy of time-of-flight (TOF) and extend the lowest detection limit of particle size, a cylindrical miniaturized transducer using polyvinylidene fluoride (PVDF) films is designed. Besides, the development of range-gating technique for the identification of transmission and reflection waves in scanning is discussed. A particle system with four iron particles is then investigated numerically and experimentally to evaluate these proposed methods. The sound pressure distribution in imaging area is predicted numerically, followed by the analysis of the relationship between the emitting surface width of transducer and particle size. After the processing of experimental data for effective waveform extraction and fusion, the comparison between reconstructed results from transmission-mode (TM), reflection-mode (RM), and dual-mode reconstructions is carried out and the latter manifests obvious improvements from the blurring reduction to the enhancement of particle boundary.

  20. Noncontact ultrasonic nondestructive evaluation/inspection using laser generation and air coupled transducer

    International Nuclear Information System (INIS)

    Jhang, Kyung Young; Kim, Hong Joon; Cemiglia, Donatella; Djordjevic, Boro

    2001-01-01

    Ultrasonic MDE/I methods have been demonstrated as very effective tool in characterization of cracks and structural defects such as bond-line failures. Most of the ultrasonic testing is performed using conventional contact ultrasonic transducers that cannot be readily adapted to automation and field application. However, for large area inspection contact type is time consuming and as a result, it is important to develop a rapid and more efficient ultrasonic technique. In this paper, laser generation and air-coupled detection of ultrasound is proposed as a solution of non-contact method with no requirement of a coupling medium, and the bond quality of adhesively bonded and riveted aluminum lap splice joints is investigated as an application. A Q-switched Nd:YAG laser and a periodic transmission mask are used to generate a selected Lamb mode. The experimental show that multi-line laser source produces significant directed ultrasound and that the presence of defects can be detected reliably from the attenuation of signal amplitude. These results demonstrate that the proposed technique is well suitable and flexible for non-contact NDE/I applications.

  1. Ultrasonically assisted extraction of calcium and ash from char

    Science.gov (United States)

    Mathumba, E. E.; Mbaya, R. K. K.; Kolesnikov, A.

    2018-03-01

    This study characterized and removed calcium and ash content from char to improve the chemical quality of char as reductant for titanium smelting application. Calcium in char can be classified in two parts: mineral matter and cationic metals associated with organic matrix. Virgin and chemically treated char was characterized by using ISO 1171, wet chemistry methods, ISO 19579, XRF, and B.E.T. methods. In this present work, demineralization of char with mild chemical leachants such as acetic acid, citric acid, gluconic acid and Ethylene Diamine Tetra Acetic acid with three different ultrasonic power input (150 W, 270 W and 300 W) and semi-dual frequency of 40 kHz tank was investigated. Actual power dissipated into the system was calculated from the calorimetric measurement. An optimum set of process parameters are identified and validated. The ultrasound technology was compared with soaking technology to determine the efficiency of ultrasound system for the removal of calcium. The removal of calcium was exponentially higher with ultrasonic treatment than without it. Results revealed that mild chemical reagents do not harm the carbon content of char. It is evident from the results that amongst the leachants used; acetic and citric acid has caused significant removal of mineral phases.

  2. Binary solvent extraction system and extraction time effects on phenolic antioxidants from kenaf seeds (Hibiscus cannabinus L.) extracted by a pulsed ultrasonic-assisted extraction.

    Science.gov (United States)

    Wong, Yu Hua; Lau, Hwee Wen; Tan, Chin Ping; Long, Kamariah; Nyam, Kar Lin

    2014-01-01

    The aim of this study was to determine the best parameter for extracting phenolic-enriched kenaf (Hibiscus cannabinus L.) seeds by a pulsed ultrasonic-assisted extraction. The antioxidant activities of ultrasonic-assisted kenaf seed extracts (KSE) were determined by a 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging capacity assay, 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid) (ABTS) radical scavenging assay, β -carotene bleaching inhibition assay, and ferric reducing antioxidant power (FRAP) assay. Total phenolic content (TPC) and total flavonoid content (TFC) evaluations were carried out to determine the phenolic and flavonoid contents in KSE. The KSE from the best extraction parameter was then subjected to high performance liquid chromatography (HPLC) to quantify the phenolic compounds. The optimised extraction condition employed 80% ethanol for 15 min, with the highest values determined for the DPPH, ABTS, and FRAP assay. KSE contained mainly tannic acid (2302.20 mg/100 g extract) and sinapic acid (1198.22 mg/100 g extract), which can be used as alternative antioxidants in the food industry.

  3. Binary Solvent Extraction System and Extraction Time Effects on Phenolic Antioxidants from Kenaf Seeds (Hibiscus cannabinus L.) Extracted by a Pulsed Ultrasonic-Assisted Extraction

    Science.gov (United States)

    Lau, Hwee Wen; Nyam, Kar Lin

    2014-01-01

    The aim of this study was to determine the best parameter for extracting phenolic-enriched kenaf (Hibiscus cannabinus L.) seeds by a pulsed ultrasonic-assisted extraction. The antioxidant activities of ultrasonic-assisted kenaf seed extracts (KSE) were determined by a 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging capacity assay, 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid) (ABTS) radical scavenging assay, β-carotene bleaching inhibition assay, and ferric reducing antioxidant power (FRAP) assay. Total phenolic content (TPC) and total flavonoid content (TFC) evaluations were carried out to determine the phenolic and flavonoid contents in KSE. The KSE from the best extraction parameter was then subjected to high performance liquid chromatography (HPLC) to quantify the phenolic compounds. The optimised extraction condition employed 80% ethanol for 15 min, with the highest values determined for the DPPH, ABTS, and FRAP assay. KSE contained mainly tannic acid (2302.20 mg/100 g extract) and sinapic acid (1198.22 mg/100 g extract), which can be used as alternative antioxidants in the food industry. PMID:24592184

  4. Binary Solvent Extraction System and Extraction Time Effects on Phenolic Antioxidants from Kenaf Seeds (Hibiscus cannabinus L. Extracted by a Pulsed Ultrasonic-Assisted Extraction

    Directory of Open Access Journals (Sweden)

    Yu Hua Wong

    2014-01-01

    Full Text Available The aim of this study was to determine the best parameter for extracting phenolic-enriched kenaf (Hibiscus cannabinus L. seeds by a pulsed ultrasonic-assisted extraction. The antioxidant activities of ultrasonic-assisted kenaf seed extracts (KSE were determined by a 2,2-diphenyl-1-picrylhydrazyl (DPPH radical scavenging capacity assay, 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid (ABTS radical scavenging assay, β-carotene bleaching inhibition assay, and ferric reducing antioxidant power (FRAP assay. Total phenolic content (TPC and total flavonoid content (TFC evaluations were carried out to determine the phenolic and flavonoid contents in KSE. The KSE from the best extraction parameter was then subjected to high performance liquid chromatography (HPLC to quantify the phenolic compounds. The optimised extraction condition employed 80% ethanol for 15 min, with the highest values determined for the DPPH, ABTS, and FRAP assay. KSE contained mainly tannic acid (2302.20 mg/100 g extract and sinapic acid (1198.22 mg/100 g extract, which can be used as alternative antioxidants in the food industry.

  5. Air-Coupled Ultrasonic Receivers with High Electromechanical Coupling PMN-32%PT Strip-Like Piezoelectric Elements

    Directory of Open Access Journals (Sweden)

    Rymantas J. Kazys

    2017-10-01

    Full Text Available For improvement of the efficiency of air-coupled ultrasonic transducers PMN-32%PT piezoelectric crystals which possess very high piezoelectric properties may be used. The electromechanical coupling factor of such crystals for all main vibration modes such as the thickness extension and transverse extension modes is more than 0.9. Operation of ultrasonic transducers with such piezoelectric elements in transmitting and receiving modes is rather different. Therefore, for transmission and reception of ultrasonic signals, separate piezoelectric elements with different dimensions must be used. The objective of this research was development of novel air-coupled ultrasonic receivers with PMN-32%PT strip-like piezoelectric elements vibrating in a transverse-extension mode with electromechanically controlled operation and suitable for applications in ultrasonic arrays. Performance of piezoelectric receivers made of the PMN-32%PT strip-like elements vibrating in this mode may be efficiently controlled by selecting geometry of the electrodes covering side surfaces of the piezoelectric element. It is equivalent to introduction of electromechanical damping which does not require any additional backing element. For this purpose; we have proposed the continuous electrodes to divide into two pairs of electrodes. The one pair is used to pick up the electric signal; another one is exploited for electromechanical damping. Two types of electrodes may be used—rectangular or non-rectangular—with a gap between them directed at some angle, usually 45°. The frequency bandwidth is wider (up to 9 kHz in the case of non-rectangular electrodes. The strip-like acoustic matching element bonded to the tip of the PMN-32%PT crystal may significantly enhance the performance of the ultrasonic receiver. It was proposed to use for this purpose AIREX T10.110 rigid polymer foam, the acoustic impedance of which is close to the optimal value necessary for matching with air. It was

  6. A comparison of accelerated solvent extraction, Soxhlet extraction, and ultrasonic-assisted extraction for analysis of terpenoids and sterols in tobacco.

    Science.gov (United States)

    Shen, Jinchao; Shao, Xueguang

    2005-11-01

    The performance of accelerated solvent extraction in the analysis of terpenoids and sterols in tobacco samples was investigated and compared with those of Soxhlet extraction and ultrasonically assisted extraction with respect to yield, extraction time, reproducibility and solvent consumption. The results indicate that although the highest yield was achieved by Soxhlet extraction, ASE appears to be a promising alternative to classical methods since it is faster and uses less solvent, especially when applied to the investigation of large batch tobacco samples. However, Soxhlet extraction is still the preferred method for analyzing sterols since it gives a higher extraction efficiency than other methods.

  7. Ultrasonic Extraction of Antioxidants from Chinese Sumac (Rhus typhina L.) Fruit Using Response Surface Methodology and Their Characterization

    OpenAIRE

    Lai, Jixiang; Wang, Huifang; Wang, Donghui; Fang, Fang; Wang, Fengzhong; Wu, Tao

    2014-01-01

    For the first time, response surface methodology (RSM) using a Box-Behnken Design (BBD) was employed to optimize the conditions for ultrasonic assisted extraction (UAE) of antioxidants from Chinese sumac (Rhus typhina L.) fruits. Initially, influencing factors such as liquid-solid ratio, duration of ultrasonic assisted extraction, pH range, extraction temperature and ethanol concentration were identified using single-factor experiments. Then, with respect to the three most significant influen...

  8. Comparison of Enzymatic and Ultrasonic Extraction of Albumin from Defatted Pumpkin (Cucurbita pepo)
Seed Powder.

    Science.gov (United States)

    Tu, Gia Loi; Bui, Thi Hoang Nga; Tran, Thi Thu Tra; Ton, Nu Minh Nguyet; Man Le, Van Viet

    2015-12-01

    In this study, ultrasound- and enzyme-assisted extractions of albumin (water-soluble protein group) from defatted pumpkin ( Cucurbita pepo ) seed powder were compared. Both advanced extraction techniques strongly increased the albumin yield in comparison with conventional extraction. The extraction rate was two times faster in the ultrasonic extraction than in the enzymatic extraction. However, the maximum albumin yield was 16% higher when using enzymatic extraction. Functional properties of the pumpkin seed albumin concentrates obtained using the enzymatic, ultrasonic and conventional methods were then evaluated. Use of hydrolase for degradation of cell wall of the plant material did not change the functional properties of the albumin concentrate in comparison with the conventional extraction. The ultrasonic extraction enhanced water-holding, oil-holding and emulsifying capacities of the pumpkin seed albumin concentrate, but slightly reduced the foaming capacity, and emulsion and foam stability.

  9. Antiproliferative activity of Curcuma phaeocaulis Valeton extract using ultrasonic assistance and response surface methodology.

    Science.gov (United States)

    Wang, Xiaoqin; Jiang, Ying; Hu, Daode

    2017-01-02

    The objective of the study was to optimize the ultrasonic-assisted extraction of curdione, furanodienone, curcumol, and germacrone from Curcuma phaeocaulis Valeton (Val.) and investigate the antiproliferative activity of the extract. Under the suitable high-performance liquid chromatography condition, the calibration curves for these four tested compounds showed high levels of linearity and the recoveries of these four compounds were between 97.9 and 104.3%. Response surface methodology (RSM) combining central composite design and desirability function (DF) was used to define optimal extraction parameters. The results of RSM and DF revealed that the optimum conditions were obtained as 8 mL g -1 for liquid-solid ratio, 70% ethanol concentration, and 20 min of ultrasonic time. It was found that the surface structures of the sonicated herbal materials were fluffy and irregular. The C. phaeocaulis Val. extract significantly inhibited the proliferation of RKO and HT-29 cells in vitro. The results reveal that the RSM can be effectively used for optimizing the ultrasonic-assisted extraction of bioactive components from C. phaeocaulis Val. for antiproliferative activity.

  10. Biochemical Characterization of Tunisian Cichorium Intybus L. Roots and Optimization of Ultrasonic Inulin Extraction

    Directory of Open Access Journals (Sweden)

    Youkabed Ouederni Zarroug

    2016-11-01

    Full Text Available In this study Cichorium intybus L. roots were tested for its chemical composition, antioxidant activity, and phenolic profile. Optimization of ultrasonic inulin extraction using response surface methodology (RSM was further investigated. Chicory roots were found to have high value of total carbohydrates (70.43%, soluble fiber (66.93, Neutral detergent fiber (NDF (33.07%, potassium (380 mg/100g, calcium (540 mg/100g and sodium (140 mg/100g. Chicory roots exhibit a high content of flavonoids, polyphenols, and tannins. Antioxidant activity measurement reveals the capacity of Chicory roots to scavenge diphenylpicrylhydrazyl (DPPH radicals. Phenolic acids profile shows the abundance of vanillic acid (19.64% followed by protocatechuic acid (15.67%. The effect of three independent variables namely extraction time, the ratio of water to raw material and temperature on inulin extraction was studied. Optimum deciding responses were Inulin content, Total Soluble Solids (TSS content and Water produced inulin yield. The optimal ultrasonic extraction conditions were: extraction time 87 min, liquid to solid ratio 38 (ml/g and ultrasonic temperature 61 ̊ C. Under these conditions, the inulin content, TSS content and produced inulin yield were 35.92%, 24.72%, and 32.53%, respectively. The produced inulin was characterized by the Fourier infrared transformation (FTIR and observed by means of scanning electron microscopy (SEM.  

  11. Effect of Ultrasonic-Assisted Extraction on Phenolic Content of Avocado

    International Nuclear Information System (INIS)

    Rafidah Husen; Andou, Y.; Amin Ismail; Shirai, Y.

    2014-01-01

    This study evaluate the effect of ultrasonic application in the extraction process on total phenolic content (TPC) of Hass avocado (Persea americana Mill) pulp. In this study, the solid/ solvent ratio of 1/30 (wt/ vol) and extraction temperature of 40 degree Celsius gave higher TPC value. This ratio and temperature was applied in the ultrasonic-assisted extraction (UAE) of avocado pulp. This study then compared the TPC obtained from the avocado pulp extract without involving ultrasonic and the TPC obtained from the UAE. Results showed that the TPC value of avocado pulp was significantly higher in the UAE (235.77 mg GAE/ 100g dried sample) compared to the TPC in the non-UAE (166.32 mg GAE/ 100g dried sample). The increase in the TPC was between ∼31 % and ∼41 % when 5 to 20 min of ultra sonication applied in the extraction. Ultra sonication duration of 15 min gave the highest TPC where the value was significantly higher compared to the other duration. (author)

  12. Ionic Liquid-Based Ultrasonic/Microwave-Assisted Extraction of ...

    African Journals Online (AJOL)

    Conclusion: Compared with traditional methods, IL-UMAE method uses Ionic liquid-solvent which greatly shortens the extraction time. IL-UMAE as a simple, effective and environmentally friendly approach shows a broad prospect for active ingredient extraction. Keywords: Dioscorea zingiberensis Steroidal saponins, Ionic ...

  13. Ultrasonic-assisted extraction of phenolic and antioxidative compounds from lizard tail (Houttuynia cordata Thunb.

    Directory of Open Access Journals (Sweden)

    Trakul Prommajak

    2014-02-01

    Full Text Available Lizard tail (Houttuynia cordata Thunb. is an Asian herb which has many biological activities, including antioxidative property from polyphenolic compounds. Response surface methodology and Box-Behnken design were employed to study the effect of extraction temperature (30 to 70°C, extraction time (10 to 30 min, ethanol concentration (30 to 70%, and solvent to sample ratio (2 to 6 ml/g on ultrasonic-assisted extraction of phenolic compounds from lizard tail and antioxidant capacity of the herb extract. Extraction temperature was the most relevant factor on the responses. Optimal condition was the extraction temperature of 70°C for 30 min, using 60% ethanol concentration at the solvent to sample ratio of 5 ml/g. Model adequacies were confirmed by extraction at the optimal condition and normality of standardized residuals.

  14. Bi-directional ultrasonic wave coupling to FBGs in continuously bonded optical fiber sensing.

    Science.gov (United States)

    Wee, Junghyun; Hackney, Drew; Bradford, Philip; Peters, Kara

    2017-09-01

    Fiber Bragg grating (FBG) sensors are typically spot-bonded onto the surface of a structure to detect ultrasonic waves in laboratory demonstrations. However, to protect the rest of the optical fiber from any environmental damage during real applications, bonding the entire length of fiber, called continuous bonding, is commonly done. In this paper, we investigate the impact of continuously bonding FBGs on the measured Lamb wave signal. In theory, the ultrasonic wave signal can bi-directionally transfer between the optical fiber and the plate at any adhered location, which could potentially produce output signal distortion for the continuous bonding case. Therefore, an experiment is performed to investigate the plate-to-fiber and fiber-to-plate signal transfer, from which the signal coupling coefficient of each case is theoretically estimated based on the experimental data. We demonstrate that the two coupling coefficients are comparable, with the plate-to-fiber case approximately 19% larger than the fiber-to-plate case. Finally, the signal waveform and arrival time of the output FBG responses are compared between the continuous and spot bonding cases. The results indicate that the resulting Lamb wave signal output is only that directly detected at the FBG location; however, a slight difference in signal waveform is observed between the two bonding configurations. This paper demonstrates the practicality of using continuously bonded FBGs for ultrasonic wave detection in structural health monitoring (SHM) applications.

  15. Effect of ultrasonic treatment on total phenolic extraction from Lavandula pubescens and its application in palm olein oil industry.

    Science.gov (United States)

    Rashed, Marwan M A; Tong, Qunyi; Abdelhai, Mandour H; Gasmalla, Mohammed A A; Ndayishimiye, Jean B; Chen, Long; Ren, Fei

    2016-03-01

    The aims of the current study were to evaluate the best technique for total phenolic extraction from Lavandula pubescens (Lp) and its application in vegetable oil industries as alternatives of synthetic food additives (TBHQ and BHT). To achieve these aims, three techniques of extraction were used: ultrasonic-microwave (40 kHz, 50 W, microwave power 480 W, 5 min), ultrasonic-homogenizer (20 kHz, 150 W, 5 min) and conventional maceration as a control. By using the Folin-Ciocalteu method, the total phenolic contents (TPC) (mg gallic acid equivalent/g dry matter) were found to be 253.87, 216.96 and 203.41 for ultrasonic-microwave extract, ultrasonic-homogenizer extract and maceration extract, respectively. The ultrasonic-microwave extract achieved the higher scavenger effect of DPPH (90.53%) with EC50 (19.54 μg/mL), and higher inhibition of β-carotene/linoleate emulsion deterioration (94.44%) with IC50 (30.62 μg/mL). The activity of the ultrasonic-microwave treatment could prolong the induction period (18.82 h) and oxidative stability index (1.67) of fresh refined, bleached and deodorized palm olein oil (RBDPOo) according to Rancimat assay. There was an important synergist effect between citric acid and Lp extracts in improving the oxidative stability of fresh RBDPOo. The results of this work also showed that the ultrasonic-microwave assisted extract was the most effective against Gram-positive and Gram-negative strains that were assessed in this study. The uses of ultrasonic-microwave could induce the acoustic cavitation and rupture of plant cells, and this facilitates the flow of solvent into the plant cells and enhances the desorption from the matrix of solid samples, and thus would enhance the efficiency of extraction based on cavitation phenomenon. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Ultrasonic-assisted extraction and in-vitro antioxidant activity of polysaccharide from Hibiscus leaf.

    Science.gov (United States)

    Afshari, Kasra; Samavati, Vahid; Shahidi, Seyed-Ahmad

    2015-03-01

    The effects of ultrasonic power, extraction time, extraction temperature, and the water-to-raw material ratio on extraction yield of crude polysaccharide from the leaf of Hibiscus rosa-sinensis (HRLP) were optimized by statistical analysis using response surface methodology. The response surface methodology (RSM) was used to optimize HRLP extraction yield by implementing the Box-Behnken design (BBD). The experimental data obtained were fitted to a second-order polynomial equation using multiple regression analysis and also analyzed by appropriate statistical methods (ANOVA). Analysis of the results showed that the linear and quadratic terms of these four variables had significant effects. The optimal conditions for the highest extraction yield of HRLP were: ultrasonic power, 93.59 W; extraction time, 25.71 min; extraction temperature, 93.18°C; and the water to raw material ratio, 24.3 mL/g. Under these conditions, the experimental yield was 9.66±0.18%, which is well in close agreement with the value predicted by the model 9.526%. The results demonstrated that HRLP had strong scavenging activities in vitro on DPPH and hydroxyl radicals. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. Comparative study on conventional, ultrasonication and microwave assisted extraction of γ-oryzanol from rice bran.

    Science.gov (United States)

    Kumar, Pramod; Yadav, Devbrat; Kumar, Pradyuman; Panesar, Paramjeet Singh; Bunkar, Durga Shankar; Mishra, Diwaker; Chopra, H K

    2016-04-01

    In present study, conventional, ultrasonic and microwave assisted extraction methods were compared with the aim of optimizing best fitting solvent and method, solvent concentration and digestion time for high yield of γ-oryzanol from rice bran. Petroleum ether, hexane and methanol were used to prepare extracts. Extraction yield were evaluated for giving high crude oil yield, total phenolic content (TPC) and γ-oryzanol content. Gas chromatography-mass spectrophotometry was used for the determination of γ-oryzanol concentration. The highest concentration of γ-oryzanol was detected in methanolic extracts of microwave treatment (85.0 ppm) followed by ultrasonication (82.0 ppm) and conventional extraction method (73.5 ppm). Concentration of γ-oryzanol present in the extracts was found to be directly proportional to the total phenolic content. A combination of 80 % methanolic concentration and 55 minutes digestion time of microwave treatment yielded the best extraction method for TPC and thus γ-oryzanol (105 ppm).

  18. Ultrasonic-Assisted Extraction and Antioxidant Activity of Flavonoids ...

    African Journals Online (AJOL)

    Lee WC, Yusof Y, Hamid NSA, Baharin BS. Optimizing conditions for hot water extraction of banana juice using response surface methodology (RSM). J Food. Eng 2006; 75: 473-479. 11. Proestos C, Sereli D, Komaitis M. Analysis of flavonoids and phenolic acids in Greek aromatic plants: Investigation of their antioxidant ...

  19. Ultrasonic extraction, antioxidant and anticancer activities of novel polysaccharides from Chuanxiong rhizome.

    Science.gov (United States)

    Hu, Jie; Jia, Xuejing; Fang, Xiaobin; Li, Peng; He, Chengwei; Chen, Meiwan

    2016-04-01

    Ultrasonic-assisted extraction technology was employed to prepare Ligusticum chuanxiong Hort polysaccharide. Single factor test and orthogonal experimental design were used to optimize the extraction conditions. The results showed that the optimal extraction conditions consisted of ultrasonic temperature of 80°C, ultrasonic time of 40 min and water to raw material ratio of 30 mL/g. Three novel polysaccharides fractions, LCX0, LCX1 and LCX2, were isolated and purified from the crude polysaccharides using DEAE-52 cellulose and Sephadex G-100 column chromatography. The molecular weight and monosaccharide composition of three LCX polysaccharides fractions were analyzed with gel permeation chromatography (GPC) and HPLC analysis, respectively. Furthermore, the antioxidant and in vitro anticancer activities of the polysaccharides were investigated. Compared with LCX0, LCX2 and LCX1 showed relative higher antioxidant activity and inhibitory activity to the growth of HepG2, SMMC7721, A549 and HCT-116 cells. It is suggested that the novel polysaccharides from rhizome of L. chuanxiong could be promising bioactive macromolecules for biomedical use. Copyright © 2016. Published by Elsevier B.V.

  20. Feature extraction for ultrasonic sensor based defect detection in ceramic components

    Science.gov (United States)

    Kesharaju, Manasa; Nagarajah, Romesh

    2014-02-01

    High density silicon carbide materials are commonly used as the ceramic element of hard armour inserts used in traditional body armour systems to reduce their weight, while providing improved hardness, strength and elastic response to stress. Currently, armour ceramic tiles are inspected visually offline using an X-ray technique that is time consuming and very expensive. In addition, from X-rays multiple defects are also misinterpreted as single defects. Therefore, to address these problems the ultrasonic non-destructive approach is being investigated. Ultrasound based inspection would be far more cost effective and reliable as the methodology is applicable for on-line quality control including implementation of accept/reject criteria. This paper describes a recently developed methodology to detect, locate and classify various manufacturing defects in ceramic tiles using sub band coding of ultrasonic test signals. The wavelet transform is applied to the ultrasonic signal and wavelet coefficients in the different frequency bands are extracted and used as input features to an artificial neural network (ANN) for purposes of signal classification. Two different classifiers, using artificial neural networks (supervised) and clustering (un-supervised) are supplied with features selected using Principal Component Analysis(PCA) and their classification performance compared. This investigation establishes experimentally that Principal Component Analysis(PCA) can be effectively used as a feature selection method that provides superior results for classifying various defects in the context of ultrasonic inspection in comparison with the X-ray technique.

  1. Optimization of ultrasonic-assisted extraction of natural antioxidants from rice bran using response surface methodology.

    Science.gov (United States)

    Tabaraki, Reza; Nateghi, Ashraf

    2011-11-01

    Ultrasonic technology was applied for extraction of polyphenols and antioxidants from the rice bran using ethanol as a food grade solvent. Response surface methodology (RSM) was used to optimize experimental conditions for extraction of polyphenols and antioxidants. Three independent variables such as solvent percentage (%), temperature (°C) and time (min) were studied. Effect of ethanol concentration was found to be significant on all responses. Total phenolic content (TPC) varied from 2.37 to 6.35mg gallic acid equivalent/g of dry sample. Antioxidant activity of the extracts was determined by the ferric reducing antioxidant power (FRAP) assay and scavenging activity of 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical. FRAP and DPPH values varied from 31.74 to 57.23μmol Fe(2+)/g of dry sample and 16.88% to 55.61% inhibition, respectively. Extraction yields ranged from 11 to 20.2%. Optimal ultrasonic-assisted extraction (UAE) conditions were identified as 65-67% ethanol, 51-54°C, 40-45min. The experimental values agreed with those predicted by SRM models, thus indicating suitability of the model employed and the success of RSM in optimizing the extraction conditions. Copyright © 2011 Elsevier B.V. All rights reserved.

  2. Ultrasonication-Assisted Solvent Extraction of Quercetin Glycosides from ‘Idared’ Apple Peels

    Directory of Open Access Journals (Sweden)

    Gwendolyn M. Huber

    2011-11-01

    Full Text Available Quercetin and quercetin glycosides are physiologically active flavonol molecules that have been attributed numerous health benefits. Recovery of such molecules from plant matrices depends on a variety of factors including polarity of the extraction solvent. Among the solvents of a wide range of dielectric constants, methanol recovered the most quercetin and its glycosides from dehydrated ‘Idared’ apple peels. When ultra-sonication was employed to facilitate the extraction, exposure of 15 min of ultrasound wavelengths of dehydrated apple peel powder in 80% to 100% (v/v methanol in 1:50 (w:v solid to solvent ratio provided the optimum extraction conditions for quercetin and its glycosides. Acidification of extraction solvent with 0.1% (v/v or higher concentrations of HCl led to hydrolysis of naturally occurring quercetin glycosides into the aglycone as an extraction artifact.

  3. Characterization of water absorption by CFRP using air-coupled ultrasonic testing

    International Nuclear Information System (INIS)

    Lee, Joo Min; Lee, Joo Sung; Park, Ik Keun; Kim, Yong Kwon

    2014-01-01

    Carbon-fiber-reinforced plastic (CFRP) composites are increasingly being used in a variety of industry applications, such as aircraft, automobiles, and ships because of their high specific stiffness and high specific strength. Aircraft are exposed to high temperatures and high humidity for a long duration during flights. CFRP materials of the aircraft can absorb water, which could decrease the adhesion strength of these materials and cause their volumes to change with variation in internal stress. Therefore, it is necessary to estimate the characteristics of CFRP composites under actual conditions from the viewpoint of aircraft safety. In this study air-coupled ultrasonic testing (ACUT) was applied to the evaluation of water absorption properties of CFRP composites. CFRP specimens were fabricated and immersed in distilled water at 75 degree C for 30, 60, and 120 days, after which their ultrasonic images were obtained by ACUT. The water absorption properties were determined by quantitatively analyzing the changes in ultrasonic signals. Further, shear strength was applied to the specimens to verify the changes in their mechanical properties for water absorption.

  4. Characterization of water absorption by CFRP using air-coupled ultrasonic testing

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Joo Min; Lee, Joo Sung; Park, Ik Keun [Seoul National University of Science and Technology, Seoul (Korea, Republic of); Kim, Yong Kwon [Technology Research and Development Institute, KEPCO Plant Service and Engineering Co., Ltd, Naju (Korea, Republic of)

    2014-04-15

    Carbon-fiber-reinforced plastic (CFRP) composites are increasingly being used in a variety of industry applications, such as aircraft, automobiles, and ships because of their high specific stiffness and high specific strength. Aircraft are exposed to high temperatures and high humidity for a long duration during flights. CFRP materials of the aircraft can absorb water, which could decrease the adhesion strength of these materials and cause their volumes to change with variation in internal stress. Therefore, it is necessary to estimate the characteristics of CFRP composites under actual conditions from the viewpoint of aircraft safety. In this study air-coupled ultrasonic testing (ACUT) was applied to the evaluation of water absorption properties of CFRP composites. CFRP specimens were fabricated and immersed in distilled water at 75 degree C for 30, 60, and 120 days, after which their ultrasonic images were obtained by ACUT. The water absorption properties were determined by quantitatively analyzing the changes in ultrasonic signals. Further, shear strength was applied to the specimens to verify the changes in their mechanical properties for water absorption.

  5. [Optimization of ultrasonic extraction process for Xiaoqinglong granules by Box-Behnken in condition of medium scale].

    Science.gov (United States)

    Wang, Zheng-Kuan; Shi, Xiao-Meng; Liu, Yuan; Zhang, Qing-Fen; Wu, Jian-Xiong; Bi, Yu-An; Wang, Zhen-Zhong; Xiao, Wei

    2016-02-01

    This paper is to investigate the optimization conditions of ultrasonic technique for extraction process of Xiaoqinglong granules in medium scale. First of all, single factor experiment was used to determine the overall impact tendency and range of each factor; secondly, Box-Behnken method was used for optimization and detecting the content of paeoniflorin, ephedrine hydrochloride, glycyrrhizic acid of the liquid medicine. Their respective extraction rate was calculated and the comprehensive evaluation was carried out. The results were used as the evaluation basis for the efficacy of Xiaoqinglong granules ultrasonic extraction. The test results showed that the optimum extraction process of Xiaoqinglong granules by ultrasonic extraction was under the following conditions: ultrasonic power 600 W, liquid-solid ratio 10∶1, extraction for 31 min. Under this condition, the predicted value of extraction rate for Xiaoqinglong granules was 85.90%, and the test value was 85.87%. The mathematical model(P<0.01) established in this paper was significant, and can be used for the analysis and prediction of the ultrasonic extraction process of Xiaoqinglong granules. Copyright© by the Chinese Pharmaceutical Association.

  6. Ultrasonic-assisted Aqueous Extraction and Physicochemical Characterization of Oil from Clanis bilineata.

    Science.gov (United States)

    Sun, Mingmei; Xu, Xiao; Zhang, Qiuqin; Rui, Xin; Wu, Junjun; Dong, Mingsheng

    2018-02-01

    Ultrasound-assisted aqueous extraction (UAAE) was used to extract oil from Clanis bilineata (CB), a traditional edible insect that can be reared on a large scale in China, and the physicochemical property and antioxidant capacity of the UAAE-derived oil (UAAEO) were investigated for the first time. UAAE conditions of CB oil was optimized using response surface methodology (RSM) and the highest oil yield (19.47%) was obtained under optimal conditions for ultrasonic power, extraction temperature, extraction time, and ultrasonic interval time at 400 W, 40°C, 50 min, and 2 s, respectively. Compared with Soxhlet extraction-derived oil (SEO), UAAEO had lower acid (AV), peroxide (PV) and p-anisidine values (PAV) as well as higher polyunsaturated fatty acids contents and thermal stability. Furthermore, UAAEO showed stronger antioxidant activities than those of SEO, according to DPPH radical scavenging and β-carotene bleaching tests. Therefore, UAAE is a promising process for the large-scale production of CB oil and CB has a developing potential as functional oil resource.

  7. The Effect of Ultrasonic Waves on Sugar Extraction and Mechanical Properties of Sugar Beet

    Directory of Open Access Journals (Sweden)

    K Hedayati

    2013-09-01

    Full Text Available Sugar, which can be extracted from sugar cane and sugar beet, is one of the most important ingredients of food. Conducting more research to increase the extraction efficiency of sugar is necessary due to high production of sugar beet and its numerous processing units in northern Khorasan province. In this research, the effect of temperature, time and the frequency of ultrasonic waves on mechanical properties of sugar beet and its extraction rate of sugar in moisture content of 75% were studied. In this regard, an ultrasonic bath in laboratory scale was used. The studied parameters and their levels were frequency in three levels (zero, 25 and 45 KHz, temperature in three levels (25, 50 and 70 ° C and the imposed time of ultrasonic waves in three levels (10, 20 and 30 min. Samples were prepared using planned experiments and the results were compared with control sugar beet samples. A Saccharimeter was used to measure the concenteration of sugar in samples. Two different types of probe including semi-spherical end and the other one with sharpened edges were used to measure mechanical properties. The studied parameters of frequency, temperature and time showed significant effect on sugar extraction and their resulted effect in optimized levels revealed up to 56% increase in sugar extraction compared with control samples. The obtained values of elastic modulus and shear modulus showed a decreasing trend. The obtained values of total energy of rupture, the total energy of shear, the maximum force of rupture, and the yield point of rupture showed an increasing trend. The frequency had no significant effect on the yield point of rupture and shear force.

  8. Production of glutinous rice flour from broken rice via ultrasonic assisted extraction of amylose.

    Science.gov (United States)

    Setyawati, Yohana Dwi; Ahsan, Sitti Faika; Ong, Lu Ki; Soetaredjo, Felycia Edi; Ismadji, Suryadi; Ju, Yi-Hsu

    2016-07-15

    In this study, a modified aqueous leaching method by complex formation of amylose with glycerol was employed for reducing the amylose content of starch in broken white rice to less than 2%, so that the resulting starch can be classified to that of glutinous rice flour. By employing ultrasonication in alkaline condition, extraction of amylose could be performed by washing at lower temperature in shorter time compared to the existing aqueous leaching method. The effects of glycerol concentration, alkali concentration, ultrasonication and treatment time on the amylose content of the treated starch were systematically investigated. Under optimum condition, amylose content of broken white rice starch can be reduced from 27.27% to 1.43% with a yield of 80.42%. The changes in the physicochemical properties of the rice flour before and after treatment were studied. Copyright © 2016 Elsevier Ltd. All rights reserved.

  9. [Optimization of ultrasonic-assisted extraction of total flavonoids from leaves of the Artocarpus heterophyllus by response surface methodology].

    Science.gov (United States)

    Wang, Hong-wu; Liu, Yan-qing; Wang, Yuan-hong

    2011-07-01

    To investigate the ultrasonic-assisted extract on of total flavonoids from leaves of the Artocarpus heterophyllus. Investigated the effects of ethanol concentration, extraction time, and liquid-solid ratio on flavonoids yield. A 17-run response surface design involving three factors at three levels was generated by the Design-Expert software and experimental data obtained were subjected to quadratic regression analysis to create a mathematical model describing flavonoids extraction. The optimum ultrasonic assisted extraction conditions were: ethanol volume fraction 69.4% and liquid-solid ratio of 22.6:1 for 32 min. Under these optimized conditions, the yield of flavonoids was 7.55 mg/g. The Box-Behnken design and response surface analysis can well optimize the ultrasonic-assisted extraction of total flavonoids from Artocarpus heterophyllus.

  10. Ultrasonic extraction of polysaccharides from Laminaria japonica and their antioxidative and glycosidase inhibitory activities

    Science.gov (United States)

    Wan, Peng; Yang, Xiaoman; Cai, Bingna; Chen, Hua; Sun, Huili; Chen, Deke; Pan, Jianyu

    2015-08-01

    In the present study, ultrasonic extraction technique (UET) is used to improve the yield of polysaccharides from Laminaria japonica (LJPs). And their antioxidative as well as glycosidase inhibitory activities are investigated. Box-Behnken design (BBD) combined with response surface methodology (RSM) is applied to optimize ultrasonic extraction for polysaccharides. The optimized conditions are obtained as extraction time at 54 min, ultrasonic power at 1050 W, extraction temperature at 80°C and ratio of material to solvent at 1:50 (g mL-1). Under these optimal ultrasonic extraction conditions, an actual experimental yield (5.75% ± 0.3%) is close to the predicted result (5.67%) with no significant difference ( P > 0.05). Vitro antioxidative and glycosidase inhibitory activities tests indicate that the crude polysaccharides (LJP) and two major ethanol precipitated fractions (LJP1 and LJP2) are in a concentration-dependent manner. LJP2 (30%-60% ethanol precipitated polysaccharides) possesses the strongest α-glucosidase inhibitory activity and moderate scavenging activity against hydroxyl radicals (66.09% ± 2.19%, 3.0 mg mL-1). Also, the inhibitory activity against α-glucosidase (59.08% ± 3.79%, 5.0 mg mL-1) is close to that of acarbose (63.99% ± 3.27%, 5.0 mg mL-1). LJP1 (30% ethanol precipitated polysaccharides) exhibits the strongest scavenging activity against hydroxyl radicals (99.80% ± 0.00%, 3.0 mg mL-1) and moderate α-glucosidase inhibitory activity (47.76% ± 1.92%, 5.0 mg mL-1). LJP shows the most remarkable DPPH scavenging activity (66.20% ± 0.11%, 5.0 mg mL-1) but weakest α-glucosidase inhibitory activity (37.77% ± 1.30%, 5.0 mg mL-1). However, all these LJPs exert weak inhibitory effects against α-amylase. These results show that UET is an effective method for extracting bioactive polysaccharides from seaweed materials. LJP1 and LJP2 can be developed as a potential ingredient in hypoglycemic agents or functional food for the management of

  11. Comparative evaluation of maceration and ultrasonic-assisted extraction of phenolic compounds from fresh olives.

    Science.gov (United States)

    Deng, Junlin; Xu, Zhou; Xiang, Chunrong; Liu, Jing; Zhou, Lijun; Li, Tian; Yang, Zeshen; Ding, Chunbang

    2017-07-01

    Ultrasonic-assisted extraction (UAE) and maceration extraction (ME) were optimized using response surface methodology (RSM) for total phenolic compounds (TPC) from fresh olives. The main phenolic compounds and antioxidant activity of TPC were also investigated. The optimized result for UAE was 22mL/g of liquid-solid ratio, 47°C of extraction temperature and 30min of extraction time, 7.01mg/g of yielding, and for ME was 24mL/g of liquid-solid ratio, 50°C of extraction temperature and 4.7h of extraction time, 5.18mg/g of yielding. The HPLC analysis revealed that the extracts by UAE and ME possessed 14 main phenolic compounds, and UAE exhibited more amounts of all phenols than ME. The most abundant phenolic compounds in olive extracts were hydroxytyrosol, oleuropein and rutin. Both extracts showed excellent antioxidant activity in a dose-dependent manner. Taken together, UAE could effectively increase the yield of phenolic compounds from olives. In addition these phenolic compounds could be used as a potential source of natural antioxidants. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. A method for the preparation of curcumin by ultrasonic-assisted ammonium sulfate/ethanol aqueous two phase extraction.

    Science.gov (United States)

    Xu, Guangkuan; Hao, Changchun; Tian, Suyang; Gao, Feng; Sun, Wenyuan; Sun, Runguang

    2017-01-15

    This study investigated a new and easy-to-industrialized extracting method for curcumin from Curcuma longa rhizomes using ultrasonic extraction technology combined with ammonium sulfate/ethanol aqueous two-phase system (ATPS), and the preparation of curcumin using the semi-preparative HPLC. The single-factor experiments and response surface methodology (RSM) were utilized to determine the optimal material-solvent ratio, ultrasonic intensity (UI) and ultrasonic time. The optimum extraction conditions were finally determined to be material-solvent rate of 3.29:100, ultrasonic intensity of 33.63W/cm 2 and ultrasonic time of 17min. At these optimum conditions, the extraction yield could reach 46.91mg/g. And the extraction yields of curcumin remained stable in the case of amplification, which indicated that scale-up extraction was feasible and efficient. Afterwards, the semi-preparative HPLC experiment was carried out, in which optimal preparation conditions were elected according to the single factor experiment. The prepared curcumin was obtained and the purity could up to 85.58% by the semi-preparative HPLC. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Application of Box-Behnken design for ultrasonic-assisted extraction of polysaccharides from Paeonia emodi.

    Science.gov (United States)

    Ahmad, Ajaz; Alkharfy, Khalid M; Wani, Tanveer A; Raish, Mohammad

    2015-01-01

    The objective of the present work was to study the ultrasonic assisted extraction and optimization of polysaccharides from Paeonia emodi and evaluation of its anti-inflammatory response. Specifically, the optimization of polysaccharides was carried out using Box-Behnken statistical experimental design. Response surface methodology (RSM) of three factors (extraction temperature, extraction time and liquid solid ratio) was employed to optimize the percentage yield of the polysaccharides. The experimental data were fitted to quadratic response surface models using multiple regression analysis with high coefficient of determination value (R) of 0.9906. The highest polysaccharide yield (8.69%) as per the Derringer's desirability prediction tool was obtained under the optimal extraction condition (extraction temperature 47.03 °C, extraction time 15.68 min, and liquid solid ratio 1.29 ml/g) with a desirability value of 0.98. These optimized values of tested parameters were validated under similar conditions (n = 6), an average of 8.13 ± 2.08% of polysaccharide yield was obtained in an optimized extraction conditions with 93.55% validity. The anti-inflammatory effect of polysaccharides of P. emodi were studied on carrageenan induced paw edema. In vivo results showed that the P. emodi 200mg/kg of polysaccharide extract exhibited strong potential against inflammatory response induced by 1% suspension of carrageenean in normal saline. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. Approaches for on-line coupling of extraction and chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Hyoetylaeinen, Tuulia; Riekkola, Marja-Liisa [Laboratory of Analytical Chemistry, Department of Chemistry, University of Helsinki, P.O. Box 55, 00014, Helsinki (Finland)

    2004-04-01

    This review provides an overview of the approaches available in order to perform on-line coupling of various extraction techniques with liquid and gas chromatography, for the analysis of semivolatile and nonvolatile analytes in liquid and solid samples. The main focus is on the instrumental set-up of these techniques. Selected real applications are described by way of illustration. The extraction methods suitable for on-line coupling covered in this review are: liquid-liquid extraction, solid-phase extraction, membrane-based techniques, pressurised liquid extraction, supercritical fluid extraction, and microwave- and sonication-assisted extractions. The following systems are not covered in this review: on-line coupled solid-phase extraction-liquid chromatography, purge-and-trap-GC, and membrane extraction with a sorbent interface-GC. (orig.)

  15. Enzymolysis-ultrasonic assisted extraction, chemical characteristics and bioactivities of polysaccharides from corn silk.

    Science.gov (United States)

    Chen, Shuhan; Chen, Haixia; Tian, Jingge; Wang, Jia; Wang, Yanwei; Xing, Lisha

    2014-01-30

    An enzymolysis-ultrasonic assisted extraction (EUAE) procedure of corn silk polysaccharides (CSPS) was established and the physicochemical properties, antioxidant and anticancer activities of CSPS were studied. Orthogonal test and response surface methodology were applied to optimize the extraction parameters. The optimum enzymolysis and ultrasonic conditions were cellulase content of 7.5% for 150 min at 55 °C and liquid-solid ratio of 31.8 for 34.2 min at 66.3 °C, respectively. Under these conditions, the yield of CSPS increased from 4.56% to 7.10%. CSPS obtained by hot water and EUAE were composed of rhamnose, arabinose, xylose, mannose, galactose and glucose with molecular ratios of 4.17:17.33:5.59:18.65:19.11:35.14 and 8.83:15.77:7.92:12.39:11.15:43.94, respectively. Their molecular weight distributions were 10.52 × 10(4) and 6.88 × 10(4)Da, respectively. CSPS obtained by EUAE showed morphological and conformation changes and higher antioxidant and anticancer activities compared with CSPS extracted by hot water. Copyright © 2013 Elsevier Ltd. All rights reserved.

  16. Effect of coffee reduction on constituent concentration in an energy-efficient process of ultrasonic extraction

    Directory of Open Access Journals (Sweden)

    Wang Cheng-Chi

    2015-01-01

    Full Text Available Coffee is one of the popular beverage; its constituents include caffeine, oxidation resistant aromatic constituents, protein, tannin, and fat. It is indicated in literatures that a proper amount of coffee stimulates the brain and enhances memory, but excessive coffee causes negative results, such as coronary artery disease, high blood pressure, heart disease and kidney disease. This study used high-performance ultrasonic process to discuss the effect of pulverized coffee reduction on the constituent concentration. It further compared the constituent concentrations obtained in different extraction periods. The experimental results show that the coffee aroma constituents can be extracted effectively by ultrasonic process without any organic solvent, and the constituent concentration does not decrease with the addition of pulverized coffee. Therefore, the consumption of pulverized coffee can be reduced greatly by using the proposed. The time of extraction process can be shortened, so as to save energy. The most important point is to reduce the enterprises manufacturing cost and to increase the profit.

  17. Effect of ultrasonic degradation of hyaluronic acid extracted from rooster comb on antioxidant and antiglycation activities.

    Science.gov (United States)

    Hafsa, Jawhar; Chaouch, Mohamed Aymen; Charfeddine, Bassem; Rihouey, Christophe; Limem, Khalifa; Le Cerf, Didier; Rouatbi, Sonia; Majdoub, Hatem

    2017-12-01

    Recently, low-molecular-weight hyaluronic acid (LMWHA) has been reported to have novel features, such as free radical scavenging activities, antioxidant activities and dietary supplements. In this study, hyaluronic acid (HA) was extracted from rooster comb and LMWHA was obtained by ultrasonic degradation in order to assess their antioxidant and antiglycation activities. Molecular weight (Mw) and the content of glucuronic acid (GlcA) were used as the index for comparison of the effect of ultrasonic treatment. The effects on the structure were determined by ultraviolet (UV) spectra and Fourier transform infrared spectra (FTIR). The antioxidant activity was determined by three analytical assays (DPPH, NO and TBARS), and the inhibitory effect against glycated-BSA was also assessed. The GlcA content of HA and LMWHA was estimated at about 48.6% and 47.3%, respectively. The results demonstrate that ultrasonic irradiation decreases the Mw (1090-181 kDa) and intrinsic viscosity (1550-473 mL/g), which indicate the cleavage of the glycosidic bonds. The FTIR and UV spectra did not significantly change before and after degradation. The IC 50 value of HA and LWMHA was 1.43, 0.76 and 0.36 mg/mL and 1.20, 0.89 and 0.17 mg/mL toward DPPH, NO and TBARS, respectively. Likewise LMWHA exhibited significant inhibitory effects on the AGEs formation than HA. The results demonstrated that the ultrasonic irradiation did not damage and change the chemical structure of HA after degradation; furthermore, decreasing Mw and viscosity of LMWHA after degradation may enhance the antioxidant and antiglycation activity.

  18. Optimization of ultrasonic assisted extraction of antioxidants from black soybean (Glycine max var) sprouts using response surface methodology.

    Science.gov (United States)

    Lai, Jixiang; Xin, Can; Zhao, Ya; Feng, Bing; He, Congfen; Dong, Yinmao; Fang, Yun; Wei, Shaomin

    2013-01-16

    Response surface methodology (RSM) using a central composite design (CCD) was employed to optimize the conditions for extraction of antioxidants from black soybean (Glycine max var) sprouts. Three influencing factors: liquid-solid ratio, period of ultrasonic assisted extraction and extraction temperature were investigated in the ultrasonic aqueous extraction. Then Response Surface Methodology (RSM) was applied to optimize the extraction process focused on DPPH radical-scavenging capacity of the antioxidants with respect to the above influencing factors. The best combination of each significant factor was determined by RSM design and optimum pretreatment conditions for maximum radical-scavenging capacity were established to be liquid-solid ratio of 29.19:1, extraction time of 32.13 min, and extraction temperature of 30 °C. Under these conditions, 67.60% of DPPH radical-scavenging capacity was observed experimentally, similar to the theoretical prediction of 66.36%.

  19. Ultrasonic nebulization extraction/low pressure photoionization mass spectrometry for direct analysis of chemicals in matrices.

    Science.gov (United States)

    Liu, Chengyuan; Zhu, Yanan; Zhou, Zhongyue; Yang, Jiuzhong; Qi, Fei; Pan, Yang

    2015-09-03

    A novel ultrasonic nebulization extraction/low-pressure photoionization (UNE-LPPI) system has been designed and employed for the rapid mass spectrometric analysis of chemicals in matrices. An ultrasonic nebulizer was used to extract the chemicals in solid sample and nebulize the solvent in the nebulization cell. Aerosols formed by ultrasonic were evaporated by passing through a transferring tube, and desolvated chemicals were ionized by the emitted light (10.6 eV) from a Krypton discharge lamp at low pressure (∼68 Pa). First, a series of semi/non-volatile compounds with different polarities, such as polycyclic aromatic hydrocarbons (PAHs), amino acids, dipeptides, drugs, nucleic acids, alkaloids, and steroids were used to test the system. Then, the quantification capability of UNE-LPPI was checked with: 1) pure chemicals, such as 9,10-phenanthrenequinone and 1,4-naphthoquinone dissolved in solvent; 2) soil powder spiked with different amounts of phenanthrene and pyrene. For pure chemicals, the correlation coefficient (R(2)) for the standard curve of 9,10-phenanthrenequinone in the range of 3 ng-20 μg mL(-1) was 0.9922, and the measured limits of detection (LOD) was 1 ng ml(-1). In the case of soil powder, linear relationships for phenanthrene and pyrene from 10 to 400 ng mg(-1) were obtained with correlation coefficients of 0.9889 and 0.9893, respectively. At last, the feasibility of UNE-LPPI for the detection of chemicals in real matrices such as tablets and biological tissues (tea, Citrus aurantium peel and sage (Salvia officinalis) leaf) were successfully demonstrated. Copyright © 2015 Elsevier B.V. All rights reserved.

  20. Ultrasonic wave propagation in viscoelastic cortical bone plate coupled with fluids: a spectral finite element study.

    Science.gov (United States)

    Nguyen, Vu-Hieu; Naili, Salah

    2013-01-01

    This work deals with the ultrasonic wave propagation in the cortical layer of long bones which is known as being a functionally graded anisotropic material coupled with fluids. The viscous effects are taken into account. The geometrical configuration mimics the one of axial transmission technique used for evaluating the bone quality. We present a numerical procedure adapted for this purpose which is based on the spectral finite element method (FEM). By using a combined Laplace-Fourier transform, the vibroacoustic problem may be transformed into the frequency-wavenumber domain in which, as radiation conditions may be exactly introduced in the infinite fluid halfspaces, only the heterogeneous solid layer needs to be analysed using FEM. Several numerical tests are presented showing very good performance of the proposed approach. We present some results to study the influence of the frequency on the first arriving signal velocity in (visco)elastic bone plate.

  1. Air-coupled ultrasonic through-transmission thickness measurements of steel plates.

    Science.gov (United States)

    Waag, Grunde; Hoff, Lars; Norli, Petter

    2015-02-01

    Non-destructive ultrasonic testing of steel structures provide valuable information in e.g. inspection of pipes, ships and offshore structures. In many practical applications, contact measurements are cumbersome or not possible, and air-coupled ultrasound can provide a solution. This paper presents air-coupled ultrasonic through-transmission measurements on a steel plate with thicknesses 10.15 mm; 10.0 mm; 9.8 mm. Ultrasound pulses were transmitted from a piezoelectric transducer at normal incidence, through the steel plate, and were received at the opposite side. The S1, A2 and A3 modes of the plate are excited, with resonance frequencies that depend on the material properties and the thickness of the plate. The results show that the resonances could be clearly identified after transmission through the steel plate, and that the frequencies of the resonances could be used to distinguish between the three plate thicknesses. The S1-mode resonance was observed to be shifted 10% down compared to a simple plane wave half-wave resonance model, while the A2 and S2 modes were found approximately at the corresponding plane-wave resonance frequencies. A model based on the angular spectrum method was used to predict the response of the through-transmission setup. This model included the finite aperture of the transmitter and receiver, and compressional and shear waves in the solid. The model predicts the frequencies of the observed modes of the plate to within 1%, including the down-shift of the S1-mode. Copyright © 2014 Elsevier B.V. All rights reserved.

  2. Optimisation of ultrasonic-assisted extraction of phenolic compounds, antioxidants, and anthocyanins from sugar beet molasses.

    Science.gov (United States)

    Chen, Mingshun; Zhao, Yi; Yu, Shujuan

    2015-04-01

    Response surface methodology was used to optimise experimental conditions for ultrasonic-assisted extraction (UAE) of functional components from sugar beet molasses. The central composite design (CCD) was used for the optimisation of extraction parameters in terms of total phenolic contents, antioxidant activities and anthocyanins. Result suggested the optimal conditions obtained by RSM for UAE from sugar beet molasses were as follows: HCl concentration 1.55-1.72 mol/L, ethanol concentration 57-63% (v/v), extraction temperature 41-48 °C, and extraction time 66-73 min. In the optimal conditions, the experimental total phenolic contents were 17.36 mg GAE/100mL, antioxidant activity was 16.66 mg TE/g, and total anthocyanins were 31.81 mg/100g of the sugar beet molasses extract, which were well matched the predicted values. Teen compounds, i.e. gallic acid, vanillin, hydroxybenzoic acid, syringic acid, cyanidin-3-O-rutinoside, cyanidin-3-O-glucoside, catechin, delphinidin-3-O-rutinoside, delphinidin-3-O-glucuronide and ferulic acid were determined by HPLC-DAD-MS/MS in sugar beet molasses. Copyright © 2014 Elsevier Ltd. All rights reserved.

  3. Ionic liquids based simultaneous ultrasonic and microwave assisted extraction of phenolic compounds from burdock leaves

    International Nuclear Information System (INIS)

    Lou Zaixiang; Wang Hongxin; Zhu Song; Chen Shangwei; Zhang Ming; Wang Zhouping

    2012-01-01

    The ionic liquids based simultaneous ultrasonic and microwave assisted extraction (IL-UMAE) technique was first proposed and applied to isolate compounds. The ionic liquids comprising a range of four anions, five 1-alkyl-3-methylimidazolium derivatives were designed and prepared. The results suggested that varying the anion and cation both had apparent effects on the extraction of phenolics. The results also showed that irradiation power, time and solid–liquid ratio significantly affected the yields. The yields of caffeic acid and quercetin obtained by IL-UMAE were higher than those by regular UMAE. Compared with conventional heat-reflux extraction (HRE), the proposed approach exhibited higher efficiency (8–17% enhanced) and shorter extraction time (from 5 h to 30 s). The results indicated ILUMAE to be a fast and efficient extraction technique. Moreover, the proposed method was validated by the reproducibility and recovery experiments. The ILUMAE method provided good recoveries (from 96.1% to 105.3%) with RSD lower than 5.2%, which indicated that the proposed method was credible. Based on the designable nature of ionic liquids, and the rapid and highly efficient performance of the proposed approach, ILUMAE provided a new alternative for preparation of various useful substances from solid samples.

  4. Ultrasonic-Assisted Extraction of Raspberry Seed Oil and Evaluation of Its Physicochemical Properties, Fatty Acid Compositions and Antioxidant Activities.

    Directory of Open Access Journals (Sweden)

    Hui Teng

    Full Text Available Ultrasonic-assisted extraction was employed for highly efficient separation of aroma oil from raspberry seeds. A central composite design with two variables and five levels was employed and effects of process variables of sonication time and extraction temperature on oil recovery and quality were investigated. Optimal conditions predicted by response surface methodology were sonication time of 37 min and extraction temperature of 54°C. Specifically, ultrasonic-assisted extraction (UAE was able to provide a higher content of beneficial unsaturated fatty acids, whereas conventional Soxhlet extraction (SE resulted in a higher amount of saturated fatty acids. Moreover, raspberry seed oil contained abundant amounts of edible linoleic acid and linolenic acid, which suggest raspberry seeds could be valuable edible sources of natural γ-linolenic acid products. In comparison with SE, UAE exerted higher free radical scavenging capacities. In addition, UAE significantly blocked H2O2-induced intracellular reactive oxygen species (ROS generation.

  5. Extraction of intracellular protein from Chlorella pyrenoidosa using a combination of ethanol soaking, enzyme digest, ultrasonication and homogenization techniques.

    Science.gov (United States)

    Zhang, Ruilin; Chen, Jian; Zhang, Xuewu

    2018-01-01

    Due to the rigid cell wall of Chlorella species, it is still challenging to effectively extract significant amounts of protein. Mass methods were used for the extraction of intracellular protein from microalgae with biological, mechanical and chemical approaches. In this study, based on comparison of different extraction methods, a new protocol was established to maximize extract amounts of protein, which was involved in ethanol soaking, enzyme digest, ultrasonication and homogenization techniques. Under the optimized conditions, 72.4% of protein was extracted from the microalgae Chlorella pyrenoidosa, which should contribute to the research and development of Chlorella protein in functional food and medicine. Copyright © 2017 Elsevier Ltd. All rights reserved.

  6. Wave energy extraction by coupled resonant absorbers.

    Science.gov (United States)

    Evans, D V; Porter, R

    2012-01-28

    In this article, a range of problems and theories will be introduced that will build towards a new wave energy converter (WEC) concept, with the acronym 'ROTA' standing for resonant over-topping absorber. First, classical results for wave power absorption for WECs constrained to operate in a single degree of freedom will be reviewed and the role of resonance in their operation highlighted. Emphasis will then be placed on how the introduction of further resonances can improve power take-off characteristics by extending the range of frequencies over which the efficiency is close to a theoretical maximum. Methods for doing this in different types of WECs will be demonstrated. Coupled resonant absorbers achieve this by connecting a WEC device equipped with its own resonance (determined from a hydrodynamic analysis) to a new system having separate mass/spring/damper characteristics. It is shown that a coupled resonant effect can be realized by inserting a water tank into a WEC, and this idea forms the basis of the ROTA device. In essence, the idea is to exploit the coupling between the natural sloshing frequencies of the water in the internal tank and the natural resonance of a submerged buoyant circular cylinder device that is tethered to the sea floor, allowing a rotary motion about its axis of attachment.

  7. Ultrasonic microdialysis coupled with capillary electrophoresis electrochemiluminescence study the interaction between trimetazidine dihydrochloride and human serum albumin.

    Science.gov (United States)

    Sun, Shuangjiao; Long, Chanjuan; Tao, Chunyao; Meng, Sa; Deng, Biyang

    2014-12-03

    The paper describes a homemade ultrasonic microdialysis device coupled with capillary electrophoresis electrochemiluminescence (CE-ECL) for studying the interaction between human serum albumin (HSA) and trimetazidine dihydrochloride (TMZ). The time required for equilibrium by ultrasonic microdialysis was 45min, which was far less than that by traditional dialysis (240min). It took 80min to achieve the required combination equilibrium by normal incubation and only 20min by ultrasonic. Compared with traditional dialysis, the use of ultrasonic microdialysis simplified experimental procedures, shortened experimental time and saved consumption of sample. A simple, sensitive and selective determination of TMZ was developed using CE-ECL and the parameters that affected ECL intensity were optimized. Under the optimized conditions, the linear range of TMZ was from 0.075 to 80μmol/L (r(2)=0.9974). The detection limit was 26nmol/L with RSD of 2.8%. The number of binding sites and binding constant were 1.54 and 15.17L/mol, respectively. Copyright © 2014 Elsevier B.V. All rights reserved.

  8. Optimization for ultrasonic-microwave synergistic extraction of polysaccharides from Cornus officinalis and characterization of polysaccharides.

    Science.gov (United States)

    Yin, Xiulian; You, Qinghong; Jiang, Zhonghai; Zhou, Xinghai

    2016-02-01

    Ultrasonic-microwave synergistic extraction (UMSE) of polysaccharides from Cornus officinalis was optimized by response surface methodology (RSM). The effect of four different factors on the yield of C. officinalis polysaccharides (COP) was studied. RSM results showed that the optimal conditions were extraction time of 31.49823 min, microwave power of 99.39769 W, and water-to-raw material ratio of 28.16273. The COP yield was 11.38±0.31% using the modified optimal conditions, which was consistent with the value predicted by the model. The crude COP was purified by DEAE-Cellulose 52 chromatography and Sephadex G-100 chromatography. Five fractions, namely, crude COP, COP-1, COP-2, COP-3, and COP-4, were obtained. Monosaccharide composition analysis revealed that the COP was composed of glucose, arabinose, fucose, xylose, mannose, and rhamnose. Preliminary structural characterizations of COP were conducted by scanning electron microscopy and Fourier transform infrared spectroscopy. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Ultrasonic extraction of antioxidants from Chinese sumac (Rhus typhina L.) fruit using response surface methodology and their characterization.

    Science.gov (United States)

    Lai, Jixiang; Wang, Huifang; Wang, Donghui; Fang, Fang; Wang, Fengzhong; Wu, Tao

    2014-06-27

    For the first time, response surface methodology (RSM) using a Box-Behnken Design (BBD) was employed to optimize the conditions for ultrasonic assisted extraction (UAE) of antioxidants from Chinese sumac (Rhus typhina L.) fruits. Initially, influencing factors such as liquid-solid ratio, duration of ultrasonic assisted extraction, pH range, extraction temperature and ethanol concentration were identified using single-factor experiments. Then, with respect to the three most significant influencing factors, the extraction process focusing on the DPPH· scavenging capacity of antioxidants was optimized using RSM. Results showed that the optimal conditions for antioxidant extraction were 13.03:1 (mL/g) liquid-solid ratio, 16.86 min extraction time and 40.51% (v/v) ethanol, and the desirability was 0.681. The UPLC-ESI-MS analysis results revealed eleven kinds of phenolic compounds, including four major rare anthocyanins, among the antioxidants. All these results suggest that UAE is efficient at extracting antioxidants and has the potential to be used in industry for this purpose.

  10. Ultrasonic Extraction of Antioxidants from Chinese Sumac (Rhus typhina L. Fruit Using Response Surface Methodology and Their Characterization

    Directory of Open Access Journals (Sweden)

    Jixiang Lai

    2014-06-01

    Full Text Available For the first time, response surface methodology (RSM using a Box-Behnken Design (BBD was employed to optimize the conditions for ultrasonic assisted extraction (UAE of antioxidants from Chinese sumac (Rhus typhina L. fruits. Initially, influencing factors such as liquid-solid ratio, duration of ultrasonic assisted extraction, pH range, extraction temperature and ethanol concentration were identified using single-factor experiments. Then, with respect to the three most significant influencing factors, the extraction process focusing on the DPPH· scavenging capacity of antioxidants was optimized using RSM. Results showed that the optimal conditions for antioxidant extraction were 13.03:1 (mL/g liquid-solid ratio, 16.86 min extraction time and 40.51% (v/v ethanol, and the desirability was 0.681. The UPLC-ESI-MS analysis results revealed eleven kinds of phenolic compounds, including four major rare anthocyanins, among the antioxidants. All these results suggest that UAE is efficient at extracting antioxidants and has the potential to be used in industry for this purpose.

  11. Geometrical Feature Extraction from Ultrasonic Time Frequency Responses: An Application to Nondestructive Testing of Materials

    Directory of Open Access Journals (Sweden)

    Naranjo Valery

    2010-01-01

    Full Text Available Signal processing is an essential tool in nondestructive material characterization. Pulse-echo inspection with ultrasonic energy provides signals (A-scans that can be processed in order to obtain parameters which are related to physical properties of inspected materials. Conventional techniques are based on the use of a short-term frequency analysis of the A-scan, obtaining a time-frequency response (TFR, to isolate the evolution of the different frequency-dependent parameters. The application of geometrical estimators to TFRs provides an innovative way to complement conventional techniques based on the one-dimensional evolution of an A-scan extracted parameter (central or centroid frequency, bandwidth, etc.. This technique also provides an alternative method of obtaining similar meaning and less variance estimators. A comparative study of conventional versus new proposed techniques is presented in this paper. The comparative study shows that working with binarized TFRs and the use of shape descriptors provide estimates with lower bias and variance than conventional techniques. Real scattering materials, with different scatterer sizes, have been measured in order to demonstrate the usefulness of the proposed estimators to distinguish among scattering soft tissues. Superior results, using the proposed estimators in real measures, were obtained when classifying according to mean scatterer size.

  12. Response Surface Methodology Optimization of Ultrasonic-Assisted Extraction of Acer Truncatum Leaves for Maximal Phenolic Yield and Antioxidant Activity.

    Science.gov (United States)

    Yang, Lingguang; Yin, Peipei; Fan, Hang; Xue, Qiang; Li, Ke; Li, Xiang; Sun, Liwei; Liu, Yujun

    2017-02-04

    This study is the first to report the use of response surface methodology to improve phenolic yield and antioxidant activity of Acer truncatum leaves extracts (ATLs) obtained by ultrasonic-assisted extraction. The phenolic composition in ATLs extracted under the optimized conditions were characterized by UPLC-QTOF-MS/MS. Solvent and extraction time were selected based on preliminary experiments, and a four-factors-three-levels central composite design was conducted to optimize solvent concentration ( X ₁), material-to-liquid ratio ( X ₂), ultrasonic temperature ( X ₃) and power ( X ₄) for an optimal total phenol yield ( Y ₁) and DPPH• antioxidant activity ( Y ₂). The results showed that the optimal combination was ethanol:water ( v : v ) 66.21%, material-to-liquid ratio 1:15.31 g/mL, ultrasonic bath temperature 60 °C, power 267.30 W, and time 30 min with three extractions, giving a maximal total phenol yield of 7593.62 mg gallic acid equivalent/100 g d.w. and a maximal DPPH• antioxidant activity of 74,241.61 μmol Trolox equivalent/100 g d.w. Furthermore, 22 phenolics were first identified in ATL extract obtained under the optimized conditions, indicating that gallates, gallotannins, quercetin, myricetin and chlorogenic acid derivatives were the main phenolic components in ATL. What's more, a gallotannins pathway existing in ATL from gallic acid to penta- O -galloylglucoside was proposed. All these results provide practical information aiming at full utilization of phenolics in ATL, together with fundamental knowledge for further research.

  13. Optimization of ultrasonic-assisted extraction of antioxidant compounds from Guava (Psidium guajava L.) leaves using response surface methodology.

    Science.gov (United States)

    Kong, Fansheng; Yu, Shujuan; Feng, Zeng; Wu, Xinlan

    2015-01-01

    To optimization of extraction of antioxidant compounds from guava (Psidium guajava L.) leaves and showed that the guava leaves are the potential source of antioxidant compounds. The bioactive polysaccharide compounds of guava leaves (P. guajava L.) were obtained using ultrasonic-assisted extraction. Extraction was carried out according to Box-Behnken central composite design, and independent variables were temperature (20-60°C), time (20-40 min) and power (200-350 W). The extraction process was optimized by using response surface methodology for the highest crude extraction yield of bioactive polysaccharide compounds. The optimal conditions were identified as 55°C, 30 min, and 240 W. 1,1-diphenyl-2-picryl-hydrazyl and hydroxyl free radical scavenging were conducted. The results of quantification showed that the guava leaves are the potential source of antioxidant compounds.

  14. Use of a Combined Technology of Ultrasonication, Three-Phase Partitioning, and Aqueous Enzymatic Oil Extraction for the Extraction of Oil from Spirogyra sp.

    Directory of Open Access Journals (Sweden)

    Adisheshu Reddy

    2014-01-01

    Full Text Available Algal oil from Spirogyra sp. was extracted using a combined technology of ultrasonication, three-phase partitioning, and aqueous enzymatic oil extraction. Ultrasonication was done to rupture the cell wall and papain was used for an easier release of the trapped oil. The salt concentration for three-phase partitioning, preincubation period with (or without the protease, and its operational temperature were optimized for a maximum possible yield of the oil and the effect of ultrasonication, and three-phase partitioning with (or without the protease were studied. It was found that under optimized conditions at 50% ammonium sulphate concentration using tert-butanol (in 1 : 1, v/v ratio a presonicated and papain treated algal suspension could produce 24% (w/w, dry weight oil within few hours which was ten times higher as compared to the oil obtained by Soxhlet extraction using hexane and two times higher than the oil obtained without using the protease.

  15. Pipe Wall Thickness Monitoring Using Dry-Coupled Ultrasonic Waveguide Technique

    International Nuclear Information System (INIS)

    Cheong, Yong Moo; Kim, Ha Nam; Kim, Hong Pyo

    2012-01-01

    In order to monitor a corrosion or FAC (Flow Accelerated Corrosion) in a pipe, there is a need to measure pipe wall thickness at high temperature. Ultrasonic thickness gauging is the most commonly used non-destructive testing technique for wall thickness measurement. However, current commonly available ultrasonic transducers cannot withstand high temperatures, such as above 200 .deg. C. It is therefore necessary to carry out manual measurements during plant shutdowns. The current method thus reveals several disadvantages: inspection have to be performed during shutdowns with the possible consequences of prolonging down time and increasing production losses, insulation has to be removed and replaced for each manual measurement, and scaffolding has to be installed to inaccessible areas, resulting in considerable cost for interventions. It has been suggested that a structural health monitoring approach with permanently installed ultrasonic thickness gauges could have substantial benefits over current practices. The main reasons why conventional piezoelectric ultrasonic transducers cannot be used at high temperatures are that the piezo-ceramic becomes depolarized at temperature above the Curie temperature and because differential thermal expansion of the substrate, couplant, and piezoelectric materials cause failure. In this paper, a shear horizontal waveguide technique for wall thickness monitoring at high temperature is investigated. Two different designs for contact to strip waveguide are shown and the quality of output signal is compared and reviewed. After a success of acquiring high quality ultrasonic signal, experiment on the wall thickness monitoring at high temperature is planned

  16. Ultrasonic-assisted enzymatic extraction of phenolics from broccoli (Brassica oleracea L. var. italica) inflorescences and evaluation of antioxidant activity in vitro.

