High performance liquid chromatographic hydrocarbon group-type analyses of mid-distillates employing fuel-derived fractions as standards

Science.gov (United States)

Seng, G. T.; Otterson, D. A.

1983-01-01

Two high performance liquid chromatographic (HPLC) methods have been developed for the determination of saturates, olefins and aromatics in petroleum and shale derived mid-distillate fuels. In one method the fuel to be analyzed is reacted with sulfuric acid, to remove a substantial portion of the aromatics, which provides a reacted fuel fraction for use in group type quantitation. The second involves the removal of a substantial portion of the saturates fraction from the HPLC system to permit the determination of olefin concentrations as low as 0.3 volume percent, and to improve the accuracy and precision of olefins determinations. Each method was evaluated using model compound mixtures and real fuel samples.

Thermal soil desorption for total petroleum hydrocarbon testing on gas chromatographs

International Nuclear Information System (INIS)

Mott, J.

1995-01-01

Testing for total petroleum hydrocarbons (TPH) is one of the most common analytical tests today. A recent development in chromatography incorporates Thermal Soil Desorption technology to enable analyses of unprepared soil samples for volatiles such as BTEX components and semi-volatiles such as diesel, PCBs, PAHs and pesticides in the same chromatogram, while in the field. A gas chromatograph is the preferred method for determining TPH because the column in a GC separates the individual hydrocarbons compounds such as benzene and toluene from each other and measures each individually. A GC analysis will determine not only the total amount of hydrocarbon, but also whether it is gasoline, diesel or another compound. TPH analysis with a GC is typically conducted with a Flame Ionization Detector (FID). Extensive field and laboratory testing has shown that incorporation of a Thermal Soil Desorber offers many benefits over traditional analytical testing methods such as Headspace, Solvent Extraction, and Purge and Trap. This paper presents the process of implementing Thermal Soil Desorption in gas chromatography, including procedures for, and advantages of faster testing and analysis times, concurrent volatile and semi-volatile analysis, minimized sample manipulation, single gas (H 2 ) operation, and detection to the part-per billion levels

High-pressure liquid chromatographic assay of Bay n 7133 in human serum.

OpenAIRE

Fasching, C E; Hughes, C E; Hector, R F; Peterson, L R

1984-01-01

A high-pressure liquid chromatographic method that includes a Sep-Pak (Waters Associates, Inc., Milford , Mass.) preparation of human serum was employed for the quantitative assay of Bay n 7133. Drug levels of 0.1 to 20 micrograms/ml could be detected. No interference from amphotericin B was found in the chromatographic analysis of Bay n 7133.

Detection of radiation-induced hydrocarbons in Camembert irradiated before and after the maturing process-comparison of florisil column chromatography and on-line coupled liquid chromatography-gas chromatography

International Nuclear Information System (INIS)

Schulzki, G.; Spiegelberg, A.; Bögl, K.W.; Schreiber, G.A.

1995-01-01

The influence of the maturing process on the detection of radiation-induced volatile hydrocarbons in the fat of Camembert has been investigated. Two analytical methods for separation of the hydrocarbon fraction from the lipid were applied: Florisil column chromatography with subsequent gas chromatographic-mass spectrometric (GC-MS) determination as well as on-line coupled liquid chromatography-GC-MS. The maturing process had no influence on the detection of radiation-induced volatiles. Comparable results were achieved with both analytical methods. However, preference is given to the more effective on-line coupled LC-GC method

Detection of radiation-induced hydrocarbons in irradiated fish and prawns by means of on-line coupled liquid chromatography-gas chromatography

International Nuclear Information System (INIS)

Schulzki, G.; Spiegelberg, A.; Bogl, K.W.; Schreiberg, G.A.

1997-01-01

Radiation-induced hydrocarbons were analyzed in a fatty (halibut) and a lean fish (cod) as well as in a prawn species by on-line coupled liquid chromatography (LC) -gas chromatography (GC) combined with mass spectrometry. In irradiated halibut which is known to contain mainly saturated and monounsaturated fatty acids, all expected radiolytic alkanes, alkenes, and alkadienes could be detected. The yields of the C(n-1) and C(n-2:1) hydrocarbons were comparable to those found in irradiated lipids of terrestrial animals and plants. However, in cod and prawns which contain high levels of polyunsaturated fatty acids (PUFA), the C(n-1) hydrocarbons were found in concentrations which were up to 10 times higher whereas the C(n-2:1) products were again comparable to those of terrestrial animals and plants. The identification of radiation-induced hydrocarbons in fish lipids was achieved by transfer of the hydrocarbons from the LC column to the gas chromatographic column in fractions differing in their degree of unsaturation. For the first time, radiation-induced hydrocarbons with more than four double bonds generated from polyunsaturated fatty acids (20:4 omega 6 and 20:5 omega 3) could be identified

Formation of hydrocarbons in irradiated Brazilian beans: gas chromatographic analysis to detect radiation processing

International Nuclear Information System (INIS)

Villavicencio, A.L.C.H.; Mancini-Filho, J.; Hartmann, M.; Ammon, J.; Delincee, H.

1997-01-01

Radiation processing of beans, which are a major source of dietary protein in Brazil, is a valuable alternative to chemical fumigation to combat postharvest losses due to insect infestation. To ensure free consumer choice, irradiated food will be labeled as such, and to enforce labeling, analytical methods to detect the irradiation treatment in the food product itself are desirable. In two varieties of Brazilian beans, Carioca and Macacar beans, the radiolytic formation of hydrocarbons formed after alpha and beta cleavage, with regard to the carbonyl group in triglycerides, have been studied. Using gas chromatographic analysis of these radiolytic hydrocarbons, different yields per precursor fatty acid are observed for the two types of beans. However, the typical degradation pattern allows the identification of the irradiation treatment in both bean varieties, even after 6 months of storage

Catalytic conversion of carboxylic acids in bio-oil for liquid hydrocarbons production

International Nuclear Information System (INIS)

Wang, Shurong; Guo, Zuogang; Cai, Qinjie; Guo, Long

2012-01-01

Bio-oil must be upgraded to be suitable for use as a high-grade transport fuel. Crude bio-oil has a high content of carboxylic acids which can cause corrosion, and the high oxygen content of these acids also reduces the oil’s heating value. In this paper, acetic acid and propanoic acid were chosen as the model carboxylic acids in bio-oil. Their behavior in the production of liquid hydrocarbons during a catalytic conversion process was investigated in a micro-fixed bed reactor. The liquid organic phase from this catalytic conversion process mainly consisted of liquid hydrocarbons and phenol derivatives. Under the condition of low Liquid Hourly Space Velocity (LHSV), the liquid organic phase from acetic acid cracking had a selectivity of 22% for liquid hydrocarbons and a selectivity of 65% for phenol derivatives. The composition of the organic products changed considerably with the LHSV increasing to 3 h −1 . The selectivity for liquid hydrocarbons increased up to 52% while that for phenol derivatives decreased to 32%. Propanoic acid performed much better in producing liquid hydrocarbons than acetic acid. Its selectivity for liquid hydrocarbons was as high as 80% at LHSV = 3 h −1 . A mechanism for this catalytic conversion process was proposed according to the analysis of the components in the liquid organic phases. The pathways of the main compounds formation in the liquid organic phases were proposed, and the reason why liquid hydrocarbons were more effectively produced when using propanoic acid rather than acetic acid was also successfully explained. In addition, BET and SEM characterization were used to analyze the catalyst coke deposition. -- Graphical abstract: Display Omitted Highlights: ► High content of carboxylic acids in bio-oil causes its corrosiveness. ► Acetic acid and propanoic acid are two dominant acids in bio-oil. ► Liquid hydrocarbons were produced by cracking of these two dominant acids. ► A mechanism model was proposed to explain

Process for recovery of liquid hydrocarbons

Energy Technology Data Exchange (ETDEWEB)

Millar, J.F.; Cockshott, J.E.

1978-04-11

Methane is recovered as a gas for discharge to a pipeline from a gas stream containing methane and heavier hydrocarbons, principally ethane and propane. Separation is accomplished by condensing the heavier hydrocarbons and distilling the methane therefrom. A liquid product (LPG) comprising the heavier hydrocarbons is subsequently recovered and transferred to storage. Prior to being discharged to a pipeline, the recovered methane gas is compressed and in undergoing compression the gas is heated. The heat content of the gas is employed to reboil the refrigerant in an absorption refrigeration unit. The refrigeration unit is used to cool the LPG prior to its storage.

The reformation of liquid hydrocarbons in an aqueous discharge reactor

International Nuclear Information System (INIS)

Zhang, Xuming; Cha, Min Suk

2015-01-01

We present an aqueous discharge reactor for the reformation of liquid hydrocarbons. To increase a dielectric constant of a liquid medium, we added distilled water to iso-octane and n-dodecane. As expected, we found decreased discharge onset voltage and increased discharge power with increased water content. Results using optical emission spectroscopy identified OH radicals and O atoms as the predominant oxidative reactive species with the addition of water. Enriched CH radicals were also visualized, evidencing the existence of cascade carbon–carbon cleavage and dehydrogenation processes in the aqueous discharge. The gaseous product consisted primarily of hydrogen, carbon monoxide, and unsaturated hydrocarbons. The composition of the product was readily adjustable by varying the volume of water added, which demonstrated a significant difference in composition with respect to the tested liquid hydrocarbon. In this study, we found no presence of CO 2 emissions or the contamination of the reactor by solid carbon deposition. These findings offer a new approach to the reforming processes of liquid hydrocarbons and provide a novel concept for the design of a practical and compact plasma reformer. (paper)

The reformation of liquid hydrocarbons in an aqueous discharge reactor

KAUST Repository

Zhang, Xuming

2015-04-21

We present an aqueous discharge reactor for the reformation of liquid hydrocarbons. To increase a dielectric constant of a liquid medium, we added distilled water to iso-octane and n-dodecane. As expected, we found decreased discharge onset voltage and increased discharge power with increased water content. Results using optical emission spectroscopy identified OH radicals and O atoms as the predominant oxidative reactive species with the addition of water. Enriched CH radicals were also visualized, evidencing the existence of cascade carbon-carbon cleavage and dehydrogenation processes in the aqueous discharge. The gaseous product consisted primarily of hydrogen, carbon monoxide, and unsaturated hydrocarbons. The composition of the product was readily adjustable by varying the volume of water added, which demonstrated a significant difference in composition with respect to the tested liquid hydrocarbon. In this study, we found no presence of CO2 emissions or the contamination of the reactor by solid carbon deposition. These findings offer a new approach to the reforming processes of liquid hydrocarbons and provide a novel concept for the design of a practical and compact plasma reformer. © 2015 IOP Publishing Ltd.

Radiolysis of hydrocarbons in liquid phase (Modern state of problem)

International Nuclear Information System (INIS)

Saraeva, V.V.

1986-01-01

Problems of ionizing radiation effect on hydrocarbons and hydrocarbon systems in a liquid phase are considered. Modern representations on the mechanism of hydrocarbon radiolysis are presented. Electron moderation and ion-electron pair formation, behaviour of charged particles, excited states, radical formation and their reactions are discussed. Behaviour of certain hydrocarbon classes: alkanes, cyclic hydrocarbons, olefines, aromatic hydrocarbons as well as different hydrocarbon mixtures is considered in detail. Radiation-chemical changes in organic coolants and ways of increasing radiation resistance are considered. Polyphenyl compounds are noted to be most perspective here

High-performance liquid-chromatographic separation of subcomponents of antimycin-A

Science.gov (United States)

Abidi, S.L.

1988-01-01

Using a reversed-phase high-performance liquid chromatographic (HPLC) technique, a mixture of antimycins A was separated into eight hitherto unreported subcomponents, Ala, Alb, A2a, A2b, A3a, A3b, A4a, and A4b. Although a base-line resolution of the known four major antimycins Al, A2, A3, and A4 was readily achieved with mobile phases containing acetate buffers, the separation of the new antibiotic subcomponents was highly sensitive to variation in mobile phase conditions. The type and composition of organic modifiers, the nature of buffer salts, and the concentration of added electrolytes had profound effects on capacity factors, separation factors, and peak resolution values. Of the numerous chromatographic systems examined, a mobile phase consisting of methanol-water (70:30) and 0.005 M tetrabutylammonium phosphate at pH 3.0 yielded the most satisfactory results for the separation of the subcomponents. Reversed-phase gradient HPLC separation of the dansylated or methylated antibiotic compounds produced superior chromatographic characteristics and the presence of added electrolytes was not a critical factor for achieving separation. Differences in the chromatographic outcome between homologous and structural isomers were interpretated based on a differential solvophobic interaction rationale. Preparative reversed-phase HPLC under optimal conditions enabled isolation of pure samples of the methylated antimycin subcomponents for use in structural studies.

Stereospecific high-performance liquid chromatographic assay of sotalol in plasma.

Science.gov (United States)

Carr, R A; Foster, R T; Bhanji, N H

1991-09-01

A convenient high-performance liquid chromatographic (HPLC) assay was developed for determination of sotalol (STL) enantiomers in plasma. Following addition of the internal standard (IS; racemic atenolol), enantiomers of STL and IS were extracted using ethyl acetate. After evaporation of the organic layer, samples were derivatized with a solution of S-(+)-1-(1-naphthyl)ethyl isocyanate (NEIC). The resulting diastereomers were chromatographed with normal-phase HPLC with chloroform:hexane:methanol [65:33:2 (v/v)] as the mobile phase at a flow rate of 2 ml/min. The fluorescence detection wavelength was set at 220 nm for excitation with no emission filter. The suitability of the assay for pharmacokinetic studies was determined by measuring STL enantiomers in the plasma of a healthy subject after administration of a single 160-mg oral, racemic dose of STL.

Supercooled liquid vapour pressures and related thermodynamic properties of polycyclic aromatic hydrocarbons determined by gas chromatography.

Science.gov (United States)

Haftka, Joris J H; Parsons, John R; Govers, Harrie A J

2006-11-24

A gas chromatographic method using Kováts retention indices has been applied to determine the liquid vapour pressure (P(i)), enthalpy of vaporization (DeltaH(i)) and difference in heat capacity between gas and liquid phase (DeltaC(i)) for a group of polycyclic aromatic hydrocarbons (PAHs). This group consists of 19 unsubstituted, methylated and sulphur containing PAHs. Differences in log P(i) of -0.04 to +0.99 log units at 298.15K were observed between experimental values and data from effusion and gas saturation studies. These differences in log P(i) have been fitted with multilinear regression resulting in a compound and temperature dependent correction. Over a temperature range from 273.15 to 423.15K, differences in corrected log P(i) of a training set (-0.07 to +0.03 log units) and a validation set (-0.17 to 0.19 log units) were within calculated error ranges. The corrected vapour pressures also showed a good agreement with other GC determined vapour pressures (average -0.09 log units).

Incorporation of ionic liquid into porous polymer monoliths to enhance the separation of small molecules in reversed-phase high-performance liquid chromatography.

Science.gov (United States)

Wang, Jiafei; Bai, Ligai; Wei, Zhen; Qin, Junxiao; Ma, Yamin; Liu, Haiyan

2015-06-01

An ionic liquid was incorporated into the porous polymer monoliths to afford stationary phases with enhanced chromatographic performance for small molecules in reversed-phase high-performance liquid chromatography. The effect of the ionic liquid in the polymerization mixture on the performance of the monoliths was studied in detail. While monoliths without ionic liquid exhibited poor resolution and low efficiency, the addition of ionic liquid to the polymerization mixture provides highly increased resolution and high efficiency. The chromatographic performances of the monoliths were demonstrated by the separations of various small molecules including aromatic hydrocarbons, isomers, and homologues using a binary polar mobile phase. The present column efficiency reached 27 000 plates/m, which showed that the ionic liquid monoliths are alternative stationary phases in the separation of small molecules by high-performance liquid chromatography. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The combination of the liquid chromatograph with the nuclear magnetic resonance spectrometer

International Nuclear Information System (INIS)

Scott, R.P.W.

1986-01-01

The association of the liquid chromatograph with the NMR spectrometer would be a very powerful analytical system for the separation and identification of unknown mixtures. There are, however, some serious difficulties involved with the association of these two techniques. The historical development of NMR chromatography is outlined and some problems are discussed. (Auth.)

Comparison of core-shell and totally porous ultra high performance liquid chromatographic stationary phases based on their selectivity towards alfuzosin compounds.

Science.gov (United States)

Szulfer, Jarosław; Plenis, Alina; Bączek, Tomasz

2014-06-13

This paper focuses on the application of a column classification system based on the Katholieke Universiteit Leuven for the characterization of physicochemical properties of core-shell and ultra-high performance liquid chromatographic stationary phases, followed by the verification of the reliability of the obtained column classification in pharmaceutical practice. In the study, 7 stationary phases produced in core-shell technology and 18 ultra-high performance liquid chromatographic columns were chromatographically tested, and ranking lists were built on the FKUL-values calculated against two selected reference columns. In the column performance test, an analysis of alfuzosin in the presence of related substances was carried out using the brands of the stationary phases with the highest ranking positions. Next, a system suitability test as described by the European Pharmacopoeia monograph was performed. Moreover, a study was also performed to achieve a purposeful shortening of the analysis time of the compounds of interest using the selected stationary phases. Finally, it was checked whether methods using core-shell and ultra-high performance liquid chromatographic columns can be an interesting alternative to the high-performance liquid chromatographic method for the analysis of alfuzosin in pharmaceutical practice. Copyright © 2014 Elsevier B.V. All rights reserved.

High-performance liquid chromatographic method for guanylhydrazone compounds.

Science.gov (United States)

Cerami, C; Zhang, X; Ulrich, P; Bianchi, M; Tracey, K J; Berger, B J

1996-01-12

A high-performance liquid chromatographic method has been developed for a series of aromatic guanylhydrazones that have demonstrated therapeutic potential as anti-inflammatory agents. The compounds were separated using octadecyl or diisopropyloctyl reversed-phase columns, with an acetonitrile gradient in water containing heptane sulfonate, tetramethylammonium chloride, and phosphoric acid. The method was used to reliably quantify levels of analyte as low as 785 ng/ml, and the detector response was linear to at least 50 micrograms/ml using a 100 microliters injection volume. The assay system was used to determine the basic pharmacokinetics of a lead compound, CNI-1493, from serum concentrations following a single intravenous injection in rats.

Gas-liquid chromatographic determination of resmethrin in corn, cornmeal, flour, and wheat.

Science.gov (United States)

Simonaitis, R A; Cail, R S

1975-09-01

A gas-liquid chromatographic (GLC) method was developed for the determination of residues of resmethrin ((5-benzyl-3-furyl)methyl cis-trans-(+/-)-2,2-dimethyl-3-(2-methylpropenyl)-cyclopropanecarboxylate) in corn, cornmeal, flour, and wheat. The commodity, fortified with resmethrin, was extracted by tumbling with pentane and transferred to acetonitrile, the fat was partitioned off, and the sample was chromatographed with 3% ethyl acetate in pentane on Florisil containing 0.5% water. The resmethrin residue was determined by GLC with a flame ionization detector. The results were compared with known standards that had undergone the same cleanup procedures. The method was sensitive to concentrations of resmethrin to 0.2 ppm, recoveries averaged 83%, and reproducibility was good.

Motor fuels by hydrogenation of liquid hydrocarbons

Energy Technology Data Exchange (ETDEWEB)

1938-05-07

A process is disclosed for the production of knock-stable low-boiling motor fuels by conversion of liquid hydrocarbons which are vaporizable under the reaction conditions, which comprises passing the initial material at a temperature above 380/sup 0/C in a true vapor phase under pressure of more than 40 atmospheres together with hydrogen and gaseous hydrocarbons containing more than 1 carbon atom in the molecule in an amount by volume larger than that of the hydrogen over catalysts stable to poisoning stationarily confined in the reaction vessel.

Influence of adhesion on aerobic biodegradation and bioremediation of liquid hydrocarbons.

Science.gov (United States)

Abbasnezhad, Hassan; Gray, Murray; Foght, Julia M

2011-11-01

Biodegradation of poorly water-soluble liquid hydrocarbons is often limited by low availability of the substrate to microbes. Adhesion of microorganisms to an oil-water interface can enhance this availability, whereas detaching cells from the interface can reduce the rate of biodegradation. The capability of microbes to adhere to the interface is not limited to hydrocarbon degraders, nor is it the only mechanism to enable rapid uptake of hydrocarbons, but it represents a common strategy. This review of the literature indicates that microbial adhesion can benefit growth on and biodegradation of very poorly water-soluble hydrocarbons such as n-alkanes and large polycyclic aromatic hydrocarbons dissolved in a non-aqueous phase. Adhesion is particularly important when the hydrocarbons are not emulsified, giving limited interfacial area between the two liquid phases. When mixed communities are involved in biodegradation, the ability of cells to adhere to the interface can enable selective growth and enhance bioremediation with time. The critical challenge in understanding the relationship between growth rate and biodegradation rate for adherent bacteria is to accurately measure and observe the population that resides at the interface of the hydrocarbon phase. © Springer-Verlag 2011

Storing of Extracts in Polypropylene Microcentrifuge Tubes Yields Contaminant Peak During Ultra-flow Liquid Chromatographic Analysis.

Science.gov (United States)

Kshirsagar, Parthraj R; Hegde, Harsha; Pai, Sandeep R

2016-05-01

This study was designed to understand the effect of storage in polypropylene microcentrifuge tubes and glass vials during ultra-flow liquid chromatographic (UFLC) analysis. One ml of methanol was placed in polypropylene microcentrifuge tubes (PP material, Autoclavable) and glass vials (Borosilicate) separately for 1, 2, 4, 8, 10, 20, 40, and 80 days intervals stored at -4°C. Contaminant peak was detected in methanol stored in polypropylene microcentrifuge tubes using UFLC analysis. The contaminant peak detected was prominent, sharp detectable at 9.176 ± 0.138 min on a Waters 250-4.6 mm, 4 μ, Nova-Pak C18 column with mobile phase consisting of methanol:water (70:30). It was evident from the study that long-term storage of biological samples prepared using methanol in polypropylene microcentrifuge tubes produce contaminant peak. Further, this may mislead in future reporting an unnatural compound by researchers. Long-term storage of biological samples prepared using methanol in polypropylene microcentrifuge tubes produce contaminant peakContamination peak with higher area under the curve (609993) was obtained in ultra-flow liquid chromatographic run for methanol stored in PP microcentrifuge tubesContamination peak was detected at retention time 9.113 min with a lambda max of 220.38 nm and 300 mAU intensity on the given chromatographic conditionsGlass vials serve better option over PP microcentrifuge tubes for storing biological samples. Abbreviations used: UFLC: Ultra Flow Liquid Chromatography; LC: Liquid Chromatography; MS: Mass spectrometry; AUC: Area Under Curve.

Recovering valuable liquid hydrocarbons

Energy Technology Data Exchange (ETDEWEB)

Pier, M

1931-06-11

A process for recovering valuable liquid hydrocarbons from coking coal, mineral coal, or oil shale through treatment with hydrogen under pressure at elevated temperature is described. Catalysts and grinding oil may be used in the process if necessary. The process provides for deashing the coal prior to hydrogenation and for preventing the coking and swelling of the deashed material. During the treatment with hydrogen, the coal is either mixed with coal low in bituminous material, such as lean coal or active coal, as a diluent or the bituminous constituents which cause the coking and swelling are removed by extraction with solvents. (BLM)

Liquid chromatographic and spectrophotometric methods for the determination of erythromycin stearate and trimethoprim in tablets

OpenAIRE

Hassib, Sonia T.; Farag, Awatef E.; Elkady, Ehab F.

2011-01-01

Simple, accurate and precise reversed-phase liquid chromatographic (LC) and spectrophotometric methods have been developed and validated for the determination of erythromycin stearate (ERS) and trimethoprim (TMP) in mixture. In LC method, chromatographic separation was achieved on a Symmetry® Waters C18 column (150 × 4.6 mm, 5 μm) based on isocratic elution using a mobile phase consisting of potassium dihydrogen phosphate buffer pH (9):acetonitrile:water (25:100:50, v/v/v) at a flow rate of 1...

Liquid chromatographic separation of terpenoid pigments in foods and food products.

Science.gov (United States)

Cserháti, T; Forgács, E

2001-11-30

The newest achievements in the use of various liquid chromatographic techniques such as adsorption and reversed-phase thin-layer chromatography and HPLC employed for the separation and quantitative determination of terpenoid-based color substances in foods and food products are reviewed. The techniques applied for the analysis of individual pigments and pigments classes are surveyed and critically evaluated. Future trends in the separation and identification of pigments in foods and food products are delineated.

Method of cleansing and refining of liquid hydrocarbons and derivatives of hydrocarbons

Energy Technology Data Exchange (ETDEWEB)

Hahn, C A; Nielsen, H

1934-10-11

A process is described for cleaning and refining liquid hydrocarbons and derivatives by utilization of acids, followed by washing partly with a basic solution, partly with clean water. The process is characterized by using, in connection with the acid solutions mentioned, a strong solution of a mixture of sulfuric acid and phosphoric acid.

High Performance Liquid Chromatographic Analysis of Phytoplankton Pigments Using a C16-Amide Column

Science.gov (United States)

A reverse-phase high performance liquid chromatographic (RP-HPLC) method was developed to analyze in a single run, most polar and non-polar chlorophylls and carotenoids from marine phytoplankton. The method is based on a RP-C16-Amide column and a ternary gradient system consistin...

Decomposition of pilocarpine eye drops assessed by a highly efficient high pressure liquid chromatographic method

NARCIS (Netherlands)

Kuks, P. F.; Weekers, L. E.; Goldhoorn, P. B.

1990-01-01

A rapid high-resolution high pressure liquid chromatographic method was developed for assaying pilocarpine. Pilocarpine in ophthalmic solutions decomposes fairly rapidly to give isopilocarpine, pilocarpic acid and isopilocarpic acid. The quality of an ophthalmic solution can be assessed by assaying

Sample enrichment for gas chromatographic mass spectrometric analysis of polynuclear aromatic hydrocarbons in water and in organic mixtures

Energy Technology Data Exchange (ETDEWEB)

Bruner, F.; Furlani, G.; Mangani, F.

1984-10-19

Among the extraction and preconcentration steps used for polynuclear aromatic hydrocarbons, Soxhlet extraction is largely used for atmospheric dust or other solid material, while liquid-liquid extraction is the method which has been suggested for extraction from water. The use of graphitized carbon black for liquid-solid extraction and preconcentration from water was explored. The properties of different kinds of graphitized carbon black as traps for the extraction and preconcentration of polynuclear aromatic hydrocarbons from water and mineral oil were determined. The best results were obtained with Carbopack F, eluted with toluene at 100 C. Graphitized carbon black is preferred because of its thermal and chemical stability and its high purity, exhibiting no bleeding and possessing high sensitivity. 9 references, 2 figures, 2 tables.

Determination of aromatic and PAH (polycyclic aromatic hydrocarbons) content of oily wastewaters

Energy Technology Data Exchange (ETDEWEB)

Lysyj, I.; Russell, E.C.

1978-08-01

An analytical scheme was developed for determining the total organic content and hydrocarbon concentration from a one-liter portion of a wastewater sample, and determining the volatile, suspended, and water-soluble fractions from a second, two-liter portion. Analyses of untreated and treated bilge wastewater from the U.S. Army Fort Eustis, Va., facility showed 10-300 ppm suspended organics and 10-300 ppm dissolved organics in the untreated bilge, and no suspended matter, but 700-2000 ppm dissolved organics, in the treated bilge wastewaters. Of the dissolved organics in untreated and treated wastewater, 70 and 10%, respectively, were extracted with chloroform; the organics in the treated water were probably biologically derived from petroleum degradation. Gas chromatographic/mass spectroscopic and high-pressure liquid chromatographic analyses of the chloroform extracts showed about equal parts of phenolic compounds and aromatic hydrocarbons, small amounts of heterocyclics, and traces of polycyclic aromatics in the untreated wastewater, and mainly phenolics in the treated water.

Absorbent agents for clean-up of liquid hydrocarbons

International Nuclear Information System (INIS)

Waldmann, J.J.

1993-01-01

A method is described for absorbing liquid hydrocarbon from a liquid hydrocarbon-contaminated substrate comprising applying to said contaminated substrate an effective amount of a chemical absorbent composition of formula: A m B n C p wherein A m is an acid leached bentonite in a form of hydrous silicate of alumina modified by a hydrophobic alkyl (C 12 -C 24 ) amine which has been double protonized by an aliphatic acid with C 1 -C 18 carbon atoms in which m = 0 to 100% by weight of the composition; B n is a modified aminoplast resin comprised of cyanoguanidine-melamine-urea-formaldehyde in a foam form in which n is 0 to 100% by weight; and C p is a siliceous support-modified hydrophobic material in which p is 0 to 100% by weight; provided that at least one of m and n is a positive numerical value

Hydro-carbon liquid for use in motors

Energy Technology Data Exchange (ETDEWEB)

Cobbett, G T.B.

1907-03-15

A process for the manufacture of liquid hydro-carbon mixtures suitable as a fuel for internal-combustion engines is disclosed, which consists in dissolving a suitable quantity of shale oil, which has been purified with sulfuric acid, in petroleum spirit, then purifying the solution with sulfuric acid and subsequently with oxalic acid or other suitable decolorizing agent.

Methods of producing alkylated hydrocarbons from an in situ heat treatment process liquid

Science.gov (United States)

Roes, Augustinus Wilhelmus Maria [Houston, TX; Mo, Weijian [Sugar Land, TX; Muylle, Michel Serge Marie [Houston, TX; Mandema, Remco Hugo [Houston, TX; Nair, Vijay [Katy, TX

2009-09-01

A method for producing alkylated hydrocarbons is disclosed. Formation fluid is produced from a subsurface in situ heat treatment process. The formation fluid is separated to produce a liquid stream and a first gas stream. The first gas stream includes olefins. The liquid stream is fractionated to produce at least a second gas stream including hydrocarbons having a carbon number of at least 3. The first gas stream and the second gas stream are introduced into an alkylation unit to produce alkylated hydrocarbons. At least a portion of the olefins in the first gas stream enhance alkylation.

Gas condensate--raw material for producing liquid paraffin hydrocarbons

Energy Technology Data Exchange (ETDEWEB)

Aliyeva, R.B.; Alikishi-Zade, G.Yu.; Kuliyev, A.M.; Leonidov, A.N.; Pereverzev, A.N.

1980-01-01

The problem of efficient utilization of gas condensates as raw material for removal of a valuable product, liquid paraffins, is examined. A classification of gas condensates is given which is used as raw material for removing these hydrocarbons: gas condensate with high content of n-alkanes (25-40 mass percent), with average content (18-25 mass percent), with low content (12-18 mass percent), light weight fractions compositions, which do not contain fractions up to 200/sup 0/, and also, content ofless than 12% n-alkanes. Gas condensate I-III groups are 30% of the total reserve of gas condensate. Liquid paraffins hydrocarbons, produced from fractions of diesel fuel, which has been removed from Shatlyk gas condensate under conditions which simulate virtual processes of caramide deparaffinization meet all requirements without additional refining.

Investigation of Factors Influencing Dispersion of Liquid Hydrocarbons in Porous Media

Directory of Open Access Journals (Sweden)

Hussain Ali Baker

2016-08-01

Full Text Available An experimental work has been done to study the major factors that affect the axial dispersion of some hydrocarbons during liquid-liquid miscible displacement. Kerosene and gas oil are used as displacing phase while seven liquid hydrocarbons of high purity represent the displaced phase, three of the liquids are aromatics and the rest are of paraffinic base. In conducting the experiments, two packed beds of different porosity and permeability are used as porous media. The results showed that the displacement process is not a piston flow, breakthrough of displacing fluids are shown before one pore volume has been injected. The processes are stable with no evidence of viscous fingering. Dispersion model as adapted by Brigham et.al (1961 is used to determine the axial dispersion coefficient of displacing fluid. The results show an increasing in dispersion coefficient as the interstitial velocity and viscosity ratio increases.

Liquid-liquid equilibria for binary and ternary systems containing glycols, aromatic hydrocarbons, and water: Experimental measurements and modeling with the CPA EoS

DEFF Research Database (Denmark)

Folas, Georgios; Kontogeorgis, Georgios; Michelsen, Michael Locht

2006-01-01

Liquid-liquid equilibrium data of four binary glycol + aromatic hydrocarbon systems and three ternary systems containing water have been measured at atmospheric pressure. The measured systems are monoethylene glycol (MEG) + benzene or toluene, triethylene glycol (TEG) + benzene or toluene, MEG...... + water + benzene, MEG + water + toluene, and TEG + water + toluene. The binary systems are correlated with the Cubic-Plus-Association (CPA) equation of state while the ternary systems are predicted from interaction parameters obtained from the binary systems. Very satisfactory liquid-liquid equilibrium...... correlations are obtained for the binary systems using temperature-independent interaction parameters, while adequate predictions are achieved for multicomponent water + glycol + aromatic hydrocarbons systems when accounting for the solvation between the aromatic hydrocarbons and glycols or water....

New Insight into the Kinetics of Deep Liquid Hydrocarbon Cracking and Its Significance

Directory of Open Access Journals (Sweden)

Wenzhi Zhao

2017-01-01

Full Text Available The deep marine natural gas accumulations in China are mainly derived from the cracking of liquid hydrocarbons with different occurrence states. Besides accumulated oil in reservoir, the dispersed liquid hydrocarbon in and outside source also is important source for cracking gas generation or relayed gas generation in deep formations. In this study, nonisothermal gold tube pyrolysis and numerical calculations as well as geochemical analysis were conducted to ascertain the expulsion efficiency of source rocks and the kinetics for oil cracking. By determination of light liquid hydrocarbons and numerical calculations, it is concluded that the residual bitumen or hydrocarbons within source rocks can occupy about 50 wt.% of total oil generated at oil generation peak. This implies that considerable amounts of natural gas can be derived from residual hydrocarbon cracking and contribute significantly to the accumulation of shale gas. Based on pyrolysis experiments and kinetic calculations, we established a model for the cracking of oil and its different components. In addition, a quantitative gas generation model was also established to address the contribution of the cracking of residual oil and expulsed oil for natural gas accumulations in deep formations. These models may provide us with guidance for gas resource evaluation and future gas exploration in deep formations.

High-performance liquid chromatographic analysis of methadone hydrochloride oral solution.

Science.gov (United States)

Beasley, T H; Ziegler, H W

1977-12-01

A direct and rapid high-performance liquid chromatographic assay for methadone hydrochloride in a flavored oral solution dosage form is described. A syrup sample, one part diluted with three parts of water, is introduced onto a column packed with octadecylsilane bonded on 10 micrometer porous silica gel (reversed phase). A formic acid-ammonium formate-buffered mobile phase is linear programmed with acetonitrile. The absorbance is monitored continuously at 280 or 254 nm, using a flow-through, UV, double-beam photometer. An aqueous methadone hydrochloride solution is used for external standardization. The relative standard deviation was not more than 1.0%. Drug recovery from a syrup base was better than 99.8%.

Improvement of mineral oil saturated and aromatic hydrocarbons determination in edible oil by liquid-liquid-gas chromatography with dual detection.

Science.gov (United States)

Zoccali, Mariosimone; Barp, Laura; Beccaria, Marco; Sciarrone, Danilo; Purcaro, Giorgia; Mondello, Luigi

2016-02-01

Mineral oils, which are mainly composed of saturated hydrocarbons and aromatic hydrocarbons, are widespread food contaminants. Liquid chromatography coupled to gas chromatography with flame ionization detection represents the method of choice to determine these two families. However, despite the high selectivity of this technique, the presence of olefins (particularly squalene and its isomers) in some samples as in olive oils, does not allow the correct quantification of the mineral oil aromatic hydrocarbons fraction, requiring additional off-line tools to eliminate them. In the present research, a novel on-line liquid chromatography coupled to gas chromatography method is described for the determination of hydrocarbon contamination in edible oils. Two different liquid chromatography columns, namely a silica one (to retain the bulk of the matrix) and a silver-ion one (which better retains the olefins), were coupled in series to obtain the mineral oil aromatic hydrocarbons hump free of interfering peaks. Furthermore, the use of a simultaneous dual detection, flame ionization detector and triple quadrupole mass spectrometer allowed us not only to quantify the mineral oil contamination, but also to evaluate the presence of specific markers (i.e. hopanes) to confirm the petrogenic origin of the contamination. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Liquid chromatographic determination of saccharin in beverages and desserts: complementary collaborative study.

Science.gov (United States)

Sjöberg, A M

1988-01-01

A complementary collaborative study was conducted on a liquid chromatographic method for determination of saccharin in accordance with the latest international recommendations. One industrial and 6 official food control laboratories analyzed 3 samples of a juice, a soft drink, and a dessert at concentration levels of 26-90 mg/L, 33-73 mg/L, and 56-147 mg/kg, respectively. Blind duplicates and a blank were supplied for each type of material at each concentration level. The beverage was chromatographed directly and the dessert was extracted with ethanol before chromatography. Average recoveries were 95-107%. The reproducibility relative standard deviations were 6.4-7.3% for the juice, 9.2-20.6% for the soft drink, and 13.4-16.2% for the dessert. The outlier percentage was 14.3%. The results were compared with those of an earlier collaborative study by Nordic laboratories and with general collaborative results obtained by AOAC.

Sorption and chromatographic techniques for processing liquid waste of nuclear fuel cycle

International Nuclear Information System (INIS)

Gelis, V.M.; Milyutin, V.V.; Chuveleva, E.A.; Maslova, G.B.; Kudryavtseva, S.P.; Firsova, L.A.; Kozlitin, E.A.

2000-01-01

In the spent nuclear fuel processing procedures the significant quantity of high level liquid waste containing long-lived high toxic radionuclides of cesium, strontium, promethium, americium, curium, etc. is generated. Separation of those radionuclides from the waste not merely simplifies the further safe waste handling but also reduces the waste processing operation costs due to the market value of certain individual radionuclide preparations. Recovery and separation of high grade pure long-lived radionuclide preparations is frequently performed by means of chromatographic techniques. (authors)

Valorization of biogas into liquid hydrocarbons in plasma-catalyst reactor

Science.gov (United States)

Nikravech, Mehrdad; Rahmani, Abdelkader; Labidi, Sana; Saintini, Noiric

2016-09-01

Biogas represents an important source of renewable energy issued from biological degradation of biomass. It is planned to produce in Europe the amount of biogas equivalent to 6400 kWh electricity and 4500 kteo (kilo tons equivalent oil) in 2020. Currently the biogas is used in cogeneration engines to produce heat and electricity directly in farms or it is injected in gas networks after purification and odorisation. The aim of this work is to propose a third option that consists of valorization of biogas by transformation into liquid hydrocarbons like acetone, methanol, ethanol, acetic acid etc. These chemicals, among the most important feed materials for chemical industries, retain CO2 molecules participating to reduce the greenhouse gas emissions and have high storage energy capacity. We developed a low temperature atmospheric plasma-catalyst reactor (surface dielectric barrier discharge) to transform biogas into chemicals. The conversion rates of CH4 and CO2 are respectively about 50% and 30% depending on operational conditions. The energetic cost is 25 eV/molecule. The yields of liquid hydrocarbon reaches currently 10% wt. More the 11 liquid chemicals are observed in the liquid fraction. Acknowledgements are due to SPC Programme Energie de demain.

Chemometric strategy for automatic chromatographic peak detection and background drift correction in chromatographic data.

Science.gov (United States)

Yu, Yong-Jie; Xia, Qiao-Ling; Wang, Sheng; Wang, Bing; Xie, Fu-Wei; Zhang, Xiao-Bing; Ma, Yun-Ming; Wu, Hai-Long

2014-09-12

Peak detection and background drift correction (BDC) are the key stages in using chemometric methods to analyze chromatographic fingerprints of complex samples. This study developed a novel chemometric strategy for simultaneous automatic chromatographic peak detection and BDC. A robust statistical method was used for intelligent estimation of instrumental noise level coupled with first-order derivative of chromatographic signal to automatically extract chromatographic peaks in the data. A local curve-fitting strategy was then employed for BDC. Simulated and real liquid chromatographic data were designed with various kinds of background drift and degree of overlapped chromatographic peaks to verify the performance of the proposed strategy. The underlying chromatographic peaks can be automatically detected and reasonably integrated by this strategy. Meanwhile, chromatograms with BDC can be precisely obtained. The proposed method was used to analyze a complex gas chromatography dataset that monitored quality changes in plant extracts during storage procedure. Copyright © 2014 Elsevier B.V. All rights reserved.

The reformation of liquid hydrocarbons in an aqueous discharge reactor

KAUST Repository

Zhang, Xuming; Cha, Min

2015-01-01

deposition. These findings offer a new approach to the reforming processes of liquid hydrocarbons and provide a novel concept for the design of a practical and compact plasma reformer. © 2015 IOP Publishing Ltd.

Characterization of crude oils and petroleum products: (I Elution liquid chromatographic separation and gas chromatographic analysis of crude oils and petroleum products

Directory of Open Access Journals (Sweden)

E.O. Odebunmi

2002-12-01

Full Text Available Some physical and chemical properties of samples of light, medium and heavy Nigerian crude oils and petroleum products including gasoline, kerosene and engine oil have been measured and are reported in this paper. The crude oils and petroleum products have also been characterized by fractional distillation and elution liquid chromatography. The fractions obtained from elution liquid chromatography were analyzed using gas chromatography (GC. The GC fractions were identified by comparing the retention time of peaks in the unknown samples with those of components of calibration standard mixtures. The importance of the physico-chemical properties and the significance of the fractional distillation and chromatographic separation methods to industrial process operations have been discussed.

High-resolution gas chromatographic analysis of polycyclic aromatic hydrocarbons and aliphatic hydrocarbons

International Nuclear Information System (INIS)

Perez, M.; Gonzalez, D.

1988-01-01

A study of the analysis by gas chromatography of aromatic polycyclic hydrocarbons and aliphatic hydrocarbons is presented. The separation has been carried out by glass and fused silica capillary column in two different polar stationary phases OV-1 and SE-54. The limitation and the advantages of the procedure are discussed in terms of separation, sensitivity and precision. (Author) 20 refs

A liquid hydrocarbon deuteron source for neutron generators

Science.gov (United States)

Schwoebel, P. R.