    Science.gov (United States)

    Wu, Hao; Zhu, Junxiang; Yang, Long; Wang, Ran; Wang, Chengrong

    2015-06-01

    An efficient ultrasonic-assisted enzymatic extraction technique was applied to extracting phenolics from broccoli inflorescences without organic solvents. The synergistic model of enzymolysis and ultrasonication simultaneously was selected, and the enzyme combination was optimized by orthogonal test: cellulase 7.5 mg/g FW (fresh weight), pectinase 10 mg/g FW, and papain 1.0 mg/g FW. The operating parameters in ultrasonic-assisted enzymatic extraction were optimized with response surface methodology using Box-Behnken design. The optimal extraction conditions were as follows: ultrasonic power, 440 W; liquid to material ratio, 7.0:1 mL/g; pH value of 6.0 at 54.5 ℃ for 10 min. Under these conditions, the extraction yield of phenolics achieved 1.816 ± 0.0187 mg gallic acid equivalents/gram FW. The free radical scavenging activity of ultrasonic-assisted enzymatic extraction extracts was determined by 1,1-diphenyl-2-picrylhydrazyl·assay with EC50 values of 0.25, and total antioxidant activity was determined by ferric reducing antioxidant power assay with ferric reducing antioxidant power value of 0.998 mmol FeSO4/g compared with the referential ascorbic acid of 1.184 mmol FeSO4/g. © The Author(s) 2014 Reprints and permissions: sagepub.co.uk/journalsPermissions.nav.

  17. Determination of bisphenol-type endocrine disrupting compounds in food-contact recycled-paper materials by focused ultrasonic solid-liquid extraction and ultra performance liquid chromatography-high resolution mass spectrometry.

    Science.gov (United States)

    Pérez-Palacios, David; Fernández-Recio, Miguel Ángel; Moreta, Cristina; Tena, María Teresa

    2012-09-15

    Focused ultrasonic solid-liquid extraction (FUSLE) and reverse-phase ultra performance liquid chromatography (UPLC) coupled to a quadrupole-time of flight mass spectrometer (Q-TOF-MS) was applied to the determination of bisphenol-type endocrine disrupting compounds (EDCs) in food-contact recycled-paper materials. Recycled paper is a potential source of EDCs. Bisphenol A (BPA), bisphenol F (BPF) and their derivatives bisphenol A diglycidyl ether (BADGE) and bisphenol F diglycidyl ether (BFDGE) are used for the production of epoxy resins employed in the formulation of printing inks. The FUSLE of bisphenol-type EDCs from packaging is reported for the first time. First, different extraction solvents were studied and methanol was selected. Then, the main FUSLE factors affecting the extraction efficiency (solvent volume, extraction time and ultrasonic irradiation power) were studied by means of a central composite design. The FUSLE conditions selected for further experiments were 20 ml of methanol at ultrasonic amplitude of 100% for 5s. Finally, the number of extraction cycles necessary for complete extraction was established in two. The analysis of the FUSLE extracts was carried out by UPLC-Q-TOF-MS with electrospray ionization and the determination of the four analytes took place in only 4 min. The FUSLE and UPLC-ESI-QTOF-MS method was validated and applied to the analysis of different food-contact recycled-paper-based materials and packaging. The proposed method provided recoveries from 72% to 97%, repeatability and intermediate precision under 9% and 14%, respectively, and detection limits of 0.33, 0.16, 0.65 and 0.40 μg/g for BPA, BPF, BADGE and BFDGE, respectively. The analysis of paper and cardboard samples confirmed the presence of EDCs in these packaging. Copyright © 2012 Elsevier B.V. All rights reserved.

  18. [Remediation efficiency of lead-contaminated soil at an industrial site by ultrasonic-assisted chemical extraction].

    Science.gov (United States)

    Wang, Xin-jie; Huang, Jin-lou; Liu, Zhi-qiang; Yue, Xi

    2013-09-01

    This research chose five lead-contaminated sites of a lead-acid battery factory to analyze the speciation distribution and concentration of lead. Under the same conditions (0.1 mol x L(-1) EDTA,30 min, 25 degrees C), the removal effect of heavy metal was compared between ultrasonic-assisted chemical extraction (UCE) and conventional chemical extraction ( CCE), and the variation of lead speciation was further explored. The results showed that the lead removal efficiency of UCE was significantly better than CCE. The lead removal efficiency of WS, A, B, C and BZ was 10.06%, 48.29%, 48.69%, 53.28% and 36.26% under CCE. While the removal efficiency of the UCE was 22.42%, 69.31%, 71.00%, 74.49% and 71.58%, with the average efficiency higher by 22%. By comparing the speciation distribution of the two washing methods, it was found that the acid extractable content maintained or decreased after UCE, whereas it showed an increasing trend after CCE. The reduction effect of the reducible was as high as 98% by UCE. UCE also showed a more efficient reduction effect of the organic matter-sulfite bounded form and the residual form. Hence, it is feasible to improve the washing efficiency of heavy metal contained in soil by conducting the cleaning process with the help of ultrasonic wave, which is a simple and fast mean to remove lead from contaminated sites.

  19. Multiple heavy metals extraction and recovery from hazardous electroplating sludge waste via ultrasonically enhanced two-stage acid leaching.

    Science.gov (United States)

    Li, Chuncheng; Xie, Fengchun; Ma, Yang; Cai, Tingting; Li, Haiying; Huang, Zhiyuan; Yuan, Gaoqing

    2010-06-15

    An ultrasonically enhanced two-stage acid leaching process on extracting and recovering multiple heavy metals from actual electroplating sludge was studied in lab tests. It provided an effective technique for separation of valuable metals (Cu, Ni and Zn) from less valuable metals (Fe and Cr) in electroplating sludge. The efficiency of the process had been measured with the leaching efficiencies and recovery rates of the metals. Enhanced by ultrasonic power, the first-stage acid leaching demonstrated leaching rates of 96.72%, 97.77%, 98.00%, 53.03%, and 0.44% for Cu, Ni, Zn, Cr, and Fe respectively, effectively separated half of Cr and almost all of Fe from mixed metals. The subsequent second-stage leaching achieved leaching rates of 75.03%, 81.05%, 81.39%, 1.02%, and 0% for Cu, Ni, Zn, Cr, and Fe that further separated Cu, Ni, and Zn from mixed metals. With the stabilized two-stage ultrasonically enhanced leaching, the resulting over all recovery rates of Cu, Ni, Zn, Cr and Fe from electroplating sludge could be achieved at 97.42%, 98.46%, 98.63%, 98.32% and 100% respectively, with Cr and Fe in solids and the rest of the metals in an aqueous solution discharged from the leaching system. The process performance parameters studied were pH, ultrasonic power, and contact time. The results were also confirmed in an industrial pilot-scale test, and same high metal recoveries were performed. Copyright 2010 Elsevier B.V. All rights reserved.

  20. Optimization of ultrasonic-assisted extraction of total carotenoids from peach palm fruit (Bactris gasipaes) by-products with sunflower oil using response surface methodology.

    Science.gov (United States)

    Ordóñez-Santos, Luis Eduardo; Pinzón-Zarate, Lina Ximena; González-Salcedo, Luis Octavio

    2015-11-01

    The present study reports on the extraction of total carotenoids from peach palm fruit by-products with sunflower oil. Response surface methodology (RSM) was used to investigate the effect of process variables on the ultrasound-assisted extraction (UAE). Three independent variables including ultrasonic intensity (764-1528, W/m(2)), temperature (25-45°C), and the extraction time (10-30 min). According to the results, the optimal UAE condition was obtained with an ultrasonic intensity of 1528 W/m(2), extraction temperature of 35°C and extraction time of 30 min. At these conditions, extraction maximum extraction of total carotenoids as 163.47 mg/100 g dried peel. The experimental values under optimal condition were in good consistent with the predicted values. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Optimization of Ultrasonic-Assisted Extraction of Flavonoid Compounds and Antioxidants from Alfalfa Using Response Surface Method

    Directory of Open Access Journals (Sweden)

    Chang-Liang Jing

    2015-08-01

    Full Text Available Ultrasonic-assisted extraction (UAE was used to extract flavonoid-enriched antioxidants from alfalfa aerial part. Response surface methodology (RSM, based on a four-factor, five-level central composite design (CCD, was employed to obtain the optimal extraction parameters, in which the flavonoid content was maximum and the antioxidant activity of the extracts was strongest. Radical scavenging capacity of the extracts, which represents the amounts of antioxidants in alfalfa, was determined by using 2,2′-azino-bis (3-ethylbenzothiazoline-6-sulphonicacid (ABTS and 2,2′-diphenyl-1-picrylhydrazyl (DPPH methods. The results showed good fit with the proposed models for the total flavonoid extraction (R2 = 0.9849, for the antioxidant extraction assayed by ABTS method (R2 = 0.9764, and by DPPH method (R2 = 0.9806. Optimized extraction conditions for total flavonoids was a ratio of liquid to solid of 57.16 mL/g, 62.33 °C, 57.08 min, and 52.14% ethanol. The optimal extraction parameters of extracts for the highest antioxidant activity by DPPH method was a ratio of liquid to solid 60.3 mL/g, 54.56 °C, 45.59 min, and 46.67% ethanol, and by ABTS assay was a ratio of liquid to solid 47.29 mL/g, 63.73 °C, 51.62 min, and 60% ethanol concentration. Our work offers optimal extraction conditions for total flavonoids and antioxidants from alfalfa.

  2. Optimization of Ultrasonic-Assisted Extraction of Flavonoid Compounds and Antioxidants from Alfalfa Using Response Surface Method.

    Science.gov (United States)

    Jing, Chang-Liang; Dong, Xiao-Fang; Tong, Jian-Ming

    2015-08-26

    Ultrasonic-assisted extraction (UAE) was used to extract flavonoid-enriched antioxidants from alfalfa aerial part. Response surface methodology (RSM), based on a four-factor, five-level central composite design (CCD), was employed to obtain the optimal extraction parameters, in which the flavonoid content was maximum and the antioxidant activity of the extracts was strongest. Radical scavenging capacity of the extracts, which represents the amounts of antioxidants in alfalfa, was determined by using 2,2'-azino-bis (3-ethylbenzothiazoline-6-sulphonicacid) (ABTS) and 2,2'-diphenyl-1-picrylhydrazyl (DPPH) methods. The results showed good fit with the proposed models for the total flavonoid extraction (R² = 0.9849), for the antioxidant extraction assayed by ABTS method (R² = 0.9764), and by DPPH method (R² = 0.9806). Optimized extraction conditions for total flavonoids was a ratio of liquid to solid of 57.16 mL/g, 62.33 °C, 57.08 min, and 52.14% ethanol. The optimal extraction parameters of extracts for the highest antioxidant activity by DPPH method was a ratio of liquid to solid 60.3 mL/g, 54.56 °C, 45.59 min, and 46.67% ethanol, and by ABTS assay was a ratio of liquid to solid 47.29 mL/g, 63.73 °C, 51.62 min, and 60% ethanol concentration. Our work offers optimal extraction conditions for total flavonoids and antioxidants from alfalfa.

  3. Research on Effective Electric-Mechanical Coupling Coefficient of Sandwich Type Piezoelectric Ultrasonic Transducer Using Bending Vibration Mode

    Directory of Open Access Journals (Sweden)

    Qiang Zhang

    2015-01-01

    Full Text Available An analytical model on electromechanical coupling coefficient and the length optimization of a bending piezoelectric ultrasonic transducer are proposed. The piezoelectric transducer consists of 8 PZT elements sandwiched between four thin electrodes, and the PZT elements are clamped by a screwed connection between fore beam and back beam. Firstly, bending vibration model of the piezoelectric transducer is built based on the Timoshenko beam theory. Secondly, the analytical model of effective electromechanical coupling coefficient is built based on the bending vibration model. Energy method and electromechanical equivalent circuit method are involved in the modelling process. To validate the analytical model, sandwich type piezoelectric transducer example in second order bending vibration mode is analysed. Effective electromechanical coupling coefficient of the transducer is optimized with simplex reflection technique, and the optimized ratio of length of the transducers is obtained. Finally, experimental prototypes of the sandwich type piezoelectric transducers are fabricated. Bending vibration mode and impedance of the experimental prototypes are tested, and electromechanical coupling coefficient is obtained according to the testing results. Results show that the analytical model is in good agreement with the experimental model.

  4. Novel Budesonide Particles for Dry Powder Inhalation Prepared Using a Microfluidic Reactor Coupled With Ultrasonic Spray Freeze Drying.

    Science.gov (United States)

    Saboti, Denis; Maver, Uroš; Chan, Hak-Kim; Planinšek, Odon

    2017-07-01

    Budesonide (BDS) is a potent active pharmaceutical ingredient, often administered using respiratory devices such as metered dose inhalers, nebulizers, and dry powder inhalers. Inhalable drug particles are conventionally produced by crystallization followed by milling. This approach tends to generate partially amorphous materials that require post-processing to improve the formulations' stability. Other methods involve homogenization or precipitation and often require the use of stabilizers, mostly surfactants. The purpose of this study was therefore to develop a novel method for preparation of fine BDS particles using a microfluidic reactor coupled with ultrasonic spray freeze drying, and hence avoiding the need of additional homogenization or stabilizer use. A T-junction microfluidic reactor was employed to produce particle suspension (using an ethanol-water, methanol-water, and an acetone-water system), which was directly fed into an ultrasonic atomization probe, followed by direct feeding to liquid nitrogen. Freeze drying was the final preparation step. The result was fine crystalline BDS powders which, when blended with lactose and dispersed in an Aerolizer at 100 L/min, generated fine particle fraction in the range 47.6% ± 2.8% to 54.9% ± 1.8%, thus exhibiting a good aerosol performance. Subsequent sample analysis confirmed the suitability of the developed method to produce inhalable drug particles without additional homogenization or stabilizers. The developed method provides a viable solution for particle isolation in microfluidics in general. Copyright © 2017 American Pharmacists Association®. All rights reserved.

  5. Extraction of flavonoids from garden (Salvia officinalis L. and glutinous (Salvia glutinosa L. sage by ultrasonic and classical maceration

    Directory of Open Access Journals (Sweden)

    DRAGAN T. VELICKOVIC

    2007-01-01

    Full Text Available Flavonoids were analysed in the extracts of garden (Salvia officinalis L. and glutinous (Salvia glutinosa L. sage. Ultrasonic extraction (20 minutes at 40 °C and classical maceration (6 h at room temperature of the extractable substances from dried herbs and dried residual plant materials from which the essential oil had previously been removed by hydrodistillation were performed with petroleum ether, 70 % aqueous solution of ethanol and water. It was found that the extracts from both plants contained flavonoids, but their compositions were dependent of the plant species, the polarity of the extracting solvent and the extraction technique applied. Apigenin and its derivatives (e.g., apigenin 4'-methyl ether, scutellarein 6-methyl ether, isoscutellarein 8-methyl ether, luteolin and 6-OH-luteolin-6-methyl ether where distinctive for S. officinalis. Apigenin, luteolin, 6-OH-luteolin-6-methyl ether, kaempherol 3-methyl ether, kaempherol 3,7-dimethyl ether, quercetin 3,7,3'-trimethyl ether and quercetin 3,7,3',4'-tetramethyl ether were distinctive for S. glutinosa. The flavonoids were also detected in considerable quantities in the plant material from which the essential oils had been already removed. Hence, this industrial waste plant material might be further used as a source of the flavonoids.

  6. Multi-target determination of organic ultraviolet absorbents in organism tissues by ultrasonic assisted extraction and ultra-high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Peng, Xianzhi; Jin, Jiabin; Wang, Chunwei; Ou, Weihui; Tang, Caiming

    2015-03-06

    A sensitive and reliable method was developed for multi-target determination of 13 most widely used organic ultraviolet (UV) absorbents (including UV filters and UV stabilizers) in aquatic organism tissues. The organic UV absorbents were extracted using ultrasonic-assisted extraction, purified via gel permeation chromatography coupled with silica gel column chromatography, and determined by ultra-high performance liquid chromatography-tandem mass spectrometry. Recoveries of the UV absorbents from organism tissues mostly ranged from 70% to 120% from fish filet with satisfactory reproducibility. Method quantification limits were 0.003-1.0ngg(-1) dry weight (dw) except for 2-ethylhexyl 4-methoxycinnamate. This method has been applied to analysis of the UV absorbents in wild and farmed aquatic organisms collected from the Pearl River Estuary, South China. 2-Hydroxy-4-methoxybenzophenone and UV-P were frequently detected in both wild and farmed marine organisms at low ngg(-1)dw. 3-(4-Methylbenzylidene)camphor and most of the benzotriazole UV stabilizers were also frequently detected in maricultured fish. Octocrylene and 2-ethylhexyl 4-methoxycinnamate were not detected in any sample. This work lays basis for in-depth study about bioaccumulation and biomagnification of the UV absorbents in marine environment. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Copper clean-up procedure for ultrasonic extraction and analysis of pyrethroid and phenylpyrazole pesticides in sediments by gas chromatography-electron capture detection

    International Nuclear Information System (INIS)

    Wu Jun; Lin Youjian; Lu Jian; Wilson, Chris

    2011-01-01

    A rapid ultrasonic extraction method coupled with a heated-copper clean-up procedure for removing interfering constituents was developed for analyzing pyrethroid and phenylpyrazole pesticides in sediments. Incubation of the 60 mL extract with 12 g copper granules at 60 o C for 2 h was determined to be the optimal conditions for removing the interfering constituents. Eleven pyrethroid and phenylpyrazole pesticides were spiked into sediment samples to determine the effectiveness of the ultrasonic extraction method. The average recoveries of pyrethroids and phenylpyrazoles in sediment at 4 o C storage on day 0, 1, 7, 14, and 21 ranged from 98.6 to 120.0%, 79.2 to 116.0%, 85.0 to 119.7%, 93.6 to 118.7%, and 92.1 to 118.2%, respectively, with all percent relative standard deviations less than 10% (most o C. Recoveries of the pesticides ranged from 98.6% to 120.0% for lowest fortification level (2-16 μg kg -1 ), from 97.8% to 117.9% for middle fortification level (10-80 μg kg -1 ), and from 94.3% to 118.1% for highest fortification level (20-160 μg kg -1 ). Relative standard deviations of pesticide recoveries were usually less than 7%. Method detection limits of target pesticides ranged from 0.22 μg kg -1 to 3.72 μg kg -1 . Furthermore, field sediment samples collected from four residential lakes during a three-month monitoring period were analyzed to evaluate the effectiveness of this method. Bifenthrin was detected in all of sediment samples (highest concentration 260.33 ± 41.71 μg kg -1 , lowest concentration 5.68 ± 0.38 μg kg -1 ), and fipronil sulfone was detected at least once in sediment samples collected from three sites with concentrations ranging from 1.73 ± 0.53 to 7.53 ± 0.01 μg kg -1 . - Highlights: → A rapid extraction and copper-based clean-up method was developed. → Recoveries after storage at 4 o C for 21 d ranged from 79.2 to 120.0%. → Percent relative standard deviations less than 10% (most -1 to 3.72 μg kg -1 .

  8. Rapid determination of volatile constituents in safflower from Xinjiang and Henan by ultrasonic-assisted solvent extraction and GC–MS

    OpenAIRE

    Jia, Ling-Han; Liu, Yi; Li, Yu-Zhen

    2011-01-01

    The total volatile components were extracted from safflower by ultrasonic-assisted solvent extraction (USE) and their chemical constituents were analyzed by gas chromatographyâmass spectrometry (GCâMS) to provide scientific basis for the quality control of safflower. Five different solvents (diethyl ether, ethanol, ethyl acetate, dichloromethane and acetone) were used and compared in terms of number of volatile components extracted and the peak areas of these components in TIC. The results sh...

  9. Triple degree-of-freedom piezoelectric ultrasonic micromotor via flexural-axial coupled vibration.

    Science.gov (United States)

    Khoo, Ter Fong; Dang, Dinh Huy; Friend, James; Oetomo, Denny; Yeo, Leslie

    2009-08-01

    Actuators remain a limiting factor in robotics, especially in microrobotics where the power density of actuators is a problem. A 3 x 3 x 8.7 mm 3-axis piezoelectric ultrasonic micromotor system is described here in an effort to help solve this problem. Formed from 4 bulk lead zirconate titanate (PZT) thickness-polarized elements placed around the periphery of a rectangular rod, the stator is designed to combine axial and flexural vibrations in a way that permits rotation of a hardened steel ball as a rotor about an arbitrary axis. A simple prototype of the micromotor was found to produce at least a rotation speed of 10.4 rad/s with 4 microN-m torque about all 3 orthogonal directions at an excitation frequency of about 221 kHz, demonstrating the feasibility of a 3 degree-of-freedom millimeter-scale piezoelectric motor.

  10. Optimization of ultrasonic-assisted extraction of phenolic antioxidants from Malus baccata (Linn.) Borkh. using response surface methodology.

    Science.gov (United States)

    Wang, Lu; Wang, Zhenyu; Li, Xiaoyu

    2013-05-01

    In this study, the optimum extraction conditions for maximum recovery of the content of total phenolics (TPC) and total antioxidant abilities were analyzed for Malus baccata (Linn.) Borkh. using response surface methodology. The effects of ethanol percentage (X1 ,%), ultrasonic power (X2 , W) and extraction temperature (X3 , °C) on the total phenolic content (Y1 ) and antioxidant ability (Y2 ) were evaluated. A second-order polynomial model produced a satisfactory fitting of the experimental data with regard to total phenolic content (R(2) = 0.9942, P antioxidant ability (R(2) = 0.9966, P extraction temperature of 51.1°C for TPC and 60.5%, 311.4 W, 51.6°C for antioxidant ability, the predicted values agreed well with the experimental values. Results implied that the major phenolic compounds in obtained extracts as chlorogenic acid, quercetin-3-gal/glu, quercetin-3-xyl/ara, phloretin-2-xyloside, quercetin-3- rhamnoside, and phloridzin. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Analysis of Trace Quaternary Ammonium Compounds (QACs) in Vegetables Using Ultrasonic-Assisted Extraction and Gas Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Xiang, Lei; Wang, Xiong-Ke; Li, Yan-Wen; Huang, Xian-Pei; Wu, Xiao-Lian; Zhao, Hai-Ming; Li, Hui; Cai, Quan-Ying; Mo, Ce-Hui

    2015-08-05

    A reliable, sensitive, and cost-effective method was developed for determining three quaternary ammonium compounds (QACs) including dodecyltrimethylammonium chloride, cetyltrimethylammonium chloride, and didodecyldimethylammonium chloride in various vegetables using ultrasonic-assisted extraction and gas chromatography-mass spectrometry. The variety and acidity of extraction solvents, extraction times, and cleanup efficiency of sorbents were estimated to obtain an optimized procedure for extraction of the QACs in nine vegetable matrices. Excellent linearities (R(2) > 0.992) were obtained for the analytes in the nine matrices. The limits of detection and quantitation were 0.7-6.0 and 2.3-20.0 μg/kg (dry weight, dw) in various matrices, respectively. The recoveries in the nine matrices ranged from 70.5% to 108.0% with relative standard deviations below 18.0%. The developed method was applied to determine the QACs in 27 vegetable samples collected from Guangzhou in southern China, showing very high detection frequency with a concentration of 23-180 μg/kg (dw).

  12. Optimization of oil yield from Hevea brasiliensis seeds through ultrasonic-assisted solvent extraction via response surface methodology

    Directory of Open Access Journals (Sweden)

    Val Irvin F. Mabayo

    2018-01-01

    Full Text Available The demand for oil has been increasing vastly over time, and the source of this has slowly been diminishing. The use of non-food feedstock is seen as a promising alternative source for the production of bio-based fuel. In this study, rubber (Hevea brasiliensis seeds were utilized as biomass in bio-oil production considering that these are non-edible and considered wastes in rubber tree plantations. In the oil extraction process, the rubber seed kernels were oven dried at 100 °C for 24 h, powdered and then dried further at 105 °C for 4 h. After characterization, optimization study was done using Design Expert 7.0 software through central composite design of the response surface methodology. Ultrasonication technology was employed in the oil extraction process which significantly reduced the reaction time needed for extraction to 15 min compared the conventional extraction method of at least 8 h. An optimum rubber seed oil (RSO yield of 30.3 ± 0.3% was obtained using 15 g biomass, 5:1 n-hexane to biomass (mL g−1 ratio, 50 μm resonance amplitude and 60 ± 5 °C temperature at 15 min reaction time. The oil yield at optimum condition was found to have 0.89 g mL−1 density at room temperature, 26.7 cSt kinematic viscosity at 40 °C and high heating value of 39.2 MJ kg−1. The Fourier Transform Infrared Radiation spectroscopy analysis of the RSO, at optimum condition, showed the presence of carboxylic acid and ester carbonyl functional groups which are good indicators as a potential source of biodiesel. Keywords: Hevea brasiliensis, Oil extraction, Optimization, Response surface methodology, Rubber seed oil, Ultrasonic-assisted solvent extraction

  13. Microwave-assisted extraction and ultrasonic extraction to determine polycyclic aromatic hydrocarbons in needles and bark of Pinus pinaster Ait. and Pinus pinea L. by GC-MS.

    Science.gov (United States)

    Ratola, Nuno; Lacorte, Sílvia; Barceló, Damià; Alves, Arminda

    2009-01-15

    Two different extraction strategies (microwave-assisted extraction (MAE) and ultrasonic extraction (USE)) were tested in the extraction of the 16 US Environmental Protection Agency (EPA) polycyclic aromatic hydrocarbons (PAHs) from pine trees. Extraction of needles and bark from two pine species common in the Iberian Peninsula (Pinus pinaster Ait. and Pinus pinea L.) was optimized using two amounts of sample (1g and 5 g) and two PAHs spiking levels (20 ng/g and 100 ng/g). In all cases, the clean-up procedure following extraction consisted in solid-phase extraction (SPE) with alumina cartridges. Quantification was done by gas chromatography (GC) with mass spectrometry (MS), using five deuterated PAH surrogate standards as internal standards. Limits of detection were globally below 0.2 ng/g. The method was robust for the matrices studied regardless of the extraction procedures. Recovery values between 70 and 130% were reached in most cases, except for high molecular weight PAHs (indeno[1,2,3-cd]pyrene, dibenzo[a,h]anthracene and benzo[ghi]perylene). A field study with naturally contaminated samples from eight sites (four in Portugal and four in Catalonia, Spain) showed that needles are more suitable biomonitors for PAHs, yielding concentrations from 2 to 17 times higher than those found in bark. The levels varied according to the sampling site, with the sum of the individual PAH concentrations between 213 and 1773 ng/g (dry weight). Phenanthrene was the most abundant PAH, followed by fluoranthene, naphthalene and pyrene.

  14. Multielement detection limits and sample nebulization efficiencies of an improved ultrasonic nebulizer and a conventional pneumatic nebulizer in inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

    Olson, K.W.; Haas, W.J. Jr.; Fassel, V.A.

    1977-01-01

    Two important aspects of the analytical performance of a newly developed ultrasonic nebulizer and a specially designed pneumatic nebulizer have been compared for use in inductively coupled plasma--atomic emission spectroscopy (ICP-AES). The ultrasonic nebulizer, when combined with a conventional aerosol desolvation apparatus, provided an order of magnitude or more improvement in simultaneous multielement detection limits as compared to those obtained when the pneumatic nebulizer was used either with or without desolvation. Application of a novel method for direct measurement of the overall efficiency of nebulization to the two systems showed that an approximately tenfold greater rate of sample delivery to the plasma torch was primarily responsible for the superior detection limits afforded by the ultrasonic nebulizer. A unique feature of the ultrasonic nebulizer described is the protection against chemical attack which is achieved by completely enclosing the transducer in an acoustically coupled borosilicate glass cylinder. Direct sample introduction, convenient sample change, and rapid cleanout are other important characteristics of the system which make it an attractive alternate to pneumatic nebulizer systems

  15. Ultrasonic Testing

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Hyeong Jun; Kuk, Jeong Han

    2002-02-15

    This book introduces ultrasonic testing, which tells of outline of ultrasonic testing, principle of ultrasonic testing, prosperities of ultrasonic waves, radiographic test and ultrasonic test, basic theory on ultrasonic testing, mode conversion, transmission and diffraction, ultrasonic flaw detection and probe, standard test piece and reference test piece, like KS(JIS) ASME and ASTM, classification and properties of ultrasonic testing, straight beam method, angle beam method, ASME SEC.V.Art.5 ASTMA 388 and KS B 0817 Korean industrial standard.

  16. Ionic Liquid-Based Ultrasonic-Assisted Extraction of Secoisolariciresinol Diglucoside from Flaxseed (Linum usitatissimum L. with Further Purification by an Aqueous Two-Phase System

    Directory of Open Access Journals (Sweden)

    Zhi-Jian Tan

    2015-09-01

    Full Text Available In this work, a two-step extraction methodology of ionic liquid-based ultrasonic-assisted extraction (IL-UAE and ionic liquid-based aqueous two-phase system (IL-ATPS was developed for the extraction and purification of secoisolariciresinol diglucoside (SDG from flaxseed. In the IL-UAE step, several kinds of ILs were investigated as the extractants, to identify the IL that affords the optimum extraction yield. The extraction conditions such as IL concentration, ultrasonic irradiation time, and liquid–solid ratio were optimized using response surface methodology (RSM. In the IL-ATPS step, ATPS formed by adding kosmotropic salts to the IL extract was used for further separation and purification of SDG. The most influential parameters (type and concentration of salt, temperature, and pH were investigated to obtain the optimum extraction efficiency. The maximum extraction efficiency was 93.35% under the optimal conditions of 45.86% (w/w IL and 8.27% (w/w Na2SO4 at 22 °C and pH 11.0. Thus, the combination of IL-UAE and IL-ATPS makes up a simple and effective methodology for the extraction and purification of SDG. This process is also expected to be highly useful for the extraction and purification of bioactive compounds from other important medicinal plants.

  17. Optimization of ultrasonic-assisted extraction of bioactive alkaloid compounds from rhizoma coptidis (Coptis chinensis Franch.) using response surface methodology.

    Science.gov (United States)

    Teng, Hui; Choi, Yong Hee

    2014-01-01

    The optimum extraction conditions for the maximum recovery of total alkaloid content (TAC), berberine content (BC), palmatine content (PC), and the highest antioxidant capacity (AC) from rhizoma coptidis subjected to ultrasonic-assisted extraction (UAE) were determined using response surface methodology (RSM). Central composite design (CCD) with three variables and five levels was employed, and response surface plots were constructed in accordance with a second order polynomial model. Analysis of variance (ANOVA) showed that the quadratic model was well fitted and significant for responses of TAC, BC, PC, and AA. The optimum conditions obtained through the overlapped contour plot were as follows: ethanol concentration of 59%, extraction time of 46.57min, and temperature of 66.22°C. Verification experiment was carried out, and no significant difference was found between observed and estimated values for each response, suggesting that the estimated models were reliable and valid for UAE of alkaloids. Crown Copyright © 2013. Published by Elsevier Ltd. All rights reserved.

  18. Ceratonia siliqua L. hydroethanolic extract obtained by ultrasonication: antioxidant activity, phenolic compounds profile and effects in yogurts functionalized with their free and microencapsulated forms.

    Science.gov (United States)

    Rached, Irada; Barros, Lillian; Fernandes, Isabel P; Santos-Buelga, Celestino; Rodrigues, Alírio E; Ferchichi, Ali; Barreiro, Maria Filomena; Ferreira, Isabel C F R

    2016-03-01

    Bioactive extracts were obtained from powdered carob pulp through an ultrasound extraction process and then evaluated in terms of antioxidant activity. Ten minutes of ultrasonication at 375 Hz were the optimal conditions leading to an extract with the highest antioxidant effects. After its chemical characterization, which revealed the preponderance of gallotannins, the extract (free and microencapsulated) was incorporated in yogurts. The microspheres were prepared using an extract/sodium alginate ratio of 100/400 (mg mg(-1)) selected after testing different ratios. The yogurts with the free extract exhibited higher antioxidant activity than the samples added with the encapsulated extracts, showing the preserving role of alginate as a coating material. None of the forms significantly altered the yogurt's nutritional value. This study confirmed the efficiency of microencapsulation to stabilize functional ingredients in food matrices maintaining almost the structural integrity of polyphenols extracted from carob pulp and furthermore improving the antioxidant potency of the final product.

  19. Determination of hexachlorobutadiene, pentachlorobenzene, and hexachlorobenzene in waste incineration fly ash using ultrasonic extraction followed by column cleanup and GC-MS analysis.

    Science.gov (United States)

    Zhang, Haiyan; Jiang, Lei; Zhou, Xin; Zeng, Tao; He, Zhiqiao; Huang, Xinwen; Chen, Jianmeng; Song, Shuang

    2018-03-01

    Hexachlorobutadiene (HCBD) was listed as a new controlling persistent organic pollutant in the Stockholm Convention because of its wide industrial applications and potential genotoxicity and carcinogenicity. However, only limited information exists on the release of HCBD from unintentional sources, such as waste incineration. Identification and quantification of HCBD in fly ash, one of the major outputs of waste incineration, is imperative. This work presents a simple method for determining HCBD in waste incineration fly ash based on ultrasonic extraction coupled with a silica gel-Florisil column cleanup followed by gas chromatography-mass spectrometry detection. Two typical persistent organic pollutants, pentachlorobenzene (PeCB) and hexachlorobenzene (HCB), were measured simultaneously. The parameters that influence the extraction efficiency and the quality of instrument detection were studied. Under the optimum experimental conditions, high sensitivity (detection limit 0.25-0.53 ng g -1 ), acceptable recoveries (64.0-71.4%) at spiking levels of 5-500 ng g -1 , and good repeatability [relative standard deviation (n = 3) of 14% or less] were achieved for all target analytes. The validation of this method was performed by analysis of six real fly ash samples from different waste incinerators in eastern China. The concentrations of HCBD detected in these samples (1.39-97.6 ng g -1 ) were comparable to those of PeCB (1.22-150 ng g -1 ) and HCB (0.82-120 ng g -1 ), indicating that the residual HCBD as well as PeCB and HCB in waste incineration fly ash should not be ignored. The results confirm for the first time that waste incineration is an unintentional source of HCBD in China. Graphical abstract An analytical method for hexachlorobutadiene, pentachlorobenzene, and hexachlorobenzene in fly ash from waste incineration. GC-MS gas chromatography-mass spectrometry, Ph-d10 phenanthrene-d 10 .

  20. Effect of Ultrasonic Extraction on Production and Structural Changes of C-Phycocyanin from Marine Spirulina maxima.

    Science.gov (United States)

    Choi, Woon Yong; Lee, Hyeon Yong

    2018-01-11

    This work first showed that very high amounts of phycocyanins, such as 11.3 mg/mL C-phycocyanin (C-PC), 3.1 mg/mL allophycocyanin (APC), and 0.8 mg/mL phycoerythrin (PE), can be obtained using an ultrasonic extraction process (UE) with a 60 kHz frequency and 3 h of process time at 25 °C, without any other pretreatments. These yields were higher than those from most conventional water extractions at 4 °C for 24 h (Control condition) or at 25 °C for 24 h (WE), namely, 9.8 and 5.7 mg/mL C-PC, 2.3 and 1.2 mg/mL APC, and 0.7 and 0.3 mg/mL PE, respectively. These yields were also shown to be even higher than yields from other reported data. Structural changes in C-PC in the extracts were also found for the first time, according to extraction conditions, showing that the total concentration of C-PC and of the α-subunit of C-PC in the UE were much higher than in the WE, with little difference in the amount of β-subunit of C-PC in the UE or WE. It was also shown that the structural changes in C-PC in the WE decreased both antioxidant and anti-inflammation activities-29.83% vs. 32.09% of α,α-diphenyl-β-picrylhydrazyl (DPPH) scavenging activity and 8.21 vs. 7.25 µM of NO production for the WE and UE, respectively-while the UE, with similar patterns to standard C-PC, showed very high biological effects, which may suggest that the biologically active part is the α-subunit of C-PC, not the β-subunit.

  1. Effect of Ultrasonic Extraction on Production and Structural Changes of C-Phycocyanin from Marine Spirulina maxima

    Directory of Open Access Journals (Sweden)

    Woon Yong Choi

    2018-01-01

    Full Text Available This work first showed that very high amounts of phycocyanins, such as 11.3 mg/mL C-phycocyanin (C-PC, 3.1 mg/mL allophycocyanin (APC, and 0.8 mg/mL phycoerythrin (PE, can be obtained using an ultrasonic extraction process (UE with a 60 kHz frequency and 3 h of process time at 25 °C, without any other pretreatments. These yields were higher than those from most conventional water extractions at 4 °C for 24 h (Control condition or at 25 °C for 24 h (WE, namely, 9.8 and 5.7 mg/mL C-PC, 2.3 and 1.2 mg/mL APC, and 0.7 and 0.3 mg/mL PE, respectively. These yields were also shown to be even higher than yields from other reported data. Structural changes in C-PC in the extracts were also found for the first time, according to extraction conditions, showing that the total concentration of C-PC and of the α-subunit of C-PC in the UE were much higher than in the WE, with little difference in the amount of β-subunit of C-PC in the UE or WE. It was also shown that the structural changes in C-PC in the WE decreased both antioxidant and anti-inflammation activities—29.83% vs. 32.09% of α,α-diphenyl-β-picrylhydrazyl (DPPH scavenging activity and 8.21 vs. 7.25 µM of NO production for the WE and UE, respectively—while the UE, with similar patterns to standard C-PC, showed very high biological effects, which may suggest that the biologically active part is the α-subunit of C-PC, not the β-subunit.

  2. Artificial Intelligence Assists Ultrasonic Inspection

    Science.gov (United States)

    Schaefer, Lloyd A.; Willenberg, James D.

    1992-01-01

    Subtle indications of flaws extracted from ultrasonic waveforms. Ultrasonic-inspection system uses artificial intelligence to help in identification of hidden flaws in electron-beam-welded castings. System involves application of flaw-classification logic to analysis of ultrasonic waveforms.

  3. Determination of low cadmium concentrations in wine by on-line preconcentration in a knotted reactor coupled to an inductively coupled plasma optical emission spectrometer with ultrasonic nebulization

    Energy Technology Data Exchange (ETDEWEB)

    Lara, R.F. [Inst. de Investigaciones Mineras, Universidad Nacional de San Juan (Argentina); Wuilloud, R.G.; Salonia, J.A. [Dept. of Analytical Chemistry, National University of San Luis (Argentina); Olsina, R.A.; Martinez, L.D. [Dept. of Analytical Chemistry, National University of San Luis (Argentina); Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET) (Argentina)

    2001-12-01

    An on-line cadmium preconcentration and determination system implemented with inductively coupled plasma optical emission spectrometry (ICP-OES) associated to flow injection (FI) with ultrasonic nebulization system (USN) was studied. The cadmium was retained as the cadmium-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol, Cd-(5-Br-PADAP), complex, at pH 9.5. The cadmium complex was removed from the knotted reactor (KR) with 3.0 mol/L nitric acid. A total enhancement factor of 216 was obtained with respect to ICP-OES using pneumatic nebulization (12 for USN and 18 for KR) with a preconcentration time of 60 s. The value of the detection limit for the preconcentration of 5 mL of sample solution was 5 ng/L. The precision for 10 replicate determinations at the 5 {mu}g/L Cd level was 2.9% relative standard deviation (RSD), calculated from the peak heights obtained. The calibration graph using the preconcentration system for cadmium was linear with a correlation coefficient of 0.9998 at levels near the detection limits up to at least 1000 {mu}g/L. The method was successfully applied to the determination of cadmium in wine samples. (orig.)

  4. Ultrasonically extracted β-d-glucan from artificially cultivated mushroom, characteristic properties and antioxidant activity.

    Science.gov (United States)

    Alzorqi, Ibrahim; Sudheer, Surya; Lu, Ting-Jang; Manickam, Sivakumar

    2017-03-01

    Ganoderma mushroom cultivated recently in Malaysia to produce chemically different nutritional fibers has attracted the attention of the local market. The extraction methods, molecular weight and degree of branching of (1-3; 1-6)-β-d-glucan polysaccharides is of prime importance to determine its antioxidant bioactivity. Therefore three extraction methods i.e. hot water extraction (HWE), soxhlet extraction (SE) and ultrasound assisted extraction (US) were employed to study the total content of (1-3; 1-6)-β-d-glucans, degree of branching, structural characteristics, monosaccharides composition, as well as the total yield of polysaccharides that could be obtained from the artificially cultivated Ganoderma. The physical characteristics by HPAEC-PAD, HPGPC and FTIR, as well as the antioxidant in vitro assays of DPPH scavenging activity and ferric reducing power (FRAP) indicated that (1-3; 1-6)-β-d-glucans of Malaysian mushroom have better antioxidant activity, higher molecular weight and optimal degree of branching when extracted by US in comparison with conventional methods. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Optimization of Ionic Liquid Based Simultaneous Ultrasonic- and Microwave-Assisted Extraction of Rutin and Quercetin from Leaves of Velvetleaf (Abutilon theophrasti by Response Surface Methodology

    Directory of Open Access Journals (Sweden)

    Chunjian Zhao

    2014-01-01

    Full Text Available An ionic liquids based simultaneous ultrasonic and microwave assisted extraction (ILs-UMAE method has been proposed for the extraction of rutin (RU, quercetin (QU, from velvetleaf leaves. The influential parameters of the ILs-UMAE were optimized by the single factor and the central composite design (CCD experiments. A 2.00 M 1-butyl-3-methylimidazolium bromide ([C4mim]Br was used as the experimental ionic liquid, extraction temperature 60°C, extraction time 12 min, liquid-solid ratio 32 mL/g, microwave power of 534 W, and a fixed ultrasonic power of 50 W. Compared to conventional heating reflux extraction (HRE, the RU and QU extraction yields obtained by ILs-UMAE were, respectively, 5.49 mg/g and 0.27 mg/g, which increased, respectively, 2.01-fold and 2.34-fold with the recoveries that were in the range of 97.62–102.36% for RU and 97.33–102.21% for QU with RSDs lower than 3.2% under the optimized UMAE conditions. In addition, the shorter extraction time was used in ILs-UMAE, compared with HRE. Therefore, ILs-UMAE was a rapid and an efficient method for the extraction of RU and QU from the leaves of velvetleaf.

  6. Strong coupling constant extraction from high-multiplicity Z +jets observables

    Science.gov (United States)

    Johnson, Mark; Maître, Daniel

    2018-03-01

    We present a strong coupling constant extraction at next-to-leading order QCD accuracy using ATLAS Z +2 ,3,4 jets data. This is the first extraction using processes with a dependency on high powers of the coupling constant. We obtain values of the strong coupling constant at the Z mass compatible with the world average and with uncertainties commensurate with other next-to-leading order extractions at hadron colliders. Our most conservative result for the strong coupling constant is αS(MZ)=0.117 8-0.0043+0.0051 .

  7. Rapid determination of volatile constituents in safflower from Xinjiang and Henan by ultrasonic-assisted solvent extraction and GC–MS

    Directory of Open Access Journals (Sweden)

    Ling-Han Jia

    2011-08-01

    Full Text Available The total volatile components were extracted from safflower by ultrasonic-assisted solvent extraction (USE and their chemical constituents were analyzed by gas chromatography–mass spectrometry (GC–MS to provide scientific basis for the quality control of safflower. Five different solvents (diethyl ether, ethanol, ethyl acetate, dichloromethane and acetone were used and compared in terms of number of volatile components extracted and the peak areas of these components in TIC. The results showed that USE could be used as an efficient and rapid method for extracting the volatile components from safflower. It also could be found that the number of components in the TIC of ethyl acetate extract was more than that in the TIC of other solvent ones. Meanwhile, the volatile components of safflower from Xinjiang Autonomous Region and Henan Province of China were different in chemical components and relative contents. It could be concluded that both the extraction solvents and geographical origin of safflower are responsible for these differences. The experimental results also indicated that USE/GC–MS is a simple, rapid and effective method to analyze the volatile oil components of safflower. Keywords: Safflower, Ultrasonic solvent extraction, Gas chromatography–mass spectrometry (GC–MS

  8. Copper clean-up procedure for ultrasonic extraction and analysis of pyrethroid and phenylpyrazole pesticides in sediments by gas chromatography-electron capture detection

    Energy Technology Data Exchange (ETDEWEB)

    Wu Jun; Lin Youjian; Lu Jian; Wilson, Chris, E-mail: pcwilson@ufl.edu

    2011-08-15

    A rapid ultrasonic extraction method coupled with a heated-copper clean-up procedure for removing interfering constituents was developed for analyzing pyrethroid and phenylpyrazole pesticides in sediments. Incubation of the 60 mL extract with 12 g copper granules at 60 {sup o}C for 2 h was determined to be the optimal conditions for removing the interfering constituents. Eleven pyrethroid and phenylpyrazole pesticides were spiked into sediment samples to determine the effectiveness of the ultrasonic extraction method. The average recoveries of pyrethroids and phenylpyrazoles in sediment at 4 {sup o}C storage on day 0, 1, 7, 14, and 21 ranged from 98.6 to 120.0%, 79.2 to 116.0%, 85.0 to 119.7%, 93.6 to 118.7%, and 92.1 to 118.2%, respectively, with all percent relative standard deviations less than 10% (most < 6%). This illustrated the stability of pyrethroids and phenylpyrazoles in sediment during sediment aging at 4 {sup o}C. Recoveries of the pesticides ranged from 98.6% to 120.0% for lowest fortification level (2-16 {mu}g kg{sup -1}), from 97.8% to 117.9% for middle fortification level (10-80 {mu}g kg{sup -1}), and from 94.3% to 118.1% for highest fortification level (20-160 {mu}g kg{sup -1}). Relative standard deviations of pesticide recoveries were usually less than 7%. Method detection limits of target pesticides ranged from 0.22 {mu}g kg{sup -1} to 3.72 {mu}g kg{sup -1}. Furthermore, field sediment samples collected from four residential lakes during a three-month monitoring period were analyzed to evaluate the effectiveness of this method. Bifenthrin was detected in all of sediment samples (highest concentration 260.33 {+-} 41.71 {mu}g kg{sup -1}, lowest concentration 5.68 {+-} 0.38 {mu}g kg{sup -1}), and fipronil sulfone was detected at least once in sediment samples collected from three sites with concentrations ranging from 1.73 {+-} 0.53 to 7.53 {+-} 0.01 {mu}g kg{sup -1}. - Highlights: {yields} A rapid extraction and copper-based clean-up method was

  9. Optimization of Ultrasonic-Assisted Enzymatic Extraction Conditions for Improving Total Phenolic Content, Antioxidant and Antitumor Activities In Vitro from Trapa quadrispinosa Roxb. Residues.

    Science.gov (United States)

    Li, Feng; Mao, Yi-Dan; Wang, Yi-Fan; Raza, Aun; Qiu, Li-Peng; Xu, Xiu-Quan

    2017-03-06

    Stems are the important residues of Trapa quadrispinosa Roxb., which are abundant in phenolic compounds. Ultrasonic-assisted enzymatic extraction (UAEE) is confirmed as a novel extraction technology with main advantages of enhancing extraction yield and physiological activities of the extracts from various plants. In this study, UAEE was applied to obtain the highest yield of phenolic content, strongest antioxidant, and antitumor activities and to optimize the extraction conditions using response surface methodology (RSM). The extracts from the stems of T. quadrispinosa were characterized by determination of their antioxidant activities through 2,2-azinobis(3-ethylbenzthiazoline)-6-sulfonic acid (ABTS), 1,1-Diphenyl-2-picrylhydrazxyl (DPPH) radical scavenging, total antioxidant capacity (TAC), ferric reducing antioxidant capacity (FRAC) methods and of their antitumor activity by MTT method. The selected key independent variables were cellulase concentration ( X ₁: 1.5%-2.5%), extraction time ( X ₂: 20-30 min) and extraction temperature ( X ₃: 40-60 °C). The optimal extraction conditions for total phenolic content (TPC) value of the extracts were determined as 1.74% cellulase concentration, 25.5 min ultrasonic extraction time and 49.0 °C ultrasonic temperature. Under these conditions, the highest TPC value of 53.6 ± 2.2 mg Gallic acid equivalent (GAE)/g dry weight (DW) was obtained, which agreed well with the predicted value (52.596 mg GAE/g·DW. Furthermore, the extracts obtained from UAEE presented highest antioxidant activities through ABTS, DPPH, TAC and FRAC methods were of 1.54 ± 0.09 mmol Trolox equivalent (TE)/g·DW; 1.45 ± 0.07 mmol·TE/g·DW; 45.2 ± 2.2 mg·GAE/g·DW; 50.4 ± 2.6 μmol FeSO₄ equivalent/g·DW and lowest IC 50 values of 160.4 ± 11.6 μg/mL, 126.1 ± 10.8 μg/mL, and 178.3 ± 13.1 μg/mL against Hela, HepG-2 and U251 tumor cells, respectively. The results indicated that the UAEE was an efficient alternative to improve

  10. Comparative studies on conventional (water-hot acid) and non-conventional (ultrasonication) procedures for extraction and chemical characterization of pectin from peel waste of mango cultivar chaunsa

    International Nuclear Information System (INIS)

    Kausar, S.; Saeed, A.

    2015-01-01

    Pectin, a naturally occurring heteropolysaccharide, is widely used as a functional ingredient in food and pharmaceutical industries due to its gelling and stabilizing properties. During the present study pectin was extracted from peel of mango (cultivar Chaunsa) using conventional (water-hot acid) and non-conventional (ultrasonication) methods. In conventional method, HNO/sub 3/, H/sub 2/SO/sub 4/, or HCl was used under variable conditions of pH (2.0, 2.5, 3.0), temperature (70, 80, 90, 100 degree C), duration of extraction (30, 60, 90, 120 min), and solvents (ethanol, methanol, acetone, isopropyl alcohol). Maximum yield of 16.6 g pectin 100 g/sup -1/ peel was obtained with HNO/sub 3/ at pH 2.5, 90 degree C, 90 min extraction, and ethanol. Whereas in non-conventional method, ultrasonication was used for different time intervals (10, 20, 40 min) using HNO/sub 3/ at pH 2.5 and 90 degree C. Maximum yield of 15.8 g pectin 100 g/sup -1/ peel was obtained by this method in 20 min. Pectin extracted by the above two methods was found to be of high quality as was determined in respect of methoxyl and galacturonic acid contents, degree of esterification, equivalent weight, and FTIR spectra. Extraction of pectin from mango peel by employing non-conventional method (ultrasonication) was observed to be an energy efficient method due to its less extraction time (20 min as compared to 90 min in conventional method) suggesting its suitability on commercial scale for the extraction of pectin from mango and other available fruit peel wastes. (author)

  11. Development of a Post-Processing Algorithm for Accurate Human Skull Profile Extraction via Ultrasonic Phased Arrays

    Science.gov (United States)

    Al-Ansary, Mariam Luay Y.

    Ultrasound Imaging has been favored by clinicians for its safety, affordability, accessibility, and speed compared to other imaging modalities. However, the trade-offs to these benefits are a relatively lower image quality and interpretability, which can be addressed by, for example, post-processing methods. One particularly difficult imaging case is associated with the presence of a barrier, such as a human skull, with significantly different acoustical properties than the brain tissue as the target medium. Some methods were proposed in the literature to account for this structure if the skull's geometry is known. Measuring the skull's geometry is therefore an important task that requires attention. In this work, a new edge detection method for accurate human skull profile extraction via post-processing of ultrasonic A-Scans is introduced. This method, referred to as the Selective Echo Extraction algorithm, SEE, processes each A-Scan separately and determines the outermost and innermost boundaries of the skull by means of adaptive filtering. The method can also be used to determine the average attenuation coefficient of the skull. When applied to simulated B-Mode images of the skull profile, promising results were obtained. The profiles obtained from the proposed process in simulations were found to be within 0.15lambda +/- 0.11lambda or 0.09 +/- 0.07mm from the actual profiles. Experiments were also performed to test SEE on skull mimicking phantoms with major acoustical properties similar to those of the actual human skull. With experimental data, the profiles obtained with the proposed process were within 0.32lambda +/- 0.25lambda or 0.19 +/- 0.15mm from the actual profile.

  12. Multi-criteria optimization for ultrasonic-assisted extraction of antioxidants from Pericarpium Citri Reticulatae using response surface methodology, an activity-based approach.

    Science.gov (United States)

    Zeng, Shanshan; Wang, Lu; Zhang, Lei; Qu, Haibin; Gong, Xingchu

    2013-06-01

    An activity-based approach to optimize the ultrasonic-assisted extraction of antioxidants from Pericarpium Citri Reticulatae (Chenpi in Chinese) was developed. Response surface optimization based on a quantitative composition-activity relationship model showed the relationships among product chemical composition, antioxidant activity of extract, and parameters of extraction process. Three parameters of ultrasonic-assisted extraction, including the ethanol/water ratio, Chenpi amount, and alkaline amount, were investigated to give optimum extraction conditions for antioxidants of Chenpi: ethanol/water 70:30 v/v, Chenpi amount of 10 g, and alkaline amount of 28 mg. The experimental antioxidant yield under the optimum conditions was found to be 196.5 mg/g Chenpi, and the antioxidant activity was 2023.8 μmol Trolox equivalents/g of the Chenpi powder. The results agreed well with the second-order polynomial regression model. This presented approach promised great application potentials in both food and pharmaceutical industries. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. A Reference-Free and Non-Contact Method for Detecting and Imaging Damage in Adhesive-Bonded Structures Using Air-Coupled Ultrasonic Transducers

    Directory of Open Access Journals (Sweden)

    Timotius Yonathan Sunarsa

    2017-12-01

    Full Text Available Adhesive bonded structures have been widely used in aerospace, automobile, and marine industries. Due to the complex nature of the failure mechanisms of bonded structures, cost-effective and reliable damage detection is crucial for these industries. Most of the common damage detection methods are not adequately sensitive to the presence of weakened bonding. This paper presents an experimental and analytical method for the in-situ detection of damage in adhesive-bonded structures. The method is fully non-contact, using air-coupled ultrasonic transducers (ACT for ultrasonic wave generation and sensing. The uniqueness of the proposed method relies on accurate detection and localization of weakened bonding in complex adhesive bonded structures. The specimens tested in this study are parts of real-world structures with critical and complex damage types, provided by Hyundai Heavy Industries® and IKTS Fraunhofer®. Various transmitter and receiver configurations, including through transmission, pitch-catch scanning, and probe holder angles, were attempted, and the obtained results were analyzed. The method examines the time-of-flight of the ultrasonic waves over a target inspection area, and the spatial variation of the time-of-flight information was examined to visualize and locate damage. The proposed method works without relying on reference data obtained from the pristine condition of the target specimen. Aluminum bonded plates and triplex adhesive layers with debonding and weakened bonding were used to examine the effectiveness of the method.

  14. THE EFFECT OF SOXHLET AND ULTRASONIC-ASSISTED EXTRACTION ON ANTIOXIDANT COMPONENTS AND ANTIOXIDANT PROPERTIES OF SELECTED SOUTH ALGERIAN RED POTATOES CULTIVARS

    Directory of Open Access Journals (Sweden)

    TOUHAMI LANEZ

    2017-12-01

    Full Text Available The present work aimed to study the effect of two different commonly applied extraction techniques for the evaluation of total phenolic contents (TPC, total flavonoid contents (TFC and total antioxidant capacity (TAC of fresh south Algerian red potatoes cultivars (Solanum tuberosum L. These techniques are namely Soxhlet extraction (SE and ultrasonic-assisted extraction combines with maceration (UAE-M for 5 min, 2 hours and 24 hours. A 40 kHz probe was used for the sonication at 3 different amplitudes (30 %, 50 %, and 70 % with a mixture of ethanol/water at ratios of 70:30 and 100 % v/v as solvent. TPC and TFC obtained using SE are respectively 13.94 mg gallic acid equivalents (GAE / g extract and 11.32 mg rutin equivalents (RE / g extract, the amount of these contents is increased to 22.29 mg GAE / g extract and 85.93 mg RE / g extract using UAE-M with 100 % ethanol at amplitude 30 % and 24 hours maceration time. HPLC analysis of samples extract shows four contents with different concentration. In addition, all the results demonstrate a statistically significant with (p < 0.001. It should be noted that the use of UAE-M proved to be faster and more efficient process when compared to Soxhlet extraction.

  15. Multi-Optimization of Ultrasonic-Assisted Enzymatic Extraction of Atratylodes macrocephala Polysaccharides and Antioxidants Using Response Surface Methodology and Desirability Function Approach.

    Science.gov (United States)

    Pu, Jin-Bao; Xia, Bo-Hou; Hu, Yi-Juan; Zhang, Hong-Jian; Chen, Jing; Zhou, Jie; Liang, Wei-Qing; Xu, Pan

    2015-12-11

    Rhizoma Atractylodes macrocephala polysaccharides (RAMP) have been reported to have a variety of important biological activities. In this study, an ultrasonic-assisted enzymatic extraction (UAEE) was employed to obtain the highest extraction yield and strongest antioxidant activity of RAMP and optimized by a multi-response optimization process. A three-level four-factor Box-Behnken design (BBD) was performed as response surface methodology (RSM) with desirability function (DF) to attain the optimal extraction parameters. The DPPH scavenging percentage was used to represent the antioxidant ability of RAMP. The maximum D value (0.328), along with the maximum yield (59.92%) and DPPH scavenging percentage (13.28%) were achieved at 90.54 min, 57.99 °C, 1.95% cellulase and 225.29 W. These values were further validated and found to be in good agreement with the predicted values. Compared to the other extraction methods, both the yield and scavenging percentage of RAMP obtained by UAEE was favorable and the method appeared to be time-saving and of high efficiency. These results demostrated that UAEE is an appropriate and effective extraction technique. Moreover, RSM with DF approach has been proved to be adequate for the design and optimization of the extraction parameters for RAMP. This work has a wide range of implications for the design and operation of polysaccharide extraction processes.

  16. FI/SI on-line solvent extraction/back extraction preconcentration coupled to direct injection nebulization inductively coupled plasma mass spectrometry for determination of copper and lead

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2002-01-01

    An automated sequential injection on-line preconcentration procedure for determination of trace levels of copper and lead via solvent extraction/back extraction coupled to ICP-MS is described. In citrate buffer of pH 3, neutral complexes between the analytes and the chelating reagent, ammonium...... loop, the content of which is subsequently introduced into the ICP-MS, via a direct injection high efficiency nebulizer (DIHEN), for quantification. Enrichment factors of 29.6 (Cu) and 23.3 (Pb), detection limits of 17 ng/l (Cu) and 11 ng/l (Pb), along with a sampling frequency of 13 s/h were obtained...

  17. Comparison of the samples injection systems with ultrasonic nebulizer and with pneumatic nebulizer for the metal determination in water by inductively coupled plasma optical emission spectrometry

    International Nuclear Information System (INIS)

    Marin, Sergio R; Pismante, Paola A

    2005-01-01

    The natural waters, depending on their use, must fulfill the exigencies and requirements that fix national and international norms. These establish conditions with respect to the concentration levels that must be some metals. In this work the development of inductively coupled plasma emission optical spectrometry with ultrasonic injection system is presented. The determination of aluminum, arsenic, barium, cadmium, zinc, cobalt, chromium, copper, iron, manganese, molybdenum, nickel, lead, strontium and vanadium, at levels of ultra-trace in water samples is studied by this technique. The wavelengths that represented better sensitivity and minors spectral interferences, were selected from the Literature specialized in the analysis of this type of material. Also the conditions of work for the ultrasonic nebulization: temperature, pressure, flow speed of argon, and flow speed of sample was determined. The greater sensitivity of the injection system by ultrasonic nebulization forehead to the injection system by pneumatic nebulization, is verified when comparing the spectral intensity of the selected wavelengths. Also the limits of detection and quantification was obtained by both systems. The validity of the results obtained in this method is verified applying the test of Fisher, who determines the degree of homogeneity of the variances, and the test of Student, to determine the trazability obtained with these values. For these studies, the certified material of reference TM-24.2 of National Water Research Institute Environment Canada (NWRI), was used. The positive answer to the criteria of evaluation E and Z-Score, obtained by this technique, allows to verify that it fulfills the exigencies to be used in the determination of metals at the required levels (au)

  18. Optimization of ultrasonic circulating extraction of samara oil from Acer saccharum using combination of Plackett-Burman design and Box-Behnken design.

    Science.gov (United States)

    Chen, Fengli; Zhang, Qiang; Fei, Shimin; Gu, Huiyan; Yang, Lei

    2017-03-01

    In this study, ultrasonic circulating extraction (UCE) technique was firstly and successfully applied for extraction of samara oil from Acer saccharum. The extraction kinetics were fitted and described, and the extraction mechanism was discussed. Through comparison, n-hexane was selected as the extraction solvent, the influence of solvent type on the responses was detailedly interpreted based on the influence of their properties on the occurrence and intensity of cavitation. Seven parameters potentially influencing the extraction yield of samara oil and content of nervonic acid, including ultrasound irradiation time, ultrasound irradiation power, ultrasound temperature, liquid-solid ratio, soaking time, particle size and stirring rate, were screened through Plackett-Burman design to determine the significant variables. Then, three parameters performed statistically significant, including liquid-solid ratio, ultrasound irradiation time and ultrasound irradiation power, were further optimized using Box-Behnken design to predict optimum extraction conditions. Satisfactory yield of samara oil (11.72±0.38%) and content of nervonic acid (5.28±0.18%) were achieved using the optimal conditions. 1% proportion of ethanol in extraction solvent, 120°C of drying temperature and 6.4% moisture were selected and applied for effective extraction. There were no distinct differences in the physicochemical properties of samara oil obtained by UCE and Soxhlet extraction, and the samara oil obtained by UCE exhibited better antioxidant activities. Therefore, UCE method has enormous potential for efficient extraction of edible oil with high quality from plant materials. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. New method based on combining ultrasonic assisted miniaturized matrix solid-phase dispersion and homogeneous liquid-liquid extraction for the determination of some organochlorinated pesticides in fish

    International Nuclear Information System (INIS)

    Rezaei, Farahnaz; Hosseini, Mohammad-Reza Milani

    2011-01-01

    Highlights: → Ultrasonic assisted miniaturized matrix solid-phase dispersion combined with HLLE was developed as a new method for the extraction of OCPs in fish. → The goal of this combination was to enhance the selectivity of HLLE procedure and to extend its application in biological samples. → This method proposed the advantages of good detection limits, lower consumption of reagents, and does not need any special instrumentation. - Abstract: In this study, ultrasonic assisted miniaturized matrix solid-phase dispersion (US-MMSPD) combined with homogeneous liquid-liquid extraction (HLLE) has been developed as a new method for the extraction of organochlorinated pesticides (OCPs) in fish prior to gas chromatography with electron capture detector (GC-ECD). In the proposed method, OCPs (heptachlor, aldrin, DDE, DDD, lindane and endrin) were first extracted from fish sample into acetonitrile by US-MMSPD procedure, and the extract was then used as consolute solvent in HLLE process. Optimal condition for US-MMSPD step was as follows: volume of acetonitrile, 1.5 mL; temperature of ultrasound, 40 deg. C; time of ultrasound, 10 min. For HLLE step, optimal results were obtained at the following conditions: volume of chloroform, 35 μL; volume of aqueous phase, 1.5 mL; volume of double distilled water, 0.5 mL; time of centrifuge, 10 min. Under the optimum conditions, the enrichment factors for the studied compounds were obtained in the range of 185-240, and the overall recoveries were ranged from 39.1% to 81.5%. The limits of detection were 0.4-1.2 ng g -1 and the relative standard deviations for 20 ng g -1 of the OCPs, varied from 3.2% to 8% (n = 4). Finally, the proposed method has been successfully applied to the analysis of the OCPs in real fish sample, and satisfactory results were obtained.

  20. New method based on combining ultrasonic assisted miniaturized matrix solid-phase dispersion and homogeneous liquid-liquid extraction for the determination of some organochlorinated pesticides in fish

    Energy Technology Data Exchange (ETDEWEB)

    Rezaei, Farahnaz [Department of Analytical Chemistry, Faculty of Chemistry, Iran University of Science and Technology, Narmak, Tehran 16846 (Iran, Islamic Republic of); Hosseini, Mohammad-Reza Milani, E-mail: drmilani@iust.ac.ir [Department of Analytical Chemistry, Faculty of Chemistry, Iran University of Science and Technology, Narmak, Tehran 16846 (Iran, Islamic Republic of); Electroanalytical Chemistry Research Center, Iran University of Science and Technology, Narmak, Tehran 16846 (Iran, Islamic Republic of)

    2011-09-30

    Highlights: {yields} Ultrasonic assisted miniaturized matrix solid-phase dispersion combined with HLLE was developed as a new method for the extraction of OCPs in fish. {yields} The goal of this combination was to enhance the selectivity of HLLE procedure and to extend its application in biological samples. {yields} This method proposed the advantages of good detection limits, lower consumption of reagents, and does not need any special instrumentation. - Abstract: In this study, ultrasonic assisted miniaturized matrix solid-phase dispersion (US-MMSPD) combined with homogeneous liquid-liquid extraction (HLLE) has been developed as a new method for the extraction of organochlorinated pesticides (OCPs) in fish prior to gas chromatography with electron capture detector (GC-ECD). In the proposed method, OCPs (heptachlor, aldrin, DDE, DDD, lindane and endrin) were first extracted from fish sample into acetonitrile by US-MMSPD procedure, and the extract was then used as consolute solvent in HLLE process. Optimal condition for US-MMSPD step was as follows: volume of acetonitrile, 1.5 mL; temperature of ultrasound, 40 deg. C; time of ultrasound, 10 min. For HLLE step, optimal results were obtained at the following conditions: volume of chloroform, 35 {mu}L; volume of aqueous phase, 1.5 mL; volume of double distilled water, 0.5 mL; time of centrifuge, 10 min. Under the optimum conditions, the enrichment factors for the studied compounds were obtained in the range of 185-240, and the overall recoveries were ranged from 39.1% to 81.5%. The limits of detection were 0.4-1.2 ng g{sup -1} and the relative standard deviations for 20 ng g{sup -1} of the OCPs, varied from 3.2% to 8% (n = 4). Finally, the proposed method has been successfully applied to the analysis of the OCPs in real fish sample, and satisfactory results were obtained.

  1. Ultrasonic signature

    International Nuclear Information System (INIS)

    Borloo, E.; Crutzen, S.

    1974-12-01

    The unique and tamperproof identification technique developed at Ispra is based on ultrasonic Non-Destructive-Techniques. Reading fingerprints with ultrasonic requires high reproducibility of standard apparatus and transducers. The present report gives an exhaustive description of the ultrasonic technique developed for identification purposes. Different applications of the method are described

  2. Influence of conventional and ultrasonic-assisted extraction on phenolic contents, betacyanin contents, and antioxidant capacity of red dragon fruit (Hylocereus polyrhizus).

    Science.gov (United States)

    Ramli, Nurul Shazini; Ismail, Patimah; Rahmat, Asmah

    2014-01-01

    The aim of this study was to examine the effects of extraction methods on antioxidant capacities of red dragon fruit peel and flesh. Antioxidant capacities were measured using ethylenebenzothiozoline-6-sulfonic acid (ABTS) radical cation assay and ferric reducing antioxidant power assay (FRAP). Total phenolic content (TPC) was determined using Folin-Ciocalteu reagent while quantitative determination of total flavonoid content (TFC) was conducted using aluminium trichloride colorimetric method. Betacyanin content (BC) was measured by spectrophotometer. Red dragon fruit was extracted using conventional (CV) and ultrasonic-assisted extraction (UE) technique to determine the most efficient way of extracting its antioxidant components. Results indicated that UE increased TFC, reduced the extraction yield, BC, and TPC, but exhibited the strongest scavenging activity for the peel of red dragon fruit. In contrast, UE reduced BC, TFC, and scavenging activity but increased the yield for the flesh. Nonetheless, UE slightly increases TPC in flesh. Scavenging activity and reducing power were highly correlated with phenolic and flavonoid compounds. Conversely, the scavenging activity and reducing power were weakly correlated with betacyanin content. This work gives scientific evidences for the consideration of the type of extraction techniques for the peel and flesh of red dragon fruit in applied research and food industry.

  3. Influence of Conventional and Ultrasonic-Assisted Extraction on Phenolic Contents, Betacyanin Contents, and Antioxidant Capacity of Red Dragon Fruit (Hylocereus polyrhizus

    Directory of Open Access Journals (Sweden)

    Nurul Shazini Ramli

    2014-01-01

    Full Text Available The aim of this study was to examine the effects of extraction methods on antioxidant capacities of red dragon fruit peel and flesh. Antioxidant capacities were measured using ethylenebenzothiozoline-6-sulfonic acid (ABTS radical cation assay and ferric reducing antioxidant power assay (FRAP. Total phenolic content (TPC was determined using Folin-Ciocalteu reagent while quantitative determination of total flavonoid content (TFC was conducted using aluminium trichloride colorimetric method. Betacyanin content (BC was measured by spectrophotometer. Red dragon fruit was extracted using conventional (CV and ultrasonic-assisted extraction (UE technique to determine the most efficient way of extracting its antioxidant components. Results indicated that UE increased TFC, reduced the extraction yield, BC, and TPC, but exhibited the strongest scavenging activity for the peel of red dragon fruit. In contrast, UE reduced BC, TFC, and scavenging activity but increased the yield for the flesh. Nonetheless, UE slightly increases TPC in flesh. Scavenging activity and reducing power were highly correlated with phenolic and flavonoid compounds. Conversely, the scavenging activity and reducing power were weakly correlated with betacyanin content. This work gives scientific evidences for the consideration of the type of extraction techniques for the peel and flesh of red dragon fruit in applied research and food industry.

  4. Ultrasonic testing

    Energy Technology Data Exchange (ETDEWEB)

    Song, Sung Jin [Sungkwunkwan Univ., Seoul (Korea, Republic of); Jeong, Hyun Jo [Wonkwang Univ., Iksan (Korea, Republic of)

    2004-02-15

    For the proper performance of ultrasonic testing of steel welded joints, and anisotropic material it is necessary to have sound understanding on the underlying physics. To provide such an understanding, it is beneficial to have simulation tools for ultrasonic testing. In order to address such a need, we develop effective approaches to simulate angle beam ultrasonic testing with a personal computer. The simulation is performed using ultrasonic measurement models based on the computationally efficient multi-Gaussian beams. This reach will describe the developed ultrasonic testing models together with the experimental verification of their accuracy.

  5. Study of supercritical CO2 extraction and nanofiltration membrane separation coupling

    International Nuclear Information System (INIS)

    Sarrade, S.