2017-06-01

Experimental studies of a deuteron spark source for neutron generators using hydrogen isotope fusion reactions are reported. The ion source uses a spark discharge between electrodes coated with a deuterated hydrocarbon liquid, here Santovac 5, to inhibit permanent electrode erosion and extend the lifetime of high-output neutron generator spark ion sources. Thompson parabola mass spectra show that principally hydrogen and deuterium ions are extracted from the ion source. Hydrogen is the chief residual gas phase species produced due to source operation in a stainless-steel vacuum chamber. The prominent features of the optical emission spectra of the discharge are C+ lines, the hydrogen Balmer Hα-line, and the C2 Swan bands. Operation of the ion source was studied in a conventional laboratory neutron generator. The source delivered an average deuteron current of ˜0.5 A nominal to the target in a 5 μs duration pulse at 1 Hz with target voltages of -80 to -100 kV. The thickness of the hydrocarbon liquid in the spark gap and the consistency thereof from spark to spark influences the deuteron yield and plays a role in determining the beam-focusing characteristics through the applied voltage necessary to break down the spark gap. Higher breakdown voltages result in larger ion beam spots on the target and vice-versa. Because the liquid self-heals and thereby inhibits permanent electrode erosion, the liquid-based source provides long life, with 104 pulses to date, and without clear evidence that, in principle, the lifetime could not be much longer. Initial experiments suggest that an alternative cylindrical target-type generator design can extract approximately 10 times the deuteron current from the source. Preliminary data using the deuterated source liquid as a neutron-producing target are also presented.

Core-shell in liquid chromatography: application for determining sulphonamides in feed and meat using conventional chromatographic systems

Directory of Open Access Journals (Sweden)

Antonio Armentano

2016-12-01

Full Text Available A C18 column packed with core-shell particles was used for the chromatographic separation of sulphonamides in feed and meat by a conventional high performance liquid chromatography system coupled with a diode array detector. Two analytical methods, already used in our laboratory, have been modified without any changes in the extraction and clean-up steps and in the liquid chromatography instrumentation. Chromatographic conditions applied on a traditional 5-μm column have been optimized on a column packed with 2.6 μm core-shell particles. A binary mobile phase [acetate buffer solution at pH 4.50 and a mixture of methanol acetonitrile 50: 50 (v/v] was employed in gradient mode at the flow rate of 1.2 mL with an injection volume of 6 μL. These chromatographic conditions allow the separation of 13 sulphonamides with an entire run of 13 minutes. Preliminary studies have been carried out comparing blanks and spiked samples of feed and meat. A good resolution and the absence of interferences were achieved in chromatograms for both matrices. Since no change was made to the sample preparation, the optimized method does not require a complete revalidation and can be used to make routine analysis faster.

Electron localization in liquid hydrocarbons: The Anderson model

International Nuclear Information System (INIS)

Hug, Gordon L.; Mozumder, A.

2008-01-01

Anderson's model is applied for initial localization in liquid hydrocarbons (particularly n-alkanes) in conjunction with certain results of scaling theory. Medium connectivity is calculated using experimental X-ray data on liquid structure, from which critical disorder (W/V) c is computed, where W is diagonal disorder and V is the transfer energy. Actual W prevailing in the liquid is computed from anisotropic molecular polarizability. V is estimated by a heuristic procedure originating in scaling theory. These values are used to compute the percentage of initially delocalized states available for low-energy electrons in alkane liquids. This percentage decreases monotonically from methane (100%) to n-pentane and beyond (0%). In ethane and propane, the initial states are highly delocalized (97.6% and 83.9%, respectively). Subsequent trapping changes the situation as evidenced in mobility studies. Butane presents a partially, intermediate delocalized case (53.2%)

Liquid chromatographic separation of zalcitabine and its stereoisomers.

Science.gov (United States)

Scypinski, S; Ross, A J

1994-10-01

A liquid chromatographic method capable of separating and quantitating the stereoisomers of zalcitabine has been developed and validated. The separation was achieved with an Astec Cyclobond I--RSP column and a mobile phase of 0.25% triethylamine in water adjusted to a pH of 6.5 with glacial acetic acid. All enantiomers were found to exhibit a linear response in the range of 0.1-10% in the presence of 100% zalcitabine. Precision of analysis was found to be less than 1.5% at a level of 1% relative to zalcitabine. The limit of detection for two of the three enantiomeric impurities was determined to be 0.05% relative to zalcitabine. The detection limit for the third was found to be 0.1%. This method was successfully applied to the analysis of reference standards and several production scale batches. All of these materials were found to be stereochemically pure to a level of 99.8% or better.

Development and validation of micellar liquid chromatographic methods for the determination of antibiotics in different matrixes.

Science.gov (United States)

Rambla-Alegre, Maria; Esteve-Romero, Josep; Carda-Broch, Samuel

2011-01-01

Antibiotics are the most important bioactive and chemotherapeutic compounds to be produced by microbiological synthesis, and they have proved their worth in a variety of fields, such as medicinal chemistry, agriculture, and the food industry. Interest in antibiotics has grown in parallel with an increasingly high degree of productivity in the field of analytical applications. Therefore, it is necessary to develop chromatographic procedures capable of determining various drugs simultaneously in the shortest possible time. Micellar liquid chromatography (MLC) is an RP-HPLC technique that offers advantages over conventional HPLC as far as sample preparation, selectivity, and versatility are concerned. Its main advantage is that samples can be injected directly into the chromatographic system with no previous preparation step. This paper mainly focuses on the results of the authors' own recent research and reports the chromatographic conditions for determination of various antibiotics (penicillins, quinolones, and sulfonamides) in different matrixes (pharmaceuticals, biological fluids, and food). The work of other authors on MLC-based antibiotic determination has been included.

Measuring Trace Hydrocarbons in Silanes

Science.gov (United States)

Lesser, L. A.

1984-01-01

Technique rapid and uses standard analytical equipment. Silane gas containing traces of hydrocarbons injected into carrier gas of moist nitrogen having about 0.2 percent water vapor. Carrier, water and silane pass through short column packed with powdered sodium hydroxide which combines moisture and silane to form nonvolatile sodium silicate. Carrier gas free of silane but containing nonreactive hydrocarbons, pass to silica-gel column where chromatographic separation takes place. Hydrocarbons measured by FID.

Improved Chromatographic Bioavailability Estimations

National Research Council Canada - National Science Library

Dorsey, John

1996-01-01

.... Since the inception of reversed phase liquid chromatography there have been many attempts to correlate chromatographic retention with bioavailability and the most often used bulk measure, the octanol...

Direct coupling of a liquid chromatograph to a continuous flow hydrogen nuclear magnetic resonance detector for analysis of petroleum and synthetic fuels

International Nuclear Information System (INIS)

Haw, J.F.; Glass, T.E.; Hausler, D.W.; Motell, E.; Dorn, H.C.

1980-01-01

Initial results obtained for a flow 1 H nuclear magnetic resonance (NMR) detector directly coupled to a liquid chromatography unit are described. Results achieved for a model mixture and several jet fuel samples are discussed. Chromatographic separation of alkanes, alkylbenzenes, and substituted naphthalenes present in the jet fuel samples are easily identified with the 1 H NMR detector. Results with our present flow 1 H NMR insert indicate that 5-Hz linewidths are readily obtainable for typical chromatographic flow rates. The limitations and advantages of this liquid chromatography detector are compared with more commonly employed detectors (e.g., refractive index detectors). 11 figures

Study of liquid hydrocarbons subjected to ionizing radiations

International Nuclear Information System (INIS)

Grob, Robert.

1977-01-01

This work is a study of liquid hydrocarbons (especially alkanes and cycloalkanes), ionized and excited by low L.E.T. high energy radiation. An analysis of radiolytical products shows a definite correlation between radiochemical yields and bond energies. The study of the influence of scavengers has been carried out and the methods for the determination of α parameters are discussed. Ionic recombination has been fully investigated: theoretical studies, based on a phenomenological model, on primary and (in presence of solute) secondary charge recombination have been performed. Secondary species were observed by use of kinetic optical absorption spectrophotometry. A good agreement with theory is obtained only when the electron scavenging before thermalization is negligible. Electron mobility in hydrocarbons has been measured and the electron scavenging rate constants have been determined using the pulse conductivity technique. Conformational analysis calculations show a correlation between the electron mobility and the electronic structure. The rate of formation of a radiolytic product and the rate of decay of its precursor have been studied for solutions of hydrocarbons and electron scavengers [fr

Abnormal tyrosine and phenylalanine metabolism in patients with tyrosyluria and phenylketonuria; gas-liquid chromatographic analysis of urinary metabolites

NARCIS (Netherlands)

Wadman, S.K.; Heiden, C. van der; Ketting, D.; Sprang, F.J. van

Gas-liquid chromatographic methods have been developed for the analysis of: urinary phenylalanine metabolites (I) in patients with phenylketonuria, tyrosine metabolites (II) in patients with a disturbed tyrosine metabolism at the level of p-hydroxyphenylpyruvate hydroxylase, and homogentisic acid in

Chromatographic separations of stereoisomers

Energy Technology Data Exchange (ETDEWEB)

Souter, R.W.

1985-01-01

This text covers both diastereomers and enantiomers; describes techniques for GC, HPLC, and other chromatographic methods; and tabulates results of various applications by both techniques and compound class. It provides current knowledge about separation mechanisms and interactions of asymmetric molecules, as well as experimental and commercial materials such as columns, instruments, and derivatization reagents. The contents also include stereoisomer separations by gas chromatography. Stereoisomer separations by high-performance liquid chromatography. Stereoisomer separations by other chromatographic techniques.

HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHIC PROFILING OF TRYPTOPHAN AND RELATED INDOLES IN BODY-FLUIDS AND TISSUES OF CARCINOID PATIENTS

NARCIS (Netherlands)

KEMA, IP; SCHELLINGS, AMJ; HOPPENBROUWERS, CJM; RUTGERS, HM; DEVRIES, EGE; MUSKIET, FAJ

1993-01-01

A high performance liquid chromatographic method with quaternary gradient elution and fluorometric detection was developed for profiling of tryptophan (TRP), 5-hydroxytryptophan, serotonin (5-HT) and 5-hydroxyindole-3-acetic acid (5-HIAA) in urine, platelet-rich plasma and (tumour) tissue of

Microwave plasmas generated in bubbles immersed in liquids for hydrocarbons reforming

International Nuclear Information System (INIS)

Levko, Dmitry; Sharma, Ashish; Raja, Laxminarayan L

2016-01-01

We present a computational modeling study of microwave plasma generated in cluster of atmospheric-pressure argon bubbles immersed in a liquid. We demonstrate that the use of microwaves allows the generation of a dense chemically active non-equilibrium plasma along the gas–liquid interface. Also, microwaves allow generation of overdense plasma in all the bubbles considered in the cluster which is possible because the collisional skin depth of the wave exceeds the bubble dimension. These features of microwave plasma generation in bubbles immersed in liquids are highly desirable for the large-scale liquid hydrocarbon reforming technologies. (letter)

Performance characteristics of bioassay, radioenzymatic assay, homogeneous enzyme immunoassay, and high-performance liquid chromatographic determination of serum gentamicin

International Nuclear Information System (INIS)

Delaney, C.J.; Opheim, K.E.; Smith, A.L.; Plorde, J.J.

1982-01-01

We compared the accuracy, precision, and between-method error of the microbiological assay, the radioenzymatic assay, the homogeneous enzyme immunoassay, and the high-performance liquid chromatographic assay for the quantitation of gentamicin in serum. Precision and accuracy were evaluated by reference samples prepared to contain 0.0 to 32.7 micrograms of gentamicin per ml. Correlations between the methods utilized patient sera with gentamicin concentrations ranging from 0.6 to 13.3 micrograms/ml. All methods were reliable within acceptable limits for routine clinical use; intermethod correlation coefficients exceeded 0.96. Relative to the microbiological assay, the alternative methods offer the advantage of rapid analysis. The elapsed times for acquiring data on a set of 10 specimens under routine operating conditions were 0.5 h by the enzyme immunoassay, 4 h by the radioenzymatic assay, 5 h by the high-performance liquid chromatographic assay, and 10 h by the microbiological assay

Phase transitions on (liquid + liquid) equilibria for (water + 1-methylnaphthalene + light aromatic hydrocarbon) ternary systems at T = (563, 573, and 583) K

International Nuclear Information System (INIS)

Togo, Masaki; Inamori, Yoshiki; Shimoyama, Yusuke

2012-01-01

Highlights: ► Mixtures of (water + 1-methylnaphthalene + light aromatic hydrocarbon) are focused. ► Phase transition pressures on (liquid + liquid) equilibria were measured. ► Effects of aromatic hydrocarbons on phase transition pressure are investigated. ► Phase transition pressures are discussed using dielectric constants of hydrocarbons. - Abstract: Phase transitions for (water + 1-methylnaphthalene + light aromatic hydrocarbon) ternary systems are observed at their (liquid + liquid) equilibria at T = (563, 573, and 583) K and (8.6 to 25.0) MPa. The phase transition pressures at T = (563, 573, and 583) K were measured for the five species of light aromatic hydrocarbons, o-, m-, p-xylenes, ethylbenzene, and mesitylene. The measurements of the phase transition pressures were carried out by changing the feed mole fraction of water and 1-methylnaphthalene in water free, respectively. Effects of the feed mole fraction of water on the phase transition pressures are very small. Increasing the feed mole fraction of 1-methylnaphthalene results in decreasing the phase transition pressures at constant temperature. The slopes depending on the feed mole fraction for 1-methylnaphthalene at the phase transition pressures are decreased with increasing temperature for (water + 1-methylnaphthalene + p-xylene), (water + 1-methylnaphthalene + o-xylene), and (water + 1-methylnaphthalene + mesitylene) systems. For xylene isomers, the highest and lowest of the phase transition pressures are obtained in the case of p- and o-xylenes, respectively. The phase transition pressures for ethylbenzene are lower than those in the case of p-xylene. The similar phase transition pressures are given for p-xylene and mesitylene.

Plasma devices for hydrocarbon reformation

KAUST Repository

Cha, Min Suk

2017-02-16

Plasma devices for hydrocarbon reformation are provided. Methods of using the devices for hydrocarbon reformation are also provided. The devices can include a liquid container to receive a hydrocarbon source, and a plasma torch configured to be submerged in the liquid. The plasma plume from the plasma torch can cause reformation of the hydrocarbon. The device can use a variety of plasma torches that can be arranged in a variety of positions in the liquid container. The devices can be used for the reformation of gaseous hydrocarbons and/or liquid hydrocarbons. The reformation can produce methane, lower hydrocarbons, higher hydrocarbons, hydrogen gas, water, carbon dioxide, carbon monoxide, or a combination thereof.

Cobalt/N-Hydroxyphthalimide(NHPI)-Catalyzed Aerobic Oxidation of Hydrocarbons with Ionic Liquid Additive

DEFF Research Database (Denmark)

Mahmood, Sajid; Xu, Bao Hua; Ren, Tian Lu

2018-01-01

A highly efficient and solvent-free system of cobalt/NHPI-catalyzed aerobic oxidation of hydrocarbons was developed using imidazolium-based ionic liquid (IL) as an additive. These amphipathic ILs were found self-assemble at the interface between the organic hydrocarbons and the aqueous phase...... the optimum reactivity. Besides, the interfacial boundary between aqueous and organic phase composed by C2-alkylated imidazolium ILs, such as [bdmim]SbF6 and [C12dmim]SbF6, not only has ternary aggregates (hydrocarbons/IL/H2O) of higher stability but renders O2 a faster diffusion rate and higher concentration......, thereby offering a high reactivity of the protocol towards hydrocarbon oxidation....

Effects of chromatographic fractions of Euphorbia hirta on the rat ...

African Journals Online (AJOL)

The effects of the chromatographic fractions of Euphorbia hirta Linn on the serum biochemical parameters in rats were investigated. The ethanolic extract of this plant was subjected to chromatographic separation using the vacuum liquid chromatographic technique, a modified form of classical column chromatography.

Comprehensive two-dimensional liquid chromatographic analysis of poloxamers.

Science.gov (United States)

Malik, Muhammad Imran; Lee, Sanghoon; Chang, Taihyun

2016-04-15

Poloxamers are low molar mass triblock copolymers of poly(ethylene oxide) (PEO) and poly(propylene oxide) (PPO), having number of applications as non-ionic surfactants. Comprehensive one and two-dimensional liquid chromatographic (LC) analysis of these materials is proposed in this study. The separation of oligomers of both types (PEO and PPO) is demonstrated for several commercial poloxamers. This is accomplished at the critical conditions for one of the block while interaction for the other block. Reversed phase LC at CAP of PEO allowed for oligomeric separation of triblock copolymers with regard to PPO block whereas normal phase LC at CAP of PPO renders oligomeric separation with respect to PEO block. The oligomeric separation with regard to PEO and PPO are coupled online (comprehensive 2D-LC) to reveal two-dimensional contour plots by unconventional 2D IC×IC (interaction chromatography) coupling. The study provides chemical composition mapping of both PEO and PPO, equivalent to combined molar mass and chemical composition mapping for several commercial poloxamers. Copyright © 2016 Elsevier B.V. All rights reserved.

Evaluation of hydrocarbon-liquid disposition. Topical report, July 1990-November 1990

International Nuclear Information System (INIS)

Gibbs, J.E.; Tannehill, C.C.

1991-08-01

The report examines the current practice and technology used in natural gas liquids (NGL) extraction in small scale gas processing facilities. The removal of NGLs from a natural gas stream is driven by two factors: (1) hydrocarbon dew point and heating value control; and (2) economic recovery of the NGLs. Wellhead condensates are purchased at a price per barrel adjusted for transportation costs. Water is disposed of by truck at an approximate cost of $1.00 per barrel. Natural gas with a BTU content greater than 1150 normally will require NGL extraction prior to pipeline delivery. NGL recovery, if not required for hydrocarbon dew point or heating value control, must be justified by the value of the liquids exceeding the sum of the following costs: BTU value of the liquids; fuel consumed in the process; operating costs for the plant; and return of the plant investment capital. Liquids are purchased based on component posted prices with the cost of transportation, component fractionation and marketing subtracted. Rich gas in small quantities is normally processed in a straight refrigeration plant. Leaner gas in larger quantities is normally processed in a cryogenic expansion plant. With current technology, there is not sufficient margin to treat lean gases on a small scale

Radioimmunoassay of methaqualone in human urine compared with chromatographic methods

International Nuclear Information System (INIS)

Mule, S.J.; Kogan, M.; Jukofsky, D.

1978-01-01

The 125 I-radioimmunoassay for methaqualone in human urine was evaluated by a comparison with newly modified gas-liquid chromatographic and thin-layer chromatographic methods. The statistically significant sensitivity value for the radioimmunoassay was at 2 μg of methaqualone per liter of urine. The coefficient of variation was 2.88 -+ 0.16% intraassay. There was cross-reactivity only with metabolites of methaqualone, 4'-hydroxymethaqualone being twice as sensitively measured as methaqualone. There was complete agreement between results by radioimmunoassay and by gas-liquid chromatography in 96.7% of the samples analyzed. Only 1.2% of the radioimmunoassay values were false positives, and 2.1% false negatives (phi = 0.8917, P < 0.001). Comparisons between the thin-layer chromatographic data and the gas--liquid chromatographic or radioimmunoassay data showed less agreement because of the 50- to 200-fold higher sensitivity of the latter techniques. Gas--liquid chromatography therefore appears to represent the best reference method for the evaluation of the radioimmunoassay, which appears to be a very sensitive and reliable technique for detecting methaqualone and its metabolites in human urine

Investigating the Effect of Column Geometry on Separation Efficiency using 3D Printed Liquid Chromatographic Columns Containing Polymer Monolithic Phases.

Science.gov (United States)

Gupta, Vipul; Beirne, Stephen; Nesterenko, Pavel N; Paull, Brett

2018-01-16

Effect of column geometry on the liquid chromatographic separations using 3D printed liquid chromatographic columns with in-column polymerized monoliths has been studied. Three different liquid chromatographic columns were designed and 3D printed in titanium as 2D serpentine, 3D spiral, and 3D serpentine columns, of equal length and i.d. Successful in-column thermal polymerization of mechanically stable poly(BuMA-co-EDMA) monoliths was achieved within each design without any significant structural differences between phases. Van Deemter plots indicated higher efficiencies for the 3D serpentine chromatographic columns with higher aspect ratio turns at higher linear velocities and smaller analysis times as compared to their counterpart columns with lower aspect ratio turns. Computational fluid dynamic simulations of a basic monolithic structure indicated 44%, 90%, 100%, and 118% higher flow through narrow channels in the curved monolithic configuration as compared to the straight monolithic configuration at linear velocities of 1, 2.5, 5, and 10 mm s -1 , respectively. Isocratic RPLC separations with the 3D serpentine column resulted in an average 23% and 245% (8 solutes) increase in the number of theoretical plates as compared to the 3D spiral and 2D serpentine columns, respectively. Gradient RPLC separations with the 3D serpentine column resulted in an average 15% and 82% (8 solutes) increase in the peak capacity as compared to the 3D spiral and 2D serpentine columns, respectively. Use of the 3D serpentine column at a higher flow rate, as compared to the 3D spiral column, provided a 58% reduction in the analysis time and 74% increase in the peak capacity for the isocratic separations of the small molecules and the gradient separations of proteins, respectively.

Prediction of vapour-liquid and vapour-liquid-liquid equilibria of nitrogen-hydrocarbon mixtures used in J-T refrigerators

Science.gov (United States)

Narayanan, Vineed; Venkatarathnam, G.

2018-03-01

Nitrogen-hydrocarbon mixtures are widely used as refrigerants in J-T refrigerators operating with mixtures, as well as in natural gas liquefiers. The Peng-Robinson equation of state has traditionally been used to simulate the above cryogenic process. Multi parameter Helmholtz energy equations are now preferred for determining the properties of natural gas. They have, however, been used only to predict vapour-liquid equilibria, and not vapour-liquid-liquid equilibria that can occur in mixtures used in cryogenic mixed refrigerant processes. In this paper the vapour-liquid equilibrium of binary mixtures of nitrogen-methane, nitrogen-ethane, nitrogen-propane, nitrogen-isobutane and three component mixtures of nitrogen-methane-ethane and nitrogen-methane-propane have been studied with the Peng-Robinson and the Helmholtz energy equations of state of NIST REFPROP and compared with experimental data available in the literature.

Liquid chromatographic determination of sennosides in Cassia angustifolia leaves.

Science.gov (United States)

Srivastava, Alpuna; Pandey, Richa; Verma, Ram K; Gupta, Madan M

2006-01-01

A simple liquid chromatographic method was developed for the determination of sennosides B and A in leaves of Cassia angustifolia. These compounds were extracted from leaves with a mixture of methanol-water (70 + 30, v/v) after defatting with hexane. Analyte separation and quantitation were achieved by gradient reversed-phase liquid chromatography and UV absorbance at 270 nm using a photodiode array detector. The method involves the use of an RP-18 Lichrocart reversed-phase column (5 microm, 125 x 4.0 mm id) and a binary gradient mobile-phase profile. The various other aspects of analysis, namely, peak purity, similarity, recovery, repeatability, and robustness, were validated. Average recoveries of 98.5 and 98.6%, with a coefficient of variation of 0.8 and 0.3%, were obtained by spiking sample solution with 3 different concentration solutions of standards (60, 100, and 200 microg/mL). Detection limits were 10 microg/mL for sennoside B and 35 microg/mL for sennoside A, present in the sample solution. The quantitation limits were 28 and 100 microg/mL. The analytical method was applied to a large number of senna leaf samples. The new method provides a reliable tool for rapid screening of C. angustifolia samples in large numbers, which is needed in breeding/genetic engineering and genetic mapping experiments.

High-performance liquid chromatographic determination of isoniazid and 1-isonicotinyl-2-lactosylhydrazine in isoniazid tablet formulations.

Science.gov (United States)

Butterfield, A G; Lovering, E G; Sears, R W

1980-02-01

A high-performance liquid chromatographic procedure is presented for the simultaneous determination of isoniazid and 1-isonicotinyl-2-lactosylhydrazine (I) in isoniazid tablet formulations. An aliquot of a diluted aqueous tablet extract is introduced onto a microparticulate cyanopropyl bonded-phase column using a valve-loop injector and chromatographed using a mobile phase of acetonitrile--0.01 M, pH 3.5 aqueous acetate buffer (5:95). Compound I can be determined at levels as low as 0.5% of the isoniazid label claim. The relative standard deviations are 0.4 and 0.7% for the simultaneous determination of isoniazid and I, respectively. Seven commercial tablet formulations contained 93.8--97.0% of the labeled isoniazid amounts and 0.3--5.8% of I, expressed as equivalent isoniazid relative to the labeled isoniazid level.

High-pressure liquid chromatographic determination of chlorphenesin carbamate and the beta-isomeric carbamate.

Science.gov (United States)

Beyer, W F

1976-12-01

A high-pressure liquid chromatographic assay was developed for the determination of chlorphenesin carbamate and its beta-isomeric carbamate. A single 4-mm i.d. X 30-cm column, prepacked with 10 micrometer fully porous silica gel particles, is used with 3% methanol in 50% water-saturated butyl chloride as the mobile phase. The procedure separates chlorphenesin carbamate from several possible impurities in addition to the beta-isomeric carbamate. The assay was applied to bulk drug and compressed tablets. The relative standard deviations for the assays of chlorphenesin carbamate and the beta-isomer are approximately 1 and 2%, respectively.

Reverse-Phase High-Performance Liquid Chromatographic Separation of Methylated and Non-Methylated Nucleic Acid Bases

OpenAIRE

Madyastha, Prema; Rao, Pratima; Deobagkar, DN; Madyastha, KM

1983-01-01

A high-performance liquid chromatographic sepration method is described for the detection of 5-methylcytosine and 6-methyladenine in nucleic acid ext. The bases were sepd. on a Waters $C18 \\mu$ Bondapak column with a water: methanol acetic acid system. Effluents were monitored by UV absorption at 254 nm. The bases were estd. by peak heights which are proportional to the amts. of the individual bases. The method is rapid, sensitive, easy to perform and reproducible.

Alternative solvent-based methyl benzoate vortex-assisted dispersive liquid-liquid microextraction for the high-performance liquid chromatographic determination of benzimidazole fungicides in environmental water samples.

Science.gov (United States)

Santaladchaiyakit, Yanawath; Srijaranai, Supalax

2014-11-01

Vortex-assisted dispersive liquid-liquid microextraction using methyl benzoate as an alternative extraction solvent for extracting and preconcentrating three benzimidazole fungicides (i.e., carbendazim, thiabendazole, and fluberidazole) in environmental water samples before high-performance liquid chromatographic analysis has been developed. The selected microextraction conditions were 250 μL of methyl benzoate containing 300 μL of ethanol, 1.0% w/v sodium acetate, and vortex agitation speed of 2100 rpm for 30 s. Under optimum conditions, preconcentration factors were 14.5-39.0 for the target fungicides. Limits of detection were obtained in the range of 0.01-0.05 μg/L. The proposed method was then applied to surface water samples and the recovery evaluations at three spiked concentration levels of 5, 30, and 50 μg/L were obtained in the range of 77.4-110.9% with the relative standard deviation water samples. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

High-performance liquid chromatographic analysis of anthraquinone compounds in the Laurera benguelensis

Science.gov (United States)

Manojlović, N.; Marković, Z.; Gritsanapan, W.; Boonpragob, K.

2009-09-01

A high-performance liquid chromatographic (HPLC) method has been developed for the characterization of anthraquinone metabolites in extracts of the lichen Laurera benguelensis. With this method four anthraquinone derivatives 1,8-dihydroxy-3-methoxy-6-methylanthraquinone, 1,8-dihydroxy-3-formyl-6-methoxyanthraquinone, 1,8-dihydroxy-3-hydroxymethyl-6-methoxy-anthraquinone and 1,3,8-trihyroxy-6-methylanthraquinone can be analyzed. Components of lichen were detected by characteristic ultraviolet spectra and relative retention times. This is first report of phytochemical analysis of L. benguelensis. Importance of this research is in recognizing some new source (lichen and its extracts) as a natural emplacement of antioxidants because oxidation with free radicals or autooxidation is big problem for preservation of food products.

[Reversed-phase high-performance liquid chromatograph--application to serum aluminium monitoring].

Science.gov (United States)

Hoshino, H; Kaneko, E

1996-01-01

High-Performance Liquid Chromatography (HPLC) with the reversed-phase partition mode separation (including ion-pair one) towards metal chelate compounds prepared in an off-line fashion (precolumn chelation) is most versatile in terms of high sensitivity with base-line flatness, unique selectivity and cost effectiveness. The extraordinary toughness to the complicated matrices encountered in clinical testing is exemplified by the successful application to the aluminium monitoring of human serum samples. The A1 chelate with 2,2'-dihydroxyazobenzene is efficiently chromatographed on a LiChroCART RP-18 column using an aqueous methanol eluent (63.6 wt%) containing tetrabutylammonium bromide as an ion-pair agent. The serum concentration level of A1 down to 6 micrograms dm-3 is readily monitored without influences from iron, chyle and haemolysis.

Storing of Extracts in Polypropylene Microcentrifuge Tubes Yields Contaminant Peak During Ultra-flow Liquid Chromatographic Analysis

OpenAIRE

Kshirsagar, Parthraj R.; Hegde, Harsha; Pai, Sandeep R.

2016-01-01

Background and Aim: This study was designed to understand the effect of storage in polypropylene microcentrifuge tubes and glass vials during ultra-flow liquid chromatographic (UFLC) analysis. Materials and Methods: One ml of methanol was placed in polypropylene microcentrifuge tubes (PP material, Autoclavable) and glass vials (Borosilicate) separately for 1, 2, 4, 8, 10, 20, 40, and 80 days intervals stored at ?4?C. Results: Contaminant peak was detected in methanol stored in polypropylene m...

Novel extension of the trap model for electrons in liquid hydrocarbons

International Nuclear Information System (INIS)

Jamal, M.A.; Watt, D.E.

1981-01-01

A novel extension for the trap model of electron mobilities in liquid hydrocarbons is described. The new model assumes: (a) two main types of electron trap exist in liquid hydrocarbons, one is deep and the second is shallow; (b) these traps are the same in all liquid alkanes. The difference in electron mobilities in different alkanes is accounted for by the difference in the frequency of electron trapping in each state. The probability of trapping in each state has been evaluated from the known structures of the normal alkanes. Electron mobilities in normal alkanes (C 3 -C 10 ) show a very good correlation with the probability of trapping in deep traps, suggesting that the C-C bonds are the main energy sinks of the electron. A mathematical formula which expresses the electron mobility in terms of the probability of trapping in deep traps has been found from the Arrhenius relationship between electron mobilities and probability of trapping. The model has been extended for branched alkanes and the relatively high electron mobilities in globular alkanes has been explained by the fact that each branch provides some degree of screening to the skeleton structure of the molecule resulting in reduction of the probability of electron interaction with the molecular skeleton. (author)

Determination of trihalomethanes in waters by ionic liquid-based single drop microextraction/gas chromatographic/mass spectrometry.

Science.gov (United States)

Aguilera-Herrador, Eva; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel

2008-10-31

A simple, rapid, solventless method for the determination of trihalomethanes (THMs) (chloroform, bromodichloromethane, dibromochloromethane and bromoform) in water samples is presented. The analytes are extracted from the headspace of the aqueous matrix into a 2 microL drop of the ionic liquid 1-octyl-3-methyl-imidazolium hexafluorophosphate working at 30 degrees C for 30 min. The separation and detection of the target compounds is accomplished by gas chromatography/mass spectrometry owing to the use of an interface that efficiently transfers the analytes extracted in the ionic liquid drop to the gas chromatograph while preventing the ionic liquid from entering the column. The detection limits obtained are below the values compelled by the legislation, ranging from 0.5 microg L(-1) for chloroform and bromodichloromethane to 0.9 microg L(-1) for dibromochloromethane. The use of ionic liquid in the extraction procedure avoids the use of organic solvents and leads to relative standard deviations that range from 3.1% to 4.8%.

Total cholesterol in serum determined by isotope dilution/mass spectrometry, with liquid-chromatographic separation

International Nuclear Information System (INIS)

Takatsu, Akiko; Nishi, Sueo

1988-01-01

We describe an accurate, precise method for determination of total serum cholesterol by isotope dilution/mass spectrometry (IDMS) with liquid chromatographic separation. After adding [3,4- 13 C] cholesterol to serum and hydrolyzing the cholesterol esters, we extract the total cholesterol. High-performance liquid chromatography (HPLC) is used to separate the extracted cholesterol for measurement by electron-impact mass spectrometry with use of a direct-insertion device. To evaluate the specificity and the accuracy of this method, we also studied the conventional IDMS method, which involves converting cholesterol to the trimethylsilyl ether and assay by gas chromatography-mass spectrometry with use of a capillary column. The coefficient of variation for the HPLC method was a little larger than for the conventional method, but mean values by each method agreed within 1% for all sera tested. (author)

Analysis and chromatographic purification of eicosanoids multiply labeled by tritium

International Nuclear Information System (INIS)

Shevchenko, V.P.; Nagaev, I.Yu.; Myasoedov, N.F.

1989-01-01

We show the possibility of analysis and chromatographic purification of eicosanoids triply labeled by tritium. The described methods allow us to isolate chromatographically pure products obtained by selective hydrogenatin, chemical, and enzyme methods, with radiochemical purity at least 95-97%. The following methods are used to analyze the reaction mixtures and to isolate the tritium-labeled eicosanoids: gas-liquid chromatography, high-efficiency liquid chromatography, and thin-layer chromatography on supports impregnated with silver nitrate

High-pressure liquid chromatographic analysis of pramoxine hydrochloride in high lipoid aerosol foam dosage form.

Science.gov (United States)

Weinberger, R; Mann, B; Posluszny, J

1980-04-01

A rapid and quantitative method for the determination of pramoxine hydrochloride by high-pressure liquid chromatography is presented. The drug is extracted as the salt from a preparation with a high lipoid composition by partitioning it to the aqueous phase of an ether-methanol-water-acetic acid system. The extract is chromatographed on an octadecylsilane bonded packing with a methanol-water-acetic acid-methanesulfonic acid mobile phase. The time required for each separation is approximately 6 min. Analytical recoveries of 100.4 +/- 1.5% were obtained.

Comparative analysis of different methods of extraction of present hydrocarbons in industrial residual waters

International Nuclear Information System (INIS)

Santa, Judith Rocio; Serrano, Martin; Stashenko, Elena

2002-01-01

A comparison among four extraction techniques such as: liquid - liquid (LLE) continuous and for lots, solid phase extraction (SPE), solid phase micro extraction (SPME) and static headspace (S-HS) was carried out. The main purpose of this research was to determine the highest recovery efficiencies and how reproducible the tests are while varying parameters such as time, extraction technique, type of solvents and others. Chromatographic parameters were optimized in order to carry out the analyses. Hydrocarbon's quantification of residual waters was achieved by using a high-resolution gas chromatography with a gas flame ionization detector (HRGC-FID). Validation of the method was carried out by analyzing real samples taken in different sampling places of the residual waters treatment plant of Ecopetrol - Barrancabermeja. The use of extraction methods that require big solvent quantities and long time for analysis are losing validity day by day. Techniques such as the HS-SPME and static HS are offered as alternatives for quantifying hydrocarbons. They show total lack of solvents, high sensibility, selectivity and the techniques are reproducible. Solid phase micro extraction (SPME) and static headspace (static HS) techniques were chosen as the extraction techniques to validate the method in real samples. Both techniques showed similar results for the determination of total hydrocarbons (in the gasoline range)

Separation of toluene from cyclic hydrocarbons using 1-butyl-3-methylimidazolium methylsulfate ionic liquid at T = 298.15 K and atmospheric pressure

International Nuclear Information System (INIS)

Dominguez, Irene; Calvar, Noelia; Gomez, Elena; Dominguez, Angeles

2011-01-01

Highlights: → [BMim][MSO 4 ] was studied as solvent to extract toluene from cyclic hydrocarbons. → (Liquid + liquid) equilibrium data were measured at 298.15K and atmospheric pressure. → Selectivity and solute distribution ratio were obtained and compared with literature. → Experimental data were satisfactorily correlated using NRTL and UNIQUAC models. → [BMim][MSO 4 ] can be used as solvent for the studied (liquid + liquid) extraction. - Abstract: In this paper the extraction of toluene from cyclic hydrocarbons (cyclohexane, or methylcyclohexane, or cyclooctane, or cyclohexene) was analyzed by liquid extraction with 1-butyl-3-methylimidazolium methylsulfate ionic liquid, [BMim][MSO 4 ], as solvent. The experimental (liquid + liquid) equilibrium (LLE) data were determined at T = 298.15 K and atmospheric pressure. Solubility curves were obtained by the cloud point method and tie-line compositions were determined by density measurement. An analysis of the influence of different cyclic hydrocarbons on the extraction was performed. The effectiveness of the extraction of toluene from cyclic hydrocarbons was evaluated by means of the solute distribution ratio and selectivity values. The degree of consistency of the experimental LLE data was ascertained using the Othmer-Tobias and Hand equations. The experimental data for the (liquid + liquid) equilibria of the ternary systems were correlated with the Non-Random Two-Liquid (NRTL) and UNIversal QUAsi-Chemical (UNIQUAC) thermodynamic models.

Carbazole angular dioxygenation and mineralization by bacteria isolated from hydrocarbon-contaminated tropical African soil.

Science.gov (United States)

Salam, L B; Ilori, M O; Amund, O O; Numata, M; Horisaki, T; Nojiri, H

2014-01-01

Four bacterial strains isolated from hydrocarbon-contaminated soils in Lagos, Nigeria, displayed extensive degradation abilities on carbazole, an N-heterocyclic aromatic hydrocarbon. Physicochemical analyses of the sampling sites (ACPP, MWO, NESU) indicate gross pollution of the soils with a high hydrocarbon content (157,067.9 mg/kg) and presence of heavy metals. Phylogenetic analysis of the four strains indicated that they were identified as Achromobacter sp. strain SL1, Pseudomonas sp. strain SL4, Microbacterium esteraromaticum strain SL6, and Stenotrophomonas maltophilia strain BA. The rates of degradation of carbazole by the four isolates during 30 days of incubation were 0.057, 0.062, 0.036, and 0.050 mg L(-1) h(-1) for strains SL1, SL4, SL6, and BA. Gas chromatographic (GC) analyses of residual carbazole after 30 days of incubation revealed that 81.3, 85, 64.4, and 76 % of 50 mg l(-1) carbazole were degraded by strains SL1, SL4, SL6, and BA, respectively. GC-mass spectrometry and high-performance liquid chromatographic analyses of the extracts from the growing and resting cells of strains SL1, SL4, and SL6 cultured on carbazole showed detection of anthranilic acid and catechol while these metabolites were not detected in strain BA under the same conditions. This study has established for the first time carbazole angular dioxygenation and mineralization by isolates from African environment.

Chromatographic behavior of small organic compounds in low-temperature high-performance liquid chromatography using liquid carbon dioxide as the mobile phase.

Science.gov (United States)

Motono, Tomohiro; Nagai, Takashi; Kitagawa, Shinya; Ohtani, Hajime

2015-07-01

Low-temperature high-performance liquid chromatography, in which a loop injector, column, and detection cell were refrigerated at -35ºC, using liquid carbon dioxide as the mobile phase was developed. Small organic compounds (polyaromatic hydrocarbons, alkylbenzenes, and quinones) were separated by low-temperature high-performance liquid chromatography at temperatures from -35 to -5ºC. The combination of liquid carbon dioxide mobile phase with an octadecyl-silica (C18 ) column provided reversed phase mode separation, and a bare silica-gel column resulted in normal phase mode separation. In both the cases, nonlinear behavior at approximately -15ºC was found in the relationship between the temperature and the retention factors of the analytes (van't Hoff plots). In contrast to general trends in high-performance liquid chromatography, the decrease in temperature enhanced the separation efficiency of both the columns. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

INTERLABORATORY STUDY OF A THERMOSPRAY-LIQUID CHROMATOGRAPHIC/MASS SPECTROMETRIC METHOD FOR SELECTED N-METHYL CARBAMATES, N-METHYL CARBAMOYLOXIMES, AND SUBSTITUTED UREA PESTICIDES

Science.gov (United States)

A thermospray-liquid chromatographic/mass spectrometric (TS-LC/MS) method was evaluated in an interlaboratory study for determining 3 N-methyl carbamates (bendiocarb, carbaryl, and carbofuran), 3-N-methyl carbamoyloximes (aldicarb, methomyl, and oxamyl), 2 substituted urea pestic...

Liquid chromatographic determination with fluorescence detection of B6 vitamers and riboflavin in milk and pharmaceuticals

International Nuclear Information System (INIS)

Gatti, R.; Gioia, M.G.

2005-01-01

A simple, reliable and selective high performance liquid chromatographic method with fluorescence detection at different programmed wavelengths has been developed for the simultaneous analysis of B 6 vitamers (pyridoxal 5'-phosphate, 4-pyridoxic acid, pyridoxal, pyridoxine and pyridoxamine) and Vitamin B 2 in commercial vitaminized milk and in woman milk. The chromatographic separations were performed on a reversed phase octyl column by using a mobile phase consisting of sodium pentanesulfonate in 1% acetic acid-methanol-tetrahydrofuran under gradient elution conditions. The fluorescence intensity of pyridoxal 5'-phosphate was enhanced by post-column photochemical conversion, giving significantly different fluorescence spectra by a on-line photoreactor switched OFF and ON under irradiation at 254 nm. In addition, a simple and rapid method in isocratic conditions without the need of photochemical conversion was proposed for the analysis of Vitamin B 6 and Vitamin B 2 in pharmaceuticals. Linearity, precision, recovery, selectivity and sensitivity were found satisfactory for each analysed compound. Quantitation limits ranged from 26 to 240 fmol

A Selective High Performance Liquid Chromatographic Method to Follow the Hydrolytic Degradation of Nicardipine Hydrochloride

Directory of Open Access Journals (Sweden)

K. E. Ibrahim

2010-01-01

Full Text Available A simple, stability indicating, reverse phase high performance liquid chromatographic method was developed and validated for determination of nicardipine hydrochloride (NC in the presence of its degradation products. The chromatographic separation was performed on Hypersil, BDS-C18, 30 cm × 3.9 mm id, at ambient temperature with UV-detection at 254 nm. A mixture of 20% (v/v aqueous 0.01 M sodium acetate∕acetic acid buffer (pH 4.5 and 80% acetonitrile was used as the mobile phase at a flow rate of 1.5 mL min-1, losartan was used as internal standard. The calibration curve is linear over the concentration range 5-40 μg mL-1, with a regression coefficient of 0.9984 and the % recovery was 99.78±0.17. The method was used to investigate the kinetics of alkaline, acids induced degradation, effect of buffer concentration and temperature. The degradation followed first-order kinetics. The rate constant, half-life time, and activation energy were calculated

The quasi-ballistic model of electron mobility in liquid hydrocarbons

International Nuclear Information System (INIS)

Mozumder, A.

1996-01-01

A phenomenological theory of low-mobility liquid hydrocarbons is developed which includes electron ballistic motion in the quasi-free state, in competition with diffusion and trapping. For most low-mobility liquids the theory predicts consistently the effective mobility and activation energy, in agreement with experiments, using quasi-free mobility and trap density respectively as ∼ 100 cm 2 v -1 s -1 and ∼ 10 19 cm -3 . Field dependence of mobility if theoretically of quadratic type for relatively small fields, agreeing approximately with experimental data for n-hexane. Electron scavenging with ''good'' scavengers occurs via the quasi-free state at nearly diffusion-controlled rate; however the effect of large mean free path is seen clearly. (author)

Identification of radiation-induced hydrocarbons in halibut, cod and prawns by on-line coupled LC-GC/MS technique

International Nuclear Information System (INIS)

Spiegelberg, A.; Schulzki, G.; Boegl, K.W.; Schreiber, G.A.

1997-01-01

Radiation-induced hydrocarbons were analysed in a fatty (halibut) and a lean fish (cod) as well as in a prawn species by on-line coupled liquid chromatography (LC) - gas chromatography (GC) combined with mass spectrometrical detection. In irradiated halibut which contains mainly saturated and monounsaturated fatty acids all expected radiolytic alkanes, alkenes and alkadienes could be detected. The yields of the C n-1 and C n-2:1 hydrocarbons were comparable with those found in irradiated lipids of land animals and plants. However, in cod and the prawn species which contain high levels of polyunsaturated fatty acids (PUFA), the C n-1 hydrocarbons were found in concentrations up to tenfold higher whereas the C n-2:1 products were again comparable to those of land animals and plants. The identification of radiation-induced hydrocarbons in fish lipids was achieved by transfer of the hydrocarbons from the LC column to the gas chromatographic column in fractions differing in the degree of unsaturation. For the first time radiation induced hydrocarbons with more than four double bonds generated from polyunsaturated fatty acids (20:4ω6 and 20:5ω3) could be identified. (orig.) [de

Activity coefficients at infinite dilution of hydrocarbons in glycols: Experimental data and thermodynamic modeling with the GCA-EoS

International Nuclear Information System (INIS)

González Prieto, Mariana; Williams-Wynn, Mark D.; Bahadur, Indra; Sánchez, Francisco A.; Mohammadi, Amir H.

2017-01-01

Highlights: • Experimental infinite dilution activity coefficients of hydrocarbons in glycols. • Inverse gas-liquid chromatography technique. • Solutes investigated include n-alkanes, 1-alkenes, and cycloalkanes. • Highly non-ideal systems are modeled with the GCA-EoS. - Abstract: The infinite dilution activity coefficients for 12 non-polar hydrocarbon solutes in the solvents, monoethylene and diethylene glycol, were measured using the gas-liquid chromatography technique. Pre-saturation of the carrier gas was required to avoid solvent loss from the chromatographic column during the measurements that were carried out at T = (303.15, 313.15 and 323.15) K for monoethylene glycol and at T = (304.15, 313.15 and 323.15) K for diethylene glycol. The solutes investigated include n-alkanes, 1-alkenes, and cycloalkanes. The new data are compared with the highly scattered data that is available in the open literature. Finally, these highly non-ideal systems are modeled with the GCA-EoS.

Liquid-chromatographic determination of sarafloxacin residues in channel catfish muscle-tissue

Science.gov (United States)

Meinertz, J.R.; Dawson, V.K.; Gingerich, W.H.; Cheng, B.; Tubergen, M.M.

1994-01-01

A liquid chromatographic method is described for the determination of sarafloxacin hydrochloride residues i n channel catfish (ictalurus punctatus) fillets. Sarafloxacin was extracted from fillet tissue with acetonitrile=water (1 + 1). The extract was centrifuged and the supernatant was partitioned with hexane. The aqueous fraction was filtered through a 0.45 Mum filter and evaporated to dryness. The sample was redissolved with 20% acetonitrile-methanol (3 + 2) and 80% trifluoroacetic acid (0.1%), Centrifuged, and filtered to remove proteins. Samples were analyzed by chromatography with gradient elution on a c18 column and with fluorescence detection (excitation at 280 nm and emission above 389 nm). Mean recoveries ranged from 85.4 To 104%, and relative standard deviations ranged from 1.06 To 5.58% In samples spiked at concentrations of 10.0-863.8 Ng/g. The method detection limit for sarafloxacin was 1.4 Ng/g.

Interlaboratory tests to identify irradiation treatment of various foods via gas chromatographic detection of hydrocarbons, ESR spectroscopy and TL analysis

Energy Technology Data Exchange (ETDEWEB)

Schreiber, G.A.; Helle, N.; Schulzki, G.; Linke, B.; Spiegelberg, A.; Mager, M.; Boegl, K.W. [BgVV - Federal Inst. for Health Protection of Consumers and Veterinary Medicine, Berlin (Germany)

1996-12-31

The gas chromatographic (GC) analysis of radiation-induced volatile hydrocarbons (HC) and 2-alkylcyclobutanones, the ESR spectroscopic detection of radiation-specific radicals and the thermoluminescence (TL) analysis of silicate mineral are the most important methods for identification of irradiated foods. After successful performance in interlaboratory studies on meat products, fish, spices, herbs and shells of nuts, all or some of these methods have been approved by national authorities in Germany and the United Kingdom. Recently, draft European Standards have been elaborated for approval by member states of the European Committee for Standardization (CEN). Several research laboratories have shown that these methods can be applied to various foods not yet tested in collaborative studies. However, for an effective application in food control it is necessary to prove their suitability in interlaboratory studies. Therefore, in 1993/94, various interlaboratory tests were organised by the BgVV. In an ESR spectroscopic test, shrimps and paprika powder were examined. Shrimps were also the subject of examination in a TL test. Finally, GC detection of radiation-induced hydrocarbons in the fat fraction of foods was used in another test to identify irradiated Camembert, avocado, papaya and mango. In the following paper, results of the interlaboratory tests are summarised. Detailed reports are published by this institute. (author).

Interlaboratory tests to identify irradiation treatment of various foods via gas chromatographic detection of hydrocarbons, ESR spectroscopy and TL analysis

International Nuclear Information System (INIS)

Schreiber, G.A.; Helle, N.; Schulzki, G.; Linke, B.; Spiegelberg, A.; Mager, M.; Boegl, K.W.

1996-01-01

The gas chromatographic (GC) analysis of radiation-induced volatile hydrocarbons (HC) and 2-alkylcyclobutanones, the ESR spectroscopic detection of radiation-specific radicals and the thermoluminescence (TL) analysis of silicate mineral are the most important methods for identification of irradiated foods. After successful performance in interlaboratory studies on meat products, fish, spices, herbs and shells of nuts, all or some of these methods have been approved by national authorities in Germany and the United Kingdom. Recently, draft European Standards have been elaborated for approval by member states of the European Committee for Standardization (CEN). Several research laboratories have shown that these methods can be applied to various foods not yet tested in collaborative studies. However, for an effective application in food control it is necessary to prove their suitability in interlaboratory studies. Therefore, in 1993/94, various interlaboratory tests were organised by the BgVV. In an ESR spectroscopic test, shrimps and paprika powder were examined. Shrimps were also the subject of examination in a TL test. Finally, GC detection of radiation-induced hydrocarbons in the fat fraction of foods was used in another test to identify irradiated Camembert, avocado, papaya and mango. In the following paper, results of the interlaboratory tests are summarised. Detailed reports are published by this institute. (author)

Mixed-mode chromatographic matrices for the resolution of transfer ribonucleic acids

NARCIS (Netherlands)

Bischoff, Rainer; Mclaughlin, L.W.

1984-01-01

Modification of approximately 65% of the amine groups of an aminopropylsilyl bonded-phase silica high-performance liquid chromatographic anion exchanger (APS-Hypersil) with organic acids containing n-alkyl moieties of different chain lengths, results in mixed mode chromatographic matrices of varying

Apparatus for utilizing liquid hydrocarbons such as shale oil, etc

Energy Technology Data Exchange (ETDEWEB)

Dorset, M

1868-02-29

The hydrocarbon liquids such as petroleum, shale oil, naphtha, cresol, coal tar, or other mineral, animal or vegetable oil are placed in a heater or special generator analogous to ordinary generators for vapors and to which the name vaporizer has been given in the description. This vaporizer is furnished with all kinds of safety devices, such as valves, manometer, float indicating the level, standard stopcock, etc., and is heated by the combustion of the vapors produced by it.

Liquid chromatographic-tandem mass spectrometric assay for ...

African Journals Online (AJOL)

Methods: Blood and urine samples were obtained from healthy volunteers who admitted to not being on any medications. The investigated analytes were chromatographically separated on a C18 column (Luna®-PFP 100Å column, 50 mm × 2.0 mm i.d., 3.0 μm) with the aid of a mobile phase containing A; acetonitrile (ACN) ...

Simultaneous derivatisation and preconcentration of parabens in food and other matrices by isobutyl chloroformate and dispersive liquid-liquid microextraction followed by gas chromatographic analysis.

Science.gov (United States)

Jain, Rajeev; Mudiam, Mohana Krishna Reddy; Chauhan, Abhishek; Ch, Ratnasekhar; Murthy, R C; Khan, Haider A

2013-11-01

A simple, rapid and economical method has been proposed for the quantitative determination of parabens (methyl, ethyl, propyl and butyl paraben) in different samples (food, cosmetics and water) based on isobutyl chloroformate (IBCF) derivatisation and preconcentration using dispersive liquid-liquid microextraction in single step. Under optimum conditions, solid samples were extracted with ethanol (disperser solvent) and 200 μL of this extract along with 50 μL of chloroform (extraction solvent) and 10 μL of IBCF was rapidly injected into 2 mL of ultra-pure water containing 150 μL of pyridine to induce formation of a cloudy state. After centrifugation, 1 μL of the sedimented phase was analysed using gas chromatograph-flame ionisation detector (GC-FID) and the peaks were confirmed using gas chromatograph-positive chemical ionisation-mass spectrometer (GC-PCI-MS). Method was found to be linear over the range of 0.1-10 μg mL(-1) with square of correlation coefficient (R(2)) in the range of 0.9913-0.9992. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.029-0.102 μg mL(-1) and 0.095-0.336 μg mL(-1) with a signal to noise ratio of 3:1 and 10:1, respectively. Copyright © 2013 Elsevier Ltd. All rights reserved.

Analysis of aliphatic and aromatic hydrocarbons in particulate matter in Madrid urban area

International Nuclear Information System (INIS)

Perez, M.; Mendez, J.; Bomboi, M.T.

1988-01-01

Levels of n-alkanes and polycyclic aromatic hydrocarbons have been measured in the air particulate matter during six months, from January to June of 1987, in an urban area of Madrid. The hydrocarbons were collected on glass fiber filters by high volumen sampling. The extraction was carried out by Sohxlet and ultrasonic techniques. The extracts were clean-up on silicagel fractionation and the chromatographic analysis was performed by capillary column gas chromatographic. Final results are discussed as well as the immission values related to the possible emission sources. (Author)

Optimization of the reversed-phase high-performance liquid chromatographic separation of synthetic estrogenic and progestogenic steroids using the multi-criteria decision making method

NARCIS (Netherlands)

Smilde, A. K.; Bruins, C. H.; Doornbos, D. A.; Vink, J.

1987-01-01

The optimization of the reversed-phase high-performance liquid chromatographic separation of a mixture of ethynylestradiol, desogestrel and three related compounds is described. A procedure is used that allows the prediction of the capacity factors of each individual synthetic steroid, depending on

Towards comprehensive hydrocarbons analysis of middle distillates by LC-GCxGC.

Science.gov (United States)

Adam, Frédérick; Bertoncini, Fabrice; Thiébaut, Didier; Esnault, Sébastien; Espinat, Didier; Hennion, M C

2007-01-01

The detailed characterization of middle distillates is essential for a better understanding of reactions involved in refining processes. Owing to a higher resolution power and an enhanced sensitivity, but especially to a group-type ordering in the chromatographic plane, comprehensive two-dimensional gas chromatography (GCxGC) offers unsurpassed characterization possibilities for petroleum samples. However, GCxGC fails to totally discriminate naphthenes from unsaturates occurring in hydrotreated diesel samples. This article aims at promoting the implementation of LC-GCxGC for the quantitative determination of hydrocarbon distribution in middle distillates, including naphthenes. In this configuration, liquid chromatography (LC) enables the separation of hydrocarbons into two fractions (viz., saturated and unsaturated) before the subsequent analysis of each fraction by GCxGC. In this paper, the choice of GCxGC conditions in order to achieve the separation and identification of hydrocarbons by chemical class is discussed; under these conditions, naphthenes are separated according to the number of saturated rings. For the first time, the presence of di-, tri-, and tetra-naphthenes resulting from the hydroconversion of aromatics can clearly be evidenced. A quantitative procedure for the determination of the distribution of hydrocarbons, including the distribution of naphthenes according to the number of saturated rings, is also proposed and discussed in detail. LC-GCxGC is found to provide an unequalled degree of information that will widely contribute to a better understanding of hydroconversion processes.

Development of Direct Reversed-Phase High Performance liquid chromatographic method for quantitative determination of gabapentin in pharmaceutical dosage

International Nuclear Information System (INIS)

Hassan, W.; Zaman, B.; Rahman, S.; Rahman, A.U.; Ali, N.; Mohammadzai, I.U.

2012-01-01

The objective of the present work was to develop and validate a rapid analytical method for quantitative determination of Gabapentin in pharmaceutical dosage tablets and capsules. An accurate, simple, and sensitive reversed-phase high performance liquid chromatographic (HPLC) method, UV detection at 215 nm and flow rate at 1.0 ml/min has been developed. Isocratic elution was used instead of gradient elution to reduce the time and cost of serial analysis. The mobile phase was a mixture of water and methanol (HPLC grade). The retention time (Rt) of Gabapentin was 4.681 +- 0.013 minutes. Recovery, Precision, accuracy, and linearity were determined for the stated method. The calibration curve was linear and the correlation coefficient was 0.9996. There was no chromatographic interference from other excipients present in dosage form. The method was validated appropriately and successfully used for determination of Gabapentin in Pharmaceutical formulations. (author)

Valorization of Waste Lipids through Hydrothermal Catalytic Conversion to Liquid Hydrocarbon Fuels with in Situ Hydrogen Production

Energy Technology Data Exchange (ETDEWEB)

Kim, Dongwook; Vardon, Derek R.; Murali, Dheeptha; Sharma, Brajendra K.; Strathmann, Timothy J.

2016-03-07

We demonstrate hydrothermal (300 degrees C, 10 MPa) catalytic conversion of real waste lipids (e.g., waste vegetable oil, sewer trap grease) to liquid hydrocarbon fuels without net need for external chemical inputs (e.g., H2 gas, methanol). A supported bimetallic catalyst (Pt-Re/C; 5 wt % of each metal) previously shown to catalyze both aqueous phase reforming of glycerol (a triacylglyceride lipid hydrolysis coproduct) to H2 gas and conversion of oleic and stearic acid, model unsaturated and saturated fatty acids, to linear alkanes was applied to process real waste lipid feedstocks in water. For reactions conducted with an initially inert headspace gas (N2), waste vegetable oil (WVO) was fully converted into linear hydrocarbons (C15-C17) and other hydrolyzed byproducts within 4.5 h, and H2 gas production was observed. Addition of H2 to the initial reactor headspace accelerated conversion, but net H2 production was still observed, in agreement with results obtained for aqueous mixtures containing model fatty acids and glycerol. Conversion to liquid hydrocarbons with net H2 production was also observed for a range of other waste lipid feedstocks (animal fat residuals, sewer trap grease, dry distiller's grain oil, coffee oil residual). These findings demonstrate potential for valorization of waste lipids through conversion to hydrocarbons that are more compatible with current petroleum-based liquid fuels than the biodiesel and biogas products of conventional waste lipid processing technologies.

A liquid chromatographic method for determination of theophylline in serum and capillary blood--a comparison.

Science.gov (United States)

Gartzke, J; Jäger, H; Vins, I

1991-01-01

A simple, fast and reliable liquid chromatographic method for the determination of theophylline in serum and capillary blood after a solid phase extraction is described for therapeutic drug monitoring. The employment of capillary blood permits the determination of an individual drug profile and other pharmacokinetic studies in neonates and infants. There were no differences in venous- and capillary-blood levels but these values compared poorly with those in serum. An adjustment of the results by correction of the different volumes of serum and blood by haematocrit was unsuccessful. Differences in the binding of theophylline to erythrocytes could be an explanation for the differences in serum at blood levels of theophylline.

Microorganism mediated liquid fuels

Energy Technology Data Exchange (ETDEWEB)

Troiano, Richard

2018-03-20

Herein disclosed is a method for producing liquid hydrocarbon product, the method comprising disintegrating a hydrocarbon source; pretreating the disintegrated hydrocarbon source; solubilizing the disintegrated hydrocarbon source to form a slurry comprising a reactant molecule of the hydrocarbon source; admixing a biochemical liquor into the slurry, wherein the biochemical liquor comprises at least one conversion enzyme configured to facilitate bond selective photo-fragmentation of said reactant molecule of the hydrocarbon source, to form liquid hydrocarbons via enzyme assisted bond selective photo-fragmentation, wherein said conversion enzyme comprises reactive sites configured to restrict said reactant molecule such that photo-fragmentation favorably targets a preselected internal bond of said reactant molecule; separating the liquid hydrocarbons from the slurry, wherein contaminants remain in the slurry; and enriching the liquid hydrocarbons to form a liquid hydrocarbon product. Various aspects of such method/process are also discussed.

Liquid chromatographic method for simultaneous determination of citalopram with NSAIDs in bulk drug, pharmaceutical formulation and human serum

International Nuclear Information System (INIS)

Ali, S.N.; Akram, S.

2017-01-01

A high performance liquid chromatographic method was developed and validated to simultaneously quantify citalopram with piroxicam, celecoxib and diclofenac sodium. Chromatographic analysis was performed at ambient temperature using Shimadzu Shim-pack CLC-ODS (M) 25M column linked to a UV-visible detector adjusted at 230 nm, employing 80:20 (v/v) methanol: water (pH 3.5) as mobile phase with flow rate 1.0 mL min-1. Validation was performed in the ranges 0.6-20, 0.9-28, 0.6-20 and 1.0-32 mu g mL-1 with lowest level corresponding to detection limit 16.45, 23.33, 27.66 and 14.44 ng mL-1 respectively. With-in the day precision ranged from 0.14-1.67% and between-day precision from 0.40-1.50%, accuracies were 99.61-100.86%. The analytes were successfully detected without any observable interference in pharmaceutical formulation and human serum samples demonstrating effectiveness of method. (author)

An innovative, simple, fast, and less toxic high-performance liquid chromatographic method for determination of prednisone in capsules

Directory of Open Access Journals (Sweden)

Pedro Henrique Reis da Silva

2017-06-01

Full Text Available ABSTRACT Prednisone is an anti-inflammatory steroid drug widely used in clinical practice. However, no high-performance liquid chromatographic (HPLC method has been described in the literature for the determination of prednisone in capsules until now. Thus, an HPLC method was developed using a C18 (250x4.0, 5 µm column, with methanol:water (70:30 as mobile phase at a flow rate of 1 mL/min and detection at 240 nm. The developed method was validated following current Brazilian legislation. Additionally, linearity was assessed by evaluating the assumptions of normality, homoscedasticity, and independency of residuals, and the fit to the linear model. The method showed linearity (r2>0.99 over the range of 14.0-26.0 µg/mL, selectivity, precision (RSD<2.0%, robustness, and accuracy (average recovery of 100.05%. The chromatographic procedure was applied for assay and uniformity content determination of three different batches of prednisone capsules, showing to be suitable for their quality control.

Incorporation of metal-organic framework HKUST-1 into porous polymer monolithic capillary columns to enhance the chromatographic separation of small molecules.

Science.gov (United States)

Yang, Shengchao; Ye, Fanggui; Lv, Qinghui; Zhang, Cong; Shen, Shufen; Zhao, Shulin

2014-09-19

Metal-organic framework (MOF) HKUST-1 nanoparticles have been incorporated into poly(glycidyl methacrylate-co-ethylene dimethacrylate) (HKUST-1-poly(GMA-co-EDMA)) monoliths to afford stationary phases with enhanced chromatographic performance of small molecules in the reversed phase capillary liquid chromatography. The effect of HKUST-1 nanoparticles in the polymerization mixture on the performance of the monolithic column was explored in detail. While the bare poly(GMA-co-EDMA) monolith exhibited poor resolution (RsHKUST-1 nanoparticles to the polymerization mixture provide high increased resolution (Rs≥1.3) and high efficiency ranged from 16,300 to 44,300plates/m. Chromatographic performance of HKUST-1-poly(GMA-co-EDMA) monolith was demonstrated by separation of various analytes including polycyclic aromatic hydrocarbons, ethylbenzene and styrene, phenols and aromatic acids using a binary polar mobile phase (CH3CN/H2O). The HKUST-1-poly(GMA-co-EDMA) monolith displayed enhanced hydrophobic and π-π interaction characteristics in the reversed phase separation of test analytes compared to the bare poly(GMA-co-EDMA) monolith. The experiment results showed that HKUST-1-poly(GMA-co-EDMA) monoliths are an alternative to enhance the chromatographic separation of small molecules. Copyright © 2014 Elsevier B.V. All rights reserved.

Development of a screening method for the determination of total polynuclear aromatic hydrocarbons (PAH) in water and wastewater

International Nuclear Information System (INIS)

Riggin, R.; Strup, P.; Billets, S.

1983-01-01

Polynuclear aromatic hydrocarbons (PAHs) represent an important class of organic compounds from an environmental standpoint, due to known human carcinogenicity of some members. Consequently, there is a great need for monitoring the PAH concentration of a variety of media, including water and industrial wastewater. Recently, the United States Environmental Protection Agency (U.S. EPA) developed a sensitive analytical method, designated Test Method 610, for the determination of priority pollutant PAHs in aqueous industrial discharges. This method employs reversed phase high performance liquid chromatography (HPLC) with ultraviolet (UV) and fluorescence detection to determine all sixteen priority pollutant PAHs in a single chromatographic separation

Performance of chromatographic systems to model soil-water sorption.

Science.gov (United States)

Hidalgo-Rodríguez, Marta; Fuguet, Elisabet; Ràfols, Clara; Rosés, Martí

2012-08-24

A systematic approach for evaluating the goodness of chromatographic systems to model the sorption of neutral organic compounds by soil from water is presented in this work. It is based on the examination of the three sources of error that determine the overall variance obtained when soil-water partition coefficients are correlated against chromatographic retention factors: the variance of the soil-water sorption data, the variance of the chromatographic data, and the variance attributed to the dissimilarity between the two systems. These contributions of variance are easily predicted through the characterization of the systems by the solvation parameter model. According to this method, several chromatographic systems besides the reference octanol-water partition system have been selected to test their performance in the emulation of soil-water sorption. The results from the experimental correlations agree with the predicted variances. The high-performance liquid chromatography system based on an immobilized artificial membrane and the micellar electrokinetic chromatography systems of sodium dodecylsulfate and sodium taurocholate provide the most precise correlation models. They have shown to predict well soil-water sorption coefficients of several tested herbicides. Octanol-water partitions and high-performance liquid chromatography measurements using C18 columns are less suited for the estimation of soil-water partition coefficients. Copyright © 2012 Elsevier B.V. All rights reserved.

A gas/liquid chromatographic-mass spectrometric method for the rapid screening of 250 pesticides in aqueous matrices

Energy Technology Data Exchange (ETDEWEB)

Chandramouli, B.; Harvan, D.; Brittain, S.; Hass, R. [Eno River Labs, LLC. Durham, NC (United States)

2004-09-15

Pesticide residues in food present a potentially serious and significant cause for concern. Many pesticides have been associated with significant health effects to the nervous and endocrine systems and some have been deemed carcinogenic. There are many well-established techniques for pesticide analysis. However, commercial pesticide methods have traditionally only been available for specific pesticide families, such as chlorinated pesticides or herbicides, and at detection limits ranging from 0.05 ppb to 1 ppm in aqueous matrices. Techniques that can quickly screen for the presence/absence of pesticide residues in food matrices are critical in ensuring the safety of food and water. This paper outlines a combined Gas Chromatographic-High Resolution Mass Spectrometric (GC-HRMS) and Liquid Chromatographic Tandem Mass Spectrometric (LC-MS/MS) screening assay for 250 pesticides that was developed for use in water, and soda samples at screening levels ranging from 0.1-5 ppb. The pesticides selected have been identified by the European Union as being of concern and the target of possible legislation. The list encompasses a variety of pesticide classes and compound groupings.

Measurements of activity coefficients at infinite dilution of aromatic and aliphatic hydrocarbons, alcohols, and water in the new ionic liquid [EMIM][SCN] using GLC

International Nuclear Information System (INIS)

Domanska, Urszula; Marciniak, Andrzej

2008-01-01

A new ionic liquid was chosen for the separation of aromatic hydrocarbons from aliphatic hydrocarbons. The activity coefficients at infinite dilution, γ 13 ∞ for 29 solutes: alkanes, alkenes, alkynes, cycloalkanes, aromatic hydrocarbons, alcohols, and water in the ionic liquid 1-ethyl-3-methyl-imidazolium thiocyanate [EMIM][SCN] were determined by gas-liquid chromatography at the temperatures from 298.15 K to 368.15 K. The values of the partial molar excess enthalpies at infinite dilution ΔH 1 E,∞ were calculated from the experimental γ 13 ∞ values obtained over the temperature range. The selectivities for the hexane/benzene and cyclohexane/benzene separation problems were calculated from the γ 13 ∞ and compared to the other ionic liquids, NMP and sulfolane, taken from the recent literature. This work demonstrates that with chosen ionic liquid it is possible to separate different organic compounds with the highest selectivity ever published

Liquid chromatographic and ultraviolet spectrophotometric determination of bevantolol and hydrochlorothiazide in feeds.

Science.gov (United States)

Spurlock, C H; Schneider, H G

1984-01-01

Separate assay methods have been developed for the 2 components of an 80 + 20 drug blend of bevantolol and hydrochlorothiazide (HCT) in admixtures with animal feed. Drug/diet admixtures are extracted with methanol for reverse phase ion-pair liquid chromatographic (LC) assay of bevantolol, and with acetonitrile for ultraviolet spectrophotometric assay of HCT. Bevantolol, a cardioselective beta blocker, is separated from soluble feed components with an RP-18 column, using methanol-water-acetic acid (60 + 40 + 1) containing 0. 005M octane-sulfonic acid, sodium salt, as ion-pairing reagent. HCT is determined spectrophotometrically in acetonitrile extracts, using a suitable blank extract as reference. Average recovery of HCT from an admixture of 0.5 mg blend/g diet is 94.5% +/- 4.3 RSD and at 2.0 mg/g, 101.5% +/- 3.5 RSD. Bevantolol recovery from the same admixtures is 101.8% +/- 2.7 RSD and 99.0% +/- 3.5 RSD, respectively, using the method as described.

Using Ionic Liquids in Selective Hydrocarbon Conversion Processes

Energy Technology Data Exchange (ETDEWEB)

Tang, Yongchun; Periana, Roy; Chen, Weiqun; van Duin, Adri; Nielsen, Robert; Shuler, Patrick; Ma, Qisheng; Blanco, Mario; Li, Zaiwei; Oxgaard, Jonas; Cheng, Jihong; Cheung, Sam; Pudar, Sanja

2009-09-28

This is the Final Report of the five-year project Using Ionic Liquids in Selective Hydrocarbon Conversion Processes (DE-FC36-04GO14276, July 1, 2004- June 30, 2009), in which we present our major accomplishments with detailed descriptions of our experimental and theoretical efforts. Upon the successful conduction of this project, we have followed our proposed breakdown work structure completing most of the technical tasks. Finally, we have developed and demonstrated several optimized homogenously catalytic methane conversion systems involving applications of novel ionic liquids, which present much more superior performance than the Catalytica system (the best-to-date system) in terms of three times higher reaction rates and longer catalysts lifetime and much stronger resistance to water deactivation. We have developed in-depth mechanistic understandings on the complicated chemistry involved in homogenously catalytic methane oxidation as well as developed the unique yet effective experimental protocols (reactors, analytical tools and screening methodologies) for achieving a highly efficient yet economically feasible and environmentally friendly catalytic methane conversion system. The most important findings have been published, patented as well as reported to DOE in this Final Report and our 20 Quarterly Reports.

DETERMINATION OF SOLID-LIQUID EQUILIBRIA DATA FOR MIXTURES OF HEAVY HYDROCARBONS IN A LIGHT SOLVENT

Energy Technology Data Exchange (ETDEWEB)

F.V. Hanson; J.V. Fletcher; Karthik R.

2003-06-01

A methodology was developed using an FT-IR spectroscopic technique to obtain solid-liquid equilibria (SLE) data for mixtures of heavy hydrocarbons in significantly lighter hydrocarbon diluents. SLE was examined in multiple Model Oils that were assembled to simulate waxes. The various Model oils were comprised of C-30 to C-44 hydrocarbons in decane. The FT-IR technique was used to identify the wax precipitation temperature (WPT). The DSC technique was also used in the identification of the onset of the two-phase equilibrium in this work. An additional Model oil made up of C-20 to C-30 hydrocarbons in decane was studied using the DSC experiment. The weight percent solid below the WPT was calculated using the FT-IR experimental results. The WPT and the weight percent solid below the WPT were predicted using an activity coefficient based thermodynamic model. The FT-IR spectroscopy method is found to successfully provide SLE data and also has several advantages over other laboratory-based methods.

A multiresidue method by high performance liquid chromatography-based fractionation and gas chromatographic determination of trace levels of pesticides in air and water.

Science.gov (United States)

Seiber, J N; Glotfelty, D E; Lucas, A D; McChesney, M M; Sagebiel, J C; Wehner, T A

1990-01-01

A multiresidue analytical method is described for pesticides, transformation products, and related toxicants based upon high performance liquid chromatographic (HPLC) fractionation of extracted residue on a Partisil silica gel normal phase column followed by selective-detector gas chromatographic (GC) determination of components in each fraction. The HPLC mobile phase gradient (hexane to methyl t-butyl ether) gave good chromatographic efficiency, resolution, reproducibility and recovery for 61 test compounds, and allowed for collection in four fractions spanning polarities from low polarity organochlorine compounds (fraction 1) to polar N-methylcarbamates and organophosphorus oxons (fraction 4). The multiresidue method was developed for use with air samples collected on XAD-4 and related trapping agents, and water samples extracted with methylene chloride. Detection limits estimated from spiking experiments were generally 0.3-1 ng/m3 for high-volume air samples, and 0.01-0.1 microgram/L for one-liter water samples. Applications were made to determination of pesticides in fogwater and air samples.

Plasma devices for hydrocarbon reformation

KAUST Repository

Cha, Min

2017-01-01

Plasma devices for hydrocarbon reformation are provided. Methods of using the devices for hydrocarbon reformation are also provided. The devices can include a liquid container to receive a hydrocarbon source, and a plasma torch configured

The development of a high performance liquid chromatograph with a sensitive on-stream radioactivity monitor for the analysis of 3H- and 14C-labelled gibberellins

International Nuclear Information System (INIS)

Reeve, D.R.; Yokota, T.; Nash, L.; Crozier, A.

1976-01-01

The development of a high performance liquid chromatograph for the separation of gibberellins is described. The system combines high efficiency, peak capacity, and sample capacity with rapid speed of analysis. In addition, the construction details of a sensitive on-stream radioactivity monitor are outlined. The overall versatility of the chromatograph has been demonstrated by the separation of a range of 3 H- and 14 C-labelled gibberellins and gibberellin precursors. The system also has considerable potential for the analysis of abscisic acid and acidic and neutral indoles. (author)

Detection of radiation-induced hydrocarbons in baked sponged cake prepared with irradiated liquid egg

Science.gov (United States)

Schulzki, G.; Spiegelberg, A.; Bögl, K. W.; Schreiber, G. A.

1995-02-01

For identification of irradiated food, radiation-induced volatile hydrocarbons (HC) are determined by gas chromatography in the non-polar fraction of fat. However, in complex food matrices the detection is often disturbed by fat-associated compounds. On-line coupling of high performance liquid chromatography (LC) and gas chromatography (GC) is very efficient to remove such compounds from the HC fraction. The high sensitivity of this fast and efficient technique is demonstrated by the example of detection of radiation-induced HC in fat isolated from baked sponge cake which had been prepared with irradiated liquid egg.

Enrichment of light hydrocarbon mixture

Science.gov (United States)

Yang,; Dali, [Los Alamos, NM; Devlin, David [Santa Fe, NM; Barbero, Robert S [Santa Cruz, NM; Carrera, Martin E [Naperville, IL; Colling, Craig W [Warrenville, IL

2010-08-10

Light hydrocarbon enrichment is accomplished using a vertically oriented distillation column having a plurality of vertically oriented, nonselective micro/mesoporous hollow fibers. Vapor having, for example, both propylene and propane is sent upward through the distillation column in between the hollow fibers. Vapor exits neat the top of the column and is condensed to form a liquid phase that is directed back downward through the lumen of the hollow fibers. As vapor continues to ascend and liquid continues to countercurrently descend, the liquid at the bottom of the column becomes enriched in a higher boiling point, light hydrocarbon (propane, for example) and the vapor at the top becomes enriched in a lower boiling point light hydrocarbon (propylene, for example). The hollow fiber becomes wetted with liquid during the process.

SIMULTANEOUS ANALYSIS OF AZIDOTHYMIDINE AND ITS MONOPHOSPHATE, DIPHOSPHATE AND TRIPHOSPHATE DERIVATIVES IN BIOLOGICAL-FLUIDS, TISSUE AND CULTURED-CELLS BY A RAPID HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHIC METHOD

NARCIS (Netherlands)

MOLEMA, G; JANSEN, RW; Visser, Jan; MEIJER, DKF

1992-01-01

A rapid high-performance liquid chromatographic (HPLC) method for the simultaneous analysis of the antiviral drug azidothymidine (AZT), AZT monophosphate, AZT diphosphate and AZT triphosphate, with ultraviolet detection in the nanomolar range, is described. Determination of these compounds in vitro

Inductively coupled plasma emission spectrometric detection of simulated high performance liquid chromatographic peaks

International Nuclear Information System (INIS)

Fraley, D.M.; Yates, D.; Manahan, S.E.

1979-01-01

Because of its multielement capability, element-specificity, and low detection limits, inductively coupled plasma optical emission spectrometry (ICP) is a very promising technique for the detection of specific elemental species separated by high performance liquid chromatography (HPLC). This paper evaluated ICP as a detector for HPLC peaks containing specific elements. Detection limits for a number of elements have been evaluated in terms of the minimum detectable concentration of the element at the chromatographic peak maximum. The elements studies were Al, As, B, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, Sb, Se, Sr, Ti, V, and Zn. In addition, ICP was compared with atomic absorption spectrometry for the detection of HPLC peaks composed of EDTA and NTA chelates of copper. Furthermore, ICP was compared to uv solution absorption for the detection of copper chelates. 6 figures, 4 tables

Method for the simultaneous determination of monoaromatic and polycyclic aromatic hydrocarbons in industrial effluents using dispersive liquid-liquid microextraction with gas chromatography-mass spectrometry.

Science.gov (United States)

Makoś, Patrycja; Fernandes, André; Boczkaj, Grzegorz

2018-02-23

We present a new method for simultaneous determination of 22 monoaromatic and polycyclic aromatic hydrocarbons in postoxidative effluents from the production of petroleum bitumen using dispersive liquid-liquid microextraction coupled to gas chromatography and mass spectrometry. The eight extraction parameters including the type and volume of extraction and disperser solvent, pH, salting out effect, extraction, and centrifugation time were optimized. The low detection limit ranging from 0.36 to 28 μg/L, limit of quantitation (1.1-84 μg/L), good reproducibility, and wide linear ranges, as well as the recoveries ranging from 71.74 to 114.67% revealed that the new method allows the determination of aromatic hydrocarbons at low concentration levels in industrial effluents having a very complex composition. The developed method was applied to the determination of content of mono- and polycyclic aromatic hydrocarbons in samples of raw postoxidative effluents in which 15 compounds were identified at concentrations ranging from 1.21 to 1017.0 μg/L as well as in effluents after chemical treatment. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Extraction of polycyclic aromatic hydrocarbons from smoked fish using pressurized liquid extraction with integrated fat removal

DEFF Research Database (Denmark)

Lund, Mette; Duedahl-Olesen, Lene; Christensen, Jan H.

2009-01-01

Quantification of polycyclic aromatic hydrocarbons (PAHs) in smoked fish products often requires multiple clean-up steps to remove fat and other compounds that may interfere with the chemical analysis. We present a novel pressurized liquid extraction (PLE) method that integrates exhaustive...

Liquid chromatographic determination of polyphenenols in czech beers during brewing proces

Directory of Open Access Journals (Sweden)

Chunsriimyatav Ganbaatar

2015-05-01

Full Text Available High performance liquid chromatographic (HPLC/UV method was adapted for simultaneous determination of seven polyphenols, including derivatives of benzoic (gallic and vanillic acids and cinnamic acids (p-coumaric, ferulic and sinapic acids, flavan-3-ols (catechin and flavonols (rutin in worts and beers at the various stages of the brewing process. Based on the semi-quantitative HPLC analysis, total polyphenols chromatographic index (TPCI was in the ranges of 5.18 - 19.4 mg/L and 7.37 - 20.7 mg/L for all worts and beers, respectively. The HPLC analyses showed that relatively high levels of (+-catechin and gallic acid were in all the worts and the beers, while the values were much lower for ferulic acid, rutin, vanillic acid, sinapic acid and p-coumaric acid. Polyphenols with relatively high concentrations, that were detected in all tested worts and beers, were gallic acid (1.29 - 4.75 mg/L resp. 2.59 - 4.97 mg/L, (+-catechin (1.66 - 7.95 mg/L resp. 4.70 - 10.0 mg/L and ferulic acid (0.41 - 4.53 mg/L resp. 1.05 - 2.87 mg/L. On the other side, the sinapic acid (0.72 - 1.59 mg/L resp. 0.72 - 2.5 mg/L, rutin (1.17 - 2.03 mg/L resp. 1.16 - 2.85 mg/L, p-coumaric acid (ND - 4.73 mg/L resp. ND - 1.44 mg/L and vanillic acid (ND - 1.52 mg/L resp. 0.75 - 1.81 mg/L were detected in lowest concentrations. In both, worts and beers investigated in this study, the changes in the contents of individual polyphenols were not uniform. In the case of some polyphenols, a decrease in the content was observed after boiling the worts with hops or after the main fermentation until maturation and filtration, but with some polyphenols, the concentrations were constant until the end of the process or even increased.

Guidelines for Constructing Natural Gas and Liquid Hydrocarbon Pipelines Through Areas Prone to Landslide and Subsidence Hazards

Science.gov (United States)

2009-01-01

These guidelines provide recommendations for the assessment of new and existing natural gas and liquid hydrocarbon pipelines subjected to potential ground displacements resulting from landslides and subsidence. The process of defining landslide and s...

Liquid chromatographic and spectrophotometric methods for the determination of erythromycin stearate and trimethoprim in tablets

Directory of Open Access Journals (Sweden)

Sonia T. Hassib

2011-12-01

Full Text Available Simple, accurate and precise reversed-phase liquid chromatographic (LC and spectrophotometric methods have been developed and validated for the determination of erythromycin stearate (ERS and trimethoprim (TMP in mixture. In LC method, chromatographic separation was achieved on a Symmetry® Waters C18 column (150 × 4.6 mm, 5 μm based on isocratic elution using a mobile phase consisting of potassium dihydrogen phosphate buffer pH (9:acetonitrile:water (25:100:50, v/v/v at a flow rate of 1.6 ml min−1 with UV detection at 210 nm for ERS and 280 nm for TMP. Besides, two spectrophotometric methods were applied after reaction with perchloric acid (12 M which gives a colored product with ERS. Then, the spectral interference between the colored product of ERS and TMP was resolved by either ratio spectra derivative spectrophotometry in the first spectrophotometric method or chemometric techniques, namely classical least-squares (CLS, principal component regression (PCR and partial least-squares regression (PLS in the second spectrophotometric method. The results were statistically compared using one-way analysis of variance (ANOVA. The methods developed were satisfactorily applied to the analysis of the pharmaceutical preparation containing the two drugs and proved to be specific and accurate for the quality control of the cited drugs in pharmaceutical dosage forms.