    1994-12-01

    The aim of this thesis is to study the coupling of two extraction techniques, nanofiltering and supercritical fluids, designing and building an experimental device that enables both supercritical CO 2 extraction and nanofiltering membrane separation. The purpose is to reach high splitting up levels on small molecule mixtures. The document is divided in four parts : a bibliographic study on these two techniques; a description of the membranes and the products, as well as the experimental device; the characterization and modelization of transfer mechanism in aqueous solutions; a presentation of the results obtained by coupling the two techniques. (TEC). 45 tabs., 70 figs., 98 refs

  6. Ultrasonic extraction of pectin from Opuntia ficus indica cladodes after mucilage removal: Optimization of experimental conditions and evaluation of chemical and functional properties.

    Science.gov (United States)

    Bayar, Nadia; Bouallegue, Tahani; Achour, Mabrouka; Kriaa, Mouna; Bougatef, Ali; Kammoun, Radhouane

    2017-11-15

    Ultrasonic assisted extraction (UAE) of pectin from Opuntia ficus indica (OFI) cladodes after mucilage removal was attempted using the response surface methodology. The process variables were optimized by the isovariant central composite design in order to improve the pectin extraction yield. The optimum condition obtained was: sonication time 70min, temperature 70°C, pH 1.5 and the water-material ratio 30ml/g. This condition was validated and the performance of experimental extraction was 18.14%±1.41%, which was closely linked to the predicted value (19.06%). Thus, UAE present a promising alternative to conventional extraction process thanks to its high efficiency which was achieved in less time and at lower temperatures. The pectin extracted by UAE from OFI cladodes (UAEPC) has a low degree of esterification, high uronic acid content, important functional properties and good anti-radical activity. These results are in favor of the use of UAEPC as potential additive in food industry. Copyright © 2017. Published by Elsevier Ltd.

  7. Procedure for the creation of reproducible acoustic coupling using the ultrasonic contact method for nondestructive testing of materials

    International Nuclear Information System (INIS)

    Tomilov, B.V.

    1979-01-01

    The transducer is pressed to the specimen, a lubricating coating being applied as an intermediate layer. By means of a vibrator belonging to the transducer there are generated vibrations, the growth rate of the amplitude of the reflected signal picked up being observed. This growth rate is monotonously decreasing. If the growth rate is abruptly decreasing or if the amplitude of the measured signal remains constant the vibrator is turned off, because now good acoustic contact is established. After a short time of waiting for the residual stress of the transducer to decay, recording of the ultrasonic parameters may then be taken up. The method can be applied to thickness measurements and inhomogeneous materials with low surface quality. (RW) [de

  8. Dual ultrasonic-assisted dispersive liquid-liquid microextraction coupled with microwave-assisted derivatization for simultaneous determination of 20(S)-protopanaxadiol and 20(S)-protopanaxatriol by ultra high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Zhao, Xian-En; Lv, Tao; Zhu, Shuyun; Qu, Fei; Chen, Guang; He, Yongrui; Wei, Na; Li, Guoliang; Xia, Lian; Sun, Zhiwei; Zhang, Shijuan; You, Jinmao; Liu, Shu; Liu, Zhiqiang; Sun, Jing; Liu, Shuying

    2016-03-11

    This paper, for the first time, reported a speedy hyphenated technique of low toxic dual ultrasonic-assisted dispersive liquid-liquid microextraction (dual-UADLLME) coupled with microwave-assisted derivatization (MAD) for the simultaneous determination of 20(S)-protopanaxadiol (PPD) and 20(S)-protopanaxatriol (PPT). The developed method was based on ultra high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) detection using multiple-reaction monitoring (MRM) mode. A mass spectrometry sensitizing reagent, 4'-carboxy-substituted rosamine (CSR) with high reaction activity and ionization efficiency was synthesized and firstly used as derivatization reagent. Parameters of dual-UADLLME, MAD and UHPLC-MS/MS conditions were all optimized in detail. Low toxic brominated solvents were used as extractant instead of traditional chlorinated solvents. Satisfactory linearity, recovery, repeatability, accuracy and precision, absence of matrix effect and extremely low limits of detection (LODs, 0.010 and 0.015ng/mL for PPD and PPT, respectively) were achieved. The main advantages were rapid, sensitive and environmentally friendly, and exhibited high selectivity, accuracy and good matrix effect results. The proposed method was successfully applied to pharmacokinetics of PPD and PPT in rat plasma. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. Development of an interface for directly coupled solid-phase extraction and GC-MS analysis

    NARCIS (Netherlands)

    Öllers, M.J.H.; van Lieshout, H.P.M.; Janssen, J.G.M.; Cramers, C.A.M.G.

    Solid-phase extraction (SPE) is widely used as a sample preparation technique in numerous application areas of chromatography. Large-volume injection is an attractive technique for coupling SPE to gas chromatography (GC) because it provides improved detection limits and circumvents the need for

  10. Supercritical fluid extraction-capillary gas chromatography: on-line coupling with a programmed temperature vaporizer

    NARCIS (Netherlands)

    Houben, R.J.; Janssen, J.G.M.; Leclercq, P.A.; Rijks, J.A.; Cramers, C.A.M.G.

    1990-01-01

    A simple and versatile system is described for the on-line coupling of SFE to capillary GC. The interfacing consists of a programmed temperature vaporizer (PTV) injector. With this injector it is possible to combine solute trapping, elimination of a high flow of extraction fluid, and quantitative

  11. Non-contact fluid characterization in containers using ultrasonic waves

    Science.gov (United States)

    Sinha, Dipen N [Los Alamos, NM

    2012-05-15

    Apparatus and method for non-contact (stand-off) ultrasonic determination of certain characteristics of fluids in containers or pipes are described. A combination of swept frequency acoustic interferometry (SFAI), wide-bandwidth, air-coupled acoustic transducers, narrowband frequency data acquisition, and data conversion from the frequency domain to the time domain, if required, permits meaningful information to be extracted from such fluids.

  12. Ultrasonic physics

    CERN Document Server

    Richardson, E G

    1962-01-01

    Ultrasonic Physics, Second Edition, provides an introduction to the fundamental principles of ultrasonic physics. The book opens with a discussion of the sources of ultrasound. This is followed by separate chapters on the properties and detection of ultrasonic radiation; measurement of propagation constants, i.e., the velocity and absorption, of ultrasound; ultrasound propagation in gases, liquids, and solids; and ultrasound propagation in aerosols, suspensions, and emulsions. The final chapter covers miscellaneous physical and physico-chemical actions, including dispersion and coagulation of

  13. Ultrasonic slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry for the determination of Cr, Fe, Cu, Zn and Se in cereals

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Shih-Yi [Department of Chemistry, National Sun Yat-sen University, Kaohsiung 80424, Taiwan (China); Jiang, Shiuh-Jen, E-mail: sjjiang@faculty.nsysu.edu.tw [Department of Chemistry, National Sun Yat-sen University, Kaohsiung 80424, Taiwan (China); Department of Medical Laboratory Science and Biotechnology, Kaohsiung Medical University, Kaohsiung 80708, Taiwan (China); Sahayam, A.C. [National Centre for Compositional Characterisation of Materials (CCCM), Hyderabad (India)

    2014-11-01

    Ultrasonic slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry (USS-ETV-ICP-MS) has been applied to determine Cr, Fe, Cu, Zn and Se in several cereal samples. Thioacetamide was used as the modifier to enhance the ion signals. The background ions at the masses of interest were reduced in intensity significantly by using 1.0 mL min{sup −1} methane (CH{sub 4}) as reaction cell gas in the dynamic reaction cell (DRC). Since the sensitivities of Cr, Fe, Cu, Zn and Se in different matrices were quite different, standard addition and isotope dilution methods were used for the determination of Cr, Fe, Cu, Zn and Se in these cereal samples. The method detection limits estimated from standard addition curves were about 1, 10, 4, 12 and 2 ng g{sup −1} for Cr, Fe, Cu, Zn and Se, respectively, in original cereal samples. This procedure has been applied to the determination of Cr, Fe, Cu, Zn and Se whose concentrations are in μg g{sup −1} (except Cr and Se) in standard reference materials (SRM) of National institute of standards and technology (NIST), NIST SRM 1568a Rice Flour and NIST SRM 1567a Wheat Flour and two cereal samples purchased from a local market. The analysis results of reference materials agreed with certified values at 95% confidence level according to Student's T-test. The results for the real world cereal samples were also found to be in good agreement with the pneumatic nebulization DRC ICP-MS results of the sample solutions. - Highlights: • Determination of Cr, Fe, Cu, Zn and Se in cereal samples • Ultrasonic slurry sampling in combination with DRC-ICP-MS • Better sensitivity with thioacetamide modifier in ETV • Decreased sample preparation time with solid sampling • Validation with NIST SRM 1568a Rice Flour and NIST SRM 1567a Wheat Flour.

  14. Ultrasonic slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry for the determination of Cr, Fe, Cu, Zn and Se in cereals

    International Nuclear Information System (INIS)

    Huang, Shih-Yi; Jiang, Shiuh-Jen; Sahayam, A.C.

    2014-01-01

    Ultrasonic slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry (USS-ETV-ICP-MS) has been applied to determine Cr, Fe, Cu, Zn and Se in several cereal samples. Thioacetamide was used as the modifier to enhance the ion signals. The background ions at the masses of interest were reduced in intensity significantly by using 1.0 mL min −1 methane (CH 4 ) as reaction cell gas in the dynamic reaction cell (DRC). Since the sensitivities of Cr, Fe, Cu, Zn and Se in different matrices were quite different, standard addition and isotope dilution methods were used for the determination of Cr, Fe, Cu, Zn and Se in these cereal samples. The method detection limits estimated from standard addition curves were about 1, 10, 4, 12 and 2 ng g −1 for Cr, Fe, Cu, Zn and Se, respectively, in original cereal samples. This procedure has been applied to the determination of Cr, Fe, Cu, Zn and Se whose concentrations are in μg g −1 (except Cr and Se) in standard reference materials (SRM) of National institute of standards and technology (NIST), NIST SRM 1568a Rice Flour and NIST SRM 1567a Wheat Flour and two cereal samples purchased from a local market. The analysis results of reference materials agreed with certified values at 95% confidence level according to Student's T-test. The results for the real world cereal samples were also found to be in good agreement with the pneumatic nebulization DRC ICP-MS results of the sample solutions. - Highlights: • Determination of Cr, Fe, Cu, Zn and Se in cereal samples • Ultrasonic slurry sampling in combination with DRC-ICP-MS • Better sensitivity with thioacetamide modifier in ETV • Decreased sample preparation time with solid sampling • Validation with NIST SRM 1568a Rice Flour and NIST SRM 1567a Wheat Flour

  15. New Analysis Scheme of Flow-Acoustic Coupling for Gas Ultrasonic Flowmeter with Vortex near the Transducer

    Directory of Open Access Journals (Sweden)

    Yanzhao Sun

    2018-04-01

    Full Text Available Ultrasonic flowmeters with a small or medium diameter are widely used in process industries. The flow field disturbance on acoustic propagation caused by a vortex near the transducer inside the sensor as well as the mechanism and details of flow-acoustic interaction are needed to strengthen research. For that reason, a new hybrid scheme is proposed; the theories of computational fluid dynamics (CFD, wave acoustics, and ray acoustics are used comprehensively by a new step-by-step method. The flow field with a vortex near the transducer, and its influence on sound propagation, receiving, and flowmeter performance are analyzed in depth. It was found that, firstly, the velocity and vortex intensity distribution were asymmetric on the sensor cross-section and acoustic path. Secondly, when passing through the vortex zone, the central ray trajectory was deflected significantly. The sound pressure on the central line of the sound path also changed. Thirdly, the pressure deviation becomes larger with as the flow velocity increases. The deviation was up to 17% for different velocity profiles in a range of 0.6 m/s to 53 m/s. Lastly, in comparison to the theoretical value, the relative deviation of the instrument coefficient for the velocity profile with a vortex near the transducer reached up to −17%. In addition, the rationality of the simulation was proved by experiments.

  16. New Analysis Scheme of Flow-Acoustic Coupling for Gas Ultrasonic Flowmeter with Vortex near the Transducer.

    Science.gov (United States)

    Sun, Yanzhao; Zhang, Tao; Zheng, Dandan

    2018-04-10

    Ultrasonic flowmeters with a small or medium diameter are widely used in process industries. The flow field disturbance on acoustic propagation caused by a vortex near the transducer inside the sensor as well as the mechanism and details of flow-acoustic interaction are needed to strengthen research. For that reason, a new hybrid scheme is proposed; the theories of computational fluid dynamics (CFD), wave acoustics, and ray acoustics are used comprehensively by a new step-by-step method. The flow field with a vortex near the transducer, and its influence on sound propagation, receiving, and flowmeter performance are analyzed in depth. It was found that, firstly, the velocity and vortex intensity distribution were asymmetric on the sensor cross-section and acoustic path. Secondly, when passing through the vortex zone, the central ray trajectory was deflected significantly. The sound pressure on the central line of the sound path also changed. Thirdly, the pressure deviation becomes larger with as the flow velocity increases. The deviation was up to 17% for different velocity profiles in a range of 0.6 m/s to 53 m/s. Lastly, in comparison to the theoretical value, the relative deviation of the instrument coefficient for the velocity profile with a vortex near the transducer reached up to -17%. In addition, the rationality of the simulation was proved by experiments.

  17. New Analysis Scheme of Flow-Acoustic Coupling for Gas Ultrasonic Flowmeter with Vortex near the Transducer

    Science.gov (United States)

    Zhang, Tao; Zheng, Dandan

    2018-01-01

    Ultrasonic flowmeters with a small or medium diameter are widely used in process industries. The flow field disturbance on acoustic propagation caused by a vortex near the transducer inside the sensor as well as the mechanism and details of flow-acoustic interaction are needed to strengthen research. For that reason, a new hybrid scheme is proposed; the theories of computational fluid dynamics (CFD), wave acoustics, and ray acoustics are used comprehensively by a new step-by-step method. The flow field with a vortex near the transducer, and its influence on sound propagation, receiving, and flowmeter performance are analyzed in depth. It was found that, firstly, the velocity and vortex intensity distribution were asymmetric on the sensor cross-section and acoustic path. Secondly, when passing through the vortex zone, the central ray trajectory was deflected significantly. The sound pressure on the central line of the sound path also changed. Thirdly, the pressure deviation becomes larger with as the flow velocity increases. The deviation was up to 17% for different velocity profiles in a range of 0.6 m/s to 53 m/s. Lastly, in comparison to the theoretical value, the relative deviation of the instrument coefficient for the velocity profile with a vortex near the transducer reached up to −17%. In addition, the rationality of the simulation was proved by experiments. PMID:29642577

  18. Ceria nanocubic-ultrasonication assisted dispersive liquid-liquid microextraction coupled with matrix assisted laser desorption/ionization mass spectrometry for pathogenic bacteria analysis.

    Science.gov (United States)

    Abdelhamid, Hani Nasser; Bhaisare, Mukesh L; Wu, Hui-Fen

    2014-03-01

    A new ceria (CeO2) nanocubic modified surfactant is used as the basis of a novel nano-based microextraction technique for highly sensitive detection of pathogenic bacteria (Pseudomonas aeruginosa and Staphylococcus aureus). The technique uses ultrasound enhanced surfactant-assisted dispersive liquid-liquid microextraction (UESA-DLLME) with and without ceria (CeO2) followed by matrix assisted laser desorption/ionization mass spectrometry (MALDI-MS). In order to achieve high separation efficiency, we investigated the influential parameters, including extraction time of ultrasonication, type and volume of the extraction solvent and surfactant. Among various surfactants, the cationic surfactants can selectively offer better extraction efficiency on bacteria analysis than that of the anionic surfactants due to the negative charges of bacteria cell membranes. Extractions of the bacteria lysate from aqueous samples via UESA-DLLME-MALDI-MS were successfully achieved by using cetyltrimethyl ammonium bromide (CTAB, 10.0 µL, 1.0×10(-3) M) as surfactants in chlorobenzene (10.0 µL) and chloroform (10.0 µL) as the optimal extracting solvent for P. aeruginosa and S. aureus, respectively. Ceria nanocubic was synthesized, and functionalized with CTAB (CeO2@CTAB) and then characterized using transmission electron microscopy (TEM) and optical spectroscopy (UV and FTIR). CeO2@CTAB demonstrates high extraction efficiency, improve peaks ionization, and enhance resolution. The prime reasons for these improvements are due to the large surface area of nanoparticles, and its absorption that coincides with the wavelength of MALDI laser (337 nm, N2 laser). CeO2@CTAB-based microextraction offers lowest detectable concentrations tenfold lower than that of without nanoceria. The present approach has been successfully applied to detect pathogenic bacteria at low concentrations of 10(4)-10(5) cfu/mL (without ceria) and at 10(3)-10(4) cfu/mL (with ceria) from bacteria suspensions. Finally, the

  19. Development of an Ultrasonication-Assisted Extraction Based HPLC With a Fluorescence Method for Sensitive Determination of Aflatoxins in Highly Acidic Hibiscus sabdariffa.

    Science.gov (United States)

    Liu, Xiaofei; Ying, Guangyao; Sun, Chaonan; Yang, Meihua; Zhang, Lei; Zhang, Shanshan; Xing, Xiaoyan; Li, Qian; Kong, Weijun

    2018-01-01

    The high acidity and complex components of Hibiscus sabdariffa have provided major challenges for sensitive determination of trace aflatoxins. In this study, sample pretreatment of H. sabdariffa was systematically developed for sensitive high performance liquid chromatography-fluorescence detection (HPLC-FLD) after ultrasonication-assisted extraction, immunoaffinity column (IAC) clean-up and on-line post-column photochemical derivatization (PCD). Aflatoxins B 1 , B 2 , G 1 , G 2 were extracted from samples by using methanol/water (70:30, v/v ) with the addition of NaCl. The solutions were diluted 1:8 with 0.1 M phosphate buffer (pH 8.0) to negate the issues of high acidity and matrix interferences. The established method was validated with satisfactory linearity ( R > 0.999), sensitivity (limits of detection (LODs) and limits of quantitation (LOQs) of 0.15-0.65 and 0.53-2.18 μg/kg, respectively), precision (RSD sabdariffa samples indicated that one sample incubated with Aspergillus flavus was positive with aflatoxin B 1 (AFB 1 ) at 3.11 μg/kg. The strategy developed in this study also has the potential to reliably extract and sensitively detect more mycotoxins in other complex acidic matrices, such as traditional Chinese medicines, foodstuffs, etc.

  20. Effect of ultrasonic extraction conditions on antioxidative and immunomodulatory activities of a Ganoderma lucidum polysaccharide originated from fermented soybean curd residue.

    Science.gov (United States)

    Shi, Min; Yang, Yingnan; Hu, Xuansheng; Zhang, Zhenya

    2014-07-15

    A crude Ganoderma lucidum polysaccharide (GLPL) was extracted from fermented soybean curd residue by ultrasonic assisted extraction. The optimal extraction conditions were 30 min at 80 °C with 80 W and water to solid ratio of 10, and with this method 115.47 ± 2.95 mg/g of GLPL yield was obtained. Additionally, the antioxidant and immunomodulatory activities of GLPL were investigated. The results showed that GLPL exhibited strong antioxidant effects, which included scavenging activities against DPPH radicals, hydrogen oxide and ABTS radicals with IC50 values of 0.23, 0.48 and 0.69 mg/mL, respectively. For immunomodulatory activities, GLPL was shown to strongly stimulate the proliferation of macrophages (158.02 ± 13.12%), the production of nitric oxide and phagocytosis (21.16 ± 1.65 μM), and, at 40.00 μg/mL, protected macrophage from Doxorubicin (DOX) (0.16 ± 0.003). Copyright © 2014 Elsevier Ltd. All rights reserved.

  1. Extraction of surface plasmons in organic light-emitting diodes via high-index coupling.

    Science.gov (United States)

    Scholz, Bert J; Frischeisen, Jörg; Jaeger, Arndt; Setz, Daniel S; Reusch, Thilo C G; Brütting, Wolfgang

    2012-03-12

    The efficiency of organic light-emitting diodes (OLEDs) is still limited by poor light outcoupling. In particular, the excitation of surface plasmon polaritons (SPPs) at metal-organic interfaces represents a major loss channel. By combining optical simulations and experiments on simplified luminescent thin-film structures we elaborate the conditions for the extraction of SPPs via coupling to high-index media. As a proof-of-concept, we demonstrate the possibility to extract light from wave-guided modes and surface plasmons in a top-emitting white OLED by a high-index prism.

  2. Ultrasonic-assisted extraction combined with sample preparation and analysis using LC-ESI-MS/MS allowed the identification of 24 new phenolic compounds in pecan nut shell [Carya illinoinensis (Wangenh) C. Koch] extracts.

    Science.gov (United States)

    Hilbig, Josiane; Alves, Victor Rodrigues; Müller, Carmen Maria Olivera; Micke, Gustavo Amadeu; Vitali, Luciano; Pedrosa, Rozangela Curi; Block, Jane Mara

    2018-04-01

    Ultrasonic-assisted extraction combined with statistical tools (factorial design, response surface methodology and kinetics) were used to evaluate the effects of the experimental conditions of temperature, solid-to-solvent ratio, ethanol concentration and time for the extraction of the total phenolic content from pecan nut shells. The optimal conditions for the aqueous and hydroalcoholic extract (with 20% v/v of ethanol) were 60 and 80 °C; solid to solvent ratio of 30 mL·g -1 (for both) and extraction time of 35 and 25 min, respectively. Using these optimize extraction conditions, 426 and 582 mg GAE·g -1 of phenolic compounds, from the aqueous and hydroalcoholic phases respectively, were obtained. In addition, the analysis of the phenolic compounds using the LC-ESI-MS/MS system allowed the identification of 29 phenolic compounds, 24 of which had not been reported in literature for this raw material yet. Copyright © 2018. Published by Elsevier Ltd.

  3. Extraction of Z' coupling data from Z' → jj at the LHC and SSC

    International Nuclear Information System (INIS)

    Rizzo, T.G.

    1993-06-01

    A recent analysis has shown that it may be possible at the SSC to extract information about Z' couplings via the decay Z' → jj. This technique was found to be useful for some extended electroweak models provided the Z' is relatively light. In the present paper, the authors generalize this procedure to the LHC and to Z''s which are more massive than 1 TeV

  4. Process Optimization of Ultrasonic-Assisted Extraction of Arabinogalactan from Dihydroquercetin Extracted Residues by Response Surface Methodology and Evaluation of Its Antioxidant Activity

    Directory of Open Access Journals (Sweden)

    Zaizhi Liu

    2013-01-01

    Full Text Available Ultrasound was used for the extraction of larch arabinogalactan from Larix gmelinii. The optimal conditions for ultrasound extraction were determined by response surface methodology. Specifically, the Box-Behnken design was employed to evaluate the effects of three independent variables: ultrasound time, temperature, and liquid-solid ratio. The highest arabinogalactan yield (11.18% was obtained under the optimal extraction condition (extraction temperature 41.5°C, extraction time 24.3 min, and liquid-solid ratio 40 mL/g. In addition, the antioxidant activity of arabinogalactan that was extracted from dihydroquercetin extraction residues exhibited a moderate and concentration-dependent hydroxyl radical-scavenging capacity, ferric-reducing power, and reducing power. The wood material was characterized before and after processing by scanning electron microscopy and Fourier-transform infrared spectroscopy.

  5. Ionic liquid and aqueous two-phase extraction based on salting-out coupled with high-performance liquid chromatography for the determination of seven rare ginsenosides in Xue-Sai-Tong injection.

    Science.gov (United States)

    Li, Lan-Jie; Jin, Yong-Ri; Wang, Xiao-Zhong; Liu, Ying; Wu, Qian; Shi, Xiao-Lei; Li, Xu-Wen

    2015-09-01

    A method of ionic liquid salt aqueous two-phase extraction coupled with high-performance liquid chromatography has been developed for the analysis of seven rare ginsenosides including Rg6 , F4 , 20(S)-Rg3 , 20(R)-Rg3 , Rk3 , Rk1 , and Rg5 in Xue-Sai-Tong injection. The injection was mixed with ionic liquid 1-butyl-3-methylimidazolium bromide aqueous solution, and a mixture was obtained. With the addition of sodium dodecyl sulfate and dipotassium phosphate into the mixture, the aqueous two-phase mixture was formed after ultrasonic treatment and centrifuged. Rare ginsenosides were extracted into the upper phase. To obtain a high extraction factors, various influences were considered systematically, such as the volume of ionic liquid, the category and amount of salts, the amount of sodium dodecyl sulfate, the pH value of system, and the time of ultrasonic treatment. Under the optimal condition, rare ginsenosides in Xue-Sai-Tong injection were enriched and detected, the recoveries of seven rare ginsenosides ranged from 90.05 to 112.55%, while relative standard deviations were lower than 2.50%. The developed method was reliable, rapid and sensitive for the determination of seven rare ginsenosides in the injections. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Assessment of pesticide contamination in soil samples from an intensive horticulture area, using ultrasonic extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Gonçalves, C; Alpendurada, M F

    2005-03-15

    In order to reduce the amount of sample to be collected and the time consumed in the analytical process, a broad range of analytes should be preferably considered in the same analytical procedure. A suitable methodology for pesticide residue analysis in soil samples was developed based on ultrasonic extraction (USE) and gas chromatography-mass spectrometry (GC-MS). For this study, different classes of pesticides were selected, both recent and old persistent molecules: parent compounds and degradation products, namely organochlorine, organophosphorous and pyrethroid insecticides, triazine and acetanilide herbicides and other miscellaneous pesticides. Pesticide residues could be detected in the low- to sub-ppb range (0.05-7.0mugkg(-1)) with good precision (7.5-20.5%, average 13.7% R.S.D.) and extraction efficiency (69-118%, average 88%) for the great majority of analytes. This methodology has been applied in a monitoring program of soil samples from an intensive horticulture area in Póvoa de Varzim, North of Portugal. The pesticides detected in four sampling programs (2001/2002) were the following: lindane, dieldrin, endosulfan, endosulfan sulfate, 4,4'-DDE, 4,4'-DDD, atrazine, desethylatrazine, alachlor, dimethoate, chlorpyrifos, pendimethalin, procymidone and chlorfenvinphos. Pesticide contamination was investigated at three depths and in different soil and crop types to assess the influence of soil characteristics and trends over time.

  7. Ultrasonic inspection

    International Nuclear Information System (INIS)

    Satittada, Gannaga

    1984-01-01

    Ultrasonic inspection is one of the most widely used methods for nondestructive inspection. The beam of high-frequency sound wave, ultrasonic wave, is introduced into the material. It travels through the material with some attendant loss of energy and can be reflected at interfaces. The reflected beam is detected and analyzed. Ultrasonic inspection is used to detect flaws in metal parts as well as in welded, brazed and bonded joints during research work and developing production and service. It is also used to detect and locate porosity, pipe, and flakes. In addition, it can be used for the measurement of metal thickness. Ultrasonic inspection is therefore used for quality control and material inspection in all major industries

  8. Effects of push/pull perfusion and ultrasonication on the extraction efficiencies of phthalate esters in sports drink samples using on-line hollow-fiber liquid-phase microextraction.

    Science.gov (United States)

    Chao, Yu-Ying; Lee, Chien-Hung; Chien, Tzu-Yang; Shih, Yu-Hsuan; Lu, Yin-An; Kuo, Ting-Hsuan; Huang, Yeou-Lih

    2013-08-28

    In previous studies, we developed a process, on-line ultrasound-assisted push/pull perfusion hollow-fiber liquid-phase microextraction (UA-PPP-HF-LPME), combining the techniques of push/pull perfusion (PPP) and ultrasonication with hollow-fiber liquid-phase microextraction (HF-LPME), to achieve rapid extraction of acidic phenols from water samples. In this present study, we further evaluated three more-advanced and novel effects of PPP and ultrasonication on the extraction efficiencies of neutral high-molecular-weight phthalate esters (HPAEs) in sports drinks. First, we found that inner-fiber fluid leakage occurs only in push-only perfusion-based and pull-only perfusion-based HF-LPME, but not in the PPP mode. Second, we identified a significant negative interaction between ultrasonication and temperature. Third, we found that the extraction time of the newly proposed system could be shortened by more than 93%. From an investigation of the factors affecting UA-PPP-HF-LPME, we established optimal extraction conditions and achieved acceptable on-line enrichment factors of 92-146 for HPAEs with a sampling time of just 2 min.

  9. Ultrasonic mammography

    International Nuclear Information System (INIS)

    Hueneke, B.

    1982-01-01

    608 women are examined by means of ultrasonic mammography during the period of 1 year. 432 patients were examined with the compound method with the U.I. Octoson, a water tank scanner, and 176 patients with the real time method with a directly connected linear-array-scanner. The following results were obtained at the end of the examination period: In the ultrasonic and also in the X-ray mammogram tumour diameters can be determined with an error rate of +- 30%. In the diagnosing of carcinomas, a significant dependence of the exactness on the sice of the tumour is found for the combination of the five methods tested (clinical examination, X-ray mammography, ultrasonic mammography, thermography, cytology). Classifying the individual methods with regard to their exactness, X-ray mammography ranks in front of ultrasonic mammography. Mastopathic changes in the breast can be screened by means of ultrasonic mammography. The structure of the changes can be determined more exactly than with an X-ray picture which is due to the possibility of differentiating solid and cystic structures. In diagnosing fibro-adenomas and establishing diagnoses on young women with dense gland bodies, ultrasonic mammography is superior to radiology both in the ability of screening a finding of a fibro-adenoma (US=88%, X-ray=75%) and in the possibility of classifying it as ''more benign than malignant''. (orig./MG) [de

  10. Development of an Ultrasonication-Assisted Extraction Based HPLC With a Fluorescence Method for Sensitive Determination of Aflatoxins in Highly Acidic Hibiscus sabdariffa

    Directory of Open Access Journals (Sweden)

    Xiaofei Liu

    2018-04-01

    Full Text Available The high acidity and complex components of Hibiscus sabdariffa have provided major challenges for sensitive determination of trace aflatoxins. In this study, sample pretreatment of H. sabdariffa was systematically developed for sensitive high performance liquid chromatography-fluorescence detection (HPLC-FLD after ultrasonication-assisted extraction, immunoaffinity column (IAC clean-up and on-line post-column photochemical derivatization (PCD. Aflatoxins B1, B2, G1, G2 were extracted from samples by using methanol/water (70:30, v/v with the addition of NaCl. The solutions were diluted 1:8 with 0.1 M phosphate buffer (pH 8.0 to negate the issues of high acidity and matrix interferences. The established method was validated with satisfactory linearity (R > 0.999, sensitivity (limits of detection (LODs and limits of quantitation (LOQs of 0.15–0.65 and 0.53–2.18 μg/kg, respectively, precision (RSD <11%, stability (RSD of 0.2–3.6%, and accuracy (recovery rates of 86.0–102.3%, which all met the stipulated analytical requirements. Analysis of 28 H. sabdariffa samples indicated that one sample incubated with Aspergillus flavus was positive with aflatoxin B1 (AFB1 at 3.11 μg/kg. The strategy developed in this study also has the potential to reliably extract and sensitively detect more mycotoxins in other complex acidic matrices, such as traditional Chinese medicines, foodstuffs, etc.

  11. Ultrasonic energy enhanced the efficiency of advance extraction methodology for enrichment of trace level of copper in serum samples of patients having neurological disorders.

    Science.gov (United States)

    Arain, Mariam S; Kazi, Tasneem G; Afridi, Hassan I; Ali, Jamshed; Akhtar, Asma

    2017-07-01

    An innovative dual dispersive ionic liquid based on ultrasound assisted microextraction (UDIL-μE), for the enrichment of trace levels of copper ion (Cu 2+ ), in serum (blood) of patients suffering from different neurological disorders. The enriched metal ions were subjected to flame atomic absorption spectrometry (FAAS). In the UDIL-μE method, the extraction solvent, ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate [C 4 mim][PF 6 ], was dispersed into the aqueous samples using an ultrasonic bath. The(PAN) 1-(2-pyridylazo)-2-naphthol was used as ligand for the complexation of Cu ion in IL (as extracting solvent). The various variables such as sonication time, pH, concentration of complexing agent, time and rate of centrifugation, IL volume that affect the extraction process were optimized. The enhancement factor (EF) and detection limit (LOD) was found under favorable condition was 31 and 0.36μgL -1 , respectively. Reliability of the proposed method was checked by relative standard deviation (%RSD), which was found to be <5%. The accuracy of developed procedure was assured by using certified reference material (CRM) of blood serum. The developed procedure was applied successfully to the analysis of concentration of Cu ion in blood serum of different neurological disorders subjects and referents of same age group. It was observed that the levels of Cu ion was two folds higher in serum samples of neurological disorders patients as related to normal referents of same age group. Copyright © 2016. Published by Elsevier B.V.

  12. Speciation analysis of mercury by dispersive solid-phase extraction coupled with capillary electrophoresis.

    Science.gov (United States)

    Li, Jinhua; Liu, Junying; Lu, Wenhui; Gao, Fangfang; Wang, Liyan; Ma, Jiping; Liu, Huitao; Liao, Chunyang; Chen, Lingxin

    2018-04-23

    A pretreatment method of dispersive solid-phase extraction (DSPE) along with back-extraction followed by CE-UV detector was developed for the determination of mercury species in water samples. Sulfhydryl-functionalized SiO 2 microspheres (SiO 2 -SH) were synthesized and used as DSPE adsorbents for selective extraction and enrichment of three organic mercury species namely ethylmercury (EtHg), methylmercury (MeHg), and phenylmercury (PhHg), along with L-cysteine (L-cys) containing hydrochloric acid as back-extraction solvent. Several main extraction parameters were systematically investigated including sample pH, amount of adsorbent, extraction and back-extraction time, volume of eluent, and concentration of hydrochloric acid. Under optimal conditions, good linearity was achieved with correlation coefficients over 0.9990, in the range of 4-200 μg/L for EtHg, and 2-200 μg/L for MeHg and PhHg. The LODs were obtained of 1.07, 0.34, and 0.24 μg/L for EtHg, MeHg, and PhHg, respectively, as well as the LOQs were 3.57, 1.13, and 0.79 μg/L, respectively, with enrichment factors ranging from 109 to 184. Recoveries were attained with tap and lake water samples in a range of 62.3-107.2%, with relative standard deviations of 3.5-10.1%. The results proved that the method of SiO 2 -SH based DSPE coupled with CE-UV was a simple, rapid, cost-effective, and eco-friendly alternative for the determination of mercury species in water samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Super-pixel extraction based on multi-channel pulse coupled neural network

    Science.gov (United States)

    Xu, GuangZhu; Hu, Song; Zhang, Liu; Zhao, JingJing; Fu, YunXia; Lei, BangJun

    2018-04-01

    Super-pixel extraction techniques group pixels to form over-segmented image blocks according to the similarity among pixels. Compared with the traditional pixel-based methods, the image descripting method based on super-pixel has advantages of less calculation, being easy to perceive, and has been widely used in image processing and computer vision applications. Pulse coupled neural network (PCNN) is a biologically inspired model, which stems from the phenomenon of synchronous pulse release in the visual cortex of cats. Each PCNN neuron can correspond to a pixel of an input image, and the dynamic firing pattern of each neuron contains both the pixel feature information and its context spatial structural information. In this paper, a new color super-pixel extraction algorithm based on multi-channel pulse coupled neural network (MPCNN) was proposed. The algorithm adopted the block dividing idea of SLIC algorithm, and the image was divided into blocks with same size first. Then, for each image block, the adjacent pixels of each seed with similar color were classified as a group, named a super-pixel. At last, post-processing was adopted for those pixels or pixel blocks which had not been grouped. Experiments show that the proposed method can adjust the number of superpixel and segmentation precision by setting parameters, and has good potential for super-pixel extraction.

  14. The coupling of rapidly synergistic cloud point extraction with thermospray flame furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Wen, X.; Deng, Q.; Guo, J.; Zhao, X.; Zhao, Y.; Ji, S.

    2012-01-01

    Rapidly synergistic cloud point extraction (RS-CPE) was coupled with thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) to result in new CPE patterns and accelerated (1 min) protocols. It is demonstrated, for the case of copper (II) ion, that TS-FF-AAS improves the sampling efficiency and the sensitivity of FAAS determinations. Problems of nebulization associated with previous methods based on the coupling of FAAS and RS-CPE are overcome. TS-FF-AAS also improves sensitivity and gives a limit of detection for copper of 0.20 μg L -1 , which is better by a factor of 32. Compared to direct FAAS, the factor is 114. (author)

  15. Binary Solvent Extraction of Tocols, γ-Oryzanol, and Ferulic Acid from Rice Bran Using Alkaline Treatment Combined with Ultrasonication.

    Science.gov (United States)

    Truong, Hoa Thi; Luu, Phuong Duc; Imamura, Kiyoshi; Matsubara, Takeo; Takahashi, Hideki; Takenaka, Norimichi; Boi, Luu Van; Maeda, Yasuaki

    2017-06-21

    Alkaline treatment (Alk) combined with ultrasound-assisted extraction (UAE) (Alk+UAE) was examined as a means of extracting tocols and γ-oryzanol from rice bran into an organic phase while simultaneously recovering ferulic acid into an aqueous phase. The tocols and γ-oryzanol/ferulic acid yields were determined using high-performance liquid chromatography with fluorescence and UV detection. The effects of extraction conditions were evaluated by varying the Alk treatment temperature and extraction duration. The maximum yields of tocols and γ-oryzanol were obtained at 25 °C over a time span of 30 min. When the temperature was increased to 80 °C, the yield of ferulic acid increased dramatically, whereas the recovery of γ-oryzanol slightly decreased. Employing the Alk+UAE procedure, the recovered concentrations of tocols, γ-oryzanol, and ferulic acid were in the ranges of 146-518, 1591-3629, and 352-970 μg/g, respectively. These results are in good agreement with those reported for rice bran samples from Thailand.

  16. Developments in coupled solid-phase extraction-capillary electrophoresis 2013-2015.

    Science.gov (United States)

    Ramautar, Rawi; Somsen, Govert W; de Jong, Gerhardus J

    2016-01-01

    An overview of the design and application of coupled solid-phase extraction-capillary electrophoresis (SPE-CE) systems reported in the literature between July 2013 and June 2015 is provided in this paper. The present article is a continuation of our previous review papers on this topic which covered the time period 2000-2013 (Electrophoresis 2008, 29, 108-128; Electrophoresis 2010, 31, 44-54; Electrophoresis 2012, 33, 243-250; Electrophoresis 2014, 35, 128-137). The use of in-line and on-line SPE-CE approaches is treated and outlined in this review. Recent advancements, such as, for example, the use of aptamers as affinity material for in-line SPE-CE, the use of a bead string design for in-line fritless SPE-CE, and new interfacing techniques for the on-line coupling of SPE to CE, are outlined. Selected examples demonstrate the applicability of the coupled SPE-CE systems for biomedical, pharmaceutical, environmental, and food studies. A complete overview of the recent SPE-CE studies is given in table format, providing information on sample type, SPE sorbent, coupling mode, detection mode, and LOD. Finally, some general conclusions and perspectives are provided. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. A novel technology coupling extraction and foam fractionation for separating the total saponins from Achyranthes bidentata.

    Science.gov (United States)

    Ding, Linlin; Wang, Yanji; Wu, Zhaoliang; Liu, Wei; Li, Rui; Wang, Yanyan

    2016-10-02

    A novel technology coupling extraction and foam fractionation was developed for separating the total saponins from Achyranthes bidentata. In the developed technology, the powder of A. bidentata was loaded in a nylon filter cloth pocket with bore diameter of 180 µm. The pocket was fixed in the bulk liquid phase for continuously releasing saponins. Under the optimal conditions, the concentration and the extraction rate of the total saponins in the foamate by the developed technology were 73.5% and 416.2% higher than those by the traditional technology, respectively. The foamates obtained by the traditional technology and the developed technology were analyzed by ultraperformance liquid chromatography-mass spectrometry to determine their ingredients, and the results appeared that the developed technology exhibited a better performance for separating saponins than the traditional technology. The study is expected to develop a novel technology for cost effectively separating plant-derived materials with surface activity.

  18. Dispersive liquid-liquid microextraction coupled with magnetic nanoparticles for extraction of zearalenone in wheat samples

    Directory of Open Access Journals (Sweden)

    Mitra Amoli-Diva

    2017-01-01

    Full Text Available A new, sensitive and fast dispersive liquid-liquid microextraction (DLLME coupled with micro-solid phase extraction (μ-SPE was developed for determination of zearalenone (ZEN in wheat samples. The DLLME was performed using acetonitrile/water (80:20 v/v as the disperser solvent and 1-octanol as the extracting solvent.  The acetonitrile/water (80:20 v/v solvent was also used to extract ZEN from solid wheat matrix, and was directly applied as the disperser solvent for DLLME process. Additionally, hydrophobic oleic-acid-modified magnetic nanoparticles were used in μ-SPE approach to retrieve the analyte from the DLLME step. So, the method uses high surface area and strong magnetism properties of these nanoparticles to avoid time-consuming column-passing processes in traditional SPE. Main parameters affecting the extraction efficiency and signal enhancement were investigated and optimized. Under the optimum conditions, the calibration curve showed a good linearity in the range of 0.1-500 μg kg−1 (R2=0.9996 with low detection limit of 83 ng g−1. The intra-day and inter-day precisions (as RSD % in the range of 2.6-4.3 % and high recoveries ranging from 91.6 to 99.1 % were obtained. The pre-concentration factor was 3. The method is simple, inexpensive, accurate and remarkably free from interference effects.

  19. Ultrasonic slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry for the determination of Cr, Fe, Cu, Zn and Se in cereals

    Science.gov (United States)

    Huang, Shih-Yi; Jiang, Shiuh-Jen; Sahayam, A. C.

    2014-11-01

    Ultrasonic slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry (USS-ETV-ICP-MS) has been applied to determine Cr, Fe, Cu, Zn and Se in several cereal samples. Thioacetamide was used as the modifier to enhance the ion signals. The background ions at the masses of interest were reduced in intensity significantly by using 1.0 mL min- 1 methane (CH4) as reaction cell gas in the dynamic reaction cell (DRC). Since the sensitivities of Cr, Fe, Cu, Zn and Se in different matrices were quite different, standard addition and isotope dilution methods were used for the determination of Cr, Fe, Cu, Zn and Se in these cereal samples. The method detection limits estimated from standard addition curves were about 1, 10, 4, 12 and 2 ng g- 1 for Cr, Fe, Cu, Zn and Se, respectively, in original cereal samples. This procedure has been applied to the determination of Cr, Fe, Cu, Zn and Se whose concentrations are in μg g- 1 (except Cr and Se) in standard reference materials (SRM) of National institute of standards and technology (NIST), NIST SRM 1568a Rice Flour and NIST SRM 1567a Wheat Flour and two cereal samples purchased from a local market. The analysis results of reference materials agreed with certified values at 95% confidence level according to Student's T-test. The results for the real world cereal samples were also found to be in good agreement with the pneumatic nebulization DRC ICP-MS results of the sample solutions.

  20. Rapid gas chromatography with flame photometric detection of multiple organophosphorus pesticides in Salvia miltiorrhizae after ultrasonication assisted one-step extraction.

    Science.gov (United States)

    Zhang, Shanshan; Liu, Xiaofei; Qin, Jia'an; Yang, Meihua; Zhao, Hongzheng; Wang, Yong; Guo, Weiying; Ma, Zhijie; Kong, Weijun

    2017-11-15

    A simple and rapid gas chromatography-flame photometric detection (GC-FPD) method was developed for the determination of 12 organophosphorus pesticides (OPPs) in Salvia miltiorrhizae by using ultrasonication assisted one-step extraction (USAE) without any clean-up steps. Some crucial parameters such as type of extraction solvent were optimized to improve the method performance for trace analysis. Any clean-up steps were negligent as no interferences were detected in the GC-FPD chromatograms for sensitive detection. Under the optimized conditions, limits of detection (LODs) and quantitation (LOQs) for all pesticides were in the range of 0.001-0.002mg/kg and 0.002-0.01mg/kg and 0.002-0.01mg/kg, respectively, which were all below the regulatory maximum residue limits suggested. RSDs for method precision (intra- and inter-day variations) were lower than 6.8% in approval with international regulations. Average recovery rates for all pesticides at three fortification levels (0.5, 1.0 and 5.0mg/kg) were in the range of 71.2-101.0% with relative standard deviations (RSDs) pesticide (dimethoate) out of the 12 targets was simultaneously detected in four samples at concentrations of 0.016-0.02mg/kg. Dichlorvos and omethoate were found in the same sample from Sichuan province at 0.004 and 0.027mg/kg, respectively. Malathion and monocrotophos were determined in the other two samples at 0.014 and 0.028mg/kg, respectively. All the positive samples were confirmed by LC-MS/MS. The simple, reliable and rapid USAE-GC-FPD method with many advantages over traditional techniques would be preferred for trace analysis of multiple pesticides in more complex matrices. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Optimization of ultrasonic extraction and analyses methodology by HPLC for determination of diuron and its metabolites in soil cultivation of sugar cane

    Directory of Open Access Journals (Sweden)

    Maria Josefa Santos Yabe

    2009-03-01

    Full Text Available Diuron, N-(3,4-dichlorophenyl-N, N-dimethylurea can be transformed into the soil through the biodegradation of 3-(3,4-dichlorophenyl-3-methylurea (DCPMU, 3.4-diclorofenilureia (DCPU and 3,4-dichloroaniline (DCA. This study aimed to optimize and validate a method of extraction and analysis of these substances in the soil by HPLC/DAD. There was extracted with methanol in the bath ultrasonic and analysis in a liquid chromatograph/detector brand Waters. The condition of analysis optimized for separation of analytes was mobile phase methanol: water 50:50 (v / v, flow 1 mL min-1. Wavelength of 240 nm was selected for the DCA and 254 nm for diuron, DCPMU and DCPU. It was used column and pre column Waters Xterra RP18, 5 um, 4.6 and 3.9 x 150 mm x 20 mm. The calibration curve was obtained from the fortification of the soil with the mixture of patterns in the range of 5 mg Kg-1 to 200 mg Kg-1 of soil. The recovery was obtained in two concentration levels of 5 and 200 mg. Kg-1 of soil was between 85 and 99%. The repeatability was 0.78%, 2.20%, 2.17% and 1.72% and intermediate precision was 2.48%, 2.11%, 3.10% and 2.77% for diuron, DCPMU, DCPU and DCA, respectively. The limit of quantification was 1.25 mg Kg-1 soil. The concentration of diuron found in some bioaugmented soil samples ranged from 5.5 to 8.9 mg Kg-1 soil, but was not detected the presence of their metabolites.

  2. Ultrasonic neuromodulation

    Science.gov (United States)

    Naor, Omer; Krupa, Steve; Shoham, Shy

    2016-06-01

    Ultrasonic waves can be non-invasively steered and focused into mm-scale regions across the human body and brain, and their application in generating controlled artificial modulation of neuronal activity could therefore potentially have profound implications for neural science and engineering. Ultrasonic neuro-modulation phenomena were experimentally observed and studied for nearly a century, with recent discoveries on direct neural excitation and suppression sparking a new wave of investigations in models ranging from rodents to humans. In this paper we review the physics, engineering and scientific aspects of ultrasonic fields, their control in both space and time, and their effect on neuronal activity, including a survey of both the field’s foundational history and of recent findings. We describe key constraints encountered in this field, as well as key engineering systems developed to surmount them. In closing, the state of the art is discussed, with an emphasis on emerging research and clinical directions.

  3. Fabricating and Characterizing the Microfluidic Solid Phase Extraction Module Coupling with Integrated ESI Emitters

    Directory of Open Access Journals (Sweden)

    Hangbin Tang

    2018-05-01

    Full Text Available Microfluidic chips coupling with mass spectrometry (MS will be of great significance to the development of relevant instruments involving chemical and bio-chemical analysis, drug detection, food and environmental applications and so on. In our previous works, we proposed two types of microfluidic electrospray ionization (ESI chip coupling with MS: the two-phase flow focusing (FF ESI microfluidic chip and the corner-integrated ESI emitter, respectively. However the pretreatment module integrated with these ESI emitters is still a challenging problem. In this paper, we concentrated on integrating the solid phase micro-extraction (SPME module with our previous proposed on-chip ESI emitters; the fabrication processes of such SPME module are fully compatible with our previous proposed ESI emitters based on the multi-layer soft lithography. We optimized the structure of the integrated chip and characterized its performance using standard samples. Furthermore, we verified its abilities of salt removal, extraction of multiple analytes and separation through on-chip elution using mimic biological urine spiked with different drugs. The results indicated that our proposed integrated module with ESI emitters is practical and effective for real biological sample pretreatment and MS detection.

  4. Exercise capacity in the Bidirectional Glenn physiology: Coupling cardiac index, ventricular function and oxygen extraction ratio.

    Science.gov (United States)

    Vallecilla, Carolina; Khiabani, Reza H; Trusty, Phillip; Sandoval, Néstor; Fogel, Mark; Briceño, Juan Carlos; Yoganathan, Ajit P

    2015-07-16

    In Bi-directional Glenn (BDG) physiology, the superior systemic circulation and pulmonary circulation are in series. Consequently, only blood from the superior vena cava is oxygenated in the lungs. Oxygenated blood then travels to the ventricle where it is mixed with blood returning from the lower body. Therefore, incremental changes in oxygen extraction ratio (OER) could compromise exercise tolerance. In this study, the effect of exercise on the hemodynamic and ventricular performance of BDG physiology was investigated using clinical patient data as inputs for a lumped parameter model coupled with oxygenation equations. Changes in cardiac index, Qp/Qs, systemic pressure, oxygen extraction ratio and ventricular/vascular coupling ratio were calculated for three different exercise levels. The patient cohort (n=29) was sub-grouped by age and pulmonary vascular resistance (PVR) at rest. It was observed that the changes in exercise tolerance are significant in both comparisons, but most significant when sub-grouped by PVR at rest. Results showed that patients over 2 years old with high PVR are above or close to the upper tolerable limit of OER (0.32) at baseline. Patients with high PVR at rest had very poor exercise tolerance while patients with low PVR at rest could tolerate low exercise conditions. In general, ventricular function of SV patients is too poor to increase CI and fulfill exercise requirements. The presented mathematical model provides a framework to estimate the hemodynamic performance of BDG patients at different exercise levels according to patient specific data. Published by Elsevier Ltd.

  5. Ultrasonic flowmeters

    International Nuclear Information System (INIS)

    Wittekind, W.D.

    1979-01-01

    A prototype ultrasonic flowmeter was assembled and tested. The theoretical basis of this prototype ultrasonic flowmeter is reviewed; the equipment requirements for a portable unit are discussed; the individual electronic modules contained in the prototype are described; the operating procedures and configuration are explained; and the data from preliminary calibrations are presented. The calibration data confirm that the prototype operates according to theoretical predictions and can indeed provide nonintrusive flow measurements to predicted accuracies for pipes larger than two inches, under single phase stable flow conditions

  6. Coupling a Transient Solvent Extraction Module with the Separations and Safeguards Performance Model

    Energy Technology Data Exchange (ETDEWEB)

    de Almeida, Valmor F [ORNL; Birdwell Jr, Joseph F [ORNL; DePaoli, David W [ORNL; Gauld, Ian C [ORNL

    2009-10-01

    A past difficulty in safeguards design for reprocessing plants is that no code existed for analysis and evaluation of the design. A number of codes have been developed in the past, but many are dated, and no single code is able to cover all aspects of materials accountancy, process monitoring, and diversion scenario analysis. The purpose of this work was to integrate a transient solvent extraction simulation module developed at Oak Ridge National Laboratory, with the SSPM Separations and Safeguards Performance Model, developed at Sandia National Laboratory, as a first step toward creating a more versatile design and evaluation tool. The SSPM was designed for materials accountancy and process monitoring analyses, but previous versions of the code have included limited detail on the chemical processes, including chemical separations. The transient solvent extraction model is based on the ORNL SEPHIS code approach to consider solute build up in a bank of contactors in the PUREX process. Combined, these capabilities yield a much more robust transient separations and safeguards model for evaluating safeguards system design. This coupling and the initial results are presented. In addition, some observations toward further enhancement of separations and safeguards modeling based on this effort are provided, including: items to be addressed in integrating legacy codes, additional improvements needed for a fully functional solvent extraction module, and recommendations for future integration of other chemical process modules.

  7. Sugaring-out extraction of acetoin from fermentation broth by coupling with fermentation.

    Science.gov (United States)

    Dai, Jian-Ying; Ma, Lin-Hui; Wang, Zhuang-Fei; Guan, Wen-Tian; Xiu, Zhi-Long

    2017-03-01

    Acetoin is a natural flavor and an important bio-based chemical which could be separated from fermentation broth by solvent extraction, salting-out extraction or recovered in the form of derivatives. In this work, a novel method named as sugaring-out extraction coupled with fermentation was tried in the acetoin production by Bacillus subtilis DL01. The effects of six solvents on bacterial growth and the distribution of acetoin and glucose in different solvent-glucose systems were explored. The operation parameters such as standing time, glucose concentration, and volume ratio of ethyl acetate to fermentation broth were determined. In a system composed of fermentation broth, glucose (100%, m/v) and two-fold volume of ethyl acetate, nearly 100% glucose was distributed into bottom phase, and 61.2% acetoin into top phase without coloring matters and organic acids. The top phase was treated by vacuum distillation to remove solvent and purify acetoin, while the bottom phase was used as carbon source to produce acetoin in the next batch of fermentation.

  8. Coupling a transient solvent extraction module with the separations and safeguards performance model.

    Energy Technology Data Exchange (ETDEWEB)

    DePaoli, David W. (Oak Ridge National Laboratory, Oak Ridge, TN); Birdwell, Joseph F. (Oak Ridge National Laboratory, Oak Ridge, TN); Gauld, Ian C. (Oak Ridge National Laboratory, Oak Ridge, TN); Cipiti, Benjamin B.; de Almeida, Valmor F. (Oak Ridge National Laboratory, Oak Ridge, TN)

    2009-10-01

    A number of codes have been developed in the past for safeguards analysis, but many are dated, and no single code is able to cover all aspects of materials accountancy, process monitoring, and diversion scenario analysis. The purpose of this work was to integrate a transient solvent extraction simulation module developed at Oak Ridge National Laboratory, with the Separations and Safeguards Performance Model (SSPM), developed at Sandia National Laboratory, as a first step toward creating a more versatile design and evaluation tool. The SSPM was designed for materials accountancy and process monitoring analyses, but previous versions of the code have included limited detail on the chemical processes, including chemical separations. The transient solvent extraction model is based on the ORNL SEPHIS code approach to consider solute build up in a bank of contactors in the PUREX process. Combined, these capabilities yield a more robust transient separations and safeguards model for evaluating safeguards system design. This coupling and initial results are presented. In addition, some observations toward further enhancement of separations and safeguards modeling based on this effort are provided, including: items to be addressed in integrating legacy codes, additional improvements needed for a fully functional solvent extraction module, and recommendations for future integration of other chemical process modules.

  9. Continuous production of biodiesel from microalgae by extraction coupling with transesterification under supercritical conditions.

    Science.gov (United States)

    Zhou, Dan; Qiao, Baoquan; Li, Gen; Xue, Song; Yin, Jianzhong

    2017-08-01

    Raw material for biodiesel has been expanded from edible oil to non-edible oil. In this study, biodiesel continuous production for two kinds of microalgae Chrysophyta and Chlorella sp. was conducted. Coupling with the supercritical carbon dioxide extraction, the oil of microalgae was extracted firstly, and then sent to the downstream production of biodiesel. The residue after decompression can be reused as the material for pharmaceuticals and nutraceuticals. Results showed that the particle size of microalgae, temperature, pressure, molar ration of methanol to oil, flow of CO 2 and n-hexane all have effects on the yield of biodiesel. With the optimal operation conditions: 40mesh algae, extraction temperature 60°C, flow of n-hexane 0.4ml/min, reaction temperature: 340°C, pressure: 18-20MPa, CO 2 flow of 0.5L/min, molar ration of methanol to oil 84:1, a yield of 56.31% was obtained for Chrysophyta, and 63.78% for Chlorella sp. due to the higher lipid content. Copyright © 2017. Published by Elsevier Ltd.

  10. Development of an Ionic Liquid-Based Ultrasonic/Microwave-Assisted Simultaneous Distillation and Extraction Method for Separation of Camptothecin, 10-Hydroxycamptothecin, Vincoside-Lactam, and Essential Oils from the Fruits of Camptotheca acuminata Decne

    Directory of Open Access Journals (Sweden)

    Chunjian Zhao

    2016-10-01

    Full Text Available An ionic liquid-based ultrasonic/microwave-assisted simultaneous distillation and extraction (IL-UMASDE method for isolating camptothecin (CPT, 10-hydroxycamptothecin (HCPT, vincoside-lactam (VCS-LT, and essential oils (EOs from Camptotheca acuminata Decne fruits was developed. The important parameters were optimized using single-factor and central composite design experiments. The optimum conditions were 0.75 M 1-octyl-3-methylimidazolium ([C8mim]Br as the extraction solvent, a liquid–solid ratio of 13.7 mL/g, an extraction time of 33.2 min, a microwave power of 582 W, and a fixed ultrasonic power of 50 W. The yields of CPT, HCPT, and VCS-LT obtained under the optimum conditions were 2.463, 0.164, and 0.297 mg/g, respectively; these are 1.08-, 1.12-, and 1.04-fold higher, respectively, than those obtained by conventional 55% ethanol heat reflux extraction (HRE. The extraction time for the equilibrium yields of CPT, HCPT and VCS-LT using IL-UMASDE was 33.6%, 58.5%, 63.1%, and 66.8%, respectively, less than the corresponding times using IL-MASDE, IL-ultrasonic-assisted extraction (IL-UAE, 55% ethanol UAE and 55% ethanol HRE. The yield of EOs obtained using IL-UMASDE was 0.793 mg/g, i.e., 1.31-fold higher than that obtained by conventional hydrodistillation extraction (HDE. The components of the EOs obtained using IL-UMASDE and HDE were similar. The extraction time for the equilibrium yields of EOs using IL-UMASDE is 33.6%, 58.5%, 52.6%, and 72.3% lower than those for IL-MASDE, water-UMASDE, water-MASDE, and HDE, respectively. Compared with other extraction methods, IL-UMASDE gave the highest yields of CPT, HCPT, VCS-LT, and EOs and also had the shortest extraction time. IL-UMASDE is a potential green and highly efficient technique for the extraction of CPT, HCPT, VCS-LT, and EOs from Camptotheca acuminata Decne fruits.

  11. Ultrasonic inspection development at HEDL

    International Nuclear Information System (INIS)

    Day, C.K.; Mech, S.J.; Michaels, T.E.; Dixon, N.E.

    1978-01-01

    Ultrasonic testing methods and equipment are being developed to support preservice and in-service inspection of selected FFTF welds. A digital computer system is employed in the analysis of both simulated FFTF pipe sections and plate specimens containing fatigue cracks. It is anticipated that test evaluation standards containing fatigue cracks will partially eliminate questions formerly associated with weld test calibration producers by providing natural cracks which follow grain boundaries and stress patterns resembling piping situ conditions. Studies have revealed that commercial transducers may satisfy LMFBR ultrasonic pipe inspection applications: The test system evaluation included transducers and wedge coupling and fluid coupling materials which exhibited acceptable performance at temperatures to 2300C. Results are presented that demonstrate the feasibility of ultrasonic inspection of components immersed in sodium at temperatures to 2600C. (UK)

  12. Electromagnetic Coupling Between High Intensity LHC Beams and the Synchrotron Radiation Monitor Light Extraction System

    CERN Document Server

    Andreazza, W; Bravin, E; Caspers, F; Garlasch`e, M; Gras, J; Goldblatt, A; Lefevre, T; Jones, R; Metral, E; Nosych, A; Roncarolo_, F; Salvant, B; Trad, G; Veness, R; Vollinger, C; Wendt, M

    2013-01-01

    The CERN LHC is equipped with two Synchrotron Radiation Monitor (BSRT) systems used to characterise transverse and longitudinal beam distributions. Since the end of the 2011 LHC run the light extraction system, based on a retractable mirror, has suffered deformation and mechanical failure that is correlated to the increase in beam intensity. Temperature probes have associated these observations to a strong heating of the mirror support with a dependence on the longitudinal bunch length and shape, indicating the origin as electromagnetic coupling between the beam and the structure. This paper combines all this information with the aim of characterising and improving the system in view of its upgrade during the current LHC shutdown. Beam-based observations are presented along with electromagnetic and thermomechanical simulations and complemented by laboratory measurements, including the study of the RF properties of different mirror bulk and coating materials.

  13. Tetraquark candidate Zc(3900) from coupled-channel scattering - how to extract hadronic interactions? -

    Science.gov (United States)

    Ikeda, Yoichi

    2018-03-01

    We present recent progress of lattice QCD studies on hadronic interactions which play a crucial role to understand the properties of atomic nuclei and hadron resonances. There are two methods, the plateau method (or the direct method) and the HAL QCD method, to study the hadronic interactions. In the plateau method, the determination of a ground state energy from the temporal correlation functions of multi-hadron systems is a key to reliably extract the physical observables. It turns out that, due to the contamination of excited elastic scattering states nearby, one can easily be misled by a fake plateau into extracting the ground state energy. We introduce a consistency check (sanity check) which can rule out obviously false results obtained from a fake plateau, and find that none of the results obtained at the moment for two-baryon systems in the plateau method pass the test. On the other hand, the HAL QCD method is free from the fake-plateau problem. We investigate the systematic uncertainties of the HAL QCD method, which are found to be well controlled. On the basis of the HAL QCD method, the structure of the tetraquark candidate Zc(3900), which was experimentally reported in e+e- collisions, is studied by the s-wave two-meson coupled-channel scattering. The results show that the Zc(3900) is not a conventional resonance but a threshold cusp. A semi-phenomenological analysis with the coupled-channel interaction to the experimentally observed decay mode is also presented to confirm the conclusion.

  14. Lamb wave extraction of dispersion curves in micro/nano-plates using couple stress theories

    Science.gov (United States)

    Ghodrati, Behnam; Yaghootian, Amin; Ghanbar Zadeh, Afshin; Mohammad-Sedighi, Hamid

    2018-01-01

    In this paper, Lamb wave propagation in a homogeneous and isotropic non-classical micro/nano-plates is investigated. To consider the effect of material microstructure on the wave propagation, three size-dependent models namely indeterminate-, modified- and consistent couple stress theories are used to extract the dispersion equations. In the mentioned theories, a parameter called 'characteristic length' is used to consider the size of material microstructure in the governing equations. To generalize the parametric studies and examine the effect of thickness, propagation wavelength, and characteristic length on the behavior of miniature plate structures, the governing equations are nondimensionalized by defining appropriate dimensionless parameters. Then the dispersion curves for phase and group velocities are plotted in terms of a wide frequency-thickness range to study the lamb waves propagation considering microstructure effects in very high frequencies. According to the illustrated results, it was observed that the couple stress theories in the Cosserat type material predict more rigidity than the classical theory; so that in a plate with constant thickness, by increasing the thickness to characteristic length ratio, the results approach to the classical theory, and by reducing this ratio, wave propagation speed in the plate is significantly increased. In addition, it is demonstrated that for high-frequency Lamb waves, it converges to dispersive Rayleigh wave velocity.

  15. Identification of organic sulfur compounds in coal bitumen obtained by different extraction techniques using comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Machado, Maria Elisabete; Cappelli Fontanive, Fernando; Bastos Caramao, Elina; Alcaraz Zini, Claudia [Universidade Federal do Rio Grande do Sul, Instituto de Quimica, Porto Alegre, RS (Brazil); Oliveira, Jose Vladimir de [URI, Universidade Regional Integrada do Alto Uruguai e das Missoes, Erechim, RS (Brazil)

    2011-11-15

    The determination of organic sulfur compounds (OSC) in coal is of great interest. Technically and operationally these compounds are not easily removed and promote corrosion of equipment. Environmentally, the burning of sulfur compounds leads to the emission of SO{sub x} gases, which are major contributors to acid rain. Health-wise, it is well known that these compounds have mutagenic and carcinogenic properties. Bitumen can be extracted from coal by different techniques, and use of gas chromatography coupled to mass spectrometric detection enables identification of compounds present in coal extracts. The OSC from three different bitumens were tentatively identified by use of three different extraction techniques: accelerated solvent extraction (ASE), ultrasonic extraction (UE), and supercritical-fluid extraction (SFE). Results obtained from one-dimensional gas chromatography (1D GC) coupled to quadrupole mass spectrometric detection (GC-qMS) and from two-dimensional gas chromatography with time-of-flight mass spectrometric detection (GC x GC-TOFMS) were compared. By use of 2D GC, a greater number of OSC were found in ASE bitumen than in SFE and UE bitumens. No OSC were identified with 1D GC-qMS, although some benzothiophenes and dibenzothiophenes were detected by use of EIM and SIM modes. GC x GC-TOFMS applied to investigation of OSC in bitumens resulted in analytical improvement, as more OSC classes and compounds were identified (thiols, sulfides, thiophenes, naphthothiophenes, benzothiophenes, and benzonaphthothiophenes). The roof-tile effect was observed for OSC and PAH in all bitumens. Several co-elutions among analytes and with matrix interferents were solved by use of GC x GC. (orig.)

  16. Simple and accurate measurement of carbamazepine in surface water by use of porous membrane-protected micro-solid-phase extraction coupled with isotope dilution mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Teo, Hui Ling [Chemical Metrology Division, Applied Sciences Group, Health Sciences Authority, 1 Science Park Road, #01-05/06, The Capricorn, Singapore Science Park II, Singapore 117528 (Singapore); Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543 (Singapore); Wong, Lingkai [Chemical Metrology Division, Applied Sciences Group, Health Sciences Authority, 1 Science Park Road, #01-05/06, The Capricorn, Singapore Science Park II, Singapore 117528 (Singapore); Liu, Qinde, E-mail: liu_qinde@hsa.gov.sg [Chemical Metrology Division, Applied Sciences Group, Health Sciences Authority, 1 Science Park Road, #01-05/06, The Capricorn, Singapore Science Park II, Singapore 117528 (Singapore); Teo, Tang Lin; Lee, Tong Kooi [Chemical Metrology Division, Applied Sciences Group, Health Sciences Authority, 1 Science Park Road, #01-05/06, The Capricorn, Singapore Science Park II, Singapore 117528 (Singapore); Lee, Hian Kee, E-mail: chmleehk@nus.edu.sg [Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543 (Singapore)

    2016-03-17

    To achieve fast and accurate analysis of carbamazepine in surface water, we developed a novel porous membrane-protected micro-solid-phase extraction (μ-SPE) method, followed by liquid chromatography-isotope dilution tandem mass spectrometry (LC-IDMS/MS) analysis. The μ-SPE device (∼0.8 × 1 cm) was fabricated by heat-sealing edges of a polypropylene membrane sheet to devise a bag enclosing the sorbent. The analytes (both carbamazepine and isotope-labelled carbamazepine) were first extracted by μ-SPE device in the sample (10 mL) via agitation, then desorbed in an organic solvent (1 mL) via ultrasonication. Several parameters such as organic solvent for pre-conditioning of μ-SPE device, amount of sorbent, adsorption time, and desorption solvent and time were investigated to optimize the μ-SPE efficiency. The optimized method has limits of detection and quantitation estimated to be 0.5 ng L{sup −1} and 1.6 ng L{sup −1}, respectively. Surface water samples spiked with different amounts of carbamazepine (close to 20, 500, and 1600 ng L{sup −1}, respectively) were analysed for the validation of method precision and accuracy. Good precision was obtained as demonstrated by relative standard deviations of 0.7% for the samples with concentrations of 500 and 1600 ng kg{sup −1}, and 5.8% for the sample with concentration of 20 ng kg{sup −1}. Good accuracy was also demonstrated by the relative recoveries in the range of 96.7%–103.5% for all samples with uncertainties of 1.1%–5.4%. Owing to the same chemical properties of carbamazepine and isotope-labelled carbamazepine, the isotope ratio in the μ-SPE procedure was accurately controlled. The use of μ-SPE coupled with IDMS analysis significantly facilitated the fast and accurate measurement of carbamazepine in surface water. - Highlights: • μ-SPE coupled with IDMS for the measurement of carbamazepine. • The method is the first report of coupling μ-SPE with IDMS. • μ-SPE is fast, time

  17. Simultaneous determination of a variety of endocrine disrupting compounds in carrot, lettuce and amended soil by means of focused ultrasonic solid-liquid extraction and dispersive solid-phase extraction as simplified clean-up strategy.

    Science.gov (United States)

    Mijangos, L; Bizkarguenaga, E; Prieto, A; Fernández, L A; Zuloaga, O

    2015-04-10

    The present study is focused on the development of an analytical method based on focused ultrasonic solid-liquid extraction (FUSLE) followed by dispersive solid-phase extraction (dSPE) clean-up and liquid chromatography-triple quadrupole tandem mass spectrometry (LC-MS/MS) optimised for the simultaneous analysis of certain endocrine disrupting compounds (EDCs), including alkylphenols (APs), bisphenol A (BPA), triclosan (TCS) and several hormones and sterols in vegetables (lettuce and carrot) and amended soil samples. Different variables affecting the chromatographic separation, the electrospray ionisation and mass spectrometric detection were optimised in order to improve the sensitivity of the separation and detection steps. Under the optimised extraction conditions (sonication of 5min at 33% of power with pulse times on of 0.8s and pulse times off of 0.2s in 10mL of n-hexane:acetone (30:70, v:v) mixture using an ice bath), different dSPE clean-up sorbents, such as Florisil, Envi-Carb, primary-secondary amine bonded silica (PSA) and C18, or combinations of them were evaluated for FUSLE extracts before LC-MS/MS. Apparent recoveries and precision in terms of relative standard deviation (RSDs %) of the method were determined at two different fortification levels (according to the matrix and the analyte) and values in the 70-130% and 2-27% ranges, respectively, were obtained for most of the target analytes and matrices. Matrix-matched calibration approach and the use of labelled standards as surrogates were needed for the properly quantification of most analytes and matrices. Method detection limits (MDLs), estimated with fortified samples, in the ranges of 0.1-100ng/g for carrot, 0.2-152ng/g for lettuce and 0.9-31ng/g for amended soil were obtained. The developed methodology was applied to the analysis of 11 EDCs in both real vegetable bought in a local market and in compost (from a local wastewater treatment plant, WWTP) amended soil samples. Copyright © 2015

  18. Under sodium ultrasonic imaging system for PFBR

    International Nuclear Information System (INIS)

    Patankar, V.H.; Lalwani, S.K.; Agashe, A.A.