A rapid hydrophilic interaction liquid chromatographic determination of glimepiride in pharmaceutical formulations

Directory of Open Access Journals (Sweden)

Si Zhou

2017-09-01

Full Text Available Glimepiride is one of the most widely prescribed antidiabetic drugs and contains both hydrophobic and hydrophilic functional groups in its molecules, and thus could be analyzed by either reversed-phase high performance liquid chromatography (HPLC or hydrophilic interaction liquid chromatography (HILIC. In the literature, however, only reversed-phase HPLC has been reported. In this study, a simple, rapid and accurate hydrophilic interaction liquid chromatographic method was developed for the determination of glimepiride in pharmaceutical formulations. The analytical method comprised a fast ultrasound-assisted extraction with acetonitrile as a solvent followed by HILIC separation and quantification using a Waters Spherisorb S5NH2 hydrophilic column with a mobile phase consisting of acetonitrile and aqueous acetate buffer (5.0 mM. The retention time of glimepiride increased slightly with decrease of mobile phase pH value from 6.8 to 5.8 and of acetonitrile content from 60% to 40%, indicating that both hydrophilic, ionic, and hydrophobic interactions were involved in the HILIC retention and elution mechanisms. Quantitation was carried out with a mobile phase of 40% acetonitrile and 60% aqueous acetate buffer (5.0 mM at pH 6.3, by relating the peak area of glimepiride to that of the internal standard, with a detection limit of 15.0 μg/L. UV light absorption responses at 228 nm were linear over a wide concentration range from 50.0 μg/L to 6.00 mg/L. The recoveries of the standard added to pharmaceutical tablet samples were 99.4–103.0% for glimepiride, and the relative standard deviation for the analyte was less than 1.0%. This method has been successfully applied to determine the glimepiride contents in pharmaceutical formulations.

Development of Chromatographic Fingerprints of Eurycoma longifolia (Tongkat Ali Roots Using Online Solid Phase Extraction-Liquid Chromatography (SPE-LC

Directory of Open Access Journals (Sweden)

Nor Nasriah Zaini

2016-04-01

Full Text Available E. longifolia is attracting interest due to its pharmacological properties and pro-vitality effects. In this study, an online SPE-LC approach using polystyrene divinyl benzene (PSDVB and C18 columns was developed in obtaining chromatographic fingerprints of E. longifolia. E. longifolia root samples were extracted using pressurized liquid extraction (PLE technique prior to online SPE-LC. The effects of mobile phase compositions and column switching time on the chromatographic fingerprint were optimized. Validation of the developed method was studied based on eurycomanone. Linearity was in the range of 5 to 50 µg∙mL−1 (r2 = 0.997 with 3.2% relative standard deviation of peak area. The developed method was used to analyze 14 E. longifolia root samples and 10 products (capsules. Selected chemometric techniques: cluster analysis (CA, discriminant analysis (DA, and principal component analysis (PCA were applied to the fingerprint datasets of 37 selected peaks to evaluate the ability of the chromatographic fingerprint in classifying quality of E. longifolia. Three groups were obtained using CA. DA yielded 100% correlation coefficient with 19 discriminant compounds. Using PCA, E. longifolia root samples were clearly discriminated from the products. This study showed that the developed online SPE-LC method was able to provide comprehensive evaluation of E. longifolia samples for quality control purposes.

Liquid chromatographic determination of pioglitazone in pharmaceuticals, serum and urine samples

International Nuclear Information System (INIS)

Abro, K.; Memon, N.; Bhanger, M.I.; Mahesar, S.A.; Parveen, S.

2011-01-01

A rapid and reliable analytical method based on high-performance liquid chromatography (HPLC) with UV detection (221 nm) has been developed for the determination of the anti-hyper glycemic agent Pioglitazone in pharmaceutical formulations and biological fluids (serum and urine) after clean-up with solid-phase extraction. Chromatographic separation was achieved with a Chromolith Performance RP-18e (10 4.6mm) column using mobile phase composition of acetonitrile: mixed phosphate buffer (pH 2.5; 10mM) (30:70, v/v) with a flow rate of 2.0mL/min. The total run time was 2 min. under optimized conditions. The calibration curve was found to be linear in the range of 1-10 mu g mL/sup -1/ with regression coefficient of 0.9996, and the lower limit of detection 72 ng/20 mu L injection. The method has been validated for the system suitability, linearity, precision and accuracy, limits of detection, specificity, stability and robustness. The %recovery of Pioglitazone in pharmaceutical formulations was found to be 104.7%. The assay has been applied successfully to the pharmaceutical Tablet samples and biological fluids (serum and urine) of healthy volunteers. (author)

Detection of radiation-induced hydrocarbons in baked sponge cake prepared with irradiated liquid egg

International Nuclear Information System (INIS)

Schulzki, G.; Spiegelberg, A.; Boegl, K.W.; Schreiber, G.A.

1995-01-01

For identification of irradiated food, radiation-induced volatile hydrocarbons (HC) are determined by gas chromatography in the non-polar fraction of fat. However, in complex food matrices the detection is often disturbed by fat-associated compounds. On-line coupling of high performance liquid chromatography (LC) and gas chromatography (GC) is very efficient to remove such compounds from the HC fraction. The high sensitivity of this fast and efficient technique is demonstrated by the example of detection of radiation-induced HC in fat isolated from baked sponge cake which had been prepared with irradiated liquid egg. (Author)

Gas chromatography-mass spectrometry and high-performance liquid chromatographic analyses of thermal degradation products of common plastics

OpenAIRE

Pacakova, V.; Leclercq, P.A.

1991-01-01

The thermo-oxidation of five commonly used materials, namely low-density polyethylene, retarded polyethylene, paper with a polyethylene foil, a milk package and filled polypropylene, was studied. Capillary gas chromatography and gas chromatography-mass spectrometry were used to analyze the volatile degradation products, while high-performance liquid chromatography was employed to measure polycyclic aromatic hydrocarbons. The results are discussed from the point of view of toxicity of the prod...

A novel two-dimensional liquid chromatographic system for the online toxicity prediction of pharmaceuticals and related substances

Energy Technology Data Exchange (ETDEWEB)

Li, Jian; Xu, Li [Tongji School of Pharmacy, Huazhong University of Science and Technology, Wuhan 430030 (China); Shi, Zhi-guo, E-mail: shizg@whu.edu.cn [Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu, Min [Hubei Instrument for Food and Drug Control, Wuhan (China)

2015-08-15

Highlights: • A novel two-dimensional liquid chromatographic system was developed. • The 1st dimension was ODS to separate components in the sample. • The 2nd dimension was biopartitioning micellar chromatography to predict toxicity. • The system was used to screen toxicity of pharmaceuticals and related substances. • It was promising for fast online toxicity screening of complex sample in one step. - Abstract: In this study, a novel two-dimensional liquid chromatographic (2D-LC) system was developed for simultaneous separation and toxicity prediction of pharmaceutical and its related substances. A conventional ODS column was used on the 1st-D to separate the sample; while, bio-partitioning micellar chromatography served as the 2nd-D to predict toxicity of the components. The established system was tested for the toxicity of ibuprofen and its impurities with known toxicity. With only one injection, ibuprofen and its impurities were separated on the 1st-D; and LC50 values of individual impurity were obtained based on the quantitative retention–activity relationships, which agreed well with the reported data. Furthermore, LC50 values of photolysis transformation products (TPs) of carprofen, ketoprofen and diclofenac acid (as unknown compounds) were screened in this 2D-LC system, which could be an indicator of the toxicity of these TPs and was meaningful for the environmental monitoring and drinking water treatment. The established 2D-LC system was cost-effective, time-saving and reliable, and was promising for fast online screening of toxicity of known and unknown analytes in the complex sample in a single step. It may find applications in environment, pharmaceutical and food, etc.

A novel two-dimensional liquid chromatographic system for the online toxicity prediction of pharmaceuticals and related substances

International Nuclear Information System (INIS)

Li, Jian; Xu, Li; Shi, Zhi-guo; Hu, Min

2015-01-01

Highlights: • A novel two-dimensional liquid chromatographic system was developed. • The 1st dimension was ODS to separate components in the sample. • The 2nd dimension was biopartitioning micellar chromatography to predict toxicity. • The system was used to screen toxicity of pharmaceuticals and related substances. • It was promising for fast online toxicity screening of complex sample in one step. - Abstract: In this study, a novel two-dimensional liquid chromatographic (2D-LC) system was developed for simultaneous separation and toxicity prediction of pharmaceutical and its related substances. A conventional ODS column was used on the 1st-D to separate the sample; while, bio-partitioning micellar chromatography served as the 2nd-D to predict toxicity of the components. The established system was tested for the toxicity of ibuprofen and its impurities with known toxicity. With only one injection, ibuprofen and its impurities were separated on the 1st-D; and LC50 values of individual impurity were obtained based on the quantitative retention–activity relationships, which agreed well with the reported data. Furthermore, LC50 values of photolysis transformation products (TPs) of carprofen, ketoprofen and diclofenac acid (as unknown compounds) were screened in this 2D-LC system, which could be an indicator of the toxicity of these TPs and was meaningful for the environmental monitoring and drinking water treatment. The established 2D-LC system was cost-effective, time-saving and reliable, and was promising for fast online screening of toxicity of known and unknown analytes in the complex sample in a single step. It may find applications in environment, pharmaceutical and food, etc

Stacking faults and mechanisms strain-induced transformations of hcp metals (Ti, Mg) during mechanical activation in liquid hydrocarbons

Science.gov (United States)

Lubnin, A. N.; Dorofeev, G. A.; Nikonova, R. M.; Mukhgalin, V. V.; Lad'yanov, V. I.

2017-11-01

The evolution of the structure and substructure of metals Ti and Mg with hexagonal close-packed (hcp) lattice is studied during their mechanical activation in a planetary ball mill in liquid hydrocarbons (toluene, n-heptane) and with additions of carbon materials (graphite, fullerite, nanotubes) by X-ray diffraction, scanning electron microscopy, and chemical analysis. The temperature behavior and hydrogen-accumulating properties of mechanocomposites are studied. During mechanical activation of Ti and Mg, liquid hydrocarbons decay, metastable nanocrystalline titanium carbohydride Ti(C,H) x and magnesium hydride β-MgH2 are formed, respectively. The Ti(C,H) x and MgH2 formation mechanisms during mechanical activation are deformation ones and are associated with stacking faults accumulation, and the formation of face-centered cubic (fcc) packing of atoms. Metastable Ti(C,H)x decays at a temperature of 550°C, the partial reverse transformation fcc → hcp occurs. The crystalline defect accumulation (nanograin boundaries, stacking faults), hydrocarbon destruction, and mechanocomposite formation leads to the enhancement of subsequent magnesium hydrogenation in the Sieverts reactor.

Use of adsorption and gas chromatographic techniques in estimating biodegradation of indigenous crude oils

International Nuclear Information System (INIS)

Kokub, D.; Allahi, A.; Shafeeq, M.; Khalid, Z.M.; Malik, K.A.; Hussain, A.

1993-01-01

Indigenous crude oils could be degraded and emulsified upto varying degree by locally isolated bacteria. Degradation and emulsification was found to be dependent upon the chemical composition of the crude oils. Tando Alum and Khashkheli crude oils were emulsified in 27 and 33 days of incubation respectively. While Joyamair crude oil and not emulsify even mainly due to high viscosity of this oil. Using adsorption chromatographic technique, oil from control (uninoculated) and bio degraded flasks was fractioned into the deasphaltened oil containing saturate, aromatic, NSO (nitrogen, sulphur, oxygen) containing hydrocarbons) and soluble asphaltenes. Saturate fractions from control and degraded oil were further analysed by gas liquid chromatography. From these analyses, it was observed that saturate fraction was preferentially utilized and the crude oils having greater contents of saturate fraction were better emulsified than those low in this fraction. Utilization of various fractions of crude oils was in the order saturate> aromatic> NSO. (author)

Simple fluorimetric liquid chromatographic method for the analysis of undecylenic acid and zinc undecylenate in pharmaceutical preparations.

Science.gov (United States)

Lin, Ming-Chun; Wu, Hsin-Lung; Kou, Hwang-Shang; Wu, Shou-Mei

2006-06-30

A simple and selective liquid chromatographic method is described for the analysis of undecylenic acid (UA) and zinc undecylenate (ZnUA) in pharmaceutical preparations. The method is based on the derivatization of the analytes extracted from various samples with 2-(2-naphthoxy)ethyl 2-(piperidino)ethanesulfonate. The resulting derivative was analyzed by liquid chromatography with fluorimetric detection. The quantitation of the method is in the range of 3.0-50.0 microM UA with a detection limit of about 0.3 microM (S/N = 3 with 10 microl injection). We found that acetonitrile is a selective solvent for differentially dissolving UA from coexisted ZnUA in compound formulation. This results in the specific analysis of UA in the presence of ZnUA and simply analyzing the coexisted ZnUA by the value of total UA (UA+ZnUA) minus that of UA. Application of the method to the analysis of undecylenic acid and zinc undecylenate in ointment, powder and solution preparations proved feasible.

Application of ionic liquids in liquid chromatography and electrodriven separation.

Science.gov (United States)

Huang, Yi; Yao, Shun; Song, Hang

2013-08-01

Ionic liquids (ILs) are salts in the liquid state at ambient temperature, which are nonvolatile, nonflammable with high thermal stability and dissolve easily for a wide range of inorganic and organic materials. As a kind of potential green solvent, they show high efficiency and selectivity in the field of separation research, especially in instrumental analysis. Thus far, ILs have been successfully applied by many related researchers in high-performance liquid chromatography and capillary electrophoresis as chromatographic stationary phases, mobile phase additives or electroosmotic flow modifiers. This paper provides a detailed review of these applications in the study of natural products, foods, drugs and other fine chemicals. Furthermore, the prospects of ILs in liquid chromatographic and electrodriven techniques are discussed.

Remediation of hydrocarbons in crude oil-contaminated soils using Fenton's reagent.

Science.gov (United States)

Ojinnaka, Chukwunonye; Osuji, Leo; Achugasim, Ozioma

2012-11-01

Sandy soil samples spiked with Bonny light crude oil were subsequently treated with Fenton's reagent at acidic, neutral, and basic pH ranges. Oil extracts from these samples including an untreated one were analyzed 1 week later with a gas chromatograph to provide evidence of hydrocarbon depletion by the oxidant. The reduction of three broad hydrocarbon groups-total petroleum hydrocarbon (TPH); benzene, toluene, ethylbenzene, and xylene (BTEX); and polycyclic aromatic hydrocarbon (PAH) were investigated at various pHs. Hydrocarbon removal was efficient, with treatment at the acidic pH giving the highest removal of about 96% for PAH, 99% for BTEX, and some TPH components experiencing complete disappearance. The four-ringed PAHs were depleted more than their three-ringed counterparts at the studied pH ranges.

High performance liquid chromatographic determination of glucosamine in rat plasma.

Science.gov (United States)

Aghazadeh-Habashi, Ali; Sattari, Saeed; Pasutto, Franco; Jamali, Fakhreddin

2002-01-01

A high performance liquid chromatographic method was developed for the determination of glucosamine (GlcN) in rat plasma. Internal standard, galactosamine, was added to 100 micro L of plasma containing GlcN followed by precipitation of plasma proteins with acetonitrile. Evaporation of the decanted supernatant solution was accelerated by the addition of methanol. GlcN was derivatized by addition of a solution containing 1-naphthyl isothiocyanate. Sample cleanup included passage through an anion exchange cartridge. Analysis was accomplished by injection of 0.1 mL of the sample solution into an isocratic HPLC system consisting of a C18 column, a mobile phase of acetonitrile: water: acetic acid: triethylamine (4.5: 95.5:0.1:0.05), a flow rate of 0.9 mL/min, and a UV detector set at 254 nm. Galactosamine and GlcN appeared 26 and 29 min post-injection, respectively. The assay was linear over the range of 1.25-400 micro g/mL (CV<10%) with a detection limit of 0.63 microg/mL and a limit of quantification of 1.25 microg/mL. The method was applied to the determination of GlcN in rat plasma after oral administration of 350 mg/kg of GlcN hydrochloride. The present assay is specific, sensitive, precise, and accurate and is suitable for pharmacokinetic studies.

Pyrolysis gas chromatographic atomic emission detection for sediments, coals and other petrochemical precursors

Energy Technology Data Exchange (ETDEWEB)

Seeley, J.A.; Zeng, Y.D.; Uden, P.C.; Eglinton, T.I.; Ericson, I. (Massachusetts University, Amherst, MA (USA). Dept. of Chemistry)

1992-09-01

On-line flash pyrolysis coupled to a capillary gas chromatograph for the characterization of marine sediments, coals and other heterogeneous solid samples is described. A helium microwave-induced plasma is used for chromatographic detection by atomic emission spectrometry. Simultaneous multi-element detection is achieved with a photodiode array detector. The optical path of the gas chromatographic atomic emission detector is purged with helium, allowing simultaneous, sensitive detection of atomic emission from sulfur 181 nm, phosphorous 186 nm, arsenic 189 nm, selenium 196 nm and carbon 193 nm. Several sediment and coal samples have been analysed for their carbon, nitrogen, sulfur, oxygen, phosphorous, arsenic and selenium content. Qualitative information indicating the occurrence and distribution of these elements in the samples can be used to gauge the relative stage of diagenetic evolution of the samples and provide information on their depositional environment. In some instances the chromatographic behaviour of the compounds produced upon pyrolysis is improved through on-line alkylation. This on-line derivatization is achieved by adding liquid reagents to the pyrolysis probe or by adding liquid reagents to the pyrolysis probe or by adding solid reagents either to the solid sample or by packing the reagent in the injection port of the chromatograph.

Determination of solute descriptors by chromatographic methods

International Nuclear Information System (INIS)

Poole, Colin F.; Atapattu, Sanka N.; Poole, Salwa K.; Bell, Andrea K.

2009-01-01

The solvation parameter model is now well established as a useful tool for obtaining quantitative structure-property relationships for chemical, biomedical and environmental processes. The model correlates a free-energy related property of a system to six free-energy derived descriptors describing molecular properties. These molecular descriptors are defined as L (gas-liquid partition coefficient on hexadecane at 298 K), V (McGowan's characteristic volume), E (excess molar refraction), S (dipolarity/polarizability), A (hydrogen-bond acidity), and B (hydrogen-bond basicity). McGowan's characteristic volume is trivially calculated from structure and the excess molar refraction can be calculated for liquids from their refractive index and easily estimated for solids. The remaining four descriptors are derived by experiment using (largely) two-phase partitioning, chromatography, and solubility measurements. In this article, the use of gas chromatography, reversed-phase liquid chromatography, micellar electrokinetic chromatography, and two-phase partitioning for determining solute descriptors is described. A large database of experimental retention factors and partition coefficients is constructed after first applying selection tools to remove unreliable experimental values and an optimized collection of varied compounds with descriptor values suitable for calibrating chromatographic systems is presented. These optimized descriptors are demonstrated to be robust and more suitable than other groups of descriptors characterizing the separation properties of chromatographic systems.

Determination of solute descriptors by chromatographic methods.

Science.gov (United States)

Poole, Colin F; Atapattu, Sanka N; Poole, Salwa K; Bell, Andrea K

2009-10-12

The solvation parameter model is now well established as a useful tool for obtaining quantitative structure-property relationships for chemical, biomedical and environmental processes. The model correlates a free-energy related property of a system to six free-energy derived descriptors describing molecular properties. These molecular descriptors are defined as L (gas-liquid partition coefficient on hexadecane at 298K), V (McGowan's characteristic volume), E (excess molar refraction), S (dipolarity/polarizability), A (hydrogen-bond acidity), and B (hydrogen-bond basicity). McGowan's characteristic volume is trivially calculated from structure and the excess molar refraction can be calculated for liquids from their refractive index and easily estimated for solids. The remaining four descriptors are derived by experiment using (largely) two-phase partitioning, chromatography, and solubility measurements. In this article, the use of gas chromatography, reversed-phase liquid chromatography, micellar electrokinetic chromatography, and two-phase partitioning for determining solute descriptors is described. A large database of experimental retention factors and partition coefficients is constructed after first applying selection tools to remove unreliable experimental values and an optimized collection of varied compounds with descriptor values suitable for calibrating chromatographic systems is presented. These optimized descriptors are demonstrated to be robust and more suitable than other groups of descriptors characterizing the separation properties of chromatographic systems.

Determination of drugs in biological fluids by direct injection of samples for liquid-chromatographic analysis.

Science.gov (United States)

Mullett, Wayne M

2007-03-10

The analysis of drugs in various biological fluids is an important criterion for the determination of the physiological performance of a drug. After sampling of the biological fluid, the next step in the analytical process is sample preparation. The complexity of biological fluids adds to the challenge of direct determination of the drug by chromatographic analysis, therefore demanding a sample preparation step that is often time-consuming, tedious, and frequently overlooked. However, direct on-line injection methods offer the advantage of reducing sample preparation steps and enabling effective pre-concentration and clean-up of biological fluids. These procedures can be automated and therefore reduce the requirements for handling potentially infectious biomaterial, improve reproducibility, and minimize sample manipulations and potential contamination. The objective of this review is to present an overview of the existing literature with emphasis on advances in automated sample preparation methods for liquid-chromatographic methods. More specifically, this review concentrates on the use of direct injection techniques, such as restricted-access materials, turbulent-flow chromatography and other automated on-line solid-phase extraction (SPE) procedures. It also includes short overviews of emerging automated extraction-phase technologies, such as molecularly imprinted polymers, in-tube solid-phase micro-extraction, and micro-extraction in a packed syringe for a more selective extraction of analytes from complex samples, providing further improvements in the analysis of biological materials. Lastly, the outlook for these methods and potential new applications for these technologies are briefly discussed.

Total Hydrocarbon Content (THC) Testing in Liquid Oxygen (LOX)

Science.gov (United States)

Meneghelli, B. J.; Obregon, R. E.; Ross, H. R.; Hebert, B. J.; Sass, J. P.; Dirschka, G. E.

2016-01-01

The measured Total Hydrocarbon Content (THC) levels in liquid oxygen (LOX) systems at Stennis Space Center (SSC) have shown wide variations. Examples of these variations include the following: 1) differences between vendor-supplied THC values and those obtained using standard SSC analysis procedures; and 2) increasing THC values over time at an active SSC test stand in both storage and run vessels. A detailed analysis of LOX sampling techniques, analytical instrumentation, and sampling procedures will be presented. Additional data obtained on LOX system operations and LOX delivery trailer THC values during the past 12-24 months will also be discussed. Field test results showing THC levels and the distribution of the THC's in the test stand run tank, modified for THC analysis via dip tubes, will be presented.

SHPOLSKII FLUOROMETRIC-DETERMINATION OF POLYCYCLIC AROMATIC-HYDROCARBONS IN COMPLEX ENVIRONMENTAL-SAMPLES

NARCIS (Netherlands)

ARIESE, F; GOOIJER, C; Velthorst, N.H.; Hofstraat, J.W.

1991-01-01

High-resolution fluorimetry in low-temperature n-alkane Shpol'skii matrices is a powerful technique for the analysis of rigid, non-polar compounds like polycyclic aromatic hydrocarbons. Because of the method's sensitivity and selectivity, sample clean-up, preconcentration and even chromatographic

Development of liquid chromatographic methods for the determination of phytosterols in Standard Reference Materials containing saw palmetto.

Science.gov (United States)

Bedner, Mary; Schantz, Michele M; Sander, Lane C; Sharpless, Katherine E

2008-05-23

Liquid chromatographic (LC) methods using atmospheric pressure chemical ionization/mass spectrometric (APCI-MS) detection were developed for the separation and analysis of the phytosterols campesterol, cycloartenol, lupenone, lupeol, beta-sitosterol, and stigmasterol. Brassicasterol and cholesterol were also included for investigation as internal standards. The methods were used to identify and quantify the phytosterols in each of two Serenoa repens (saw palmetto) Standard Reference Materials (SRMs) developed by the National Institute of Standards and Technology (NIST). Values obtained by LC-MS were compared to those obtained using the more traditional approach of gas chromatography with flame ionization detection. This is the first reported use of LC-MS to determine phytosterols in saw palmetto dietary supplement materials.

High performance liquid chromatographic determination of vanadium in crude oils and cobalt and iron in pharmaceutical preparations

International Nuclear Information System (INIS)

Khuhawar, M.Y.; Lanjwani, S.N.; Khaskhely, G.Q.

1993-01-01

High performance liquid Chromatographic (HPLC) method has ben developed for the determination of vanadium in crude oils, based on acid decomposition of oils, followed by complexation with bis (salicylaldehyde) tetramethyl ethylenediamine (H2SA2Ten). The complex is extracted in organic phase and is separated from copper and nickel using normal phase HPLC column. Detection is achieved using spectrophtmetric detector. The vanadium in oil is obtained at sub microgram/g level. Similarly cobalt(II), cobalt(III) and iron(II) are separated on reversed phase HPLC column. Pre column derivatization is used to develop HPLC method for the determination of cobalt and iron in pharmaceutical preparations. Finally results are compared using atomic absorption spectrometer. (author)

Certification of selected polynuclear aromatic hydrocarbons in standard reference material 1580, 'Organics in Shale Oil'. Final report

Energy Technology Data Exchange (ETDEWEB)

May, W.E.; Brown-Thomas, J.M.; Hilpert, L.R.; Wise, S.A.

1981-01-01

Two independent analytical methods were developed and used to certify the concentrations of five polynuclear aromatic hydrocarbons (PAH) in a shale oil sample (SRM 1580). In the sequential high-performance liquid chromatographic method, PAH are isolated from the matrix by chromatography on an aminosilane column. The individual analyte species were separated, identified, and quantified by chromatography on an octadecylsilane column with spectrofluorimetric detection. Dilution of the sample in methylene chloride was the only sample preparation step necessary prior to analysis by gas chromatography/mass spectrometry (GC/MS). The GC/MS determinations were performed using selected ion monitoring (SIM) and a standard addition technique for quantification. The polynuclear aromatic hydrocarbons of interest were separated on a 30 m SE-52 wall coated open tubular column interfaced to a quadrupole mass spectrometer through a 25 cm length of Pt/Ir tubing (0.15 mm i.d.). Excellent agreement was observed between the data obtained from these methods.

Correlations between chromatographic parameters and bioactivity predictors of potential herbicides.

Science.gov (United States)

Janicka, Małgorzata

2014-08-01

Different liquid chromatography techniques, including reversed-phase liquid chromatography on Purosphere RP-18e, IAM.PC.DD2 and Cosmosil Cholester columns and micellar liqud chromatography with a Purosphere RP-8e column and using buffered sodium dodecyl sulfate-acetonitrile as the mobile phase, were applied to study the lipophilic properties of 15 newly synthesized phenoxyacetic and carbamic acid derivatives, which are potential herbicides. Chromatographic lipophilicity descriptors were used to extrapolate log k parameters (log kw and log km) and log k values. Partitioning lipophilicity descriptors, i.e., log P coefficients in an n-octanol-water system, were computed from the molecular structures of the tested compounds. Bioactivity descriptors, including partition coefficients in a water-plant cuticle system and water-human serum albumin and coefficients for human skin partition and permeation were calculated in silico by ACD/ADME software using the linear solvation energy relationship of Abraham. Principal component analysis was applied to describe similarities between various chromatographic and partitioning lipophilicities. Highly significant, predictive linear relationships were found between chromatographic parameters and bioactivity descriptors. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Chromatographic analysis and purification of multiply tritium-labelled eicosanoids

International Nuclear Information System (INIS)

Shevchenko, V.P.; Nagaev, I.Yu.; Myasoedov, N.F.

1988-01-01

A comparative study of different chromatographic techniques (gas-liquid (GLC), thin-layer (TLC), liquid (LC), high-pressure liquid (HPLC) chromatography) is presented. They were applied to the analysis and preparative purification of tritium-labelled eicosanoids with a molar radioactivity of 1.8-8.8 TBq/mmol, obtained by selective hydrogenation and by chemical or enzymic methods. The possibility of analyzing reaction mixtures and isolating individual multiply labelled eicosanoids with a chemical and radiochemical purity of 95-98% was demonstrated. Special features of HPLC for high molar radioactivity eicosanoids are considered. (author) 9 refs.; 6 tabs

Liquid-chromatographic analysis for cyclosporine with use of a microbore column and small sample volume.

Science.gov (United States)

Annesley, T; Matz, K; Balogh, L; Clayton, L; Giacherio, D

1986-07-01

This liquid-chromatographic assay requires 0.2 to 0.5 mL of whole blood, avoids the use of diethyl ether, and consumes only 10 to 20% of the solvents used in prior methods. Sample preparation involves an acidic extraction with methyl-t-butyl ether, performed in a 13 X 100 mm disposable glass tube, then a short second extraction of the organic phase with sodium hydroxide. After evaporation of the methyl-t-butyl ether, chromatography is performed on an "Astec" 2.0-mm (i.d.) octyl column. We compared results by this procedure with those by use of earlier larger-scale extractions and their respective 4.6-mm (i.d.) columns; analytical recoveries of cyclosporins A and D were comparable with previous findings and results for patients' specimens were equivalent, but the microbore columns provided greatly increased resolution and sensitivity.

High-performance liquid chromatographic quantitation of desmosine plus isodesmosine in elastin and whole tissue hydrolysates

International Nuclear Information System (INIS)

Soskel, N.T.

1987-01-01

Quantitation of desmosine and isodesmosine, the major crosslinks in elastin, has been of interest because of their uniqueness and use as markers of that protein. Accurate measurement of these crosslinks may allow determination of elastin degradation in vivo and elastin content in tissues, obviating lengthy extraction procedures. We have developed a method of quantitating desmosine plus isodesmosine in hydrolysates of tissue and insoluble elastin using high-performance liquid chromatographic separation and absorbance detection that is rapid (21-35 min) and sensitive (accurate linearity from 100 pmol to 5 nmol). This method has been used to quantitate desmosines in elastin from bovine nuchal ligament and lung and in whole aorta from hamsters. The ability to completely separate [ 3 H]lysine from desmosine plus isodesmosine allows the method to be used to study incorporation of lysine into crosslinks in elastin

Ion-pair high performance liquid chromatographic retention behavior of salicylic acid and its derivatives

Energy Technology Data Exchange (ETDEWEB)

Lee, K.W.; Chung, Y.S. [Chungbuk National University, Cheongju (Korea); Oh, S.K. [Handok Pharmaceuticals Co. Ltd., Chungbuk (Korea)

1999-06-01

The ion-pair high performance liquid chromatographic elution behavior of salicylic acid and its derivatives was studied with measuring capacity factor, k', changing the concentration of ion-pairing reagent (tetrabutylammonium chloride, TBACl) in mobile phase. As a result, it was found that k' of the samples increase at pH 7.2 as the TBACl concentration increase. The derivatives of salicylic acid were separated each other at an optimum mobile phase condition which was found from the observation of the retention behavior. The optimum mobile phase condition was methanol solution(MeOH:H{sub 2}O 30:70) containing 20 mM TBACl for the determination of salicylic acid and methanol solution (MeOH:H{sub 2}O 20:80) containing 40 mM TBACl for p-aminosalicylic acid at pH 7.2. The method has been applied for the analysis of the contents of salicylic acid derivatives in an aspirin tablet and a tuberculosis curing agent. 8 refs., 4 figs., 2 tabs.

Determination of membrane degradation products in the product water of polymer electrolyte membrane fuel cells using liquid chromatography mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Zedda, Marco

2011-05-12

The predominant long term failure of polymer electrolyte membranes (PEM) is caused by hydroxyl radicals generated during fuel cell operation. These radicals attack the polymer, leading to chain scission, unzipping and consequently to membrane decomposition products. The present work has investigated decomposition products of novel sulfonated aromatic hydrocarbon membranes on the basis of a product water analysis. Degradation products from the investigated membrane type and the possibility to detect these compounds in the product water for diagnostic purposes have not been discovered yet. This thesis demonstrates the potential of solid phase extraction and liquid chromatography tandem mass spectrometry (SPE-LC-MS/MS) for the extraction, separation, characterization, identification and quantification of membrane degradation products in the product water of fuel cells. For this purpose, several polar aromatic hydrocarbons with different functional groups were selected as model compounds for the development of reliable extraction, separation and detection methods. The results of this thesis have shown that mixed mode sorbent materials with both weak anion exchange and reversed phase retention properties are well suited for reproducible extraction of both molecules and ions from the product water. The chromatographic separation of various polar aromatic hydrocarbons was achieved by means of phase optimized liquid chromatography using a solvent gradient and on a C18 stationary phase. Sensitive and selective detection of model compounds could be successfully demonstrated by the analysis of the product water using tandem mass spectrometry. The application of a hybrid mass spectrometer (Q Trap) for the characterization of unknown polar aromatic hydrocarbons has led to the identification and confirmation of 4-hydroxybenzoic acid in the product water. In addition, 4-HBA could be verified as a degradation product resulting from PEM decomposition by hydroxyl radicals using an

Process for treating hydrocarbons, etc

Energy Technology Data Exchange (ETDEWEB)

1933-09-15

A process is described for treating simultaneously bituminous substances and hydrocarbon oils for the production of low-boiling hydrocarbons and volatilization of the bituminous substances, characterized by the fact that it consists of heating a current of charge constituted by a mixture of the bituminous substances and hydrocarbon oils, to a high temperature, passing the heated current into a zone of extended reaction where the vapors are separated from the liquid or solid residue to favor transformation of the liquid hydrocarbons and volatilization of the bituminous substances, owing to the utilization of a heating agent carried to a high temperature being brought in contact with the heated charge in order to communicate its heat to the charge, while this later presents itself as relatively fine pellet or in the condition of distinct particles, particularly separated from one another.

Liquid chromatographic determination of seven antioxidants in dry food.

Science.gov (United States)

Page, B D; Charbonneau, C F

1989-01-01

The liquid chromatographic determinative step of the official method for propyl gallate, trihydroxybutyrophenone, tert-butylhydroquinone, nordihydroguaiaretic acid, butylated hydroxyanisole (BHA), 3,5-di-tert-butyl-4-hydroxymethylphenol, and butylated hydroxytoluene (BHT) in fats and oils has been applied to their determination in a number of dry foods. A representative sample (10 g) is homogenized first with hexane (25 mL), then with 5 mL added water, and finally with 75 mL added acetonitrile. The hexane and acetonitrile are decanted, filtered, and separated; the hexane and rehydrated food are reextracted with 2 additional portions of acetonitrile, and the combined acetonitrile extracts are concentrated and diluted to 10 mL. An aliquot is analyzed as described in the official method, using a 150 x 4.6 mm 5 microns C-18 column. The need for rehydration to maximize the recovery of BHA and other antioxidants from marketplace dry food samples such as potato flakes, dry coffee whiteners, and dessert topping mixes was demonstrated. Rehydration was not required for cheese snacks, breakfast cereals, cake mixes, and some other foods. The need for rehydration should be determined by analyzing other foods with and without the addition of water. Potato and corn chips, popcorn and cheese snacks, breakfast cereals, dry beverage mixes, rice, potato flakes, french fried potatoes, and cake mixes were spiked with the above antioxidants at 10-50 ppm. Overall recoveries ranged from 64.3 to 105.6% and repeatabilities ranged from 0.7 to 10.8%. A total of 109 samples of the above foods were analyzed, and 64% contained detectable (greater than 1-2 ppm) antioxidants, mainly BHA and BHT.

Quantification of 16 polycyclic aromatic hydrocarbons in cigarette smoke condensate using stable isotope dilution liquid chromatography with atmospheric-pressure photoionization tandem mass spectrometry.

Science.gov (United States)

Zhang, Xiaotao; Hou, Hongwei; Chen, Huan; Liu, Yong; Wang, An; Hu, Qingyuan

2015-09-17

A stable isotope dilution liquid chromatography with tandem mass spectrometry method for the analysis of 16 polycyclic aromatic hydrocarbons in cigarette smoke condensate was developed and validated. Compared with previously reported methods, this method has lower limits of detection (0.04-1.35 ng/cig). Additionally, the proposed method saves time, reduces the number of separation steps, and reduces the quantity of solvent needed. The new method was applied to evaluate polycyclic aromatic hydrocarbon content in 213 commercially available cigarettes in China, under the International Standardization Organization smoking regime and the Health Canadian intense smoking regime. The results showed that the total polycyclic aromatic hydrocarbon content was more than two times higher in samples from the Health Canadian intense smoking regime than in samples from the International Standardization Organization smoking regime (1189.23 vs. 2859.50 ng/cig, ppolycyclic aromatic hydrocarbons (and total polycyclic aromatic hydrocarbons) increased with labeled tar content in both of the tested smoking regimes. There was a positive correlation between total polycyclic aromatic hydrocarbons under the International Standardization Organization smoking regime with that under the Health Canadian intense smoking regime. The proposed liquid chromatography with tandem mass spectrometry method is satisfactory for the rapid, sensitive, and accurately quantitative evaluation of polycyclic aromatic hydrocarbon content in cigarette smoke condensate, and it can be applied to assess potential health risks from smoking. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

Evaluation of the performance and response of the bacharach TLV sniffer and H-Nu photoionization gas analyzer to common hydrocarbon solvents.

Science.gov (United States)

Chelton, C F; Zakraysek, N; Lautner, G M; Confer, R G

1983-10-01

Two direct reading instruments, the H-Nu PI 101 photoionization analyzer and the J.W. Bacharach TLV Sniffer, were evaluated under laboratory conditions to determine their performance characteristics when challenged by vapors of common hydrocarbon solvent mixtures. Each instrument was evaluated against the manufacturer's recommended test solvent for rise time, fall time, noise, span drift, zero drift, position sensitivity, battery life, and recharge time. The precision, accuracy, and operating linear range were also determined for the test solvents and some petroleum solvent mixtures which are common refinery products. For these latter mixtures, correction factors are presented which allow for an improved estimate of ambient concentrations when monitoring with each of these instruments. All tests except operating humidity range were performed by challenging each instrument with a known concentration of hydrocarbon generated by evaporating calculated liquid volumes into a static chamber. Humidity tests were performed using a dynamic dilution apparatus generating a fixed concentration of hydrocarbon while relative humidity was varied. Concentrations in both systems were verified by gas injection into gas chromatograph. Each instrument performed well when challenged by manufacturers' recommended test solvents. Humidity was shown to influence each instrument's readings. Also, the instruments were shown to have application as monitors of airborne concentrations of common hydrocarbon solvent mixtures.

Impurity analysis in EC-99mTC radiotracer using chromatographic techniques

International Nuclear Information System (INIS)

Almeida, E.V.; Fukumori, N.T.O.; Mengatti, J.; Silva, C.P.G.; Matsuda, M.M.N.

2008-01-01

The objective of this study was to develop two chromatographic methods of impurity analysis in radiotracer 99m Tc-EC: the Thin Layer Chromatography (TLC) and the High Performance Liquid Chromatography Reversed Phase (HPLC-RP)

Liquid Chromatographic-Chemometric Techniques for the Simultaneous HPLC Determination of Lansoprazole, Amoxicillin and Clarithromycin in Commercial Preparation.

Science.gov (United States)

Aktas, A Hakan; Saridag, Ayse Mine

2017-09-01

Two multivariate calibration-prediction techniques, principal component regression (PCR) and partial least-squares regression (PLSR) were applied to the chromatographic multicomponent analysis of the drug containing lansoprazole (LAN), clarithromycin (CLA) and amoxicillin (AMO). Optimum chromatographic separation of LAN, CLA and AMO with atorvastatin as the internal standard (IS) was obtained by using Xterra® RP18 column 5 μm 4.6 × 250 mm2, and 25 mM ammonium chloride buffer prepared ammonium chloride, acetonitrile and bidistilled water (45:45:10 v/v) as the mobile phase at flow rate 1.0 mL/min. The high pressure liquid chromatography data sets consisting of the ratios of analyte peak areas to the IS peak area were obtained by using diode array detector detection at five wavelengths (205, 210, 215, 220 and 225 nm). LC-chemometric calibration for LAN, CLA and AMO were separately constructed by using the relationship between the peak-area ratio and training sets for each analyte. A series of synthetic solutions containing different concentrations of LAN, CLA and AMO were used to check the prediction ability of the PCR and PLS. Both of the two-chemometric methods in this study can be satisfactorily used for the quantitative analysis and for dissolutions tests of multicomponent commercial drug. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Liquid chromatographic method for determining the concentration of bisazir in water

Science.gov (United States)

Scholefield, Ronald J.; Slaght, Karen S.; Allen, John L.

1997-01-01

Barrier dams, traps, and lampricides are the techniques currently used by the Great Lakes Fishery Commission to control sea lampreys (Petromyzon marinus) in the Great Lakes. To augment these control techniques, a sterile-male-release research program was initiated at the Lake Huron Biological Station. Male sea lampreys were sterilized by intraperitoneal injection of the chemical sterilant P,P-bis(1-aziridinyl)-N-methylphosphinothioic amide (bisazir). An analytical method was needed to quantitate the concentration of bisazir in water and to routinely verify that bisazir (>25 μg/L) does not persist in the treated effluent discharged from the sterilization facility to Lake Huron. A rapid, accurate, and sensitive liquid chromatographic (LC) method was developed for determining bisazir in water. Bisazir was dissolved in Lake Huron water; extracted and concentrated on a C18 solid-phase extraction column; eluted with methanol; and quantitated by reversed-phase LC using a C18 column, a mobile phase of 70% water and 30% methanol (v/v), and UV detection (205 nm). Bisazir retention time was 7-8 min; total run time was about 20 min. Method detection limit for bisazir dissolved in Lake Huron water was about 15 μg/L. Recovery from Lake Huron water fortified with bisazir at 100 μg/L was 94% (95% confidence interval, 90.2-98.2%).

Development and Validation of Liquid Chromatographic Method for Estimation of Naringin in Nanoformulation

Directory of Open Access Journals (Sweden)

Kranti P. Musmade

2014-01-01

Full Text Available A simple, precise, accurate, rapid, and sensitive reverse phase high performance liquid chromatography (RP-HPLC method with UV detection has been developed and validated for quantification of naringin (NAR in novel pharmaceutical formulation. NAR is a polyphenolic flavonoid present in most of the citrus plants having variety of pharmacological activities. Method optimization was carried out by considering the various parameters such as effect of pH and column. The analyte was separated by employing a C18 (250.0 × 4.6 mm, 5 μm column at ambient temperature in isocratic conditions using phosphate buffer pH 3.5: acetonitrile (75 : 25% v/v as mobile phase pumped at a flow rate of 1.0 mL/min. UV detection was carried out at 282 nm. The developed method was validated according to ICH guidelines Q2(R1. The method was found to be precise and accurate on statistical evaluation with a linearity range of 0.1 to 20.0 μg/mL for NAR. The intra- and interday precision studies showed good reproducibility with coefficients of variation (CV less than 1.0%. The mean recovery of NAR was found to be 99.33 ± 0.16%. The proposed method was found to be highly accurate, sensitive, and robust. The proposed liquid chromatographic method was successfully employed for the routine analysis of said compound in developed novel nanopharmaceuticals. The presence of excipients did not show any interference on the determination of NAR, indicating method specificity.

Geochemical assessment of light gaseous hydrocarbons in near-surface soils of Kutch-Saurashtra: Implication for hydrocarbon prospects

Science.gov (United States)

Rao, P. Lakshmi Srinivasa; Madhavi, T.; Srinu, D.; Kalpana, M. S.; Patil, D. J.; Dayal, A. M.

2013-02-01

Light hydrocarbons in soil have been used as direct indicators in geochemical hydrocarbon exploration, which remains an unconventional path in the petroleum industry. The occurrence of adsorbed soil gases, methane and heavier homologues were recorded in the near-surface soil samples collected from Kutch-Saurashtra, India. Soil gas alkanes were interpreted to be derived from deep-seated hydrocarbon sources and have migrated to the surface through structural discontinuities. The source of hydrocarbons is assessed to be thermogenic and could have been primarily derived from humic organic matter with partial contribution from sapropelic matter. Gas chromatographic analyses of hydrocarbons desorbed from soil samples through acid extraction technique showed the presence of methane through n-butane and the observed concentrations (in ppb) vary from: methane (C1) from 4-291, ethane (C2) from 0-84, propane (C3) from 0-37, i-butane (iC4) from 0-5 and n-butane (nC4) from 0-4. Carbon isotopes measured for methane and ethane by GC-C-IRMS, range between -42.9‰ to -13.3‰ (Pee Dee Belemnite - PDB) and -21.2‰ to -12.4‰ (PDB), respectively. The increased occurrence of hydrocarbons in the areas near Anjar of Kutch and the area south to Rajkot of Saurashtra signifies the area potential for oil and gas.

Radioactivity monitor for high-performance liquid chromatography

International Nuclear Information System (INIS)

Reeve, D.R.; Crozier, A.

1977-01-01

The coupling of a homogeneous radioactivity monitor to a liquid chromatograph involves compromises between the sensitivity of the monitor and the resolution and speed of analysis of the chromatograph. The theoretical relationships between these parameters are considered and expressions derived which make it possible to calculate suitable monitor operating conditions for most types of high-performance liquid chromatography

Total hydrocarbon content (THC) testing in liquid oxygen (LOX) systems

Science.gov (United States)

Meneghelli, B. J.; Obregon, R. E.; Ross, H. R.; Hebert, B. J.; Sass, J. P.; Dirschka, G. E.

2015-12-01

The measured Total Hydrocarbon Content (THC) levels in liquid oxygen (LOX) systems at Stennis Space Center (SSC) have shown wide variations. Examples of these variations include the following: 1) differences between vendor-supplied THC values and those obtained using standard SSC analysis procedures; and 2) increasing THC values over time at an active SSC test stand in both storage and run vessels. A detailed analysis of LOX sampling techniques, analytical instrumentation, and sampling procedures will be presented. Additional data obtained on LOX system operations and LOX delivery trailer THC values during the past 12-24 months will also be discussed. Field test results showing THC levels and the distribution of the THC's in the test stand run tank, modified for THC analysis via dip tubes, will be presented.

General and selective isolation procedure for high-performance liquid chromatographic determination of anabolic steroids in tissues.

Science.gov (United States)

Laganà, A; Marino, A

1991-12-27

A multi-residue method has been developed for the determination of anabolic steroids in animal tissue. The analytes are extracted from tissue with methanol and the extract is subjected to two solid-phase extractions, one using a non-specific adsorbing material, such as graphitized carbon black (Carbopack B), and the other Amberlite CG-400 I in the OH form. This procedure allowed the neutral anabolics (testosterone, trenbolone and progesterone) to be isolated and separated from the acidic type (phenolic group), such as diethylstilbestrol, oestradiol, zeranol/zearalenone and their respective metabolites. The determination was effected using high-performance liquid chromatography with different detectors (ultraviolet, fluorimetric and electrochemical). Several analytical parameters were studied: chromatographic conditions, recoveries, evaporation step, solvent flow-rate, cartridges reusability, interference of plastic cartridges. For all the anabolics investigated the recoveries were greater than 83.6%.

[Simultaneous analysis of aromatic aldehydes and coumarins with high pressure liquid chromatography. Application to wines and brandies stored in oak barrels].

Science.gov (United States)

Salagoity-Auguste, M H; Tricard, C; Sudraud, P

1987-04-17

Aromatic aldehydes (vanillin, syringaldehyde, coniferaldehyde and sinapaldehyde) and coumarins (esculetin, umbelliferone, scopoletin and methylumbelliferone) are natural wood compounds. Storage of wines and brandies in oak barrels increases notably aldehydes and coumarins (particularly scopoletin) concentrations. These compounds were separated by high-performance liquid chromatography, on hydrocarbon bonded reversed-phase packings, with a water-acetonitrile elution gradient. They were first extracted from wines and brandies by diethyl ether and then injected on chromatographic column. A double detection was used to determine simultaneously aromatic aldehydes and coumarins by UV absorption and fluorescence respectively.

Determination of the isotope distribution in 14C-labelled hydrocarbons by thermal fragmentation

International Nuclear Information System (INIS)

Kopinke, F.D.; Dermietzel, J.; Jockisch, W.; Raeuber, G.

1986-01-01

The gas chromatographic analysis of pyrolysis products of properly labelled hydrocarbons allows a definite and quantitative determination of the 14 C-distribution in those compounds. For this purpose a simple, fast, and versatilely applicable method has been developed and described

Imaging fluid/solid interactions in hydrocarbon reservoir rocks.

Science.gov (United States)

Uwins, P J; Baker, J C; Mackinnon, I D

1993-08-01

The environmental scanning electron microscope (ESEM) has been used to image liquid hydrocarbons in sandstones and oil shales. Additionally, the fluid sensitivity of selected clay minerals in hydrocarbon reservoirs was assessed via three case studies: HCl acid sensitivity of authigenic chlorite in sandstone reservoirs, freshwater sensitivity of authigenic illite/smectite in sandstone reservoirs, and bleach sensitivity of a volcanic reservoir containing abundant secondary chlorite/corrensite. The results showed the suitability of using ESEM for imaging liquid hydrocarbon films in hydrocarbon reservoirs and the importance of simulating in situ fluid-rock interactions for hydrocarbon production programmes. In each case, results of the ESEM studies greatly enhanced prediction of reservoir/borehole reactions and, in some cases, contradicted conventional wisdom regarding the outcome of potential engineering solutions.

Polycyclic aromatic hydrocarbons residues in Gentile di maiale, a smoked meat product typical of some mountain areas in Latina province (Central Italy

Directory of Open Access Journals (Sweden)

Giuseppe Carrabs

2014-05-01

Full Text Available Gentile di maiale is a typical meat product prepared in some traditional plants of Latina Province (Central Italy. It is obtained from dehydration, salting, smoking and ripening of swine rectum. Aim of this study was to evaluate the influence of the traditional smoking process on polycyclic aromatic hydrocarbons (PAHs content by means of high-performance liquid chromatographic/fluorescence detection. Polycyclic aromatic hydrocarbons detected in 8 samples of raw material (swine rectum and samples of smoked gentile were: benzo[a]anthracene, chrisene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a] pyrene, benzo[a,h]anthracene. Their residues were detected in all samples of finished product. European Regulation 835/2011 established two levels of PAHs content in meat products. According to first levels, in force until September 2014, only 2 out of 8 samples exceeded legal limit. According to the subsequent, more restrictive, limits all samples would be non-compliant. An improvement and a standardisation of traditional smoking procedures are recommended.

Detection of monohydroxylated polycyclic aromatic hydrocarbons in urine and particulate matter using LC separations coupled with integrated SPE and fluorescence detection or coupled with high-resolution time-of-flight mass spectrometry.

Science.gov (United States)

Lintelmann, Jutta; Wu, Xiao; Kuhn, Evelyn; Ritter, Sebastian; Schmidt, Claudia; Zimmermann, Ralf

2018-05-01

A high-performance liquid chromatographic (HPLC) method with integrated solid-phase extraction for the determination of 1-hydroxypyrene and 1-, 2-, 3-, 4- and 9-hydroxyphenanthrene in urine was developed and validated. After enzymatic treatment and centrifugation of 500 μL urine, 100 μL of the sample was directly injected into the HPLC system. Integrated solid-phase extraction was performed on a selective, copper phthalocyanine modified packing material. Subsequent chromatographic separation was achieved on a pentafluorophenyl core-shell column using a methanol gradient. For quantification, time-programmed fluorescence detection was used. Matrix-dependent recoveries were between 94.8 and 102.4%, repeatability and reproducibility ranged from 2.2 to 17.9% and detection limits lay between 2.6 and 13.6 ng/L urine. A set of 16 samples from normally exposed adults was analyzed using this HPLC-fluorescence detection method. Results were comparable with those reported in other studies. The chromatographic separation of the method was transferred to an ultra-high-performance liquid chromatography pentafluorophenyl core-shell column and coupled to a high-resolution time-of-flight mass spectrometer (HR-TOF-MS). The resulting method was used to demonstrate the applicability of LC-HR-TOF-MS for simultaneous target and suspect screening of monohydroxylated polycyclic aromatic hydrocarbons in extracts of urine and particulate matter. Copyright © 2018 John Wiley & Sons, Ltd.

Preparation, characterization and application of a reversed phase liquid chromatography/hydrophilic interaction chromatography mixed-mode C18-DTT stationary phase.

Science.gov (United States)

Wang, Qing; Long, Yao; Yao, Lin; Xu, Li; Shi, Zhi-Guo; Xu, Lanying

2016-01-01

A mixed-mode chromatographic stationary phase, C18-DTT (dithiothreitol) silica (SiO2) was prepared through "thiol-ene" click chemistry. The obtained material was characterized by fourier transform infrared spectroscope, nitrogen adsorption analysis and contact angle analysis. Chromatographic performance of the C18-DTT was systemically evaluated by studying the effect of acetonitrile content, pH, buffer concentration of the mobile phase and column temperature. It was demonstrated that the novel stationary phase possessed reversed phase liquid chromatography (RPLC)/hydrophilic interaction liquid chromatography (HILIC) mixed-mode property. The stop-flow test revealed that C18-DTT exhibited excellent compatibility with 100% aqueous mobile phase. Additionally, the stability and column-to-column reproducibility of the C18-DTT material were satisfactory, with relative standard deviations of retention factor of the tested analytes (verapamil, fenbufen, guanine, tetrandrine and nicotinic acid) in the range of 1.82-3.72% and 0.85-1.93%, respectively. Finally, the application of C18-DTT column was demonstrated in the separation of non-steroidal anti-inflammatory drugs, aromatic carboxylic acids, alkaloids, nucleo-analytes and polycyclic aromatic hydrocarbons. It had great resolving power in the analysis of various compounds in HILIC and RPLC chromatographic conditions and was a promising RPLC/HILIC mixed-mode stationary phase. Copyright © 2015 Elsevier B.V. All rights reserved.

Production of light hydrocarbons, etc. [from heavy hydrocarbons

Energy Technology Data Exchange (ETDEWEB)

1937-10-07

A process is given for the production of light hydrocarbons of the gasoline type and, if desired, of the middle-oil type, from liquid or fusible heavy or medium heavy hydrocarbon materials. The process comprises subjecting the said initial materials in the first stage to catalytic hydrofining, separating the lower boiling constituents and the hydrogenating gas from the resulting products and then subjecting the higher boiling constituents in a second stage to a splitting destructive hydrogenation and then recycling substantially the entire reaction mixture obtained in the second stage to the frst stage.

Hydrocarbon-degrading bacteria isolation and surfactant influence ...

African Journals Online (AJOL)

Hydrocarbons are substantially insoluble in water, often remaining partitioned in the non-aqueous phase liquid (NAPL). However, there had been little or no attempts to advance the bioavailability of hydrocarbons through the use of surfactants. This study was conducted based on the need to isolate hydrocarbon degrading ...

Gas chromatographic determination of polycyclic aromatic hydrocarbons in water and smoked rice samples after solid-phase microextraction using multiwalled carbon nanotube loaded hollow fiber.

Science.gov (United States)

Matin, Amir Abbas; Biparva, Pourya; Gheshlaghi, Mohammad

2014-12-29

A novel solid-phase microextraction fiber was prepared based on multiwalled carbon nanotubes (MWCNTs) loaded on hollow fiber membrane pores. Stainless steel wire was used as unbreakable support. The major advantages of the proposed fiber are its (a) high reproducibility due to the uniform structure of the hollow fiber membranes, (b) high extraction capacity related to the porous structure of the hollow fiber and outstanding adsorptive characteristics of MWCNTs. The proposed fiber was applied for the microextraction of five representative polycyclic aromatic hydrocarbons (PAHs) from aqueous media (river and hubble-bubble water) and smoked rice samples followed by gas chromatographic determination. Analytical merits of the method, including high correlation coefficients [(0.9963-0.9992) and (0.9982-0.9999)] and low detection limits [(9.0-13.0ngL(-1)) and (40.0-150.0ngkg(-1))] for water and rice samples, respectively, made the proposed method suitable for the ultra-trace determination of PAHs. Copyright © 2014 Elsevier B.V. All rights reserved.

Characterizing the selectivity of stationary phases and organic modifiers in reversed-phase high-performance liquid chromatographic systems by a general solvation equation using gradient elution.

Science.gov (United States)

Du, C M; Valko, K; Bevan, C; Reynolds, D; Abraham, M H

2000-11-01

Retention data for a set of 69 compounds using rapid gradient elution are obtained on a wide range of reversed-phase stationary phases and organic modifiers. The chromatographic stationary phases studied are Inertsil (IN)-ODS, pentafluorophenyl, fluoro-octyl, n-propylcyano, Polymer (PLRP-S 100), and hexylphenyl. The organic solvent modifiers are 2,2,2-trifluoroethanol (TFE); 1,1,1,3,3,3-hexafluoropropan-2-ol (HFIP); isopropanol; methanol (MeOH); acetonitrile (AcN); tetrahydrofuran; 1,4-dioxane; N,N-dimethylformamide; and mixed solvents of dimethylsulfoxide (DMSO) with AcN and DMSO with MeOH (1:1). A total of 25 chromatographic systems are analyzed using a solvation equation. In general, most of the systems give reasonable statistics. The selectivity of the reversed phase-high-performance liquid chromatographic (HPLC) systems with respect to the solute's dipolarity-polarity, hydrogen-bond acidity, and basicity are reflected in correspondingly large coefficients in the solvation equation. We wanted to find the most orthogonal HPLC systems, showing the highest possible selectivity difference in order to derive molecular descriptors using the gradient retention times of a compound. We selected eight chromatographic systems that have a large range of coefficients of interest (s, a, and b) similar to those found in water-solvent partitions used previously to derive molecular descriptors. The systems selected are IN-ODS phases with AcN, MeOH, TFE, and HFIP as mobile phase, PLRP-S 100 phase with AcN, propylcyano phase with AcN and MeOH, and fluorooctyl phase with TFE. Using the retention data obtained for a compound in the selected chromatographic systems, we can estimate the molecular descriptors with the faster and simpler gradient elution method.

Study and ICH validation of a reverse-phase liquid chromatographic method for the quantification of the intact monoclonal antibody cetuximab

Directory of Open Access Journals (Sweden)

Antonio Martínez-Ortega

2016-04-01

Full Text Available Cetuximab (CTX is a potent chimeric mouse/human monoclonal antibody (mAb approved worldwide for treatment of metastatic colorectal cancer. Among the various biological and physical analyses performed for full study on this biopharmaceutic, the determination of the concentration preparations throughout manufacturing and subsequent handling in hospital is particularly relevant. In the present work, the study and validation of a method for quantifying intact CTX by reverse-phase high-performance liquid chromatography with diode array detection ((RPHPLC/DAD is presented. With that end, we checked the performance of a chromatographic method for quantifying CTX and conducted a study to validate the method as stability-indicating in accordance with the International Conference on Harmonization guidelines (ICH for biotechnological drugs; therefore, we evaluated linearity, accuracy, precision, detection and quantification limits, robustness and system suitability. The specificity of the method and the robustness of the mAb formulation against external stress factors were estimated by comprehensive chromatographic analysis by subjecting CTX to several informative stress conditions. As demonstrated, the method is rapid, accurate, and reproducible for CTX quantification. It was also successfully used to quantify CTX in a long-term stability study performed under hospital conditions.

Method for chromatographically recovering scandium and yttrium

International Nuclear Information System (INIS)

Snyder, T.S.; Stoltz, R.A.

1991-01-01

This paper describes a method for chromatographically recovering scandium and yttrium from the residue of a sand chlorinator. It comprises: providing a residue from a sand chlorinator, the residue containing scandium, yttrium, sodium, calcium and at least one radioactive metal of the group consisting of radium, thorium and uranium; digesting the residue with an acid to produce an aqueous liquid containing scandium, yttrium, sodium, calcium and at least one radioactive metal of the group consisting of radium, thorium and uranium; feeding the metal containing liquid through a cation exchanger; eluding the cation exchanger with an acid eluant to to produce: a first eluate containing at least half of the total weight of the calcium and sodium in the feed liquid; a second eluate containing at least half of the total weight of the one or more radioactive metals in the feed liquid; a third eluate containing at least half of the yttrium in the feed liquid, and a fourth eluate containing at least half of the weight of the scandium in the feed liquid

New liquid chromatographic-chemometric approach for the determination of sunset yellow and tartrazine in commercial preparation.

Science.gov (United States)

Dinç, Erdal; Aktaş, A Hakan; Ustündağ, Ozgür

2005-01-01

A new liquid chromatographic (LC)-chemometric approach was developed for the determination of sunset yellow (SUN) and tartrazine (TAR) in commercial preparations. This approach uses LC and chemometric calibration methods, i.e., classical least-squares (CLS), principal component regression (PCR), and partial-least squares (PLS), simultaneously. The combined LC-chemometric approaches, denoted as LC-CLS, LC-PCR, and LC-PLS, are based on photodiode array (PDA) detection at multiple wavelengths. Optimum chromatographic separation of SUN and TAR with allura red as the internal standard (IS) was obtained by using a Waters Symmetry C18 column, 5 microm, 4.6 x 250 mm, and 0.2 M acetate buffer (pH 5)-acetonitrile-methano-bidistilled water (55 + 20 + 15 + 10, v/v) as the mobile phase at a flow rate of 1.9 mL/min. The LC data sets consisting of the ratios of analyte peak areas to the IS peak area were obtained by using PDA detection at 5 wavelengths (465, 470, 475, 480, and 485 nm). LC-chemometric calibrations for SUN and TAR were separately constructed by using the relationship between the peak-area ratio and the training sets for each colorant. LC-chemometric approaches were tested for different synthetic mixtures containing SUN and TAR in the presence of the IS. These LC-chemometric calibrations were applied to a commercial preparation of the 2 colorants. The experimental results of the LC-chemometric approaches were compared with those obtained by a developed classical LC method using single-wavelength detection.

Ion chromatographic determination of Di-n-butyl phosphate in degraded organic solvent

International Nuclear Information System (INIS)

Velavendan, P.; Pandey, N.K.; Kamachi Mudali, U.; Natarajan, R.

2011-01-01

In the present work a method for the determination of Di-n-butyl phosphate in organic streams using Ion Chromatography technique is developed and described here. The method involves the separation of Di-n-butyl phosphate (DBP) from 30% TBP-NPH (Tri-n-butylphosphate diluted in Normal Paraffin Hydrocarbon) and uranium/nitric acid matrix by an extraction of DBP in alkaline medium and subsequent ion-exchange separation in ion chromatography column followed by suppressed conductivity detection. Direct determination of DBP in lean/loaded organic solvent will lead to in accurate determination of DBP due to organic interference. DBP is quantified to lower limit of 1 ppm with 3% RSD. The results obtained with ion chromatographic technique are compared with those obtained by standard gas chromatographic technique. The developed method is much faster and total analysis can be completed within two hours. (author)

Column Liquid Chromatography.

Science.gov (United States)

Majors, Ronald E.; And Others

1984-01-01

Reviews literature covering developments of column liquid chromatography during 1982-83. Areas considered include: books and reviews; general theory; columns; instrumentation; detectors; automation and data handling; multidimensional chromatographic and column switching techniques; liquid-solid chromatography; normal bonded-phase, reversed-phase,…

Ballistic Evaporation and Solvation of Helium Atoms at the Surfaces of Protic and Hydrocarbon Liquids.

Science.gov (United States)

Johnson, Alexis M; Lancaster, Diane K; Faust, Jennifer A; Hahn, Christine; Reznickova, Anna; Nathanson, Gilbert M

2014-11-06

Atomic and molecular solutes evaporate and dissolve by traversing an atomically thin boundary separating liquid and gas. Most solutes spend only short times in this interfacial region, making them difficult to observe. Experiments that monitor the velocities of evaporating species, however, can capture their final interactions with surface solvent molecules. We find that polarizable gases such as N2 and Ar evaporate from protic and hydrocarbon liquids with Maxwell-Boltzmann speed distributions. Surprisingly, the weakly interacting helium atom emerges from these liquids at high kinetic energies, exceeding the expected energy of evaporation from salty water by 70%. This super-Maxwellian evaporation implies in reverse that He atoms preferentially dissolve when they strike the surface at high energies, as if ballistically penetrating into the solvent. The evaporation energies increase with solvent surface tension, suggesting that He atoms require extra kinetic energy to navigate increasingly tortuous paths between surface molecules.

Determination of polynuclear hydrocarbons

Energy Technology Data Exchange (ETDEWEB)

Lodge, Jr, J P

1963-01-01

At the present time, the method of choice for the determination of polynuclear hydrocarbons appears to be the following, (a) extraction of the benzene-soluble fraction from the gross collected particulate matter, (b) one pass through a chromatographic column of partially deactivated alumina, (c) spectral examination of the fractions and (d) the application of appropriate chemical tests as indicated by the previous step. Using this method, the presence of pyrene, fluoranthene, one of the benzofluorenes, chrysens, benz(a)anthracene, benzo(a)pyrene, benzo(e)pyrene, benzo(k)fluoranthene, anthanthrene, and coronene was demonstrated in the air of numerous American cities, and benzo(a)pyrene was measured at some 130 sites. Invaluable as such accurate determinations may be for research purposes, they are still too costly and time-consuming for routine survey purposes. While studies on the subject are by no means complete, they indicate the validity of piperonal chloride test as a general index of polycyclic hydrocarbons. This procedure is described in this paper. 7 references.

Binary liquid-liquid equilibria of aniline-paraffin and furfural-paraffin systems

Energy Technology Data Exchange (ETDEWEB)

Sen, S.C.; Maity, S.; Ganguli, K.; Ray, P. (Calcutta Univ., (India))

1991-12-01

Liquid-liquid-equilibria (L-L-E) of hydrocarbon containing systems are of considerable commercial importance to refineries. But prediction of L-L-E of such systems is extremely difficult owing to the complex nature of the petroleum fluids. For treating such complex mixtures, a continuous component method is appropriate and for representing such liquids, a group contribution model like the UNIFAC is extremely convenient. It is, however, necessary to determine the appropriate group interaction parameters, and also to test the applicability of the UNIFAC method to these cases. Binary liquid-liquid-equilibria data for several aniline-paraffin and furfural-paraffin systems have been taken. These data along with data for other aniline-hydrocarbon and furfural-hydrocarbon systems from literature have been correlated using the UNIFAC model. The UNIFAC group interaction parameters have been found to have a linear temperature dependence. The CH{sub 2} groups in cyclo and non-cyclo paraffins require different interaction parameters. It was also found that a scaling of the combinatorial term is necessary for higher molecular weight hydrocarbons. 13 refs., 12 figs., 5 tabs.

Polycyclic Aromatic Hydrocarbons in Fine Particulate Matter Emitted from Burning Kerosene, Liquid Petroleum Gas, and Wood Fuels in Household Cookstoves

Science.gov (United States)

This study measured polycyclic aromatic hydrocarbon (PAH) composition in particulate matter emissions from residential cookstoves. A variety of fuel and cookstove combinations were examined, including: (i) liquid petroleum gas (LPG), (ii) kerosene in a wick stove, (iii) wood (10%...

Converting of oil shale and biomass into liquid hydrocarbons via pyrolysis

International Nuclear Information System (INIS)

Kılıç, Murat; Pütün, Ayşe Eren; Uzun, Başak Burcu; Pütün, Ersan

2014-01-01

Highlights: • Co-processing of oil shale with an arid land biomass for hydrocarbon production. • Co-pyrolysis in TGA and fixed-bed reactor. • Characterization of oil and char. - Abstract: In this study, co-pyrolytic behaviors of oil shale and Euphorbia rigida were investigated at different temperatures in a fixed bed reactor at 450, 500, and 550 °C with a heating rate of 10 °C/min in the presence of nitrogen atmosphere. The obtained solid product (char) and liquid product (tar) were analyzed by using different types of characterization techniques. Experimental results showed co-pyrolysis of oil shale and biomass could be an environmental friendly way for the transformation of these precursors into valuable products such as chemicals or fuels

High-performance Liquid Chromatographic Ultraviolet Detection of Nilotinib in Human Plasma from Patients with Chronic Myelogenous Leukemia, and Comparison with Liquid Chromatography-Tandem Mass Spectrometry.

Science.gov (United States)

Nakahara, Ryosuke; Satho, Yuhki; Itoh, Hiroki

2016-11-01

A method for determining nilotinib concentration in human plasma is proposed using high-performance liquid chromatography and ultraviolet detection. Nilotinib and the internal standard dasatinib were separated using a mobile phase of 0.5% Na 2 PO 4 H 2 O (pH 2.5)-acetonitrile-methanol (55:25:20, v/v/v) on a Capcell Pak C18 MG II column (250 × 4.6 mm) at a flow rate of 1.0 ml/min, and ultraviolet measurement at 250 nm. The calibration curve exhibited linearity over the nilotinib concentration range of 50-2,500 ng/ml at 250 nm, with relative standard deviations (n = 5) of 7.1%, 2.5%, and 2.9% for 250, 1,500, and 2,500 ng/ml, respectively. The detection limit for nilotinib was 5 ng/ml due to three blank determinations (ρ = 3). This method was successfully applied to assaying nilotinib in human plasma samples from patients with chronic myelogenous leukemia. In addition, we compared the results with those measured by liquid chromatography-tandem mass spectrometry (LC-MS/MS) at BML, Inc. (a commercial laboratory). A strong correlation was observed between the nilotinib concentrations measured by our high-performance liquid chromatographic method and those obtained by LC/MS-MS (r 2 = 0.988, P < 0.01). © 2016 Wiley Periodicals, Inc.

Magnetic ionic liquids as non-conventional extraction solvents for the determination of polycyclic aromatic hydrocarbons.

Science.gov (United States)

Trujillo-Rodríguez, María J; Nacham, Omprakash; Clark, Kevin D; Pino, Verónica; Anderson, Jared L; Ayala, Juan H; Afonso, Ana M

2016-08-31

This work describes the applicability of magnetic ionic liquids (MILs) in the analytical determination of a group of heavy polycyclic aromatic hydrocarbons. Three different MILs, namely, benzyltrioctylammonium bromotrichloroferrate (III) (MIL A), methoxybenzyltrioctylammonium bromotrichloroferrate (III) (MIL B), and 1,12-di(3-benzylbenzimidazolium) dodecane bis[(trifluoromethyl)sulfonyl)]imide bromotrichloroferrate (III) (MIL C), were designed to exhibit hydrophobic properties, and their performance examined in a microextraction method for hydrophobic analytes. The magnet-assisted approach with these MILs was performed in combination with high performance liquid chromatography and fluorescence detection. The study of the extraction performance showed that MIL A was the most suitable solvent for the extraction of polycyclic aromatic hydrocarbons and under optimum conditions the fast extraction step required ∼20 μL of MIL A for 10 mL of aqueous sample, 24 mmol L(-1) NaOH, high ionic strength content of NaCl (25% (w/v)), 500 μL of acetone as dispersive solvent, and 5 min of vortex. The desorption step required the aid of an external magnetic field with a strong NdFeB magnet (the separation requires few seconds), two back-extraction steps for polycyclic aromatic hydrocarbons retained in the MIL droplet with n-hexane, evaporation and reconstitution with acetonitrile. The overall method presented limits of detection down to 5 ng L(-1), relative recoveries ranging from 91.5 to 119%, and inter-day reproducibility values (expressed as relative standard derivation) lower than 16.4% for a spiked level of 0.4 μg L(-1) (n = 9). The method was also applied for the analysis of real samples, including tap water, wastewater, and tea infusion. Copyright © 2016 Elsevier B.V. All rights reserved.

Ionic Liquid-Liquid Chromatography: A New General Purpose Separation Methodology

OpenAIRE

Brown, Leslie; Earle, Martyn J; Gilea, Manuela; Plechkova, Natalia V; Seddon, Kenneth R

2017-01-01

Ionic liquids can form biphasic solvent systems with many organic solvents and water, and these solvent systems can be used in liquid-liquid separations and countercurrent chromatography. The wide range of ionic liquids that can by synthesised, with specifically tailored properties, represents a new philosophy for the separation of organic, inorganic and bio-based materials. A customised countercurrent chromatograph has been designed and constructed specifically to allow the more viscous char...

Comparative in vitro assessment of tolterodine tartrate tablets by high performance liquid chromatographic (HPLC

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Hossein Danafar

2016-06-01

Full Text Available Tolterodine tartrate, is a new, potent and competitive muscarinic receptor antagonist in clinical development for the treatment of urge incontinence and other symptoms of unstable bladder. The purpose of this study is to establish a reliable and quick method for the assignment of tolterodine tartrate by high performance liquid chromatography with ultraviolet detection (HPLC-UV. A rapid  and  sensitive  high  performance  liquid  chromatographic  (HPLC  method  has  been developed  for  determination  of  tolterodine tartrate.  Mobile phase was composed of phosphate acetate 0.1 M (pH 2.5-acetonitrile (50:50 v/v with a flow rate of 1.2 ml/min. The eluted peaks were detected by a UV detector was set at wavelength of 285 nm. The method was validated in the range of tolterodine tartrate concentrations from 10 to 100 µg/ml. The limits of detection (LOD and quantitation (LOQ of the method were 5 and 10 µg/ml, respectively. The average drug recovery was 98.20 % throughout the linear concentration range. The average within-run and between-run accuracy values of 98.56 % and 99.11 % respectively. Statistical  assessment  of  various  in  vitro  dissolution  parameters  and  assay  results was  also  conducted  to  establish  if  there were  any significant difference among them. The validated HPLC method has been used successfully to study tolterodine tartrate.

Calculation of Interfacial Tensions of Hydrocarbon-water Systems under Reservoir Conditions

DEFF Research Database (Denmark)

Zuo, You-Xiang; Stenby, Erling Halfdan

1998-01-01

Assuming that the number densities of each component in a mixture are linearly distributed across the interface between the coexisting vapor-liquid or liquid-liquid phases, we developed in this research work a linear-gradient-theory (LGT) model for computing the interfacial tension of hydrocarbon......-brine systems. The new model was tested on a number of hydrocarbon-water/brine mixtures and two crude oil-water systems under reservoir conditions. The results show good agreement between the predicted and the experimental interfacial tension data.......Assuming that the number densities of each component in a mixture are linearly distributed across the interface between the coexisting vapor-liquid or liquid-liquid phases, we developed in this research work a linear-gradient-theory (LGT) model for computing the interfacial tension of hydrocarbon-water...... mixtures on the basis of the SRK equation of state. With this model, it is unnecessary to solve the time-consuming density-profile equations of the gradient-theory model. In addition, a correlation was developed for representing the effect of electrolytes on the interfacial tension of hydrocarbon...

Degradation of hydrocarbons in crude oil by the ascomycete Pseudallescheria boydii (Microascaceae)

International Nuclear Information System (INIS)

April, T. M.; Abbott, S. P.; Foght, J. M.; Currah, R. S.

1998-01-01

Four strains of Pseudallescheria boydii were isolated from oil-soaked soils in British Columbia and Alberta and compared with strains from cattle dung and raw sewage. Variations in morphology, colony appearance, colony diameter and temperature tolerance were found among the strains. Three of the strains isolated from oil-contaminated soils and the strain from sewage were tested for their ability to utilize hydrocarbons as the sole carbon source. Gas chromatographic analysis of the residual oil revealed that the strains isolated from the oil-contaminated soil degraded the linear aliphatics. The strain derived from sewage utilized volatile n-alkenes (ethane, propane, butane) but did not utilize the liquid saturate compounds. Since certain strains of Pseudallescheria boydii are known to be pathogenic, cautious handling of these fungi was recommended. However, under properly controlled conditions, selected non-pathogenic strains of the fungi may be used as an integral and effective part of intrinsic bioremediation processes. 39 refs., 3 tabs., 7 figs

Aliphatic Hydrocarbons from Lignocellulose by Pyrolysis over Cesium-Modified Amorphous Silica Alumina Catalysts

NARCIS (Netherlands)

Zabeti, M.; Sai Sankar Gupta, Karthick Babu; Raman, G.; Lefferts, Leon; Schallmoser, Stefan; Lercher, Johannes A.; Seshan, K.

2015-01-01

Cesium-modified amorphous silica alumina (Cs/ASA) is a promising catalyst for the production of hydrocarbons through pyrolysis of biomass. Catalytic pyrolysis of pinewood over Cs/ASA in a pyrolyzer system in conjunction with a gas chromatograph and mass spectrometer resulted in a 22% yield of

Nonionic diethanolamide amphiphiles with isoprenoid-type hydrocarbon chains: thermotropic and lyotropic liquid crystalline phase behaviour

Energy Technology Data Exchange (ETDEWEB)

Sagnella, Sharon M.; Conn, Charlotte E.; Krodkiewska, Irena; Drummond, Calum J. (CSIRO/MSE)

2014-09-24

The thermotropic and lyotropic liquid crystalline phase behaviour of a series of diethanolamide amphiphiles with isoprenoid-type hydrocarbon chains (geranoyl, H-farnesoyl, and phytanoyl) has been investigated. When neat, both H-farnesoyl and phytanoyl diethanolamide form a smectic liquid crystalline structure at sub-zero temperatures. In addition, all three diethanolamides exhibit a glass transition temperature at around -73 C. Geranoyl diethanolamide forms a lamellar crystalline phase with a lattice parameter of 17.4 {angstrom} following long term storage accompanied by the loss of the glass transition. In the presence of water, H-farnesoyl and phytanoyl diethanolamide form lyotropic liquid crystalline phases, whilst geranoyl diethanolamide forms an L{sub 2} phase. H-farnesoyl diethanolamide forms a fluid lamellar phase (L{sub {alpha}}) at room temperature and up to {approx} 40 C. Phytanoyl diethanolamide displays a rich mesomorphism forming the inverse diamond (Q{sub II}{sup D}) and gyroid (Q{sub II}{sup G}) bicontinuous cubic phases in addition to an L{sub {alpha}} phase.

Hydrocarbon composition products of the catalytic recycling plastics waste

Directory of Open Access Journals (Sweden)

Zhaksyntay Kairbekov

2013-09-01

Full Text Available The paper represents the IR spectroscopy results of the hydrocarbon composition of products, which is obtained from catalytic processing of plastic wastes. The optimal conditions for the hydrogenation with to producny liquid of products are identified.  These liquid products are enriched with aromatics, paraffinic- naphthenic and unsaturated hydrocarbons. The main characteristics of the distillates received by hydrogenation of plastics (as density, refractive index, iodine number, pour point, cloud point, filtering, sulfur content,  fractional and composition of the hydrocarbon group.

Cuticle hydrocarbons in saline aquatic beetles

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María Botella-Cruz

2017-07-01

Full Text Available Hydrocarbons are the principal component of insect cuticle and play an important role in maintaining water balance. Cuticular impermeability could be an adaptative response to salinity and desiccation in aquatic insects; however, cuticular hydrocarbons have been poorly explored in this group and there are no previous data on saline species. We characterized cuticular hydrocarbons of adults and larvae of two saline aquatic beetles, namely Nebrioporus baeticus (Dytiscidae and Enochrus jesusarribasi (Hydrophilidae, using a gas chromatograph coupled to a mass spectrometer. The CHC profile of adults of both species, characterized by a high abundance of branched alkanes and low of unsaturated alkenes, seems to be more similar to that of some terrestrial beetles (e.g., desert Tenebrionidae compared with other aquatic Coleoptera (freshwater Dytiscidae. Adults of E. jesusarribasi had longer chain compounds than N. baeticus, in agreement with their higher resistance to salinity and desiccation. The more permeable cuticle of larvae was characterized by a lower diversity in compounds, shorter carbon chain length and a higher proportion of unsaturated hydrocarbons compared with that of the adults. These results suggest that osmotic stress on aquatic insects could exert a selection pressure on CHC profile similar to aridity in terrestrial species.

Gas chromatographic column for the Viking 1975 molecular analysis experiment

Science.gov (United States)

Novotny, M.; Hayes, J. M.; Bruner, F.; Simmonds, P. G.

1975-01-01

A gas chromatographic column has been developed for use in the remote analysis of the Martian surface. The column, which utilizes a liquid-modified organic adsorbent (Tenax) as the stationary phase, provides efficient transmission and resolution of nanogram quantities of organic materials in the presence of millionfold excesses of water and carbon dioxide.

Speciation of eight arsenic compounds in human urine by high performance liquid chromatography with inductively coupled plasma mass spectrometric detection using antimonate for internal chromatographic standardization

DEFF Research Database (Denmark)

Larsen, Erik Huusfeldt; Pritzl, G.; Hansen, S. H.

1993-01-01

Four anionic and four cationic arsenic compounds in urine were separated by anion- and cation-exchange high-performance liquid chromatography and detected by inductively coupled plasma mass spectrometry (ICP-MS) at m/z 75. The species were the anions arsenite, arsenate, monomethylarsonate...... and dimethylarsinate and the cations arsenobetaine, trimethylarsine oxide, arsenocholine and the tetramethylarsonium ion. Hexahydroxyantimonate(III) was co-chromatographed with the arsenic anions but detected at m/z 121 and used as an internal standard for their qualitative analysis. Arsenite was prone to oxidation....... The argon chloride interference at m/z 75 was eliminated by chromatographic separation of the chloride present in the sample from the arsenic analytes. The ClO+ ion detected at m/z 51 and 53 was used to monitor the retention time of chloride in the anion-exchange system. The chloride eluted about 100 s...

Reversed-phase liquid chromatographic profile of free amino acids in strawberry-tree (Arbutus unedo L.) honey.

Science.gov (United States)

Spano, Nadia; Piras, Irene; Ciulu, Marco; Floris, Ignazio; Panzanelli, Angelo; Pilo, Maria I; Piu, Paola C; Sanna, Gavino

2009-01-01

The typical profile of the free amino acids contained in strawberry-tree (Arbutus unedo L.) honey is reported for the first time. An optimized reversed-phase liquid chromatographic (RP-LC) method with phenyl isothiocyanate precolumn derivatization was used. Fourteen free amino acids were identified and quantified in 16 analytical samples. Proline (65.63%) was found to be the most abundant free amino acid, followed by glutamic acid (6.49%), arginine (5.21%), alanine (5.17%), and phenylalanine (4.97%). The total free amino acid content of strawberry-tree honey (average value, 436 mg/kg) was found to be low in comparison to amounts cited in the literature concerning unifloral honeys. The analytical method was optimized and fully validated in terms of detection and quantitation limits, precision (by testing repeatability and reproducibility), linearity, and bias (by means of recovery tests). The acceptability of the validation protocol results was verified using Horwitz's mathematical model and AOAC guidelines.

High-performance liquid chromatographic assay for two rifamycin-derived hypocholesterolemic agents in liver and biological fluids.

Science.gov (United States)

Moore, D J; Perrino, P J; Klerer, C P; Robertson, P

1993-02-26

CGP 43371 (compound I), a mono-pivaloyl oxazole derivative of a 3-piperazino-rifamycin, has been in clinical trials as a potential hypocholesterolemic agent. A reversed-phase high-performance liquid chromatographic (HPLC) assay was developed using a C18 column and a gradient solvent system of methanol-0.1 M sodium acetate, pH 4.5, at a flow-rate of 1 ml/min. The compound and internal standard (rifampicin) were detected by their ultraviolet absorption at 254 nm. Isolation of the compounds from plasma and liver homogenates was accomplished by precipitation of proteins with acetonitrile, followed by evaporation under nitrogen and reconstitution in methanol. Bile, lymph and urine were injected onto the HPLC column without pretreatment. Calibration curves were linear (r > 0.999) over the concentration range 0.25-20.0 micrograms/ml. The assay procedure was also applicable to other rifamycin derivatives and was able to distinguish between molecular species containing small differences in functionality.

Gas-liquid chromatographic determination of aniline metabolites of substituted urea and carbamate herbicides in aqueous solution.

Science.gov (United States)

Hargesheimer, E E; Coutts, R T; Pasutto, F M

1981-07-01

A simple gas-liquid chromatographic (GLC) method has been developed which provides sensitivity and specificity for the analysis of complex mixtures of the commonly occurring herbicide metabolites aniline, 3-chloroaniline, 4-chloroaniline, 4-bromoaniline, and 3-chloro-4-methylaniline. All of these anilines react with acetic anhydride directly in basified aqueous solution. Further reaction of the acetylated anilines with trifluoroacetic anhydride gave diacyl derivatives which were readily resolved by gas chromatography. The structures of the N-acetylated and N-trifluoroacetylated derivatives of benzylamine (internal standard) and the anilines were confirmed by GLC-mass spectrometry. In distilled water the minimum detectable concentrations of aniline and the substituted anilines, using electron capture GLC, are 0.1 nmole/100 mL and 0.05 nmole/100 mL, respectively. The detection limit for the anilines is 1 nmole/100 mL distilled water, using GLC with flame ionization detection. The technique was applied to the determination of anilines added to urine samples obtained from the general population.