    2014-01-01

    Under Sodium UltraSonic Scanner (USUSS) has been developed to detect the growth and protrusion of fuel sub-assemblies of PFBR, submerged in liquid sodium by using the ultrasonic imaging technique during reactor shut-down when liquid sodium is at 180 ℃. The imaging is carried out prior to every Fuel handling operation. Electronics Division, BARC has designed and developed an 8-Channel Ultrasonic Imaging System (UIS) which consists of 4 downward viewing and 4 side viewing ultrasonic transducers alongwith pulser-receiver, signal processing electronics hardware and software. An automated mechanical scanner developed by IGCAR houses sodium immersible transducers to image the fuel sub assemblies. The system has been successfully tested with dummy protruding and grown FSAs, submerged under liquid sodium. Such ultrasonic imaging systems are not available to India from international market. The USUSS developed indigenously has all the features available in similar systems developed by other countries. After every imaging campaign, the mechanical scanner containing ultrasonic transducers is stored in the Argon filled storage-pit. Before every campaign of USUSS, it is necessary to check the healthiness of the sodium immersible and contaminated ultrasonic transducers, as the under-sodium scanner is decontaminated once in five years. For this purpose, a novel Non Contact Ultrasonic Inspection System (NCUIS) has been designed and developed by Electronics Division, BARC to check the functionality of the high-temperature and contaminated transducers of USUSS, using air-coupled ultrasonic technique. (author)

  19. High-Yield Preparation and Electrochemical Properties of Few-Layer MoS2 Nanosheets by Exfoliating Natural Molybdenite Powders Directly via a Coupled Ultrasonication-Milling Process

    Science.gov (United States)

    Dong, Huina; Chen, Deliang; Wang, Kai; Zhang, Rui

    2016-09-01

    Cost-effective and scalable preparation of two-dimensional (2D) molybdenum disulfide (MoS2) has been the bottleneck that limits their applications. This paper reports a novel coupled ultrasonication-milling (CUM) process to exfoliate natural molybdenite powders to achieve few-layer MoS2 (FL-MoS2) nanosheets in the solvent of N-methyl-2-pyrrolidone (NMP) with polyvinylpyrrolidone (PVP) molecules. The synergistic effect of ultrasonication and sand milling highly enhanced the exfoliation efficiency, and the precursor of natural molybdenite powders minimizes the synthetic cost of FL-MoS2 nanosheets. The exfoliation of natural molybdenite powders was conducted in a home-made CUM system, mainly consisting of an ultrasonic cell disruptor and a ceramic sand mill. The samples were characterized by X-ray diffraction, UV-vis spectra, Raman spectra, FT-IR, SEM, TEM, AFM, and N2 adsorption-desorption. The factors that influence the exfoliation in the CUM process, including the initial concentration of natural molybdenite powders ( C in, 15-55 g L-1), ultrasonic power ( P u, 200-350 W), rotation speed of sand mill ( ω s, 1500-2250 r.p.m), exfoliation time ( t ex, 0.5-6 h), and the molar ratio of PVP unit to MoS2 ( R pm, 0-1), were systematically investigated. Under the optimal CUM conditions (i.e., C in = 45 g L-1, P u = 280 W, ω s = 2250 r.p.m and R pm = 0.5), the yield at t ex = 6 h reaches 21.6 %, and the corresponding exfoliation rate is as high as 1.42 g L-1 h-1. The exfoliation efficiency of the CUM mode is much higher than that of either the ultrasonication (U) mode or the milling (M) mode. The synergistic mechanism and influencing rules of the CUM process in exfoliating natural molybdenite powders were elaborated. The as-obtained FL-MoS2 nanosheets have a high specific surface area of 924 m2 g-1 and show highly enhanced electrocatalytic performance in hydrogen evolution reaction and good electrochemical sensing property in detecting ascorbic acid. The CUM process

  20. Numerical simulation of the heat extraction in EGS with thermal-hydraulic-mechanical coupling method based on discrete fractures model

    International Nuclear Information System (INIS)

    Sun, Zhi-xue; Zhang, Xu; Xu, Yi; Yao, Jun; Wang, Hao-xuan; Lv, Shuhuan; Sun, Zhi-lei; Huang, Yong; Cai, Ming-yu; Huang, Xiaoxue

    2017-01-01

    The Enhanced Geothermal System (EGS) creates an artificial geothermal reservoir by hydraulic fracturing which allows heat transmission through the fractures by the circulating fluids as they extract heat from Hot Dry Rock (HDR). The technique involves complex thermal–hydraulic–mechanical (THM) coupling process. A numerical approach is presented in this paper to simulate and analyze the heat extraction process in EGS. The reservoir is regarded as fractured porous media consisting of rock matrix blocks and discrete fracture networks. Based on thermal non-equilibrium theory, the mathematical model of THM coupling process in fractured rock mass is used. The proposed model is validated by comparing it with several analytical solutions. An EGS case from Cooper Basin, Australia is simulated with 2D stochastically generated fracture model to study the characteristics of fluid flow, heat transfer and mechanical response in geothermal reservoir. The main parameters controlling the outlet temperature of EGS are also studied by sensitivity analysis. The results shows the significance of taking into account the THM coupling effects when investigating the efficiency and performance of EGS. - Highlights: • EGS reservoir comprising discrete fracture networks and matrix rock is modeled. • A THM coupling model is proposed for simulating the heat extraction in EGS. • The numerical model is validated by comparing with several analytical solutions. • A case study is presented for understanding the main characteristics of EGS. • The THM coupling effects are shown to be significant factors to EGS's running performance.

  1. Comparison of extraction and clean-up techniques for the ...

    African Journals Online (AJOL)

    user

    ultrasonication and mechanical shaking used in the extraction of a low-level PAH soil certified ... hydrocarbons (PAHs), soil, solid phase extraction (SPE), soxhlet extraction, ultrasonication. ... soxhlet) (Lopez-Avila et al., 1993) supercritical fluid.

  2. Determination of major aromatic constituents in vanilla using an on-line supercritical fluid extraction coupled with supercritical fluid chromatography.

    Science.gov (United States)

    Liang, Yanshan; Liu, Jiaqi; Zhong, Qisheng; Shen, Lingling; Yao, Jinting; Huang, Taohong; Zhou, Ting

    2018-04-01

    An on-line supercritical fluid extraction coupled with supercritical fluid chromatography method was developed for the determination of four major aromatic constituents in vanilla. The parameters of supercritical fluid extraction were systematically investigated using single factor optimization experiments and response surface methodology by a Box-Behnken design. The modifier ratio, split ratio, and the extraction temperature and pressure were the major parameters which have significant effects on the extraction. While the static extraction time, dynamic extraction time, and recycle time had little influence on the compounds with low polarity. Under the optimized conditions, the relative extraction efficiencies of all the constituents reached 89.0-95.1%. The limits of quantification were in the range of 1.123-4.747 μg. The limits of detection were in the range of 0.3368-1.424 μg. The recoveries of the four analytes were in the range of 76.1-88.9%. The relative standard deviations of intra- and interday precision ranged from 4.2 to 7.6%. Compared with other off-line methods, the present method obtained higher extraction yields for all four aromatic constituents. Finally, this method has been applied to the analysis of vanilla from different sources. On the basis of the results, the on-line supercritical fluid extraction-supercritical fluid chromatography method shows great promise in the analysis of aromatic constituents in natural products. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Measurement of jet production with the ATLAS detector and extraction of the strong coupling constant

    CERN Document Server

    Sawyer, Lee; The ATLAS collaboration

    2017-01-01

    The production of jets at hadron colliders provides a stringent test of perturbative QCD at the highest energies. The process can also be used to probe the gluon density function of the proton. Specific topologies can be used to extract the strong coupling constant. The ATLAS collaboration has recently measured the inclusive jet production cross section in data collected at a center-of-mass energy of 8TeV and 13TeV. The measurements have been performed differentially in jet rapidity and transverse momentum. The collaboration also presents a first measurement of the di-jet cross section at a center-of-mass energy of 13TeV as a function of the di-jet mass and rapidity. The results have been compared with state-of-the-art theory predictions at NLO in pQCD, interfaced with different parton distribution functions and can be used to constrain the proton structure. We also present new measurements of transverse energy-energy correlations (TEEC) and their associated asymmetries (ATEEC) in multi-jet events at a center...

  4. A simple and efficient ultrasonic-assisted extraction procedure combined with UV-Vis spectrophotometry for the pre-concentration and determination of folic acid (vitamin B9) in various sample matrices.

    Science.gov (United States)

    Gürkan, Ramazan; Altunay, Nail

    2016-07-01

    A simple and efficient ultrasonic-assisted extraction (UAE) procedure has been proposed for the pre-concentration of (2S)-2-[(4-{[(2-amino-4-hydroxypteridin-yl)methyl]amino}phenyl)formamido]pentanedioic acid (folic acid) in vegetables, pharmaceuticals and foods prior to determination at 540 nm using UV-Vis spectrophotometry. The method is based on hydrophobic ternary complex formation of folic acid with silver ions in the presence of cetyltrimethylammonium bromide (CTAB) as a sensitivity enhancer counter ion at pH 7.0, and then extraction into a micellar phase of polyethylene glycol monoalkyl ether (Genapol X-080). The impacts on the extraction efficiency and complex formation of analytical parameters such as sample pH, concentration of silver, concentration of surfactants and extraction time, ultrasonic time and sample volume, were investigated and optimised in detail. The matrix effect on the pre-concentration and determination of folic acid was investigated, and it was observed that the proposed method was highly selective against possible matrix co-extractives. Under optimised conditions, a good linear relationship between the analytical signal and folic acid concentration was obtained in the range of 0.6-180 μg l(-1) with a detection limit of 0.19 μg l(-1) and quantification limit of 0.63 μg l(-1). The applicability was evaluated using samples fortified at different concentration levels, and recoveries higher than 94.1% were obtained. The precision as the percent relative standard deviation (RSD%) was in range of 2.5-3.8% (10 and 40 μg l(-1), n = 5). The proposed method was validated by analysis of two standard reference materials (SRMs) and various real samples, and satisfactory results were obtained.

  5. Ultrasonic hydrometer

    Science.gov (United States)

    Swoboda, Carl A.

    1984-01-01

    The disclosed ultrasonic hydrometer determines the specific gravity (density) of the electrolyte of a wet battery, such as a lead-acid battery. The hydrometer utilizes a transducer that when excited emits an ultrasonic impulse that traverses through the electrolyte back and forth between spaced sonic surfaces. The transducer detects the returning impulse, and means measures the time "t" between the initial and returning impulses. Considering the distance "d" between the spaced sonic surfaces and the measured time "t", the sonic velocity "V" is calculated with the equation "V=2d/t". The hydrometer also utilizes a thermocouple to measure the electrolyte temperature. A hydrometer database correlates three variable parameters including sonic velocity in and temperature and specific gravity of the electrolyte, for temperature values between 0.degree. and 40.degree. C. and for specific gravity values between 1.05 and 1.30. Upon knowing two parameters (the calculated sonic velocity and the measured temperature), the third parameter (specific gravity) can be uniquely found in the database. The hydrometer utilizes a microprocessor for data storage and manipulation. The disclosed modified battery has a hollow spacer nub on the battery side wall, the sonic surfaces being on the inside of the nub and the electrolyte filling between the surfaces to the exclusion of intervening structure. An accessible pad exposed on the nub wall opposite one sonic surface allows the reliable placement thereagainst of the transducer.

  6. A fast, simple and green method for the extraction of carbamate pesticides from rice by microwave assisted steam extraction coupled with solid phase extraction.

    Science.gov (United States)

    Song, Weitao; Zhang, Yiqun; Li, Guijie; Chen, Haiyan; Wang, Hui; Zhao, Qi; He, Dong; Zhao, Chun; Ding, Lan

    2014-01-15

    This paper presented a fast, simple and green sample pretreatment method for the extraction of 8 carbamate pesticides in rice. The carbamate pesticides were extracted by microwave assisted water steam extraction method, and the extract obtained was immediately applied on a C18 solid phase extraction cartridge for clean-up and concentration. The eluate containing target compounds was finally analysed by high performance liquid chromatography with mass spectrometry. The parameters affecting extraction efficiency were investigated and optimised. The limits of detection ranging from 1.1 to 4.2ngg(-1) were obtained. The recoveries of 8 carbamate pesticides ranged from 66% to 117% at three spiked levels, and the inter- and intra-day relative standard deviation values were less than 9.1%. Compared with traditional methods, the proposed method cost less extraction time and organic solvent. Copyright © 2013 Elsevier Ltd. All rights reserved.

  7. Ultrasonically-assisted Thermal Stir Welding System

    Science.gov (United States)

    Ding, R. Jeffrey (Inventor)

    2014-01-01

    A welding head assembly has a work piece disposed between its containment plates' opposing surfaces with the work piece being maintained in a plastic state thereof at least in a vicinity of the welding head assembly's stir rod as the rod is rotated about its longitudinal axis. The welding head assembly and the work piece experience relative movement there between in a direction perpendicular to the rod's longitudinal axis as the work piece is subjected to a compressive force applied by the containment plates. A first source coupled to the first containment plate applies a first ultrasonic wave thereto such that the first ultrasonic wave propagates parallel to the direction of relative movement. A second source coupled to the second containment plate applies a second ultrasonic wave thereto such that the second ultrasonic wave propagates parallel to the direction of relative movement.propagates parallel to the direction of relative movement.

  8. [Analysis of saponins from panax notoginseng using pressurized solvent extraction coupled with liquid chromatography-electrospray mass spectrum].

    Science.gov (United States)

    Wan, Jianbo; Li, Changming; Li, Shaopin; Kong, Lingyi; Wang, Yitao

    2005-10-01

    To establish a method for qualitative analysis of saponins from Panax notoginseng using pressurized solvent extraction coupled with LC-ESI-MS. The PSE technology was applied to the process of extraction for Panax notoginseng, and the negative ion detection and multiple reaction monitoring model were used. The saponins were investigated based on total ion chromatogram (TIC) and MRM chromatogram. According to the fragment character of saponins, the molecular weight and their structures could be identified. The method can be used for qualitative analysis of saponins from Panax notoginseng.

  9. Pressurized liquid extraction using water/isopropanol coupled with solid-phase extraction cleanup for industrial and anthropogenic waste-indicator compounds in sediment

    Science.gov (United States)

    Burkhardt, M.R.; ReVello, R.C.; Smith, S.G.; Zaugg, S.D.

    2005-01-01

    A broad range of organic compounds is recognized as environmentally relevant for their potential adverse effects on human and ecosystem health. This method was developed to better determine the distribution of 61 compounds that are typically associated with industrial and household waste as well as some that are toxic and known (or suspected) for endocrine-disrupting potential extracted from environmental sediment samples. Pressurized liquid extraction (PLE) coupled with solid-phase extraction (SPE) was used to reduce sample preparation time, reduce solvent consumption to one-fifth of that required using dichloromethane-based Soxhlet extraction, and to minimize background interferences for full scan GC/MS analysis. Recoveries from spiked Ottawa sand, commercially available topsoil, and environmental stream sediment, fortified at 4-720 ??g per compound, averaged 76 ?? 13%. Initial method detection limits for single-component compounds ranged from 12.5 to 520 ??g/kg, based on 25 g samples. Results from 103 environmental sediment samples show that 36 out of 61 compounds (59%) were detected in at least one sample with concentrations ranging from 20 to 100,000 ??g/kg. The most frequently detected compound, beta-sitosterol, a plant sterol, was detected in 87 of the 103 (84.5%) environmental samples with a concentration range 360-100,000 ??g/kg. Results for a standard reference material using dichloromethane Soxhlet-based extraction are also compared. ?? 2004 Published by Elsevier B.V.

  10. Optimization of the Ultrasonic-Assisted Extraction of Phenolic Compounds from Oryza Sativa L. ‘Violet Nori’ and Determination of the Antioxidant Properties of its Caryopses and Leaves

    Directory of Open Access Journals (Sweden)

    Federica Turrini

    2018-04-01

    Full Text Available ‘Violet Nori’ is a new spontaneous growing violet rice variety showing a peculiar violet color in its fresh leaves as well. In this paper, the antioxidant properties and the content of total phenols, radical scavengers, and anthocyanins in ‘Violet Nori’ caryopses, flour, and leaves are explored and compared. Ultrasonic-Assisted Extraction (UAE is employed for the extraction of phenolic compounds, improving the extraction conditions by Design of Experiments (DoE. The obtained results show that the Radical Scavenging Activities (RSAs, the Total Phenolic Contents (TPCs, and the anthocyanin amounts (1000–1500 μg/g, expressed as cyanidin-3-glucoside of ‘Violet Nori’ caryopses are higher than those in the other analyzed colored rice samples (300–900 μg/g as cyanidin-3-glucoside, with the exception of the cultivars ‘Artemide’ and ‘Nerone’, which show comparable values of RSAs and TPCs. The study of ‘Violet Nori’ leaves at different plant maturation stages shows that their anthocyanin content is 2–3 times higher than in the caryopses and in the flour, reaching the highest levels at about 60 days from seeding. Thus, the estimated extraction yield of 4 kg anthocyanins/t makes fresh leaves very interesting for the extraction of anthocyanins on an industrial scale, whereas violet caryopses are a very interesting dietetic source of valuable anthocyanins and other antioxidant compounds.

  11. The determination of organochlorine pesticides based on dynamic microwave-assisted extraction coupled with on-line solid-phase extraction of high-performance liquid chromatography

    International Nuclear Information System (INIS)

    Chen Ligang; Ding Lan; Jin Haiyan; Song Daqian; Zhang Huarong; Li Jiantao; Zhang Kun; Wang Yutang; Zhang Hanqi

    2007-01-01

    A rapid technique based on dynamic microwave-assisted extraction coupled with on-line solid-phase extraction of high-performance liquid chromatography (DMAE-SPE-HPLC) has been developed. A TM 010 microwave resonance cavity built in the laboratory was applied to concentrate the microwave energy. The sample placed in the zone of microwave irradiation was extracted with 95% acetonitrile (ACN) aqueous solution which was driven by a peristaltic pump at a flow rate of 1.0 mL min -1 . The extraction can be completed in a recirculating system in 10 min. When a number of extraction cycles were completed, the extract (1 mL) was diluted on-line with water. Then the extract was loaded into an SPE column where the analytes were retained while the unretained matrix components were washed away. Subsequently, the analytes were automatically transferred from the SPE column to the analytical column and determined by UV detector at 238 nm. The technique was used for determination of organochlorine pesticides (OCPs) in grains, including wheat, rice, corn and bean. The limits of detection of OCPs are in the range of 19-37 ng g -1 . The recoveries obtained by analyzing the four spiked grain samples are in the range of 86-105%, whereas the relative standard deviation (R.S.D.) values are <8.7% ranging from 1.2 to 8.7%. Our method was demonstrated to be fast, accurate, and precise. In addition, only small quantities of solvent and sample were required

  12. Extraction inductively coupled plasma-optical emission spectrometry (ICP-OES). Determination of traces of phosphorus in tungsten

    International Nuclear Information System (INIS)

    Bauer, G.; Wegscheider, W.; Mueller, K.

    1989-01-01

    A method for the separation and preconcentration of traces of phosphorus from tungsten was developed. Solid phase extraction of the phosphovanadomolybdate complex performed on a micro-column was applied. Phosphorus was determined by optical emission spectroscopy (OES) with inductively coupled plasma (ICP) excitation. A limit of detection of 0,4 μg/g P with respect to the solid phase is obtained. By directly coupling the extraction/elution step to the ICP instrument a detection limit of 0,06 μg/g P in W was achieved. Besides, the complexity of spectral evaluation in ICP-OES determinations of traces in spectralline-rich matrices is discussed. (Authors)

  13. Couplings

    Science.gov (United States)

    Stošić, Dušan; Auroux, Aline

    Basic principles of calorimetry coupled with other techniques are introduced. These methods are used in heterogeneous catalysis for characterization of acidic, basic and red-ox properties of solid catalysts. Estimation of these features is achieved by monitoring the interaction of various probe molecules with the surface of such materials. Overview of gas phase, as well as liquid phase techniques is given. Special attention is devoted to coupled calorimetry-volumetry method. Furthermore, the influence of different experimental parameters on the results of these techniques is discussed, since it is known that they can significantly influence the evaluation of catalytic properties of investigated materials.

  14. Preconcentration of uranium in water samples using dispersive liquid-liquid micro- extraction coupled with solid-phase extraction and determination with inductively coupled plasma-optical emission spectrometry

    Directory of Open Access Journals (Sweden)

    M. Rezaee,

    2015-10-01

    Full Text Available A new liquid phase microextraction method based on the dispersion of an extraction solvent into aqueous phase coupled with solid-phase extraction was investigated for the extraction, preconcentration and determination of uranium in water samples. 1-(2-Pyridylazo-2-naphthol reagent (PAN at pH 6.0 was used as a chelating agent prior to extraction. After concentration and purification of the samples in SPE C18 sorbent, 1.5 mL elution sample containing 40.0 µL chlorobenzene was injected into the 5.0 mL pure water. After extraction and centrifuging, the sedimented phase was evaporated and the residue was dissolved in nitric acid (0.5 M and was injected by injection valve into the ICP-OES. Some important extraction parameters, such as sample solution flow rate, sample pH, type and volume of extraction and disperser solvents as well as the salt addition were studied and optimized. Under the optimum conditions, the calibration graph was linear in the range of 0.5-500 µg L-1. The detection limit was 0.1 µg L-1. The relative standard deviation (RSD at 5.0 µg L-1 concentration level was 6.6%. Finally, the developed method was successfully applied to the extraction and determination of uranium in the well, river, mineral, waste and tap water samples and satisfactory results were obtained.DOI: http://dx.doi.org/10.4314/bcse.v29i3.4

  15. Arsenic removal from As-hyperaccumulator Pteris vittata biomass: Coupling extraction with precipitation.

    Science.gov (United States)

    da Silva, Evandro B; de Oliveira, Letuzia M; Wilkie, Ann C; Liu, Yungen; Ma, Lena Q

    2018-02-01

    Proper disposal of As-hyperaccumulator Pteris vittata biomass (Chinese brake fern) enhances its application in phytoremediation. The goal of this study was to optimize As removal from P. vittata (PV) biomass by testing different particle sizes, extractants, extraction times and solid-to-liquid ratios. PV biomass was extracted using different extractants followed by different Mg-salts to recover soluble As via precipitation. Water-soluble As in PV biomass varied from 6.8% to 61% of total As depending on extraction time, with 99% of As being arsenate (AsV). Extraction with 2.1% HCl, 2.1% H 3 PO 4 , 1 M NaOH and 50% ethanol recovered 81, 78, 47 and 14% of As from PV biomass. A follow-up extraction using HCl recovered 27-32% with ethanol recovering only 5%. Though ethanol showed the lowest extractable As, residual As in the biomass was also the lowest. Among the extractants, 35% ethanol was the best to remove As from PV biomass. Approximately 90% As was removed from PV biomass using particle size phytoremediation more feasible. Published by Elsevier Ltd.

  16. Direct coupling of electromembrane extraction to mass spectrometry – Advancing the probe functionality toward measurements of zwitterionic drug metabolites

    DEFF Research Database (Denmark)

    Kige Rye, Torstein; Fuchs, David; Pedersen-Bjergaard, Stig

    2017-01-01

    A triple-flow electromembrane extraction (EME) probe was developed and coupled directly to electrospray-ionization mass spectrometry (ESI-MS). Metabolic reaction mixtures (pH 7.4) containing drug substances and related metabolites were continuously drawn (20 μL/min) into the EME probe in one flow......-nitrophenyl octyl ether (and for some experiments containing 30% triphenyl phosphate (TPP)), and into 20 μL min-1 of formic acid as acceptor phase, which was introduced through a third flow channel. The acceptor phase was pumped directly to the MS system, and the ion intensity of extracted analytes......, the system can potentially be used for direct analysis of various kinds of chemical reactions that have to be run at pH conditions unfavorable for direct analyte extractions....

  17. Apparatus for ultrasonic nebulization

    International Nuclear Information System (INIS)

    Olson, K.W.; Haas, W.J. Jr.; Fassel, V.A.

    1978-01-01

    An improved apparatus is described for ultrasonic nebulization of liquid samples or suspensions in which the piezoelectric transducer is protected from chemical attack and erosion. The transducer is protected by being bonded to the inner surface of a glass plate which forms one end wall of a first hollow body provided with apparatus for circulating a fluid for cooling and stabilizing the transducer. The glass plate, which is one-half wavelength in thickness to provide an acoustically coupled outer nebulizing surface, seals an opening in a second hollow body which encloses an aerosol mixing chamber. The second body includes apparatus for delivering the sample solution to the nebulizing surface, a gas inlet for providing a flow of carrier gas for transporting the aerosol of the nebulized sample and an aerosol outlet

  18. Direct coupling of electromembrane extraction to mass spectrometry - Advancing the probe functionality toward measurements of zwitterionic drug metabolites.

    Science.gov (United States)

    Rye, Torstein Kige; Fuchs, David; Pedersen-Bjergaard, Stig; Petersen, Nickolaj Jacob

    2017-08-29

    A triple-flow electromembrane extraction (EME) probe was developed and coupled directly to electrospray-ionization mass spectrometry (ESI-MS). Metabolic reaction mixtures (pH 7.4) containing drug substances and related metabolites were continuously drawn (20 μL/min) into the EME probe in one flow channel, and mixed inside the probe with 7.5 μL min -1 of 1 M formic acid as make-up flow from a second flow channel. Following this acidification, the drug substances and their related metabolites were continuously extracted by EME at 400 V, across a supported liquid membrane (SLM) comprising 2-nitrophenyl octyl ether (and for some experiments containing 30% triphenyl phosphate (TPP)), and into 20 μL min -1 of formic acid as acceptor phase, which was introduced through a third flow channel. The acceptor phase was pumped directly to the MS system, and the ion intensity of extracted analytes was followed continuously as function of time. The triple-flow EME probe was used for co-extraction of positively charged parent drugs and their zwitterionic drug metabolites (hydroxyzine and its carboxylic acid metabolite cetirizine; and vortioxetine and its carboxylic acid metabolite Lu AA34443). While the zwitterionic metabolites could not be extracted at pH 7.4, it was shown that by acidifying the sample solution the zwitterionic metabolites could be extracted effectively. Various extraction parameters like make-up flow, extraction voltage and SLM composition were optimized for simultaneous extraction of parent drugs and metabolites. It was found that TPP added to the SLM improved extraction efficiencies of certain drug metabolites. Finally the optimized and characterized triple-flow EME probe was used for online studying the in-vitro metabolism of hydroxyzine and vortioxetine by rat liver microsomes. Due to the automated pre-extraction acidification of the rat liver microsomal solutions, it was possible to continuously monitor formation of the zwitterionic drug

  19. Analytical evaluation of nebulizers for the introduction of acetic acid extracts aiming at the determination of trace elements by inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Gois, Jefferson S. de; Maranhao, Tatiane de A. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-970, Florianopolis, SC (Brazil); Oliveira, Fernando J.S. [Petroleo Brasileiro S.A., Gerencia de Meio Ambiente, Rio de Janeiro, RJ (Brazil); Frescura, Vera L.A.; Curtius, Adilson J. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-970, Florianopolis, SC (Brazil); Borges, Daniel L.G., E-mail: daniel.borges@ufsc.br [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-970, Florianopolis, SC (Brazil)

    2012-11-15

    Most of the official procedures aiming at classification of solid waste toxicity take into account metal solubility and bioavailability by means of extraction experiments using acetic acid solutions. Hence, the aim of this work was to investigate and optimize conditions to suppress the effect of acetic acid on the determination of trace elements using inductively coupled plasma mass spectrometry. The performance of four nebulizers (cross-flow (CFN), ultrasonic (USN), Meinhard (MN) and MicroMist (MMN)) were compared as to their efficiency in minimizing spectral and non-spectral effects on the determination of Ag, As, Ba, Cd, Cr, Hg, Pb and Se, with the ultimate goal to analyze acetic acid extracts obtained from solid waste residues. Operating conditions (desolvation temperatures for USN, RF power and nebulizer gas flow rates) were optimized individually for each nebulizer and for all analytes maintained in 0.14 mol L{sup -1} HNO{sub 3} solutions and in solutions prepared with acetic acid and acetic acid + NaOH, adjusted to pH 2.88 and 4.93, respectively. Pronounced non-spectral interferences for {sup 75}As and {sup 82}Se were observed in the presence of acetic acid for CF and MN, although to a less extent also for MMN and USN. Signal increase for blank solutions measured at m/z 208 ({sup 208}Pb) for CFN and MN, 107 ({sup 107}Ag) for USN and MN coupled to a cyclonic chamber and, m/z 82 ({sup 82}Se) for USN was observed, indicating an increased risk of spectral interference upon an increase in the concentration of acetic acid. Signal increase at specific m/z ratios, however, was not significant when the MMN was used, with the exception of m/z 52 ({sup 52}Cr) in acetic acid solutions, arising from the formation of {sup 40}Ar{sup 12}C{sup +}. This same effect was noticed for all nebulizers, although at noticeably different intensities. A signal stability study was performed, demonstrating that variations in the analytical signal were within a 20% range for all analytes

  20. Sorptive extraction using polydimethylsiloxane/metal-organic framework coated stir bars coupled with high performance liquid chromatography-fluorescence detection for the determination of polycyclic aromatic hydrocarbons in environmental water samples.

    Science.gov (United States)

    Hu, Cong; He, Man; Chen, Beibei; Zhong, Cheng; Hu, Bin

    2014-08-22

    In this work, metal-organic frameworks (MOFs, Al-MIL-53-NH₂) were synthesized via the hydrothermal method, and novel polydimethylsiloxane/metal-organic framework (PDMS/MOFs, PDMS/Al-MIL-53-NH₂)-coated stir bars were prepared by the sol-gel technique. The preparation reproducibility of the PDMS/MOFs-coated stir bar was good, with relative standard deviations (RSDs) ranging from 4.8% to 14.9% (n=7) within one batch and from 6.2% to 16.9% (n=6) among different batches. Based on this fact, a new method of PDMS/MOFs-coated stir bar sorptive extraction (SBSE) and ultrasonic-assisted liquid desorption (UALD) coupled with high performance liquid chromatography-fluorescence detection (HPLC-FLD) was developed for the determination of polycyclic aromatic hydrocarbons (PAHs) in environmental water samples. To obtain the best extraction performance for PAHs, several parameters affecting SBSE, such as extraction time, stirring rate, and extraction temperature, were investigated. Under optimal experimental conditions, wide linear ranges and good RSDs (n=7) were obtained. With enrichment factors (EFs) of 16.1- to 88.9-fold (theoretical EF, 142-fold), the limits of detection (LODs, S/N=3) of the developed method for the target PAHs were found to be in the range of 0.05-2.94 ng/L. The developed method was successfully applied to the analysis of PAHs in Yangtze River and East Lake water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Effective coupling functions extracted from the scattering experiments with polarized protons at moderate energies

    International Nuclear Information System (INIS)

    Barut, A.O.; Anders, T.B.; Jachmann, W.

    1992-06-01

    The experimental data for the polarization asymmetries of pp-scattering available at the scattering angle θ = 90 deg. and at various moderate energies, as well as at E = 2.4434 GeV and various scattering angles are described by smooth phenomenological coupling functions for scalar, vector, tensor and the ''magnetic moment'' couplings as well as the corresponding parity conserving axial couplings. The analysis shows a predominant role of the ''axial magnetic moment'', the axial scalar, and the axial vector interactions. Moreover, the data contain oscillations of the type sin(qw 0 -π)/(qw 0 -π), where q is the square root of the energy-momentum transfer. The oscillations have amplitudes of 5%, and a constant frequency w o = 2π/0.88 m p . They arise from oscillating modulations up to 25% of the non-axial coupling functions. 8 refs, 21 figs, 4 tabs

  2. Tetraquark candidate Zc(3900 from coupled-channel scattering - how to extract hadronic interactions? -

    Directory of Open Access Journals (Sweden)

    Ikeda Yoichi

    2018-01-01

    On the basis of the HAL QCD method, the structure of the tetraquark candidate Zc(3900, which was experimentally reported in e+e- collisions, is studied by the s-wave two-meson coupled-channel scattering. The results show that the Zc(3900 is not a conventional resonance but a threshold cusp. A semi-phenomenological analysis with the coupled-channel interaction to the experimentally observed decay mode is also presented to confirm the conclusion.

  3. Simultaneous analysis of nucleobases, nucleosides and ginsenosides in ginseng extracts using supercritical fluid chromatography coupled with single quadrupole mass spectrometry.

    Science.gov (United States)

    Huang, Yang; Zhang, Tingting; Zhao, Yumei; Zhou, Haibo; Tang, Guangyun; Fillet, Marianne; Crommen, Jacques; Jiang, Zhengjin

    2017-09-10

    Nucleobases, nucleosides and ginsenosides, which have a significant impact on the physiological activity of organisms, are reported to be the active components of ginseng, while they are less present in ginseng extracts. Few analytical methods have been developed so far to simultaneously analyze these three classes of compounds with different polarities present in ginseng extracts. In the present study, a simple and efficient analytical method was successfully developed for the simultaneous separation of 17 nucleobases, nucleosides and ginsenosides in ginseng extracts using supercritical fluid chromatography coupled with single quadrupole mass spectrometry (SFC-MS). The effect of various experimental factors on the separation performance, such as the column type, temperature and backpressure, the type of modifier and additive, and the concentration of make-up solvent were systematically investigated. Under the selected conditions, the developed method was successfully applied to the quality evaluation of 14 batches of ginseng extracts from different origins. The results obtained for the different batches indicate that this method could be employed for the quality assessment of ginseng extracts. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Speciation of the immediately mobilisable As(III), As(V), MMA and DMA in river sediments by high performance liquid chromatography-hydride generation-atomic fluorescence spectrometry following ultrasonic extraction

    International Nuclear Information System (INIS)

    Huerga, A.; Lavilla, I.; Bendicho, C.

    2005-01-01

    In this work, a fast method is developed for the speciation of As(III), As(V), MMA and DMA in the immediately mobilisable fraction of river sediments (i.e. water-soluble and phosphate-exchangeable) by high performance liquid chromatography-hydride generation-atomic fluorescence detection (HPLC-HG-AFD) after extraction using focused ultrasound. The influence of relevant parameters influencing an ion-pairing chromatographic separation following isocratic elution (i.e. amount of MeOH in the mobile phase, ion pair reagent concentration, pH, flow rate) was studied. Focused ultrasound transmitted from an ultrasonic probe provided the same extractable contents as conventional extraction with no changes in the species distribution. The effect of the drying step over extraction of As species was investigated. The following drying procedures were compared: freeze-, oven-, microwave- and air-drying. No influence of the drying operation on the water-extractable fraction was observed. However, freeze- and air-drying yielded significantly higher phosphate-extractable amounts of As(III) and As(V) as compared to oven and microwaves. Detection limits for the As species were in the range 1.3-4.1 ng/g for the water-soluble fraction and 1.6-4.8 ng/g for the phosphate buffer exchangeable fraction. The method was applied to the speciation of immediately mobilisable As(III), As(V), DMA and MMA in 11 sediment samples collected along the beds of the Louro River (southern Galicia, Spain)

  5. Graphite Microstructural Characterization Using Time-Domain and Correlation-Based Ultrasonics

    Energy Technology Data Exchange (ETDEWEB)

    Spicer, James [Johns Hopkins Univ., Baltimore, MD (United States)

    2017-12-06

    Among techniques that have been used to determine elastic modulus in nuclear graphites, ultrasonic methods have enjoyed wide use and standards using contacting piezoelectric tranducers have been developed to ensure repeatability of these types of measurements. However, the use of couplants and the pressures used to effectively couple transducers to samples can bias measurements and produce results that are not wholly related to the properties of the graphite itself. In this work, we have investigated the use of laser ultrasonic methods for making elastic modulus measurements in nuclear graphites. These methods use laser-based transmitters and receivers to gather data and do not require use of ultrasonic couplants or mechanical contact with the sample. As a result, information directly related to the elastic responses of graphite can be gathered even if the graphite is porous, brittle and compliant. In particular, we have demonstrated the use of laser ultrasonics for the determination of both Young’s modulus and shear modulus in a range of nuclear graphites including those that are being considered for use in future nuclear reactors. These results have been analyzed to assess the contributions of porosity and microcracking to the elastic responses of these graphites. Laser-based methods have also been used to assess the moduli of NBG-18 and IG-110 where samples of each grade were oxidized to produce specific changes in porosity. These data were used to develop new models for the elastic responses of nuclear graphites and these models have been used to infer specific changes in graphite microstructure that occur during oxidation that affect elastic modulus. Specifically, we show how ultrasonic measurements in oxidized graphites are consistent with nano/microscale oxidation processes where basal plane edges react more readily than basal plane surfaces. We have also shown the use of laser-based methods to perform shear-wave birefringence measurements and have shown

  6. Ultrasonic unit for line-by-line ultrasonic scanning of bodies

    International Nuclear Information System (INIS)

    Soldner, R.

    1978-01-01

    The ultrasonic unit for medical diagnostics operates by the sectorial scanning principle, which avoids direct coupling of the transducer head to the surface of the body. For this purpose, several transmitter/receiver units (approx. 100) are arranged on a partial ring of a circular arc and the ultrasonic beams, which can be triggered sequentially in time, are directed at a common intersection behind the ultrasonic window of the unit, i.e., outside the unit. A mechanical system is employed to set and adjust the partial ring carrying the transmitter/receiver units. (DG) [de

  7. SIMPLE METHOD FOR ESTIMATING POLYCHLORINATED BIPHENYL CONCENTRATIONS ON SOILS AND SEDIMENTS USING SUBCRITICAL WATER EXTRACTION COUPLED WITH SOLID-PHASE MICROEXTRACTION. (R825368)

    Science.gov (United States)

    A rapid method for estimating polychlorinated biphenyl (PCB) concentrations in contaminated soils and sediments has been developed by coupling static subcritical water extraction with solid-phase microextraction (SPME). Soil, water, and internal standards are placed in a seale...

  8. Improved extraction of hydrologic information from geophysical data through coupled hydrogeophysical inversion

    Energy Technology Data Exchange (ETDEWEB)

    Hinnell, A.C.; Ferre, T.P.A.; Vrugt, J.A.; Huisman, J.A.; Moysey, S.; Rings, J.; Kowalsky, M.B.

    2009-11-01

    There is increasing interest in the use of multiple measurement types, including indirect (geophysical) methods, to constrain hydrologic interpretations. To date, most examples integrating geophysical measurements in hydrology have followed a three-step, uncoupled inverse approach. This approach begins with independent geophysical inversion to infer the spatial and/or temporal distribution of a geophysical property (e.g. electrical conductivity). The geophysical property is then converted to a hydrologic property (e.g. water content) through a petrophysical relation. The inferred hydrologic property is then used either independently or together with direct hydrologic observations to constrain a hydrologic inversion. We present an alternative approach, coupled inversion, which relies on direct coupling of hydrologic models and geophysical models during inversion. We compare the abilities of coupled and uncoupled inversion using a synthetic example where surface-based electrical conductivity surveys are used to monitor one-dimensional infiltration and redistribution.

  9. Image processing applied to automatic detection of defects during ultrasonic examination

    International Nuclear Information System (INIS)

    Moysan, J.

    1992-10-01

    This work is a study about image processing applied to ultrasonic BSCAN images which are obtained in the field of non destructive testing of weld. The goal is to define what image processing techniques can bring to ameliorate the exploitation of the data collected and, more precisely, what image processing can do to extract the meaningful echoes which enable to characterize and to size the defects. The report presents non destructive testing by ultrasounds in the nuclear field and it indicates specificities of the propagation of ultrasonic waves in austenitic weld. It gives a state of the art of the data processing applied to ultrasonic images in nondestructive evaluation. A new image analysis is then developed. It is based on a powerful tool, the co-occurrence matrix. This matrix enables to represent, in a whole representation, relations between amplitudes of couples of pixels. From the matrix analysis, a new complete and automatic method has been set down in order to define a threshold which separates echoes from noise. An automatic interpretation of the ultrasonic echoes is then possible. Complete validation has been done with standard pieces

  10. Accelerated Aging of the Traditional Greek Distillate Tsipouro Using Wooden Chips. Part I: Effect of Static Maceration vs. Ultrasonication on the Polyphenol Extraction and Antioxidant Activity

    Directory of Open Access Journals (Sweden)

    Theodora Taloumi

    2017-01-01

    Full Text Available The Greek traditional grape marc distillate Tsipouro was subjected to accelerated aging, using wooden chips from acacia, cherry, chestnut and oak wood. The processes included treatments under static maceration and ultrasonication and the evolution of the total polyphenol concentration was monitored over a period of 30 days. During this period, leaching of polyphenols from the chips into the distillate was found to obey first-order kinetics, but no statistical differences were shown between the two treatments regarding the enrichment of the liquid in polyphenolic substances. The determination of the antioxidant activity demonstrated that aging with chestnut chips may provide Tsipouro with particularly strong radical scavenging and reducing effects, highlighting its importance as a material that could be used to turn distillates into foods with functional properties.

  11. Direct coupling of a flow-flow electromembrane extraction probe to LC-MS

    DEFF Research Database (Denmark)

    Fuchs, David; Gabel-Jensen, Charlotte; Jensen, Henrik

    2016-01-01

    the fully automated EME-LC-MS system offers a significant time saving and in addition demonstrates increased sensitivity as the analytes were automatically enriched during the extraction process. The experiment revealed 6 to 16 times higher S/N ratios of the EME-LC-MS method compared to protein...... precipitation followed by LC-MS and thus concomitantly lower LOD and LOQ. The setup integrates a complete analytical workflow of rapid extraction, enrichment, separation and detection of analytes in a fully automated manner. These attributes make the developed system a powerful alternative approach for a wide...

  12. Simultaneous multi-mycotoxin determination in nutmeg by ultrasound-assisted solid-liquid extraction and immunoaffinity column clean-up coupled with liquid chromatography and on-line post-column photochemical derivatization-fluorescence detection.

    Science.gov (United States)

    Kong, Wei-Jun; Liu, Shu-Yu; Qiu, Feng; Xiao, Xiao-He; Yang, Mei-Hua

    2013-05-07

    A simple and sensitive analytical method based on ultrasound-assisted solid-liquid extraction and immunoaffinity column clean-up coupled with high performance liquid chromatography and on-line post-column photochemical derivatization-fluorescence detection (USLE-IAC-HPLC-PCD-FLD) has been developed for simultaneous multi-mycotoxin determination of aflatoxins B1, B2, G1, G2 (AFB1, AFB2, AFG1, AFG2) and ochratoxin A (OTA) in 13 edible and medicinal nutmeg samples marketed in China. AFs and OTA were extracted from nutmeg samples by ultrasonication using a methanol : water (80 : 20, v/v) solution, followed by an IAC clean-up step. Different USL extraction conditions, pre-processing ways for nutmeg sample and clean-up columns for mycotoxins, as well as HPLC-PCD-FLD parameters (mobile phase, column temperature, elution procedure, excitation and emission wavelengths) were optimized. This method, which was appraised for analyzing nutmeg samples, showed satisfactory results with reference to limits of detection (LODs) (from 0.02 to 0.25 μg kg(-1)), limits of quantification (LOQs) (from 0.06 to 0.8 μg kg(-1)), linear ranges (up to 30 ng mL(-1) for AFB1, AFG1 and OTA and 9 ng mL(-1) for AFB2 and AFG2), intra- and inter-day variability (all application of developed method in nutmeg samples have elucidated that four samples were detected with contamination of AFs and one with OTA. AFB1 was the most frequently found mycotoxin in 30.8% of nutmeg samples at contamination levels of 0.73-16.31 μg kg(-1). At least two different mycotoxins were co-occurred in three samples, and three AFs were simultaneously detected in one sample.

  13. A simple crunching of the AGS 'bare' machine ORM data - February 2007 - to extract some aspects of AGS transverse coupling at injection and extraction

    International Nuclear Information System (INIS)

    Ahrens, L.

    2010-01-01

    The objective of this note is to (once again) explore the AGS 'ORM' (orbit response matrix) data taken (by Operations) early during the 2007 run with an AGS bare machine and gold beam. Indeed the present motivation is to extract as much information about the AGS inherent transverse coupling as possible - from general arguments and the copious ORM data. And taking this one step further, (though not accomplished yet) the goal really should be to tell the model how to describe this coupling. 'Bare' as used here means the AGS with no quadrupole, sextupole or octupole magnets powered. Only the main (combined-function) magnet string and dipole bumps necessary to optimize beam survival are powered. 'ORM data' means the systematic recording of the equilibrium orbit beam position monitor response to powering individual dipole corrector magnets. The 'matrix' results from looking at the effect of each of the (12 superperiods X 4 dipoles per superperiod) 'kicks' on each of the (12 X 6) pick up electrodes (pues) in each transverse plane. So then we have two (48 X 72) matrices of numbers from the ORM data. (Though 'pue' usually refers to the hardware in the vacuum chamber and 'bpm' to the beam position monitoring system, the two labels will be used casually here.) The exercise is carried out at two magnet rigidities, injection (AGS field ∼434 Gauss) and extraction to RHIC (∼9730 Gauss), - a ratio of rigidities of about 22.4. Since we stick with a bare machine, we are also stuck with the bare tunes which means the tunes are rather close together and near 8.75. Injection: (h,v) ∼ (8.73, 8.76).

  14. Pyrazine-functionalized calix[4]arenes: synthesis by palladium-catalyzed cross-coupling with phosphorus pronucleophiles and metal ion extraction properties

    NARCIS (Netherlands)

    Nikishkin, N.; Huskens, Jurriaan; Ansari, S.A.; Mohapatra, P.K.; Verboom, Willem

    2013-01-01

    A series of pyrazine-based calix[4]arene extractants was prepared by a stepwise functionalization, comprising palladium-catalyzed exhaustive cross-coupling of di- and tetrasubstituted calix[4]arenes bearing chloropyrazine moieties. The extraction behavior of the synthesized ligands was studied on

  15. Determine bond strength by ultrasonic measurement

    International Nuclear Information System (INIS)

    Brown, C.M.

    1978-01-01

    Application of ultrasonic methods for the evaluation and measurement of bond strength has been the object of numerous investigations in the last fifteen years. Some investigators have reported good success (in limited application) while others have experienced dismal failure. One problem common to all investigations was the difficulty in extracting and isolating the many components which comprise the ultrasonic signal reflected from a bonded interface. Part of this problem was due to manually extracting individual parameters from large volumes of raw data. However, with the vast technology now available in the field of signal analysis and computerized data processing, it is feasible to isolate and analyze individual parameters within the ultrasonic signal for great volumes of raw data

  16. Development of a simple extraction cell with bi-directional continuous flow coupled on-line to ICP-MS for assessment of elemental associations in solid samples

    DEFF Research Database (Denmark)

    Buanuam, Janya; Tiptanasup, Kasipa; Shiowatana, Juwadee

    2006-01-01

    A continuous-flow system comprising a novel, custom-built extraction module and hyphenated with inductively coupled plasma-mass spectrometric (ICP-MS) detection is proposed for assessing metal mobilities and geochemical associations in soil compartments as based on using the three step BCR (now...... the Measurements and Testing Programme of the European Commission) sequential extraction scheme. Employing a peristaltic pump as liquid driver, alternate directional flows of the extractants are used to overcome compression of the solid particles within the extraction unit to ensure a steady partitioning flow rate...... and thus to maintain constant operationally defined extraction conditions. The proposed flow set-up is proven to allow for trouble-free handling of soil samples up to 1 g and flow rates ≤ 10 mL min–1. The miniaturized extraction system was coupled to ICP-MS through a flow injection interface in order...

  17. Determination of the major constituents in fruit of Arctium lappa L. by matrix solid-phase dispersion extraction coupled with HPLC separation and fluorescence detection.

    Science.gov (United States)

    Liu, He; Zhang, Yupu; Sun, Yantao; Wang, Xue; Zhai, Yujuan; Sun, Ye; Sun, Shuo; Yu, Aimin; Zhang, Hanqi; Wang, Yinghua

    2010-10-15

    The arctiin and arctigenin in the fruit of Arctium lappa L. were extracted by matrix solid-phase dispersion (MSPD) and determined by high-performance liquid chromatography (HPLC) with fluorescence detection. The experimental conditions for the MSPD were optimized. Silica gel was selected as dispersion adsorbent and methanol as elution solvent. The calibration curve showed good relationship (r>0.9998) in the concentration range of 0.010-5.0μgmL(-1) for arctiin and 0.025-7.5μgmL(-1) for arctigenin. The recoveries were between 74.4% and 100%. The proposed method consumed less sample, time and solvent compared with conventional methods, including ultrasonic and Soxhlet extraction. Copyright © 2010 Elsevier B.V. All rights reserved.

  18. Ultrasonic horn design for ultrasonic machining technologies

    Directory of Open Access Journals (Sweden)

    Naď M.

    2010-07-01

    Full Text Available Many of industrial applications and production technologies are based on the application of ultrasound. In many cases, the phenomenon of ultrasound is also applied in technological processes of the machining of materials. The main element of equipments that use the effects of ultrasound for machining technology is the ultrasonic horn – so called sonotrode. The performance of ultrasonic equipment, respectively ultrasonic machining technologies depends on properly designed of sonotrode shape. The dynamical properties of different geometrical shapes of ultrasonic horns are presented in this paper. Dependence of fundamental modal properties (natural frequencies, mode shapes of various sonotrode shapes for various geometrical parameters is analyzed. Modal analyses of the models are determined by the numerical simulation using finite element method (FEM design procedures. The mutual comparisons of the comparable parameters of the various sonotrode shapes are presented.

  19. Determination of Five Major 8-Prenylflavones in Leaves of Epimedium by Solid-Phase Extraction Coupled with Capillary Electrophoresis

    Science.gov (United States)

    Xie, Juan-ping; Xiang, Ji-ming; Zhu, Zhong-liang

    2016-01-01

    A simple, accurate and reproducible method which is based on the capillary electrophoresis, coupled with solid-phase extraction, has been developed for simultaneous determination of multiple 8-prenylflavones from Chinese Herba Epimedii. In this study, the author has mainly illustrated the experimental process and research results of five major components including epimedin C, icariin, diphylloside A, epimedoside A and icarisoside A that have been extracted and identified from Herba Epimedii for the first time. Experimental conditions have been optimized to achieve the best separation efficiency for the following factors: the buffer pH, buffer concentration and applied voltage. The experiment can be conducted through two separable stages: the first stage is to obtain the crude extracts through the solid-phase extraction; and the second stage is to further separate five major components by using the capillary electrophoresis. The separation of the five components and the analysis of the experiment are relatively fast and can be completed within 20 min. The concentration ranges of the construction of standard curves of five major 8-prenylflavones are 32.0–395.0, 23.4–292.0, 42.1–526.0, 18.8–233.5 and 29.7–371.0 µg mL−1 respectively, which have showed acceptable linearity with a correlation coefficient, r ≥ 0.999. The coefficient varies within 2.0% for both intra- and inter-days tests. The recoveries of five components range from 92.3 to 104.1%. The relative standard deviations of recoveries of five components range from 1.2 and 2.8%. This new method will facilitate the extraction and expedite the determination of medical components from Herba Epimedii. PMID:26865656

  20. Reliable, rapid and simple method for the analysis of phthalates in sediments by ultrasonic solvent extraction followed by head space-solid phase microextraction gas chromatography mass spectrometry determination.

    Science.gov (United States)

    Fernández-González, V; Moscoso-Pérez, C; Muniategui-Lorenzo, S; López-Mahía, P; Prada-Rodríguez, D

    2017-01-01

    In this work, a new reliable, simple and fast method for the determination of six PAEs in sediments, based on ultrasonic solvent extraction (USE) followed by head space solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry determination (GC-MS), is proposed. The extraction parameters were studied, and the most favourable conditions were selected. The analytical features of the method were calculated: matrix effect, accuracy (ranged from 90% to 111%), repeatability and intermediate precision (RSD <10%), detection and quantification limits of the method (ranged from 0.001µgg -1 (DOP) to 0.142µgg -1 (DEP)), and satisfactory results were obtained. Major advantages of this approach are low consumption of reagents and solvents, no clean-up or evaporation steps were required and minimum sample manipulation. In addition, cross contamination from glassware, solvents and samples is minimized, thus procedural blanks are keeping to a minimum.. The applicability of the proposed method was demonstrated analysing sediment samples from Galician coast (NW Spain). The proposed method allows the application in routine laboratory conditions and its implementation in environmental monitoring studies under the European Water Framework Directive (WFD) and Marine Strategy Framework Directive (MSFD). Copyright © 2016 Elsevier B.V. All rights reserved.

  1. A new ultrasonic-assisted cloud-point-extraction procedure for pre-concentration and determination of ultra-trace levels of copper in selected beverages and foods by flame atomic absorption spectrometry.

    Science.gov (United States)

    Altunay, Nail; Gürkan, Ramazan; Orhan, Ulaş

    2015-01-01

    A new ultrasonic-assisted cloud-point-extraction (UA-CPE) method was developed for the pre-concentration of Cu(II) in selected beverage and food samples prior to flame atomic absorption spectrometric (FAAS) analysis. For this purpose, Safranin T was used as an ion-pairing reagent based on charge transfer in the presence of oxalate as the primary chelating agent at pH 10. Non-ionic surfactant, poly(ethyleneglycol-mono-p-nonylphenylether) (PONPE 7.5) was used as an extracting agent in the presence of NH4Cl as the salting out agent. The variables affecting UA-CPE efficiency were optimised in detail. The linear range for Cu(II) at pH 10 was 0.02-70 µg l(-)(1) with a very low detection limit of 6.10 ng l(-)(1), while the linear range for Cu(I) at pH 8.5 was 0.08-125 µg l(-)(1) with a detection limit of 24.4 ng l(-)(1). The relative standard deviation (RSD %) was in the range of 2.15-4.80% (n = 5). The method was successfully applied to the quantification of Cu(II), Cu(I) and total Cu in selected beverage and food samples. The accuracy of the developed method was demonstrated by the analysis of two standard reference materials (SRMs) as well as recoveries of spiked samples.

  2. Electromembrane extraction of heavy metal cations followed by capillary electrophoresis with capacitively coupled contactless conductivity detection

    Czech Academy of Sciences Publication Activity Database

    Kubáň, Pavel; Strieglerová, Lenka; Gebauer, Petr; Boček, Petr

    2011-01-01

    Roč. 32, č. 9 (2011), s. 1025-1032 ISSN 0173-0835 R&D Projects: GA ČR GA203/08/1536; GA ČR GAP206/10/1219; GA AV ČR IAA400310703 Institutional research plan: CEZ:AV0Z40310501 Keywords : capillary electrophoresis * electromembrane extraction * heavy metal cations Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.303, year: 2011

  3. Measurement of jet production with the ATLAS detector and extraction of the strong coupling constant

    CERN Document Server

    Marceca, Gino; The ATLAS collaboration

    2017-01-01

    The inclusive-jet cross-section at 8 TeV and the inclusive-jet and dijet cross-sections at 13 TeV with the ATLAS detector are presented. NLO QCD calculations, and NNLO for the inclusive-jet measurement at 13 TeV, are compared to the measurements. The extraction of $\\alpha_{s}$ from the measurement of the transverse energy-energy correlation at 8 TeV with the ATLAS detector is also presented.

  4. Oxidative Desulfurization of Gasoline by Ionic Liquids Coupled with Extraction by Organic Solvents

    OpenAIRE

    Abro, Rashid; Gao, Shurong; Chen, Xiaochun; Yu, Guangren; Abdeltawab, Ahmed A.; Al-Deyab, Salem S.

    2016-01-01

    In this work, desulfurization of real fluidized catalytic cracking (FCC) gasoline was investigated in dual steps; first in oxidative desulfurization (ODS) using imidazolium and pyrrolidonium based Brønsted acidic ionic liquids (ILs) as solvent and catalyst and hydrogen peroxide as oxidant. In second step, extractive desulfurization took place using organic solvents of furfural, furfural alcohol and ethylene glycol. Variety of factors such as temperature, time, mass ratio of oil/ILs and regene...

  5. Hybrid Multiphase CFD Solver for Coupled Dispersed/Segregated Flows in Liquid-Liquid Extraction

    Directory of Open Access Journals (Sweden)

    Kent E. Wardle

    2013-01-01

    Full Text Available The flows in stage-wise liquid-liquid extraction devices include both phase segregated and dispersed flow regimes. As a additional layer of complexity, for extraction equipment such as the annular centrifugal contactor, free-surface flows also play a critical role in both the mixing and separation regions of the device and cannot be neglected. Traditionally, computional fluid dynamics (CFD of multiphase systems is regime dependent—different methods are used for segregated and dispersed flows. A hybrid multiphase method based on the combination of an Eulerian multifluid solution framework (per-phase momentum equations and sharp interface capturing using Volume of Fluid (VOF on selected phase pairs has been developed using the open-source CFD toolkit OpenFOAM. Demonstration of the solver capability is presented through various examples relevant to liquid-liquid extraction device flows including three-phase, liquid-liquid-air simulations in which a sharp interface is maintained between each liquid and air, but dispersed phase modeling is used for the liquid-liquid interactions.

  6. Reinforcement of poly(amide-imide) containing N-trimellitylimido-L-phenylalanine by using nano α-Al2O3 surface-coupled with bromo-flame retardant under ultrasonic irradiation technique

    Science.gov (United States)

    Mallakpour, Shadpour; Khadem, Elham

    2014-10-01

    By the uniform dispersion of nanoparticles into a polymer matrix, a substantial improvement of physicochemical properties can be attained. In this study, a series of poly(amide-imide)/Al2O3 nanocomposites (PANC)s based on various amounts of modified α-Al2O3 nanoparticles (ANP)s were prepared using the ultrasonic irradiation method. In the process of manufacturing the nanocomposites (NC)s, severe agglomeration of ANPs into the polymer matrix can be reduced using 2,3,4,5-tetrabromo-6-[(4-hydroxyphenyl)carbamoyl]benzoic acid as novel coupling agent. The effects of modified ANPs on the morphology and properties of the polymer matrix were studied by means of Fourier transform infrared spectroscopy, X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy and thermal gravimetric analysis (TGA). The results obtained by TGA showed that the thermal stability of the NCs was improved with the addition of the small amounts of ANPs as effective thermal degradation resistant reinforcement.

  7. Development of injection moulded, ultrasonically welded immiscible phase filtration devices

    DEFF Research Database (Denmark)

    Kistrup, Kasper

    for ultrasonic welding, suitable for microfluidic systems. A methodology has been established where energy directors can be quickly added to existing mould inserts, using laser micromachining. The produced device was performance tested by isolating methicillin-resistant Staphylococcus aureus from bovine whole....... The device appliesmagnetic bead-based solid-phase extraction for nucleic acid extraction from biological samples, using the immiscible phase filtration (IPF) approach. Device development has employed injection moulding for part fabrication and ultrasonic welding for bonding. Rapid prototyping...

  8. Electromagnetic ultrasonic guided waves

    CERN Document Server

    Huang, Songling; Li, Weibin; Wang, Qing

    2016-01-01

    This book introduces the fundamental theory of electromagnetic ultrasonic guided waves, together with its applications. It includes the dispersion characteristics and matching theory of guided waves; the mechanism of production and theoretical model of electromagnetic ultrasonic guided waves; the effect mechanism between guided waves and defects; the simulation method for the entire process of electromagnetic ultrasonic guided wave propagation; electromagnetic ultrasonic thickness measurement; pipeline axial guided wave defect detection; and electromagnetic ultrasonic guided wave detection of gas pipeline cracks. This theory and findings on applications draw on the author’s intensive research over the past eight years. The book can be used for nondestructive testing technology and as an engineering reference work. The specific implementation of the electromagnetic ultrasonic guided wave system presented here will also be of value for other nondestructive test developers.

  9. Determination of chlorinated polycyclic aromatic hydrocarbons in water by solid-phase extraction coupled with gas chromatography and mass spectrometry.

    Science.gov (United States)

    Wang, Xianli; Kang, Haiyan; Wu, Junfeng

    2016-05-01

    Given the potential risks of chlorinated polycyclic aromatic hydrocarbons, the analysis of their presence in water is very urgent. We have developed a novel procedure for determining chlorinated polycyclic aromatic hydrocarbons in water based on solid-phase extraction coupled with gas chromatography and mass spectrometry. The extraction parameters of solid-phase extraction were optimized in detail. Under the optimal conditions, the proposed method showed wide linear ranges (1.0-1000 ng/L) with correlation coefficients ranging from 0.9952 to 0.9998. The limits of detection and the limits of quantification were in the range of 0.015-0.591 and 0.045-1.502 ng/L, respectively. Recoveries ranged from 82.5 to 102.6% with relative standard deviations below 9.2%. The obtained method was applied successfully to the determination of chlorinated polycyclic aromatic hydrocarbons in real water samples. Most of the chlorinated polycyclic aromatic hydrocarbons were detected and 1-monochloropyrene was predominant in the studied water samples. This is the first report of chlorinated polycyclic aromatic hydrocarbons in water samples in China. The toxic equivalency quotients of chlorinated polycyclic aromatic hydrocarbons in the studied tap water were 9.95 ng the toxic equivalency quotient m(-3) . 9,10-Dichloroanthracene and 1-monochloropyrene accounted for the majority of the total toxic equivalency quotients of chlorinated polycyclic aromatic hydrocarbons in tap water. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Comparison of inductively coupled plasma mass spectrometry and colorimetric determination of total and extractable phosphorus in soils

    International Nuclear Information System (INIS)

    Ivanov, Krasimir; Zaprjanova, Penka; Petkova, Milena; Stefanova, Violeta; Kmetov, Veselin; Georgieva, Deyana; Angelova, Violina

    2012-01-01

    The most widely used method for determination of total phosphorus in soils is perchloric acid digestion, followed by a colorimetric assay to measure the concentration of P in solution. The first part of this study compares an alternative digestion method, using aqua regia (ISO 11466 and EPA Method 3052), with perchloric acid digestion procedure, and also compares inductively coupled plasma mass spectroscopy (ICP-MS) with colorimetry for the measurement of P on the basis of five internationally certified standard soils and 20 real-life soils with widely different extractability of phosphorus. The phosphorus concentration was determined by means of the reduced phosphomolybdenum blue and ICP-MS. The relationship between methods has been examined statistically. Good agreement of the results from colorimetry and ICP-MS was established for all certified soils. The microwave-assisted digestion with aqua regia was comparable, both in precision and accuracy, with the hot plate aqua regia method. The phosphorus concentration found with the HF + HClO 4 digestion method was in good agreement with the certified mean values, while the superiority in extracting phosphorus, when compared to other methods, was obvious. Soil testing for plant-available phosphorus in Bulgaria and many European countries is most commonly conducted using acid Ca-lactate extraction (Egner–Riehm test) and alkaline sodium bicarbonate extraction (BDS ISO 11263:2002), based on Olsen test, followed by a colorimetric assay to measure the concentration of P in solution. The second part of this study reports the differences between Egner–Riehm test and BDS ISO 11263:2002 measured colorimetrically and by ICP-MS. Fifty soils were selected from South Bulgaria to represent a wide range of soil properties. It was established that ICP-MS consistently yielded significantly higher P concentrations than the colorimetric method in both extraction tests, and the relative differences were greatest in soils with lower P

  11. Comparison of inductively coupled plasma mass spectrometry and colorimetric determination of total and extractable phosphorus in soils

    Energy Technology Data Exchange (ETDEWEB)

    Ivanov, Krasimir, E-mail: kivanov1@abv.bg [Department of Chemistry, University of Agriculture, Plovdiv (Bulgaria); Zaprjanova, Penka [Tobacco and Tobacco Products Institute, Plovdiv (Bulgaria); Petkova, Milena [Department of Chemistry, University of Agriculture, Plovdiv (Bulgaria); Stefanova, Violeta; Kmetov, Veselin; Georgieva, Deyana [Department of Analytical Chemistry, Plovdiv University ' Paisii Hilendarski,' Plovdiv (Bulgaria); Angelova, Violina [Department of Chemistry, University of Agriculture, Plovdiv (Bulgaria)

    2012-05-15

    The most widely used method for determination of total phosphorus in soils is perchloric acid digestion, followed by a colorimetric assay to measure the concentration of P in solution. The first part of this study compares an alternative digestion method, using aqua regia (ISO 11466 and EPA Method 3052), with perchloric acid digestion procedure, and also compares inductively coupled plasma mass spectroscopy (ICP-MS) with colorimetry for the measurement of P on the basis of five internationally certified standard soils and 20 real-life soils with widely different extractability of phosphorus. The phosphorus concentration was determined by means of the reduced phosphomolybdenum blue and ICP-MS. The relationship between methods has been examined statistically. Good agreement of the results from colorimetry and ICP-MS was established for all certified soils. The microwave-assisted digestion with aqua regia was comparable, both in precision and accuracy, with the hot plate aqua regia method. The phosphorus concentration found with the HF + HClO{sub 4} digestion method was in good agreement with the certified mean values, while the superiority in extracting phosphorus, when compared to other methods, was obvious. Soil testing for plant-available phosphorus in Bulgaria and many European countries is most commonly conducted using acid Ca-lactate extraction (Egner-Riehm test) and alkaline sodium bicarbonate extraction (BDS ISO 11263:2002), based on Olsen test, followed by a colorimetric assay to measure the concentration of P in solution. The second part of this study reports the differences between Egner-Riehm test and BDS ISO 11263:2002 measured colorimetrically and by ICP-MS. Fifty soils were selected from South Bulgaria to represent a wide range of soil properties. It was established that ICP-MS consistently yielded significantly higher P concentrations than the colorimetric method in both extraction tests, and the relative differences were greatest in soils with lower

  12. Ultrasonic testing device

    International Nuclear Information System (INIS)

    Lawrie, W.E.

    1978-01-01

    The ultrasonic transmitter made of polarized ferroelectric ceramic material (lead zirconate titanate) is arranged in a strip carrier which allows it to be introduced between the fuel elements of a fuel subassembly in a water cooled nuclear reactor. The ultrasonic transmitter is insulated relative to the carrier. The echo of the ra dal ultrasonic pulse is recorded which changes as faulty water filled fuel elements are detected. (RW) [de

  13. Box-Behnken design for optimum extraction of biogenetic chemicals from P. lanceolata with an energy audit (thermal × microwave × acoustic): a case study of HPTLC determination with additional specificity using on-line/off-line coupling with DAD/NIR/ESI-MS.

    Science.gov (United States)

    Srivastava, Pooja; Ajayakumar, P V; Shanker, Karuna

    2014-01-01

    The genus Pluchea comprises about 80 species distributed worldwide, out of them, only Pluchea lanceolata (DC.) Oliv. & Hiern, is used extensively in the traditional system of India. No chromatographic method is available for its quality. To perform the energy audit for the extraction of biogenetic pentacyclic triterpene, its acetate and sterol from P. lanceolata utilising organic and four alternative solvents. Additionally to resolve the uncertainty of TLC determination, on-line/off-line coupling with a diode-array detector (DAD), and near-infrared (NIR) and electrospray ionisation (ESI) MS was introduced. The extraction of taraxasterol (Tx), taraxasterol acetate (TxAc) and stigmasterol (St) from P. lanceolata was performed using three energy modes. The effects of different operating parameters were studied for optimum extraction yield using the design of experiments, that is, the central composite design and Box-Behnken design. In addition to the retention factor (Rf ) and visible spectral matching, two additional optical spectroscopic techniques, that is, NIR and ESI-MS, were applied for extended specificity. The method was developed for Tx, TxAc and St determination using HPTLC at 645 nm. The optimum extraction yield of targeted compounds was found to be higher with organic solvents than eco-friendly surfactants. The pulse ultrasonic assisted extraction (PUAE) has resulted in optimum extraction of compounds comparable to hot extraction. Both NIR and ESI-MS provided extended specificity in determination. The 5/1-PUAE was determined to be effective, reproducible, simple and energy efficient for the determination of Tx, TxAc and St in P. lanceolata. The offline coupling of NIR and ESI-MS with HPTLC led to considerable improvement in specificity. Copyright © 2014 John Wiley & Sons, Ltd.

  14. Extraction and analysis of silver and gold nanoparticles from biological tissues using single particle inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Gray, Evan P; Coleman, Jessica G; Bednar, Anthony J; Kennedy, Alan J; Ranville, James F; Higgins, Christopher P

    2013-12-17

    Expanded use of engineered nanoparticles (ENPs) in consumer products increases the potential for environmental release and unintended biological exposures. As a result, measurement techniques are needed to accurately quantify ENP size, mass, and particle number distributions in biological matrices. This work combines single particle inductively coupled plasma mass spectrometry (spICPMS) with tissue extraction to quantify and characterize metallic ENPs in environmentally relevant biological tissues for the first time. ENPs were extracted from tissues via alkaline digestion using tetramethylammonium hydroxide (TMAH). Method development was performed using ground beef and was verified in Daphnia magna and Lumbriculus variegatus . ENPs investigated include 100 and 60 nm Au and Ag stabilized by polyvynylpyrrolidone (PVP). Mass- and number-based recovery of spiked Au and Ag ENPs was high (83-121%) from all tissues tested. Additional experiments suggested ENP mixtures (60 and 100 nm Ag ENPs) could be extracted and quantitatively analyzed. Biological exposures were also conducted to verify the applicability of the method for aquatic organisms. Size distributions and particle number concentrations were determined for ENPs extracted from D. magna exposed to 98 μg/L 100 nm Au and 4.8 μg/L 100 nm Ag ENPs. The D. magna nanoparticulate body burden for Au ENP uptake was 613 ± 230 μg/kgww, while the measured nanoparticulate body burden for D. magna exposed to Ag ENPs was 59 ± 52 μg/kgww. Notably, the particle size distributions determined from D. magna tissues suggested minimal shifts in the size distributions of ENPs accumulated, as compared to the exposure media.

  15. Microwave assisted extraction of iodine and bromine from edible seaweed for inductively coupled plasma-mass spectrometry determination.

    Science.gov (United States)

    Romarís-Hortas, Vanessa; Moreda-Piñeiro, Antonio; Bermejo-Barrera, Pilar

    2009-08-15

    The feasibility of microwave energy to assist the solubilisation of edible seaweed samples by tetramethylammonium hydroxide (TMAH) has been investigated to extract iodine and bromine. Inductively coupled plasma-mass spectrometry (ICP-MS) has been used as a multi-element detector. Variables affecting the microwave assisted extraction/solubilisation (temperature, TMAH volume, ramp time and hold time) were firstly screened by applying a fractional factorial design (2(5-1)+2), resolution V and 2 centre points. When extracting both halogens, results showed statistical significance (confidence interval of 95%) for TMAH volume and temperature, and also for the two order interaction between both variables. Therefore, these two variables were finally optimized by a 2(2)+star orthogonal central composite design with 5 centre points and 2 replicates, and optimum values of 200 degrees C and 10 mL for temperature and TMAH volume, respectively, were found. The extraction time (ramp and hold times) was found statistically non-significant, and values of 10 and 5 min were chosen for the ramp time and the hold time, respectively. This means a fast microwave heating cycle. Repeatability of the over-all procedure has been found to be 6% for both elements, while iodine and bromine concentrations of 24.6 and 19.9 ng g(-1), respectively, were established for the limit of detection. Accuracy of the method was assessed by analyzing the NIES-09 (Sargasso, Sargassum fulvellum) certified reference material (CRM) and the iodine and bromine concentrations found have been in good agreement with the indicative values for this CRM. Finally, the method was applied to several edible dried and canned seaweed samples.