A high performance liquid chromatographic assay of Mefloquine in saliva after a single oral dose in healthy adult Africans

Directory of Open Access Journals (Sweden)

Gbotosho Grace O

2012-02-01

Full Text Available Abstract Background Mefloquine-artesunate is a formulation of artemisinin based combination therapy (ACT recommended by the World Health Organization and historically the first ACT used clinically. The use of ACT demands constant monitoring of therapeutic efficacies and drug levels, in order to ensure that optimum drug exposure is achieved and detect reduced susceptibility to these drugs. Quantification of anti-malarial drugs in biological fluids other than blood would provide a more readily applicable method of therapeutic drug monitoring in developing endemic countries. Efforts in this study were devoted to the development of a simple, field applicable, non-invasive method for assay of mefloquine in saliva. Methods A high performance liquid chromatographic method with UV detection at 220 nm for assaying mefloquine in saliva was developed and validated by comparing mefloquine concentrations in saliva and plasma samples from four healthy volunteers who received single oral dose of mefloquine. Verapamil was used as internal standard. Chromatographic separation was achieved using a Hypersil ODS column. Results Extraction recoveries of mefloquine in plasma or saliva were 76-86% or 83-93% respectively. Limit of quantification of mefloquine was 20 ng/ml. Agreement between salivary and plasma mefloquine concentrations was satisfactory (r = 0.88, p Conclusion Disposition of mefloquine in saliva paralleled that in plasma, making salivary quantification of mefloquine potentially useful in therapeutic drug monitoring.

Chromatographic determination of Terbinafine in presence of its Photodegradation products

International Nuclear Information System (INIS)

Abdel-Moety, E.M.; Kelani, K.O.; Abou Al-Alamein, A.M.

2003-01-01

Two different chromatographic techniques have been developed for the determination of terbinafine hydrochloride in presence of its photodegradation products. The first method depends on coupling the TLC- fractionation, on silicia gel 60F254 utilizing chloroform+methanol+25% aq. ammonia ( 12: 0.1:0.1,by volumes), with the direct scanning at 284nm. The second method describes a liquid chromatographic separation of terbinafine and its photolytic degradates on a reversed-phase column[u-Bondapak-TMC 18 (10um,25cmx4.6mm,i.d.)] using a mobile phase containing methanol+water= 80:20 (v/v) with UV-detection at 284 nm. The proposed methods showed significant stability-indication with good linearity, precision and reproducibility. (author)

Validation of a liquid chromatographic method for the pharmaceutical quality control of products containing elacridar

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Emilia Sawicki

2016-08-01

Full Text Available Many anticancer drugs have an impaired bioavailability and poor brain penetration because they are substrates to drug efflux pumps such as P-glycoprotein and Breast Cancer Resistance Protein. Elacridar is a strong inhibitor of these two drug efflux pumps and therefore has great potential to improve oral absorption and brain penetration of many anticancer drugs. Currently, a clinical formulation of elacridar is unavailable and therefore the pharmaceutical development of a drug product is highly warranted. This also necessitates the availability of an analytical method for its quality control. A reverse-phase high-performance liquid chromatographic method with ultraviolet detection was developed for the pharmaceutical quality control of products containing elacridar as the active pharmaceutical ingredient. The analytical method was validated for linearity, accuracy, precision, selectivity, carry-over, stability of stock and reference solutions, stability of the final extract, stability-indicating capability and impurity testing. We found that elacridar is unstable in aqueous solutions that are exposed to light because a hydroxylation product of elacridar is formed. Therefore, sample solutions with elacridar must be protected from light.

Preparation of milk samples for immunoassay and liquid chromatographic screening using matrix solid-phase dispersion.

Science.gov (United States)

Barker, S A; Long, A R

1994-01-01

The use of drugs to maintain the health and maximize the output of dairy cattle has made the monitoring of milk for such agents essential. Screening tests based on immunological, microbial inhibition, and bacterial receptor assays have been developed for the detection of violative levels of therapeutic substances. However, such assays are not infallible, and false positive or negative results can occur when contaminants bind receptors or compete for the binding of the target residues. Such effects may arise from dietary sources, diseases, or other variables. Thus, a violation by such a test is not definitive until further confirmation is obtained. Our laboratory has developed extraction procedures for several drugs used in dairy production. Our method uses matrix solid-phase dispersion (MSPD) to isolate drugs away from contaminants and to eliminate many possible interferences. MSPD can also be used to enhance the specificity of such assays by fractionating various classes of drugs that may cross-react. Similarly, such methods may be used for liquid chromatographic screening and confirmation of a suspect sample.

Micellar Liquid Chromatographic Determination of Carbaryl and 1-Naphthol in Water, Soil, and Vegetables

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Mei-Liang Chin-Chen

2012-01-01

Full Text Available A liquid chromatographic procedure has been developed for the determination of carbaryl, a phenyl-N-methylcarbamate, and its main metabolite 1-naphthol, using a C18 column (250’mm’ × ’4.6’mm with a micellar mobile phase and fluorescence detection at maximum excitation/emission wavelengths of 225/333’nm, respectively. In the optimization step, surfactants sodium dodecyl sulphate (SDS, Brij-35 and N-cetylpyridinium chloride monohydrate, and organic solvents propanol, butanol, and pentanol were considered. The selected mobile phase was 0.15’M SDS-6% (v/v-pentanol-0.01’M NaH2PO4 buffered at pH 3. Validation studies, according to the ICH Tripartite Guideline, included linearity (r>0.999, limit of detection (5 and 18’ng mL-1, for carbaryl and 1-naphthol, resp., and limit of quantification (15 and 50’ng mL-1, for carbaryl and 1-naphthol, resp., with intra- and interday precisions below 1%, and robustness parameters below 3%. The results show that the procedure was adequate for the routine analysis of these two compounds in water, soil, and vegetables samples.

Comparison of chromatographic methods for the determination of bound glycerol in biodiesel

Energy Technology Data Exchange (ETDEWEB)

Foglia, T.A.; Jones, K.C.; Nunez, A.; Phillips, J.G. [U.S. Dept. of Agriculture, Agricultural Research Service, Eastern Regional Research Center, Wyndmoor, PA (United States); Mittelbach, M. [Inst. for Chemistry, Univ. of Graz, Graz (Austria)

2004-09-01

An important fuel criterion for biodiesel is bound glycerol, which is a function of the residual amount of triglycerides and partial glycerides in the biodiesel. Either high-temperature gas chromatography or high performance liquid chromatography can be used for determining these minor but important components in biodiesel. In this paper we have conducted a statistical study on the accuracy of the two methods for ascertaining the bound glycerol in biodiesel fuels obtained from different feedstocks. Analysis of variance showed that with one exception, namely diacylglycerols in some soy oil based biodiesel, there was no statistical difference in bound glycerol for the biodiesel samples analyzed or a difference between methods. Operationally, the high performance liquid chromatographic method is superior to the high temperature gas chromatographic method in that it requires no sample derivatization, has shorter analysis times, and is directly applicable to most biodiesel fuels. (orig.)

Development and evaluation of a gas chromatographic method for the determination of triazine herbicides in natural water samples

Science.gov (United States)

Steinheimer, T.R.; Brooks, M.G.

1984-01-01

A multi-residue method is described for the determination of triazine herbicides in natural water samples. The technique uses solvent extraction followed by gas chromatographic separation and detection employing nitrogen-selective devices. Seven compounds can be determined simultaneously at a nominal detection limit of 0.1 ??g/L in a 1-litre sample. Three different natural water samples were used for error analysis via evaluation of recovery efficiencies and estimation of overall method precision. As an alternative to liquid-liquid partition (solvent extraction) for removal of compounds of interest from water, solid-phase extraction (SPE) techniques employing chromatographic grade silicas with chemically modified surfaces have been examined. SPE is found to provide rapid and efficient concentration with quantitative recovery of some triazine herbicides from natural water samples. Concentration factors of 500 to 1000 times are obtained readily by the SPE technique.A multi-residue method is described for the determination of triazine herbicides in natural water samples. The technique uses solvent extraction followed by gas chromatographic separation and detection employing nitrogen-selective devices. Seven compounds can be determined simultaneously at a nominal detection limit of 0. 1 mu g/L in a 1-litre sample. As an alternative to liquid-liquid partition (solvent extraction) for removal of compounds of interest from water, solid-phase extraction (SPE) techniques employing chromatographic grade silicas with chemically modified surfaces have been examined. SPE is found to provide rapid and efficient concentration with quantitative recovery of some triazine herbicides from natural water samples. Concentration factors of 500 to 1000 times are obtained readily by the SPE technique.

Isotope separations using chromatographic methods

International Nuclear Information System (INIS)

Leseticky, L.

1985-01-01

A survey is given of chromatographic separations of compounds only differing in isotope composition. Isotope effects on physical properties which allow chromatographic separation (vapour tension, adsorption heat, partition coefficient) are very small, with the exception of the simplest molecules. Therefore, separation factors only assume the value of several per cent. From this ensues the necessity of using columns which are specially and very carefully prepared and have a separation efficiency of the order of 10 4 theoretical plates. Briefly discussed is liquid chromatography on ion exchangers which with a varied degree of success was used for separating simple inorganic compounds or ions. Ion exchange chromatography of amino acids labelled with tritium, and chromatography of tritium labelled steroids also provided only a certain degree of separation. A detailed analysis is presented of gas chromatography separation of various deuterium and tritium labelled low-molecular compounds, to which a number of studies has been devoted in the literature. Very promising is the method of complexation gas chromatography based on the reversible formation of a complex of the ligand (the compound being separated) and the compound of the (transition) metal as the steady-state phase. (author)

Liquid hydrocarbons from coal beds – risk factor for the underground work environment - Case study

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Tomescu Cristian

2017-01-01

Full Text Available Liquid hydrocarbons from the coal bed and surrounding rocks, besides the stored gases, methane, carbon dioxide, carbon oxide, generate the increase of the risk factor from the occupational health and safety point of view. If for reducing the gas concentrations level and the methane emissions in order to increase the safety in exploitation exist well-known solutions and methods, the oxidation or self-oxidation of the hydrocarbons from the coal bed generate a series of compounds, reaction products over maximum admitted concentrations which give birth to a toxic atmosphere and which is hazardous for workers, at the same time inducing an error in noting the occurrence of a spontaneous combustion phenomena, a major risk for the workers and for the mineral resource. This paper represents a case study performed in one underground mine unit from Jiu Valley and presents the analysis for underground environment factors monitoring and for solutions for diminishing the OHS risk factors.

Use of laminar chromatographic methods for determination of separation conditions in column extraction chromatography

International Nuclear Information System (INIS)

Ghersini, G.; Cerrai, E.

1978-01-01

Possibilities of using laminar chromatographic methods (paper and thin-layer chromatography) to determine optimal separation conditions in column extraction chromatography are analysed. Most of the given laminar methods are presented as Rf-spectra, i.e. as dependences of Rf found experimentally on eluating solution component concentration. Interrelation between Rf and distribution coefficients of corresponding liquid extraction systems and retention volumes of chromatographic columns is considered. Literature data on extraction paper and thin-layer chromatography of elements with various immovable phases are presented

Simple gas chromatographic method for furfural analysis.

Science.gov (United States)

Gaspar, Elvira M S M; Lopes, João F

2009-04-03

A new, simple, gas chromatographic method was developed for the direct analysis of 5-hydroxymethylfurfural (5-HMF), 2-furfural (2-F) and 5-methylfurfural (5-MF) in liquid and water soluble foods, using direct immersion SPME coupled to GC-FID and/or GC-TOF-MS. The fiber (DVB/CAR/PDMS) conditions were optimized: pH effect, temperature, adsorption and desorption times. The method is simple and accurate (RSDfurfurals will contribute to characterise and quantify their presence in the human diet.

Analysis of aliphatic and aromatic hydrocarbons in particulate matter in Madrid urban area. Analisis de hidrocarburos aromaticos policiclicos e hidrocarburos alifaticos en aerosoles de la zona urbana de Madrid

Energy Technology Data Exchange (ETDEWEB)

Perez, M.; Mendez, J.; Bomboi, M.T.

1988-02-01

Levels of n-alkanes and polycyclic aromatic hydrocarbons have been measured in the air particulate matter during six months, from January to June of 1987, in an urban area of Madrid. The hydrocarbons were collected on glass fiber filter by high volume sampling. The extraction was varried out by sohxlet and ultrasonic techniques. The extracts were clean-up on silica gel fractionation and the chromatographic analysis was performed by capillary coluymn gas chromatographic. Final results are discussed as well as the inmission values related to the possible emission sources.

Pyrolysis of municipal plastic wastes for recovery of gasoline-range hydrocarbons

Energy Technology Data Exchange (ETDEWEB)

Demirbas, Ayhan [Department of Chemical Engineering, Selcuk University, Konya (Turkey)

2004-08-01

This paper describes non-catalytic pyrolysis of plastic waste materials. Three types of waste plastics were used in this study: polystyrene (PS), polyethylene (PE) and polypropylene (PP). Under pyrolysis conditions, plastic wastes can be decomposed into three fractions: gas, liquid and solid residue. The liquid products are usually composed of higher boiling point hydrocarbons. In order to obtain useful gasoline-range hydrocarbons from the pyrolytic oil, fractional distillation is preferred for product separation. More valuable chemical raw materials including benzene, toluene and other condensed aromatic hydrocarbons may be obtained by refining the pyrolytic oil. The results showed that waste PS yielded higher liquid, and waste PE and PP yielded higher gaseous products. The dominant pyrolytic liquid product of PS waste was styrene.

Measurement Uncertainty of Liquid Chromatographic Analyses Visualized by Ishikawa Diagrams

OpenAIRE

Meyer, Veronika R.

2017-01-01

Ishikawa, or cause-and-effect diagrams, help to visualize the parameters that influence a chromatographic analysis. Therefore, they facilitate the set up of the uncertainty budget of the analysis, which can then be expressed in mathematical form. If the uncertainty is calculated as the Gaussian sum of all uncertainty parameters, it is necessary to quantitate them all, a task that is usually not practical. The other possible approach is to use the intermediate precision as a base for the uncer...

Hydrocarbons

Energy Technology Data Exchange (ETDEWEB)

1927-02-22

Coal tar, mineral oils, bitumens, coal extraction products, hydrogenation products of coal, oil schists can be atomized and heated with steam to decompose pyrogenetically and form gases rich in olefins which may be heated with or without pressure and with or without catalysts to produce liquid hydrocarbons of low boiling point, some of which may be aromatic. The apparatus should be lined with copper, silica, or ferrosilicon to prevent contact of the bases with iron which causes deposition of soot. Catalysts used may be metal oxides, silica, graphite, active charcoal, mica, pumice, porcelain, barium carbonate, copper, silver, gold, chromium, boron, or their compounds. At temperatures from 300 to 400/sup 0/C, olefins are produced. At higher temperatures, naphthenes and benzene hydrocarbons are produced.

Development and validation of high-perfomance liquid chromatographic method for determination of ofloxacin and lomefloxacin in human plasma

Directory of Open Access Journals (Sweden)

DRAGICA ZENDELOVSKA

2005-12-01

Full Text Available Ahigh-performance liquid chromatographicmethod for the determination of ofloxacin and lomefloxacin in human plasma has been developed and validated. The effect of organic modifiers on the retention of the investigated drugs was investigated. Asimple isocratic chromatographic assay with UV-detection at 280 nm was performed on a Hibar Lichrospher 100 RP 8 column (250×4.6 mm, 5 mm. Merck, Germany using a mixture of acetonitrile and 0.5 % triethylamine in water (pH adjusted to 2.5 with H3PO4 (15:85, V/V as the mobile phase at flow rate of 1.2 mL min-1. The calibration curves were linear in the concentration ragne of 0.5 – 6.0 mg mL-1 for ofloxacin and 0.2-4.5 mg mL-1 for lomefloxacin.

High performance liquid chromatographic determination of ...

African Journals Online (AJOL)

STORAGESEVER

2010-02-08

) high performance liquid chromatography (HPLC) grade .... applications. These are important requirements if the reagent is to be applicable to on-line pre or post column derivatisation in a possible automation of the analytical.

Extending the basic function of lattice oxygen in lepidocrocite titanate - The conversion of intercalated fatty acid to liquid hydrocarbon fuels

Science.gov (United States)

Maluangnont, Tosapol; Arsa, Pornanan; Sooknoi, Tawan

2017-12-01

We report herein the basicity of the external and internal lattice oxygen (OL) in lepidocrocite titanates with respect to CO2 and palmitic acid, respectively. Several compositions have been tested with different types of the metal M aliovalently (co)substituted for Ti, K0.8[MyTi2-y]O4 (M = Li, Mg, Fe, Co, Ni, Cu, Zn, Cu/Ni and Cu/Zn). The low CO2 desorption peak temperature (70-100 °C) suggests that the external OL sites are weakly basic similar to TiO2. However, the internal OL sites are sufficiently basic to deprotonate palmitic acid, forming the intercalated potassium palmitate at the interlayer spaces. The latter serves as a two-dimensional (2D) molecular reactor for the production of liquid hydrocarbon fuels via deoxygenation under atmospheric N2. A relationship has been observed between the yield of the liquid products vs the partial charge of the lattice oxygen (δO). Since the deoxygenation pathway is highly dependent on the metal substitution, the redox-active sites might also play some roles. The co-substituted K0.8[Cu0.2Ni0.2]Ti1.6O4 produced 68.0% yield of the liquid products, with 51% saturated and 15% unsaturated C15 hydrocarbons at 350 °C.

Inverse Opal Photonic Crystals as an Optofluidic Platform for Fast Analysis of Hydrocarbon Mixtures.

Science.gov (United States)

Xu, Qiwei; Mahpeykar, Seyed Milad; Burgess, Ian B; Wang, Xihua

2018-06-13

Most of the reported optofluidic devices analyze liquid by measuring its refractive index. Recently, the wettability of liquid on various substrates has also been used as a key sensing parameter in optofluidic sensors. However, the above-mentioned techniques face challenges in the analysis of the relative concentration of components in an alkane hydrocarbon mixture, as both refractive indices and wettabilities of alkane hydrocarbons are very close. Here, we propose to apply volatility of liquid as the key sensing parameter, correlate it to the optical property of liquid inside inverse opal photonic crystals, and construct powerful optofluidic sensors for alkane hydrocarbon identification and analysis. We have demonstrated that via evaporation of hydrocarbons inside the periodic structure of inverse opal photonic crystals and observation of their reflection spectra, an inverse opal film could be used as a fast-response optofluidic sensor to accurately differentiate pure hydrocarbon liquids and relative concentrations of their binary and ternary mixtures in tens of seconds. In these 3D photonic crystals, pure chemicals with different volatilities would have different evaporation rates and can be easily identified via the total drying time. For multicomponent mixtures, the same strategy is applied to determine the relative concentration of each component simply by measuring drying time under different temperatures. Using this optofluidic sensing platform, we have determined the relative concentrations of ternary hydrocarbon mixtures with the difference of only one carbon between alkane hydrocarbons, which is a big step toward detailed hydrocarbon analysis for practical use.

Gamma irradiation of hydrocarbon-liquid nitrogen systems and the synthesis of ammonia

International Nuclear Information System (INIS)

Fleming, H.L.

1982-01-01

The 60 Co-gamma radiolysis of hydrocarbons (HC)-liquid N 2 mixtures at 77 0 K and 1.8 atm of pressure was investigated. Batch irradiation studies of methane, ethane, and ethylene and semibatch studies of methane were made in the presence and absence of transition metal oxide catalysts. In noncatalyzed systems, the effects of varying the radiation dose, total dose, solute feed rate and concentration and liquid N 2 volume were investigated. NH 3 was found to be the major N-containing product in the alkane solute system. N 2 and HC radical addition was found to be the predominate initial reaction for nitrogeneous product formation. Results of scavenger studies indicate that excited N 2 played a lesser role in precursor formation. All product yields were found to be dependent upon the H-containing species availability in the liquid N 2 solution. Production rates were limited by HC solubility. The use of the transition metal oxide supported catalyst greatly increased product formation in all systems. Product yields were found to be dependent upon the available catalyst surface area, metal loading, and reduction techniques for each metal examined. As evidenced by the radiation lag time studies, the stability of the N 2 precursors on the catalyst surface was believed to be a significant factor in reaction enhancement. Energy transfer from the catalyst to the absorbates was examined and could not be ruled out

Liquid chromatographic method for the simultaneous determination of cefalexin and trimethoprim in dog plasma and application to the pharmacokinetic studies of a coformulated preparation.

Science.gov (United States)

Qi, Meiling; Wang, Peng; Sun, Ping; Liu, Xia

2006-03-07

A liquid chromatographic method is described for the simultaneous determination of cefalexin and trimethoprim in dog plasma. A simple protein precipitation procedure was adopted for the sample preparation with satisfactory extraction recoveries for both analytes. Chromatographic separation of the analytes was achieved on a C(18) column using a mixture of 2 mol/l formate buffer (pH 3.5), methanol and acetonitrile (22:7:7, v/v/v) containing a 0.002 mol/l sodium dodecyl sulfate as mobile phase and detection was performed at 240 nm. The linearity was obtained over the concentration ranges of 1.0-100.0 microg/ml for cefalexin and 0.5-50.0 microg/ml for trimethoprim. For each level of QC samples including the lower limit of quantification, both inter- and intra-day precisions (R.S.D.) were trimethoprim, and accuracy (RE) was -1.4% for cefalexin and -3.0% for trimethoprim. The present LC method was successfully applied to the pharmacokinetic studies of coformulated cefalexin dispersible tablets after oral administration to beagle dogs.

Urea functionalized surface-bonded sol-gel coating for on-line hyphenation of capillary microextraction with high-performance liquid chromatography.

Science.gov (United States)

Jillani, Shehzada Muhammad Sajid; Alhooshani, Khalid

2018-03-30

Sol-gel urea functionalized-[bis(hydroxyethyl)amine] terminated polydimethylsiloxane coating was developed for capillary microextraction-high performance liquid chromatographic analysis from aqueous samples. A fused silica capillary is coated from the inside with surface bonded coating material and is created through in-situ sol-gel reaction. The urea-functionalized coating was immobilized to the inner surface of the capillary by the condensation reaction of silanol groups of capillary and sol-solution. The characterization of the coating material was successfully done by using X-ray photoelectron spectroscopy, thermogravimetric analysis, field emission scanning electron microscope, and energy dispersive X-ray spectrometer. To make a setup of online capillary microextraction-high performance liquid chromatography, the urea functionalized capillary was installed in the HPLC manual injection port. The analytes of interest were pre-concentrated in the coated sampling loop, desorbed by the mobile phase, chromatographically separated on C-18 column, and analyzed by UV detector. Sol-gel coated capillaries were used for online extraction and high-performance liquid chromatographic analysis of phenols, ketones, aldehydes, and polyaromatic hydrocarbons. This newly developed coating showed excellent extraction for a variety of analytes ranging from highly polar to non-polar in nature. The analysis using sol-gel coating showed excellent overall sensitivity in terms of lower detection limits (S/N = 3) for the analytes (0.10 ng mL -1 -14.29 ng mL -1 ) with acceptable reproducibility that is less than 12.0%RSD (n = 3). Moreover, the capillary to capillary reproducibility of the analysis was also tested by changing the capillary of the same size. This provided excellent%RSD of less than 10.0% (n = 3). Copyright © 2018 Elsevier B.V. All rights reserved.

Identification and Characterisation of Major Hydrocarbons in ...

African Journals Online (AJOL)

Identification and Characterisation of Major Hydrocarbons in Thermally Degraded Low Density Polyethylene Films. ... There were alkanes, alkenes, halogenated alkanes, and very few aromatics in the liquid product and, the hydrocarbons were observed to range between C10 - C27. The FTIR and GC-MS results show the ...

[Determination of phthalate plasticizers in foods by high performance liquid chromatography with gel permeation chromatographic clean-up].

Science.gov (United States)

Zhang, Chunyu; Wang, Hui; Zhang, Xiaohui; Ma, Zhongqiang; Deng, Wanmei; Hu, Ke; Ding, Mingyu

2011-12-01

A method of gel permeation chromatography-high performance liquid chromatography (GPC-HPLC) was established for the simultaneous determination of 5 main phthalate plasticizers in foods (edible oil, instant noodles, fried pastries, Saqima, etc.). The samples were extracted with petroleum ether in an ultrasonator, purified by a GPC column, and analyzed by HPLC. The chromatographic separation was achieved on a Labtech-C18 column (250 mm x 4.6 mm, 5 microm) using acetonitrile and water mixture as the mobile phases in a gradient elution mode. The developed method exhibited a linear correlation coefficient of more than 0.997 and the detection limits of 3.25 - 13.4 microg/L. The spike recoveries were between 70.4% and 113.6% with the relative standard deviations (RSDs, n = 3) of 0.3% - 5.8% at the spiked level of 50 mg/L. This method is simple, rapid and practical, and can be used for the simultaneous determination of PAEs in grease food samples.

Rapid ion-pair liquid chromatographic method for the determination of fenbendazole marker residue in fermented dairy products.

Science.gov (United States)

Vousdouka, Venetia I; Papapanagiotou, Elias P; Angelidis, Apostolos S; Fletouris, Dimitrios J

2017-04-15

A simple, rapid and sensitive liquid chromatographic method that allows for the quantitative determination of fenbendazole residues in fermented dairy products is described. Samples were extracted with a mixture of acetonitrile-phosphoric acid and the extracts were defatted with hexane to be further partitioned into ethyl acetate. The organic layer was evaporated to dryness and the residue was reconstituted in mobile phase. Separation of fenbendazole and its sulphoxide, sulphone, and p-hydroxylated metabolites was carried out isocratically with a mobile phase containing both positively and negatively charged pairing ions. Overall recoveries ranged from 79.8 to 88.8%, while precision data, based on within and between days variations, suggested an overall relative standard deviation of 6.3-11.0%. The detection and quantification limits were lower than 9 and 21μg/kg, respectively. The method has been successfully applied to quantitate fenbendazole residues in Feta cheese and yoghurt made from spiked and incurred ovine milk. Copyright © 2016 Elsevier Ltd. All rights reserved.

Characterization of Chinese rice wine taste attributes using liquid chromatographic analysis, sensory evaluation, and an electronic tongue.

Science.gov (United States)

Yu, HaiYan; Zhao, Jie; Li, Fenghua; Tian, Huaixiang; Ma, Xia

2015-08-01

To evaluate the taste characteristics of Chinese rice wine, wine samples sourced from different vintage years were analyzed using liquid chromatographic analysis, sensory evaluation, and an electronic tongue. Six organic acids and seventeen amino acids were measured using high performance liquid chromatography (HPLC). Five monosaccharides were measured using anion-exchange chromatography. The global taste attributes were analyzed using an electronic tongue (E-tongue). The correlations between the 28 taste-active compounds and the sensory attributes, and the correlations between the E-tongue response and the sensory attributes were established via partial least square discriminant analysis (PLSDA). E-tongue response data combined with linear discriminant analysis (LDA) were used to discriminate the Chinese rice wine samples sourced from different vintage years. Sensory evaluation indicated significant differences in the Chinese rice wine samples sourced from 2003, 2005, 2008, and 2010 vintage years in the sensory attributes of harmony and mellow. The PLSDA model for the taste-active compounds and the sensory attributes showed that proline, fucose, arabinose, lactic acid, glutamic acid, arginine, isoleucine, valine, threonine, and lysine had an influence on the taste characteristic of Chinese rice wine. The Chinese rice wine samples were all correctly classified using the E-tongue and LDA. The electronic tongue was an effective tool for rapid discrimination of Chinese rice wine. Copyright © 2015 Elsevier B.V. All rights reserved.

Trace determination of volatile polycyclic aromatic hydrocarbons in natural waters by magnetic ionic liquid-based stir bar dispersive liquid microextraction.

Science.gov (United States)

Benedé, Juan L; Anderson, Jared L; Chisvert, Alberto

2018-01-01

In this work, a novel hybrid approach called stir bar dispersive liquid microextraction (SBDLME) that combines the advantages of stir bar sorptive extraction (SBSE) and dispersive liquid-liquid microextraction (DLLME) has been employed for the accurate and sensitive determination of ten polycyclic aromatic hydrocarbons (PAHs) in natural water samples. The extraction is carried out using a neodymium stir bar magnetically coated with a magnetic ionic liquid (MIL) as extraction device, in such a way that the MIL is dispersed into the solution at high stirring rates. Once the stirring is ceased, the MIL is magnetically retrieved onto the stir bar, and subsequently subjected to thermal desorption (TD) coupled to a gas chromatography-mass spectrometry (GC-MS) system. The main parameters involved in TD, as well as in the extraction step affecting the extraction efficiency (i.e., MIL amount, extraction time and ionic strength) were evaluated. Under the optimized conditions, the method was successfully validated showing good linearity, limits of detection and quantification in the low ng L -1 level, good intra- and inter-day repeatability (RSD < 13%) and good enrichment factors (18 - 717). This sensitive analytical method was applied to the determination of trace amounts of PAHs in three natural water samples (river, tap and rainwater) with satisfactory relative recovery values (84-115%), highlighting that the matrices under consideration do not affect the extraction process. Copyright © 2017 Elsevier B.V. All rights reserved.

Liquid chromatographic studies on the behaviour of Pu(III), Pu(IV) and Pu(VI) on a RP stationary phase in presence of α-hydroxyisobutyric acid as a chelating agent

Energy Technology Data Exchange (ETDEWEB)

Jaison, P.G.; Kumar, Pranaw; Telmore, Vijay M. [Bhabha Atomic Research Centre, Mumbai (India). Fuel Chemistry Division

2017-06-01

Since plutonium possesses multiple oxidation states which can coexist in solution, a method for the identification of these oxidation states is important to understand its chemical processes. Liquid chromatographic studies were carried out to compare the chromatographic behaviour of different oxidation states of Pu in presence of the eluent, α-hydroxyisobutyric acid (HIBA). The three oxidation states of Pu viz. Pu(III), Pu(IV) and Pu(VI) were separated under optimised conditions. It was seen that the presence of the complexing agent influences the equilibrium of Pu(III)/(IV) as well as Pu(IV)/(VI) systems. Pu(III) to Pu(IV) conversion was found to be enhanced by high pH and concentration of HIBA whereas a relatively low pH and high concentration of HIBA promotes the conversion of Pu(VI) to Pu(IV).

Autothermal reforming of liquid hydrocarbons for H{sub 2} production

Energy Technology Data Exchange (ETDEWEB)

Palm, C.; Montel, S.; Cremer, P.; Peters, R.; Stolten, D. [Forschungszentrum Juelich GmbH (Germany). Inst. for Materials and Processes in Energy Systems IWV-3: Process Engineering

2001-07-01

The process of autothermal reforming of hydrocarbons can be used for the production of hydrogen within a fuel cell system. The application of three precious metal catalysts for the autothermal reforming of alkane mixtures with boiling ranges between 235 and 325 C was examined. The experiments were carried out at n(O{sub 2})/n(C) = 0.40, n(H{sub 2}O)/n(C) = 2.20, a catalyst bed temperature between 730 and 570 C and a hydrocarbon feed of 30 g/h. The catalysts yielded different hydrocarbon conversions, which can be explained by differences in the activity for the steam reforming reaction. The most active catalyst was also successfully utilized in the conversion of 400 g/h hydrocarbon feed. (orig.)

Recovering low-boiling hydrocarbons, etc

Energy Technology Data Exchange (ETDEWEB)

Pier, M

1934-10-03

A process is described for the recovery of low-boiling hydrocarbons of the nature of benzine through treatment of liquid carbonaceous materials with hydrogen under pressure at raised temperature, suitably in the presence of catalysts. Middle oils (practically saturated with hydrogen) or higher boiling oils at a temperature above 500/sup 0/ (with or without the addition of hydrogen) containing cyclic hydrocarbons not saturated with hydrogen are changed into low boiling hydrocarbons of the nature of benzine. The cracking takes place under strongly hydrogenating conditions (with the use of a strongly active hydrogenating catalyst or high pressure) at temperatures below 500/sup 0/. If necessary, the constituents boiling below 200/sup 0/ can be reconverted into cyclic hydrocarbons partially saturated with hydrogen. (BLM)

Derivatization reactions in the gas—liquid chromatographic analysis of drugs in biological fluids

NARCIS (Netherlands)

Hulshoff, A.; Lingeman, H.

1984-01-01

Alkylation, acylation, silylation and other derivatization reactions applied to the gas chromatographic analysis of drugs in biological matrices are reviewed. Reaction conditions are discussed in relation to reaction mechanisms. Detector-oriented labelling of drugs, and derivatization with chiral

Quantification of petroleum-type hydrocarbons in avian tissue

Energy Technology Data Exchange (ETDEWEB)

Gay, M.L.; Belisle, A.A.; Patton, J.F.

1980-01-04

Methods were developed for the analysis of 16 hydrocarbons in avian tissue. Mechanical extraction with pentane was followed by clean-up on Florisil and Silicar. Residues were determined by gas-liquid chromatography and gas-liquid, chromatography-mass spectrometry. The method was applied to the analysis of liver, kidney, fat, and brain tissue of mallard ducks (Anas platyrhynchos) fed a mixture of hydrocarbons. Measurable concentrations of all compounds analyzed were present in all tissues except brain. Highest concentrations were in fat.

High performance liquid chromatographic separation of thirteen drugs collected in Chinese Pharmacopoeia 2010(Ch.P2010 on cellulose ramification chiral stationary phase

Directory of Open Access Journals (Sweden)

Ying Zhou

2012-02-01

Full Text Available The enantiomers separation of thirteen drugs collected in Ch.P2010 was performed on chiral stationary phase of cellulose ramification (chiralpak OD and chiralpak OJ by high performance liquid chromatographic (HPLC methods, which included ibuprofen (C1, ketoprofen (C2, nitrendipine (C3, nimodipine (C4, felodipine (C5, omeprazole (C6, praziquantel (C7, propranolol hydrochloride (C8, atenolol (C9, sulpiride (C10, clenbuterol hydrochloride (C11, verapamil hydrochloride (C12, and chlorphenamine maleate (C13. The mobile phase consisted of isopropanol and n-hexane. The detection wavelength was set at 254 nm and the flow rate was 0.7 mL/min. The enantiomers separation of these thirteen racemates on chiralpak OD column and chiralpak OJ column was studied, while the effects of proportion of organic additives, alcohol displacer and temperature on the separation were studied. And the mechanism of some of racemates was discussed. The results indicated that thirteen chiral drugs could be separated on chiral stationary phase of cellulose ramification in normal phase chromatographic system. The chromatographic retention and resolution of enantiomers could be adjusted by factors including column temperature and the concentration of alcohol displacer and organic alkaline modifier in mobile phase. It was shown that the resolution was improved with reducing concentration of alcohol displacer. When concentration of organic alkaline modifier was 0.2% (v/v, the resolution and the peak shape were fairly good. Most racemates mentioned above had better resolution at column temperature of 25 °C. When racemates were separated, the temperature should be kept so as to obtain stable separation results. Keywords: HPLC, Chiral stationary phase, Optical enantiomers, Cellulose ramification

Radioimmunoassay and liquid-chromatographic analysis for free cortisol in urine compared with isotope dilution-mass spectrometry

International Nuclear Information System (INIS)

Lantto, O.

1982-01-01

Three different routine methods for analysis for urinary cortisol with those by a highly specific reference method based on isotope dilution-mass spectrometry (I) were compared. A ''high-performance'' liquid-chromatographic method (II) gave the most comparable results (regression coefficient 0.86, intercept 9 nmol/L). For some urines much lower values were obtained by I than by II. Two radioimmunoassay (III) methods, one involving direct assay and one involving extraction, gave less-accurate results (regression coefficients of 1.87 and 1.52 and intercepts of 86 and 12 nmol/L, respectively), although values obtained by III and by I correlated well (r = 0.95-0.99), indicating a relation between the free cortisol and the compounds interfering in III. The apparent accuracy for the extraction method was improved by using as calibration standards urine samples previously assayed by I (regression coefficient 0.90, intercept 6 nmol/L). All four methods investigated showed a statistically significant sex-related difference in 24-h urinary cortisol excretion; evidently such a finding should be a prerequisite in any such method proposed for routine use

Holdup of O/W emulsion in a packed column for liquid membrane separation of hydrocarbon; Tankasuiso no ekimaku bunri ni okeru jutento nai no emarushon horudo appu

Energy Technology Data Exchange (ETDEWEB)

Egashira, R.; Sugimoto, T.; Kawasaki, J. [Tokyo Inst. of Technology, Tokyo (Japan). Faculty of Engineering

1993-07-10

Liquid membrane separation of hydrocarbon is an energy saving separation method that is expected of practical use. If the method uses a packed column, the holdup of O/W emulsion affects the effective contact area and residence time of the emulsion. Therefore, this paper describes an attempt to correlate the dynamic emulsion holdup in a packed column in liquid membrane separation of hydrocarbon with property values of the emulsion and external oil phase, and operation variables. The experiment used a mixture of toluene + n - heptane + n - decane for oil phase in the O/W emulsion and saponin aqueous solution for liquid phase (liquid membrane phase). The packed column with an inner diameter of 37 mm used stainless steel McMahon packing. As a result of the experiment, the dynamic emulsion holdup showed a correlation according to the Reynolds number and Galilei number, regardless of whether the emulsion permeates the liquid membrane. The correlation made it possible to estimate in a simple manner the emulsion holdup in the packed column when this separation method is used. 5 refs., 3 figs., 3 tabs.

Multivariate curve-resolution analysis of pesticides in water samples from liquid chromatographic-diode array data.

Science.gov (United States)

Maggio, Rubén M; Damiani, Patricia C; Olivieri, Alejandro C

2011-01-30

Liquid chromatographic-diode array detection data recorded for aqueous mixtures of 11 pesticides show the combined presence of strongly coeluting peaks, distortions in the time dimension between experimental runs, and the presence of potential interferents not modeled by the calibration phase in certain test samples. Due to the complexity of these phenomena, data were processed by a second-order multivariate algorithm based on multivariate curve resolution and alternating least-squares, which allows one to successfully model both the spectral and retention time behavior for all sample constituents. This led to the accurate quantitation of all analytes in a set of validation samples: aldicarb sulfoxide, oxamyl, aldicarb sulfone, methomyl, 3-hydroxy-carbofuran, aldicarb, propoxur, carbofuran, carbaryl, 1-naphthol and methiocarb. Limits of detection in the range 0.1-2 μg mL(-1) were obtained. Additionally, the second-order advantage for several analytes was achieved in samples containing several uncalibrated interferences. The limits of detection for all analytes were decreased by solid phase pre-concentration to values compatible to those officially recommended, i.e., in the order of 5 ng mL(-1). Copyright © 2010 Elsevier B.V. All rights reserved.

Liquid chromatographic determination of chloramine-T and its primary degradation product, p-toluenesulfonamide, in water

Science.gov (United States)

Dawson, Verdel K.; Davis, Ruth A.

1997-01-01

N-sodium-N-chloro-rho-toluenesulfonamide (chloramine-T) effectively controls bacterial gill disease (BGD) in cultured fishes, BGD, a common disease of hatchery-reared salmonids, causes more fish losses than any other disease among these species. This study describes a liquid chromatographic (LC) method that is capable of direct, simultaneous analysis of chloramine-T and its primary degradation product, rho-toluenesulfonamide (rho-TSA), in water. The procedure involves reversed-phase (C-18) LC analysis with ion suppression, using 0.01 M phosphate buffer at pH 3. The mobile phase is phosphate buffer-acetonitrile (60 + 40) at 1 mL/min. Both chemicals can be detected with a UV spectrophotometer at 229 nm; the method is linear up to 40 mg, chloramine-T or rho-TSA/L. Mean recoveries were 96.4 +/- 6.1% for water samples fortified with 0.03 mg chloramine-T/L and 95.3 +/- 4.6% for water samples fortified with 0.005 mg rho-TSA/L. Limits of detection without sample enrichment for chloramine-T and rho-TSA are 0.01 mg/L and 0.001 mg/L, respectively.

Carbon nanotube-based benzyl polymethacrylate composite monolith as a solid phase extraction adsorbent and a stationary phase material for simultaneous extraction and analysis of polycyclic aromatic hydrocarbon in water.

Science.gov (United States)

Al-Rifai, Asma'a; Aqel, Ahmad; Wahibi, Lamya Al; ALOthman, Zeid A; Badjah-Hadj-Ahmed, Ahmed-Yacine

2018-02-02

A composite of multi-walled carbon nanotubes incorporated into a benzyl methacrylate-co-ethylene dimethacrylate porous monolith was prepared, characterized and used as solid phase adsorbent and as stationary phase for simultaneous extraction and separation of ten polycyclic aromatic hydrocarbons, followed by nano-liquid chromatography analysis. The extraction and chromatographic parameters were optimized with regard to the extraction efficiency and the quality of chromatographic analytes separation. Under the optimized conditions, all PAHs were separated in 13 min with suitable resolution values (Rs = 1.74-3.98). Addition of a small amount of carbon nanotubes (0.1% with respect to monomers) to the polymerization mixture increased the efficiency for the separation column to over 41,700 plates m -1 for chrysene at flow rate of 0.5 μL min -1 . The method showed a wide linear range (1-500 μg L -1 with R 2 more than 0.9938), acceptable extraction repeatability (RSDs extraction cartridges) and satisfactory detection limits (0.02-0.22 μg L -1 ). Finally, the proposed method was successfully applied to the detection of polycyclic aromatic hydrocarbons in environmental water samples. After a simple extraction procedure with preconcentration factor equal to 100, the average recovery values in ultra-pure, tap and sea water samples were found to be in the range 81.3-95.4% with %RSD less than 6.4. Again, the presence of carbon nanotubes (0.3% relatively to monomers) in native polymer enhanced the extraction performance for the solid phase adsorbent up to 78.4%. The application of the monoliths modified with CNTs in extraction and nano-scale liquid chromatography for analysis of environmental samples offered several advantages; it demonstrated an acceptable precision, low detection limits, good reproducibility, satisfying recoveries and wide dynamic linear ranges. Copyright © 2018. Published by Elsevier B.V.

Underground disposal of tanks containing liquid and inflammable hydrocarbons; Mise sous talus ou sous terre des reservoirs contenant des hydrocarbures liquides inflammables

Energy Technology Data Exchange (ETDEWEB)

Kukuczka, P.; Giovannini, B.; Caumont, M.; Varin, F

2001-09-15

The protection from thermal and mechanical stresses, of hazardous products tanks, by earth covering, is often used since many years in France and in many countries of Europe. In the case of hydrocarbons tanks, only small capacity tanks are covering. The aim of this report is to evaluate the feasibility of this technique for big capacity tanks as refinery tanks. It details the different typologies of tanks containing inflammable liquids and the associated systems, examines if the covering technique presents some special difficulties and precises the specifications needed for the new tanks being covering. (A.L.B.)

Systematic evaluation of commercially available ultra-high performance liquid chromatography columns for drug metabolite profiling: optimization of chromatographic peak capacity.

Science.gov (United States)

Dubbelman, Anne-Charlotte; Cuyckens, Filip; Dillen, Lieve; Gross, Gerhard; Hankemeier, Thomas; Vreeken, Rob J

2014-12-29

The present study investigated the practical use of modern ultra-high performance liquid chromatography (UHPLC) separation techniques for drug metabolite profiling, aiming to develop a widely applicable, high-throughput, easy-to-use chromatographic method, with a high chromatographic resolution to accommodate simultaneous qualitative and quantitative analysis of small-molecule drugs and metabolites in biological matrices. To this end, first the UHPLC system volume and variance were evaluated. Then, a mixture of 17 drugs and various metabolites (molecular mass of 151-749Da, logP of -1.04 to 6.7), was injected on six sub-2μm particle columns. Five newest generation core shell technology columns were compared and tested against one column packed with porous particles. Two aqueous (pH 2.7 and 6.8) and two organic mobile phases were evaluated, first with the same flow and temperature and subsequently at each column's individual limit of temperature and pressure. The results demonstrated that pre-column dead volume had negligible influence on the peak capacity and shape. In contrast, a decrease in post-column volume of 57% resulted in a substantial (47%) increase in median peak capacity and significantly improved peak shape. When the various combinations of stationary and mobile phases were used at the same flow rate (0.5mL/min) and temperature (45°C), limited differences were observed between the median peak capacities, with a maximum of 26%. At higher flow though (up to 0.9mL/min), a maximum difference of almost 40% in median peak capacity was found between columns. The finally selected combination of solid-core particle column and mobile phase composition was chosen for its selectivity, peak capacity, wide applicability and peak shape. The developed method was applied to rat hepatocyte samples incubated with the drug buspirone and demonstrated to provide a similar chromatographic resolution, but a 6 times higher signal-to-noise ratio than a more traditional UHPLC

Changes in liquid water alter nutrient bioavailability and gas diffusion in frozen antarctic soils contaminated with petroleum hydrocarbons.

Science.gov (United States)

Harvey, Alexis Nadine; Snape, Ian; Siciliano, Steven Douglas

2012-02-01

Bioremediation has been used to remediate petroleum hydrocarbon (PHC)-contaminated sites in polar regions; however, limited knowledge exists in understanding how frozen conditions influence factors that regulate microbial activity. We hypothesized that increased liquid water (θ(liquid) ) would affect nutrient supply rates (NSR) and gas diffusion under frozen conditions. If true, management practices that increase θ(liquid) should also increase bioremediation in polar soils by reducing nutrient and oxygen limitations. Influence of θ(liquid) on NSR was determined using diesel-contaminated soil (0-8,000 mg kg(-1)) from Casey Station, Antarctica. The θ(liquid) was altered between 0.007 and 0.035 cm(3) cm(-3) by packing soil cores at different bulk densities. The nutrient supply rate of NH 4+ and NO 3-, as well as gas diffusion coefficient, D(s), were measured at two temperatures, 21°C and -5°C, to correct for bulk density effects. Freezing decreased NSR of both NH 4+ and NO 3-, with θ(liquid) linked to nitrate and ammonia NSR in frozen soil. Similarly for D(s), decreases due to freezing were much more pronounced in soils with low θ(liquid) compared to soils with higher θ(liquid) contents. Additional studies are needed to determine the relationship between degradation rates and θ(liquid) under frozen conditions. Copyright © 2011 SETAC.

Treatment of hydrocarbon oils

Energy Technology Data Exchange (ETDEWEB)

1936-02-22

A process is described for refining a mixture of liquid hydrocarbons containing harmful substances, this process permitting the operation, which consists in treating the liquid mixture at a temperature higher than 200/sup 0/C with a solid catalyst of phosphoric acid, consisting of phosphoric acid deposited on a solid support of the type of metallurgical coke, for a time sufficient to convert the harmful components to inoffensive substances.

Formaldehyde, methanol and hydrocarbon emissions from methanol-fueled cars

International Nuclear Information System (INIS)

Williams, R.L.; Lipari, F.; Potter, R.A.

1990-01-01

Exhaust and evaporative emissions tests were conducted on several methanol- and gasoline-fueled vehicles. Separate samples for chromatographic analysis of formaldehyde, methanol, and individual hydrocarbons were collected in each of the three phases of the driving cycle and in each of the two portions of the evaporative emissions test. One vehicle, equipped with an experimental variable-fuel engine, was tested using methanol/gasoline fuel mixtures of 100, 85, 50, 15, and 0 percent methanol. Combustion-generated hydrocarbons were lowest using methanol fuel, and increased several-fold as the gasoline fraction was increased. Gasoline components in the exhaust increased from zero as the gasoline fraction of the fuel was increased. On the other hand, formaldehyde emissions were several times higher using methanol fuel than they were using gasoline. A dedicated methanol car and the variable-fuel car gave similar emissions patterns when they both were tested using methanol fuel. The organic-carbon composition of the exhaust was 85-90 percent methanol, 5-7 percent formaldehyde, and 3-9 percent hydrocarbons. Several cars that were tested using gasoline emitted similar distributions of hydrocarbons, even through the vehicles represented a broad range of current and developmental engine families and emissions control systems

Characterizing Dissolved Gases in Cryogenic Liquid Fuels

Science.gov (United States)

Richardson, Ian A.

Pressure-Density-Temperature-Composition (PrhoT-x) measurements of cryogenic fuel mixtures are a historical challenge due to the difficulties of maintaining cryogenic temperatures and precision isolation of a mixture sample. For decades NASA has used helium to pressurize liquid hydrogen propellant tanks to maintain tank pressure and reduce boil off. This process causes helium gas to dissolve into liquid hydrogen creating a cryogenic mixture with thermodynamic properties that vary from pure liquid hydrogen. This can lead to inefficiencies in fuel storage and instabilities in fluid flow. As NASA plans for longer missions to Mars and beyond, small inefficiencies such as dissolved helium in liquid propellant become significant. Traditional NASA models are unable to account for dissolved helium due to a lack of fundamental property measurements necessary for the development of a mixture Equation Of State (EOS). The first PrhoT-x measurements of helium-hydrogen mixtures using a retrofitted single-sinker densimeter, magnetic suspension microbalance, and calibrated gas chromatograph are presented in this research. These measurements were used to develop the first multi-phase EOS for helium-hydrogen mixtures which was implemented into NASA's Generalized Fluid System Simulation Program (GFSSP) to determine the significance of mixture non-idealities. It was revealed that having dissolved helium in the propellant does not have a significant effect on the tank pressurization rate but does affect the rate at which the propellant temperature rises. PrhoT-x measurements are conducted on methane-ethane mixtures with dissolved nitrogen gas to simulate the conditions of the hydrocarbon seas of Saturn's moon Titan. Titan is the only known celestial body in the solar system besides Earth with stable liquid seas accessible on the surface. The PrhoT-x measurements are used to develop solubility models to aid in the design of the Titan Submarine. NASA is currently designing the submarine

Ionic Liquid-Liquid Chromatography: A New General Purpose Separation Methodology.

Science.gov (United States)

Brown, Leslie; Earle, Martyn J; Gîlea, Manuela A; Plechkova, Natalia V; Seddon, Kenneth R

2017-08-10

Ionic liquids can form biphasic solvent systems with many organic solvents and water, and these solvent systems can be used in liquid-liquid separations and countercurrent chromatography. The wide range of ionic liquids that can by synthesised, with specifically tailored properties, represents a new philosophy for the separation of organic, inorganic and bio-based materials. A customised countercurrent chromatograph has been designed and constructed specifically to allow the more viscous character of ionic liquid-based solvent systems to be used in a wide variety of separations (including transition metal salts, arenes, alkenes, alkanes, bio-oils and sugars).

Recovery of hydrocarbon oils

Energy Technology Data Exchange (ETDEWEB)

1941-02-10

A process is disclosed for recovery of hydrocarbon oils, especially lubricating oils or diesel oils, through pressure hydrogenation of distillation, extraction of hydrogenation products from coal or coaly materials or from oils such as mineral oils or tars in liquid phase by use in a reaction vessel of fixed-bed catalysts, characterized in that as starting material is employed material which has been freed of asphaltic and resinous material by hydrogenation refining, vacuum-steam distillation, treatment with hydrogen-rich hydrocarbons (hydroforming), or sulfuric acid.

Analysis of monoterpene hydrocarbons in rural atmospheres

International Nuclear Information System (INIS)

Holdren, M.W.; Westberg, H.H.; Zimmerman, P.R.

1979-01-01

Gas chromatographic/mass spectrometric analysis of monoterpenes from a rural forested site in the northwestern United States is described. Use of a glass capillary column provided excellent resolution of the hydrocarbons. Increased sensitivity and specificity of the mass spectrometer detector over the flame ionization detector were demonstrated for trace (parts per trillion) atmospheric hydrocarbons. As little as 10 ppt of compound was detectable in 100-cc air samples. Two analytical methods (cryogenic and solid adsorbent--Tenax-GC) were used in the collection of ambient air. Analytical results from the two techniques compared very well. Rural concentrations of the monoterpenes varied considerably depending upon location within the forest canopy. The concentration of individual species never exceeded 1 ppb of compound during a 10-month sampling period. The monoterpene total for all samples fell in the range of 0.5- to 16-ppb compound for C 10 terpene

Supercritical Fluid Chromatographic Separation of Dimethylpolysiloxane Polymer

Energy Technology Data Exchange (ETDEWEB)

Pyo, Dong Jin; Lim, Chang Hyun [Kangwon National University, Chuncheon (Korea, Republic of)

2005-02-15

Water was used as a polar modifier and a μ-porasil column as a saturator column. The μ-porasil column was inserted between the pump outlet and the injection valve. During the passage of the supercritical fluid mobile phase through the silica column, a polar modifier (water) can be dissolved in the pressurized supercritical fluid. Dimethylpolysiloxane polymer has been known as more polar polymer than polystyrene polymer. Dimethylpolysiloxane polymer has never been separated using water modified mobile phase. In this paper, using a μ-porasil column as a saturator column, excellent supercritical fluid chromatograms of dimethylpolysiloxane oligomers were obtained. The use of compressed (dense) gases and supercritical fluids as chromatographic mobile phases in conjunction with liquid chromatographic (LC)-type packed columns was first reported by Klesper et al. in 1962. During its relatively short history, supercritical fluid chromatography (SFC) has become an attractive alternative to GC and LC in certain industrially important applications. SFC gives the advantage of high efficiency and allows the analysis of nonvolatile or thermally labile mixtures.

Supercritical Fluid Chromatographic Separation of Dimethylpolysiloxane Polymer

International Nuclear Information System (INIS)

Pyo, Dong Jin; Lim, Chang Hyun

2005-01-01

Water was used as a polar modifier and a μ-porasil column as a saturator column. The μ-porasil column was inserted between the pump outlet and the injection valve. During the passage of the supercritical fluid mobile phase through the silica column, a polar modifier (water) can be dissolved in the pressurized supercritical fluid. Dimethylpolysiloxane polymer has been known as more polar polymer than polystyrene polymer. Dimethylpolysiloxane polymer has never been separated using water modified mobile phase. In this paper, using a μ-porasil column as a saturator column, excellent supercritical fluid chromatograms of dimethylpolysiloxane oligomers were obtained. The use of compressed (dense) gases and supercritical fluids as chromatographic mobile phases in conjunction with liquid chromatographic (LC)-type packed columns was first reported by Klesper et al. in 1962. During its relatively short history, supercritical fluid chromatography (SFC) has become an attractive alternative to GC and LC in certain industrially important applications. SFC gives the advantage of high efficiency and allows the analysis of nonvolatile or thermally labile mixtures

Multidimensional High-Resolution Gas Chromatographic Investigations of Hydrocarbon Fuels and Various Turbine Engine Fuel Precursors.

Science.gov (United States)

1985-08-01

time were spurious transits observed during the recording of the chromatographic output data. *Packaged gas purification filters supplied by Alltech ... Alltech ) that were needed for these unusual installations. When the column diameters were small and of comparable size, the assembly attach- ments at...into an MDGC system has definite advantages as separations can be made faster and with greater detectability. However, specific precautions must be

Effect of Ce2O3, La2O3 and ZnO additives on the oxygenates conversion into liquid hydrocarbons

Science.gov (United States)

Kachalov, V. V.; Lavrenov, V. A.; Lishchiner, I. I.; Malova, O. V.; Tarasov, A. L.; Zaichenko, V. M.

2018-01-01

A selective modifying effect of cerium, magnesium and zinc oxide additives on the activity and the selectivity of a pentasil group zeolite catalyst in the reaction of conversion of oxygenates (methanol and dimethyl ether) to liquid hydrocarbons was found. It was found that zinc oxide contributes to the stable operation of the zeolite catalyst in the conversion of oxygenates in the synthesis gas stream and leads to the production of gasolines with low durene content (not more than 6.1 wt%). The obtained results demonstrate the rationale for producing hydrocarbons from synthesis gas without the stage of oxygenate separation with their subsequent conversion to synthetic gasoline.

Flow measurement of liquid hydrocarbons with positive displacement meters: the correction for slippage

International Nuclear Information System (INIS)

García-Berrocal, Agustín; Montalvo, Cristina; Balbás, Miguel; Blázquez, Juan

2013-01-01

In the oil industry, the economical and fiscal impact of the measurements accuracy on the custody transfer operations implies fulfilling strict requirements of legal metrology. In this work, we focus on the positive displacement meters (PD meters) for refined liquid hydrocarbons. The state of the art of the lack of accuracy due to slippage flow in these meters is revised. The slippage flow due to the pressure drop across the device has been calculated analytically by applying the Navier–Stokes equation. No friction with any wall of the slippage channel has been neglected and a more accurate formula than the one found in the literature has been obtained. PD meters are calibrated against a bidirectional prover in order to obtain their meter factor which allows correction of their indications. Instead of the analytical model, an empirical one is proposed to explain the variation of the meter factor of the PD meters with flow rate and temperature for a certain hydrocarbon. The empirical model is based on the historical calibration data, of 9 years on average, of 25 m with four types of refined hydrocarbon. This model has been statistically validated by linear least-squares fitting. By using the model parameters, we can obtain the meter factor corresponding to different conditions of temperature and flow rate from the conditions in which the devices were calibrated. The flow parameter is such that a 10% flow rate variation implies a meter factor variation lower than 0.01%. A rule of thumb value for the temperature parameter is 0.005% per degree Celsius. The model residuals allow surveillance of the device drift and quantifying its contribution to the meter factor uncertainty. The observed drift is 0.09% at 95% confidence level in the analyzed population of meters. (paper)

Reliable Correlation for Liquid-Liquid Equilibria Outside the Critical Region

DEFF Research Database (Denmark)

Ruszczynski, Lukasz; Zubov, Alexandr; O’Connell, John P.

2017-01-01

, uncertainty analysis of regression results, obtained parameters, and predicted mole fractions has been formulated. The procedure is applied to three cases: hydrocarbons + water, ionic liquids + water, and nitroethane + hydrocarbons. The model has four parameters in the most basic formulation. Depending upon...

Validation of high-performance liquid chromatographic method for analysis of fluconazole in microemulsions and liquid crystals

Directory of Open Access Journals (Sweden)

Hilris Rocha e Silva

2014-04-01

Full Text Available In recent decades, there has been a significant increase in the incidence of fungal diseases. Certain fungal diseases cause cutaneous lesions and in the usual treatment, generally administred orally, the drug reaches the site of action with difficulty and its concentration is too low. An approach much explored in recent years is the development of nanotechnology-based drug delivery systems, and microemulsions (ME and liquid crystals (LC are promising. ME and LC were developed with oleic acid or copaiba oil as the oil phase, propoxyl (5OP ethoxyl (20 OE cetyl alcohol as surfactant and water. An analytical method to assess the incorporation of fluconazole (FLU in the systems under study was validated according to guidelines of the International Conference on Harmonization (ICH guidelines and the Brazilian Food, Drug and Sanitation Agency (ANVISA. The method was conducted on a C18-RP column (250 × 4.6 mm i.d., maintained at room temperature. The mobile phase consisted of acetonitrile and water (50:50, v/v, run at a flow rate of 1.0mL/min and using ultraviolet detection at 210nm. The chromatographic separation was obtained with a retention time of 6.3min, and was linear in the range of 20-400 µg/mL (r2=0.9999. The specificity showed no interference of the excipients. The accuracy was 100.76%. The limits of detection and quantitation were 0.057 and 0.172 µg.mL-1, respectively. Moreover, method validation demonstrated satisfactory results for precision and robustness. The proposed method was applied for the analysis of the incorporation of FLU in ME and LC, contributing to improve the quality control and to assure the therapeutic efficacy.

A simple high-performance liquid chromatographic method for the estimation of boswellic acids from the market formulations containing Boswellia serrata extract.

Science.gov (United States)

Shah, Shailesh A; Rathod, Ishwarsinh S; Suhagia, Bhanubhai N; Pandya, Saurabh S; Parmar, Vijay K

2008-09-01

A simple, rapid, and reproducible reverse-phase high-performance liquid chromatographic method is developed for the estimation of boswellic acids, the active constituents in Boswellia serrata oleo-gum resin. The chromatographic separation is performed using a mobile phase consisting of acetonitrile-water (90:10, % v/v) adjusted to pH 4 with glacial acetic acid on a Kromasil 100 C18 analytical column with flow rate of 2.0 mL/min and detection at 260 nm. The elution times are 4.30 and 7.11 min for 11-keto beta-boswellic acid (11-KBA) and 3-acetyl 11-keto beta-boswellic acid (A-11-KBA), respectively. The calibration curve is linear in the 11.66-58.30 microg/mL and 6.50-32.50 microg/mL range for 11-KBA and A-11-KBA, respectively. The limits of detection are 2.33 microg/mL and 1.30 microg/mL for 11-KBA and A-11-KBA, respectively. The mean recoveries are 98.24% to 104.17% and 94.12% to 105.92% for 11-KBA and A-11-KBA, respectively. The inter- and intra-day variation coefficients are less than 5%. The present method is successfully applied for the estimation of boswellic acids from the market formulations containing Boswellia serrata extract.

Coffee contains cholinomimetic compound distinct from caffeine. I: Purification and chromatographic analysis.

Science.gov (United States)

Tse, S Y

1991-07-01

Both regular and decaffeinated coffees were found to have cholinomimetic actions when tested in urethane-anesthetized rats. These actions were distinct from those of caffeine and reversible by atropine. The bioactive fraction was purified from alcoholic extracts of instant decaffeinated coffee by liquid column chromatography and preparative TLC. The purified compound showed similar pharmacological actions as the starting material. Chromatographic behavior was further characterized by analytical TLC and HPLC. Chromatographic analyses of extracts of green coffee beans and roasted ground coffees showed that the cardioactive compound was only present in roasted coffees. Similar analyses of other commonly consumed beverages, including teas and cocoa, showed that this compound was not present in beverages besides coffee.

Application of the cubic-plus-association (CPA) equation of state to complex mixtures with aromatic hydrocarbons

DEFF Research Database (Denmark)

Folas, Georgios; Kontogeorgis, Georgios; Michelsen, Michael Locht

2006-01-01

The cubic-plus-association (CPA) equation of state is applied to phase equilibria of mixtures containing alcohols, glycols, water, and aromatic or olefinic hydrocarbons. Previously, CPA has been successfully used for mixtures containing various associating compounds (alcohols, glycols, amines......, organic acids, and water) and aliphatic hydrocarbons. We show in this work that the model can be satisfactorily extended to complex vapor-liquid-liquid equilibria with aromatic or olefinic hydrocarbons. The solvation between aromatics/olefinics and polar compounds is accounted for. This is particularly...... important for mixtures containing water and glycols, but less so for mixtures with alcohols. For water/hydrocarbons, a single binary interaction parameter which accounts for the solvation is fitted to the experimental liquid-liquid equilibria (LLE) data. The interaction parameter of the physical term...

[Development of an automatic vacuum liquid chromatographic device and its application in the separation of the components from Schisandra chinensis (Turz) Baill].

Science.gov (United States)

Zhu, Jingbo; Liu, Baoyue; Shan, Shibo; Ding, Yanl; Kou, Zinong; Xiao, Wei

2015-08-01

In order to meet the needs of efficient purification of products from natural resources, this paper developed an automatic vacuum liquid chromatographic device (AUTO-VLC) and applied it to the component separation of petroleum ether extracts of Schisandra chinensis (Turcz) Baill. The device was comprised of a solvent system, a 10-position distribution valve, a 3-position changes valve, dynamic axis compress chromatographic columns with three diameters, and a 10-position fraction valve. The programmable logic controller (PLC) S7- 200 was adopted to realize the automatic control and monitoring of the mobile phase changing, column selection, separation time setting and fraction collection. The separation results showed that six fractions (S1-S6) of different chemical components from 100 g Schisandra chinensis (Turcz) Baill. petroleum ether phase were obtained by the AUTO-VLC with 150 mm diameter dynamic axis compress chromatographic column. A new method used for the VLC separation parameters screened by using multiple development TLC was developed and confirmed. The initial mobile phase of AUTO-VLC was selected by taking Rf of all the target compounds ranging from 0 to 0.45 for fist development on the TLC; gradient elution ratio was selected according to k value (the slope of the linear function of Rf value and development times on the TLC) and the resolution of target compounds; elution times (n) were calculated by the formula n ≈ ΔRf/k. A total of four compounds with the purity more than 85% and 13 other components were separated from S5 under the selected conditions for only 17 h. Therefore, the development of the automatic VLC and its method are significant to the automatic and systematic separation of traditional Chinese medicines.

An improved high-performance liquid chromatographic method for simultaneous determination of tocopherols, tocotrienols and γ-oryzanol in rice.

Science.gov (United States)

Huang, Shao-Hua; Ng, Lean-Teik

2011-07-22

An improved normal phase high performance liquid chromatographic (NP-HPLC) method was developed for simultaneous quantification of eight vitamin E isomers (α-, β-, γ- and δ-tocopherols and α-, β-, γ- and δ-tocotrienols) and γ-oryzanol in rice. A complete separation of all compounds was achieved within 25 min using an Inertsil CN-3, SIL-100A 5 μM (4.6 mm × 250 mm) column and an isocratic elution system of hexane/isopropanol/ethylacetate/acetic acid (97.6:0.8:0.8:0.8, v/v/v/v) at a flow rate varying from 0.7 to 1.5 mL min(-1). A linear correlation coefficient (r(2)>0.99) and high reproducibility were obtained at concentrations ranging 0.05-10 μg mL(-1) for vitamin E isomers and 0.5-500 μg mL(-1) for γ-oryzanol. This method proved to be rapid, accurate and reproducible. Copyright © 2011 Elsevier B.V. All rights reserved.

Chromatographic separation of radioactive noble gases from xenon

Science.gov (United States)

Akerib, D. S.; Araújo, H. M.; Bai, X.; Bailey, A. J.; Balajthy, J.; Beltrame, P.; Bernard, E. P.; Bernstein, A.; Biesiadzinski, T. P.; Boulton, E. M.; Bramante, R.; Cahn, S. B.; Carmona-Benitez, M. C.; Chan, C.; Chiller, A. A.; Chiller, C.; Coffey, T.; Currie, A.; Cutter, J. E.; Davison, T. J. R.; Dobi, A.; Dobson, J. E. Y.; Druszkiewicz, E.; Edwards, B. N.; Faham, C. H.; Fiorucci, S.; Gaitskell, R. J.; Gehman, V. M.; Ghag, C.; Gibson, K. R.; Gilchriese, M. G. D.; Hall, C. R.; Hanhardt, M.; Haselschwardt, S. J.; Hertel, S. A.; Hogan, D. P.; Horn, M.; Huang, D. Q.; Ignarra, C. M.; Ihm, M.; Jacobsen, R. G.; Ji, W.; Kamdin, K.; Kazkaz, K.; Khaitan, D.; Knoche, R.; Larsen, N. A.; Lee, C.; Lenardo, B. G.; Lesko, K. T.; Lindote, A.; Lopes, M. I.; Manalaysay, A.; Mannino, R. L.; Marzioni, M. F.; McKinsey, D. N.; Mei, D.-M.; Mock, J.; Moongweluwan, M.; Morad, J. A.; Murphy, A. St. J.; Nehrkorn, C.; Nelson, H. N.; Neves, F.; O'Sullivan, K.; Oliver-Mallory, K. C.; Palladino, K. J.; Pease, E. K.; Pech, K.; Phelps, P.; Reichhart, L.; Rhyne, C.; Shaw, S.; Shutt, T. A.; Silva, C.; Solovov, V. N.; Sorensen, P.; Stephenson, S.; Sumner, T. J.; Szydagis, M.; Taylor, D. J.; Taylor, W.; Tennyson, B. P.; Terman, P. A.; Tiedt, D. R.; To, W. H.; Tripathi, M.; Tvrznikova, L.; Uvarov, S.; Verbus, J. R.; Webb, R. C.; White, J. T.; Whitis, T. J.; Witherell, M. S.; Wolfs, F. L. H.; Yazdani, K.; Young, S. K.; Zhang, C.

2018-01-01

The Large Underground Xenon (LUX) experiment operates at the Sanford Underground Research Facility to detect nuclear recoils from the hypothetical Weakly Interacting Massive Particles (WIMPs) on a liquid xenon target. Liquid xenon typically contains trace amounts of the noble radioactive isotopes 85Kr and 39Ar that are not removed by the in situ gas purification system. The decays of these isotopes at concentrations typical of research-grade xenon would be a dominant background for a WIMP search experiment. To remove these impurities from the liquid xenon, a chromatographic separation system based on adsorption on activated charcoal was built. 400 kg of xenon was processed, reducing the average concentration of krypton from 130 ppb to 3.5 ppt as measured by a cold-trap assisted mass spectroscopy system. A 50 kg batch spiked to 0.001 g/g of krypton was processed twice and reduced to an upper limit of 0.2 ppt.

Evaluation of the phase ratio for three C18 high performance liquid chromatographic columns.

Science.gov (United States)

Caiali, Edvin; David, Victor; Aboul-Enein, Hassan Y; Moldoveanu, Serban C

2016-02-26

For a chromatographic column, phase ratio Φ is defined as the ratio between the volume of the stationary phase Vst and the void volume of the column V0, and it is an important parameter characterizing the HPLC process. Although apparently simple, the evaluation of Φ presents difficulties because there is no sharp boundary between the mobile phase and the stationary phase. In addition, the boundary depends not only on the nature of the stationary phase, but also on the composition of the mobile phase. In spite of its importance, phase ratio is seldom reported for commercially available HPLC columns and the data typically provided by the vendors about the columns do not provide key information that would allow the calculation of Φ based on Vst and V0 values. A different procedure for the evaluation of Φ is based on the following formula: log k'j=a log Kow,j+log Φ, where k'j is the retention factor for a compound j that must be a hydrocarbon, Kow,j is the octanol/water partition coefficient, and a is a proportionality constant. Present study describes the experimental evaluation of Φ based on the measurement of k'j for the compounds in the homologous series between benzene and butylbenzene for three C18 columns: Gemini C18, Luna C18 both with 5 μm particles, and a Chromolith Performance RP-18. The evaluation was performed for two mobile phase systems at different proportions of methanol/water and acetonitrile/water. The octanol/water partition coefficients were obtained from the literature. The results obtained in the study provide further support for the new procedure for the evaluation of phase ratio. Copyright © 2016 Elsevier B.V. All rights reserved.

Surface-bonded ionic liquid stationary phases in high-performance liquid chromatography--a review.

Science.gov (United States)

Pino, Verónica; Afonso, Ana M

2012-02-10

Ionic liquids (ILs) are a class of ionic, nonmolecular solvents which remain in liquid state at temperatures below 100°C. ILs possess a variety of properties including low to negligible vapor pressure, high thermal stability, miscibility with water or a variety of organic solvents, and variable viscosity. IL-modified silica as novel high-performance liquid chromatography (HPLC) stationary phases have attracted considerable attention for their differential behavior and low free-silanol activity. Indeed, around 21 surface-confined ionic liquids (SCIL) stationary phases have been developed in the last six years. Their chromatographic behavior has been studied, and, despite the presence of a positive charge on the stationary phase, they showed considerable promise for the separation of neutral solutes (not only basic analytes), when operated in reversed phase mode. This aspect points to the potential for truly multimodal stationary phases. This review attempts to summarize the state-of-the-art about SCIL phases including their preparation, chromatographic behavior, and analytical performance. Copyright © 2011 Elsevier B.V. All rights reserved.

Separation of benzene from alkanes using 1-ethyl-3-methylpyridinium ethylsulfate ionic liquid at several temperatures and atmospheric pressure: Effect of the size of the aliphatic hydrocarbons

International Nuclear Information System (INIS)

Gonzalez, Emilio J.; Calvar, Noelia; Gomez, Elena; Dominguez, Angeles

2010-01-01

The ionic liquid 1-ethyl-3-methylpyridinium ethylsulfate, [EMpy][ESO 4 ], was studied for the separation of benzene from aliphatic hydrocarbons (octane or nonane) by solvent extraction through the determination of the (liquid + liquid) equilibrium (LLE) of the ternary systems: {octane (1) + benzene (2) + [EMpy][ESO 4 ] (3)} and {nonane (1) + benzene (2) + [EMpy][ESO 4 ] (3)} at T = (283.15 and 298.15) K and atmospheric pressure. Binodal curves were determined using the 'cloud point' method, and tie-line compositions were obtained by density measurements. The values of selectivity and distribution coefficient, derived from the tie-line data, were used to decide if this ionic liquid can be used as potential solvent for the separation of benzene from aliphatic hydrocarbons using liquid extraction. These results were analyzed and compared to those previously reported for the systems {hexane + benzene + [EMpy][ESO 4 ]} and {heptane + benzene + [EMpy][ESO 4 ]}. The experimental results show that this ionic liquid is suitable for the extraction of benzene from mixtures containing octane and nonane. The consistency of tie-line data was ascertained by applying the Othmer-Tobias and Hand equations. The experimental results for the ternary systems were well correlated with the NRTL model. No literature data were found for the mixtures discussed in this paper.

Peak distortion in the column liquid chromatographic determination of omeprazole dissolved in borax buffer.

Science.gov (United States)

Arvidsson, T; Collijn, E; Tivert, A M; Rosén, L

1991-11-22

Injection of a sample containing omeprazole dissolved in borax buffer (pH 9.2) into a reversed-phase liquid chromatographic system consisting of a mixture of acetonitrile and phosphate buffer (pH 7.6) as the mobile phase and a C18 surface-modified silica as the solid phase resulted under special conditions in split peaks of omeprazole. The degree of peak split and the retention time of omeprazole varied with the concentration of borax in the sample solution and the ionic strength of the mobile phase buffer as well as with the column used. Borax is eluted from the column in a broad zone starting from the void volume of the column. The retention is probably due to the presence of polyborate ions. The size of the zone varies with the concentration of borax in the sample injected. In the borax zone the pH is increased compared with the pH of the mobile phase, and when omeprazole (a weak acid) is co-eluting in the borax zone its retention is affected. In the front part and in the back part of the borax zone, pH gradients are formed, and these gradients can induce the peak splitting. When the dissolving medium is changed to a phosphate buffer or an ammonium buffer at pH 9 no peak distortion of omeprazole is observed.

Liquid chromatographic determination of oxytetracycline in edible fish fillets from six species of fish

Science.gov (United States)

Meinertz, J.R.; Stehly, G.R.; Gingerich, W.H.

1998-01-01

The approved use of oxytetracycline (OTC) in U.S. Aquaculture is limited to specific diseases in salmonids and channel catfish. OTC may also be effective in controlling diseases in other fish species important to public aquaculture, but before approved use of OTC can be augmented, an analytical method for determining OTC in fillet tissue from multiple species of fish will be required to support residue depletion studies. The objective of this study was to develop and validate a liquid chromatographic (LC) method that is accurate, precise, and sensitive for OTC in edible fillets from multiple species of fish. Homogenized fillet tissues from walleye, Atlantic salmon, striped bass, white sturgeon, rainbow trout, and channel catfish were fortified with OTC at nominal concentrations of 10, 20, 100, 1000, and 5000 ng/g. In tissues fortified with OTC at 100, 1000, and 5000 ng/g, mean recoveries ranged from 83 to 90%, and relative standard deviations (RSDs) ranged from 0.9 to 5.8%. In all other tissues, mean recoveries ranged from 59 to 98%, and RSDs ranged from 3.3 to 20%. Method quantitation limits ranged from 6 to 22 ng/g for the 6 species. The LC parameters produced easily integratable OTC peaks without coelution of endogenous compounds. The method is accurate, precise, and sensitive for OTC in fillet tissue from 6 species of fish from 5 phylogenetically diverse groups.

Study of stationary phase stability from a column with chromatographic material for steady state treatment of an effluent and/or waste containing Th-232

International Nuclear Information System (INIS)

Felinto, Maria Claudia Franca da Cunha; Martinz, Daniel Ortiz

1999-01-01

This work relates the behavior of a new chromatographic material, AMBERCMPO I, that has been studied to remove actinide elements from the High Level Liquid Waste. It gives emphasis to the behavior of chromatographic materials to the extraction of Th 4+ and its performance after some operation cycle. (author)

Distribution of volatile liquid hydrocarbons in the vicinity of power/desalination plants in Kuwait

International Nuclear Information System (INIS)

Saeed, T.; Khordagui, H; AI-Bloushi, A.

1999-01-01

Volatile liquid hydrocarbons (VLHs) represent some 40% of crude oil and are considered to be the most toxic compounds of petroleum other than the carcinogenic polycyclic aromatic hydrocarbons. The distribution of these compounds in Kuwait's coastal waters in the vicinity and at the inlets of power plants was assessed. About 200 samples were collected from selected sampling stations over the four seasons. The VLHs in the samples were concentrated using Grob's closed-loop technique and analysed by GC using FID and confirmed by GC/MS. The results showed that VLHs were ubiquitous in the coastal water of Kuwait. The detected levels (ranged from 307 to 7882 ng/l in Kuwait Bay and from 331 to 5017 ng/l in the south) were comparable to the levels found in other parts of the world and were not alarming. However, the spotty higher levels encountered gave reason for some concern. Benzenoids (originating from petroleum) predominated, representing roughly 70% of the total VLHs. The levels were relatively low at the intake of the power plant located in the Kuwait Bay (annual average 677 ng/l) while higher levels (annual average 3006 ng/l) were encountered at the intake of the plant located at the south of oil the loading terminals and refineries. (author)

Production of hydrocarbons of value

Energy Technology Data Exchange (ETDEWEB)

1931-06-16

A process is described for the production of hydrocarbons of great value by treating with heat and pressure carbonaceous materials such as coals, tars, mineral oils, and products of distillation and transformation of these materials, also for the refining with heat and pressure of mixed liquid hydrocarbons by means of hydrogen gas, preferably in the presence of catalysts, consisting in using as the hydrogenating gas that obtained by gasification of combustible solids after partial or complete cleaning at atmospheric or elevated pressures, by means of solid adsorbents, chemical agents or catalysts, or mixtures of these agents, the hydrocarbons being characterized by strong unsaturation, and the presence of oxygen, sulfur compounds, and oxides of nitrogen.

Process for desulfurizing hydrocarbons

Energy Technology Data Exchange (ETDEWEB)

1937-04-12

A process is described for the desulfurization of a mixture of hydrocarbons, and in particular hydrocarbons containing less than 7 atoms of carbon and sulfur compounds of the type of sulfur carbonyl, characterized by the fact that the mixture, preferably in the liquid phase, is brought in contact with a solution of caustic alkali, essentially anhydrous or preferably with a solution of alkali hydroxide in an organic hydroxy nonacid solvent, for example, an alcohol, or with an alkaline alcoholate, under conditions suitable to the formation of hydrogen sulfide which produces a hydrocarbon mixture free from sulfur compounds of the sulfur carbonyl type but containing hydrogen sulfide, and that it is treated, following mixing, having beem submitted to the first treatment, by means of aqueous alkaline hydroxide to eliminate the hydrogen sulfide.

Unconventional hydrocarbons. New prospects for the para-petroleum industry

International Nuclear Information System (INIS)

Bennaceur, Kamel

2011-01-01

Unconventional hydrocarbons represent a significant potential despite complications in extracting them. The International Energy Agency's annual report in 2008 estimated that 9 trillion barrels of liquid hydrocarbons could be produced - a figure to be compared with the current production of 1,1 trillion barrels and the 1,3-1,4 trillion barrels of proven reserves. This estimate includes the potential production from heavy oils, shale oil and tar belts as well as the liquid hydrocarbons obtained by converting coal and natural gas. The IAE's 2009 report estimates resources in gas at more than 850 trillion cubic meters (T m"3), as compared with the 80 T m"3 now being produced and the 187 T m"3 of proven reserves

A modified free-volume-based model for predicting vapor-liquid and solid-liquid equilibria for size asymmetric systems

DEFF Research Database (Denmark)

Radfarnia, H.R.; Ghotbi, C.; Taghikhani, V.

2005-01-01

The main purpose of this work is to present a free-volume combinatorial term in predicting vapor-liquid equilibrium (VLE) and solid-liquid equilibrium (SLE) of polymer/solvent and light and heavy hydrocarbon/hydrocarbon mixtures. The proposed term is based on a modification of the original Freed ...

Waste Plastic Converting into Hydrocarbon Fuel Materials

Energy Technology Data Exchange (ETDEWEB)

Sarker, Moinuddin; Mamunor Rashid, Mohammad; Molla, Mohammad

2010-09-15

The increased demand and high prices for energy sources are driving efforts to convert organic compounds into useful hydrocarbon fuels. Although much of this work has focused on biomass, there are strong benefits to deriving fuels from waste plastic material. Natural State Research Inc. (NSR) has invented a simple and economically viable process to decompose the hydrocarbon polymers of waste plastic into the shorter chain hydrocarbon of liquid fuel (patent pending). The method and principle of the production / process will be discussed. Initial tests with several widely used polymers indicate a high potential for commercialization.

Decontamination of hydrocarbon contaminated soil

International Nuclear Information System (INIS)

Smith, A.J.

1991-01-01

This patent describes the method of treating hydrocarbon contaminated soil. It comprises forming the soil into a flowing particulate stream, forming an aqueous liquid mixture of water and treating substance that reacts with hydrocarbon to form CO 2 and water, dispersing the liquid mixture into the particulate soil stream to wet the particulate, allowing the substance to react with the wetted soil particulate to thereby form CO 2 and water, thereby the resultant soil is beneficially treated, the stream being freely projected to dwell at a level and then fall, and the dispersing includes spraying the liquid mixture into the projected stream at the dwell, the substance consisting of natural bacteria, and at a concentration level in the mixture of between 100 to 3,000 PPM of bacteria to water, the soil forming step including impacting the soil to reduce it to particles less than about 1 inches in cross dimension, and including forming the wetting particulate into a first layer on a surface to allow the substance to react

Modified Dispersive Liquid-Liquid Micro Extraction Using Green Solvent for Determination of Polycyclic Aromatic Hydrocarbons (PAHs) in Vegetable Samples

International Nuclear Information System (INIS)

Kin, C.M.; Shing, W.L.

2016-01-01

According to International Agency for Research on Cancer (IARC), most of Polycyclic Aromatic Hydrocarbons (PAHs) known as genotoxic human carcinogen and mutagenic. PAHs represent as poorly degradable pollutants that exist in soils, sediments, surface water and atmosphere. A simple, rapid and sensitive extraction method termed modified Dispersive Liquid-Liquid Micro extraction (DLLME) using green solvent was developed to determine PAHs in vegetable samples namely radish, cabbage and cucumber prior to Gas Chromatography Flame Ionization Detection (GC-FID). The extraction method is based on replacing chlorinated organic extraction solvent in the conventional DLLME with low toxic solvent, 1-bromo-3-methylbutane without using dispersive solvent. Several experimental factors such as type and volume of extraction solvents, extraction time, confirmation of 12 PAHs by GC-MS, recovery percentages on vegetable samples and the comparative analysis with conventional DLLME were carried out. Both DLLME were successfully extracted 12 types of PAHs. In modified DLLME, the recoveries of the analytes obtained were in a range of 72.72 - 88.07 % with RSD value below 7.5 % which is comparable to the conventional DLLME. The use of microliter of low toxic extraction solvent without addition of dispersive solvent caused the method is economic and environmental friendly which is fulfill the current requirement, green chemistry based analytical method. (author)

Application of fission track analysis to hydrocarbon exploration

International Nuclear Information System (INIS)

Duddy, I.R.; Green, P.F.; Gleadow, A.J.W.; Marshallsea, S.; Tingate, P.; Laslett, G.M.; Hegarty, K.A.; Lovering, J.F.