  16. 超声波萃取-高效液相色谱测定电子产品中多溴二苯醚%Determination of Polybrominated Diphenyl Ethers in Electrotechnical Products by Ultrasonic Extraction-HPLC

    Institute of Scientific and Technical Information of China (English)

    郑灿城; 赵兴茂; 邓华丽

    2012-01-01

    文章采用超声波萃取-高效液相色谱建立了测定电子电器产品中的方法:选用正丙醇作为萃取剂,采用超声波萃取装置对电子电器产品中的溴系阻燃剂,以甲醇/超纯水为流动相,在反相C18色谱柱上进行梯度淋洗,检测波长226 nm,该方法对于9种目标多溴二苯醚的回收率为92%~96%,相对标准偏(RSD)均小于5%,该方法的检测限为〈0.1 mg/kg,具有良好的准确性和精密度。可以满足RoHS指令中溴阻燃剂的测定分析。如用该方法对普通电路板进行测定,可知道其中PBDE-209的含量约为314.7436 mg/kg。%Established and tested the PBDEs which in electronic products using Ultrasonic extraction-HPLC: using propanol as solvent,adopting Ultrasonic extracted PBEDs from the electronic products,agent to methanol/ water as mobile phase,in reverse phase chromatographic column on C18 gradient elution,detected wavelength 226 nm,this method for goals more biphenyl ether bromide that the recovery was 92 %~96 %,the relative standard partial(RSD) were less than 5 %,the method of detection limit for 0.1 mg/kg,with good accuracy and precision.The experiment showed that the method can meet the testing needs of the work which the RoHS carry out testing of PBDEs in many electronic products,such as to circuit board,can know which were PBDE-209 content is about 314.7436 mg/kg.

  17. Multivariate analysis of the volatile components in tobacco based on infrared-assisted extraction coupled to headspace solid-phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Yang, Yanqin; Pan, Yuanjiang; Zhou, Guojun; Chu, Guohai; Jiang, Jian; Yuan, Kailong; Xia, Qian; Cheng, Changhe

    2016-11-01

    A novel infrared-assisted extraction coupled to headspace solid-phase microextraction followed by gas chromatography with mass spectrometry method has been developed for the rapid determination of the volatile components in tobacco. The optimal extraction conditions for maximizing the extraction efficiency were as follows: 65 μm polydimethylsiloxane-divinylbenzene fiber, extraction time of 20 min, infrared power of 175 W, and distance between the infrared lamp and the headspace vial of 2 cm. Under the optimum conditions, 50 components were found to exist in all ten tobacco samples from different geographical origins. Compared with conventional water-bath heating and nonheating extraction methods, the extraction efficiency of infrared-assisted extraction was greatly improved. Furthermore, multivariate analysis including principal component analysis, hierarchical cluster analysis, and similarity analysis were performed to evaluate the chemical information of these samples and divided them into three classifications, including rich, moderate, and fresh flavors. The above-mentioned classification results were consistent with the sensory evaluation, which was pivotal and meaningful for tobacco discrimination. As a simple, fast, cost-effective, and highly efficient method, the infrared-assisted extraction coupled to headspace solid-phase microextraction technique is powerful and promising for distinguishing the geographical origins of the tobacco samples coupled to suitable chemometrics. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Applied orthogonal design for filtrating conditions of ultrasonic ...

    African Journals Online (AJOL)

    user

    2011-03-28

    Mar 28, 2011 ... ultrasonic-assisted extraction from plant-chicory. Yuyan Liu1 ... leaves are grown for consumption in salads and vege- ..... *The highest extraction percentage of the levels is highlighted in bold; **It is the ordinal numeral for the range sequence ..... of mass transfer in supercritical CO2 extraction processes.

  19. EXTRACT

    DEFF Research Database (Denmark)

    Pafilis, Evangelos; Buttigieg, Pier Luigi; Ferrell, Barbra

    2016-01-01

    The microbial and molecular ecology research communities have made substantial progress on developing standards for annotating samples with environment metadata. However, sample manual annotation is a highly labor intensive process and requires familiarity with the terminologies used. We have the...... and text-mining-assisted curation revealed that EXTRACT speeds up annotation by 15-25% and helps curators to detect terms that would otherwise have been missed.Database URL: https://extract.hcmr.gr/......., organism, tissue and disease terms. The evaluators in the BioCreative V Interactive Annotation Task found the system to be intuitive, useful, well documented and sufficiently accurate to be helpful in spotting relevant text passages and extracting organism and environment terms. Comparison of fully manual...

  20. Extraction of butyltins from sediments and their determination by liquid chromatography interfaced to inductively coupled plasma atomic emission detector

    International Nuclear Information System (INIS)

    Rivaro, P.; Frache, R.

    2000-01-01

    A liquid-liquid extraction of the butyltin compounds from sediment, suitable for their subsequent following determination by high performance liquid chromatography-hydride generation inductively coupled plasma atomic emission detector system, is proposed. Recoveries of 86%, 80% and 42% for tributyltin (TBT), dibutyltin (DBT) and monobutyltin (MBT) respectively were achieved. The relative detection limits of butyltin compounds by this method ranged from 27 to 62 ng of tin per gram of dry sediment. The method was applied to real sediment samples collected in the Venice lagoon (Italy). The results showed that, despite the restrictions on the use of butyltin contained in antifoulting paints, a considerable amount of organotin compounds is still present in Venice sediments [it

  1. Determination of chiral pharmaceuticals and illicit drugs in wastewater and sludge using microwave assisted extraction, solid-phase extraction and chiral liquid chromatography coupled with tandem mass spectrometry.

    Science.gov (United States)

    Evans, Sian E; Davies, Paul; Lubben, Anneke; Kasprzyk-Hordern, Barbara

    2015-07-02

    This is the first study presenting a multi-residue method allowing for comprehensive analysis of several chiral pharmacologically active compounds (cPACs) including beta-blockers, antidepressants and amphetamines in wastewater and digested sludge at the enantiomeric level. Analysis of both the liquid and solid matrices within wastewater treatment is crucial to being able to carry out mass balance within these systems. The method developed comprises filtration, microwave assisted extraction and solid phase extraction followed by chiral liquid chromatography coupled with tandem mass spectrometry to analyse the enantiomers of 18 compounds within all three matrices. The method was successfully validated for 10 compounds within all three matrices (amphetamine, methamphetamine, MDMA, MDA, venlafaxine, desmethylvenlafaxine, citalopram, metoprolol, propranolol and sotalol), 7 compounds validated for the liquid matrices only (mirtazapine, salbutamol, fluoxetine, desmethylcitalopram, atenolol, ephedrine and pseudoephedrine) and 1 compound (alprenolol) passing the criteria for solid samples only. The method was then applied to wastewater samples; cPACs were found at concentration ranges in liquid matrices of: 1.7 ng L(-1) (metoprolol) - 1321 ng L(-1) (tramadol) in influent,

  2. Ultrasonic monitoring system

    International Nuclear Information System (INIS)

    McLain, R.E.

    1975-01-01

    The ultrasonic monitoring system is used in LMFBR's, BWR's or PWR's. A remotely controlled, movable instrument carrier may be used which contains the piezo-electric transducer and is connected to the main control console by a transmission cable. An excitation pulse coming from a pulse generator is used to excite the transducer with a maximum of energy, independent of the length of the transmission line. Pulse width and pulse amplitude can be set without any direct interference into the transducer. For this purpose, a resistor whose impedance has been matched to that of the transmission line is connected to the input of the transmission line. Moreover, a capacitor for generation of the excitation pulse is coupled with the transmission line by means of a four-layer switching diode and is discharged. For termination of the excitation and the control pulses, respectively, another four-layer switching diode connected parallel to the capacitor quickly discharges the capacitor. The capacitor and the capacitance of the line constitute a voltage divider. In this way it is possible to change the length of the transmission line and, to safeguard the generation of a pulse of the desired amplitude, only vary the capacitance of the capacitor. (DG/RF) [de

  3. Ultrasonic flow meter

    NARCIS (Netherlands)

    Lötters, Joost Conrad; Snijders, G.J.; Volker, A.W.F.

    2014-01-01

    The invention relates to an ultrasonic flow meter comprising a flow tube for the fluid whose flow rate is to be determined. The flow meter comprises a transmitting element for emitting ultrasonic waves, which is provided on the outer jacket of the flow tube. A receiving element, which is provided on

  4. Examples of coupled human and environmental systems from the extractive industry and hydropower sector interfaces.

    Science.gov (United States)

    Castro, Marcia C; Krieger, Gary R; Balge, Marci Z; Tanner, Marcel; Utzinger, Jürg; Whittaker, Maxine; Singer, Burton H

    2016-12-20

    Large-scale corporate projects, particularly those in extractive industries or hydropower development, have a history from early in the twentieth century of creating negative environmental, social, and health impacts on communities proximal to their operations. In many instances, especially for hydropower projects, the forced resettlement of entire communities was a feature in which local cultures and core human rights were severely impacted. These projects triggered an activist opposition that progressively expanded and became influential at both the host community level and with multilateral financial institutions. In parallel to, and spurred by, this activism, a shift occurred in 1969 with the passage of the National Environmental Policy Act in the United States, which required Environmental Impact Assessment (EIA) for certain types of industrial and infrastructure projects. Over the last four decades, there has been a global movement to develop a formal legal/regulatory EIA process for large industrial and infrastructure projects. In addition, social, health, and human rights impact assessments, with associated mitigation plans, were sequentially initiated and have increasingly influenced project design and relations among companies, host governments, and locally impacted communities. Often, beneficial community-level social, economic, and health programs have voluntarily been put in place by companies. These flagship programs can serve as benchmarks for community-corporate-government partnerships in the future. Here, we present examples of such positive phenomena and also focus attention on a myriad of challenges that still lie ahead.

  5. PDF constraints and extraction of the strong coupling constant from the inclusive jet cross section at 7 TeV

    CERN Document Server

    CMS Collaboration

    2013-01-01

    The recent CMS measurement of the inclusive jet cross section at 7~TeV extends the accessible phase space in jet transverse momentum up to 2 TeV and ranges up to 2.5 in absolute jet rapidity. At the same time the experimental uncertainties are smaller than in previous publications such that these data constrain the parton distribution functions of the proton, notably for the gluon at high fractions of the proton momentum, and provide valuable input to determine the strong coupling at high momentum scales. The impact on the extraction of the parton distribution functions is investigated. Using predictions from theory at next-to-leading order, complemented with electroweak corrections, the strong coupling constant is determined from the inclusive jet cross section to be $\\alpha_S(M_Z) = 0.1185 \\pm 0.0019\\,\\mathrm{(exp.)} \\pm 0.0028\\,\\mathrm{(\\mathrm{PDF})} \\pm 0.0004\\,\\mathrm{(\\mathrm{NP})} ^{+0.0055}_{-0.0022}\\,\\mathrm{(\\mathrm{scale})}$, which is in agreement with the world average.

  6. Ultrasonic decontamination robot

    International Nuclear Information System (INIS)

    Patenaude, R.S.

    1984-01-01

    An ultrasonic decontamination robot removes radioactive contamination from the internal surface of the inlet and outlet headers, divider plate, tube sheet, and lower portions of tubes of a nuclear power plant steam generator. A programmable microprocessor controller guides the movement of a robotic arm mounted in the header manway. An ultrasonic transducer having a solvent delivery subsystem through which ultrasonic action is achieved is moved by the arm over the surfaces. A solvent recovery suction tube is positioned within the header to remove solvent therefrom while avoiding interference with the main robotic arm. The solvent composition, temperature, pressure, viscosity, and purity are controlled to optimize the ultrasonic scrubbing action. The ultrasonic transducer is controlled at a power density, frequency, and on-off mode cycle such as to optimize scrubbing action within the range of transducer-to-surface distance and solvent layer thickness selected for the particular conditions encountered. Both solvent and transducer control actions are optimized by the programmable microprocessor. (author)

  7. [Determination of short chain chlorinated paraffins in leather products by solid phase extraction coupled with gas chromatography-mass spectrometry].

    Science.gov (United States)

    Zhang, Weiya; Wan, Xin; Li, Lixia; Wang, Chengyun; Jin, Shupei; Xing, Jun

    2014-10-01

    The short chain chlorinated paraffins (SCCPs) are the additives frequently used in the leather production in China, but they have been put into the list of forbidden chemicals issued by European Union recently. In fact, there is not a commonly recognized method for the determination of the SCCPs in the leather products due to the serious matrix interferences from the leather products and the complex chemical structures of the SCCPs. A method of solid phase extraction coupled with gas chromatography-mass spectrometry (SPE-GC-MS) was established for the determination of the SCCPs in the leather products after the optimization of the SPE conditions. It was found that the interferences from the leather products were thor- oughly separated from the analyte of the SCCPs on a home-made solid phase extraction (SPE) column filled with silica packing while eluted with a mixed solvent of n-hexane-methylene chloride (2:1, v/v). With this method, the recoveries for the SCCPs spiked in the real leather samples varied from 90.47% to 99.00% with the relative standard deviations (RSDs) less than 6.7%, and the limits of detection (LODs) were between 0.069 and 0.110 mg/kg. This method is suitable for qualitative and quantitative analysis of SCCPs in the leather products.

  8. Determination of semicarbazide in fish by molecularly imprinted stir bar sorptive extraction coupled with high performance liquid chromatography.

    Science.gov (United States)

    Tang, Tang; Wei, Fangdi; Wang, Xu; Ma, Yujie; Song, Yueyue; Ma, Yunsu; Song, Quan; Xu, Guanhong; Cen, Yao; Hu, Qin

    2018-02-15

    A novel molecularly imprinted stir bar (MI-SB) for sorptive extraction of semicarbazide (SEM) was prepared in present paper. The coating of the stir bar was characterized by scanning electron microscopy, Fourier-transform infrared spectroscopy, dynamic adsorption and static adsorption tests. The saturated adsorption of MI-SB was about 4 times over that of non-imprinted stir bar (NI-SB). The selectivity of MI-SB for SEM was much better than NI-SB. A method to determine SEM was established by coupling MI-SB sorptive extraction with HPLC-UV. The liner range was 1-100ng/mL for SEM with a correlation coefficient of 0.9985. The limit of detection was about 0.59ng/mL, which was below the minimum required performance limit of SEM in meat products regulated by European Union. The method was applied to the determination of SEM in fish samples with satisfactory results. Copyright © 2018 Elsevier B.V. All rights reserved.

  9. Fundamental studies of the plasma extraction and ion beam formation processes in inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Niu, Hongsen.

    1995-01-01

    The fundamental and practical aspects are described for extracting ions from atmospheric pressure plasma sources into an analytical mass spectrometer. Methodologies and basic concepts of inductively coupled plasma mass spectrometry (ICP-MS) are emphasized in the discussion, including ion source, sampling interface, supersonic expansion, slumming process, ion optics and beam focusing, and vacuum considerations. Some new developments and innovative designs are introduced. The plasma extraction process in ICP-MS was investigated by Langmuir measurements in the region between the skimmer and first ion lens. Electron temperature (T e ) is in the range 2000--11000 K and changes with probe position inside an aerosol gas flow. Electron density (n e ) is in the range 10 8 --10 10 -cm at the skimmer tip and drops abruptly to 10 6 --10 8 cm -3 near the skimmer tip and drops abruptly to 10 6 --10 8 cm -3 downstream further behind the skimmer. Electron density in the beam leaving the skimmer also depends on water loading and on the presence and mass of matrix elements. Axially resolved distributions of electron number-density and electron temperature were obtained to characterize the ion beam at a variety of plasma operating conditions. The electron density dropped by a factor of 101 along the centerline between the sampler and skimmer cones in the first stage and continued to drop by factors of 10 4 --10 5 downstream of skimmer to the entrance of ion lens. The electron density in the beam expansion behind sampler cone exhibited a 1/z 2 intensity fall-off (z is the axial position). An second beam expansion originated from the skimmer entrance, and the beam flow underwent with another 1/z 2 fall-off behind the skimmer. Skimmer interactions play an important role in plasma extraction in the ICP-MS instrument

  10. Degradation of amaranth dye in alkaline medium by ultrasonic cavitation coupled with electrochemical oxidation using a boron-doped diamond anode

    International Nuclear Information System (INIS)

    Barros, Willyam R.P.; Steter, Juliana R.; Lanza, Marcos R.V.; Motheo, Artur J.

    2014-01-01

    Amaranth dye is used widely in the processing of paper, textiles, foods, cosmetics, beverages and medicines, and effluents contaminated with this compound are discharged daily into the environment. Recent studies have shown that azo dyes, especially those such as amaranth dye that have been classified as endocrine disruptors, may cause adverse effects to animal and human health. This paper describes the application of electrochemical oxidation (with a boron-doped diamond BDD thin-film anode) coupled with ultrasound sonolysis (20 kHz and 523 W cm −2 ) to the removal of amaranth dye from dilute alkaline solution. The electrochemical and sonoelectrochemical processes (ECh and SECh, respectively) were carried out at constant current density (10 to 50 mA cm −2 ) in a single compartment cylindrical cell. Sonolysis was virtually less useful for the decolorization and degradation of amaranth dye, whilst ECh and SECh were more effective in degrading the dye with almost complete removal (90 - 95%) attained after 90 min of experiment at an applied current density of 50 mA cm −2 . Degradation of the dye followed pseudo first-order kinetics in both processes, but the rate of reaction was faster with the SECh treatment confirming a synergistic effect between the cavitation process and the electrochemical system. Additionally, at low applied current densities (10 and 25 mA cm −2 ), SECh was considerably more effective than ECh for the amaranth dye mineralization. Although at 35 and 50 mA cm −2 , the two processes showed the respective removal of total organic carbon values: (i) 85% for the ECh and 90% for the SECh at 35 mA cm −2 ; (ii) 96% for the ECh and 98% for the SECh at 50 mA cm −2 . It is concluded that SECh presented the most favorable results for the decontamination of wastewaters containing azo dye compounds

  11. Bead Injection Extraction Chromatography using High-capacity Lab-on-Valve as a Front End to Inductively Coupled Plasma Mass Spectrometry for Rapid Urine Radiobioassay

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per

    2013-01-01

    A novel bead injection (BI) extraction chromatographic microflow system exploiting high-capacity lab-on-valve (LOV) platform coupled with inductively coupled plasma mass spectrometric detection is developed for rapid and automated determination of plutonium in human urine. A microconduit (1 m......L) incorporated within the LOV processing unit is loaded on-line with a metered amount of disposable extraction chromatographic resin (up to 330 mg of TEVA) through programmable beads transport. Selective capture and purification of plutonium onto the resin beads is then performed by pressure driven flow after...

  12. Multi-contaminant analysis of organophosphate and halogenated flame retardants in food matrices using ultrasonication and vacuum assisted extraction, multi-stage cleanup and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Xu, Fuchao; García-Bermejo, Ángel; Malarvannan, Govindan; Gómara, Belén; Neels, Hugo; Covaci, Adrian

    2015-07-03

    A multi-residue analytical method was developed for the determination of a range of flame retardants (FRs), including polybrominated diphenyl ethers (PBDEs), emerging halogenated FRs (EFRs) and organophosphate FRs (PFRs), in food matrices. An ultrasonication and vacuum assisted extraction (UVAE), followed by a multi-stage clean-up procedure, enabled the removal of up to 1g of lipid from 2.5 g of freeze-dried food samples and significantly reduce matrix effects. UVAE achieves a waste factor (WF) of about 10%, while the WFs of classical QuEChERS methods range usually between 50 and 90%. The low WF of UVAE leads to a dramatic improvement in the sensitivity along with saving up to 90% of spiking (internal) standards. Moreover, a two-stage clean-up on Florisil and aminopropyl silica was introduced after UVAE, for an efficient removal of pigments and residual lipids, which led to cleaner extracts than normally achieved by dispersive solid phase extraction (d-SPE). In this way, the extracts could be concentrated to low volumes, e.g. analysis of PFRs was performed on GC-EI-MS, while PBDEs and EFRs were measured by GC-ECNI-MS. Validation tests were performed with three food matrices (lean beef, whole chicken egg and salmon filet), obtaining acceptable recoveries (66-135%) with good repeatability (RSD 1-24%, mean 7%). Method LOQs ranged between 0.008 and 0.04 ng/g dw for PBDEs, between 0.08 and 0.20 ng/g dw for EFRs, and between 1.4 and 3.6 ng/g dw for PFRs. The method was further applied to eight types of food samples (including meat, eggs, fish, and seafood) with lipid contents ranging from 0.1 to 22%. Various FRs were detected above MLOQ levels, demonstrating the wide-range applicability of our method. To the best of our knowledge, this is the first method reported for simultaneous analysis of brominated and organophosphate FRs in food matrices. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. [Determination of fatty acid esters of chloropropanediols in diet samples by gas chromatography-mass spectrometry coupled with solid-supported liquid-liquid extraction].

    Science.gov (United States)

    Gao, Jie; Liu, Qing; Han, Feng; Miao, Hong; Zhao, Yunfeng; Wu, Yongning

    2014-05-01

    To establish a method for the determination of fatty acid esters of 3-monochloropropane-1, 2-diol (3-MCPD) and 2-monochloropropane-1, 3-diol (2-MCPD) in diet samples by gas chromatography-mass spectrometry (GC-MS) with solid-supported liquid-liquid extraction (SLE). Diet samples were ultrasonically extracted by hexane, followed by ester cleavage reaction with sodium methylate in methanol, and then purified by solid-supported liquid-liquid extraction. (SLE) using diatomaceous earth as the sorbent. After derivatization with heptafluorobutyrylimidazole, the analytes were detected by GC-MS and quantified by the deuterated internal standards. The limits of detection (LODs) of 3-MCPD esters and 2-MCPD esters in different diet samples were 0.002 - 0.005 mg/kg and 0.002 - 0.006 mg/kg. The average recoveries of 3-MCPD esters and 2-MCPD esters at the spiking levels of 0.05 and 0.1 mg/kg in the diet samples were in the range of 65.9% - 104.2% and 75.4% - 118.0%, respectively, with the relative standard deviations in the range of 2.2% - 14.2% and 0.8% - .13.9%. The method is simple, accurate and rugged for the determination of fatty acid esters of 3-MCPD and 2-MCPD in diet samples.

  14. Development of a magnetic solid-phase extraction coupled with high-performance liquid chromatography method for the analysis of polyaromatic hydrocarbons.

    Science.gov (United States)

    Ma, Yan; Xie, Jiawen; Jin, Jing; Wang, Wei; Yao, Zhijian; Zhou, Qing; Li, Aimin; Liang, Ying

    2015-07-01

    A novel magnetic solid phase extraction coupled with high-performance liquid chromatography method was established to analyze polyaromatic hydrocarbons in environmental water samples. The extraction conditions, including the amount of extraction agent, extraction time, pH and the surface structure of the magnetic extraction agent, were optimized. The results showed that the amount of extraction agent and extraction time significantly influenced the extraction performance. The increase in the specific surface area, the enlargement of pore size, and the reduction of particle size could enhance the extraction performance of the magnetic microsphere. The optimized magnetic extraction agent possessed a high surface area of 1311 m(2) /g, a large pore size of 6-9 nm, and a small particle size of 6-9 μm. The limit of detection for phenanthrene and benzo[g,h,i]perylene in the developed analysis method was 3.2 and 10.5 ng/L, respectively. When applied to river water samples, the spiked recovery of phenanthrene and benzo[g,h,i]perylene ranged from 89.5-98.6% and 82.9-89.1%, respectively. Phenanthrene was detected over a concentration range of 89-117 ng/L in three water samples withdrawn from the midstream of the Huai River, and benzo[g,h,i]perylene was below the detection limit. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Ultrasonic colour Doppler imaging

    DEFF Research Database (Denmark)

    Evans, David H; Jensen, Jørgen Arendt; Nielsen, Michael Bachmann

    2011-01-01

    Ultrasonic colour Doppler is an imaging technique that combines anatomical information derived using ultrasonic pulse-echo techniques with velocity information derived using ultrasonic Doppler techniques to generate colour-coded maps of tissue velocity superimposed on grey-scale images of tissue...... anatomy. The most common use of the technique is to image the movement of blood through the heart, arteries and veins, but it may also be used to image the motion of solid tissues such as the heart walls. Colour Doppler imaging is now provided on almost all commercial ultrasound machines, and has been...

  16. Ultrasonic Transducer Peak-to-Peak Optical Measurement

    Directory of Open Access Journals (Sweden)

    Pavel Skarvada

    2012-01-01

    Full Text Available Possible optical setups for measurement of the peak-to-peak value of an ultrasonic transducer are described in this work. The Michelson interferometer with the calibrated nanopositioner in reference path and laser Doppler vibrometer were used for the basic measurement of vibration displacement. Langevin type of ultrasonic transducer is used for the purposes of Electro-Ultrasonic Nonlinear Spectroscopy (EUNS. Parameters of produced mechanical vibration have to been well known for EUNS. Moreover, a monitoring of mechanical vibration frequency shift with a mass load and sample-transducer coupling is important for EUNS measurement.

  17. Rapid determination of the volatile components in tobacco by ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Yang, Yanqin; Chu, Guohai; Zhou, Guojun; Jiang, Jian; Yuan, Kailong; Pan, Yuanjiang; Song, Zhiyu; Li, Zuguang; Xia, Qian; Lu, Xinbo; Xiao, Weiqiang

    2016-03-01

    An ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction was first employed to determine the volatile components in tobacco samples. The method combined the advantages of ultrasound, microwave, and headspace solid-phase microextraction. The extraction, separation, and enrichment were performed in a single step, which could greatly simplify the operation and reduce the whole pretreatment time. In the developed method, several experimental parameters, such as fiber type, ultrasound power, and irradiation time, were optimized to improve sampling efficiency. Under the optimal conditions, there were 37, 36, 34, and 36 components identified in tobacco from Guizhou, Hunan, Yunnan, and Zimbabwe, respectively, including esters, heterocycles, alkanes, ketones, terpenoids, acids, phenols, and alcohols. The compound types were roughly the same while the contents were varied from different origins due to the disparity of their growing conditions, such as soil, water, and climate. In addition, the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method was compared with the microwave-assisted extraction coupled to headspace solid-phase microextraction and headspace solid-phase microextraction methods. More types of volatile components were obtained by using the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method, moreover, the contents were high. The results indicated that the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction technique was a simple, time-saving and highly efficient approach, which was especially suitable for analysis of the volatile components in tobacco. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Development and characterization of a small electromembrane extraction probe coupled with mass spectrometry for real-time and online monitoring of in vitro drug metabolism

    DEFF Research Database (Denmark)

    Dugstad, Helene Bonkerud; Petersen, Nickolaj J.; Jensen, Henrik

    2014-01-01

    A small and very simple electromembrane extraction probe (EME-probe) was developed and coupled directly to electrospray ionization mass spectrometry (ESI-MS), and this system was used to monitor in real time in vitro metabolism by rat liver microsomes of drug substances from a small reaction...... (soft extraction). Soft extraction was mandatory in order not to affect the reaction kinetics by sample composition changes induced by the EME-probe. The EME-probe/MS-system was used to establish kinetic profiles for the in vitro metabolism of promethazine, amitriptyline and imipramine as model...

  19. Future Oil Spills and Possibilities for Intervention: A Model for the Coupled Human-Environmental Resource Extraction System

    Science.gov (United States)

    Shughrue, C. M.; Werner, B.; Nugnug, P. T.

    2010-12-01

    The catastrophic Deepwater Horizon oil spill highlights the risks for widespread environmental damage resulting from petroleum resource extraction. Possibilities for amelioration of these risks depend critically on understanding the dynamics and nonlinear interactions between various components of the coupled human-environmental resource extraction system. We use a complexity analysis to identify the levels of description and time scales at which these interactions are strongest, and then use the analysis as the basis for an agent-based numerical model with which decadal trends can be analyzed. Oil industry economic and technological activity and associated oil spills are components of a complex system that is coupled to natural environment, legislation, regulation, media, and resistance systems over annual to decadal time scales. In the model, oil spills are produced stochastically with a range of magnitudes depending on a reliability-engineering-based assessment of failure for the technology employed, human factors including compliance with operating procedures, and risks associated with the drilling environment. Oil industry agents determine drilling location and technological investment using a cost-benefit analysis relating projected revenue from added production to technology cost and government regulation. Media outlet agents reporting on the oil industry and environmental damage from oil spills assess the impacts of aggressively covering a story on circulation increases, advertiser concerns and potential loss of information sources. Environmental advocacy group agents increase public awareness of environmental damage (through media and public contact), solicit memberships and donations, and apply direct pressure on legislators for policy change. Heterogeneous general public agents adjust their desire for change in the level of regulation, contact their representatives or participate in resistance via protest by considering media sources, personal

  20. MEASUREMENT OF PYRETHROID RESIDUES IN ENVIRONMENTAL AND FOOD SAMPLES BY ENHANCED SOLVENT EXTRACTION/SUPERCRITICAL FLUID EXTRACTION COUPLED WITH GAS CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY

    Science.gov (United States)

    The abstract summarizes pyrethorid methods development research. It provides a summary of sample preparation and analytical techniques such as supercritical fluid extraction, enhance solvent extraction, gas chromatography and tandem mass spectrometry.

  1. Sensitivity enhancement in direct coupling of supported liquid membrane extractions to capillary electrophoresis by means of transient isotachophoresis and large electrokinetic injections

    Czech Academy of Sciences Publication Activity Database

    Pantůčková, Pavla; Kubáň, Pavel; Boček, Petr

    2015-01-01

    Roč. 1389, APR (2015), s. 1-7 ISSN 0021-9673 R&D Projects: GA ČR(CZ) GA13-05762S Institutional support: RVO:68081715 Keywords : capillary electrophoresis * in-line coupling * supported liquid membrane extraction Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.926, year: 2015

  2. Determination of {sup 236}U in environmental samples by single extraction chromatography coupled to triple-quadrupole inductively coupled plasma-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Guosheng [Department of Radiation Chemistry, Institute of Radiation Emergency Medicine, Hirosaki University, 66-1 Hon-cho, Hirosaki, Aomori, 036-8564 (Japan); Division of Nuclear Technology and Applications, Institute of High Energy Physics, Chinese Academy of Sciences (China); Beijing Engineering Research Center of Radiographic Techniques and Equipment, Beijing, 100049 (China); Tazoe, Hirofumi [Department of Radiation Chemistry, Institute of Radiation Emergency Medicine, Hirosaki University, 66-1 Hon-cho, Hirosaki, Aomori, 036-8564 (Japan); Yamada, Masatoshi, E-mail: myamada@hirosaki-u.ac.jp [Department of Radiation Chemistry, Institute of Radiation Emergency Medicine, Hirosaki University, 66-1 Hon-cho, Hirosaki, Aomori, 036-8564 (Japan)

    2016-11-09

    In order to measure trace {sup 236}U and {sup 236}U/{sup 238}U in environmental samples with a high matrix effect, a novel and simple method was developed that makes the digestion and purification procedures compatible with advanced triple-quadrupole inductively coupled plasma-mass spectrometry. A total dissolution of sample with HF + HNO{sub 3} + HClO{sub 4} was followed by chromatographic separation with a single resin column containing normal type DGA resin (N,N,N′,N’-tetra-n-octyldiglycolamide) as the extractant system. The analytical accuracy and precision of {sup 236}U/{sup 238}U ratios, measured as {sup 236}U{sup 16}O{sup +}/{sup 238}U{sup 16}O{sup +}, were examined by using the reference materials IAEA-135, IAEA-385, IAEA-447, and JSAC 0471. The low method detection limit (3.50 × 10{sup −6} Bq kg{sup −1}) makes it possible to perform routine monitoring of environmental {sup 236}U due to global fallout combined with the Fukushima Daiichi Nuclear Power Plant accident fallout (>10{sup −5} Bq kg{sup −1}). Finally, the developed method was successfully applied to measure {sup 236}U/{sup 238}U ratios and {sup 236}U activities in soil samples contaminated by the accident. The low {sup 236}U/{sup 238}U atom ratios ((1.50–13.5) × 10{sup −8}) and {sup 236}U activities ((2.25–14.1) × 10{sup −2} mBq kg{sup −1}) indicate {sup 236}U contamination was mainly derived from global fallout in the examined samples. - Highlights: • A simple {sup 236}U/{sup 238}U analytical method has been developed. • The separation required just one DGA column chromatography. • {sup 236}U/{sup 238}U atom ratios in soil were measured by ICP-MS/MS. • {sup 236}U/{sup 238}U atom ratios of (1.50–13.5) × 10{sup −8} were observed in Japanese samples. • {sup 236}U activities of (2.25–14.1) × 10{sup −2} mBq kg{sup −1} were found in Japanese samples.

  3. Ultrasonic testing X gammagraphy

    International Nuclear Information System (INIS)

    Mello Campos, A.M. de

    1989-01-01

    The experience of 10 years for substituting gammagraphy tests by ultrasonic tests is related. A comparative evaluation of data obtained from both techniques applied to welded butt joints is presented. (author)

  4. Ultrasonic grinding method

    International Nuclear Information System (INIS)

    Miyahara, Shuji.

    1990-01-01

    An ultrasonic generator and a liquid supply nozzle are opposed to an object to be ground and a pump is started in this state to supply an organic solvent. Matters to be decontaminated which adheres to the surface of the object to be ground and are difficult to be removed by a mere mechanical removing method can be eliminated previously by the surface active effect of the organic solvent such as ethanol prior to the oscillation of the ultrasonic generator. Subsequently, when the ultrasonic generator is oscillated, scales in the floated state can be removed simply. Further, since the organic solvent can penetrate to provide the surface active effect even in such a narrow portion that the top end of the ultrasonic generator is difficult to the intruded at the surface of the object to be ground, the decontaminating treatment can be applied also to such a narrow portion. (T.M.)

  5. Sequential cloud point extraction for the speciation of mercury in seafood by inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Li Yingjie [Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu Bin [Department of Chemistry, Wuhan University, Wuhan 430072 (China)], E-mail: binhu@whu.edu.cn

    2007-10-15

    A novel nonchromatographic speciation technique for the speciation of mercury by sequential cloud point extraction (CPE) combined with inductively coupled plasma optical emission spectrometry (ICP-OES) was developed. The method based on Hg{sup 2+} was complexed with I{sup -} to form HgI{sub 4}{sup 2-}, and the HgI{sub 4}{sup 2-} reacted with the methyl green (MG) cation to form hydrophobic ion-associated complex, and the ion-associated complex was then extracted into the surfactant-rich phase of the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114), which are subsequently separated from methylmercury (MeHg{sup +}) in the initial solution by centrifugation. The surfactant-rich phase containing Hg(II) was diluted with 0.5 mol L{sup -1} HNO{sub 3} for ICP-OES determination. The supernatant is also subjected to the similar CPE procedure for the preconcentration of MeHg{sup +} by the addition of a chelating agent, ammonium pyrrolidine dithiocarbamate (APDC), in order to form water-insolvable complex with MeHg{sup +}. The MeHg{sup +} in the micelles was directly analyzed after disposal as describe above. Under the optimized conditions, the extraction efficiency was 93.5% for Hg(II) and 51.5% for MeHg{sup +} with the enrichment factor of 18.7 for Hg(II) and 10.3 for MeHg{sup +}, respectively. The limits of detection (LODs) were 56.3 ng L{sup -1} for Hg(II) and 94.6 ng L{sup -1} for MeHg{sup +} (as Hg) with the relative standard deviations (RSDs) of 3.6% for Hg(II) and 4.5% for MeHg{sup +} (C = 10 {mu}g L{sup -1}, n = 7), respectively. The developed technique was applied to the speciation of mercury in real seafood samples and the recoveries for spiked samples were found to be in the range of 93.2-108.7%. For validation, a certified reference material of DORM-2 (dogfish muscle) was analyzed and the determined values are in good agreement with the certified values.

  6. Sequential cloud point extraction for the speciation of mercury in seafood by inductively coupled plasma optical emission spectrometry

    International Nuclear Information System (INIS)

    Li Yingjie; Hu Bin

    2007-01-01

    A novel nonchromatographic speciation technique for the speciation of mercury by sequential cloud point extraction (CPE) combined with inductively coupled plasma optical emission spectrometry (ICP-OES) was developed. The method based on Hg 2+ was complexed with I - to form HgI 4 2- , and the HgI 4 2- reacted with the methyl green (MG) cation to form hydrophobic ion-associated complex, and the ion-associated complex was then extracted into the surfactant-rich phase of the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114), which are subsequently separated from methylmercury (MeHg + ) in the initial solution by centrifugation. The surfactant-rich phase containing Hg(II) was diluted with 0.5 mol L -1 HNO 3 for ICP-OES determination. The supernatant is also subjected to the similar CPE procedure for the preconcentration of MeHg + by the addition of a chelating agent, ammonium pyrrolidine dithiocarbamate (APDC), in order to form water-insolvable complex with MeHg + . The MeHg + in the micelles was directly analyzed after disposal as describe above. Under the optimized conditions, the extraction efficiency was 93.5% for Hg(II) and 51.5% for MeHg + with the enrichment factor of 18.7 for Hg(II) and 10.3 for MeHg + , respectively. The limits of detection (LODs) were 56.3 ng L -1 for Hg(II) and 94.6 ng L -1 for MeHg + (as Hg) with the relative standard deviations (RSDs) of 3.6% for Hg(II) and 4.5% for MeHg + (C = 10 μg L -1 , n = 7), respectively. The developed technique was applied to the speciation of mercury in real seafood samples and the recoveries for spiked samples were found to be in the range of 93.2-108.7%. For validation, a certified reference material of DORM-2 (dogfish muscle) was analyzed and the determined values are in good agreement with the certified values

  7. Fundamentals of Medical Ultrasonics

    CERN Document Server

    Postema, Michiel

    2011-01-01

    This book sets out the physical and engineering principles of acoustics and ultrasound as used for medical applications. It covers the basics of linear acoustics, wave propagation, non-linear acoustics, acoustic properties of tissue, transducer components, and ultrasonic imaging modes, as well as the most common diagnostic and therapeutic applications. It offers students and professionals in medical physics and engineering a detailed overview of the technical aspects of medical ultrasonic imaging, whilst serving as a reference for clinical and research staff.

  8. Assessing ultrasonic examination results

    International Nuclear Information System (INIS)

    Deutsch, V.; Vogt, M.

    1977-01-01

    Amongst nondestructive examination methods, the ultrasonic examination plays an important role. The reason why its scope of application is so wide is because the sound conducting capacity is the only property the material of a test specimen has to have. As the fields are so manifold, only main aspects can be described briefly. The list of references, however, is very extensive and gives plenty of information of all the problems concerning the assessment of ultrasonic examination results. (orig./RW) [de

  9. Solid-Phase Extraction Coupled to a Paper-Based Technique for Trace Copper Detection in Drinking Water.

    Science.gov (United States)

    Quinn, Casey W; Cate, David M; Miller-Lionberg, Daniel D; Reilly, Thomas; Volckens, John; Henry, Charles S

    2018-03-20

    Metal contamination of natural and drinking water systems poses hazards to public and environmental health. Quantifying metal concentrations in water typically requires sample collection in the field followed by expensive laboratory analysis that can take days to weeks to obtain results. The objective of this work was to develop a low-cost, field-deployable method to quantify trace levels of copper in drinking water by coupling solid-phase extraction/preconcentration with a microfluidic paper-based analytical device. This method has the advantages of being hand-powered (instrument-free) and using a simple "read by eye" quantification motif (based on color distance). Tap water samples collected across Fort Collins, CO, were tested with this method and validated against ICP-MS. We demonstrate the ability to quantify the copper content of tap water within 30% of a reference technique at levels ranging from 20 to 500 000 ppb. The application of this technology, which should be sufficient as a rapid screening tool, can lead to faster, more cost-effective detection of soluble metals in water systems.

  10. Algorithms exploiting ultrasonic sensors for subject classification

    Science.gov (United States)

    Desai, Sachi; Quoraishee, Shafik

    2009-09-01

    Proposed here is a series of techniques exploiting micro-Doppler ultrasonic sensors capable of characterizing various detected mammalian targets based on their physiological movements captured a series of robust features. Employed is a combination of unique and conventional digital signal processing techniques arranged in such a manner they become capable of classifying a series of walkers. These processes for feature extraction develops a robust feature space capable of providing discrimination of various movements generated from bipeds and quadrupeds and further subdivided into large or small. These movements can be exploited to provide specific information of a given signature dividing it in a series of subset signatures exploiting wavelets to generate start/stop times. After viewing a series spectrograms of the signature we are able to see distinct differences and utilizing kurtosis, we generate an envelope detector capable of isolating each of the corresponding step cycles generated during a walk. The walk cycle is defined as one complete sequence of walking/running from the foot pushing off the ground and concluding when returning to the ground. This time information segments the events that are readily seen in the spectrogram but obstructed in the temporal domain into individual walk sequences. This walking sequence is then subsequently translated into a three dimensional waterfall plot defining the expected energy value associated with the motion at particular instance of time and frequency. The value is capable of being repeatable for each particular class and employable to discriminate the events. Highly reliable classification is realized exploiting a classifier trained on a candidate sample space derived from the associated gyrations created by motion from actors of interest. The classifier developed herein provides a capability to classify events as an adult humans, children humans, horses, and dogs at potentially high rates based on the tested sample

  11. Ultrasonic viewing device

    International Nuclear Information System (INIS)

    Ito, Juro.

    1979-01-01

    Purpose: To improve the safety of reactor operation by enabling to detect the states and positions of fuel assemblies over a wide range with a set of ultrasonic viewing device comprising a rotatable ultrasonic transmitter-receiver and a reflector mounted with an adjustable angle. Constitution: A driving portion for a ultrasonic viewing device is provided to a rotary plug closing the opening of a reactor vessel and a guide pipe suspending below the coolant level is provided to the driving portion. An ultrasonic transmitter-receiver is provided at the end of the holder tube in the guide pipe. A reflector is provided at the upper position of the reactor core so as to correspond to the ultrasonic transmitter-receiver. The ultrasonic transmitter-receiver, positioned by the driving portion, performs horizontal movement for scanning the entire surface of the top of the reactor core, as well as vertical movement covering the gap between the upper mechanism on the reactor and the reactor core, whereby the confirmation for the separation of the control rod and the detection for the states of the reactor core can be conducted by the reflection waves from the reflector. (Moriyama, K.)

  12. ULTRASONIC ASSEMBLY [REVIEW

    Directory of Open Access Journals (Sweden)

    PORAV Viorica

    2015-05-01

    Full Text Available The paper exposes the possibility of machine producesers to optimize the costs of clothes assembling. Ultrasonic systems being frequently utilized have many advantages on semi products of synthetic textile and technical textile. First of all, sewing – cutting process can be accomplished under high speeds and rate of losses can be minimized. Cutting seal applications are frequently used for underwear and sportswear. Slicing and unit cutting machines, as well as portable sealing machines are available for labeling sector. Products such as bag, pocket and cover can be sewed in a seamless manner for promotion purposes. All objects in terms of accessories are obtained in same standard. Our quilting machines are preferred in worldwide due to its threadless, high quality sealing. An alternative to the classic sewing assembly, with thread and needles is ultrasonic seaming. In ultrasonic welding, there are no connective bolts, nails, soldering materials, or adhesives necessary to bind the materials together. Ultrasonic is defined as acoustic frequencies above the range audible to the human ear. Ultrasonic frequencies are administered to the fabric from the sonotrode of bonding machine. The high frequency and powerful energy produced, when is release in one special environment, the ultrasound heating this environment. The ability to ultrasonic weld textiles and films depend on their thermoplastic contents and the desired end results. The paper defines the weld ability of more common textiles and films. The welding refers to all types of bonding and sealing, as in point bonding of fabric, or continuous sealing of film.

  13. Determination of crack size around rivet hole through neural network using ultrasonic Lamb wave

    International Nuclear Information System (INIS)

    Choi, Sang Woo; Lee, Joon Hyun

    1998-01-01

    Rivets are typical structural features that are potential initiation sites for fatigue crack due to combination of local stress concentration around rivet hole and moisture trapping. For the viewpoint of structural assurance, it is crucial to evaluate the size of crack around rivets by appropriate nondestructive techniques. Guided waves, which direct wave energy along the plate, carry information about the material in their path and offer a potentially more efficient tool for nondestructive inspection of structural material. Neural network that is considered to be the most suitable for pattern recognition and has been used by researchers in NDE field to classify different types of flaws and flaw size. In this study, crack size determination around rivet through a neural network based on the back-propagation algorithm has been done by extracting some feature from time-domain waveforms of ultrasonic Lamb wave for Al 2024-T3 skin panel of aircraft. Special attention was paid to reduce the coupling effect between transducer and specimen by extracting some features related to only time component data in ultrasonic waveform. It was demonstrated clearly that features extraction based on time component data of the time-domain waveform of Lamb wave was very useful to determine crack size initiated from rivet hole through neural network.

  14. Application of Orthogonal Design to Optimize Extraction of ...

    African Journals Online (AJOL)

    Purpose: To optimize the extraction technology of polysaccharides from Cynomorium songaricum Rupr by ultrasonic-assisted extraction (UAE). Methods: Four parameters including ultrasonic power, ratio of raw material to water, extraction temperature, and extraction time were optimized by orthogonal design. The effects of ...

  15. Dynamics of ultrasonic additive manufacturing.

    Science.gov (United States)

    Hehr, Adam; Dapino, Marcelo J

    2017-01-01

    Ultrasonic additive manufacturing (UAM) is a solid-state technology for joining similar and dissimilar metal foils near room temperature by scrubbing them together with ultrasonic vibrations under pressure. Structural dynamics of the welding assembly and work piece influence how energy is transferred during the process and ultimately, part quality. To understand the effect of structural dynamics during UAM, a linear time-invariant model is proposed to relate the inputs of shear force and electric current to resultant welder velocity and voltage. Measured frequency response and operating performance of the welder under no load is used to identify model parameters. Using this model and in-situ measurements, shear force and welder efficiency are estimated to be near 2000N and 80% when welding Al 6061-H18 weld foil, respectively. Shear force and welder efficiency have never been estimated before in UAM. The influence of processing conditions, i.e., welder amplitude, normal force, and weld speed, on shear force and welder efficiency are investigated. Welder velocity was found to strongly influence the shear force magnitude and efficiency while normal force and weld speed showed little to no influence. The proposed model is used to describe high frequency harmonic content in the velocity response of the welder during welding operations and coupling of the UAM build with the welder. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Method and system having ultrasonic sensor movable by translation device for ultrasonic profiling of weld samples

    Science.gov (United States)

    Panyard, James; Potter, Timothy; Charron, William; Hopkins, Deborah; Reverdy, Frederic

    2010-04-06

    A system for ultrasonic profiling of a weld sample includes a carriage movable in opposite first and second directions. An ultrasonic sensor is coupled to the carriage to move over the sample as the carriage moves. An encoder determines the position of the carriage to determine the position of the sensor. A spring is connected at one end of the carriage. Upon the carriage being moved in the first direction toward the spring such that the carriage and the sensor are at a beginning position and the spring is compressed the spring decompresses to push the carriage back along the second direction to move the carriage and the sensor from the beginning position to an ending position. The encoder triggers the sensor to take the ultrasonic measurements of the sample when the sensor is at predetermined positions while the sensor moves over the sample between the beginning and positions.

  17. Ultrasound-Assisted Extraction: Effect of Extraction Time and Solvent ...

    African Journals Online (AJOL)

    Purpose: To investigate the influence of extraction conditions assisted by ultrasound on the quality of extracts obtained from Mesembryanthemum edule shoots. Methods: The extraction procedure was carried out in an ultrasonic bath. The effect of two solvents (methanol and ethanol) and two extraction times (5 and 10 min) ...

  18. Speciation analysis of inorganic arsenic by magnetic solid phase extraction on-line with inductively coupled mass spectrometry determination.

    Science.gov (United States)

    Montoro Leal, P; Vereda Alonso, E; López Guerrero, M M; Cordero, M T Siles; Cano Pavón, J M; García de Torres, A

    2018-07-01

    Arsenic, one of the main environmental pollutants and potent natural poison, is a chemical element that is spread throughout the Earth's crust. It is well known that the toxicity of arsenic is highly dependent on its chemical forms. Generally, the inorganic species are more toxic than its organics forms, and As(III) is 60 times more toxic than As(V). In environmental waters, arsenic exists predominantly in two chemical forms: As(III) and As(V). In view of these facts, fast, sensitive, accurate and simple analytical methods for the speciation of inorganic arsenic in environmental waters are required. In this work, a new magnetic solid phase extraction with a hydride generation system was coupled on line with inductively coupled plasma mass spectrometry (MSPE-HG-ICP-MS). The new system was based on the retention of As(III) and As(V) in two knotted reactors filled with (Fe 3 O 4 ) magnetic nanoparticles functionalized with [1,5-bis (2-pyridyl) 3-sulfophenylmethylene] thiocarbonohydrazide (PSTH-MNPs). As(III) and total inorganic As were sequentially eluted in different reduction conditions. The concentration of As(V) was obtained by subtracting As(III) from total As. The system runs in a fully automated way and the method has proved to have a wide linear range and to be precise, sensitive and fast. The detection limits found were 2.7 and 3.2 ng/L for As(III) and total As, respectively; with relative standard deviations (RSDs) of 2.5% and 2.7% and a sample throughput of 14.4 h -1 . In order to validate the developed method, several certified reference samples of environmental waters including sea water, were analyzed and the determined values were in good agreement with the certified values. The proposed method was successfully applied to the speciation analysis of inorganic arsenic in well-water and sea water. Copyright © 2018 Elsevier B.V. All rights reserved.

  19. Quadrature demodulation based circuit implementation of pulse stream for ultrasonic signal FRI sparse sampling

    International Nuclear Information System (INIS)

    Shoupeng, Song; Zhou, Jiang

    2017-01-01

    Converting ultrasonic signal to ultrasonic pulse stream is the key step of finite rate of innovation (FRI) sparse sampling. At present, ultrasonic pulse-stream-forming techniques are mainly based on digital algorithms. No hardware circuit that can achieve it has been reported. This paper proposes a new quadrature demodulation (QD) based circuit implementation method for forming an ultrasonic pulse stream. Elaborating on FRI sparse sampling theory, the process of ultrasonic signal is explained, followed by a discussion and analysis of ultrasonic pulse-stream-forming methods. In contrast to ultrasonic signal envelope extracting techniques, a quadrature demodulation method (QDM) is proposed. Simulation experiments were performed to determine its performance at various signal-to-noise ratios (SNRs). The circuit was then designed, with mixing module, oscillator, low pass filter (LPF), and root of square sum module. Finally, application experiments were carried out on pipeline sample ultrasonic flaw testing. The experimental results indicate that the QDM can accurately convert ultrasonic signal to ultrasonic pulse stream, and reverse the original signal information, such as pulse width, amplitude, and time of arrival. This technique lays the foundation for ultrasonic signal FRI sparse sampling directly with hardware circuitry. (paper)

  20. A novel ultrasonic clutch using near-field acoustic levitation.

    Science.gov (United States)

    Chang, Kuo-Tsi

    2004-10-01

    This paper investigates design, fabrication and drive of an ultrasonic clutch with two transducers. For the two transducers, one serving as a driving element of the clutch is connected to a driving shaft via a coupling, and the other serving as a slave element of the clutch is connected to a slave shaft via another coupling. The principle of ultrasonic levitation is first expressed. Then, a series-resonant inverter is used to generate AC voltages at input terminals of each transducer, and a speed measuring system with optic sensors is used to find the relationship between rotational speed of the slave shaft and applied voltage of each transducer. Moreover, contact surfaces of the two transducers are coupled by the frictional force when both the two transducers are not energized, and separated using the ultrasonic levitation when at least one of the two transducers is energized at high voltages at resonance.

  1. Construction of a supercritical fluid extraction (SFE equipment: validation using annatto and fennel and extract analysis by thin layer chromatography coupled to image

    Directory of Open Access Journals (Sweden)

    Júlio Cezar Flores JOHNER

    2016-01-01

    Full Text Available Abstract The present work describes setting up a laboratory unit for supercritical fluid extraction. In addition to its construction, a survey of cost was done to compare the cost of the homemade unit with that of commercial units. The equipment was validated using an extraction of annatto seeds’ oil, and the extraction and fractionation of fennel oil were used to validate the two separators; for both systems, the solvent was carbon dioxide. The chemical profiles of annatto and fennel extracts were assessed using thin layer chromatography; the images of the chromatographic plates were processed using the free ImageJ software. The cost survey showed that the homemade equipment has a very low cost (~US$ 16,000 compared to commercial equipment. The extraction curves of annatto were similar to those obtained in the literature (yield of 3.8% oil. The separators were validated, producing both a 2.5% fraction of fennel seed extract rich in essential oils and another extract fraction composed mainly of oleoresins. The ImageJ software proved to be a low-cost tool for obtaining an initial evaluation of the chemical profile of the extracts.

  2. Ultrasonic thermometry for nuclear power plants

    International Nuclear Information System (INIS)

    Saravana Kumar, S.; Arunraj, A.L.R.; Swaminathan, K.

    2013-01-01

    Ultrasonic transducer provides a method of measurement of temperature in industrial tanks and boilers containing different liquids with varied salt content. This method is used to measure the average temperature continuously where other traditional methods available do not offer. Traditional methods used for temperature measurement like infrared thermometers, thermocouples, measures temperature at a single location. Numerous thermocouples are to be fixed at various part of the boiler in order to measure the temperature of the entire boiler, which incurs high cost. Reliability of the system decreases, with increasing number of thermocouples. When they fail at a point, the time incurred in finding the faulty part or faulty thermocouple is high. Ultrasonic transducer provides continuous measurement for all different characteristic liquids with higher accuracy and lesser response time. Fault location and clearance time is also less in ultrasonic measurement method, since only a couple of transducers used for the entire boiler structure. Additionally ultrasonic thermometry along support measuring electronic system can be built of low cost. (author)

  3. Coupled Hydro-Mechanical Simulations of CO2 Storage Supported by Pressure Management Demonstrate Synergy Benefits from Simultaneous Formation Fluid Extraction

    Directory of Open Access Journals (Sweden)

    Kempka Thomas

    2015-04-01

    Full Text Available We assessed the synergetic benefits of simultaneous formation fluid extraction during CO2 injection for reservoir pressure management by coupled hydro-mechanical simulations at the prospective Vedsted storage site located in northern Denmark. Effectiveness of reservoir pressure management was investigated by simulation of CO2 storage without any fluid extraction as well as with 66% and 100% equivalent volume formation fluid extraction from four wells positioned for geothermal heat recovery. Simulation results demonstrate that a total pressure reduction of up to about 1.1 MPa can be achieved at the injection well. Furthermore, the areal pressure perturbation in the storage reservoir can be significantly decreased compared to the simulation scenario without any formation fluid extraction. Following a stress regime analysis, two stress regimes were considered in the coupled hydro-mechanical simulations indicating that the maximum ground surface uplift is about 0.24 m in the absence of any reservoir pressure management. However, a ground uplift mitigation of up to 37.3% (from 0.24 m to 0.15 m can be achieved at the injection well by 100% equivalent volume formation fluid extraction. Well-based adaptation of fluid extraction rates can support achieving zero displacements at the proposed formation fluid extraction wells located close to urban infrastructure. Since shear and tensile failure do not occur under both stress regimes for all investigated scenarios, it is concluded that a safe operation of CO2 injection with simultaneous formation fluid extraction for geothermal heat recovery can be implemented at the Vedsted site.

  4. Ultrasonic dip seal maintenance system

    International Nuclear Information System (INIS)

    Poindexter, A.M.; Ricks, H.E.

    1978-01-01

    Disclosed is a system for removing impurities from the surfaces of liquid dip seals and for wetting the metal surfaces of liquid dip seals in nuclear components. The system comprises an ultrasonic transducer that transmits ultrasonic vibrations along an ultrasonic probe to the metal and liquid surfaces of the dip seal thereby loosening and removing those impurities

  5. Ultrasonic Stir Welding

    Science.gov (United States)

    Nabors, Sammy

    2015-01-01

    NASA Marshall Space Flight Center (MSFC) developed Ultrasonic Stir Welding (USW) to join large pieces of very high-strength metals such as titanium and Inconel. USW, a solid-state weld process, improves current thermal stir welding processes by adding high-power ultrasonic (HPU) energy at 20 kHz frequency. The addition of ultrasonic energy significantly reduces axial, frictional, and shear forces; increases travel rates; and reduces wear on the stir rod, which results in extended stir rod life. The USW process decouples the heating, stirring, and forging elements found in the friction stir welding process allowing for independent control of each process element and, ultimately, greater process control and repeatability. Because of the independent control of USW process elements, closed-loop temperature control can be integrated into the system so that a constant weld nugget temperature can be maintained during welding.

  6. Ultrasonic nondestructive materials characterization

    Science.gov (United States)

    Green, R. E., Jr.

    1986-01-01

    A brief review of ultrasonic wave propagation in solid materials is presented with consideration of the altered behavior in anisotropic and nonlinear elastic materials in comparison with isotropic and linear elastic materials. Some experimental results are described in which ultrasonic velocity and attenuation measurements give insight into materials microstructure and associated mechanical properties. Recent developments with laser beam non-contact generation and detection of ultrasound are presented. The results of several years of experimental measurements using high-power ultrasound are discussed, which provide substantial evidence of the inability of presently accepted theories to fully explain the interaction of ultrasound with solid materials. Finally, a special synchrotron X-ray topographic system is described which affords the possibility of observing direct interaction of ultrasonic waves with the microstructural features of real crystalline solid materials for the first time.

  7. Ultrasonic colour Doppler imaging

    DEFF Research Database (Denmark)

    Evans, David H.; Jensen, Jørgen Arendt; Nielsen, Michael Bachmann

    2011-01-01

    Ultrasonic colour Doppler is an imaging technique that combines anatomical information derived using ultrasonic pulse-echo techniques with velocity information derived using ultrasonic Doppler techniques to generate colour-coded maps of tissue velocity superimposed on grey-scale images of tissue...... anatomy. The most common use of the technique is to image the movement of blood through the heart, arteries and veins, but it may also be used to image the motion of solid tissues such as the heart walls. Colour Doppler imaging is now provided on almost all commercial ultrasound machines, and has been...... vectors. This review briefly introduces the principles behind colour Doppler imaging and describes some clinical applications. It then describes the basic components of conventional colour Doppler systems and the methods used to derive velocity information from the ultrasound signal. Next, a number of new...

  8. Ultrasonic tests. Pt. 2

    International Nuclear Information System (INIS)

    Goebbels, K.

    1980-01-01

    After a basic treatment of ultrasonic wave propagation, of the state-of-the-art methods and the technical background in the preceeding part, advanced ultrasonic NDT techniques are presented here. The discussion of new development includes - manipulation systems, - automation of ultrasonic testing methods, documentation and evaluation. In the middle of this part the main problem areas will be discussed: - detection of defects (e.g. in coarse grained structures and welds), - classification of defects (e.g. discrimination between crack-like and volumetric faults), - sizing of defects. Research in the field of acoustical holography, development of probes and phased arrays, electromagnetic acoustic transducers and signal enhancement are the main contributing parts to the report. (orig./RW)

  9. An improved facile method for extraction and determination of steroidal saponins in Tribulus terrestris by focused microwave-assisted extraction coupled with GC-MS.

    Science.gov (United States)

    Li, Tianlin; Zhang, Zhuomin; Zhang, Lan; Huang, Xinjian; Lin, Junwei; Chen, Guonan

    2009-12-01

    An improved fast method for extraction of steroidal saponins in Tribulus terrestris based on the use of focus microwave-assisted extraction (FMAE) is proposed. Under optimized conditions, four steroidal saponins were extracted from Tribulus terrestris and identified by GC-MS, which are Tigogenin (TG), Gitogenin (GG), Hecogenin (HG) and Neohecogenin (NG). One of the most important steroidal saponins, namely TG was quantified finally. The recovery of TG was in the range of 86.7-91.9% with RSDTribulus terrestris from different areas of occurrence. The difference in chromatographic characteristics of steroidal saponins was proved to be related to the different areas of occurrence. The results showed that FMAE-GC-MS is a simple, rapid, solvent-saving method for the extraction and determination of steroidal saponins in Tribulus terrestris.

  10. Micromachined capacitive ultrasonic immersion transducer array

    Science.gov (United States)

    Jin, Xuecheng

    Capacitive micromachined ultrasonic transducers (cMUTs) have emerged as an attractive alternative to conventional piezoelectric ultrasonic transducers. They offer performance advantages of wide bandwidth and sensitivity that have heretofore been attainable. In addition, micromachining technology, which has benefited from the fast-growing microelectronics industry, enables cMUT array fabrication and electronics integration. This thesis describes the design and fabrication of micromachined capacitive ultrasonic immersion transducer arrays. The basic transducer electrical equivalent circuit is derived from Mason's theory. The effects of Lamb waves and Stoneley waves on cross coupling and acoustic losses are discussed. Electrical parasitics such as series resistance and shunt capacitance are also included in the model of the transducer. Transducer fabrication technology is systematically studied. Device dimension control in both vertical and horizontal directions, process alternatives and variations in membrane formation, via etch and cavity sealing, and metalization as well as their impact on transducer performance are summarized. Both 64 and 128 element 1-D array transducers are fabricated. Transducers are characterized in terms of electrical input impedance, bandwidth, sensitivity, dynamic range, impulse response and angular response, and their performance is compared with theoretical simulation. Various schemes for cross coupling reduction is analyzed, implemented, and verified with both experiments and theory. Preliminary results of immersion imaging are presented using 64 elements 1-D array transducers for active source imaging.

  11. Use of focused ultrasonication in activity-based profiling of deubiquitinating enzymes in tissue.

    Science.gov (United States)

    Nanduri, Bindu; Shack, Leslie A; Rai, Aswathy N; Epperson, William B; Baumgartner, Wes; Schmidt, Ty B; Edelmann, Mariola J

    2016-12-15

    To develop a reproducible tissue lysis method that retains enzyme function for activity-based protein profiling, we compared four different methods to obtain protein extracts from bovine lung tissue: focused ultrasonication, standard sonication, mortar & pestle method, and homogenization combined with standard sonication. Focused ultrasonication and mortar & pestle methods were sufficiently effective for activity-based profiling of deubiquitinases in tissue, and focused ultrasonication also had the fastest processing time. We used focused-ultrasonicator for subsequent activity-based proteomic analysis of deubiquitinases to test the compatibility of this method in sample preparation for activity-based chemical proteomics. Copyright © 2016 Elsevier Inc. All rights reserved.

  12. Effect of ultrasonic waves on the stability of all-trans lutein and its degradation kinetics.

    Science.gov (United States)

    Song, Jiang-Feng; Li, Da-Jing; Pang, Hui-Li; Liu, Chun-Quan

    2015-11-01

    Ultrasound treatment has been widely applied in the extraction of biologically active compounds including carotenoids. However, there are few reports on their effects on the stability of these compounds. In the present study, the stability of all-trans lutein, one of the carotenoids, was investigated under the action of ultrasound. Results showed that ultrasound induced the isomerization of all-trans lutein to its isomers, namely to 13-cis lutein, 13'-cis lutein, 9-cis lutein and 9'-cis lutein as analyzed by HPLC coupled with DAD and LC-MS; and the percentage of the isomerization increased with increasing both ultrasonic frequency and power. The stability of all-trans lutein in dichloromethane was worst among multiple kinds of solvents. Interestingly, the retention rate of all-trans lutein improved as the temperature increased, which runs counter to the Arrhenius law. Under ultrasound irradiation, the degradation mechanism might be different with various temperatures, the degradation of all-trans lutein followed first-order kinetics at 20°C, while second-order kinetics was followed at 30-50°C. As the ultrasonic reaction time prolonged, lutein epoxidation nearly occurred. Those results presented here emphasized that UAE techniques should be carefully used in the extraction of all-trans lutein. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. Accelerated solvent extraction followed by on-line solid-phase extraction coupled to ion trap LC/MS/MS for analysis of benzalkonium chlorides in sediment samples

    Science.gov (United States)

    Ferrer, I.; Furlong, E.T.

    2002-01-01

    Benzalkonium chlorides (BACs) were successfully extracted from sediment samples using a new methodology based on accelerated solvent extraction (ASE) followed by an on-line cleanup step. The BACs were detected by liquid chromatography/ion trap mass spectrometry (LC/MS) or tandem mass spectrometry (MS/MS) using an electrospray interface operated in the positive ion mode. This methodology combines the high efficiency of extraction provided by a pressurized fluid and the high sensitivity offered by the ion trap MS/MS. The effects of solvent type and ASE operational variables, such as temperature and pressure, were evaluated. After optimization, a mixture of acetonitrile/water (6:4 or 7:3) was found to be most efficient for extracting BACs from the sediment samples. Extraction recoveries ranged from 95 to 105% for C12 and C14 homologues, respectively. Total method recoveries from fortified sediment samples, using a cleanup step followed by ASE, were 85% for C12BAC and 79% for C14-BAC. The methodology developed in this work provides detection limits in the subnanogram per gram range. Concentrations of BAC homologues ranged from 22 to 206 ??g/kg in sediment samples from different river sites downstream from wastewater treatment plants. The high affinity of BACs for soil suggests that BACs preferentially concentrate in sediment rather than in water.

  14. Optimization of ultrasonic extraction of mycelial polysaccharides ...

    African Journals Online (AJOL)

    ajl yemi

    2011-11-28

    Nov 28, 2011 ... Research Center for Entomogenous Fungi; BBD, Box-Behnken design; DPPH, 2 ... Dr. Y.L. Guo (Institute of Microbiology, Chinese Academy of. Sciences), is ... experimental design, data analysis, quadratic model building and.

  15. Optimization of ultrasonic extraction of mycelial polysaccharides ...

    African Journals Online (AJOL)

    ajl yemi

    2011-11-28

    Nov 28, 2011 ... air dryer and ground into powder by a muller (A11 basic, ZKA-. WERKE ..... of regression equation were taken and made to be zero. Calculating the .... ia of Dietary Supplements New York: Marcel Dekker. pp. 665-679. Hou XJ ...

  16. Polytetrafluorethylene film-based liquid-three phase micro extraction coupled with differential pulse voltammetry for the determination of atorvastatin calcium.

    Science.gov (United States)

    Ensafi, Ali A; Khoddami, Elaheh; Rezaei, Behzad

    2013-01-01

    In this paper, we describe a new combination method based on polytetrafluorethylene (PTFE) film-based liquid three-phase micro extraction coupled with differential pulse voltammetry (DPV) for the micro extraction and quantification of atorvastatin calcium (ATC) at the ultra-trace level. Different factors affecting the liquid-three phases micro extraction of atorvastatin calcium, including organic solvent, pH of the donor and acceptor phases, concentration of salt, extraction time, stirring rate and electrochemical factors, were investigated, and the optimal extraction conditions were established. The final stable signal was achieved after a 50 min extraction time, which was used for analytical applications. An enrichment factor of 21 was achieved, and the relative standard deviation (RSD) of the method was 4.5% (n = 4). Differential pulse voltammetry exhibited two wide linear dynamic ranges of 20.0-1000.0 pmol L(-1) and 0.001-11.0 µmol L(-1) of ATC. The detection limit was found to be 8.1 pmol L(-1) ATC. Finally, the proposed method was used as a new combination method for the determination of atorvastatin calcium in real samples, such as human urine and plasma.

  17. Critical comparison of the on-line and off-line molecularly imprinted solid-phase extraction of patulin coupled with liquid chromatography.

    Science.gov (United States)

    Lhotská, Ivona; Holznerová, Anežka; Solich, Petr; Šatínský, Dalibor

    2017-12-01

    Reaching trace amounts of mycotoxin contamination requires sensitive and selective analytical tools for their determination. Improving the selectivity of sample pretreatment steps covering new and modern extraction techniques is one way to achieve it. Molecularly imprinted polymers as selective sorbent for extraction undoubtedly meet these criteria. The presented work is focused on the hyphenation of on-line molecularly imprinted solid-phase extraction with a chromatography system using a column-switching approach. Making a critical comparison with a simultaneously developed off-line extraction procedure, evaluation of pros and cons of each method, and determining the reliability of both methods on a real sample analysis were carried out. Both high-performance liquid chromatography methods, using off-line extraction on molecularly imprinted polymer and an on-line column-switching approach, were validated, and the validation results were compared against each other. Although automation leads to significant time savings, fewer human errors, and required no handling of toxic solvents, it reached worse detection limits (15 versus 6 μg/L), worse recovery values (68.3-123.5 versus 81.2-109.9%), and worse efficiency throughout the entire clean-up process in comparison with the off-line extraction method. The difficulties encountered, the compromises made during the optimization of on-line coupling and their critical evaluation are presented in detail. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Ultrasonic Communication Project, Phase 1, FY1999

    Energy Technology Data Exchange (ETDEWEB)

    Haynes, H.D.; Akerman, M.A.; Baylor, V.M.

    2000-06-01

    This Phase 1 project has been successful in identifying, exploring, and demonstrating methods for ultrasonic-based communication with an emphasis on the application of digital signal processing techniques. During the project, at the direction of the agency project monitor, particular attention was directed at sending and receiving ultrasonic data through air and through pipes that would be commonly found in buildings. Efforts were also focused on development of a method for transmitting computer files ultrasonically. New methods were identified and evaluated for ultrasonic communication. These methods are based on a technique called DFS. With DFS, individual alphanumeric characters are broken down into a sequence of bits, and each bit is used to generate a discrete ultrasonic frequency. Characters are then transmitted one-bit-at-a-time, and reconstructed by the receiver. This technique was put into practice through the development of LabVIEW{trademark}VIs. These VIs were integrated with specially developed electronic circuits to provide a system for demonstrating the transmission and reception/reconstruction of typed messages and computer files. Tests were performed to determine the envelope for ultrasound transmission through pipes (with and without water) versus through air. The practical aspects of connections, efficient electronics, impedance matching, and the effect of damping mechanisms were all investigated. These tests resulted in a considerable number of reference charts that illustrate the absorption of ultrasound through different pipe materials, both with and without water, as a function of distance. Ultrasound was found to be least attenuated by copper pipe and most attenuated by PVC pipe. Water in the pipe provides additional damping and attenuation of ultrasonic signals. Dramatic improvements are observed, however, in ultrasound signal strength if the transducers are directly coupled to the water, rather than simply attaching them to the outside of

  19. Urban Heat Island Simulations in Guangzhou, China, Using the Coupled WRF/UCM Model with a Land Use Map Extracted from Remote Sensing Data

    Directory of Open Access Journals (Sweden)

    Guang Chen

    2016-07-01

    Full Text Available The Weather Research and Forecasting (WRF model coupled with an Urban Canopy Model (UCM was used for studying urban environmental issues. Because land use data employed in the WRF model do not agree with the current situation around Guangzhou, China, the performance of WRF/UCM with new land-use data extracted from Remote Sensing (RS data was evaluated in early August 2012. Results from simulations reveal that experiments with the extracted data are capable of reasonable reproductions of the majority of the observed temporal characteristics of the 2-m temperature, and can capture the characteristics of Urban Heat Island (UHI. The “UCM_12” simulation, which employed the extracted land-use data with the WRF/UCM model, provided the best reproduction of the 2-m temperature data evolution and the smallest minimum absolute average error when compared with the other two experiments without coupled UCM. The contributions of various factors to the UHI effect were analyzed by comparing the energy equilibrium processes of “UCM_12” in urban and suburban areas. Analysis revealed that energy equilibrium processes with new land use data can explain the diurnal character of the UHI intensity variation. Furthermore, land use data extracted from RS can be used to simulate the UHI.

  20. Ultrasonic weld testing.

    Science.gov (United States)

    1970-12-01

    The study was broken down into two phases. Phase I consisted of a laboratory investigation of test specimens to determine the reliability of the ultrasonic equipment and testing procedure. Phase II was a field study where the knowledge, skills and ab...

  1. Ultrasonic leak detection

    International Nuclear Information System (INIS)

    Murphy, R.V.

    1977-01-01

    A scanning ultrasonic microphone was used to detect the presence and locate the sources of hydraulic noises in piping systems in a reactor environment. The intensity changes of the noises correspond to changes of flow conditions within the system caused by throttled valves, flow rate changes, and leaks. (author)

  2. Arsenic species determination in human scalp hair by pressurized hot water extraction and high performance liquid chromatography-inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Morado Piñeiro, Andrés; Moreda-Piñeiro, Jorge; Alonso-Rodríguez, Elia; López-Mahía, Purificación; Muniategui-Lorenzo, Soledad; Prada-Rodríguez, Darío

    2013-02-15

    Analytical methods for the determination of total arsenic and arsenic species (mainly As(III) and As(V)) in human scalp hair have been developed. Inductively coupled plasma-mass spectrometry (ICP-MS) and high performance liquid chromatography (HPLC) coupled to ICP-MS have been used for total arsenic and arsenic species determination, respectively. The proposed methods include a "green", fast, high efficient and automated species leaching procedure by pressurized hot water extraction (PHWE). The operating parameters for PHWE including modifier concentration, extraction temperature, static time, extraction steps, pressure, mean particle size, diatomaceous earth (DE) mass/sample mass ratio and flush volume were studied using design of experiments (Plackett-Burman design PBD). Optimum condition implies a modifier concentration (acetic acid) of 150 mM and powdered hair samples fully mixed with diatomaceous earth (DE) as a dispersing agent at a DE mass/sample mass ratio of 5. The extraction has been carried out at 100°C and at an extraction pressure of 1500 psi for 5 min in four extraction step. Under optimised conditions, limits of quantification of 7.0, 6.3 and 50.3 ng g(-1) for total As, As(III) and As(V), respectively were achieved. Repeatability of the overall procedure (4.4, 7.2 and 2.1% for total As, As(III) and As(V), respectively) was achieved. The analysis of GBW-07601 (human hair) certified reference material was used for validation. The optimised method has been finally applied to several human scalp hair samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  3. Identification and quantification of metallothionein isoforms and superoxide dismutase in spiked liver extracts using HPLC-ESI-MS offline coupling and HPLC-ICP-MS online coupling.

    Science.gov (United States)

    Nischwitz, V; Michalke, B; Kettrup, A

    2003-01-01

    A two-dimensional chromatographic method for the characterization of metallothionein isoforms (MT) and superoxide dismutase (SOD) in spiked liver extracts was developed for the optimization of extraction procedures from liver samples. Element-specific detection (ICP-MS) and molecule-specific detection (ESI-MS) were applied for maximum species information. A special focus was laid on the quantitative data evaluation (species stoichiometry, calibration with and without matrix, recovery), which is neglected in most MT/SOD publications with hyphenated techniques. Linearity, precision (residual standard deviation of calibration curves <10%), and detection limits (<0.6 mg L(-1) for MT isoforms and 13 mg L(-1) for SOD) prove the suitability of the method for quantification. An alternative quantification is proposed for the extension towards other lesser or even unknown trace element species, especially the native porcine MT and SOD.

  4. Ultrasonic Bat Deterrent Technology

    Energy Technology Data Exchange (ETDEWEB)

    Kinzie, Kevin; Rominger, Kathryn M.

    2017-12-14

    The project objective was to advance the development and testing of an Near commercial bat-deterrent system with a goal to increase the current GE deterrent system effectiveness to over 50% with broad species applicability. Additionally, the research supported by this program has provided insights into bat behavior and ultrasonic deterrent design that had not previously been explored. Prior research and development had demonstrated the effectiveness of a commercial-grade, air-powered, ultrasonic bat deterrent to be between 30-50% depending upon the species of bat. However, the previous research provided limited insight into the behavioral responses of bats in the presence of ultrasonic deterrent sound fields that could be utilized to improve effectiveness. A unique bat flight room was utilized to observe the behavioral characteristics of bats in the presence of ultrasonic sound fields. Behavioral testing in the bat flight facility demonstrated that ultrasonic sounds similar to those produced by the GE deterrent influenced the activities and behaviors, primarily those associated with foraging, of the species exposed. The study also indicated that continuous and pulsing ultrasonic signals had a similar effect on the bats, and confirmed that as ultrasonic sounds attenuate, their influence on the bats’ activities and behavior decreases. Ground testing at Wolf Ridge Wind, LLC and Shawnee National Forest assessed both continuous and pulsing deterrent signals emitted from the GE deterrent system and further enhanced the behavioral understanding of bats in the presence of the deterrent. With these data and observations, the existing 4-nozzle continuous, or steady, emission ultrasonic system was redesigned to a 6-nozzle system that could emit a pulsing signal covering a larger air space around a turbine. Twelve GE 1.6-100 turbines were outfitted with the deterrent system and a formal three-month field study was performed using daily carcass searches beneath the 12

  5. The Elastic Constants Measurement of Metal Alloy by Using Ultrasonic Nondestructive Method at Different Temperature

    Directory of Open Access Journals (Sweden)

    Eryi Hu

    2016-01-01

    Full Text Available The ultrasonic nondestructive method is introduced into the elastic constants measurement of metal material. The extraction principle of Poisson’s ratio, elastic modulus, and shear modulus is deduced from the ultrasonic propagating equations with two kinds of vibration model of the elastic medium named ultrasonic longitudinal wave and transverse wave, respectively. The ultrasonic propagating velocity is measured by using the digital correlation technique between the ultrasonic original signal and the echo signal from the bottom surface, and then the elastic constants of the metal material are calculated. The feasibility of the correlation algorithm is verified by a simulation procedure. Finally, in order to obtain the stability of the elastic properties of different metal materials in a variable engineering application environment, the elastic constants of two kinds of metal materials in different temperature environment are measured by the proposed ultrasonic method.

  6. Industrial Applications of High Power Ultrasonics

    Science.gov (United States)

    Patist, Alex; Bates, Darren

    Since the change of the millennium, high-power ultrasound has become an alternative food processing technology applicable to large-scale commercial applications such as emulsification, homogenization, extraction, crystallization, dewatering, low-temperature pasteurization, degassing, defoaming, activation and inactivation of enzymes, particle size reduction, extrusion, and viscosity alteration. This new focus can be attributed to significant improvements in equipment design and efficiency during the late 1990 s. Like most innovative food processing technologies, high-power ultrasonics is not an off-the-shelf technology, and thus requires careful development and scale-up for each and every application. The objective of this chapter is to present examples of ultrasonic applications that have been successful at the commercialization stage, advantages, and limitations, as well as key learnings from scaling up an innovative food technology in general.

  7. Non-contact feature detection using ultrasonic Lamb waves

    Science.gov (United States)

    Sinha, Dipen N [Los Alamos, NM

    2011-06-28

    Apparatus and method for non-contact ultrasonic detection of features on or within the walls of hollow pipes are described. An air-coupled, high-power ultrasonic transducer for generating guided waves in the pipe wall, and a high-sensitivity, air-coupled transducer for detecting these waves, are disposed at a distance apart and at chosen angle with respect to the surface of the pipe, either inside of or outside of the pipe. Measurements may be made in reflection or transmission modes depending on the relative position of the transducers and the pipe. Data are taken by sweeping the frequency of the incident ultrasonic waves, using a tracking narrow-band filter to reduce detected noise, and transforming the frequency domain data into the time domain using fast Fourier transformation, if required.

  8. Ultrasonic Histotripsy for Tissue Therapy

    Science.gov (United States)

    Pahk, K. J.; Dhar, D. K.; Malago, M.; Saffari, N.

    2015-01-01

    Hepatocyte transplantation has been considered and investigated as a promising and alternative method to liver transplantation for treating liver-based metabolic disorder in newborns over the past two decades. Although some clinical trials have been conducted and shown clinical benefits and outcomes, it is difficult to deliver and achieve a desired level of integration and transplantation of hepatocytes in the liver parenchyma. To overcome this problem, this work introduces an alternative method to a portal-infused-hepatocyte cell transplantation. To improve the level of engraftment of transplantable hepatocytes, these are injected directly into cavities generated by ultrasonic histotripsy. Histotripsy is an extracorporeal noninvasive technique which has been recently developed using high intensity focused ultrasound (HIFU) for inducing tissue fractionation with no coagulative necrosis. The exact mechanisms for the tissue fractionation are not well understood yet; but the possible mechanisms are thought to be a combination of nonlinear wave propagation effect, explosive bubble growth and ultrasonic atomization. The main objectives of this work are to demonstrate the feasibility of this new cell therapy and evaluate and distinguish between the different types of cavitation activity for either a thermally or a mechanically induced lesion. In the present work, numerical studies on the bubble dynamics (the Gilmore-Akulichev bubble model coupled with the Khokhlov-Zabolotskaya-Kuznetsov equation) and both ex- and in vivo liver experiments are conducted with histological analysis (haematoxylin and eosin stain). The numerical and the experimental results suggest that (a) the acoustic emissions emitted during the thermal ablation and the histotripsy exposure can be distinguished both numerically and experimentally and (b) the proposed cell therapy may potentially form an effective and safe clinical treatment for replacing and correcting disordered hepatocytes, although the

  9. Ultrasonic Histotripsy for Tissue Therapy

    International Nuclear Information System (INIS)

    Pahk, K J; Saffari, N; Dhar, D K; Malago, M

    2015-01-01

    Hepatocyte transplantation has been considered and investigated as a promising and alternative method to liver transplantation for treating liver-based metabolic disorder in newborns over the past two decades. Although some clinical trials have been conducted and shown clinical benefits and outcomes, it is difficult to deliver and achieve a desired level of integration and transplantation of hepatocytes in the liver parenchyma. To overcome this problem, this work introduces an alternative method to a portal-infused-hepatocyte cell transplantation. To improve the level of engraftment of transplantable hepatocytes, these are injected directly into cavities generated by ultrasonic histotripsy. Histotripsy is an extracorporeal noninvasive technique which has been recently developed using high intensity focused ultrasound (HIFU) for inducing tissue fractionation with no coagulative necrosis. The exact mechanisms for the tissue fractionation are not well understood yet; but the possible mechanisms are thought to be a combination of nonlinear wave propagation effect, explosive bubble growth and ultrasonic atomization. The main objectives of this work are to demonstrate the feasibility of this new cell therapy and evaluate and distinguish between the different types of cavitation activity for either a thermally or a mechanically induced lesion. In the present work, numerical studies on the bubble dynamics (the Gilmore-Akulichev bubble model coupled with the Khokhlov-Zabolotskaya-Kuznetsov equation) and both ex- and in vivo liver experiments are conducted with histological analysis (haematoxylin and eosin stain). The numerical and the experimental results suggest that (a) the acoustic emissions emitted during the thermal ablation and the histotripsy exposure can be distinguished both numerically and experimentally and (b) the proposed cell therapy may potentially form an effective and safe clinical treatment for replacing and correcting disordered hepatocytes, although the

  10. Piezoelectric Nanotube Array for Broadband High-Frequency Ultrasonic Transducer.

    Science.gov (United States)

    Liew, Weng Heng; Yao, Kui; Chen, Shuting; Tay, Francis Eng Hock

    2018-03-01

    Piezoelectric materials are vital in determining ultrasonic transducer and imaging performance as they offer the function for conversion between mechanical and electrical energy. Ultrasonic transducers with high-frequency operation suffer from performance degradation and fabrication difficulty of the demanded piezoelectric materials. Hence, we propose 1-D polymeric piezoelectric nanostructure with controlled nanoscale features to overcome the technical limitations of high-frequency ultrasonic transducers. For the first time, we demonstrate the integration of a well-aligned piezoelectric nanotube array to produce a high-frequency ultrasonic transducer with outstanding performance. We find that nanoconfinement-induced polarization orientation and unique nanotube structure lead to significantly improved piezoelectric and ultrasonic transducing performance over the conventional piezoelectric thin film. A large bandwidth, 126% (-6 dB), is achieved at high center frequency, 108 MHz. Transmission sensitivity of nanotube array is found to be 46% higher than that of the monolithic thin film transducer attributed to the improved electromechanical coupling effectiveness and impedance match. We further demonstrate high-resolution scanning, ultrasonic imaging, and photoacoustic imaging using the obtained nanotube array transducers, which is valuable for biomedical imaging applications in the future.

  11. Determination of ketamine and its main metabolites by liquid chromatography coupled to tandem mass spectrometry in pig plasma: Comparison of extraction methods.

    Science.gov (United States)

    Ramiole, Cindy; D'Hayer, Benoit; Boudy, Vincent; Legagneux, Josette; Fonsart, Julien; Houzé, Pascal

    2017-11-30

    A rapid, sensitive and specific liquid chromatography coupled to tandem mass spectrometry method was developed for the simultaneous quantification pig plasma of ketamine and its two principal metabolites, norketamine and dehydronorketamine. Three extraction procoles were assessed including acetonitrile precipitation, Oase™ microplate extraction, and liquid-liquid extraction. Oase™ microplate extraction induced no significant matrix effect, important signal/noise ratio and good recoveries, ranging from 82 to 87% for the considered compounds. Using this extraction procedure, the assay was linear in the dynamic range 10-3000ng/mL (R 2 >0.99) regardless of the analytes. Intra- and inter-day accuracies were less than 12% for all compounds and intra- and inter-day precisions expressed as RSD were within ketamine, norketamine and dehydronorketamine concentrations up to 15,000ng/mL can be determined with good precision using appropriate sample dilution. The assay was successfully applied to pig plasma samples to determine the pharmacokinetics of ketamine and the consecutive metabolites after buccal administration of a 4mg/kg ketamine base solutions. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Online micro-solid-phase extraction based on boronate affinity monolithic column coupled with high-performance liquid chromatography for the determination of monoamine neurotransmitters in human urine.

    Science.gov (United States)

    Yang, Xiaoting; Hu, Yufei; Li, Gongke

    2014-05-16

    Quantification of monoamine neurotransmitters is very important in diagnosing and monitoring of patients with neurological disorders. We developed an online analytical method to selectively determine urinary monoamine neurotransmitters, which coupled the boronate affinity monolithic column micro-solid-phase extraction with high-performance liquid chromatography (HPLC). The boronate affinity monolithic column was prepared by in situ polymerization of vinylphenylboronic acid (VPBA) and N,N'-methylenebisacrylamide (MBAA) in a stainless capillary column. The prepared monolithic column showed good permeability, high extraction selectivity and capacity. The column-to-column reproducibility was satisfactory and the enrichment factors were 17-243 for four monoamine neurotransmitters. Parameters that influence the online extraction efficiency, including pH of sample solution, flow rate of extraction and desorption, extraction volume and desorption volume were investigated. Under the optimized conditions, the developed method exhibited low limit of detection (0.06-0.80μg/L), good linearity (with R(2) between 0.9979 and 0.9993). The recoveries in urine samples were 81.0-105.5% for four monoamine neurotransmitters with intra- and inter-day RSDs of 2.1-8.2% and 3.7-10.6%, respectively. The online analytical method was sensitive, accurate, selective, reliable and applicable to analysis of trace monoamine neurotransmitters in human urine sample. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Determination of Cd, Pb, Zn and Cu in Sediment Compartments by Sequential Extraction and Isotope Dilution Inductively Coupled Plasma Mass Spectrometry (ID-ICP-MS

    Directory of Open Access Journals (Sweden)

    Gardolinski Paulo C. F. C.

    2002-01-01

    Full Text Available Trace concentrations of Cd, Cu, Pb and Zn in four different sediment fractions extracted in sequence were determined by isotope dilution inductively coupled mass spectrometry (IDICPMS. The metals from each fraction were extracted following the sequential extraction procedure recommended by the Bureau Commun de Référence (BCR of the Commission of the European Communities. As an alternative to external calibration, the elements were quantified by spiking the extracted solutions with 112Cd, 63Cu, 208Pb and 66Zn and application of isotope dilution. The proposed approach was applied to a sample collected from a lake and two standard reference materials, NIST2704 river sediment from the National Institute of Standards & Technology and the BCR-277 estuarine sediment. Detection limits, for each extracted solution, varied from 0.31 to 0.53 mug L¹ for Cd, 0.92 to 2.9 mug L¹ for Cu, 0.22 to 1.1 mug L¹ for Pb and 1.3 to 7.6 mug L¹ for Zn. The sum of the metals concentration in the different fractions was compatible with 95% confidence level found amounts obtained with complete digestion of the samples and with the certified values of the standard reference materials.

  14. Syringe needle-based sampling coupled with liquid-phase extraction for determination of the three-dimensional distribution of l-ascorbic acid in apples.

    Science.gov (United States)

    Tang, Sheng; Lee, Hian Kee

    2016-05-15

    A novel syringe needle-based sampling approach coupled with liquid-phase extraction (NBS-LPE) was developed and applied to the extraction of l-ascorbic acid (AsA) in apple. In NBS-LPE, only a small amount of apple flesh (ca. 10mg) was sampled directly using a syringe needle and placed in a glass insert for liquid extraction of AsA by 80 μL oxalic acid-acetic acid. The extract was then directly analyzed by liquid chromatography. This new procedure is simple, convenient, almost organic solvent free, and causes far less damage to the fruit. To demonstrate the applicability of NBS-LPE, AsA levels at different sampling points in a single apple were determined to reveal the spatial distribution of the analyte in a three-dimensional model. The results also showed that this method had good sensitivity (limit of detection of 0.0097 mg/100g; limit of quantification of 0.0323 mg/100g), acceptable reproducibility (relative standard deviation of 5.01% (n=6)), a wide linear range of between 0.05 and 50mg/100g, and good linearity (r(2)=0.9921). This interesting extraction technique and modeling approach can be used to measure and monitor a wide range of compounds in various parts of different soft-matrix fruits and vegetables, including single specimens. Copyright © 2015 Elsevier Ltd. All rights reserved.

  15. A comparison of sorptive extraction techniques coupled to a new quantitative, sensitive, high throughput GC-MS/MS method for methoxypyrazine analysis in wine.

    Science.gov (United States)

    Hjelmeland, Anna K; Wylie, Philip L; Ebeler, Susan E

    2016-02-01

    Methoxypyrazines are volatile compounds found in plants, microbes, and insects that have potent vegetal and earthy aromas. With sensory detection thresholds in the low ng L(-1) range, modest concentrations of these compounds can profoundly impact the aroma quality of foods and beverages, and high levels can lead to consumer rejection. The wine industry routinely analyzes the most prevalent methoxypyrazine, 2-isobutyl-3-methoxypyrazine (IBMP), to aid in harvest decisions, since concentrations decrease during berry ripening. In addition to IBMP, three other methoxypyrazines IPMP (2-isopropyl-3-methoxypyrazine), SBMP (2-sec-butyl-3-methoxypyrazine), and EMP (2-ethyl-3-methoxypyrazine) have been identified in grapes and/or wine and can impact aroma quality. Despite their routine analysis in the wine industry (mostly IBMP), accurate methoxypyrazine quantitation is hindered by two major challenges: sensitivity and resolution. With extremely low sensory detection thresholds (~8-15 ng L(-1) in wine for IBMP), highly sensitive analytical methods to quantify methoxypyrazines at trace levels are necessary. Here we were able to achieve resolution of IBMP as well as IPMP, EMP, and SBMP from co-eluting compounds using one-dimensional chromatography coupled to positive chemical ionization tandem mass spectrometry. Three extraction techniques HS-SPME (headspace-solid phase microextraction), SBSE (stirbar sorptive extraction), and HSSE (headspace sorptive extraction) were validated and compared. A 30 min extraction time was used for HS-SPME and SBSE extraction techniques, while 120 min was necessary to achieve sufficient sensitivity for HSSE extractions. All extraction methods have limits of quantitation (LOQ) at or below 1 ng L(-1) for all four methoxypyrazines analyzed, i.e., LOQ's at or below reported sensory detection limits in wine. The method is high throughput, with resolution of all compounds possible with a relatively rapid 27 min GC oven program. Copyright © 2015

  16. Determination of organophosphorus pesticides by dispersive liquid-liquid micro extraction coupled with gas chromatography-electron capture detection

    International Nuclear Information System (INIS)

    Mohd Marsin Sanagi; Siti Umairah Mokhtar; Mazidatul Akmam Miskam; Wan Aini Wan Ibrahim

    2011-01-01

    A simple, rapid and sensitive method termed as dispersive liquid-liquid micro extraction (DLLME) combined with gas chromatography-electron capture detector (GC-ECD) was developed for the determination of selected organophosphorus pesticides (OPPs) namely chloropyrifos, dimethoate and diazinon in water sample. In this method, a mixture of carbon disulfide, CS 2 (extraction solvent) and methanol (disperser solvent) was rapidly injected using syringe into the 5.00 mL water sample to form a cloudy solution where the OPPs were extracted into the fine droplets of extraction solvent. Upon centrifugation for 3 min at 3500 rpm, the fine droplets were sedimented at the bottom of the centrifuge tube. Sedimented phase (1 μL) was injected into the GC-ECD for separation and determination of OPPs. Important extraction parameters, such as type of disperser solvent, volume of extraction solvent and volume of disperser solvent were investigated. The optimized conditions for DLLME of the selected OPPs were methanol as disperser solvent, 30 μL of extraction solvent (CS 2 ) and 1.0 mL of disperser solvent (methanol). Under the optimum extraction conditions, the method showed good linearity in the range of 0.1 to 1.0 μg/ mL with correlation coefficient (r 2 ), in the range of 0.9976 to 0.9994 and low limits of detection (LOD) between 0.047 and 0.201 μg/ mL. The proposed method provided acceptable recoveries (72.67- 144 %) with good RSDs ranging from 2.74 % to 7.48 %. This method was successfully applied to the determination of OPPs in water samples obtained from a golf course and chloropyrifos and diazinon were detected at concentration 0.18 μg/ mL and 0.07 μg/ mL, respectively. (author)

  17. Coupling continuous ultrasound-assisted extraction, preconcentration and flame atomic absorption spectrometric detection for the determination of cadmium and lead in mussel samples

    International Nuclear Information System (INIS)

    Yebra-Biurrun, M.C.; Cancela-Perez, S.; Moreno-Cid-Barinaga, A.

    2005-01-01

    Continuous ultrasound-assisted extraction has been coupled with preconcentration and flame atomic absorption spectrometry for the determination of cadmium and lead in mussel samples. Experimental designs were used for the optimisation of the leaching and preconcentration steps. The use of diluted nitric acid as extractant in the continuous mode at a flow rate of 3.5 ml min -1 and room temperature was sufficient for quantitative extraction of these trace metals. A minicolumn containing a chelating resin (Chelite P, with aminomethylphosphoric acid groups) was proved as an excellent material for the quantitative preconcentration of cadmium and lead prior to their flame atomic absorption detection. A flow injection manifold was used as interface for coupling the three analytical steps, which allowed the automation of the whole analytical process. A good precision of the whole procedure (2.0 and 2.3%), high enrichment factors (20.5 and 11.8) and a detection limit of 0.011 and 0.25 μg g -1 for cadmium and lead, respectively, were obtained for 80 mg of sample. The sample throughputs were ca. 16 and 14 samples h -1 for cadmium and lead, respectively. The accuracy of the analytical procedures was verified by using a standard reference material (BCR 278-R, mussel tissue) and the results were in good agreement with the certified values. The method was successfully applied to the determination of trace amounts of cadmium and lead in mussel samples from the coast of Galicia (NW, Spain)

  18. Metal-coated semiconductor nanostructures and simulation of photon extraction and coupling to optical fibers for a solid-state single-photon source

    International Nuclear Information System (INIS)

    Suemune, Ikuo; Nakajima, Hideaki; Liu, Xiangming; Odashima, Satoru; Asano, Tomoya; Iijima, Hitoshi; Huh, Jae-Hoon; Idutsu, Yasuhiro; Sasakura, Hirotaka; Kumano, Hidekazu

    2013-01-01

    We have realized metal-coated semiconductor nanostructures for a stable and efficient single-photon source (SPS) and demonstrated improved single-photon extraction efficiency by the selection of metals and nanostructures. We demonstrate with finite-difference time-domain (FDTD) simulations that inclination of a pillar sidewall, which changes the structure to a nanocone, is effective in improving the photon extraction efficiency. We demonstrate how such nanocone structures with inclined sidewalls are fabricated with reactive ion etching. With the optimized design, a photon extraction efficiency to outer airside as high as ∼97% generated from a quantum dot in a nanocone structure is simulated, which is the important step in realizing SPS on-demand operations. We have also examined the direct contact of such a metal-embedded nanocone structure with a single-mode fiber facet as a simple and practical method for preparing fiber-coupled SPS and demonstrated practical coupling efficiencies of ∼16% with FDTD simulation. (paper)

  19. Determination of isoquercitrin in rat plasma by high performance liquid chromatography coupled with a novel synergistic cloud point extraction.

    Science.gov (United States)

    Zhou, Jun; Sun, Jiang Bing; Wang, Qiao Feng

    2018-01-01

    A novel improved preconcentration method known as synergistic cloud point extraction was established for isoquercitrin preconcentration and determination in rat plasma prior to its determination by high performance liquid chromatography. Synergistic cloud point extraction greatly simplified isoquercitrin extraction and detection. This method was accomplished at room temperature (about 22°C) in 1min with the nonionic surfactant Tergitol TMN-6 as the extractant, n-octanol as cloud point revulsant and synergic reagent. Parameters that affect the synergistic cloud point extraction processes, such as the concentrations of Tergitol TMN-6, volume of n-octanol, sample pH, salt content and extraction time were investigated and optimized. Under the optimum conditions, the calibration curve for the analyte was linear in the range from 5 to 500ngmL -1 with the correlation coefficients greater than 0.9996. Meanwhile, limit of detection (S/N=3) was less than 1.6ngmL -1 and limit of quantification (S/N=10) was less than 5ngmL -1 . It demonstrated that the method can be successfully applied to the pharmacokinetic investigation of isoquercitrin. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. The influence of coupled synchrotron-betatron resonances on the extracted beam of the stretcher ring ELSA

    International Nuclear Information System (INIS)

    Neckenig, M.

    1987-09-01

    For the correction of the chromaticity for horizontal and vertical direction each four sextupoles are installed in ELSA. At a working point near 14/3 their influence on the quantity of the stable region of the transverse phase space is essentially smaller than that of the extraction sextupoles. On the other hand the latter lie at positions of low dispersion so that their influence on the chromaticity is negligible; therefore chromaticity correction and choice of the stable phase-space region are not strongly mutually dependent which will be of advance for the later operation. In extraction with corrected chromaticity the electrons are extracted only because of their different position in the transverse phase space which leads to a timely alteration of the η coordinate and by this to a migration of the extracted beam. Consequences of this are the strongly against extraction without chromaticity correction increased emittance and the doubled momentum uncertainty of the beam. Of advance however is the high extraction efficiency of 80% and the small number of the electrons remaining in the ring (below 2%). (orig./HSI) [de

  1. Surfactant-enhanced liquid-liquid microextraction coupled to micro-solid phase extraction onto highly hydrophobic magnetic nanoparticles

    International Nuclear Information System (INIS)

    Giannoulis, Kiriakos M.; Giokas, Dimosthenis L.; Tsogas, George Z.; Vlessidis, Athanasios G.; Zhu, Qing; Pan, Qinmin

    2013-01-01

    We are presenting a simplified alternative method for dispersive liquid-liquid microextraction (DLLME) by resorting to the use of surfactants as emulsifiers and micro solid-phase extraction (μ-SPE). In this combined procedure, DLLME of hydrophobic components is initially accomplished in a mixed micellar/microemulsion extractant phase that is prepared by rapidly mixing a non-ionic surfactant and 1-octanol in aqueous medium. Then, and in contrast to classic DLLME, the extractant phase is collected by highly hydrophobic polysiloxane-coated core-shell Fe 2 O 3 (at)C magnetic nanoparticles. Hence, the sample components are the target analyte in the DLLME which, in turn, becomes the target analyte of the μ-SPE step. This 2-step approach represents a new and simple DLLME procedure that lacks tedious steps such as centrifugation, thawing, or delicate collection of the extractant phase. As a result, the analytical process is accelerated and the volume of the collected phase does not depend on the volume of the extraction solvent. The method was applied to extract cadmium in the form of its pyrrolidine dithiocarbamate chelate from spiked water samples prior to its determination by FAAS. Detection limits were brought down to the low μg L −1 levels by preconcentrating 10 mL samples with satisfactory recoveries (96.0–108.0 %). (author)

  2. High-power ultrasonic processing: Recent developments and prospective advances

    Science.gov (United States)

    Gallego-Juarez, Juan A.

    2010-01-01

    Although the application of ultrasonic energy to produce or to enhance a wide variety of processes have been explored since about the middle of the 20th century, only a reduced number of ultrasonic processes have been established at industrial level. However, during the last ten years the interest in ultrasonic processing has revived particularly in industrial sectors where the ultrasonic technology may represent a clean and efficient tool to improve classical existing processes or an innovation alternative for the development of new processes. Such seems to be the case of relevant sectors such as food industry, environment, pharmaceuticals and chemicals manufacture, machinery, mining, etc where power ultrasound is becoming an emerging technology for process development. The possible major problem in the application of high-intensity ultrasound on industrial processing is the design and development of efficient power ultrasonic systems (generators and reactors) capable of large scale successful operation specifically adapted to each individual process. In the area of ultrasonic processing in fluid media and more specifically in gases, the development of the steppedplate transducers and other power ge with extensive radiating surface has strongly contributed to the implementation at semi-industrial and industrial stage of several commercial applications, in sectors such as food and beverage industry (defoaming, drying, extraction, etc), environment (air cleaning, sludge filtration, etc...), machinery and process for manufacturing (textile washing, paint manufacture, etc). The development of different cavitational reactors for liquid treatment in continuous flow is helping to introduce into industry the wide potential of the area of sonochemistry. Processes such as water and effluent treatment, crystallization, soil remediation, etc have been already implemented at semi-industrial and/or industrial stage. Other single advances in sectors like mining or energy have

  3. Atomic absorption determination of metals in soils using ultrasonic sample preparation

    International Nuclear Information System (INIS)

    Chmilenko, F.A.; Smityuk, N.M.; Baklanov, A.N.

    2002-01-01

    It was shown that ultrasonic treatment accelerates sample preparation of soil extracts from chernozem into different solvents by a factor of 6 to 60. These extracts are used for the atomic absorption determination of soluble species of Cd, Co, Cr, Cu, Ni, Pb, and Zn. The optimum ultrasound parameters (frequency, intensity, and treatment time) were found for preparing soil extracts containing analytes in concentrations required in agrochemical procedures. Different extractants used to extract soluble heavy metals from soils of an ordinary chernozem type in agrochemical procedures using ultrasonic treatment were classified in accordance with the element nature [ru

  4. Ultrasonic calibration assembly

    International Nuclear Information System (INIS)

    1981-01-01

    Ultrasonic transducers for in-service inspection of nuclear reactor vessels have several problems associated with them which this invention seeks to overcome. The first is that of calibration or referencing a zero start point for the vertical axis of transducer movement to locate a weld defect. The second is that of verifying the positioning (vertically or at a predetermined angle). Thirdly there is the problem of ascertaining the speed per unit distance in the operating medium of the transducer beam prior to the actual inspection. The apparatus described is a calibration assembly which includes a fixed, generally spherical body having a surface for reflecting an ultrasonic beam from one of the transducers which can be moved until the reflection from the spherical body is the highest amplitude return signal indicating radial alignment from the body. (U.K.)

  5. Pulsed ultrasonic stir welding system

    Science.gov (United States)

    Ding, R. Jeffrey (Inventor)

    2013-01-01

    An ultrasonic stir welding system includes a welding head assembly having a plate and a rod passing through the plate. The rod is rotatable about a longitudinal axis thereof. During a welding operation, ultrasonic pulses are applied to the rod as it rotates about its longitudinal axis. The ultrasonic pulses are applied in such a way that they propagate parallel to the longitudinal axis of the rod.

  6. Portable Solid Phase Micro-Extraction Coupled with Ion Mobility Spectrometry System for On-Site Analysis of Chemical Warfare Agents and Simulants in Water Samples

    Directory of Open Access Journals (Sweden)

    Liu Yang

    2014-11-01

    Full Text Available On-site analysis is an efficient approach to facilitate analysis at the location of the system under investigation as it can result in more accurate, more precise and quickly available analytical data. In our work, a novel self-made thermal desorption based interface was fabricated to couple solid-phase microextraction with ion mobility spectrometry for on-site water analysis. The portable interface can be connected with the front-end of an ion mobility spectrometer directly without other modifications. The analytical performance was evaluated via the extraction of chemical warfare agents and simulants in water samples. Several parameters including ionic strength and extraction time have been investigated in detail. The application of the developed method afforded satisfactory recoveries ranging from 72.9% to 114.4% when applied to the analysis of real water samples.

  7. Portable Solid Phase Micro-Extraction Coupled with Ion Mobility Spectrometry System for On-Site Analysis of Chemical Warfare Agents and Simulants in Water Samples

    Science.gov (United States)

    Yang, Liu; Han, Qiang; Cao, Shuya; Yang, Jie; Yang, Junchao; Ding, Mingyu

    2014-01-01

    On-site analysis is an efficient approach to facilitate analysis at the location of the system under investigation as it can result in more accurate, more precise and quickly available analytical data. In our work, a novel self-made thermal desorption based interface was fabricated to couple solid-phase microextraction with ion mobility spectrometry for on-site water analysis. The portable interface can be connected with the front-end of an ion mobility spectrometer directly without other modifications. The analytical performance was evaluated via the extraction of chemical warfare agents and simulants in water samples. Several parameters including ionic strength and extraction time have been investigated in detail. The application of the developed method afforded satisfactory recoveries ranging from 72.9% to 114.4% when applied to the analysis of real water samples. PMID:25384006

  8. Combining Recurrence Analysis and Automatic Movement Extraction from Video Recordings to Study Behavioral Coupling in Face-to-Face Parent-Child Interactions.

    Science.gov (United States)

    López Pérez, David; Leonardi, Giuseppe; Niedźwiecka, Alicja; Radkowska, Alicja; Rączaszek-Leonardi, Joanna; Tomalski, Przemysław

    2017-01-01

    The analysis of parent-child interactions is crucial for the understanding of early human development. Manual coding of interactions is a time-consuming task, which is a limitation in many projects. This becomes especially demanding if a frame-by-frame categorization of movement needs to be achieved. To overcome this, we present a computational approach for studying movement coupling in natural settings, which is a combination of a state-of-the-art automatic tracker, Tracking-Learning-Detection (TLD), and nonlinear time-series analysis, Cross-Recurrence Quantification Analysis (CRQA). We investigated the use of TLD to extract and automatically classify movement of each partner from 21 video recordings of interactions, where 5.5-month-old infants and mothers engaged in free play in laboratory settings. As a proof of concept, we focused on those face-to-face episodes, where the mother animated an object in front of the infant, in order to measure the coordination between the infants' head movement and the mothers' hand movement. We also tested the feasibility of using such movement data to study behavioral coupling between partners with CRQA. We demonstrate that movement can be extracted automatically from standard definition video recordings and used in subsequent CRQA to quantify the coupling between movement of the parent and the infant. Finally, we assess the quality of this coupling using an extension of CRQA called anisotropic CRQA and show asymmetric dynamics between the movement of the parent and the infant. When combined these methods allow automatic coding and classification of behaviors, which results in a more efficient manner of analyzing movements than manual coding.

  9. Analysis of volatiles in silver carp by headspace solid phase micro-extraction coupled with GC-MS

    International Nuclear Information System (INIS)

    Yang Yuping; Xiong Guangquan; Cheng Wei; Liao Tao; Lin Ruotai; Geng Shengrong; Li Xin; Li Xiaoding; Wu Wenjin

    2010-01-01

    In this paper, a method for the determination of volatiles using headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) was presented. The extraction conditions were optimized with reference to these volatiles as hexanal, heptanal, benzaldehyde, 1-Octen-3-ol, octanal, nonanal, decenal, 2,4-heptadienal and 2,4-decadienal. The extraction of fish muscle followed by incubation on a StableFlex divinyl benzene/Carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber during 50 in at 60 obtained the most effective extraction of the analytes. The methods by HS-SPME and GC-MS were effective in detecting volatiles in the gills, scales, viscera and fish muscles. The types of volatiles in the gill were more than other organs and the number of odors compounds was 63, and the number of volatiles in scales, viscera and fish muscles was 48, 44 and 42 respectively. (authors)

  10. Simultaneous extraction and determination of phthalate esters in aqueous solution by yolk-shell magnetic mesoporous carbon-molecularly imprinted composites based on solid-phase extraction coupled with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Yang, Rui; Liu, Yuxin; Yan, Xiangyang; Liu, Shaomin

    2016-12-01

    A rapid, sensitive and accurate method for the simultaneous extraction and determination of five types of trace phthalate esters (PAEs) in environmental water and beverage samples using magnetic molecularly imprinted solid-phase extraction (MMIP-SPE) coupled with gas chromatography-mass spectrometry (GC-MS) was developed. A novel type of molecularly imprinted polymers on the surface of yolk-shell magnetic mesoporous carbon (Fe 3 O 4 @void@C-MIPs) was used as an efficient adsorbent for selective adsorption of phthalate esters based on magnetic solid-phase extraction (MSPE). The real samples were first preconcentrated by Fe 3 O 4 @void@C-MIPs, subsequently extracted by eluent and finally determined by GC-MS after magnetic separation. Several variables affecting the extraction efficiency of the analytes, including the type and volume of the elution solvent, amount of adsorbent, extraction time, desorption time and pH of the sample solution, were investigated and optimized. Validation experiments indicated that the developed method presented good linearity (R 2 >0.9961), satisfactory precision (RSD<6.7%), and high recovery (86.1-103.1%). The limits of detection ranged from 1.6ng/L to 5.2ng/L and the enrichment factor was in the range of 822-1423. The results indicated that the novel method had the advantages of convenience, good sensitivity, and high efficiency, and it could also be successfully applied to the analysis of PAEs in real samples. Copyright © 2016. Published by Elsevier B.V.

  11. Cloud point extraction coupled with microwave-assisted back-extraction (CPE-MABE) for determination of Eszopiclone (Z-drug) using UV-Visible, HPLC and mass spectroscopic (MS) techniques: Spiked and in vivo analysis.

    Science.gov (United States)

    Kori, Shivpoojan; Parmar, Ankush; Goyal, Jony; Sharma, Shweta

    2018-02-01

    A procedure for the determination of Eszopiclone (ESZ) from complex matrices i.e. in vitro (spiked matrices), as well as in vivo (mice model) was developed using cloud point extraction coupled with microwave-assisted back-extraction (CPE-MABE). Analytical measurements have been carried using UV-Visible, HPLC and MS techniques. The proposed method has been validated according to ICH guidelines and legitimate reproducible and reliability of protocol is assessed through intraday and inter-day precision UV-Visible techniques, corresponding to assessed linearity range. The coaservate phase in CPE was back extracted under microwaves exposure, with isooctane at pre-concentration factor ~50 when 5mL of sample solution was pre-concentrated to 0.1mL. Under optimized conditions i.e. Aqueous-Triton X-114 4% (w/v), pH4.0, NaCl 4% (w/v) and equilibrium temperature of 45°C for 20min, average extraction recovery has been obtained between 89.8 and 99.2% and 84.0-99.2% from UV-Visible and HPLC analysis, respectively. The method has been successfully applied to the pharmacokinetic estimation (post intraperitoneal administration) of ESZ in mice. MS analysis precisely depicted the presence of active N‑desmethyl zopiclone in impales as well as in mice plasma. Copyright © 2018 Elsevier B.V. All rights reserved.

  12. Simple and fast analysis of tetrabromobisphenol A, hexabromocyclododecane isomers, and polybrominated diphenyl ethers in serum using solid-phase extraction or QuEChERS extraction followed by tandem mass spectrometry coupled to HPLC and GC.

    Science.gov (United States)

    Li, Jian; Chen, Tian; Wang, Yuwei; Shi, Zhixiong; Zhou, Xianqing; Sun, Zhiwei; Wang, Dejun; Wu, Yongning

    2017-02-01

    Two simplified sample preparation procedures for simultaneous extraction and clean-up of tetrabromobisphenol A, α-, β-, and γ-hexabromocyclododecane and polybrominated diphenyl ethers in human serum were developed and validated. The first procedure was based on solid-phase extraction. Sample extraction, purification, and lipid removal were carried out directly on an Oasis HLB cartridge. The second procedure was a quick, easy, cheap, effective, rugged, and safe-based approach using octadecyl-modified silica particles as a sorbent. After sample extraction and cleanup, tetrabromobisphenol A/hexabromocyclododecane was separated from polybrominated diphenyl ethers by using a Si-based cartridge. Tetrabromobisphenol A and hexabromocyclododecane were then detected by high-performance liquid chromatography coupled to tandem mass spectrometry, while polybrominated diphenyl ethers were detected by gas chromatography coupled to tandem mass spectrometry. The results of the spike recovery test using fetal bovine serum showed that the average recoveries of the analytes ranged from 87.3 to 115.3% with relative standard deviations equal to or lower than 13.4 %. Limits of detection of the analytes were in the range of 0.4-19 pg/mL except for decabromodiphenyl ether. The developed method was successfully applied to routine analysis of human serum samples from occupational workers and the general population. Extremely high serum polybrominated diphenyl ethers levels up to 3.32 × 10 4 ng/g lipid weight were found in occupational workers. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Online turbulent flow extraction coupled with liquid chromatography-tandem mass spectrometry for high throughput screening of anabolic steroids in horse urine.

    Science.gov (United States)

    Shin, Hyun Du; Suh, Joon Hyuk; Kim, Junghyun; Cho, Hyun-Deok; Lee, Su Duk; Han, Kwan Seok; Wang, Yu; Han, Sang Beom

    2017-10-25

    A high throughput method for simultaneous screening of anabolic steroids and their metabolites (4-esterendione, trenbolone, boldenone, oxandrolone, nandrolone, methandrostenolone, testosterone, 1-androstendione, ethisterone, normethandrolone, methyltestosterone, 16β-Hydroxystanozolol, epitestosterone, bolasterone, norethandrolone, danazol, stanozolol and androstadienone) in equine urine by online turbulent flow extraction coupled with liquid chromatography-tandem mass spectrometry was developed. The use of turbulent flow chromatography could simplify pretreatment of horse urine, which has complex matrices as well as high viscosity. The urine was extracted by mixed-mode cation exchange solid phase extraction, and hydrolyzed using β-glucuronidase/arylsulfatase. Then, the sample was automatically loaded on the TurboFlow Cyclone extraction column for removal of further matrix, followed by separation on a fused core C18 column before MS/MS detection. Optimization and validation of the method were discussed in detail. All analytes were rapidly detected within 10min with high sensitivity (picogram to nanogram per milliliter level), and no interference was observed. The linearity range was from 0.1-10ng/mL for nine steroids and 1.0-50ng/mL for the others, with correlation of coefficient values over 0.995. Precision and accuracy ranged from 0.1 to 14.5% and 1.7 to 12.4%, respectively. The developed method was successfully applied to the analysis of anabolic steroids in horse urine after administration of a model drug. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Analysis of iminosugars and other low molecular weight carbohydrates in Aglaonema sp. extracts by hydrophilic interaction liquid chromatography coupled to mass spectrometry.

    Science.gov (United States)

    Rodríguez-Sánchez, S; García-Sarrió, M J; Quintanilla-López, J E; Soria, A C; Sanz, M L

    2015-12-04

    A method by hydrophilic interaction liquid chromatography coupled to tandem mass spectrometry (HILIC-MS(2)) has been successfully developed for the simultaneous analysis of bioactive iminosugars and other low molecular weight carbohydrates in Aglaonema leaf extracts. Among other experimental chromatographic conditions, mobile phase eluents, additives and column temperature were evaluated in terms of retention time, resolution, peak width and symmetry provided for target carbohydrates. In general, narrow peaks (wh: 0.2-0.6min) with good symmetry (As: 0.9-1.3) and excellent resolution (Rs>1.8) were obtained for iminosugars using an acetonitrile:water gradient with 5mM ammonium acetate in both eluents at 55°C. Tandem mass spectra were used to confirm the presence of previously detected iminosugars in Aglaonema extracts and to tentatively identify for the first time others such as miglitol isomer, glycosyl-miglitol isomers and glycosyl-DMDP isomers. Concentration of total iminosugars varied from 1.35 to 2.84mgg(-1) in the extracts of the different Aglaonema samples analyzed. To the best of our knowledge, this is the first time that a HILIC-MS(2) method has been proposed for the simultaneous analysis of iminosugars and other low molecular weight carbohydrates of Aglaonema sp. extracts. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. [Determination of deoxynivalenol in grain and its products by solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Huang, Juan; Chen, Guosong; Zhang, Xiaoyan; Shen, Chongyu; Lü, Chen; Wu, Bin; Liu, Yan; Chen, Huilan; Ding, Tao

    2012-11-01

    A method was established for the determination of deoxynivalenol (vomitoxin) in grain and its products based on solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was firstly extracted by acetonitrile-water (84:16, v/v). The extract was then cleaned-up by an HLB solid phase extraction cartridge. The separation was carried out on a Phenomenex Kinetex C18 column (100 mm x4. 6 mm, 2.6 microm) with a gradient elution using 0.3% per hundred ammonia solution-acetonitrile as mobile phases. The analysis of deoxynivalenol was performed under electrospray negative ionization mode. The limit of detection (LOD, S/N= 3) and the limit of quantification (LOQ, S/N = 10) were 20 microg/kg and 50 microg/kg, respectively. A good linearity (r > 0.99) was achieved for the target compound over the range of 20-1000 pg/L. The recoveries at the three spiked levels (50, 100, 500 microg/kg) in the blank matrices such as flour, barley, soybean, rice, cornmeal, cassava and wheat, were varied from 75.6% to 111.0% with the relative standard deviations no more than 13. 0%. The method is accurate, efficient, sensitive and practical. The cost of pretreatment is obviously reduced by replacing immunoaffinity columns and Mycosep columns with HLB columns which have the same purification effect.

  16. Multipoint fiber-optic laser-ultrasonic actuator based on fiber core-opened tapers.

    Science.gov (United States)

    Tian, Jiajun; Dong, Xiaolong; Gao, Shimin; Yao, Yong

    2017-11-27

    In this study, a novel fiber-optic, multipoint, laser-ultrasonic actuator based on fiber core-opened tapers (COTs) is proposed and demonstrated. The COTs were fabricated by splicing single-mode fibers using a standard fiber splicer. A COT can effectively couple part of a core mode into cladding modes, and the coupling ratio can be controlled by adjusting the taper length. Such characteristics are used to obtain a multipoint, laser-ultrasonic actuator with balanced signal strength by reasonably controlling the taper lengths of the COTs. As a prototype, we constructed an actuator that generated ultrasound at four points with a balanced ultrasonic strength by connecting four COTs with coupling ratios of 24.5%, 33.01%, 49.51%, and 87.8% in a fiber link. This simple-to-fabricate, multipoint, laser-ultrasonic actuator with balanced ultrasound signal strength has potential applications in fiber-optic ultrasound testing technology.

  17. Electromembrane extraction of amino acids from body fluids followed by capillary electrophoresis with capacitively coupled contactless conductivity detection

    Czech Academy of Sciences Publication Activity Database

    Strieglerová, Lenka; Kubáň, Pavel; Boček, Petr

    2011-01-01

    Roč. 1218, č. 37 (2011), s. 6248-6255 ISSN 0021-9673 R&D Projects: GA ČR GAP206/10/1219 Institutional research plan: CEZ:AV0Z40310501 Keywords : electromembrane extraction * biological samples * capillary electrophoresis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.531, year: 2011

  18. Electromagnetic and ultrasonic investigations on a roman marble slab

    Science.gov (United States)

    Capizzi, Patrizia; Cosentino, Pietro L.

    2010-05-01

    The archaeological Museum of Rome (Museo delle Terme di Diocleziano) asked our group about the physical consistency of a marble slab (II - III century AD) that has recently fallen down during the transportation for an exhibition. In fact, due to insurance conflict, it was necessary to control the new fractures due to the recent accident and distinguish them from the ancient ones. The sculptured slab (today's size is 1280 x 70 x 9 cm), cut at the ends for a re-use as an inscription in the rear face, was restored (assemblage of different broken parts and cleaning) in contemporary times. We used different methodologies to investigate the slab: namely a pacometer (Protovale Elcometer) to individuate internal coupling pins, GPR (2000 MHz) and Ultrasonic (55 kHz) tomographic high-density surveys to investigate the internal extension of all the visible fractures and to search for the unknown internal ones. For every methodology used the quality of the acquired data was relatively high. They have been processed and compared to give a set of information useful for the bureaucratic problems of the Museum. Later on, the data have been processed in depth, for studying how to improve the data processing and for extracting all the information contained in the whole set of experimental data. Finally, the results of such a study in depth are exposed in detail.

  19. Recognition of work space using multiple ultrasonic sensors

    Energy Technology Data Exchange (ETDEWEB)

    Hao, J.; Pan, W.; Li, X. [China University of Mining and Technology, Xuzhou (China). College of Information & Electrical Engineering

    2000-07-01

    For applying ultrasonic sensor to the recognition of robot work space in the environment of a coal mine, a method of ultrasonic data fusion was developed with DS (Dempster-Shafer) evidence theory, which includes probability assignment of measurement system, evidence extraction and arithmetic of dynamic fusion. Finally, a computer simulation was performed and a satisfactory result was achieved in an assumed three-dimensional space with an ideal manipulator of straight rod combination. It is proved that the incomplete and unspecialized data can be processed reasonably with DS evidence theory and the method can be implemented conveniently. 6 refs., 4 figs.

  20. Simultaneous determination of platinum group elements and rhenium in rock samples using isotope dilution inductively coupled plasma mass spectrometry after cation exchange separation followed by solvent extraction

    International Nuclear Information System (INIS)

    Shinotsuka, Kazunori; Suzuki, Katsuhiko

    2007-01-01

    A simple and precise determination method for platinum group elements (PGEs) and Re in rock samples was developed using isotope dilution coupled with inductively coupled plasma mass spectrometry (ID-ICP-MS). Cation exchange separation was employed for simplicity, because it is applicable to group separation and simultaneous isotopic measurement in contrast with the widely used anion exchange separation which entails separate elution. However, its application to ID-ICP-MS has been limited due to spectral interferences from impurities retained in the PGE fraction even after ion chromatography. To overcome this limitation, solvent extraction using N-benzoyl-N-phenylhydroxylamine (BPHA) in chloroform was successfully applied for further purification. After the examination of optimum experimental parameters in cation exchange separation and solvent extraction using synthetic PGE solution, the established procedure was applied to the determination of PGEs and Re in some geochemical reference materials. The obtained results agreed well with the literature data determined using the different digestion methods (NiS fire assay and the use of a high-pressure asher) within the analytical uncertainties of each other. Significant difference in reproducibility between Ru, Ir, Pt and Os group, and Pd and Re group was observed in the results for BHVO-2 and JA-2. By considering the error factors affecting analytical reproducibility, we concluded that the difference is ascribed to the sample heterogeneity of minor minerals enriched in Ru, Ir, Pt and Os

  1. Ultrasonic attenuation in superconducting zinc

    International Nuclear Information System (INIS)

    Auluck, S.

    1978-01-01

    The differences in the Zn ultrasonic attenuation data of different workers are analyzed. The superconducting energy gaps deduced from our analysis of the ultrasonic-attenuation data of Cleavelin and Marshall are consistent with the gaps deduced from the knowledge of the Fermi surface and the electron-phonon mass enhancement factor

  2. Lumber defect detection by ultrasonics

    Science.gov (United States)

    K. A. McDonald

    1978-01-01

    Ultrasonics, the technology of high-frequency sound, has been developed as a viable means for locating most defects In lumber for use in digital form in decision-making computers. Ultrasonics has the potential for locating surface and internal defects in lumber of all species, green or dry, and rough sawn or surfaced.

  3. Response of the rf-extraction-wing balcony and floor, and the storage ring to forced and ambient vibration excitation and coupling to tunnel/basemat

    International Nuclear Information System (INIS)

    Jendrzejczyk, J.A.; Wambsganss, M.W.; Smith, R.K.; Rosas-Velez, P.

    1993-08-01

    To ensure successful operation of the APS, vibration of the storage ring quadrupole magnets must be limited to very low levels for frequencies >10 Hz. There will be many sources of vibration, such as pumps, fans, compressors, generators, and other rotating and reciprocating machinery when the APS is operational. In general, such vibration sources are isolated from the structural components and base foundations by vibration dampers and isolators. Pumps are typically mounted on seismic isolators, which are massive bases with response frequencies of <10 Hz, and fans are mounted with elastic-type isolators to minimize vibration coupling. The attenuation of expansion/isolation joints is a very important factor in predicting the response of the storage ring basemat to the various excitation sources. Several 75-hp pumps are located on the balcony of the rf extraction wing, which is close to the storage ring basemat. The pumps per se may prove to be a vibration excitation source of concern. Additional pumps will be placed in the RF extraction building and could add to the vibration levels. If the dynamic unbalance force of the pump motor, and the efficiency of the associated expansion joints were known, one could predict the response of the storage ring basemat. This information would also be useful in determining the placement of additional pumps. This report discusses vibration tests and measurements that were performed on July 28, 1993, in the rf extraction building. The purpose of the investigation was to study the efficiency of two specific expansion joints: (1) the joint that separates a structural column pad from the extraction wing floor, and (2) the joint that separates the extraction wing floor from the roof of the storage ring tunnel. A small electrodynamic exciter, with a maximum RMS force output of ∼0.5 lb at the frequencies of interest, was used

  4. Extraction of hyaluronic acid (HA) from rooster comb and characterization using flow field-flow fractionation (FlFFF) coupled with multiangle light scattering (MALS).

    Science.gov (United States)

    Kang, Dong Young; Kim, Won-Suk; Heo, In Sook; Park, Young Hun; Lee, Seungho

    2010-11-01

    Hyaluronic acid (HA) was extracted in a relatively large scale from rooster comb using a method similar to that reported previously. The extraction method was modified to simplify and to reduce time and cost in order to accommodate a large-scale extraction. Five hundred grams of frozen rooster combs yielded about 500 mg of dried HA. Extracted HA was characterized using asymmetrical flow field-flow fractionation (AsFlFFF) coupled online to a multiangle light scattering detector and a refractive index detector to determine the molecular size, molecular weight (MW) distribution, and molecular conformation of HA. For characterization of HA, AsFlFFF was operated by a simplified two-step procedure, instead of the conventional three-step procedure, where the first two steps (sample loading and focusing) were combined into one to avoid the adsorption of viscous HA onto the channel membrane. The simplified two-step AsFlFFF yielded reasonably good separations of HA molecules based on their MWs. The weight average MW (M(w) ) and the average root-mean-square (RMS) radius of HA extracted from rooster comb were 1.20×10(6) and 94.7 nm, respectively. When the sample solution was filtered through a 0.45 μm disposable syringe filter, they were reduced down to 3.8×10(5) and 50.1 nm, respectively. Copyright © 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Determination of nonylphenol isomers in landfill leachate and municipal wastewater using steam distillation extraction coupled with comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry

    Science.gov (United States)

    Zhang, Caixiang; Eganhouse, Robert P.; Pontolillo, James; Cozzarelli, Isabelle M.; Wang, Yanxin

    2012-01-01

    4-Nonylphenols (4-NPs) are known endocrine disruptors and by-products of the microbial degradation of nonylphenol polyethoxylate surfactants. One of the challenges to understanding the toxic effects of nonylphenols is the large number of isomers that may exist in environmental samples. In order to attribute toxic effects to specific compounds, a method is needed for the separation and quantitation of individual nonylphenol isomers. The pre-concentration methods of solvent sublimation, solid-phase extraction or liquid–liquid extraction prior to chromatographic analysis can be problematic because of co-extraction of thousands of compounds typically found in complex matrices such as municipal wastewater or landfill leachate. In the present study, steam distillation extraction (SDE) was found to be an effective pre-concentration method for extraction of 4-NPs from leachate and wastewater, and comprehensive two-dimensional gas chromatography (GC × GC) coupled with fast mass spectral data acquisition by time-of-flight mass spectrometry (ToFMS) enhanced the resolution and identification of 4-NP isomers. Concentrations of eight 4-NP isomers were determined in leachate from landfill cells of different age and wastewater influent and effluent samples. 4-NP isomers were about 3 times more abundant in leachate from the younger cell than the older one, whereas concentrations in wastewater effluent were either below detection limits or <1% of influent concentrations. 4-NP isomer distribution patterns were found to have been altered following release to the environment. This is believed to reflect isomer-specific degradation and accumulation of 4-NPs in the aquatic environment.

  6. Determination of occluded oxygen, nitrogen and hydrogen in zircalloy-4 by vacuum extraction coupled to gas chromatography

    International Nuclear Information System (INIS)

    Vega, O.; Imakuma, K.

    1983-01-01

    The technique of vacuum extraction at high temperatures was used for the liberation of gases from zircalloy-4 samples; oxygen, nitrogen and hydrogen were quantitatively analysed by gas chromatography. Two different sets of zircalloy-4 samples were examined. The results for O 2 , N 2 and H 2 quantitative analyses satisfy the requirements for the characterization of the zircalloy-4 quality. (C.L.B.) [pt

  7. Determination of multi-class herbicides in soil by liquid-solid extraction coupled with headspace solid phase microextraction method

    Directory of Open Access Journals (Sweden)

    Đurović-Pejčev Rada

    2016-01-01

    Full Text Available A method is described for simultaneous determination of five herbicides (metribuzin, acetochlor, clomazone, oxyfluorfen and dimethenamid belonging to different pesticides groups in soil samples. Developed headspace solid phase microextraction method (HS-SPME in combination with liquid-solid sample preparation (LS was optimized and applied in the analysis of some agricultural samples. Optimization of microextraction conditions, such as temperature, extraction time and sodium chloride (NaCl content was perfor-med using 100 μm polydimethyl-siloxane (PDMS fiber. The extraction effi-ciencies of methanol, methanol:acetone=1:1 and methanol:acetone:hexane= =2:2:1 and the optimum number of extraction steps during the sample prepa-ration, were tested, as well. Gas chromatography-mass spectrometry (GC-MS was used for detection and quantification, obtaining relative standard deviation (RSD below 13%, and recovery values higher than 83% for multiple analyses of soil samples fortified at 30 μg kg-1 of each herbicide. Limits of detection (LOD were less than 1.2 μg kg-1 for all the studied herbicides. [Projekat Ministarstva nauke Republike Srbije, br. TR31043 i br. III43005

  8. Ultrasonic inspection of austenitic welds

    International Nuclear Information System (INIS)

    Baikie, B.L.; Wagg, A.R.; Whittle, M.J.; Yapp, D.

    1976-01-01

    The ultrasonic examination of austenitic stainless steel weld metal has always been regarded as a difficult proposition because of the large and variable ultrasonic attenuations and back scattering obtained from apparently similar weld deposits. The work to be described shows how the existence of a fibre texture within each weld deposit (as a result of epitaxial growth through successive weld beads) produces a systematic variation in the ultrasonic attenuation coefficient and the velocity of sound, depending upon the angle between the ultrasonic beam and the fibre axis. Development work has shown that it is possible to adjust the welding parameters to ensure that the crystallographic texture within each weld is compatible with improved ultrasonic transmission. The application of the results to the inspection of a specific weld in type 316 weld metal is described

  9. Ultrasonic variables affecting inspection

    International Nuclear Information System (INIS)

    Lautzenheiser, C.E.; Whiting, A.R.; McElroy, J.T.

    1977-01-01

    There are many variables which affect the detection of the effects and reproducibility of results when utilizing ultrasonic techniques. The most important variable is the procedure, as this document specifies, to a great extent, the controls that are exercised over the other variables. The most important variable is personnel with regards to training, qualification, integrity, data recording, and data analysis. Although the data is very limited, these data indicate that, if the procedure is carefully controlled, reliability of defect detection and reproducibility of results are both approximately 90 percent for reliability of detection, this applies to relatively small defects as reliability increases substantially as defect size increases above the recording limit. (author)

  10. Ultrasonic texture characterization of aluminum, zirconium and titanium alloys

    International Nuclear Information System (INIS)

    Anderson, A.J.

    1997-01-01

    This work attempts to show the feasibility of nondestructive characterization of non-ferrous alloys. Aluminum alloys have a small single crystal anisotropy which requires very precise ultrasonic velocity measurements for derivation of orientation distribution coefficients (ODCs); the precision in the ultrasonic velocity measurement required for aluminum alloys is much greater than is necessary for iron alloys or other alloys with a large single crystal anisotropy. To provide greater precision, some signal processing corrections need to be applied to account for the inherent, half-bandwidth offset in triggered pulses when using a zero-crossing technique for determining ultrasonic velocity. In addition, alloys with small single crystal anisotropy show a larger dependence on the single crystal elastic constants (SCECs) when predicting ODCs which require absolute velocity measurements. Attempts were made to independently determine these elastics constants in an effort to improve correlation between ultrasonically derived ODCs and diffraction derived ODCs. The greater precision required to accurately derive ODCs in aluminum alloys using ultrasonic nondestructive techniques is easily attainable. Ultrasonically derived ODCs show good correlation with derivations made by Bragg diffraction techniques, both neutron and X-ray. The best correlation was shown when relative velocity measurements could be used in the derivations of the ODCs. Calculation of ODCs in materials with hexagonal crystallites can also be done. Because of the crystallite symmetries, more information can be extracted using ultrasonic techniques, but at a cost of requiring more physical measurements. Some industries which use materials with hexagonal crystallites, e.g. zirconium alloys and titanium, have traditionally used texture parameters which provide some specialized measure of the texture. These texture parameters, called Kearns factors, can be directly related to ODCs

  11. Ultrasonic assessment of additive manufactured Ti-6Al-4V

    Science.gov (United States)

    Schehl, Norman; Kramb, Vicki; Dierken, Josiah; Aldrin, John; Schwalbach, Edwin; John, Reji

    2018-04-01

    Additive Manufacturing (AM) processes offer the potential for manufacturing cost savings and rapid insertion into service through production of near net shape components for complicated structures. Use of these parts in high reliability applications such as those in the aerospace industry will require nondestructive characterization methods to ensure post-process material quality in as-built condition. Ultrasonic methods can be used for this quality verification. Depending on the application, the service life of AM components can be sensitive to the part surface condition. The surface roughness and layered structure inherent to the electron-beam powder-bed fusion process necessitates new approaches to evaluate subsurface material integrity in its presence. Experimental methods and data analytics may improve the evaluation of as-built additively manufactured materials. This paper discusses the assessment of additively manufactured EBM Ti-6Al-4V panels using ultrasonic methods and the data analytics applied to evaluate material integrity. The assessment was done as an exploratory study as the discontinuities of interest in these test samples were not known when the measurements were performed. Water immersion ultrasonic techniques, including pulse-echo and through transmission with 10 MHz focused transducers, were used to explore the material integrity of as-built plates. Subsequent destructive mechanical tests of specimens extracted from the plates provided fracture locations indicating critical flaws. To further understand the effect of surface-roughness, an evaluation of ultrasonic response in the presence of as-built surfaces and with the surface removed was performed. The assessment of additive manufactured EBM Ti-6Al-4V panels with ultrasonic techniques indicated that ultrasonic energy was attenuated by the as-built surface roughness. In addition, feature detection was shown to be sensitive to experimental ultrasonic parameters and flaw morphology.

  12. An Ultrasonic Pattern Recognition Approach to Welding Defect Classification

    International Nuclear Information System (INIS)

    Song, Sung Jin

    1995-01-01

    Classification of flaws in weldments from their ultrasonic scattering signals is very important in quantitative nondestructive evaluation. This problem is ideally suited to a modern ultrasonic pattern recognition technique. Here brief discussion on systematic approach to this methodology is presented including ultrasonic feature extraction, feature selection and classification. A stronger emphasis is placed on probabilistic neural networks as efficient classifiers for many practical classification problems. In an example probabilistic neural networks are applied to classify flaws in weldments into 3 classes such as cracks, porosity and slag inclusions. Probabilistic nets are shown to be able to exhibit high performance of other classifiers without any training time overhead. In addition, forward selection scheme for sensitive features is addressed to enhance network performance

  13. Wireless cardiac action potential transmission with ultrasonically inserted silicon microprobes

    International Nuclear Information System (INIS)

    Shen, C J; Ramkumar, A; Lal, A; Gilmour, R F Jr

    2011-01-01

    This paper reports on the integration of ultrasonically inserted horn-shaped cardiac probes with wireless transmission of 3D cardiac action potential measurement for applications in ex vivo preparations such as monitoring the onset of ventricular fibrillation. Ultrasonically inserted silicon horn probes permit reduced penetration force during insertion, allowing silicon, a brittle material, to penetrate cardiac tissue. The probes also allow recording from multiple sites that are lithographically defined. An application-specific integrated circuit has been designed with a 40 dB amplifying stage and a frequency modulating oscillator at 95 MHz to wirelessly transmit the recorded action potentials. This ultrasonically inserted microprobe wireless system demonstrates the initial results in wireless monitoring of 3D action potential propagation, and the extraction of parameters of interest including the action potential duration and diastolic interval

  14. Method validation for determination of metals in Vitis labrusca L. grapevine leaf extracts by inductively coupled plasma mass spectrometry (ICP-MS

    Directory of Open Access Journals (Sweden)

    LIANE V.V. BOKOWSKI

    Full Text Available ABSTRACT Vitis labrusca L. is the main species used for wine and juice production in Brazil. The grapevine leaves can be used both as functional foods and as cheapest sources for the extraction of phenolic compounds. Besides the antioxidant activity, grapevine leaves exhibited significant anti-inflammatory activity. Therefore, the aim of this study was to develop and validate an analytical methodology to determine the metals selenium (96Se, chromium (53Cr, nickel (62Ni, cadmium (111Cd and lead (206Pb in 30 samples of grapevine leaf extracts (Vitis labrusca, Bordo cultivar using inductively coupled plasma mass spectrometry (ICP-MS. To obtain the grapevine leaf extracts the samples were milled, weighed and digested in microwave oven with nitric acid. The method showed linearity, precision, accuracy and limits of quantification and detection acceptable for INMETRO protocol validation of analytical methods. Therefore, the method using ICP-MS was developed and validated to determine metals concentrations in grapevine leaves of Vitis labrusca L. and the proposed method could be applied in routine analytical laboratory.

  15. Ultra-trace determination of Persistent Organic Pollutants in Arctic ice using stir bar sorptive extraction and gas chromatography coupled to mass spectrometry.

    Science.gov (United States)

    Lacorte, S; Quintana, J; Tauler, R; Ventura, F; Tovar-Sánchez, A; Duarte, C M

    2009-12-04

    This study presents the optimization and application of an analytical method based on the use of stir bar sorptive extraction (SBSE) gas chromatography coupled to mass spectrometry (GC-MS) for the ultra-trace analysis of POPs (Persistent Organic Pollutants) in Arctic ice. In a first step, the mass-spectrometry conditions were optimized to quantify 48 compounds (polycyclic aromatic hydrocarbons, brominated diphenyl ethers, chlorinated biphenyls, and organochlorinated pesticides) at the low pg/L level. In a second step, the performance of this analytical method was evaluated to determine POPs in Arctic cores collected during an oceanographic campaign. Using a calibration range from 1 to 1800 pg/L and by adjusting acquisition parameters, limits of detection at the 0.1-99 and 102-891 pg/L for organohalogenated compounds and polycyclic aromatic hydrocarbons, respectively, were obtained by extracting 200 mL of unfiltered ice water. alpha-hexachlorocyclohexane, DDTs, chlorinated biphenyl congeners 28, 101 and 118 and brominated diphenyl ethers congeners 47 and 99 were detected in ice cores at levels between 0.5 to 258 pg/L. We emphasise the advantages and disadvantages of in situ SBSE in comparison with traditional extraction techniques used to analyze POPs in ice.

  16. Capillary electrophoresis coupled with chloroform-acetonitrile extraction for rapid and highly selective determination of cysteine and homocysteine levels in human blood plasma and urine.

    Science.gov (United States)

    Ivanov, Alexander Vladimirovich; Bulgakova, Polina Olegovna; Virus, Edward Danielevich; Kruglova, Maria Petrovna; Alexandrin, Valery Vasil'evich; Gadieva, Viktoriya Aleksandrovna; Luzyanin, Boris Petrovich; Kushlinskii, Nikolai Evgen'evich; Fedoseev, Anatolij Nikolaevich; Kubatiev, Aslan Amirkhanovich

    2017-10-01

    A rapid and selective method has been developed for highly sensitive determination of total cysteine and homocysteine levels in human blood plasma and urine by capillary electrophoresis (CE) coupled with liquid-liquid extraction. Analytes were first derivatized with 1,1'-thiocarbonyldiimidazole and then samples were purified by chloroform-ACN extraction. Electrophoretic separation was performed using 0.1 M phosphate with 30 mM triethanolamine, pH 2, containing 25 μM CTAB, 2.5 μM SDS, and 2.5% polyethylene glycol 600. Samples were injected into the capillary (with total length 32 cm and 50 μm id) at 2250 mbar*s and subsequent injection was performed for 30 s with 0.5 M KОН. The total analysis time was less than 9 min, accuracy was 98%, and precision was <2.6%. The LOD was 0.2 μM for homocysteine and 0.5 μM for cysteine. The use of liquid-liquid extraction allowed the precision and sensitivity of the CE method to be significantly increased. The validated method was applied to determine total cysteine and homocysteine content in human blood plasma and urine samples obtained from healthy volunteers and patients with kidney disorders. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Characterisation of organic compounds in aerosol particles from a finnish forest by on-line coupled supercritical fluid extraction-liquid chromatography-gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Shimmo, Masahiko; Jaentti, Jaana; Hartonen, Kari; Hyoetylaeinen, Tuulia; Riekkola, Marja-Liisa [Laboratory of Analytical Chemistry, Department of Chemistry, University of Helsinki, P.O. Box 55, 00014, Helsinki (Finland); Aalto, Pasi; Kulmala, Markku [Division of Atmospheric Sciences, Department of Physical Sciences, University of Helsinki, P.O. Box 64, 00014, Helsinki (Finland)

    2004-04-01

    During the European Union project Quantification of Aerosol Nucleation in the European Boundary Layer (QUEST), which began in spring 2003, atmospheric aerosol particles were collected in a Finnish Scots pine forest using a high-volume sampler. The organic compounds in the filter samples were then analysed by on-line coupled supercritical fluid extraction-liquid chromatography-gas chromatography-mass spectrometry (SFE-LC-GC-MS). The sample was first extracted by SFE. During LC the extracts were fractionated into three fractions according to polarity. The final separation was carried out by GC-MS. A fraction volume as high as 840 {mu}L was transferred to the GC, using the partial concurrent eluent evaporation technique. The same instrumentation, with an in-situ SFE derivatisation method, was used to analyse organic acids. Major compounds such as n-alkanes and PAH were analysed quantitatively. Their concentrations were lower than those usually observed in urban areas or in other forest areas in Europe. The wind direction was one of the most important factors affecting changes in the daily concentrations of these compounds. Scots pine needles were analysed with the same system to obtain reference data for identification of biogenic compounds in aerosol particles. Other organic compounds found in this study included hopanes, steranes, n-alkanals, n-alkan-2-ones, oxy-PAH, and alkyl-PAH; some biogenic products, including oxidation products of monoterpenes, were also identified. (orig.)

  18. Determination of selenoprotein P in human plasma by solid phase extraction and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Bendahl, L.; Sidenius, U.; Gammelgaard, Bente

    2000-01-01

    measured by inductively coupled plasma mass spectrometry (ICP-MS) monitoring the Se-82 isotope. Linear response was observed in the concentration range 0.3-70.8 mu g/l selenium as selenoprotein P with a correlation coefficient of 0.9994. The precision expressed as relative standard deviation was better...... than 2% in this range. The estimated limit of detection was 2 mu g/l and the experimentally verified quantification limit was 5 mu g/l, giving a relative standard deviation less than 2%. (C) 2000 Elsevier Science B.V. All rights reserved...

  19. Inspection of austenitic welds with ultrasonic phased array technology

    Energy Technology Data Exchange (ETDEWEB)

    Garcia, A.; Fernandez, F. [Tecnatom (Spain); Dutruc, R.; Ferriere, R. [Metalscan (France)

    2011-07-01

    This series of slides presents the use of ultrasonic phased array technology in the inspection of austenitic welds. The inspection from outside surface (the inspection is performed in contact using wedges to couple the probe to the outer surface of the component) shows that longitudinal wave is the most adequate for perpendicular scans and transversal ultrasonic wave is the most adequate for parallel scans. Detection and length sizing are performed optimally in perpendicular scans. The inspection from inside surface shows: -) Good results in the detection of defects (Sizing has met the requirements imposed by the Authority of the Russian Federation); -) The new design of the mechanical equipment and of the numerous ultrasonic beams refracted by the array probes has increased the volume inspected. The design of the mechanical equipment has also allowed new areas to be inspected (example a piping weld that was not accessible from the outer surface; -) The ultrasonic procedure and Inspection System developed have been validated by the Authority of the Russian Federation. Phase array technique supplies solutions to solve accessibility concerns and improve the ultrasonic inspections of nuclear components

  20. Acetylcholinesterase immobilized capillary reactors coupled to protein coated magnetic beads: A new tool for plant extract ligand screening

    OpenAIRE

    Vanzolini, Kenia Lourenço; Jiang, Zhengjin; Zhang, Xiaoqi; Vieira, Lucas Campos Curcino; Corrêa, Arlene Gonçalvez; Cardoso, Carmen Lucia; Cass, Quezia Bezerra; Moaddel, Ruin

    2013-01-01

    The use of immobilized capillary enzyme reactors (ICERs) and enzymes coated to magnetic beads ((NT or CT)-MB) for ligand screening has been adopted as a new technique of high throughput screening (HTS). In this work the selected target was the enzyme acetylcholinesterase (AChE), which acts on the central nervous system and is a validated target for the treatment of Alzheimer’s disease, as well as for new insecticides. A new approach for the screening of plant extracts was developed based on t...

  1. Advanced ultrasonic inspections

    International Nuclear Information System (INIS)

    Ghia, S.

    1990-08-01

    Acoustic Emission (AE) continuous monitoring and periodical inspections by advanced ultrasonic have been applied to evaluate defect evolution within a PWR reduced scale (1:5) pressure vessel subjected to cyclic mechanical fatigue test. This experimental activity has been carried out in the frame of the Primary Circuit Component Life Prediction programme. In the time period covered by this report actions were performed as following: (1) Ultrasonic examination by multifrequency acoustic holography to evaluate defect evolution subsequently repair and heat treatment of the R2 vessel carried out in March 1988. For the purpose, measurements were performed both at 0 and 200 bar of internal pressure. As uniformity of the procedures adopted, for calibration and testing, made the results comparable with the previous ones no evidence for significant growing of the examined defects has been found. (2) Acoustic emission monitoring has then been carried out during fatigue test from 416000 to 565000 fatigue cycles. Analysis of a large amount of data has been performed paying particular attention to the distinction between friction phenomena and crack growth in order to obtain a correct diagnosis of flaw evolution. The signal duration distribution and the correlation of AE appearance time versus load cycle phase were considered to characterise stick-slip processes. A general intensification of AE activity has been recorded during this last period of monitoring and previous known AE sources were confirmed together with the appearance of new AE sources some of them correlable with real defects

  2. System for ultrasonic examination

    International Nuclear Information System (INIS)

    Lund, S.A.; Kristensen, W.D.

    1987-01-01

    A computerized system for the recording of flaw images by ultrasonic examination according to the pulse-echo method includes at least one ultrasonic probe which can be moved in steps over the surface of an object along a rectilinear scanning path. Digital signals containing information on the successive positions of the sound beam, on echo amplitudes, and on the lengths of sound paths to reflectors inside the object, are processed and used for the accumulated storage of circular patterns of echo amplitude data in a matrix memory associated with a sectional plane through the object. A video screen terminal controls the system and transforms the accumulated data into displays of sectional flaw images of greatly improved precision and sharpness of definition. A gradual transfer of filtered data from a number of parallel sectional planes to three further matrix memories associated with projection planes at right angles to each other permits presentation in three dimensions of equally improved projection flaw images. (author) 2 figs

  3. Evaluation of Carbohydrates in Natural and Cultured Cordyceps by Pressurized Liquid Extraction and Gas Chromatography Coupled with Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Jia Guan

    2010-06-01

    Full Text Available Free and polymeric carbohydrates in Cordyceps, a valued edible mushroom and well-known traditional Chinese medicine, were determined using stepwise pressurized liquid extraction (PLE extraction and GC-MS. Based on the optimized PLE conditions, acid hydrolysis and derivatization, ten monosaccharides, namely rhamnose, ribose, arabinose, xylose, mannose, glucose, galactose, mannitol, fructose and sorbose in 13 samples of natural and cultured Cordyceps were qualitatively and quantitatively analyzed and compared with myo-inositol hexaacetate as internal standard. The results showed that natural C. sinensis contained more than 7.99% free mannitol and a small amount of glucose, while its polysaccharides were usually composed of mannose, glucose and galactose with a molar ratio of 1.00:16.61~3.82:1.60~1.28. However, mannitol in cultured C. sinensis and cultured C. militaris were less than 5.83%, and free glucose was only detected in a few samples, while their polysaccharides were mainly composed of mannose, glucose and galactose with molar ratios of 1.00:3.01~1.09:3.30~1.05 and 1.00:2.86~1.28:1.07~0.78, respectively. Natural and cultured Cordyceps could be discriminated by hierarchical clustering analysis based on its free carbohydrate contents.

  4. Determination of rhodium in metallic alloy and water samples using cloud point extraction coupled with spectrophotometric technique

    Science.gov (United States)

    Kassem, Mohammed A.; Amin, Alaa S.

    2015-02-01

    A new method to estimate rhodium in different samples at trace levels had been developed. Rhodium was complexed with 5-(4‧-nitro-2‧,6‧-dichlorophenylazo)-6-hydroxypyrimidine-2,4-dione (NDPHPD) as a complexing agent in an aqueous medium and concentrated by using Triton X-114 as a surfactant. The investigated rhodium complex was preconcentrated with cloud point extraction process using the nonionic surfactant Triton X-114 to extract rhodium complex from aqueous solutions at pH 4.75. After the phase separation at 50 °C, the surfactant-rich phase was heated again at 100 °C to remove water after decantation and the remaining phase was dissolved using 0.5 mL of acetonitrile. Under optimum conditions, the calibration curve was linear for the concentration range of 0.5-75 ng mL-1 and the detection limit was 0.15 ng mL-1 of the original solution. The enhancement factor of 500 was achieved for 250 mL samples containing the analyte and relative standard deviations were ⩽1.50%. The method was found to be highly selective, fairly sensitive, simple, rapid and economical and safely applied for rhodium determination in different complex materials such as synthetic mixture of alloys and environmental water samples.

  5. Arsenic speciation in edible alga samples by microwave-assisted extraction and high performance liquid chromatography coupled to atomic fluorescence spectrometry

    International Nuclear Information System (INIS)

    García-Salgado, S.; Quijano, M.A.; Bonilla, M.M.

    2012-01-01

    Highlights: ► Total As and As species were analyzed in edible marine algae. ► A microwave-assisted extraction method with deionized water was applied. ► As compounds identified comprised DMA, As(V) and four arsenosugars ► Considerably high As(V) concentrations were found in the most of the algae studied. - Abstract: Twelve commercially available edible marine algae from France, Japan and Spain and the certified reference material (CRM) NIES No. 9 Sargassum fulvellum were analyzed for total arsenic and arsenic species. Total arsenic concentrations were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) after microwave digestion and ranged from 23 to 126 μg g −1 . Arsenic species in alga samples were extracted with deionized water by microwave-assisted extraction and showed extraction efficiencies from 49 to 98%, in terms of total arsenic. The presence of eleven arsenic species was studied by high performance liquid chromatography–ultraviolet photo-oxidation–hydride generation atomic–fluorescence spectrometry (HPLC–(UV)–HG–AFS) developed methods, using both anion and cation exchange chromatography. Glycerol and phosphate sugars were found in all alga samples analyzed, at concentrations between 0.11 and 22 μg g −1 , whereas sulfonate and sulfate sugars were only detected in three of them (0.6-7.2 μg g −1 ). Regarding arsenic toxic species, low concentration levels of dimethylarsinic acid (DMA) ( −1 ) and generally high arsenate (As(V)) concentrations (up to 77 μg g −1 ) were found in most of the algae studied. The results obtained are of interest to highlight the need to perform speciation analysis and to introduce appropriate legislation to limit toxic arsenic species content in these food products.

  6. Screening and Identification for Immunological Active Components from Andrographis Herba Using Macrophage Biospecific Extraction Coupled with UPLC/Q-TOF-MS

    Directory of Open Access Journals (Sweden)

    Yaqi Wang

    2018-04-01

    Full Text Available The method of cell biospecific extraction coupled with UPLC/Q-TOF-MS has been developed as a tool for the screening and identification of potential immunological active components from Andrographis Herba (AH. In our study, a macrophage cell line (RAW264.7 was used to extract cell-combining compounds from the ethanol extract of AH. The cell binding system was then analyzed and identified by UPLC/Q-TOF-MS analysis. Finally, nine compounds, which could combine with macrophages, in an ethanol extract of AH were detected by comparing basic peak intensity (BPI profiles of macrophages before and after treatment with AH. Then they were identified as Andrographidine E (1, Andrographidine D (2, Neoandrographolide (3, Dehydroandrographolide (4, 5, 7, 2′, 3′-tetramethoxyflavone (5, β-sitosterol (7, 5-hydroxy-7, 2′, 3′-trimethoxyflavone (8 and 5-hydroxy-7, 8, 2′, 3′-tetramethoxyflavone (9, which could classified into five flavonoids, three diterpene lactones, and one sterol. Their structures were recognized by their characteristic fragment ions and fragmentations pattern of diterpene lactones and flavonoids. Additionally, the activity of compounds 3, 4, and 7 was tested in vitro. Results showed that these three compounds could decrease the release of NO (p < 0.01 in macrophages remarkably. Moreover, 3, 4, and 7 showed satisfactory dose-effect relationships and their IC50 values were 9.03, 18.18, and 13.76 μg/mL, respectively. This study is the first reported work on the screening of immunological active components from AH. The potential immunological activity of flavonoids from AH has not been reported previously.

  7. Arsenic speciation in edible alga samples by microwave-assisted extraction and high performance liquid chromatography coupled to atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Garcia-Salgado, S. [Departamento de Ingenieria Civil: Tecnologia Hidraulica y Energetica, Escuela Universitaria de Ingenieria Tecnica de Obras Publicas, Universidad Politecnica de Madrid, Alfonso XII 3 y 5, 28014 Madrid (Spain); Quijano, M.A., E-mail: marian.quijano@upm.es [Departamento de Ingenieria Civil: Tecnologia Hidraulica y Energetica, Escuela Universitaria de Ingenieria Tecnica de Obras Publicas, Universidad Politecnica de Madrid, Alfonso XII 3 y 5, 28014 Madrid (Spain); Bonilla, M.M. [Departamento de Ingenieria Civil: Tecnologia Hidraulica y Energetica, Escuela Universitaria de Ingenieria Tecnica de Obras Publicas, Universidad Politecnica de Madrid, Alfonso XII 3 y 5, 28014 Madrid (Spain)

    2012-02-10

    Highlights: Black-Right-Pointing-Pointer Total As and As species were analyzed in edible marine algae. Black-Right-Pointing-Pointer A microwave-assisted extraction method with deionized water was applied. Black-Right-Pointing-Pointer As compounds identified comprised DMA, As(V) and four arsenosugars Black-Right-Pointing-Pointer Considerably high As(V) concentrations were found in the most of the algae studied. - Abstract: Twelve commercially available edible marine algae from France, Japan and Spain and the certified reference material (CRM) NIES No. 9 Sargassum fulvellum were analyzed for total arsenic and arsenic species. Total arsenic concentrations were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) after microwave digestion and ranged from 23 to 126 {mu}g g{sup -1}. Arsenic species in alga samples were extracted with deionized water by microwave-assisted extraction and showed extraction efficiencies from 49 to 98%, in terms of total arsenic. The presence of eleven arsenic species was studied by high performance liquid chromatography-ultraviolet photo-oxidation-hydride generation atomic-fluorescence spectrometry (HPLC-(UV)-HG-AFS) developed methods, using both anion and cation exchange chromatography. Glycerol and phosphate sugars were found in all alga samples analyzed, at concentrations between 0.11 and 22 {mu}g g{sup -1}, whereas sulfonate and sulfate sugars were only detected in three of them (0.6-7.2 {mu}g g{sup -1}). Regarding arsenic toxic species, low concentration levels of dimethylarsinic acid (DMA) (<0.9 {mu}g g{sup -1}) and generally high arsenate (As(V)) concentrations (up to 77 {mu}g g{sup -1}) were found in most of the algae studied. The results obtained are of interest to highlight the need to perform speciation analysis and to introduce appropriate legislation to limit toxic arsenic species content in these food products.

  8. Determination of organophosphorus flame retardants in fish by pressurized liquid extraction using aqueous solutions and solid-phase microextraction coupled with gas chromatography-flame photometric detector.

    Science.gov (United States)

    Gao, Zhanqi; Deng, Yuehua; Yuan, Wenting; He, Huan; Yang, Shaogui; Sun, Cheng

    2014-10-31

    A novel method was developed for the determination of organophosphorus flame retardants (PFRs) in fish. The method consists of a combination of pressurized liquid extraction (PLE) using aqueous solutions and solid-phase microextraction (SPME), followed by gas chromatography-flame photometric detector (GC-FPD). The experimental parameters that influenced extraction efficiency were systematically evaluated. The optimal responses were observed by extracting 1g of fish meat with the solution of water:acetonitrile (90:10, v/v) at 150°C for 5min and acid-washed silica gel used as lipid sorbent. The obtained extract was then analyzed by SPME coupled with GC-FPD without any additional clean-up steps. Under the optimal conditions, the proposed procedure showed a wide linear range (0.90-5000ngg(-1)) obtained by analyzing the spiked fish samples with increasing concentrations of PFRs and correlation coefficient (R) ranged from 0.9900 to 0.9992. The detection limits (S/N=3) were in the range of 0.010-0.208ngg(-1) with standard deviations (RSDs) ranging from 2.0% to 9.0%. The intra-day and inter-day variations were less than 9.0% and 7.8%, respectively. The proposed method was successfully applied to the determination of PFRs in real fish samples with recoveries varying from 79.8% to 107.3%. The results demonstrate that the proposed method is highly effective for analyzing PFRs in fish samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. Imaging techniques for ultrasonic testing

    International Nuclear Information System (INIS)

    2013-01-01

    These seminar proceedings contain 16 lectures on the following topics: 1. From imaging to quantification - ultrasound methods in medical diagnostics; 2. SAFT, TOFD, Phased Array - classical applications and recent developments in ultrasonic imaging; 3. Innovative ultrasonic imaging methods in research and application; 4. Industrial ultrasonic testing of fibre-reinforced structures of complex geometry; 5. Visualisation of crack tips in the inspection of wheel set shafts with longitudinal boreholes as a means of avoiding unnecessary wheel set changes; 6. Areal analysis of the propagation of Lamb waves on curved, anisotropic structures; 7. High-resolution representation in immersion technique testing; 8. Variants in generating images from phased array measurement data - practical examples involving copper, carbon-fibre reinforced plastic and other materials; 9. GIUM - an unconventional method of microstructure imaging using ultrasonic stimulation and laser vibrometry scanning; 10. Innovative air-ultrasonic testing concepts for improved imaging; 11. Use of imaging methods for improving the quality of test results from nondestructive testing; 12. Modelling and visualisation of EMUS stimulation for transducer optimisation; 13. Use of SAFT in the manufacture of energy conversion machines; 14. Ultrasonic imaging tests for improved defect characterisation during weld seam inspection on longitudinally welded large-diameter pipes; 15. SAFT reconstruction for testing austenitic weld seams and dissimilar metal weld seams for transverse cracks; 16. Imaging-based optimisation method for quantitative ultrasonic testing of anisotropic inhomogeneous austenitic welded joints with determination and utilisation of their elastic properties. One contribution has been abstracted separately. [de

  10. Plant Extract Mediated Eco-Friendly Synthesis of Pd@Graphene Nanocatalyst: An Efficient and Reusable Catalyst for the Suzuki-Miyaura Coupling

    Directory of Open Access Journals (Sweden)

    Mujeeb Khan

    2017-01-01

    Full Text Available Suzuki-Miyaura coupling reaction catalyzed by the palladium (Pd-based nanomaterials is one of the most versatile methods for the preparation of biaryls. However, use of organic solvents as reaction medium causes a big threat to environment due to the generation of toxic byproducts as waste during the work up of these reactions. Therefore, the use of water as reaction media has attracted tremendous attention due to its environmental, economic, and safety benefits. In this study, we report on the synthesis of green Pd@graphene nanocatalyst based on an in situ functionalization approach which exhibited excellent catalytic activity towards the Suzuki–Miyaura cross-coupling reactions of phenyl halides with phenyl boronic acids under facile conditions in water. The green and environmentally friendly synthesis of Pd@graphene nanocatalyst (PG-HRG-Pd is carried out by simultaneous reduction of graphene oxide (GRO and PdCl2 using Pulicaria glutinosa extract (PGE as reducing and stabilizing agent. The phytomolecules present in the plant extract (PE not only facilitated the reduction of PdCl2, but also helped to stabilize the surface of PG-HRG-Pd nanocatalyst, which significantly enhanced the dispersibility of nanocatalyst in water. The identification of PG-HRG-Pd was established by various spectroscopic and microscopic techniques, including, high-resolution transmission electron microscopy (HRTEM, X-ray diffraction (XRD, ultraviolet–visible spectroscopy (UV-Vis, Fourier transform infrared spectroscopy (FT-IR, and Raman spectroscopy. The as-prepared PG-HRG-Pd nanocatalyst demonstrated excellent catalytic activity towards the Suzuki-Miyaura cross coupling reactions under aqueous, ligand free, and aerobic conditions. Apart from this the reusability of the catalyst was also evaluated and the catalyst yielded excellent results upon reuse for several times with marginal loss of its catalytic performance. Therefore, the method developed for the green

  11. Irradiation Testing of Ultrasonic Transducers

    International Nuclear Information System (INIS)

    Daw, J.; Rempe, J.; Palmer, J.; Tittmann, B.; Reinhardt, B.; Kohse, G.; Ramuhalli, P.; Montgomery, R.; Chien, H.T.; Villard, J.F.

    2013-06-01

    Ultrasonic technologies offer the potential for high accuracy and resolution in-pile measurement of numerous parameters, including geometry changes, temperature, crack initiation and growth, gas pressure and composition, and microstructural changes. Many Department of Energy-Office of Nuclear Energy (DOE-NE) programs are exploring the use of ultrasonic technologies to provide enhanced sensors for in-pile instrumentation during irradiation testing. For example, the ability of single, small diameter ultrasonic thermometers (UTs) to provide a temperature profile in candidate metallic and oxide fuel would provide much needed data for validating new fuel performance models. Other efforts include an ultrasonic technique to detect morphology changes (such as crack initiation and growth) and acoustic techniques to evaluate fission gas composition and pressure. These efforts are limited by the lack of existing knowledge of ultrasonic transducer material survivability under irradiation conditions. To address this need, the Pennsylvania State University (PSU) was awarded an Advanced Test Reactor National Scientific User Facility (ATR NSUF) project to evaluate promising magnetostrictive and piezoelectric transducer performance in the Massachusetts Institute of Technology Research Reactor (MITR) up to a fast fluence of at least 10 21 n/cm 2 (E> 0.1 MeV). This test will be an instrumented lead test; and real-time transducer performance data will be collected along with temperature and neutron and gamma flux data. By characterizing magnetostrictive and piezoelectric transducer survivability during irradiation, test results will enable the development of novel radiation tolerant ultrasonic sensors for use in Material and Test Reactors (MTRs). The current work bridges the gap between proven out-of-pile ultrasonic techniques and in-pile deployment of ultrasonic sensors by acquiring the data necessary to demonstrate the performance of ultrasonic transducers. (authors)

  12. Acetylcholinesterase immobilized capillary reactors coupled to protein coated magnetic beads: A new tool for plant extract ligand screening

    Science.gov (United States)

    Vanzolini, Kenia Lourenço; Jiang, Zhengjin; Zhang, Xiaoqi; Vieira, Lucas Campos Curcino; Corrêa, Arlene Gonçalvez; Cardoso, Carmen Lucia; Cass, Quezia Bezerra; Moaddel, Ruin

    2013-01-01

    The use of immobilized capillary enzyme reactors (ICERs) and enzymes coated to magnetic beads ((NT or CT)-MB) for ligand screening has been adopted as a new technique of high throughput screening (HTS). In this work the selected target was the enzyme acetylcholinesterase (AChE), which acts on the central nervous system and is a validated target for the treatment of Alzheimer’s disease, as well as for new insecticides. A new approach for the screening of plant extracts was developed based on the ligand fishing experiments and zonal chromatography. For that, the magnetic beads were used for the ligand fishing experiments and capillary bioreactors for the activity assays. The latter was employed also under non-linear conditions to determine the affinity constants of known ligands, for the first time, as well as for the active fished ligand. PMID:24148457

  13. Review of piezoelectric micromachined ultrasonic transducers and their applications

    International Nuclear Information System (INIS)

    Jung, Joontaek; Lee, Wonjun; Kang, Woojin; Shin, Eunjung; Choi, Hongsoo; Ryu, Jungho

    2017-01-01

    In recent decades, micromachined ultrasonic transducers (MUTs) have been investigated as an alternative to conventional piezocomposite ultrasonic transducers, primarily due to the advantages that microelectromechanical systems provide. Miniaturized ultrasonic systems require ultrasonic transducers integrated with complementary metal-oxide-semiconductor circuits. Hence, piezoelectric MUTs (pMUTs) and capacitive MUTs (cMUTs) have been developed as the most favorable solutions. This paper reviews the basic equations to understand the characteristics of thin-film-based piezoelectric devices and presents recent research on pMUTs, including current approaches and limitations. Methods to improve the coupling coefficient of pMUTs are also investigated, such as device structure, materials, and fabrication techniques. The device structure improvements include multielectrode pMUTs, partially clamped boundary conditions, and 3D pMUTs (curved and domed types), where the latter can provide an electromechanical coupling coefficient of up to 45%. The piezoelectric coefficient ( e 31 ) can be increased by controlling the crystal texture (seed layer of γ -Al 2 O 3 ), using single-crystal (PMN-PT) materials, or control of residual stresses (using SiO 2 layer). Arrays of pMUTs can be implemented for various applications including intravascular ultrasound, fingerprint sensors, rangefinders in air, and wireless power supply systems. pMUTs are expected to be an ideal solution for applications such as mobile biometric security (fingerprint sensors) and rangefinders due to their superior power efficiency and compact size. (topical review)

  14. Review of piezoelectric micromachined ultrasonic transducers and their applications

    Science.gov (United States)

    Jung, Joontaek; Lee, Wonjun; Kang, Woojin; Shin, Eunjung; Ryu, Jungho; Choi, Hongsoo

    2017-11-01

    In recent decades, micromachined ultrasonic transducers (MUTs) have been investigated as an alternative to conventional piezocomposite ultrasonic transducers, primarily due to the advantages that microelectromechanical systems provide. Miniaturized ultrasonic systems require ultrasonic transducers integrated with complementary metal-oxide-semiconductor circuits. Hence, piezoelectric MUTs (pMUTs) and capacitive MUTs (cMUTs) have been developed as the most favorable solutions. This paper reviews the basic equations to understand the characteristics of thin-film-based piezoelectric devices and presents recent research on pMUTs, including current approaches and limitations. Methods to improve the coupling coefficient of pMUTs are also investigated, such as device structure, materials, and fabrication techniques. The device structure improvements include multielectrode pMUTs, partially clamped boundary conditions, and 3D pMUTs (curved and domed types), where the latter can provide an electromechanical coupling coefficient of up to 45%. The piezoelectric coefficient (e 31) can be increased by controlling the crystal texture (seed layer of γ-Al2O3), using single-crystal (PMN-PT) materials, or control of residual stresses (using SiO2 layer). Arrays of pMUTs can be implemented for various applications including intravascular ultrasound, fingerprint sensors, rangefinders in air, and wireless power supply systems. pMUTs are expected to be an ideal solution for applications such as mobile biometric security (fingerprint sensors) and rangefinders due to their superior power efficiency and compact size.

  15. Determination of trace uranium by resonance fluorescence method coupled with photo-catalytic technology and dual cloud point extraction.

    Science.gov (United States)

    Li, Jiekang; Li, Guirong; Han, Qian

    2016-12-05

    In this paper, two kinds of salophens (Sal) with different solubilities, Sal1 and Sal2, have been respectively synthesized, and they all can combine with uranyl to form stable complexes: [UO2(2+)-Sal1] and [UO2(2+)-Sal2]. Among them, [UO2(2+)-Sal1] was used as ligand to extract uranium in complex samples by dual cloud point extraction (dCPE), and [UO2(2+)-Sal2] was used as catalyst for the determination of uranium by photocatalytic resonance fluorescence (RF) method. The photocatalytic characteristic of [UO2(2+)-Sal2] on the oxidized pyronine Y (PRY) by potassium bromate which leads to the decrease of RF intensity of PRY were studied. The reduced value of RF intensity of reaction system (ΔF) is in proportional to the concentration of uranium (c), and a novel photo-catalytic RF method was developed for the determination of trace uranium (VI) after dCPE. The combination of photo-catalytic RF techniques and dCPE procedure endows the presented methods with enhanced sensitivity and selectivity. Under optimal conditions, the linear calibration curves range for 0.067 to 6.57ngmL(-1), the linear regression equation was ΔF=438.0 c (ngmL(-1))+175.6 with the correlation coefficient r=0.9981. The limit of detection was 0.066ngmL(-1). The proposed method was successfully applied for the separation and determination of uranium in real samples with the recoveries of 95.0-103.5%. The mechanisms of the indicator reaction and dCPE are discussed. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Pulsed ultrasonic stir welding method

    Science.gov (United States)

    Ding, R. Jeffrey (Inventor)

    2013-01-01

    A method of performing ultrasonic stir welding uses a welding head assembly to include a plate and a rod passing through the plate. The rod is rotatable about a longitudinal axis thereof. In the method, the rod is rotated about its longitudinal axis during a welding operation. During the welding operation, a series of on-off ultrasonic pulses are applied to the rod such that they propagate parallel to the rod's longitudinal axis. At least a pulse rate associated with the on-off ultrasonic pulses is controlled.

  17. Fundamentals of ultrasonic phased arrays

    CERN Document Server

    Schmerr, Lester W

    2014-01-01

    This book describes in detail the physical and mathematical foundations of ultrasonic phased array measurements.?The book uses linear systems theory to develop a comprehensive model of the signals and images that can be formed with phased arrays. Engineers working in the field of ultrasonic nondestructive evaluation (NDE) will find in this approach a wealth of information on how to design, optimize and interpret ultrasonic inspections with phased arrays. The fundamentals and models described in the book will also be of significant interest to other fields, including the medical ultrasound and

  18. A multi-purpose ultrasonic streaming mixer for integrated magnetic bead ELISAs

    International Nuclear Information System (INIS)

    Brandhoff, Lukas; Lang, Walter; Vellekoop, Michael J; Zirath, Helene; Peham, Johannes; Wiesinger-Mayr, Herbert; Salas, Mariugenia; Haller, Anna; Spittler, Andreas; Schnetz, Guntram

    2015-01-01

    We present an ultrasonic streaming mixer for disposable and on-chip magnetic bead ELISAs. The ultrasonic transducer is placed at system-level to keep cost per chip as low as possible, and is coupled to the chip by means of a solid ultrasonic horn. The system provides mixing of liquids, as well as dispersion of the superparamagnetic beads in the ELISA. Additionally it can be used clean the chamber surface from nonspecifically bound proteins during the washing steps in the ELISA protocol. Using our system the time for the ELISA protocol has been greatly reduced down to 30 min. (paper)

  19. Facile synthesis and characterisation of AlNs using Protein Rich Solution extracted from sewage sludge and its application for ultrasonic assisted dye adsorption: Isotherms, kinetics, mechanism and RSM design.

    Science.gov (United States)

    Mary Ealias, Anu; Saravanakumar, M P

    2018-01-15

    Protein Rich Solution (PRS) was prepared from the sewage sludge with ultrasonic assistance. With PRS, aluminium based nanosheet like materials (AlNs) were synthesised for the ultrasonic removal of Congo Red (CR) and Crystal Violet (CV) dyes. PRS was characterised by UV, EEM and NMR spectral analysis. AlNs were characterised by FTIR, XRD, TGA, BET, SEM, AFM, TEM and XPS analysis. The point of zero charge of AlNs was found to be 5.4. The BET analysis ensured that the average pore diameter and total pore volume of AlNs as 8.464 nm and 0.11417 cc/g respectively. The efficacy of AlNs for the removal of toxic dyes was tested by performing Response surface methodology (RSM) designed experiments. The effect of sonication time, dosage and initial concentration on dye removal was studied at an optimised pH value. Langmuir, Freundlich and Temkin isotherm models were examined. The maximum adsorption capacity was found to be 121.951 and 105.263 mg/g for CR and CV respectively. The kinetic models like pseudo-first order, pseudo-second order, Elovich and intra-particle diffusion were examined to understand the mechanism behind it. The results revealed that the use of ultrasonication enhanced the mass transfer. The experimental studies on the influence of ultrasound power indicated a positive relation with the removal efficiency. The results of thermodynamic study revealed that the process was spontaneous and exothermic for both the dyes. The increase in ionic strength increased the removal efficiency for both CR and CV. RSM predicted the optimum adsorbent dosages as 0.16 g for 50 mg/L of CR and 0.12 g for 100 mg/L of CV dye solutions. The values of half-life and fractional adsorption for both CR and CV suggested that the low cost AlNs has high potential to remove the toxic industrial dyes. Copyright © 2017 Elsevier Ltd. All rights reserved.

  20. Ion imprinted activated carbon solid-phase extraction coupled to flame atomic absorption spectrometry for selective determination of lead ions in environmental samples

    International Nuclear Information System (INIS)

    Naraghi, Kiyana; Panahi, Homayon Ahmad; Hassani, Amir Hesam; Moniri, Elham

    2014-01-01

    A simple lead ion imprinted sorbent was synthesized by coupling activated carbon with a known metal chelating compound, iminodiacetic acid. The ion imprinted sorbent has been characterized using Fourier transform infrared spectroscopy, elemental analysis and thermogravimetric analysis and subjected for the extraction and determination of trace Pb(II) in environmental water samples. The optimum pH value for sorption of the lead ion was 6.5. The sorption capacity of lead imprinted sorbent was 42.2 mg g"−"1. The chelating imprinted sorbent can be reused for five cycles of sorption-desorption without any significant change in sorption capacity. Compared with non-imprinted polymer particles, the lead ion imprinted sorbent showed high adsorption capacity, significant selectivity, good site accessibility for Pb(II). The equilibrium adsorption data of Pb(II) by modified resin were analyzed by Langmuir, Freundlich, Temkin and Redlich-Peterson models

  1. Synthesis of palladium nanoparticles with leaf extract of Chrysophyllum cainito (Star apple) and their applications as efficient catalyst for C-C coupling and reduction reactions

    Science.gov (United States)

    Majumdar, Rakhi; Tantayanon, Supawan; Bag, Braja Gopal

    2017-10-01

    A simple green chemical method for the one-step synthesis of palladium nanoparticles (PdNPs) has been described by reducing palladium (II) chloride with the leaf extract of Chrysophyllum cainito in aqueous medium. The synthesis of the palladium nanoparticles completed within 2-3 h at room temperature, whereas on heat treatment (70-80 °C), the synthesis of colloidal PdNPs completed almost instantly. The stabilized PdNPs have been characterized in detail by spectroscopic, electron microscopic and light scattering measurements. The synthesized PdNPs have been utilized as a green catalyst for C-C coupling reactions under aerobic and phosphine-free conditions in aqueous medium. In addition, the synthesized PdNPs have also been utilized as a catalyst for a very efficient sodium borohydride reduction of 3- and 4-nitrophenols. The synthesized PdNPs can retain their catalytic activity for several months.

  2. Ion imprinted activated carbon solid-phase extraction coupled to flame atomic absorption spectrometry for selective determination of lead ions in environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Naraghi, Kiyana; Panahi, Homayon Ahmad; Hassani, Amir Hesam [Islamic Azad University, Tehran (Korea, Republic of); Moniri, Elham [Islamic Azad University, Varamin (Iran, Islamic Republic of)

    2014-10-15

    A simple lead ion imprinted sorbent was synthesized by coupling activated carbon with a known metal chelating compound, iminodiacetic acid. The ion imprinted sorbent has been characterized using Fourier transform infrared spectroscopy, elemental analysis and thermogravimetric analysis and subjected for the extraction and determination of trace Pb(II) in environmental water samples. The optimum pH value for sorption of the lead ion was 6.5. The sorption capacity of lead imprinted sorbent was 42.2 mg g{sup −1}. The chelating imprinted sorbent can be reused for five cycles of sorption-desorption without any significant change in sorption capacity. Compared with non-imprinted polymer particles, the lead ion imprinted sorbent showed high adsorption capacity, significant selectivity, good site accessibility for Pb(II). The equilibrium adsorption data of Pb(II) by modified resin were analyzed by Langmuir, Freundlich, Temkin and Redlich-Peterson models.

  3. Rapid Determination of Plutonium Isotopes in Environmental Samples Using Sequential Injection Extraction Chromatography and Detection by Inductively Coupled Plasma Mass Spectrometry

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per

    2009-01-01

    This article presents an automated method for the rapid determination of 239Pu and 240Pu in various environmental samples. The analytical method involves the in-line separation of Pu isotopes using extraction chromatography (TEVA) implemented in a sequential injection (SI) network followed...... by detection of isolated analytes with inductively coupled plasma mass spectrometry (ICP-MS). The method has been devised for the determination of Pu isotopes at environmentally relevant concentrations, whereby it has been successfully applied to the analyses of large volumes/amounts of samples, for example......, 100−200 g of soil and sediment, 20 g of seaweed, and 200 L of seawater following analyte preconcentration. The investigation of the separation capability of the assembled SI system revealed that up to 200 g of soil or sediment can be treated using a column containing about 0.70 g of TEVA resin...

  4. Computer automation of ultrasonic testing. [inspection of ultrasonic welding

    Science.gov (United States)

    Yee, B. G. W.; Kerlin, E. E.; Gardner, A. H.; Dunmyer, D.; Wells, T. G.; Robinson, A. R.; Kunselman, J. S.; Walker, T. C.

    1974-01-01

    Report describes a prototype computer-automated ultrasonic system developed for the inspection of weldments. This system can be operated in three modes: manual, automatic, and computer-controlled. In the computer-controlled mode, the system will automatically acquire, process, analyze, store, and display ultrasonic inspection data in real-time. Flaw size (in cross-section), location (depth), and type (porosity-like or crack-like) can be automatically discerned and displayed. The results and pertinent parameters are recorded.

  5. Cement-based materials' characterization using ultrasonic attenuation

    Science.gov (United States)

    Punurai, Wonsiri

    The quantitative nondestructive evaluation (NDE) of cement-based materials is a critical area of research that is leading to advances in the health monitoring and condition assessment of the civil infrastructure. Ultrasonic NDE has been implemented with varying levels of success to characterize cement-based materials with complex microstructure and damage. A major issue with the application of ultrasonic techniques to characterize cement-based materials is their inherent inhomogeneity at multiple length scales. Ultrasonic waves propagating in these materials exhibit a high degree of attenuation losses, making quantitative interpretations difficult. Physically, these attenuation losses are a combination of internal friction in a viscoelastic material (ultrasonic absorption), and the scattering losses due to the material heterogeneity. The objective of this research is to use ultrasonic attenuation to characterize the microstructure of heterogeneous cement-based materials. The study considers a real, but simplified cement-based material, cement paste---a common bonding matrix of all cement-based composites. Cement paste consists of Portland cement and water but does not include aggregates. First, this research presents the findings of a theoretical study that uses a set of existing acoustics models to quantify the scattered ultrasonic wavefield from a known distribution of entrained air voids. These attenuation results are then coupled with experimental measurements to develop an inversion procedure that directly predicts the size and volume fraction of entrained air voids in a cement paste specimen. Optical studies verify the accuracy of the proposed inversion scheme. These results demonstrate the effectiveness of using attenuation to measure the average size, volume fraction of entrained air voids and the existence of additional larger entrapped air voids in hardened cement paste. Finally, coherent and diffuse ultrasonic waves are used to develop a direct

  6. High-Efficiency On-Line Solid-Phase Extraction Coupling to 15-150 um I.D. Column Liquid Chromatography for Proteomic Analysis

    International Nuclear Information System (INIS)

    Shen, Yufeng; Moore, Ronald J.; Zhao, Rui; Blonder, Josip; Auberry, Deanna L.; Masselon, Christophe D.; Pasa Tolic, Ljiljana; Hixson, Kim K.; Auberry, Kenneth J.; Smith, Richard D.

    2003-01-01

    Flexible manipulation of various properties of proteomic samples is important for proteomic analyses, but it has been little explored for newly developed approaches based on liquid chromatography (LC) in combination with mass spectrometry (MS). With miniaturization of the LC column inner diameter dimensions (required for improving the analysis sensitivity), this issue becomes more challenging due to the small flow rates and the increasing effects of extra column volume on the separation quality and its use for resolving complex proteomic mixtures. In this study, we used commercial switching valves (150-mm channels) to implement the on-line coupling of capillary LC columns with relatively large solid phase extraction (SPE) columns operated at 10,000 psi. With optimized column connections, switching modes, and SPE column dimensions, high-efficiency on-line SPE-capillary and nanoscale LC separations were obtained with peak capacities of ∼1000 for capillaries having inner diameters between 15 to 150 mm. The on-line coupled SPE columns increased the sample processing capabilities by ∼400-fold for sample solution volume and ∼10-fold for sample mass. The proteomic applications of this on-line SPE-capillary LC system were evaluated for analysis of both soluble and membrane protein tryptic digests. Used with an ion trap tandem MS we could typically identify 1100-1500 peptides for analyses in a single 5-hour run. Peptides extracted on the SPE column and eluted from the LC column covered a hydrophilicity/hydrophobicity range that include an estimated ∼98% of all the tryptic peptides. The present implementation also facilitates automation and enables use of both disposable SPE columns and electrospray emitters, providing a robust basis for routine proteomic analyses.

  7. A solid-phase extraction procedure coupled to 1H NMR, with chemometric analysis, to seek reliable markers of the botanical origin of honey

    International Nuclear Information System (INIS)

    Beretta, Giangiacomo; Caneva, Enrico; Regazzoni, Luca; Bakhtyari, Nazanin Golbamaki; Maffei Facino, Roberto

    2008-01-01

    The aim of this work was to establish an analytical method for identifying the botanical origin of honey, as an alternative to conventional melissopalynological, organoleptic and instrumental methods (gas-chromatography coupled to mass spectrometry (GC-MS), high-performance liquid chromatography HPLC). The procedure is based on the 1 H nuclear magnetic resonance (NMR) profile coupled, when necessary, with electrospray ionisation-mass spectrometry (ESI-MS) and two-dimensional NMR analyses of solid-phase extraction (SPE)-purified honey samples, followed by chemometric analyses. Extracts of 44 commercial Italian honeys from 20 different botanical sources were analyzed. Honeydew, chestnut and linden honeys showed constant, specific, well-resolved resonances, suitable for use as markers of origin. Honeydew honey contained the typical resonances of an aliphatic component, very likely deriving from the plant phloem sap or excreted into it by sap-sucking aphids. Chestnut honey contained the typical signals of kynurenic acid and some structurally related metabolite. In linden honey the 1 H NMR profile gave strong signals attributable to the mono-terpene derivative cyclohexa-1,3-diene-1-carboxylic acid (CDCA) and to its 1-O-β-gentiobiosyl ester (CDCA-GBE). These markers were not detectable in the other honeys, except for the less common nectar honey from rosa mosqueta. We compared and analyzed the data by multivariate techniques. Principal component analysis found different clusters of honeys based on the presence of these specific markers. The results, although obviously only preliminary, suggest that the 1 H NMR profile (with HPLC-MS analysis when necessary) can be used as a reference framework for identifying the botanical origin of honey

  8. A solid-phase extraction procedure coupled to {sup 1}H NMR, with chemometric analysis, to seek reliable markers of the botanical origin of honey

    Energy Technology Data Exchange (ETDEWEB)

    Beretta, Giangiacomo [Istituto di Chimica Farmaceutica e Tossicologica ' Pietro Pratesi' , Faculty of Pharmacy, University of Milan, via Mangiagalli 25, 20133 Milan (Italy)], E-mail: giangiacomo.beretta@unimi.it; Caneva, Enrico [Ciga - Centro Interdipartimentale Grandi Apparecchiature, University of Milan, via Golgi 19, 20133 Milan (Italy); Regazzoni, Luca; Bakhtyari, Nazanin Golbamaki; Maffei Facino, Roberto [Istituto di Chimica Farmaceutica e Tossicologica ' Pietro Pratesi' , Faculty of Pharmacy, University of Milan, via Mangiagalli 25, 20133 Milan (Italy)

    2008-07-14

    The aim of this work was to establish an analytical method for identifying the botanical origin of honey, as an alternative to conventional melissopalynological, organoleptic and instrumental methods (gas-chromatography coupled to mass spectrometry (GC-MS), high-performance liquid chromatography HPLC). The procedure is based on the {sup 1}H nuclear magnetic resonance (NMR) profile coupled, when necessary, with electrospray ionisation-mass spectrometry (ESI-MS) and two-dimensional NMR analyses of solid-phase extraction (SPE)-purified honey samples, followed by chemometric analyses. Extracts of 44 commercial Italian honeys from 20 different botanical sources were analyzed. Honeydew, chestnut and linden honeys showed constant, specific, well-resolved resonances, suitable for use as markers of origin. Honeydew honey contained the typical resonances of an aliphatic component, very likely deriving from the plant phloem sap or excreted into it by sap-sucking aphids. Chestnut honey contained the typical signals of kynurenic acid and some structurally related metabolite. In linden honey the {sup 1}H NMR profile gave strong signals attributable to the mono-terpene derivative cyclohexa-1,3-diene-1-carboxylic acid (CDCA) and to its 1-O-{beta}-gentiobiosyl ester (CDCA-GBE). These markers were not detectable in the other honeys, except for the less common nectar honey from rosa mosqueta. We compared and analyzed the data by multivariate techniques. Principal component analysis found different clusters of honeys based on the presence of these specific markers. The results, although obviously only preliminary, suggest that the {sup 1}H NMR profile (with HPLC-MS analysis when necessary) can be used as a reference framework for identifying the botanical origin of honey.

  9. Ultrasonic/Sonic Rotary-Hammer Drills

    Science.gov (United States)

    Badescu, Mircea; Sherrit, Stewart; Bar-Cohen, Yoseph; Bao, Xiaoqi; Kassab, Steve

    2010-01-01

    Ultrasonic/sonic rotary-hammer drill (USRoHD) is a recent addition to the collection of apparatuses based on ultrasonic/sonic drill corer (USDC). As described below, the USRoHD has several features, not present in a basic USDC, that increase efficiency and provide some redundancy against partial failure. USDCs and related apparatuses were conceived for boring into, and/or acquiring samples of, rock or other hard, brittle materials of geological interest. They have been described in numerous previous NASA Tech Briefs articles. To recapitulate: A USDC can be characterized as a lightweight, lowpower, piezoelectrically driven jackhammer in which ultrasonic and sonic vibrations are generated and coupled to a tool bit. A basic USDC includes a piezoelectric stack, an ultrasonic transducer horn connected to the stack, a free mass ( free in the sense that it can bounce axially a short distance between hard stops on the horn and the bit), and a tool bit. The piezoelectric stack creates ultrasonic vibrations that are mechanically amplified by the horn. The bouncing of the free mass between the hard stops generates the sonic vibrations. The combination of ultrasonic and sonic vibrations gives rise to a hammering action (and a resulting chiseling action at the tip of the tool bit) that is more effective for drilling than is the microhammering action of ultrasonic vibrations alone. The hammering and chiseling actions are so effective that unlike in conventional twist drilling, little applied axial force is needed to make the apparatus advance into the material of interest. There are numerous potential applications for USDCs and related apparatuses in geological exploration on Earth and on remote planets. In early USDC experiments, it was observed that accumulation of cuttings in a drilled hole causes the rate of penetration of the USDC to decrease steeply with depth, and that the rate of penetration can be increased by removing the cuttings. The USRoHD concept provides for

  10. High resolution ultrasonic densitometer

    International Nuclear Information System (INIS)

    Dress, W.B.

    1983-01-01

    The velocity of torsional stress pulses in an ultrasonic waveguide of non-circular cross section is affected by the temperature and density of the surrounding medium. Measurement of the transit times of acoustic echoes from the ends of a sensor section are interpreted as level, density, and temperature of the fluid environment surrounding that section. This paper examines methods of making these measurements to obtain high resolution, temperature-corrected absolute and relative density and level determinations of the fluid. Possible applications include on-line process monitoring, a hand-held density probe for battery charge state indication, and precise inventory control for such diverse fluids as uranium salt solutions in accountability storage and gasoline in service station storage tanks

  11. Ultrasonic detection of solid phase mass flow ratio of pneumatic conveying fly ash

    Science.gov (United States)

    Duan, Guang Bin; Pan, Hong Li; Wang, Yong; Liu, Zong Ming

    2014-04-01

    In this paper, ultrasonic attenuation detection and weight balance are adopted to evaluate the solid mass ratio in this paper. Fly ash is transported on the up extraction fluidization pneumatic conveying workbench. In the ultrasonic test. McClements model and Bouguer-Lambert-Beer law model were applied to formulate the ultrasonic attenuation properties of gas-solid flow, which can give the solid mass ratio. While in the method of weigh balance, the averaged mass addition per second can reveal the solids mass flow ratio. By contrast these two solid phase mass ratio detection methods, we can know, the relative error is less.

  12. Simultaneous DPV determination of morphine and codeine using dsDNA modified screen printed electrode strips coupled with electromembrane extraction

    Directory of Open Access Journals (Sweden)

    Rouhollah Feizbakhsh

    2016-01-01

    Full Text Available In this work a sensitive electrochemical sensor for simultaneous determination of morphine and codeine constructed by application of disposable screen printed carbon electrode strips (SPCE modified by double strand (ds calf thymus DNA. According to the results of the modified SPCE strips and experimented parameters, we observed a considerable shift between potentials of morphine and codeine current peaks. Related to these observed shifts, we studied on the effect of the concentration of modifier and pH value on the anodic oxidation pattern of morphine and codeine in the case of optimize the method to get better signals with maximum potential distance. Also to boosting the LODs of this electroanalytical method coupled with an electro-membrane preconcentration (EME step. The calibration curve which was plotted by the variation of differential pulse voltammetry (DPV currents as a function of different morphine and codeine concentration were linear within the range of 0.7– 40 µM and 2.3- 40 µM for morphine and codeine respectively. Also the limits of detection were 0.07 µM and 0.23 µM, respectively. Finally, the proposed method was able to determine morphine and codeine simultaneously and effectively in urinary real samples

  13. Ultrasonic imaging in concrete

    International Nuclear Information System (INIS)

    Ribay, G.; Paris, O.; Rambach, J.M.

    2009-01-01

    The third and final protection barrier confining nuclear reactors is usually a concrete containment structure. Monitoring the structural integrity of these barriers is critical in ensuring the safety of nuclear power plants. The Institute for Radiological Protection and Nuclear Safety (IRSN) in France in collaboration with the French Atomic commission (CEA/LIST) has developed an ultrasonic phased-array technique capable of inspecting thick concrete walls. The non-destructive method is dedicated to detect cracks and bulk defects. Given the thickness of the structure (1.2 m) undergoing inspection and the heterogeneity of the concrete, the optimal frequency lies in the 50-300 kHz range. At these frequencies, the ultrasonic beam profiles are widespread (non-directive) with poor signal-to-noise ratio. Previous studies have shown the potential of using phased-array techniques (i.e., beam focusing and beam steering) in order to improve detection resolution and sizing accuracy. In this paper we present experimental studies performed with array up to 16 transducers working at 200 kHz. Experiments are carried out on representative concrete blocks containing artificial defects. One is a reinforced mock-up representative of the first reinforcing mesh of wall containment. Experimental results show that in spite of the reinforcement, artificial defects deep as half a meter can be detected. Reconstructed images resulting from phased array acquisitions on an artificial crack embedded in a concrete block are also presented and discussed. The presented method allows detecting oriented defects in concrete with improved signal to noise ratio and sensibility. A simulation model of the interaction of ultrasound with a heterogeneous medium like concrete is briefly commented. (authors)

  14. Monitoring sea lamprey pheromones and their degradation using rapid stream-side extraction coupled with UPLC-MS/MS

    Science.gov (United States)

    Wang, Huiyong; Johnson, Nicholas; Bernardy, Jeffrey; Hubert, Terry; Li, Weiming

    2013-01-01

    Pheromones guide adult sea lamprey (Petromyzon marinus) to suitable spawning streams and mates, and therefore, when quantified, can be used to assess population size and guide management. Here, we present an efficient sample preparation method where 100 mL of river water was spiked with deuterated pheromone as an internal standard and underwent rapid field-based SPE and elution in the field. The combination of field extraction with laboratory UPLC-MS/MS reduced the sample consumption from 1 to 0.1 L, decreased the sample process time from more than 1 h to 10 min, and increased the precision and accuracy. The sensitivity was improved more than one order of magnitude compared with the previous method. The influences of experimental conditions were assessed to optimize the separation and peak shapes. The analytical method has been validated by studies of stability, selectivity, precision, and linearity and by the determination of the limits of detection and quantification. The method was used to quantify pheromone concentration from five streams tributary to Lake Ontario and to estimate that the environmental half-life of 3kPZS is about 26 h.

  15. Determination of diethylstilbestrol in seawater by molecularly imprinted solid-phase extraction coupled with high-performance liquid chromatography.

    Science.gov (United States)

    He, Xiuping; Mei, Xiaoqi; Wang, Jiangtao; Lian, Ziru; Tan, Liju; Wu, Wei

    2016-01-15

    An effective and highly selective molecularly imprinted material was prepared by suspension polymerization for the isolation and pre-concentration of synthetic estrogen diethylstilbestrol (DES) in seawater. The obtained MIPMs were proved to have more uniform size and porous structure, with maximum adsorption capacity of 8.43 mg g(-1) almost two times more than NIPMs (4.43 mg g(-1)). The MIPMs showed no significant deterioration of the adsorption capacity after five rounds of regeneration. An off-line molecularly imprinted solid phase extraction (MISPE) method followed by HPLC-DAD was proposed for the detection of DES in seawater, and recoveries were satisfactorily higher than 77%. Four seawater samples in aquaculture area were analyzed and 0.61 ng mL(-1) DES was detected in one sample. The result demonstrated that this method can be used for the rapid separation and clean up of trace residual of DES in seawater. Copyright © 2015 Elsevier Ltd. All rights reserved.

  16. Dried Blood Spot Proteomics: Surface Extraction of Endogenous Proteins Coupled with Automated Sample Preparation and Mass Spectrometry Analysis

    Science.gov (United States)

    Martin, Nicholas J.; Bunch, Josephine; Cooper, Helen J.

    2013-08-01

    Dried blood spots offer many advantages as a sample format including ease and safety of transport and handling. To date, the majority of mass spectrometry analyses of dried blood spots have focused on small molecules or hemoglobin. However, dried blood spots are a potentially rich source of protein biomarkers, an area that has been overlooked. To address this issue, we have applied an untargeted bottom-up proteomics approach to the analysis of dried blood spots. We present an automated and integrated method for extraction of endogenous proteins from the surface of dried blood spots and sample preparation via trypsin digestion by use of the Advion Biosciences Triversa Nanomate robotic platform. Liquid chromatography tandem mass spectrometry of the resulting digests enabled identification of 120 proteins from a single dried blood spot. The proteins identified cross a concentration range of four orders of magnitude. The method is evaluated and the results discussed in terms of the proteins identified and their potential use as biomarkers in screening programs.

  17. Case studies in ultrasonic testing

    International Nuclear Information System (INIS)

    Prasad, V.; Satheesh, C.; Varde, P.V.

    2015-01-01

    Ultrasonic testing is widely used Non Destructive Testing (NDT) method and forms the essential part of In-service inspection programme of nuclear reactors. Main application of ultrasonic testing is for volumetric scanning of weld joints followed by thickness gauging of pipelines and pressure vessels. Research reactor Dhruva has completed the first In Service Inspection programme in which about 325 weld joints have been volumetrically scanned, in addition to thickness gauging of 300 meters of pipe lines of various sizes and about 24 nos of pressure vessels. Ultrasonic testing is also used for level measurements, distance measurements and cleaning and decontamination of tools. Two case studies are brought out in this paper in which ultrasonic testing is used successfully for identification of butterfly valve opening status and extent of choking in pipe lines in Dhruva reactor systems

  18. Ultrasonic Technology in Duress Alarms.

    Science.gov (United States)

    Lee, Martha A.

    2000-01-01

    Provides the pros and cons of the most commonly used technologies in personal duress alarm systems in the school environment. Discussed are radio frequency devices, infrared systems, and ultrasonic technology. (GR)

  19. Ultrasonic extensometer measures bolt preload

    Science.gov (United States)

    Daniels, C. M., Jr.

    1978-01-01

    Extensometer using ultrasonic pulse reflections to measure elongations in tightened belts and studs is much more accurate than conventional torque wrenches in application of specified preload to bolts and other threaded fasteners.

  20. Multi-residue determination of the sorption of illicit drugs and pharmaceuticals to wastewater suspended particulate matter using pressurised liquid extraction, solid phase extraction and liquid chromatography coupled with tandem mass spectrometry.

    Science.gov (United States)

    Baker, David R; Kasprzyk-Hordern, Barbara

    2011-11-04

    Presented is the first comprehensive study of drugs of abuse on suspended particulate matter (SPM) in wastewater. Analysis of SPM is crucial to prevent the under-reporting of the levels of analyte that may be present in wastewater. Analytical methods to date analyse the aqueous part of wastewater samples only, removing SPM through the use of filtration or centrifugation. The development of an analytical method to determine 60 compounds on SPM using a combination of pressurised liquid extraction, solid phase extraction and liquid chromatography coupled with tandem mass spectrometry (PLE-SPE-LC-MS/MS) is reported. The range of compounds monitored included stimulants, opioid and morphine derivatives, benzodiazepines, antidepressants, dissociative anaesthetics, drug precursors, and their metabolites. The method was successfully validated (parameters studied: linearity and range, recovery, accuracy, reproducibility, repeatability, matrix effects, and limits of detection and quantification). The developed methodology was applied to SPM samples collected at three wastewater treatment plants in the UK. The average proportion of analyte on SPM as opposed to in the aqueous phase was 10% with regard to methadone, EDDP, EMDP, BZP, fentanyl, nortramadol, norpropoxyphene, sildenafil and all antidepressants (dosulepin, amitriptyline, nortriptyline, fluoxetine and norfluoxetine). Consequently, the lack of SPM analysis in wastewater sampling protocol could lead to the under-reporting of the measured concentration of some compounds. Copyright © 2011 Elsevier B.V. All rights reserved.

  1. Arsenic fractionation in agricultural soil using an automated three-step sequential extraction method coupled to hydride generation-atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Rosas-Castor, J.M. [Universidad Autónoma de Nuevo León, UANL, Facultad de Ciencias Químicas, Cd. Universitaria, San Nicolás de los Garza, Nuevo León, C.P. 66451 Nuevo León (Mexico); Group of Analytical Chemistry, Automation and Environment, University of Balearic Islands, Cra. Valldemossa km 7.5, 07122 Palma de Mallorca (Spain); Portugal, L.; Ferrer, L. [Group of Analytical Chemistry, Automation and Environment, University of Balearic Islands, Cra. Valldemossa km 7.5, 07122 Palma de Mallorca (Spain); Guzmán-Mar, J.L.; Hernández-Ramírez, A. [Universidad Autónoma de Nuevo León, UANL, Facultad de Ciencias Químicas, Cd. Universitaria, San Nicolás de los Garza, Nuevo León, C.P. 66451 Nuevo León (Mexico); Cerdà, V. [Group of Analytical Chemistry, Automation and Environment, University of Balearic Islands, Cra. Valldemossa km 7.5, 07122 Palma de Mallorca (Spain); Hinojosa-Reyes, L., E-mail: laura.hinojosary@uanl.edu.mx [Universidad Autónoma de Nuevo León, UANL, Facultad de Ciencias Químicas, Cd. Universitaria, San Nicolás de los Garza, Nuevo León, C.P. 66451 Nuevo León (Mexico)

    2015-05-18

    Highlights: • A fully automated flow-based modified-BCR extraction method was developed to evaluate the extractable As of soil. • The MSFIA–HG-AFS system included an UV photo-oxidation step for organic species degradation. • The accuracy and precision of the proposed method were found satisfactory. • The time analysis can be reduced up to eight times by using the proposed flow-based BCR method. • The labile As (F1 + F2) was <50% of total As in soil samples from As-contaminated-mining zones. - Abstract: A fully automated modified three-step BCR flow-through sequential extraction method was developed for the fractionation of the arsenic (As) content from agricultural soil based on a multi-syringe flow injection analysis (MSFIA) system coupled to hydride generation-atomic fluorescence spectrometry (HG-AFS). Critical parameters that affect the performance of the automated system were optimized by exploiting a multivariate approach using a Doehlert design. The validation of the flow-based modified-BCR method was carried out by comparison with the conventional BCR method. Thus, the total As content was determined in the following three fractions: fraction 1 (F1), the acid-soluble or interchangeable fraction; fraction 2 (F2), the reducible fraction; and fraction 3 (F3), the oxidizable fraction. The limits of detection (LOD) were 4.0, 3.4, and 23.6 μg L{sup −1} for F1, F2, and F3, respectively. A wide working concentration range was obtained for the analysis of each fraction, i.e., 0.013–0.800, 0.011–0.900 and 0.079–1.400 mg L{sup −1} for F1, F2, and F3, respectively. The precision of the automated MSFIA–HG-AFS system, expressed as the relative standard deviation (RSD), was evaluated for a 200 μg L{sup −1} As standard solution, and RSD values between 5 and 8% were achieved for the three BCR fractions. The new modified three-step BCR flow-based sequential extraction method was satisfactorily applied for arsenic fractionation in real agricultural

  2. Dual cloud point extraction coupled with hydrodynamic-electrokinetic two-step injection followed by micellar electrokinetic chromatography for simultaneous determination of trace phenolic estrogens in water samples.

    Science.gov (United States)

    Wen, Yingying; Li, Jinhua; Liu, Junshen; Lu, Wenhui; Ma, Jiping; Chen, Lingxin

    2013-07-01

    A dual cloud point extraction (dCPE) off-line enrichment procedure coupled with a hydrodynamic-electrokinetic two-step injection online enrichment technique was successfully developed for simultaneous preconcentration of trace phenolic estrogens (hexestrol, dienestrol, and diethylstilbestrol) in water samples followed by micellar electrokinetic chromatography (MEKC) analysis. Several parameters affecting the extraction and online injection conditions were optimized. Under optimal dCPE-two-step injection-MEKC conditions, detection limits of 7.9-8.9 ng/mL and good linearity in the range from 0.05 to 5 μg/mL with correlation coefficients R(2) ≥ 0.9990 were achieved. Satisfactory recoveries ranging from 83 to 108% were obtained with lake and tap water spiked at 0.1 and 0.5 μg/mL, respectively, with relative standard deviations (n = 6) of 1.3-3.1%. This method was demonstrated to be convenient, rapid, cost-effective, and environmentally benign, and could be used as an alternative to existing methods for analyzing trace residues of phenolic estrogens in water samples.

  3. Simultaneous spectrophotometric determination of trace copper, nickel, and cobalt ions in water samples using solid phase extraction coupled with partial least squares approaches

    Science.gov (United States)

    Guo, Yugao; Zhao, He; Han, Yelin; Liu, Xia; Guan, Shan; Zhang, Qingyin; Bian, Xihui

    2017-02-01

    A simultaneous spectrophotometric determination method for trace heavy metal ions based on solid-phase extraction coupled with partial least squares approaches was developed. In the proposed method, trace metal ions in aqueous samples were adsorbed by cation exchange fibers and desorbed by acidic solution from the fibers. After the ion preconcentration process, the enriched solution was detected by ultraviolet and visible spectrophotometer (UV-Vis). Then, the concentration of heavy metal ions were quantified by analyzing ultraviolet and visible spectrum with the help of partial least squares (PLS) approaches. Under the optimal conditions of operation time, flow rate and detection parameters, the overlapped absorption peaks of mixed ions were obtained. The experimental data showed that the concentration, which can be calculated through chemometrics method, of each metal ion increased significantly. The heavy metal ions can be enriched more than 80-fold. The limits of detection (LOD) for the target analytes of copper ions (Cu2 +), cobalt ions (Co2 +) and nickel ions (Ni2 +) mixture was 0.10 μg L- 1, 0.15 μg L- 1 and 0.13 μg L- 1, respectively. The relative standard deviations (RSD) were less than 5%. The performance of the solid-phase extraction can enrich the ions efficiently and the combined method of spectrophotometric detection and PLS can evaluate the ions concentration accurately. The work proposed here is an interesting and promising attempt for the trace ions determination in water samples and will have much more applied field.

  4. Determination of steroid hormones in fish tissues by microwave-assisted extraction coupled to ultra-high performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Guedes-Alonso, Rayco; Sosa-Ferrera, Zoraida; Santana-Rodríguez, José Juan

    2017-12-15

    Steroid hormones produce adverse effects on biota as well as bioaccumulation in fish and seafood, making it necessary to develop methodologies to evaluate these compounds in samples related to the food chain. This work presents an analytical method for evaluating 15 steroid hormones in fish tissue. It is based on microwave-assisted extraction and solid-phase extraction coupled to ultra-high-performance liquid chromatography tandem mass spectrometry (MAE-SPE-UHPLC-MS/MS). The proposed method shows appropriate detection limits (0.14-49.0ngg -1 ), recoveries in the range of 50% and good repeatability. After optimization, the method was applied to different tissues from two small fishes of the Canary Islands that constitute an important level of the food web (Boops boops and Sphoeroides marmoratus) and were exposed to the outfall of the Las Palmas de Gran Canaria wastewater treatment plant. The concentrations of eight detected compounds ranged from below the quantification limits to 3.95μgg -1 . Copyright © 2017 Elsevier Ltd. All rights reserved.

  5. Selective enrichment and determination of monoamine neurotransmitters by CU(II) immobilized magnetic solid phase extraction coupled with high-performance liquid chromatography-fluorescence detection.

    Science.gov (United States)

    He, Maofang; Wang, Chaozhan; Wei, Yinmao

    2016-01-15

    In this paper, iminodiacetic acid-Cu(II) functionalized Fe3O4@SiO2 magnetic nanoparticles were prepared and used as new adsorbents for magnetic solid phase extraction (MSPE) of six monoamine neurotransmitters (MNTs) from rabbit plasma. The selective enrichment of MNTs at pH 5.0 was motivated by the specific coordination interaction between amino groups of MNTs and the immobilized Cu(II). The employed weak acidic extraction condition avoided the oxidation of MNTs, and thus facilitated operation and ensured higher recoveries. Under optimal conditions, the recoveries of six MNTs from rabbit plasma were in the range of 83.9-109.4%, with RSD of 2.0-10.0%. When coupled the Cu(II) immobilized MSPE with high-performance liquid chromatography-fluorescence detection, the method exhibited relatively lower detection limits than the previously reported methods, and the method was successfully used to determine the endogenous MNTs in rabbit plasma. The proposed method has potential application for the determination of MNTs in biological samples. Also, the utilization of coordination interaction to improve the selectivity might open another way to selectively enrich small alkaloids from complex samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. [Determination of nitroaromatics and cyclo ketones in sea water' by gas chromatography coupled with activated carbon fiber solid-phase micro-extraction].

    Science.gov (United States)

    Ma, Hanna; Zhu, Mengya; Wang, Yalin; Sun, Tonghua; Jia, Jinping

    2009-05-01

    A gas chromatography (GC) coupled with solid-phase micro-extraction using a special activated carbon fiber (ACF) was developed for the analysis of 6 nitroaromatics and cyclic ketones, nitrobenzene (NB), 1,3-dinitrobenzene (1,3-DNB), 2,4-dinitrotoluene (2,4-DNT), 2,6-dinitrotoluene (2,6-DNT), isophorone, 1,4-naphthaquinone (1,4-NPQ), in sea water samples. The sample was extracted for 30 min under saturation of NaCl at 1,500 r/min and 60 degrees C in head space. The desorption was performance at 280 degrees C for 2 min. The linear ranges were from 0.01 to 400 microg/L. The limits of detection (LODs) were 1.4 - 3.2 ng/L. This method has been successfully applied to the determination of nitroaromatics and cyclic ketones in the sea water samples obtained from East China Sea. The concentrations of nitrobenzene, 1,3-dinitrobenzene and 2,6-dinitrotoluene in the sea water sample were 0.756, 0.944, 0.890 microg/L, respectively. The recoveries were 86.3% - 101.8% with the relative standard deviations (RSDs) of 3.7% -7.8%. The method is suitable for analyzing nitroaromatics and cyclic ketones at low concentration levels in sea water samples.

  7. [Determination of 23 antibiotics and 3 β-agonists in livestock drinking water by ultra performance liquid chromatography-tandem mass spectrometry coupled with solid-phase extraction].

    Science.gov (United States)

    Shi, Ao

    2016-02-01

    A method has been developed for the simultaneous determination of 23 antibiotics (four categories) and 3 β-agonists in livestock drinking water using solid-phase extraction and ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC-ESI MS/MS). The samples were adjusted pH to 5. 0, added Na2EDTA, enriched and cleaned-up by an HLB solid-phase extraction cartridge. The target compounds were confirmed and quantified by UPLC-ESI MS/MS with external standard method for the anti- biotics and internal standard method for the β-agonists. The recoveries were assessed by using lab tap water as matrix. The average recoveries of the 23 antibiotics and the 3 β-agonists were in the range of 50. 7%-104. 6% and the relative standard deviations (RSDs) were 2. 6%-8. 8% (n= 3). Under the optimal conditions, the calibration curves of the 23 antibiotics and the 3 β-agonists showed good linearity with the correlation coefficients better than 0. 994. The limits of detection (LODs, S/N≥3) ranged from 0. 01-0. 20 ng/L. The developed method was applied to analyze the livestock drinking waters in 36 Beijing intensive livestock farms. The results showed that some antibiotics were detected.

  8. Determination of Polymer Additives-Antioxidants, Ultraviolet Stabilizers, Plasticizers and Photoinitiators in Plastic Food Package by Accelerated Solvent Extraction Coupled with High-Performance Liquid Chromatography.

    Science.gov (United States)

    Li, Bo; Wang, Zhi-Wei; Lin, Qin-Bao; Hu, Chang-Ying; Su, Qi-Zhi; Wu, Yu-Mei

    2015-07-01

    An analytical method for the quantitative determination of 4 antioxidants, 9 ultraviolet (UV) stabilizers, 12 phthalate plasticizers and 2 photoinitiators in plastic food package using accelerated solvent extraction (ASE) coupled with high-performance liquid chromatography-photodiode array detector (HPLC-PDA) has been developed. Parameters affecting the efficiency in the process such as extraction and chromatographic conditions were studied in order to determine operating conditions. The analytical method of ASE-HPLC showed good linearity with good correlation coefficients (R ≥ 0.9833). The limits of detection and quantification were between 0.03 and 0.30 µg mL(-1) and between 0.10 and 1.00 µg mL(-1) for 27 analytes. Average spiked recoveries for most analytes in samples were >70.4% at 10, 20 and 40 µg g(-1) spiked levels, except UV-9 and Irganox 1010 (58.6 and 64.0% spiked at 10 µg g(-1), respectively), the relative standard deviations were in the range from 0.4 to 15.4%. The methodology has been proposed for the analysis of 27 polymer additives in plastic food package. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  9. Lipids and Fatty Acids in Algae: Extraction, Fractionation into Lipid Classes, and Analysis by Gas Chromatography Coupled with Flame Ionization Detector (GC-FID).

    Science.gov (United States)

    Guihéneuf, Freddy; Schmid, Matthias; Stengel, Dagmar B

    2015-01-01

    Despite the number of biochemical studies exploring algal lipids and fatty acid biosynthesis pathways and profiles, analytical methods used by phycologists for this purpose are often diverse and incompletely described. Potential confusion and potential variability of the results between studies can therefore occur due to change of protocols for lipid extraction and fractionation, as well as fatty acid methyl esters (FAME) preparation before gas chromatography (GC) analyses. Here, we describe a step-by-step procedure for the profiling of neutral and polar lipids using techniques such as solid-liquid extraction (SLE), thin-layer chromatography (TLC), and gas chromatography coupled with flame ionization detector (GC-FID). As an example, in this protocol chapter, analyses of neutral and polar lipids from the marine microalga Pavlova lutheri (an EPA/DHA-rich haptophyte) will be outlined to describe the distribution of fatty acid residues within its major lipid classes. This method has been proven to be a reliable technique to assess changes in lipid and fatty acid profiles in several other microalgal species and seaweeds.

  10. Multiresidue method for detection of pesticides in beef meat using liquid chromatography coupled to mass spectrometry detection (LC-MS) after QuEChERS extraction.

    Science.gov (United States)

    Oliveira, Fabiano Aurélio da Silva; Pereira, Elba Nathália Corrêa; Gobbi, Jennifer Mattedi; Soto-Blanco, Benito; Melo, Marília Martins

    2018-01-01

    Beef meat is an important food that can be contaminated by pesticides. This study aimed to optimize a multiresidue method for identification and quantification of pesticides in beef meat by liquid chromatography coupled to mass spectrometry detection (LC-MS). The extraction and clean-up procedures were adapted from the QuECHERS method. From the 188 analytes tested, the method was validated as qualitative method for 19 compounds and as quantitative method for 152 compounds. The results were satisfactory, yielding coefficients of variation of less than 20% and recoveries ranging from 70% to 120% and expanded uncertainty of less than 50%. The quantification limit was typically 10 µg kg -1 (but 25 µg kg -1 for 12 of the compounds) and the detection limit was 5.0 µg kg -1 . Thirty-two real samples of commercialized beef meat were analyzed without any residual pesticide being found. Thus, the results showed that the multiresidue method for detecting 171 pesticides, using adapted QuECHERS for extraction and LC-MS for detection, is suitable for analyzing beef meat.

  11. Analysis of Benzo[a]pyrene in Vegetable Oils Using Molecularly Imprinted Solid Phase Extraction (MISPE Coupled with Enzyme-Linked Immunosorbent Assay (ELISA

    Directory of Open Access Journals (Sweden)

    Michael Pschenitza

    2014-05-01

    Full Text Available This paper describes the development of a molecularly imprinted polymer-based solid phase extraction (MISPE method coupled with enzyme-linked immunosorbent assay (ELISA for determination of the PAH benzo[a]pyrene (B[a]P in vegetable oils. Different molecularly imprinted polymers (MIPs were prepared using non-covalent 4-vinylpyridine/divinylbenzene co-polymerization at different ratios and dichloromethane as porogen. Imprinting was done with a template mixture of phenanthrene and pyrene yielding a broad-specific polymer for PAHs with a maximum binding capacity (Q of ~32 μg B[a]P per 50 mg of polymer. The vegetable oil/n-hexane mixture (1:1, (v/v was pre-extracted with acetonitrile, the solvent evaporated, the residue reconstituted in n-hexane and subjected to MISPE. The successive washing with n-hexane and isopropanol revealed most suitable to remove lipid matrix constituents. After elution of bound PAHs from MISPE column with dichloromethane, the solvent was evaporated, the residue reconstituted with dimethyl sulfoxide and diluted 100-fold with methanol/water (10:90, (v/v for analysis of B[a]P equivalents with an ELISA. The B[a]P recovery rates in spiked vegetable oil samples of different fatty acid composition were determined between 63% and 114%. The presence of multiple PAHs in the oil sample, because of MIP selectivity and cross-reactivity of the ELISA, could yield overestimated B[a]P values.

  12. Investigation into the behavior of metal-argon polyatomic ions (MAr+) in the extraction region of inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Ebert, Chris H.; Witte, Travis M.; Houk, R.S.

    2012-01-01

    The abundances of metal-argon polyatomic ions (MAr + ) are determined in inductively coupled plasma-mass spectrometry (ICP-MS). The ratios of MAr + abundance to that for M + ions are measured experimentally. These ratios are compared to expected values, calculated for typical plasma conditions using spectroscopic data. For all metals studied (Ti, V, Cr, Mn, Fe, Co, Ni, Cu, and Zn), the measured ratios are significantly lower than the calculated ratios. Increasing the plasma potential (and thereby increasing the ion kinetic energy) by means of a homemade guard electrode with a wide gap further reduces the MAr + /M + ratio. Implementing a skimmer cone designed for high transmission of light ions increases the MAr + abundance. Considering this evidence, the scarcity of MAr + ions is attributed to collision induced dissociation (CID), likely due to a shock wave at the tip of or in the throat of the skimmer cone. - Highlights: ► MAr + ions are less abundant in the mass spectrum than expected from the ICP. ► Increasing the plasma potential reduces their abundance further. ► The extraction lens voltage does not greatly affect the MAr + abundances. ► The weakly-bound MAr + ions are probably dissociated by collisions during extraction.

  13. A high-throughput solid-phase extraction microchip combined with inductively coupled plasma-mass spectrometry for rapid determination of trace heavy metals in natural water.

    Science.gov (United States)

    Shih, Tsung-Ting; Hsieh, Cheng-Chuan; Luo, Yu-Ting; Su, Yi-An; Chen, Ping-Hung; Chuang, Yu-Chen; Sun, Yuh-Chang

    2016-04-15

    Herein, a hyphenated system combining a high-throughput solid-phase extraction (htSPE) microchip with inductively coupled plasma-mass spectrometry (ICP-MS) for rapid determination of trace heavy metals was developed. Rather than performing multiple analyses in parallel for the enhancement of analytical throughput, we improved the processing speed for individual samples by increasing the operation flow rate during SPE procedures. To this end, an innovative device combining a micromixer and a multi-channeled extraction unit was designed. Furthermore, a programmable valve manifold was used to interface the developed microchip and ICP-MS instrumentation in order to fully automate the system, leading to a dramatic reduction in operation time and human error. Under the optimized operation conditions for the established system, detection limits of 1.64-42.54 ng L(-1) for the analyte ions were achieved. Validation procedures demonstrated that the developed method could be satisfactorily applied to the determination of trace heavy metals in natural water. Each analysis could be readily accomplished within just 186 s using the established system. This represents, to the best of our knowledge, an unprecedented speed for the analysis of trace heavy metal ions. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Determination of Three Organochlorine Pesticides in Aqueous Samples by Solid-Phase Extraction Based on Natural Nano Diatomite in Packed Syringe Coupled to Gas Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Taghani, Abdollah; Goudarzi, Nasser; Bagherian, Ghadamali; Chamjangali, Mansour Arab

    2017-01-01

    A rapid, simple, and sensitive technique is proposed based on a miniaturized solid-phase extraction method named mictroextraction in a packed syringe coupled with gas chromatography-mass spectrometry for the preconcentration and determination of three organochlorine pesticides. These include hexachlorobenzene, heptachlor and aldrine in aqueous samples. For the first time, the natural nano diatomite is used a sorbent. Based on this technique, 6.0 mg of the nano sorbent is inserted in a syringe between two polypropylene frits. The analytes would be adsorbed on the solid phase, and would subsequently be eluted using organic solvents. The influence of some important parameters, such as the solution pH, type and volume of the organic desorption solvent, and amount of sorbent on the extraction efficiency of the selected pesticides, is investigated. The proposed method shows good linearity in the range of 0.1 - 40.0 μg L -1 , and at low limits of detection in the range of 0.02 - 0.13 μg L -1 using the selected ion-monitoring mode. The reproducibility of this method was found to be in the range of 3.5 - 11.1% for the understudied pesticides. In order to evaluate the matrix effect, the developed method is also applied to the preconcentration and determination of the selected pesticides in different water samples.

  15. Pressurized liquid extraction using water/isopropanol coupled with solid-phase extraction cleanup for semivolatile organic compounds, polycyclic aromatic hydrocarbons (PAH), and alkylated PAH homolog groups in sediment

    Science.gov (United States)

    Burkhardt, M.R.; Zaugg, S.D.; Burbank, T.L.; Olson, M.C.; Iverson, J.L.

    2005-01-01

    Polycyclic aromatic hydrocarbons (PAH) are recognized as environmentally relevant for their potential adverse effects on human and ecosystem health. This paper describes a method to determine the distribution of PAH and alkylated homolog groups in sediment samples. Pressurized liquid extraction (PLE), coupled with solid-phase extraction (SPE) cleanup, was developed to decrease sample preparation time, to reduce solvent consumption, and to minimize background interferences for full-scan GC-MS analysis. Recoveries from spiked Ottawa sand, environmental stream sediment, and commercially available topsoil, fortified at 1.5-15 ??g per compound, averaged 94.6 ?? 7.8%, 90.7 ?? 5.8% and 92.8 ?? 12.8%, respectively. Initial method detection limits for single-component compounds ranged from 20 to 302 ??g/kg, based on 25 g samples. Results from 28 environmental sediment samples, excluding homologs, show 35 of 41 compounds (85.4%) were detected in at least one sample with concentrations ranging from 20 to 100,000 ??g/kg. The most frequently detected compound, 2,6-dimethylnaphthalene, was detected in 23 of the 28 (82%) environmental samples with a concentration ranging from 15 to 907 ??g/kg. The results from the 28 environmental sediment samples for the homolog series showed that 27 of 28 (96%) samples had at least one homolog series present at concentrations ranging from 20 to 89,000 ??g/kg. The most frequently detected homolog series, C2-alkylated naphthalene, was detected in 26 of the 28 (93%) environmental samples with a concentration ranging from 25 to 3900 ??g/kg. Results for a standard reference material using dichloromethane Soxhlet-based extraction also are compared. ?? 2005 Elsevier B.V. All rights reserved.

  16. Magnetic solid-phase extraction of heterocyclic pesticides in environmental water samples using metal-organic frameworks coupled to high performance liquid chromatography determination.

    Science.gov (United States)

    Ma, Jiping; Wu, Gege; Li, Shuang; Tan, Weiqiang; Wang, Xiaoyan; Li, Jinhua; Chen, Lingxin

    2018-06-08

    A simple method of magnetic solid-phase extraction (MSPE) coupled to high performance liquid chromatography (HPLC) was developed for the simultaneous extraction and determination of four kinds of heterocyclic pesticides (carbendazim, triadimefon, chlorfenapyr and fenpyroximate) in environmental water samples. Magnetic metal-organic frameworks (MOFs) of type MOF-5 were prepared and used as adsorbents of MSPE. Several main parameters influencing MSPE efficiency were investigated, including amount of magnetic MOF-5, sample solution pH, extraction time, salt concentration, type and volume of desorption solvents and desorption time. Under optimal conditions, the MSPE-HPLC method presented fast simple separation and analysis, and excellent linearity in the range of 0.3-500.0 μg/L for carbendazim and triadimefon, and 0.1-500.0 μg/L for chlorfenapyr and fenpyroximate, with correlation coefficients (r) higher than 0.9992. High sensitivity with limits of detection and quantification ranging from 0.04-0.11 μg/L and 0.13-0.35 μg/L, respectively, were achieved, as well as good precision with relative standard deviations of 2.98-7.11% (intra-day) and 3.31-7.12% (inter-day). Furthermore, the method was successfully applied to reservoir and Yellow River water samples, and satisfactory recoveries at three spiked concentration levels were between 80.20% and 108.33%.The magnetic MOF-5 composites based MSPE followed by HPLC proved promising for convenient and efficient determination of heterocyclic pesticides in environmental water samples. Copyright © 2018 Elsevier B.V. All rights reserved.

  17. Rapid identification and quantification of methamphetamine and amphetamine in hair by gas chromatography/mass spectrometry coupled with micropulverized extraction, aqueous acetylation and microextraction by packed sorbent.

    Science.gov (United States)

    Miyaguchi, Hajime; Iwata, Yuko T; Kanamori, Tatsuyuki; Tsujikawa, Kenji; Kuwayama, Kenji; Inoue, Hiroyuki

    2009-05-01

    We developed a rapid identification and quantification method for the toxicological analysis of methamphetamine and amphetamine in human hair by gas chromatography/mass spectrometry coupled with a novel combination of micropulverized extraction, aqueous acetylation and microextraction by packed sorbent (MEPS) named MiAMi-GC/MS. A washed hair sample (1-5 mg) was micropulverized for 5 min in a 2 mL plastic tube with 250 microL of water. An anion-exchange sorbent was added to adsorb anionic interferences. After removing the residue with a membrane-filter unit, sodium carbonate and acetic anhydride was admixed in turn. Acetylation was completed in approximately 20 min at room temperature. The acetylated analytes in the reaction liquid were concentrated to an octadecylsilica sorbent packed in the needle of a syringe by a CombiPAL autosampler. Elution was carried out with 50 microL of methanol, and the entire eluate injected into a gas chromatograph using a programmable temperature vaporizing (PTV) technique. The time required for sample preparation and GC/MS analysis was approximately 1 h from a washed hair sample, and an evaporation process was not required. Ranges for quantification were 0.20-50 (ng/mg) each for methamphetamine and amphetamine using 1 mg of hair. Accuracy and relative standard deviation (RSD) were evaluated intraday and interday at three concentrations, and the results were within the limit of a guidance issued by U.S. Food and Drug Administration. For identification, full-scan mass spectra of methamphetamine and amphetamine were obtained using 5 mg of fortified hair samples at 0.2 ng/mg. The extraction device of MEPS was durable for at least 300 extractions, whereas the liner of the gas chromatograph should be replaced after 20-30 times use. The carry over was estimated to be about 1-2%. This sample-preparation method coupled with GC/MS is fast and labor-saving in comparison with conventional methods.

  18. Ultrasonic sludge pretreatment under pressure.

    Science.gov (United States)

    Le, Ngoc Tuan; Julcour-Lebigue, Carine; Delmas, Henri

    2013-09-01

    The objective of this work was to optimize the ultrasound (US) pretreatment of sludge. Three types of sewage sludge were examined: mixed, secondary and secondary after partial methanisation ("digested" sludge). Thereby, several main process parameters were varied separately or simultaneously: stirrer speed, total solid content of sludge (TS), thermal operating conditions (adiabatic vs. isothermal), ultrasonic power input (PUS), specific energy input (ES), and for the first time external pressure. This parametric study was mainly performed for the mixed sludge. Five different TS concentrations of sludge (12-36 g/L) were tested for different values of ES (7000-75,000 kJ/kgTS) and 28 g/L was found as the optimum value according to the solubilized chemical oxygen demand in the liquid phase (SCOD). PUS of 75-150 W was investigated under controlled temperature and the "high power input - short duration" procedure was the most effective at a given ES. The temperature increase in adiabatic US application significantly improved SCOD compared to isothermal conditions. With PUS of 150 W, the effect of external pressure was investigated in the range of 1-16 bar under isothermal and adiabatic conditions for two types of sludge: an optimum pressure of about 2 bar was found regardless of temperature conditions and ES values. Under isothermal conditions, the resulting improvement of sludge disintegration efficacy as compared to atmospheric pressure was by 22-67% and 26-37% for mixed and secondary sludge, respectively. Besides, mean particle diameter (D[4,3]) of the three sludge types decreased respectively from 408, 117, and 110 μm to about 94-97, 37-42, and 36-40 μm regardless of sonication conditions, and the size reduction process was much faster than COD extraction. Copyright © 2013 Elsevier B.V. All rights reserved.

  19. Optimization of simultaneous ultrasonic-assisted extraction of water-soluble and fat-soluble characteristic constituents from Forsythiae Fructus Using response surface methodology and high-performance liquid chromatography.

    Science.gov (United States)

    Xia, Yong-Gang; Yang, Bing-You; Liang, Jun; Wang, Di; Yang, Qi; Kuang, Hai-Xue

    2014-07-01

    The compounds (+)-pinoresinol-β-glucoside (1) forsythiaside, (2) phillyrin (3) and phillygenin (4) were elucidated to be the characteristic constituents for quality control of Forsythiae Fructus extract by chromatographic fingerprint in 2010 edition of Chinese Pharmacopoeia due to their numerous important pharmacological actions. It is of great interest to extract these medicinally active constituents from Forsythiae Fructus simultaneously. In this study, a new ultrasound-assisted extraction (UAE) method was developed for the simultaneous extraction of biological components 1-4 in Forsythiae Fructus. The quantitative effects of extraction time, ratio of liquid to solid, extraction temperature, and methanol concentration on yield of these four important biological constituents from Forsythiae Fructus were investigated using response surface methodology with Box-Behnken design. The compounds 1-4 extracted by UAE were quantitative analysis by high-performance liquid chromatography-photodiode array detect (HPLC-PAD), and overall desirability (OD), the geometric mean of the contents of four major biological components, was used as a marker to evaluate the extraction efficiency. By solving the regression equation and analyzing 3-D plots, the optimum condition was at extraction temperature 70°C, time 60 min, ratio of liquid to solid 20, and methanol concentration 76.6%. Under these conditions, extraction yields of compounds 1-4 were 2.92 mg/g, 52.10 mg/g, 0.90 mg/g and 0.57 mg/g, respectively, which were in good agreement with the predicted OD values. In order to achieve a similar yield as UAE, soxhlet extraction required at least 6 h and maceration extraction required much longer time of 24 h. Established UAE method has been successfully applied to sample preparation for the quality control of Forsythiae Fructus. Additionally, a quadrupole time-of-flight mass spectrometry was applied to the structural confirmation of analytes from the complex matrices acquired by UAE

  20. Optimization of simultaneous ultrasonic-assisted extraction of water-soluble and fat-soluble characteristic constituents from Forsythiae Fructus Using response surface methodology and high-performance liquid chromatography

    Science.gov (United States)

    Xia, Yong-Gang; Yang, Bing-You; Liang, Jun; Wang, Di; Yang, Qi; Kuang, Hai-Xue

    2014-01-01

    Background: The compounds (+)-pinoresinol-β-glucoside (1) forsythiaside, (2) phillyrin (3) and phillygenin (4) were elucidated to be the characteristic constituents for quality control of Forsythiae Fructus extract by chromatographic fingerprint in 2010 edition of Chinese Pharmacopoeia due to their numerous important pharmacological actions. It is of great interest to extract these medicinally active constituents from Forsythiae Fructus simultaneously. Materials and Methods: In this study, a new ultrasound-assisted extraction (UAE) method was developed for the simultaneous extraction of biological components 1-4 in Forsythiae Fructus. The quantitative effects of extraction time, ratio of liquid to solid, extraction temperature, and methanol concentration on yield of these four important biological constituents from Forsythiae Fructus were investigated using response surface methodology with Box-Behnken design. The compounds 1-4 extracted by UAE were quantitative analysis by high-performance liquid chromatography-photodiode array detect (HPLC-PAD), and overall desirability (OD), the geometric mean of the contents of four major biological components, was used as a marker to evaluate the extraction efficiency. Results: By solving the regression equation and analyzing 3-D plots, the optimum condition was at extraction temperature 70°C, time 60 min, ratio of liquid to solid 20, and methanol concentration 76.6%. Under these conditions, extraction yields of compounds 1-4 were 2.92 mg/g, 52.10 mg/g, 0.90 mg/g and 0.57 mg/g, respectively, which were in good agreement with the predicted OD values. In order to achieve a similar yield as UAE, soxhlet extraction required at least 6 h and maceration extraction required much longer time of 24 h. Established UAE method has been successfully applied to sample preparation for the quality control of Forsythiae Fructus. Additionally, a quadrupole time-of-flight mass spectrometry was applied to the structural confirmation of analytes

  1. Contribution of dynamic focusing to ultrasonic defect characterization

    International Nuclear Information System (INIS)

    Mahaut, S.

    1997-01-01

    Non destructive testing of vessels of pressurized water reactors uses ultrasonic focused transducers, with spherically shaped emitting surface or requiring an acoustic lens. But a mechanically focused transducer has to be used for a given inspection zone and for a fixed control configuration. The aim of this thesis is to improve ultrasonic defect characterization using adaptive dynamic focusing. Such a technique makes use of a ultrasonic defect characterization using adaptive dynamic focusing. Such a technique makes use of an ultrasonic transducer split into an array of individually controlled elements, allowing to apply delay and amplitude laws, calculated from modeling or experimentally deduced. Acoustical characteristics of the ultrasonic beam in the inspected specimen this can be electronically controlled; refraction angle, depth focusing, beam width. We briefly describe in the first chapter a theoretical modeling of the ultrasonic field radiated through a fluid/solid interface, extended to phase array transducers. This model is based on the integral formulation of Rayleigh, modified to take into account transmission through a fluid/solid (homogeneous and isotropic), of planar or cylindrical shape. In the second chapter an experimental study of this technique, with delay and amplitude laws given from the model, is presented, showing the efficiency of this method to adjust the acoustic performances. In he third chapter, experimental delay laws, extracted from the time distribution of signals received by the array (issued from a preliminary detected reflector), are used to provide an optimal imaging of the defect. This self-focusing procedure shows to adapt to a defect without using theoretical delays. The last chapter is dedicated to different applications devoted to improved defect characterization. The first application uses amplitude distribution received by the array, pointing out geometric characteristics of the reflector, while the second application

  2. Micro-focused ultrasonic solid-liquid extraction (muFUSLE) combined with HPLC and fluorescence detection for PAHs determination in sediments: optimization and linking with the analytical minimalism concept.

    Science.gov (United States)

    Capelo, J L; Galesio, M M; Felisberto, G M; Vaz, C; Pessoa, J Costa

    2005-06-15

    Analytical minimalism is a concept that deals with the optimization of all stages of an analytical procedure so that it becomes less time, cost, sample, reagent and energy consuming. The guide-lines provided in the USEPA extraction method 3550B recommend the use of focused ultrasound (FU), i.e., probe sonication, for the solid-liquid extraction of Polycyclic Aromatic Hydrocarbons, PAHs, but ignore the principle of analytical minimalism. The problems related with the dead sonication zones, often present when high volumes are sonicated with probe, are also not addressed. In this work, we demonstrate that successful extraction and quantification of PAHs from sediments can be done with low sample mass (0.125g), low reagent volume (4ml), short sonication time (3min) and low sonication amplitude (40%). Two variables are here particularly taken into account for total extraction: (i) the design of the extraction vessel and (ii) the solvent used to carry out the extraction. Results showed PAHs recoveries (EPA priority list) ranged between 77 and 101%, accounting for more than 95% for most of the PAHs here studied, as compared with the values obtained after soxhlet extraction. Taking into account the results reported in this work we recommend a revision of the EPA guidelines for PAHs extraction from solid matrices with focused ultrasound, so that these match the analytical minimalism concept.

  3. Nonlinear ultrasonics for material state awareness

    Science.gov (United States)

    Jacobs, L. J.

    2014-02-01

    Predictive health monitoring of structural components will require the development of advanced sensing techniques capable of providing quantitative information on the damage state of structural materials. By focusing on nonlinear acoustic techniques, it is possible to measure absolute, strength based material parameters that can then be coupled with uncertainty models to enable accurate and quantitative life prediction. Starting at the material level, this review will present current research that involves a combination of sensing techniques and physics-based models to characterize damage in metallic materials. In metals, these nonlinear ultrasonic measurements can sense material state, before the formation of micro- and macro-cracks. Typically, cracks of a measurable size appear quite late in a component's total life, while the material's integrity in terms of toughness and strength gradually decreases due to the microplasticity (dislocations) and associated change in the material's microstructure. This review focuses on second harmonic generation techniques. Since these nonlinear acoustic techniques are acoustic wave based, component interrogation can be performed with bulk, surface and guided waves using the same underlying material physics; these nonlinear ultrasonic techniques provide results which are independent of the wave type used. Recent physics-based models consider the evolution of damage due to dislocations, slip bands, interstitials, and precipitates in the lattice structure, which can lead to localized damage.

  4. Ultrasonic level, temperature, and density sensor

    International Nuclear Information System (INIS)

    Rogers, S.C.; Miller, G.N.

    1982-01-01

    A sensor has been developed to measure simultaneously the level, temperature, and density of the fluid in which it is immersed. The sensor is a thin, rectangular stainless steel ribbon which acts as a waveguide and is housed in a perforated tube. The waveguide is coupled to a section of magnetostrictive magnetic-coil transducers. These tranducers are excited in an alternating sequence to interrogate the sensor with both torsional ultrasonic waves, utilizing the Wiedemann effect, and extensional ultrasonic waves, using the Joule effect. The measured torsional wave transit time is a function of the density, level, and temperature of the fluid surrounding the waveguide. The measured extensional wave transit time is a function of the temperature of the waveguide only. The sensor is divided into zones by the introduction of reflecting surfaces at measured intervals along its length. Consequently, the transit times from each reflecting surface can be analyzed to yield a temperature profile and a density profile along the length of the sensor. Improvements in acoustic wave dampener and pressure seal designs enhance the compatibility of the probe with high-temperature, high-radiation, water-steam environments and increase the likelihood of survival in such environments. Utilization of a microcomputer to automate data sampling and processing has resulted in improved resolution of the sensor

  5. Cadmium (II) imprinted 3-mercaptopropyltrimethoxysilane coated stir bar for selective extraction of trace cadmium from environmental water samples followed by inductively coupled plasma mass spectrometry detection

    International Nuclear Information System (INIS)

    Zhang Nan; Hu Bin

    2012-01-01

    Graphical abstract: Ion imprinted 3-mercaptopropyltrimethoxysilane (MPTS) coated stir bar for selective extraction of trace Cd(II). Highlights: ► Ion imprinted polymers were proposed as the coating for SBSE for the first time. ► Cd(II) imprinted MPTS-silica coating was prepared by a double-imprinting concept. ► A novel method of SBSE–ICP-MS was developed for the determination of Cd in waters. ► This method is rapid, selective, sensitive and applicable for determining trace Cd(II) in waters. - Abstract: Cd(II) imprinted 3-mercaptopropyltrimethoxysilane (MPTS)-silica coated stir bar was prepared by sol–gel technique combining with a double-imprinting concept for the first time and was employed for stir bar sorptive extraction (SBSE) of trace Cd(II) from water samples followed by inductively coupled plasma mass spectrometry (ICP-MS) detection. A tetramethoxysilane (TMOS) coating was first in situ created on the glass bar surface. Afterward, a sol solution containing MPTS as the functional precursor, ethanol as the solvent and both Cd(II) and surfactant micelles (cetyltrimethylammonium bromide, CTAB) as the template was again coated on the TMOS bar. The structures of the stir bar coating were characterized by FT-IR spectroscopy. Round-bottom vial was used for the extraction of Cd(II) by SBSE to avoid abrasion of stir bar coatings. The factors affecting the extraction of Cd(II) by SBSE such as pH, stirring rate and time, sample/elution volume and interfering ions have been investigated in detail, and the optimized experimental parameters were obtained. Under the optimized conditions, the adsorption capacities of non-imprinted and imprinted coating stir bars were found to be 0.5 μg and 0.8 μg bar −1 . The detection limit (3σ) based on three times standard deviations of the method blanks by 7 replicates was 4.40 ng L −1 and the relative standard deviation (RSD) was 3.38% (c = 1 μg L −1 , n = 7). The proposed method was successfully applied for the

  6. Cadmium (II) imprinted 3-mercaptopropyltrimethoxysilane coated stir bar for selective extraction of trace cadmium from environmental water samples followed by inductively coupled plasma mass spectrometry detection

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Nan [Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu Bin, E-mail: binhu@whu.edu.cn [Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072 (China)

    2012-04-20

    Graphical abstract: Ion imprinted 3-mercaptopropyltrimethoxysilane (MPTS) coated stir bar for selective extraction of trace Cd(II). Highlights: Black-Right-Pointing-Pointer Ion imprinted polymers were proposed as the coating for SBSE for the first time. Black-Right-Pointing-Pointer Cd(II) imprinted MPTS-silica coating was prepared by a double-imprinting concept. Black-Right-Pointing-Pointer A novel method of SBSE-ICP-MS was developed for the determination of Cd in waters. Black-Right-Pointing-Pointer This method is rapid, selective, sensitive and applicable for determining trace Cd(II) in waters. - Abstract: Cd(II) imprinted 3-mercaptopropyltrimethoxysilane (MPTS)-silica coated stir bar was prepared by sol-gel technique combining with a double-imprinting concept for the first time and was employed for stir bar sorptive extraction (SBSE) of trace Cd(II) from water samples followed by inductively coupled plasma mass spectrometry (ICP-MS) detection. A tetramethoxysilane (TMOS) coating was first in situ created on the glass bar surface. Afterward, a sol solution containing MPTS as the functional precursor, ethanol as the solvent and both Cd(II) and surfactant micelles (cetyltrimethylammonium bromide, CTAB) as the template was again coated on the TMOS bar. The structures of the stir bar coating were characterized by FT-IR spectroscopy. Round-bottom vial was used for the extraction of Cd(II) by SBSE to avoid abrasion of stir bar coatings. The factors affecting the extraction of Cd(II) by SBSE such as pH, stirring rate and time, sample/elution volume and interfering ions have been investigated in detail, and the optimized experimental parameters were obtained. Under the optimized conditions, the adsorption capacities of non-imprinted and imprinted coating stir bars were found to be 0.5 {mu}g and 0.8 {mu}g bar{sup -1}. The detection limit (3{sigma}) based on three times standard deviations of the method blanks by 7 replicates was 4.40 ng L{sup -1} and the relative standard

  7. Real-time ultrasonic weld evaluation system

    Science.gov (United States)

    Katragadda, Gopichand; Nair, Satish; Liu, Harry; Brown, Lawrence M.

    1996-11-01

    Ultrasonic testing techniques are currently used as an alternative to radiography for detecting, classifying,and sizing weld defects, and for evaluating weld quality. Typically, ultrasonic weld inspections are performed manually, which require significant operator expertise and time. Thus, in recent years, the emphasis is to develop automated methods to aid or replace operators in critical weld inspections where inspection time, reliability, and operator safety are major issues. During this period, significant advances wee made in the areas of weld defect classification and sizing. Very few of these methods, however have found their way into the market, largely due to the lack of an integrated approach enabling real-time implementation. Also, not much research effort was directed in improving weld acceptance criteria. This paper presents an integrated system utilizing state-of-the-art techniques for a complete automation of the weld inspection procedure. The modules discussed include transducer tracking, classification, sizing, and weld acceptance criteria. Transducer tracking was studied by experimentally evaluating sonic and optical position tracking techniques. Details for this evaluation are presented. Classification is obtained using a multi-layer perceptron. Results from different feature extraction schemes, including a new method based on a combination of time and frequency-domain signal representations are given. Algorithms developed to automate defect registration and sizing are discussed. A fuzzy-logic acceptance criteria for weld acceptance is presented describing how this scheme provides improved robustness compared to the traditional flow-diagram standards.

  8. STUDY ON ULTRASONIC DEGREASING OF SHEEPSKIN WASTE

    Directory of Open Access Journals (Sweden)

    BĂLĂU MÎNDRU Tudorel

    2014-05-01

    Full Text Available Leather industry is a relatively large source of waste from raw material, so skin waste recovery is a goal of clean technologies. Capitalization of skin waste aims to obtain: chemical auxiliaries, technical articles, hydrolyzed protein, artificial leather, composite building materials, heat sources and collagen biomaterials with applications in medicine, cosmetics, etc. A first step in the recovery of skin waste is the degreasing operation. Ultrasound is an effective tool to improve the efficiency of the conventional degreasing affecting the chemical substances as well as the treated skin. In addition, the processing time is reduced. Ultrasound is known to enhance the emulsification and dispersion of oils/fat. The usual degreasing methods requires more emulsifier/solvent ratio and process time for emulsification and additional solvent for washing out the emulsified fat. This paper investigates the possibility of recovery through ecological processes of leather waste from finishing operations for further capitalization. The present study aims emulsification and subsequent removal of the fat present in the chamois powder waste from polishing operation with the aid of ultrasound by an aqueous ecofriendly method. The study also took into account the ultrasonic treatment of the leather waste using trichlorethylene as a medium of propagation-degreasing, and realized a comparative analysis of efficiency of fat extraction by Soxhlet method and via ultrasonication. IR-ATR and optical microscopy highlight both morphological and chemical-structural changes of treated materials by different degreasing methods

  9. Detailed simulation of ultrasonic inspections

    International Nuclear Information System (INIS)

    Chaplin, K.R.; Douglas, S.R.; Dunford, D.

    1997-01-01

    Simulation of ultrasonic inspection of engineering components have been performed at the Chalk River Laboratories of AECL for over 10 years. The computer model, called EWE for Elastic Wave Equations, solves the Elastic Wave Equations using a novel finite difference scheme. It simulates the propagation of an ultrasonic wave from the transducer to a flaw, the scatter of waves from the flaw, and measurement of signals at a receive transducer. Regions of different materials, water and steel for example, can be simulated. In addition, regions with slightly different material properties from the parent material can be investigated. The two major types of output are displays of the ultrasonic waves inside the component and the corresponding A-scans. EPRI and other organizations have used ultrasonic models for: defining acceptable ultrasonic inspection procedures, designing and evaluating inspection techniques, and for quantifying inspection reliability. The EWE model has been applied to the inspection of large pipes in a nuclear plant, gas pipeline welds and steam generator tubes. Most recent work has dealt with the ultrasonic inspection of pressure tubes in CANDU reactors. Pressure tube inspections can reliably detect and size defects; however, there are improvements that can be made. For example, knowing the sharpness of a flaw-tip is crucial for fitness for service assessments. Computer modelling of the ultrasonic inspection of flaws with different root radius has suggested inspection techniques that provide flaw tip radius information. A preliminary investigation of these methods has been made in the laboratory. The basis for the model will be reviewed at the presentation. Then the results of computer simulations will be displayed on a PC using an interactive program that analyzes simulated A-scans. This software tool gives inspection staff direct access to the results of computer simulations. (author)

  10. Association schemes perspective of microbubble cluster in ultrasonic fields.

    Science.gov (United States)

    Behnia, S; Yahyavi, M; Habibpourbisafar, R

    2018-06-01

    Dynamics of a cluster of chaotic oscillators on a network are studied using coupled maps. By introducing the association schemes, we obtain coupling strength in the adjacency matrices form, which satisfies Markov matrices property. We remark that in general, the stability region of the cluster of oscillators at the synchronization state is characterized by Lyapunov exponent which can be defined based on the N-coupled map. As a detailed physical example, dynamics of microbubble cluster in an ultrasonic field are studied using coupled maps. Microbubble cluster dynamics have an indicative highly active nonlinear phenomenon, were not easy to be explained. In this paper, a cluster of microbubbles with a thin elastic shell based on the modified Keller-Herring equation in an ultrasonic field is demonstrated in the framework of the globally coupled map. On the other hand, a relation between the microbubble elements is replaced by a relation between the vertices. Based on this method, the stability region of microbubbles pulsations at complete synchronization state has been obtained analytically. In this way, distances between microbubbles as coupling strength play the crucial role. In the stability region, we thus observe that the problem of study of dynamics of N-microbubble oscillators reduce to that of a single microbubble. Therefore, the important parameters of the isolated microbubble such as applied pressure, driving frequency and the initial radius have effective behavior on the synchronization state. Copyright © 2018 Elsevier B.V. All rights reserved.

  11. Ultrasonic measurements and technologies

    CERN Document Server

    Kočiš, Štefan

    1996-01-01

    An impulse for writing this book has originated from the effort to sum­ marize and publicise the acquired results of a research team at the De­ partment of Automation of the Faculty of Electrical Engineering and In­ formatics, Slovak Technical University in Bratislava. The research team has been involved for a long time with control problems for machine production mechanisms and, in recent (approximately 15) years, its effort was aimed mostly at the control of electrical servosystems of robots. Within this scope, the members of the authors' staff solved the State Re­ search Task Ultrasonic sensing of the position of a robot hand, which was coordinated by the Institute of Technical Cybernetics of the Slovak Academy of Sciences in Bratislava. The problem was solved in a complex way, i.e. from a conceptual de­ sign of the measurement, through the measurement and evaluation sys­ tem, up to connection to the control system of a robot. Compensation of the atmospheric influence on the precision of measurement,...

  12. Ultrasonic-testing method

    International Nuclear Information System (INIS)

    Thome, Paul.

    1973-01-01

    Description is given of a device adapted to the detection, by means of ultrasonic waves, of all the flaws and defects included in workpieces when only one face of the latter is accessible. A beam is directed towards the rear-face of the workpiece (e.g. a plate) on which it is reflected. The image thus reflected is fed into a receiver. The latter is under the control of the displacement of that image; simultaneously a transducer checks the condition of the mirror at the places where the beam is reflected. Whenever a flow or defect comes between, a silent zone is formed. By recording the silent zones with respect to the positions of several emitters, it is possible to locates a flaw and to define the outline thereof. The apparatus comprises several ''emitter-receiver'' groups intersecting over the emitter used in order to check the good conditions of the mirror. The invention can be used for searching and identifying flaws and defects in buildings which have to be of top quality (e.g., cofferdams, nuclear devices, shipbuilding yards, aeronautics) [fr

  13. Dental hard tissue characterization using laser-based ultrasonics

    Science.gov (United States)

    Blodgett, David W.; Massey, Ward L.

    2003-07-01

    Dental health care and research workers require a means of imaging the structures within teeth in vivo. One critical need is the detection of tooth decay in its early stages. If decay can be detected early enough, the process can be monitored and interventional procedures, such as fluoride washes and controlled diet, can be initiated to help re-mineralize the tooth. Currently employed x-ray imaging is limited in its ability to visualize interfaces and incapable of detecting decay at a stage early enough to avoid invasive cavity preparation followed by a restoration. To this end, non-destructive and non-contact in vitro measurements on extracted human molars using laser-based ultrasonics are presented. Broadband ultrasonic waves are excited in the extracted sections by using a pulsed carbon-dioxide (CO2) laser operating in a region of high optical absorption in the dental hard tissues. Optical interferometric detection of the ultrasonic wave surface displacements in accomplished with a path-stabilized Michelson-type interferometer. Results for bulk and surface in-vitro characterization of caries are presented on extracted molars with pre-existing caries.

  14. Mechanical and Thermal Properties of Praseodymium Monopnictides: AN Ultrasonic Study

    Science.gov (United States)

    Bhalla, Vyoma; Kumar, Raj; Tripathy, Chinmayee; Singh, Devraj

    2013-09-01

    We have computed ultrasonic attenuation, acoustic coupling constants and ultrasonic velocities of praseodymium monopnictides PrX(X: N, P, As, Sb and Bi) along the , , in the temperature range 100-500 K using higher order elastic constants. The higher order elastic constants are evaluated using Coulomb and Born-Mayer potential with two basic parameters viz. nearest-neighbor distance and hardness parameter in the temperature range of 0-500 K. Several other mechanical and thermal parameters like bulk modulus, shear modulus, Young's modulus, Poisson ratio, anisotropic ratio, tetragonal moduli, Breazeale's nonlinearity parameter and Debye temperature are also calculated. In the present study, the fracture/toughness (B/G) ratio is less than 1.75 which implies that PrX compounds are brittle in nature at room temperature. The chosen material fulfilled Born criterion of mechanical stability. We also found the deviation of Cauchy's relation at higher temperatures. PrN is most stable material as it has highest valued higher order elastic constants as well as the ultrasonic velocity. Further, the lattice thermal conductivity using modified approach of Slack and Berman is determined at room temperature. The ultrasonic attenuation due to phonon-phonon interaction and thermoelastic relaxation mechanisms have been computed using modified Mason's approach. The results with other well-known physical properties are useful for industrial applications.

  15. Modeling of ultrasonic processes utilizing a generic software framework

    Science.gov (United States)

    Bruns, P.; Twiefel, J.; Wallaschek, J.

    2017-06-01

    Modeling of ultrasonic processes is typically characterized by a high degree of complexity. Different domains and size scales must be regarded, so that it is rather difficult to build up a single detailed overall model. Developing partial models is a common approach to overcome this difficulty. In this paper a generic but simple software framework is presented which allows to coupe arbitrary partial models by slave modules with well-defined interfaces and a master module for coordination. Two examples are given to present the developed framework. The first one is the parameterization of a load model for ultrasonically-induced cavitation. The piezoelectric oscillator, its mounting, and the process load are described individually by partial models. These partial models then are coupled using the framework. The load model is composed of spring-damper-elements which are parameterized by experimental results. In the second example, the ideal mounting position for an oscillator utilized in ultrasonic assisted machining of stone is determined. Partial models for the ultrasonic oscillator, its mounting, the simplified contact process, and the workpiece’s material characteristics are presented. For both applications input and output variables are defined to meet the requirements of the framework’s interface.

  16. An Ultrasonic Wheel-Array Probe

    Science.gov (United States)

    Drinkwater, B. W.; Brotherhood, C. J.; Freemantle, R. J.

    2004-02-01

    This paper describes the development and modeling of an ultrasonic array wheel probe scanning system. The system operates at 10 MHz using a 64 element array transducer which is 50 mm in length and located in a fluid filled wheel. The wheel is coupled to the test structure dry, or with a small amount of liquid couplant. When the wheel is rolled over the surface of the test structure a defect map (C-Scan) is generated in real-time. The tyre is made from a soft, durable polymer which has very little acoustic loss. Two application studies are presented; the inspection of sealant layers in an aluminum aircraft wing structure and the detection of embedded defects in a thick section carbon composite sample.

  17. Ultrasonic study of elastic creep in piezoceramics.

    Science.gov (United States)

    Tsaplev, V M; Konovalov, R S

    2017-11-01

    Ultrasonic method and experimental setup for study the elastic creep of piezoelectric materials are described. The results of experimental studies of time behavior of the Young's modulus and the internal friction are presented as well as the longitudinal and transversal piezomoduli and the electromechanical coupling factor. Four compositions of piezoelectric ceramics both soft and hard, based on BaTiO 3 and PZT, were compressed for a long time (0÷10 7 s) by significant static loads (0÷120MPa). The possible physical mechanisms that cause the creep are briefly considered. The concept of a spectrum of activation energies of the corresponding processes is introduced. The upper and the lower boundaries of the relaxation times spectrum were measured and corresponding activation energies were found. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Sensitive and simple determination of zwitterionic morphine in human urine based on liquid-liquid micro-extraction coupled with surface-enhanced Raman spectroscopy.

    Science.gov (United States)

    Yu, Borong; Cao, Chentai; Li, Pan; Mao, Mei; Xie, Qiwen; Yang, Liangbao

    2018-08-15

    Morphine, a kind of illicit drugs, is also one of the main heroin metabolites. In consideration of a noninvasive way to monitor and identify drug abuse during forensic cases, the urine samples are usually detected. Here, colloidal gold nanorods (Au NRs) were introduced to act as active substrate, because of the strong optical extinction and spectral tunability of the longitudinal surface plasmon resonance (SPR). Thus, well surface-enhanced Raman spectra of morphine even at low concentrations could be obtained by portable Raman spectrometer. For the complex matrix environment of urine, liquid-liquid micro-extraction (LLME), a simple and inexpensive pretreatment, was employed to avoid the interferences. And then, the coupled surface-enhanced Raman spectroscopy (SERS) can give full play to the advantages of high sensitivity and unique spectroscopic fingerprint. According to the zwitterionic structure and physicochemical parameters of morphine molecules, the pH value of urine sample was adjusted to about 9 by buffer solution (KOH/NaB 4 O 7 ) and the mixture of chloroform and isopropyl alcohol (V/V=9:1) was chosen as extractant. Moreover, such pretreatment was proved to be appropriate for separation and concentration of morphine from urine. The developed LLME-SERS method could provide a detection limit less than 1 ppm in the human urine environment and the whole process of detection just needed take 5-6 min. What's more, the results of urine samples from heroin users exhibited application value of the proposed technique. The excellent performance makes it promising to become a rapid, reliable, and on-spot analyzer, especially for public safety and healthcare. Copyright © 2018 Elsevier B.V. All rights reserved.

  19. Ultrasonic propulsion of kidney stones.

    Science.gov (United States)

    May, Philip C; Bailey, Michael R; Harper, Jonathan D

    2016-05-01

    Ultrasonic propulsion is a novel technique that uses short bursts of focused ultrasonic pulses to reposition stones transcutaneously within the renal collecting system and ureter. The purpose of this review is to discuss the initial testing of effectiveness and safety, directions for refinement of technique and technology, and opinions on clinical application. Preclinical studies with a range of probes, interfaces, and outputs have demonstrated feasibility and consistent safety of ultrasonic propulsion with room for increased outputs and refinement toward specific applications. Ultrasonic propulsion was used painlessly and without adverse events to reposition stones in 14 of 15 human study participants without restrictions on patient size, stone size, or stone location. The initial feasibility study showed applicability in a range of clinically relevant situations, including facilitating passage of residual fragments following ureteroscopy or shock wave lithotripsy, moving a large stone at the ureteropelvic junction with relief of pain, and differentiating large stones from a collection of small fragments. Ultrasonic propulsion shows promise as an office-based system for transcutaneously repositioning kidney stones. Potential applications include facilitating expulsion of residual fragments following ureteroscopy or shock wave lithotripsy, repositioning stones prior to treatment, and repositioning obstructing ureteropelvic junction stones into the kidney to alleviate acute renal colic.

  20. Ultrasonic stir welding process and apparatus

    Science.gov (United States)

    Ding, R. Jeffrey (Inventor)

    2009-01-01

    An ultrasonic stir welding device provides a method and apparatus for elevating the temperature of a work piece utilizing at least one ultrasonic heater. Instead of relying on a rotating shoulder to provide heat to a workpiece an ultrasonic heater is utilized to provide ultrasonic energy to the workpiece. A rotating pin driven by a motor assembly performs the weld on the workpiece. A handheld version can be constructed as well as a fixedly mounted embodiment.

  1. The effects of ultrasonic solidification on aluminum

    OpenAIRE

    Đorđević Slavko 1

    2003-01-01

    The effect of ultrasound on characteristics of solidified aluminum was shown. An ultrasonic head and ultrasonic system for modification was designed and applied to the crystallizing aluminum melt. The ultrasonic generator allows power of 50-500 W, amplitude of oscillations 10-100 um.m and the operating frequency of 25 kHz. Ultrasonic modification was done by ultrasound introduced from above into the melt. Microstructure photographs show decreasing of the grain size more than five times.

  2. The effects of ultrasonic solidification on aluminum

    Directory of Open Access Journals (Sweden)

    Đorđević Slavko 1

    2003-01-01

    Full Text Available The effect of ultrasound on characteristics of solidified aluminum was shown. An ultrasonic head and ultrasonic system for modification was designed and applied to the crystallizing aluminum melt. The ultrasonic generator allows power of 50-500 W, amplitude of oscillations 10-100 um.m and the operating frequency of 25 kHz. Ultrasonic modification was done by ultrasound introduced from above into the melt. Microstructure photographs show decreasing of the grain size more than five times.

  3. Statistical physics of medical ultrasonic images

    International Nuclear Information System (INIS)

    Wagner, R.F.; Insana, M.F.; Brown, D.G.; Smith, S.W.

    1987-01-01

    The physical and statistical properties of backscattered signals in medical ultrasonic imaging are reviewed in terms of: 1) the radiofrequency signal; 2) the envelope (video or magnitude) signal; and 3) the density of samples in simple and in compounded images. There is a wealth of physical information in backscattered signals in medical ultrasound. This information is contained in the radiofrequency spectrum - which is not typically displayed to the viewer - as well as in the higher statistical moments of the envelope or video signal - which are not readily accessed by the human viewer of typical B-scans. This information may be extracted from the detected backscattered signals by straightforward signal processing techniques at low resolution

  4. Ultrasonication and food technology: A review

    Directory of Open Access Journals (Sweden)

    Ishrat Majid

    2015-12-01

    Full Text Available With increasing consumers demand and tightening of food and environmental regulations, traditional food-processing techniques have lost their optimum performance which gave rise to new and powerful technologies. Ultrasonic is a one of the fast, versatile, emerging, and promising non-destructive green technology used in the food industry from last few years. The ultrasound is being carried out in various areas of food technology namely crystallization, freezing, bleaching, degassing, extraction, drying, filtration, emulsification, sterilization, cutting, etc. Ultrasound is being applied as an effective preservation tool in many food-processing fields viz. vegetables and fruits, cereal products, honey, gels, proteins, enzymes, microbial inactivation, cereal technology, water treatment, diary technology, etc. This review summarizes the latest knowledge on impact and application of ultrasound in food technology.

  5. An automated method for the analysis of phenolic acids in plasma based on ion-pairing micro-extraction coupled on-line to gas chromatography/mass spectrometry with in-liner derivatisation

    NARCIS (Netherlands)

    Peters, S.; Kaal, E.; Horsting, I.; Janssen, H.-G.

    2012-01-01

    A new method is presented for the analysis of phenolic acids in plasma based on ion-pairing ‘Micro-extraction in packed sorbent’ (MEPS) coupled on-line to in-liner derivatisation-gas chromatography-mass spectrometry (GC-MS). The ion-pairing reagent served a dual purpose. It was used both to improve

  6. Hydrogen-isotope motion in scandium studied by ultrasonic measurements

    International Nuclear Information System (INIS)

    Leisure, R.G.; Schwarz, R.B.; Migliori, A.; Torgeson, D.R.; Svare, I.

    1993-01-01

    Resonant ultrasound spectroscopy has been used to investigate ultrasonic attenuation in single crystals of Sc, ScH 0.25 , and ScD 0.18 over the temperature range of 10--300 K for frequencies near 1 MHz. Ultrasonic-attenuation peaks were observed in the samples containing H or D with the maximum attenuation occurring near 25 K for ScH 0.25 and near 50 K for ScD 0.18 . The general features of the data suggest that the motion reflected in the ultrasonic attenuation is closely related to the low-temperature motion seen in nulcear-magnetic-resonance spin-lattice-relaxation measurements. The ultrasonic results were fit with a two-level-system (TLS) model involving tunneling between highly asymmetric sites. The relaxation of the TLS was found to consist of two parts: a weakly temperature-dependent part, probably due to coupling to electrons; and a much more strongly temperature-dependent part, attributed to multiple-phonon processes. The strongly temperature-dependent part was almost two orders of magnitude faster in ScH 0.25 than in ScD 0.18 , in accordance with the idea that tunneling is involved in the motion. Surprisingly, the weakly temperature-dependent part was found to be about the same for the two isotopes. The asymmetries primarily responsible for coupling the TLS to the ultrasound are attributed to interactions between hydrogen ions that lie on adjacent c axes. The results are consistent with an isotope-independent strength for the coupling of the TLS to the ultrasound

  7. Phased laser diode array permits selective excitation of ultrasonic guided waves in coated bone-mimicking tubes

    Science.gov (United States)

    Moilanen, Petro; Salmi, Ari; Kilappa, Vantte; Zhao, Zuomin; Timonen, Jussi; Hæggström, Edward

    2017-10-01

    This paper validates simulation predictions, which state that specific modes could be enhanced in quantitative ultrasonic bone testing. Tunable selection of ultrasonic guided wave excitation is useful in non-destructive testing since it permits the mediation of energy into diagnostically useful modes while reducing the energy mediated into disturbing contributions. For instance, it is often challenging to distinguish and extract the useful modes from ultrasound signals measured in bone covered by a soft tissue. We show that a laser diode array can selectively excite ultrasound in bone mimicking phantoms. A fiber-coupled diode array (4 elements) illuminated two solid tubes (2-3 mm wall thickness) embraced by an opaque soft-tissue mimicking elastomer coating (5 mm thick). A predetermined time delay matching the selected mode and frequency was employed between the outputs of the elements. The generated ultrasound was detected by a 215 kHz piezo receiver. Our results suggest that this array reduces the disturbances caused by the elastomer cover and so pave way to permit non-contacting in vivo guided wave ultrasound assessment of human bones. The implementation is small, inexpensive, and robust in comparison with the conventional pulsed lasers.

  8. Speciation of arsenic in marine food (Anemonia sulcata) by liquid chromatography coupled to inductively coupled plasma mass spectrometry and organic mass spectrometry.

    Science.gov (United States)

    Contreras-Acuña, M; García-Barrera, T; García-Sevillano, M A; Gómez-Ariza, J L

    2013-03-22

    Arsenic species have been investigated in Anemonia sulcata, which is frequently consumed food staple in Spain battered in wheat flour and fried with olive oil. Speciation in tissue extracts was carried out by anion/cation exchange chromatography with inductively coupled plasma mass spectrometry (HPLC-(AEC/CEC)-ICP-MS). Three methods for the extraction of arsenic species were investigated (ultrasonic bath, ultrasonic probe and focused microwave) and the optimal one was applied. Arsenic speciation was carried out in raw and cooked anemone and the dominant species are dimethylarsinic acid (DMA(V)) followed by arsenobetaine (AB), As(V), monomethylarsonic acid (MA(V)), tetramethylarsonium ion (TETRA) and trimethylarsine oxide (TMAO). In addition, arsenocholine (AsC), glyceryl phosphorylarsenocholine (GPAsC) and dimethylarsinothioic acid (DMAS) were identified by liquid chromatography coupled to triple quadrupole mass spectrometry (HPLC-MS). These results are interesting since GPAsC has been previously reported in marine organisms after experimental exposure to AsC, but not in natural samples. In addition, this paper reports for the first time the identification of DMAS in marine food. Copyright © 2013 Elsevier B.V. All rights reserved.

  9. 21 CFR 872.4850 - Ultrasonic scaler.

    Science.gov (United States)

    2010-04-01

    ... DEVICES DENTAL DEVICES Surgical Devices § 872.4850 Ultrasonic scaler. (a) Identification. An ultrasonic scaler is a device intended for use during dental cleaning and periodontal (gum) therapy to remove calculus deposits from teeth by application of an ultrasonic vibrating scaler tip to the teeth. (b...

  10. Pitch-catch only ultrasonic fluid densitometer

    Science.gov (United States)

    Greenwood, M.S.; Harris, R.V.

    1999-03-23

    The present invention is an ultrasonic fluid densitometer that uses a material wedge and pitch-catch only ultrasonic transducers for transmitting and receiving ultrasonic signals internally reflected within the material wedge. Density of a fluid is determined by immersing the wedge into the fluid and measuring reflection of ultrasound at the wedge-fluid interface. 6 figs.

  11. A Simple Method for the Simultaneous Determination of Pharmaceuticals and Personal Care Products in River Sediment by Ultrasound-Assisted Extraction Followed by Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Díaz, Alejandro; Peña-Alvarez, Araceli

    2017-10-01

    A simple method was developed using ultrasound-assisted extraction (UAE) combined with solid-phase microextraction (SPME) coupled with gas chromatography-mass spectrometry (GC-MS) for the simultaneous determination of eight different pharmaceuticals and personal care products (PPCPs) (ibuprofen, 2-benzyl-4-chlorophenol, naproxen, triclosan, ketoprofen, diclofenac, bisphenol A and estrone) in river sediment. UAE conditions were optimized involving extraction variables such as extraction solvent, extraction time, sample amount, extraction temperature, pH and salt addition. A 100 mg of sediment was extracted by optimized UAE process using 7 mL deionized water (pH 3) + 1% methanol as solvent, room temperature and 1 min extraction at 70% of amplitude. A 5 mL of supernatant was subsequently extracted by SPME; the extracted analytes were derivatized on fiber in head-space mode with N-methyl-N-(tertbutyldimethylsilyl) trifluoroacetamide and then analyzed by GC-MS. The developed method was evaluated by testing: precision (CV 0.98), recoveries (56-108%), limits of detection (simple and environmentally friendly, and provides straightforward analyses of these trace organic pollutants in sediment samples. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  12. Ultrasonic techniques for fluids characterization

    CERN Document Server

    Povey, Malcolm J W

    1997-01-01

    This book is a comprehensive and practical guide to the use of ultrasonic techniques for the characterization of fluids. Focusing on ultrasonic velocimetry, the author covers the basic topics and techniques necessaryfor successful ultrasound measurements on emulsions, dispersions, multiphase media, and viscoelastic/viscoplastic materials. Advanced techniques such as scattering, particle sizing, and automation are also presented. As a handbook for industrial and scientific use, Ultrasonic Techniques for Fluids Characterization is an indispensable guide to chemists and chemical engineers using ultrasound for research or process monitoring in the chemical, food processing, pharmaceutical, cosmetic, biotechnology,and fuels industries. Key Features * Appeals to anyone using ultrasound to study fluids * Provides the first detailed description of the ultrasound profiling technique for dispersions * Describes new techniques for measuring phase transitions and nucleation, such as water/ice and oil/fat * Presents the l...

  13. Ultrasonic wave propagation in powders

    Science.gov (United States)

    Al-Lashi, R. S.; Povey, M. J. W.; Watson, N. J.

    2018-05-01

    Powder clumps (cakes) has a significant effect on the flowability and stability of powders. Powder caking is mainly caused by moisture migration due to wetting and environmental (temperature and humidity) changes. The process of moisture migration caking involves creating liquid bridges between the particles during condensation which subsequently harden to form solid bridges. Therefore, an effective and reliable technique is required to quantitatively and non-invasively monitor caking kinetics and effective stiffness. This paper describes two ultrasonic instruments (ultrasonic velocity pulse and airborne ultrasound systems) that have been used to monitor the caking phenomenon. Also, it discusses the relationship between the ultrasonic velocity and attenuation measurements and tracking caking kinetics and the effective stiffness of powders.

  14. Speciation analysis of tellurium by solid-phase extraction in the presence of ammonium pyrrolidine dithiocarbamate and inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Yu, Chunhai; Cai, Qiantao; Guo, Zhong-Xian; Yang, Zhaoguang [Centre for Advanced Water Technology, Innovation Centre (NTU), Singapore (Singapore); Khoo, Soo Beng [Department of Chemistry, National University of Singapore (Singapore)

    2003-05-01

    Under acidic conditions tellurium(IV) formed a complex with ammonium pyrrolidine dithiocarbamate (APDC). The tellurium(IV) complex was completely retained on a non-polar Isolute silica-based octadecyl (C{sub 18}) sorbent-containing solid-phase extraction (SPE) cartridge, while the uncomplexed Te(VI) passed through the cartridge and remained as a free species in the solution. Only partial Te(IV) was retained on the SPE cartridge for samples without addition of APDC. On the basis of different retention behaviours of the complexed Te(IV) and uncomplexed Te(VI), a simple and highly sensitive method is proposed for the determination of total tellurium and Te(VI) by SPE separation and inductively coupled plasma mass spectrometry (ICP-MS) detection. The Te(IV) concentration was calculated as the difference between total tellurium and Te(VI) concentrations. The detection limit (3{sigma}) is 3 ng L{sup -1} tellurium. Factors affecting the separation and detection of tellurium species were investigated. Coexisting ions did not show significant interferences with the Te(IV)-APDC complex retention and the subsequent ICP-MS detection of Te. The method has been successfully applied to the tellurium speciation analysis in waters with spiked recoveries for Te(IV) and Te(VI) of 86.0-108% and 87.1-97.4%, respectively. (orig.)

  15. On-line solid-phase extraction coupled to hydrophilic interaction chromatography-mass spectrometry for the determination of polar drugs.

    Science.gov (United States)

    Fontanals, Núria; Marcé, Rosa M; Borrull, Francesc

    2011-09-02

    The present study describes the first fully automated method based on on-line solid-phase extraction (SPE) coupled to hydrophilic interaction chromatography-electrospray-mass spectrometry (HILIC-(ESI)MS) to determine a group of polar drugs that includes illicit drugs (such as cocaine, morphine, codeine and metabolites) and pharmaceuticals in environmental water samples. The SPE was performed using a highly retentive polymeric sorbent. The HILIC separation was optimised and the initial high organic content of the chromatographic mobile phase, was also suitable for the proper on-line elution of the analytes retained in the SPE column and for enhancing the ESI ionisation efficiency. This method allows the loading of samples of up to 250ml of ultrapure water or 10ml of environmental water samples spiked at low ngl(-1) levels of the analytes. The method yields near 100% recoveries for all the analytes. The method was also validated with environmental water samples with linear ranges from 5 to 1000ngl(-1) and limits of detection ≤2ngl(-1) for most of the compounds. Copyright © 2010 Elsevier B.V. All rights reserved.

  16. A Method for Multiple Mycotoxin Analysis in Wines by Solid Phase Extraction and Multifunctional Cartridge Purification, and Ultra-High-Performance Liquid Chromatography Coupled to Tandem Mass Spectrometry

    Science.gov (United States)

    Tamura, Masayoshi; Takahashi, Ayumi; Uyama, Atsuo; Mochizuki, Naoki

    2012-01-01

    An analytical method using two solid phase extractions and ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) was developed for the identification and quantification of 14 mycotoxins (patulin, deoxynivalenol, aflatoxins B1, B2, G1, G2, M1, T-2 toxin, HT-2 toxin, zearalenone, fumonisins B1, B2, B3, and ochratoxin A) in domestic and imported wines. Mycotoxins were purified with an Oasis HLB cartridge, followed by a MultiSepTM #229 Ochra. As a result, sufficient removal of the pigments and highly polar matrices from the red wines was achieved. UHPLC conditions were optimized, and 14 mycotoxins were separated in a total of 13 min. Determinations performed using this method produced high correlation coefficients for the 14 mycotoxins (R > 0.990) and recovery rates ranging from 76 to 105% with good repeatability (relative standard deviation RSD < 12%). Twenty-seven samples of domestic and imported wines were analyzed using this method. Although ochratoxin A (OTA) and fumonisins (FMs) were detected in several samples, the FM levels were less than limits of quantification (LOQs) (1 μg/L), and even the largest of the OTA levels was below the EU regulatory level (2 μg/L). These results suggest that the health risk posed to consumers from the wines available in Japan is relatively low. PMID:22822458

  17. Multiresidue pesticide analysis of tuber and root commodities by QuEchERS extraction and ultra-performance liquid chromatography coupled to tandem mass spectrometry.

    Science.gov (United States)

    Garrido Frenich, Antonia; Martín Fernández, María del Mar; Díaz Moreno, Laura; Martínez Vidal, Jose Lúis; López-Gutiérrez, Noelia

    2012-01-01

    A simple, rapid, and reliable multiresidue method to determine 84 pesticides in potato and carrot samples by ultra-performance liquid chromatography coupled to MS/MS has been developed and fully validated for routine analysis according to ISO/IEC 17025:2005. The method makes use of a buffered Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) sample preparation procedure based on a single extraction with acidified acetonitrile, followed by partitioning with salts. Chromatographic conditions were optimized in order to achieve a rapid separation in the multiple reaction monitoring mode. Performance characteristics of the method, including an estimation of measurement uncertainty using validation data, are reported for both matrixes. Calibration curves were linear from 0.010 to 0.150 mg/kg for most compounds. The LOD and LOQ were 0.006 and 0.010 mg/kg, respectively, except for fluorocloridone, fluquinconazol, and hexitiazox, which were 0.030 and 0.050 mg/kg, respectively. Recoveries obtained were in the range 70-116%, with intraday precision values < or = 20% RSD and interday precision values < or = 25% RSD at two different concentration levels. The overall uncertainty of the method was estimated at two concentrations as being lower than 34% in all cases. The method has been applied to the analysis of 70 vegetable samples, and imidacloprid and linuron were the pesticides most frequently found in potato and carrot commodities, respectively.

  18. Automated magnetic sorbent extraction based on octadecylsilane functionalized maghemite magnetic particles in a sequential injection system coupled with electrothermal atomic absorption spectrometry for metal determination.

    Science.gov (United States)

    Giakisikli, Georgia; Anthemidis, Aristidis N

    2013-06-15

    A new automatic sequential injection (SI) system for on-line magnetic sorbent extraction coupled with electrothermal atomic absorption spectrometry (ETAAS) has been successfully developed for metal determination. In this work, we reported effective on-line immobilization of magnetic silica particles into a microcolumn by the external force of two strong neodymium iron boron (NdFeB) magnets across it, avoiding the use of frits. Octadecylsilane functionalized maghemite magnetic particles were used as sorbent material. The potentials of the system were demonstrated for trace cadmium determination in water samples. The method was based on the on-line complex formation with diethyldithiocarbamate (DDTC), retention of Cd-DDTC on the surface of the MPs and elution with isobutyl methyl ketone (IBMK). The formation mechanism of the magnetic solid phase packed column and all critical parameters (chemical, flow, graphite furnace) influencing the performance of the system were optimized and offered good analytical characteristics. For 5 mL sample volume, a detection limit of 3 ng L(-1), a relative standard deviation of 3.9% at 50 ng L(-1) level (n=11) and a linear range of 9-350 ng L(-1) were obtained. The column remained stable for more than 600 cycles keeping the cost down in routine analysis. The proposed method was evaluated by analyzing certified reference materials and natural waters. Copyright © 2013 Elsevier B.V. All rights reserved.

  19. Fast quantification of short chain fatty acids and ketone bodies by liquid chromatography-tandem mass spectrometry after facile derivatization coupled with liquid-liquid extraction.

    Science.gov (United States)

    Zeng, Mingfei; Cao, Huachuan

    2018-04-15

    Short chain fatty acids (SCFA) and ketone bodies recently emerged as important physiological relevant metabolites because of their association with microbiota, immunology, obesity and other metabolic states. They were commonly analyzed by GC-MS with long run time and laborious sample preparation. In this study we developed a novel LC-MS/MS method using fast derivatization coupled with liquid-liquid extraction to detect SCFA and ketone bodies in plasma and feces. Several different derivatization reagents were evaluated to compare the efficiency, the sensitivity and chromatographic separation of structural isomers. O‑benzylhydroxylamine was selected for its superior overall performance in reaction time and isomeric separation that allowed the measurement of each SCFAs and ketone bodies free from interferences. The derivatization procedure is facile and reproducible in aqueous-organic medium, which abolished the evaporation procedure hampering the analysis of volatile short chain acids. Enhancement in sensitivity remarkably improved the detection limit of SCFA and ketone bodies to sub-fmol level. This novel method was applied to quantify these metabolites in fecal and plasma samples from lean and DIO mouse. Copyright © 2018 Elsevier B.V. All rights reserved.

  20. Microwave-assisted Extraction of Rare Earth Elements from Petroleum Refining Catalysts and Ambient Fine Aerosols Prior to Inductively Coupled Plasma - Mass Spectrometry

    Science.gov (United States)

    Mittlefehldt, David W.; Kulkarni, Pranav; Chellam, Shankar

    2006-01-01

    In the absence of a certified reference material, a robust microwave-assisted acid digestion procedure followed by inductively coupled plasma - mass spectrometry (ICP-MS) was developed to quantify rare earth elements (REEs) in fluidized-bed catalytic cracking (FCC) catalysts and atmospheric fine particulate matter (PM2.5). High temperature (200 C), high pressure (200 psig), acid digestion (HNO3, HF, and H3BO3) with 20 minute dwell time effectively solubilized REEs from six fresh catalysts, a spent catalyst, and PM2.5. This method was also employed to measure 27 non-REEs including Na, Mg, Al, Si, K, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Zr, Mo, Cd, Cs, Ba, Pb, and U. Complete extraction of several REEs (Y, La, Ce, Pr, Nd, Tb, Dy, and Er) required HF indicating that they were closely associated with the aluminosilicate structure of the zeolite FCC catalysts. Internal standardization using 115In quantitatively corrected non-spectral interferences in the catalyst digestate matrix. Inter-laboratory comparison using ICP-optical emission spectroscopy (ICP-OES) and instrumental neutron activation analysis (INAA) demonstrated the applicability of the newly developed analytical method for accurate analysis of REEs in FCC catalysts. The method developed for FCC catalysts was also successfully implemented to measure trace to ultra-trace concentrations of La, Ce, Pr, Nd, Sm, Gd, Eu, and Dy in ambient PM2.5 in an industrial area of Houston, TX.

  1. Microwave-assisted extraction of rare earth elements from petroleum refining catalysts and ambient fine aerosols prior to inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Kulkarni, Pranav; Chellam, Shankararaman; Mittlefehldt, David W.

    2007-01-01

    A robust microwave-assisted acid digestion procedure followed by inductively coupled plasma-mass spectrometry (ICP-MS) was developed to quantify rare earth elements (REEs) in fluidized-bed catalytic cracking (FCC) catalysts and atmospheric fine particulate matter (PM 2.5 ). High temperature (200 deg. C), high pressure (200 psig), acid digestion (HNO 3 , HF and H 3 BO 3 ) with 20 min dwell time effectively solubilized REEs from six fresh catalysts, a spent catalyst and PM 2.5 . This method was also employed to measure 27 non-REEs including Na, Mg, Al, Si, K, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Zr, Mo, Cd, Cs, Ba, Pb and U. Complete extraction of several REEs (Y, La, Ce, Pr, Nd, Tb, Dy and Er) required HF indicating that they were closely associated with the aluminosilicate structure of the zeolite FCC catalysts. Internal standardization using 115 In quantitatively corrected non-spectral interferences in the catalyst digestate matrix. Inter-laboratory comparison using ICP-optical emission spectroscopy (ICP-OES) and instrumental neutron activation analysis (INAA) demonstrated the applicability of the newly developed analytical method for accurate analysis of REEs in FCC catalysts. The method developed for FCC catalysts was also successfully implemented to measure trace to ultra-trace concentrations of La, Ce, Pr, Nd, Sm, Gd, Eu and Dy in ambient PM 2.5 in an industrial area of Houston, TX

  2. Determination of biocides and pesticides by on-line solid phase extraction coupled with mass spectrometry and their behaviour in wastewater and surface water

    International Nuclear Information System (INIS)

    Singer, Heinz; Jaus, Sylvia; Hanke, Irene; Lueck, Alfred; Hollender, Juliane; Alder, Alfredo C.

    2010-01-01

    This study focused on the input of hydrophilic biocides into the aquatic environment and on the efficiency of their removal in conventional wastewater treatment by a mass flux analysis. A fully automated method consisting of on-line solid phase extraction coupled to LC-ESI-MS/MS was developed and validated for the simultaneous trace determination of different biocidal compounds (1,2-benzisothiazoline-3-one (BIT), 3-Iodo-2-propynylbutyl-carbamate (IPBC), irgarol 1051 and 2-N-octyl-4-isothiazolinone (octhilinone, OIT), carbendazim, diazinon, diuron, isoproturon, mecoprop, terbutryn and terbutylazine) and pharmaceuticals (diclofenac and sulfamethoxazole) in wastewater and surface water. In the tertiary effluent, the highest average concentrations were determined for mecoprop (1010 ng/L) which was at comparable levels as the pharmaceuticals diclofenac (690 ng/L) and sulfamethoxazole (140 ng/L) but 1-2 orders of magnitude higher than the other biocidal compounds. Average eliminations for all compounds were usually below 50%. During rain events, increased residual amounts of biocidal contaminants are discharged to receiving surface waters. - Incomplete removal of biocides and pesticides during wastewater treatment.

  3. Determination of biocides and pesticides by on-line solid phase extraction coupled with mass spectrometry and their behaviour in wastewater and surface water

    Energy Technology Data Exchange (ETDEWEB)

    Singer, Heinz; Jaus, Sylvia; Hanke, Irene; Lueck, Alfred; Hollender, Juliane [Eawag, Swiss Federal Institute of Aquatic Science and Technology, Ueberlandstrasse 133, CH-8600 Duebendorf (Switzerland); Alder, Alfredo C., E-mail: alfredo.alder@eawag.c [Eawag, Swiss Federal Institute of Aquatic Science and Technology, Ueberlandstrasse 133, CH-8600 Duebendorf (Switzerland)

    2010-10-15

    This study focused on the input of hydrophilic biocides into the aquatic environment and on the efficiency of their removal in conventional wastewater treatment by a mass flux analysis. A fully automated method consisting of on-line solid phase extraction coupled to LC-ESI-MS/MS was developed and validated for the simultaneous trace determination of different biocidal compounds (1,2-benz