1985-01-01

The temperature range over which fission tracks in apatite show observable annealing effects coincides with that responsible for the maximum generation of liquid hydrocarbons. Work is currently in progress in a number of Australian and overseas sedimentary basins, applying Apatite Fission Track Analysis (AFTA) to investigate the thermal evolution of these hydrocarbon prospective regions

Determination of C6-C10 aromatic hydrocarbons in water by purge-and-trap capillary gas chromatography

Science.gov (United States)

Eganhouse, R.P.; Dorsey, T.F.; Phinney, C.S.; Westcott, A.M.

1993-01-01

A method is described for the determination of the C6-C10 aromatic hydrocarbons in water based on purge-and-trap capillary gas chromatography with flame ionization and mass spectrometric detection. Retention time data and 70 eV mass spectra were obtained for benzene and all 35 C7-C10 aromatic hydrocarbons. With optimized chromatographic conditions and mass spectrometric detection, benzene and 33 of the 35 alkylbenzenes can be identified and measured in a 45-min run. Use of a flame ionization detector permits the simultaneous determination of benzene and 26 alkylbenzenes.

The high pressure liquid chromatography and its application to the separation of polynuclear aromatic hydrocarbons in atmospheric dust and burning residues

International Nuclear Information System (INIS)

Lopez, M.-C.

1975-09-01

A new technique of analysis is described: the high speed liquid chromatography or more exactly the high performance liquid chromatography because of the progress achieved on the new packings of the columns. The main types of chromatography, according to the phenomena involved are described: adsorption, partition, ion-exchange and exclusion chromatography. A brief outline is given of the theory for determination of stationary and mobile phases in order to obtain the optimum conditions of separation. Some exemples of possible applications are given, particularly the use of this technique for the separation of polycyclic aromatic hydrocarbons in atmospheric pollution and burning residues [fr

Development of gas chromatography-flame ionization detection system with a single column and liquid nitrogen-free for measuring atmospheric C2-C12 hydrocarbons.

Science.gov (United States)

Liu, Chengtang; Mu, Yujing; Zhang, Chenglong; Zhang, Zhibo; Zhang, Yuanyuan; Liu, Junfeng; Sheng, Jiujiang; Quan, Jiannong

2016-01-04

A liquid nitrogen-free GC-FID system equipped with a single column has been developed for measuring atmospheric C2-C12 hydrocarbons. The system is consisted of a cooling unit, a sampling unit and a separation unit. The cooling unit is used to meet the temperature needs of the sampling unit and the separation unit. The sampling unit includes a dehydration tube and an enrichment tube. No breakthrough of the hydrocarbons was detected when the temperature of the enrichment tube was kept at -90 °C and sampling volume was 400 mL. The separation unit is a small round oven attached on the cooling column. A single capillary column (OV-1, 30 m × 0.32 mm I.D.) was used to separate the hydrocarbons. An optimal program temperature (-60 ∼ 170 °C) of the oven was achieved to efficiently separate C2-C12 hydrocarbons. There were good linear correlations (R(2)=0.993-0.999) between the signals of the hydrocarbons and the enrichment amount of hydrocarbons, and the relative standard deviation (RSD) was less than 5%, and the method detection limits (MDLs) for the hydrocarbons were in the range of 0.02-0.10 ppbv for sampling volume of 400 mL. Field measurements were also conducted and more than 50 hydrocarbons from C2 to C12 were detected in Beijing city. Copyright © 2015 Elsevier B.V. All rights reserved.

A method of refining aromatic hydrocarbons from coal chemical production

Energy Technology Data Exchange (ETDEWEB)

Zieborak, K.; Koprowski, A.; Ratajczak, W.

1979-10-01

A method is disclosed for refining aromatic hydrocarbons of coal chemical production by contact of liquid aromatic hydrocarbons and their mixtures with a strongly acid macroporous sulfocationite in the H-form at atmospheric pressure and high temperature. The method is distinguished in that the aromatic hydrocarbons and their mixtures, from which alkali compounds have already been removed, are supplied for refinement with the sulfocationite with simultaneous addition of olefin derivatives of aromatic hydrocarbons, followed by separation of pure hydrocarbons by rectification. Styrene or alpha-methylstyrene is used as the olefin derivatives of the aromatic hydrocarbons. The method is performed in several stages with addition of olefin derivatives of aromatic hydrocarbons at each stage.

National Gas Survey. Synthesized gaseous hydrocarbon fuels

Energy Technology Data Exchange (ETDEWEB)

None

1978-06-01

The supply-Technical Advisory Task Force-Synthesized Gaseous Hydrocarbon Fuels considered coal, hydrocarbon liquids, oil shales, tar sands, and bioconvertible materials as potential feedstocks for gaseous fuels. Current status of process technology for each feedstock was reviewed, economic evaluations including sensitivity analysis were made, and constraints for establishment of a synthesized gaseous hydrocarbon fuels industry considered. Process technology is presently available to manufacture gaseous hydrocarbon fuels from each of the feedstocks. In 1975 there were eleven liquid feedstock SNG plants in the United States having a capacity of 1.1 billion SCFD. There can be no contribution of SNG before 1982 from plants using feedstocks other than liquids because there are no plants in operation or under construction as of 1977. Costs for SNG are higher than current regulated prices for U.S. natural gas. Because of large reserves, coal is a prime feedstock candidate although there are major constraints in the area of coal leases, mining and water permits, and others. Commercial technology is available and several new gasification processes are under development. Oil shale is also a feedstock in large supply and commercial process technology is available. There are siting and permit constraints, and water availability may limit the ultimate size of an oil shale processing industry. Under projected conditions, bioconvertible materials are not expected to support the production of large quantities of pipeline quality gas during the next decade. Production of low or medium Btu gas from municipal solid wastes can be expected to be developed in urban areas in conjunction with savings in disposal costs. In the economic evaluations presented, the most significant factor for liquid feedstock plants is the anticipated cost of feedstock and fuel. The economic viability of plants using other feedstocks is primarily dependent upon capital requirements.

Gas chromatographic isolation technique for compound-specific radiocarbon analysis

International Nuclear Information System (INIS)

Uchida, M.; Kumamoto, Y.; Shibata, Y.; Yoneda, M.; Morita, M.; Kawamura, K.

2002-01-01

Full text: We present here a gas chromatographic isolation technique for the compound-specific radiocarbon analysis of biomarkers from the marine sediments. The biomarkers of fatty acids, hydrocarbon and sterols were isolated with enough amount for radiocarbon analysis using a preparative capillary gas chromatograph (PCGC) system. The PCGC systems used here is composed of an HP 6890 GC with FID, a cooled injection system (CIS, Gerstel, Germany), a zero-dead-volume effluent splitter, and a cryogenic preparative collection device (PFC, Gerstel). For AMS analysis, we need to separate and recover sufficient quantity of target individual compounds (>50 μgC). Yields of target compounds from C 14 n-alkanes to C 40 to C 30 n-alkanes and approximately that of 80% for higher molecular weights compounds more than C 30 n-alkanes. Compound specific radiocarbon analysis of organic compounds, as well as compound-specific stable isotope analysis, provide valuable information on the origins and carbon cycling in marine system. Above PCGC conditions, we applied compound-specific radiocarbon analysis to the marine sediments from western north Pacific, which showed the possibility of a useful chronology tool for estimating the age of sediment using organic matter in paleoceanographic study, in the area where enough amounts of planktonic foraminifera for radiocarbon analysis by accelerator mass spectrometry (AMS) are difficult to obtain due to dissolution of calcium carbonate. (author)

Process of distilling heavy hydrocarbons

Energy Technology Data Exchange (ETDEWEB)

1929-12-03

This invention has for its object the distillation of heavy liquid hydrocarbons for the purpose of obtaining lighter hydrocarbons stable and immediately salable for fuels in combustion motors. The process is distinguished by the fact that the heavy hydrocarbon is distilled by means of heating to a temperature in keeping with the nature of the material to be treated up to 350/sup 0/C under pressure or without pressure the distillation being carried out on catalysts containing successively nickel, copper, and iron (3 parts of nickel, 1 part of copper, and 1 part of iron), the vapors produced by this distillation being exposed in turn to the action of catalysts of the same nature and in the same proportion.

Determination of biologically active phenols and polyphenols in various objects by chromatographic techniques

International Nuclear Information System (INIS)

Kochetova, M V; Semenistaya, E N; Larionov, Oleg G; Revina, A A

2007-01-01

Chromatographic techniques for determination of biologically active phenols and polyphenols are considered. Various methods for sample preparation and detection are compared. The advantages of high performance liquid chromatography with spectrophotometric detection for determination of antioxidants are demonstrated. Data on determination of biologically active phenols and polyphenols published in the period from 1995 to 2005 are analysed.

The gas-chromatographic and gas-chromatographic-mass-spectrometric identification of halogen-containing organic compounds

Science.gov (United States)

Gidaspov, B. V.; Zenkevich, I. G.; Rodin, A. A.

1989-09-01

The problem of identifying halogen-containing organic compounds in their gas-chromatographic and gas-chromatographic-mass-spectrometric (GC-MS) determination in different materials has been examined. Particular attention has been paid not to the complete characterisation of methods for carrying out this analysis but to the most important problem of increasing the selectivity at the stages of sampling, separation, and interpretation of the gas-chromatographic and GC-MS information. The bibliography contains 292 references.

Sheath liquid interface for the coupling of normal-phase liquid chromatography with electrospray mass spectrometry and its application to the analysis of neoflavonoids.

Science.gov (United States)

Charles, Laurence; Laure, Frédéric; Raharivelomanana, Phila; Bianchini, Jean-Pierre

2005-01-01

A novel interface that allows normal-phase liquid chromatography to be coupled with electrospray ionization (ESI) is reported. A make-up solution of 60 mM ammonium acetate in methanol, infused at a 5 microl min(-1) flow-rate at the tip of the electrospray probe, provides a sheath liquid which is poorly miscible with the chromatographic effluent, but promotes efficient ionization of the targeted analytes. Protonated molecules generated in the ESI source were subjected to tandem mass spectrometric experiments in a triple-quadrupole mass spectrometer. The main fragmentation reactions were characterized for each analyte and specific mass spectral transitions were used to acquire chromatographic data in the multiple reaction monitoring detection mode. Results obtained during optimization of the sheath liquid composition and flow-rate suggest that the electrospray process was mainly under the control of the make-up solution, and that it forms an external charged layer around a neutral chromatographic mobile phase core. This sheath liquid interface was implemented for the analysis of some neoflavonoid compounds and its performance was evaluated. Limits of detection were established for calophillolide, inophyllum B, inophyllum P and inophyllum C at 100, 25, 15 and 100 ng ml(-1), respectively.

Flow injection gas chromatography with sulfur chemiluminescence detection for the analysis of total sulfur in complex hydrocarbon matrixes.

Science.gov (United States)

Hua, Yujuan; Hawryluk, Myron; Gras, Ronda; Shearer, Randall; Luong, Jim

2018-01-01

A fast and reliable analytical technique for the determination of total sulfur levels in complex hydrocarbon matrices is introduced. The method employed flow injection technique using a gas chromatograph as a sample introduction device and a gas phase dual-plasma sulfur chemiluminescence detector for sulfur quantification. Using the technique described, total sulfur measurement in challenging hydrocarbon matrices can be achieved in less than 10 s with sample-to-sample time ideal for fast analysis or trace sulfur analysis. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Chromatographic background drift correction coupled with parallel factor analysis to resolve coelution problems in three-dimensional chromatographic data: quantification of eleven antibiotics in tap water samples by high-performance liquid chromatography coupled with a diode array detector.

Science.gov (United States)

Yu, Yong-Jie; Wu, Hai-Long; Fu, Hai-Yan; Zhao, Juan; Li, Yuan-Na; Li, Shu-Fang; Kang, Chao; Yu, Ru-Qin

2013-08-09

Chromatographic background drift correction has been an important field of research in chromatographic analysis. In the present work, orthogonal spectral space projection for background drift correction of three-dimensional chromatographic data was described in detail and combined with parallel factor analysis (PARAFAC) to resolve overlapped chromatographic peaks and obtain the second-order advantage. This strategy was verified by simulated chromatographic data and afforded significant improvement in quantitative results. Finally, this strategy was successfully utilized to quantify eleven antibiotics in tap water samples. Compared with the traditional methodology of introducing excessive factors for the PARAFAC model to eliminate the effect of background drift, clear improvement in the quantitative performance of PARAFAC was observed after background drift correction by orthogonal spectral space projection. Copyright © 2013 Elsevier B.V. All rights reserved.

The chromatographic behavior of arsenic compounds on anion exchange columns with binary organic acids as mobile phases

Energy Technology Data Exchange (ETDEWEB)

Zheng, J.; Goessler, W.; Kosmus, W. [Graz Univ. (Austria). Inst. fuer Analytische Chemie

1998-03-01

Identification and quantification of arsenic compounds was performed with high-performance liquid chromatography (HPLC) and flame atomic absorption spectrometry (FAAS) as element-specific detector. Arsenous acid, methylarsonic acid, dimethylarsinic acid, arsenic acid, arsenobetaine, and arsenocholine were separated on two anion-exchange columns (Synchropak Q 300 and PRP-X 100) with different binary organic acids as mobile phases. The influence of chromatographic parameters, such as pH and the concentration of the mobile phase were investigated. An unusual chromatographic behavior of arsenous acid was observed when tartaric acid was used as mobile phase. (orig.)

A new equation of correction of the specific volume of the hydrocarbons C1 to C8 liquids for the equation of state of Peng-Robinson

International Nuclear Information System (INIS)

Hoyos Madrigal, Bibian

2000-01-01

A new generalized correction equation for specific volume of hydrocarbon pure liquids is proposed. Which can be used in a wide temperature range and that do not require additional parameters for each substance. The equation was developed for the normal hydrocarbon series from methane to octane and the obtained results applied to other substances are analysed. A comparison is also made with the equation proposed by Peneloux et al. (1982) resulting. In all cases, in a better performance of the equation proposed in this work

Improved stochastic resonance algorithm for enhancement of signal-to-noise ratio of high-performance liquid chromatographic signal

International Nuclear Information System (INIS)

Xie Shaofei; Xiang Bingren; Deng Haishan; Xiang Suyun; Lu Jun

2007-01-01

Based on the theory of stochastic resonance, an improved stochastic resonance algorithm with a new criterion for optimizing system parameters to enhance signal-to-noise ratio (SNR) of HPLC/UV chromatographic signal for trace analysis was presented in this study. Compared with the conventional criterion in stochastic resonance, the proposed one can ensure satisfactory SNR as well as good peak shape of chromatographic peak in output signal. Application of the criterion to experimental weak signals of HPLC/UV was investigated and the results showed an excellent quantitative relationship between different concentrations and responses

Stability-indicating liquid chromatographic method for quantification of new anti-epileptic drug lacosamide in bulk and pharmaceutical formulation

Directory of Open Access Journals (Sweden)

Chhalotiya Usmangani K.

2012-01-01

Full Text Available An isocratic stability indicating reversed-phase liquid chromatographic determination was developed for the quantitative determination of lacosamide in the pharmaceutical dosage form. A Hypersil C-18, 4.5μm column with mobile phase containing acetonitrile-water (20:80, v/v was used. The flow rate was 1.0 mL min-1 and effluents were monitored at 258 nm. The retention time of lacosamide was 8.9 min. The method was found to be linear in the concentration range of 5-100 μg/ml and the recovery was found to be in the range of 99.15 - 100.09 %. The limit of detection and limit of quantification were found to be 2 μg/ml and 5 μg/ml, respectively. Lacosamide stock solutions were subjected to acid and alkali hydrolysis, chemical oxidation and dry heat degradation. The drug was found to be stable to the dry heat and acidic condition attempted. The proposed method was validated and successfully applied to the estimation of lacosamide in tablet dosage forms.

Ultra-performance liquid chromatographic determination of L-ergothioneine in commercially available classes of cow milk.

Science.gov (United States)

Sotgia, Salvatore; Pisanu, Elisabetta; Cambedda, Debora; Pintus, Gianfranco; Carru, Ciriaco; Zinellu, Angelo

2014-09-01

A new efficient and sensitive precolumn hydrophilic interaction ultra-performance liquid chromatography (HILIC-UPLC) method was established for the quantitative determination of L-ergothioneine (ERT) in milk. After derivatization of ERT with 7-diethylamino-3-[4-(iodoacetamido)phenyl]-4-methylcoumarin, chromatographic separation was achieved in a fairly short time, less than 5 min, on a 100 × 2.1 mm Waters Cortecs UPLC HILIC 1.6-μm column, by using a mixture of 30 mmol/L ammonium acetate/acetonitrile (10:90, v/v) as a mobile phase flowing isocratically at 0.9 mL/min. Limit of detection and the limit of quantification were 0.03 and 0.10 μmol/L, respectively. The method exhibited linearity in a concentration range of 0.16 and 5.08 μmol/L. Mean recovery was 106.66%, whereas intra- and interassay precisions were determined to be within 6 RSD%. On average, ERT concentration in different commercially available classes of cow milk was found to be 0.442 ± 0.191 μmol/L, with the highest levels in the ultra-high temperature milks and low values in the unprocessed and HTST whole milks. In this light, our experiments suggest that ERT could be used as a marker for the heat treatment of milk. © 2014 Institute of Food Technologists®

Assessment of chromatographic methods for the chemical stability of a new miconazole nitrate cream

International Nuclear Information System (INIS)

Garcia Pulpeiro, Oscar; Calzadilla Aguiar, Wendy; Rodriguez Bencomo, Wendy

2013-01-01

To assess the chromatographic methods for the chemical stability of a new 2 % miconazol nitrate cream. arious degradation conditions were firstly used in the raw material miconazole nitrate in order to obtain the possible degradation products of this drug and to evaluate them by thin layer chromatography-based method, which was validated to identify the degradation products in the new cream. The performance of the official method based on high resolution liquid chromatography and reported in British Pharmacopoeia 2010 was evaluated, and its selectivity against the possible degradation products were also analyzed. Both chromatographic methods were applied to the analysis of cream samples from the three pilot batches under heat stress for 30 days

[Radiation induced changes in the cuticular hydrocarbons of the granary weevil and their relationship to dessication and adult mortality]. Half-yearly report, February 15-August 14, 1986

International Nuclear Information System (INIS)

1986-01-01

Granary weevil (Sitophilus granarius) were irradiated with cesium-137 derived gamma radiation at various age groups. Hydrocarbon analysis of epicuticles were studied chromatographically and by mass spectroscopy. 3 figs., 4 tabs. (DT)

Optimization of chromatographic conditions for determination of aflatoxin B1, B2, G1 and G2 by using liquid chromatography-mass Spectrometry

Science.gov (United States)

Ramadhaningtyas, Dillani Putri; Aryana, Nurhani; Aristiawan, Yosi; Styarini, Dyah

2017-11-01

The optimization of instrument condition and chromatographic separation for analysis of aflatoxin B1, B2, G1 and G2 using liquid chromatography tandem with mass spectrometer detector was conducted in the aim to provide more accurate and reliable analysis results. The aflatoxin known to be serious threat for human health as it is classified as the carcinogenic compounds. The aflatoxin B1, B2, G1 and G2 were selected due to its extensive contamination in various agricultural commodities. The best chromatographic separation was obtained using C-18 column with gradient elution of solvent 5 mM ammonium acetate and 0.1% formic acid in methanol at 7 minutes runtime analysis. The linearity of the detector showed satisfied results as the coefficient determination found to be 0.9994, 0.9996, 0.9998 and 0.9987 for aflatoxin B1, G1, B2, and G2 respectively in the range concentration from 1 to 20 ng/g. The quantifier ion selected for the aflatoxin B1, B2, G1 and G2 was m/z 285.1, 259, 243 and 313 respectively. The instrument precision at these quantifier ions also showed satisfied result with %RSD was around 3.4 to 6.8%. The optimized method present in this study can be used for further sample analysis.

Forensic Analysis of Blue Ball point Pen Inks Using Ultraviolet-Visible Spectrometer and Ultra-Performance Liquid Chromatograph

International Nuclear Information System (INIS)

Lee, L.C.; Shandu, K.T.S.; Nor Syahirah Mohamad Razi; Ab Aziz Ishak; Khairul Osman

2015-01-01

Twelve varieties of blue ball point pens were selected and analyzed using UV-Vis spectrometer and ultra-performance liquid chromatography (UPLC). The aim of the study was to determine discrimination power (DP) of these methods in differentiating pen inks collected from the market in Malaysia. Discrimination analysis of 66 possible pen-pair of blue ball point pens was carried out via one-way ANOVA based on obtained chromatogram and spectra. A total of 18 peaks were determined as coming from inks based on the chromatographic data extracted at three different wavelengths (279, 370 and 400 nm). While for the UV-Vis spectrometer analysis, presence of peaks at 303, 545, 577 and 584 nm wavelengths were recorded. UV-Vis spectral data were mainly produced by the colorant components (for example, dyes) found in inks and UPLC may detect ink components other than dyes, for example, additives. As conclusion, the DP for UV-Vis and UPLC were determined to be 72.12 % and 98.48 %, respectively. This manuscript demonstrates the potential of UPLC for discriminating pen inks based on non-dye components. Additionally, the dye components in inks do not seem to play important role in discrimination of pen inks. (author)

Simulation of the high-pressure phase equilibria of hydrocarbon-water/brine systems

DEFF Research Database (Denmark)

Zuo, You-Xiang; Stenby, Erling Halfdan; Guo, Tian-Min

1996-01-01

The major objectives of this work are: (1) extend the modified Patel-Teja (MPT) equation of state proposed for aqueous electrolyte systems (Zuo and Guo, 1991) to describe the liquid-liquid and vapor-liquid-liquid equilibria of hydrocarbon-water/brine systems through introducing an unconventional...

Liquid chromatographic determination of urinary 2-thiothiazolidine-4-carboxylic acid, a biomarker of carbon disulphide exposure.

Science.gov (United States)

Lee, B L; Yang, X F; New, A L; Ong, C N

1995-06-23

An effective gradient high-performance liquid chromatographic method for baseline separation of urinary 2-thiothiazolidine-4-carboxylic acid (TTCA), with photodiode array detection at 271 nm was described. o-Methylhippuric acid was used as an internal standard (I.S.). A 1-ml urine sample was saturated with 300 mg of sodium sulphate, acidified with 100 microliters of 6 M hydrochloric acid, extracted twice with 2 ml of diethyl ether, and after evaporation, the residue was taken up in 1 ml of 0.1% (v/v) phosphoric acid. The two mobile phases used for gradient elution were: (A) 10 mM ammonium dihydrogenphosphate (pH 3.5) and (B) same concentration of buffer but containing 20% (v/v) of methanol (pH 4.8). The flow-rate was set at 1.0 ml/min. TTCA and I.S. were detected at 2.2 and 9.1 min, respectively. The method was validated with urine samples collected from normal subjects and workers occupationally exposed to carbon disulphide. The present method enables the detection of urinary TTCA at a concentration of 0.025 mg/l. Analytical recovery and reproducibility generally exceeded 90%. The proposed method is considered more sensitive, specific and reliable than other existing methods.

Recent development of ionic liquid stationary phases for liquid chromatography.

Science.gov (United States)

Shi, Xianzhe; Qiao, Lizhen; Xu, Guowang

2015-11-13

Based on their particular physicochemical characteristics, ionic liquids have been widely applied in many fields of analytical chemistry. Many types of ionic liquids were immobilized on a support like silica or monolith as stationary phases for liquid chromatography. Moreover, different approaches were developed to bond covalently ionic liquids onto the supporting materials. The obtained ionic liquid stationary phases show multi-mode mechanism including hydrophobic, hydrophilic, hydrogen bond, anion exchange, π-π, and dipole-dipole interactions. Therefore, they could be used in different chromatographic modes including ion-exchange, RPLC, NPLC and HILIC to separate various classes of compounds. This review mainly summarizes the immobilized patterns and types of ionic liquid stationary phases, their retention mechanisms and applications in the recent five years. Copyright © 2015 Elsevier B.V. All rights reserved.

Evaluation of highly polar ionic liquid gas chromatographic column for the determination of the fatty acids in milk fat.

Science.gov (United States)

Delmonte, Pierluigi; Fardin-Kia, Ali Reza; Kramer, John K G; Mossoba, Magdi M; Sidisky, Len; Tyburczy, Cynthia; Rader, Jeanne I

2012-04-13

The SLB-IL111, a new ionic liquid capillary column for gas chromatography available from Supelco Inc., was recently shown to provide enhanced separation of unsaturated geometric and positional isomers of fatty acid (FAs) when it was compared to cyanopropylsiloxane (CPS) columns currently recommended for the analysis of fatty acid methyl esters (FAMEs). A 200 m SLB-IL111 capillary column, operated under a combined temperature and eluent flow gradient, was successfully used to resolve most of the FAs contained in milk fat in a single 80 min chromatographic separation. The selected chromatographic conditions provided a balanced, simultaneous separation of short-chain (from 4:0), long-chain polyunsaturated fatty acids (PUFAs), and most of the unsaturated FA positional/geometric isomers contained in milk fat. Among the monounsaturated fatty acids (MUFAs), these conditions separated t11-18:1 and t10-18:1 FAs, the two most abundant trans fatty acids (t-FA) contained in most dairy products. These t-FAs reportedly have different biological activities. The conjugated linoleic acid (CLA) isomers commonly found in dairy products were separated from each other, including t7,c9-18:2 from c9,t11-18:2, which eliminated the need for their complementary silver ion HPLC analysis. The application of the SLB-IL111 column provided a complementary elution profile of FAMEs to those obtained by CPS columns, allowing for a more comprehensive FA analysis of total milk fat. The FAMEs were identified by the use of available reference materials, previously synthesized and characterized reference mixtures, and prior separations of the milk fat FAMEs by silver ion chromatography based on the number/geometry of double bonds. Published by Elsevier B.V.

Downhole fluid injection systems, CO2 sequestration methods, and hydrocarbon material recovery methods

Science.gov (United States)

Schaef, Herbert T.; McGrail, B. Peter

2015-07-28

Downhole fluid injection systems are provided that can include a first well extending into a geological formation, and a fluid injector assembly located within the well. The fluid injector assembly can be configured to inject a liquid CO2/H2O-emulsion into the surrounding geological formation. CO2 sequestration methods are provided that can include exposing a geological formation to a liquid CO2/H2O-emulsion to sequester at least a portion of the CO2 from the emulsion within the formation. Hydrocarbon material recovery methods are provided that can include exposing a liquid CO2/H2O-emulsion to a geological formation having the hydrocarbon material therein. The methods can include recovering at least a portion of the hydrocarbon material from the formation.

Industrial scale chromatographic separation of valuable compounds from biomass hydrolysates and side streams

Energy Technology Data Exchange (ETDEWEB)

Saari, P.

2011-06-15

Carbohydrates are composed of a number of various monosaccharides, glucose being the most abundant. Some of the monosaccharides are valuable compounds used in the food and pharmaceutical industries. They can be separated from biomass hydrolysates e.g. by chromatographic methods. In this thesis, chromatographic separation of valuable compounds using ion exchange resins was studied on an industrial scale. Of special interest were rare monosaccharides in biomass hydrolysates. A novel chromatographic separation process was developed for fucose, starting from pre-processed spent sulfite liquor. The core of the process consists of three chromatographic separations with different types of ion exchange resins. Chromatographic separation of galactose was tested with three biomass hydrolysates; lactose, gum arabic and hemicellulose hydrolysates. It was demonstrated that also galactose can be separated from complex carbohydrate mixtures. A recovery process for arabinose from citrus pectin liquid residual and for mannose from wood pulp hydrolysate were also developed and experimentally verified. In addition to monosaccharides, chromatographic separation of glycinebetaine from vinasse was examined with a hydrogen form weak acid cation exchange resin. The separation involves untypical peak formation depending, for example, on the pH and the cation composition. The retention mechanism was found to be hydrogen bonding between glycinebetaine and the resin. In the experimental part, all four resin types - strong acid cation, strong base anion, weak acid cation and weak base anion exchange resins - were used. In addition, adsorption equilibria data of seven monosaccharides and sucrose were measured with the resins in sodium and sulfate forms because such data have been lacking. It was found out that the isotherms of all sugars were linear under industrial conditions. A systematic method for conceptual process design and sequencing of chromatographic separation steps were developed

Accelerated solvent extraction method with one-step clean-up for hydrocarbons in soil

International Nuclear Information System (INIS)

Nurul Huda Mamat Ghani; Norashikin Sain; Rozita Osman; Zuraidah Abdullah Munir

2007-01-01

The application of accelerated solvent extraction (ASE) using hexane combined with neutral silica gel and sulfuric acid/ silica gel (SA/ SG) to remove impurities prior to analysis by gas chromatograph with flame ionization detector (GC-FID) was studied. The efficiency of extraction was evaluated based on the three hydrocarbons; dodecane, tetradecane and pentadecane spiked to soil sample. The effect of ASE operating conditions (extraction temperature, extraction pressure, static time) was evaluated and the optimized condition obtained from the study was extraction temperature of 160 degree Celsius, extraction pressure of 2000 psi with 5 minutes static extraction time. The developed ASE with one-step clean-up method was applied in the extraction of hydrocarbons from spiked soil and the amount extracted was comparable to ASE extraction without clean-up step with the advantage of obtaining cleaner extract with reduced interferences. Therefore in the developed method, extraction and clean-up for hydrocarbons in soil can be achieved rapidly and efficiently with reduced solvent usage. (author)

Simple and sensitive high performance liquid chromatographic method for the simultaneous quantitation of the phenylalanine in human plasma

Directory of Open Access Journals (Sweden)

Hossein Danafar

2015-09-01

Full Text Available Phenylalanine (Phe is the most reliable indicator for the diagnosis of phenylketonuria (PKU. The purpose of this study is to establish a reliable and quick method for the assignment of Phe in peripheral capillary blood from newborns and children by high performance liquid chromatography with ultraviolet detection (HPLC-UV. PKU is an inborn error of metabolism characterized by the inability of the body to use Phe. A rapid and sensitive high performance liquid chromatographic (HPLC method has been developed for determination of Phe in plasma. The method uses a protein precipitation step with sulfosalicilic acid for sample preparation by separation on a Nova-pack C18 column using sodium acetate buffer and acetonitrile (94: 6 v/v adjusted to pH 6.5 with glacial acetic acid. The eluted peaks detected by a UV detector was set at wavelength of 215 nm. The method was validated in the range of Phe concentrations from 0.1 to 20 µg/ml. The limits of detection (LOD and quantitation (LOQ of the method were 0.05 and 0.1 µg/ml, respectively. The average drug recovery from plasma was 88.60 percent throughout the linear concentration range., with the average within-run and between-run accuracy values of 103.3 and 115.350, respectively. The method is quick, easy, very steady and precise for the screen, assignment, and evaluation of Phe in human plasma by HPLC, which is particularly a useful way for screening and diagnosis of PKU and monitoring of a diet therapy.

Recent advances in metal-organic frameworks and covalent organic frameworks for sample preparation and chromatographic analysis.

Science.gov (United States)

Wang, Xuan; Ye, Nengsheng

2017-12-01

In the field of analytical chemistry, sample preparation and chromatographic separation are two core procedures. The means by which to improve the sensitivity, selectivity and detection limit of a method have become a topic of great interest. Recently, porous organic frameworks, such as metal-organic frameworks (MOFs) and covalent organic frameworks (COFs), have been widely used in this research area because of their special features, and different methods have been developed. This review summarizes the applications of MOFs and COFs in sample preparation and chromatographic stationary phases. The MOF- or COF-based solid-phase extraction (SPE), solid-phase microextraction (SPME), gas chromatography (GC), high-performance liquid chromatography (HPLC) and capillary electrochromatography (CEC) methods are described. The excellent properties of MOFs and COFs have resulted in intense interest in exploring their performance and mechanisms for sample preparation and chromatographic separation. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Optimization of two different dispersive liquid-liquid microextraction methods followed by gas chromatography-mass spectrometry determination for polycyclic aromatic hydrocarbons (PAHs) analysis in water.

Science.gov (United States)

Tseng, Wan-Chi; Chen, Pai-Shan; Huang, Shang-Da

2014-03-01

Novel sample preparation methods termed "up-and-down shaker-assisted dispersive liquid-liquid microextraction (UDSA-DLLME)" and "water with low concentration of surfactant in dispersed solvent-assisted emulsion dispersive liquid-liquid microextraction (WLSEME)" coupled with gas chromatography-mass spectrometry (GC-MS) have been developed for the analysis of 11 polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. For UDSA-DLLME, an up-and-down shaker-assisted emulsification was employed. Extraction was complete in 3min. Only 14 μL of 1-heptanol was required, without a dispersive solvent. Under the optimum conditions, the linear range was 0.08-100 µg L(-1), and the LODs were in the range 0.022-0.060 µg L(-1). The enrichment factors (EFs) ranged from 392 to 766. Relative recoveries were between 84% and 113% for river, lake, and field water. In WLSEME, 9 μL of 1-nonanol as extraction solvent and 240 μL of 1 mg L(-1) Triton X-100 as surfactant were mixed in a microsyringe to form a cloudy emulsified solution, which was then injected into the samples. Compared with other surfactant-assisted emulsion methods, WLSEME uses much less surfactant. The linear range was 0.08-100 µg L(-1), and the LODs were 0.022-0.13 µg L(-1). The EFs ranged from 388 to 649. The relative recoveries were 86-114% for all three water specimens. Copyright © 2013 Elsevier B.V. All rights reserved.

Effect of hydrocarbons on plasma treatment of NOx

Energy Technology Data Exchange (ETDEWEB)

Penetrante, B.M.; Pitz, W.J.; Hsaio, M.C.; Merritt, B.T.; Vogtlin, G.E. [Lawrence Livermore National Lab., CA (United States)

1997-12-31

Lean burn gasoline engine exhausts contain a significant amount of hydrocarbons in the form of propene. Diesel engine exhausts contain little gaseous hydrocarbon; however, they contain a significant amount of liquid-phase hydrocarbons (known as the volatile organic fraction) in the particulates. The objective of this paper is to examine the fate of NO{sub x} when an exhaust gas mixture that contains hydrocarbons is subjected to a plasma. The authors will show that the hydrocarbons promote the oxidation of NO to NO{sub 2}, but not the reduction of NO to N{sub 2}. The oxidation of NO to NO{sub 2} is strongly coupled with the hydrocarbon oxidation chemistry. This result suggests that gas-phase reactions in the plasma alone cannot lead to the chemical reduction of NO{sub x}. Any reduction of NO{sub x} to N{sub 2} can only be accomplished through heterogeneous reactions of NO{sub 2} with surfaces or particulates.

Determination and validation of a simple high-performance liquid chromatographic method for simultaneous assay of iprodione and vinclozolin in human urine.

Science.gov (United States)

Carlucci, Giuseppe; Pasquale, Dorina Di; Ruggieri, Fabrizio; Mazzeo, Pietro

2005-12-15

A method based on solid-phase extraction (SPE) and high-performance liquid chromatography (HPLC) was developed for the simultaneous determination of 3-(3,5-diclorophenyl)-5-ethenyl-5-methyl-2,4-oxazolidinedione (vinclozolin) and 3-(3,5-diclorophenyl)-N-(1-methylethyl)-2,4-dioxo-1-imidazolidinecarboxamide (iprodione) in human urine. Urine samples containing vinclozolin and iprodione were collected by solid phase extraction using C(18) cartridges. The chromatographic separation was achieved on a Spherisorb ODS2 (250 mm x 4.6 mm, 5 microm) column with an isocratic mobile phase of acetonitrile-water (60:40, v/v). Detection was UV absorbance at 220 nm. The calibration graphs were linear from 30 to 1000 ng/mL for the two fungicides. Intra- and inter-day R.S.D. did not exceed 2.9%. The quantitation limit was 50 ng/mL for vinclozolin and 30 ng/mL for iprodione, respectively.

Hydrocarbon source apportionment for the 1996 Paso del Norte Ozone Study

Energy Technology Data Exchange (ETDEWEB)

Fujita, E.M. [Desert Research Institute, 2215 Raggio Parkway, Reno, NV 89506-0220 (United States)

2001-08-10

The 1996 Paso del Norte (PdN) ozone study was conducted to improve current understanding of the significant meteorological and air quality processes that lead to high concentrations of ozone in El Paso, Texas (USA) and Ciudad Juarez, Chihuahua (Mexico). Two-hour canister samples were collected five times daily at 05.00-07.00 h, 07.00-09.00 h, 09.00-11.00 h, 11.00-13.00 h, and 15.00-17.00 h MST during intensive study periods at one urban and one rural site on each side of the border. An automated gas chromatograph was operated at one site in central El Paso. Source profiles (the fractional chemical composition of emissions) from motor vehicles, gasoline, liquefied petroleum gas, and commercial natural gas were combined with source profiles from other studies for input to the Chemical Mass Balance (CMB) receptor model to apportion the measured non-methane hydrocarbons (NMHC) to sources. On-road vehicle emissions accounted for one-half to two-thirds of the NMHC in Ciudad Juarez and El Paso with the highest contributions occurring during the morning and afternoon commute periods. Emissions from diesel exhaust contributed approximately 2-3% of NMHC in Ciudad Juarez and less than 2% in El Paso. The average sum of liquid gasoline and gasoline vapor increased during the day in Ciudad Juarez from 2% at 06.00 h to approximately 12% at 16.00 h. Diurnal and day-of-the-week patterns in the liquid gasoline contributions are essentially identical to the corresponding patterns for motor vehicle exhaust, which suggest that a large fraction of the liquid gasoline contribution may be associated with tailpipe emissions rather than evaporative emissions from motor vehicles or industrial sources. Including the sum of the two sources put the upper limit for tailpipe contributions at 60-70% of NMHC.

Process for scavenging hydrogen sulfide from hydrocarbon gases

International Nuclear Information System (INIS)

Fox, I.

1981-01-01

A process for scavenging hydrogen sulfide from hydrocarbon gases utilizes iron oxide particles of unique chemical and physical properties. These particles have large surface area, and are comprised substantially of amorphous Fe 2 O 3 containing a crystalline phase of Fe 2 O 3 , Fe 3 O 4 and combinations thereof. In scavenging hydrogen sulfide, the iron oxide particles are suspended in a liquid which enters into intimate mixing contact with hydrocarbon gases; the hydrogen sulfide is reacted at an exceptional rate and only acid-stable reaction products are formed. Thereafter, the sweetened hydrocarbon gases are collected

Chiral high-performance liquid chromatographic analysis of fluoxetine and norfluoxetine in rabbit plasma, urine, and vitreous humor using an acetylated beta-cyclodextrin column.

Science.gov (United States)

Yee, L; Wong, S H; Skrinska, V A

2000-10-01

Fluoxetine (Prozac) is a potent selective serotonin reuptake inhibitor used for the treatment of major depression. Both fluoxetine (F) and its demethylated metabolite, norfluoxetine (NF), are racemic. S-Fluoxetine (SF) and S-norfluoxetine (SNF) are more potent inhibitors of serotonin reuptake than R-fluoxetine (RF) and R-norfluoxetine (RNF). Quantitation of individual enantiomers may provide a greater understanding of pharmacokinetic properties. The objective of this study was to perform a limited chiral selectivity study using rabbit plasma, urine, and vitreous humor analyzed by a solid-phase extraction protocol and a newly developed chiral analysis with an acetylated beta-cyclodextrin (CD) column. Liquid chromatographic parameters for CD were as follows: a mobile phase composition of methanol/0.3% triethylamine buffer, pH 5.6, (30:70), a flow rate of 1 mL/min, detection at 214 nm, and a temperature of 40 degrees C. Elution order was SNF, SF, RNF, and RF with capacity factors of 6, 7, 8, and 9, respectively. The corresponding resolution factors were as follows: R1,2 = 0.8, R2,3 = 1.2, and R3,4 = 0.9. The conditions for solid-phase extraction were optimized for Varian Bond Elut Certify columns. Following sample application, the column was rinsed with water, acetic acid, and then with methanol. Drug enantiomers were eluted with methylene chloride, isopropanol, and ammonium hydroxide (78:20:2). After extract evaporation, the extract residue was reconstituted for high-performance liquid chromatographic analysis. To investigate chiral pharmacology, a biodistribution study was performed by administering 2 mg/kg of F to five rabbits. Blood, urine, and vitreous specimens were collected. Plasma samples collected 45 min postinjection showed nearly equal concentrations of RF and SE After 24 h, the only metabolite detected in plasma was RNF. Drugs were not detectable in vitreous humor. Urine concentrations of SNF, SF, RNF, and RF were 51, 76, 34, and 8 microg/L, respectively

Applications of electrochemically-modulated liquid chromatography (EMLC): Separations of aromatic amino acids and polycyclic aromatic hydrocarbons

Energy Technology Data Exchange (ETDEWEB)

Deng, Li [Iowa State Univ., Ames, IA (United States)

1998-03-27

The research in this thesis explores the separation capabilities of a new technique termed electrochemically-modulated liquid chromatography (EMLC). The thesis begins with a general introduction section which provides a literature review of this technique as well as a brief background discussion of the two research projects in each of the next two chapters. The two papers which follow investigate the application of EMLC to the separation of a mixture of aromatic amino acids and of a mixture of polycyclic aromatic hydrocarbons (PAHs). The last section presents general conclusions and summarizes the thesis. References are compiled in the reference section of each chapter. The two papers have been removed for separate processing.

Distilling hydrocarbons, etc

Energy Technology Data Exchange (ETDEWEB)

Turner, C

1917-11-23

In the fractional or destructive distillation of hydrocarbon oils or other liquids, the pressure in the still is raised and lowered alternately. The still is closed to raise the pressure, and is opened to lower the pressure rapidly solely by expansion of the vapors. The operation is effected without intermittent cooling, except such as may occur during the lowering of the pressure. In distilling hydrocarbon oil, pressure steam is blown into the oil until the pressure reaches 5 lb/in./sup 2/. The vapor outlet is then opened until the pressure falls to 2 lb/in./sup 2/, whereupon the vapor outlet is closed and steam is again admitted. The operation is continued until the steam, which is of 20 lb pressure, no longer effects distillation; after this stage, superheated steam is used.

Liquid chromatographic determination of CPZEN-45, a novel anti-tubercular drug, in biological samples.

Science.gov (United States)

Hanif, S N M; Hickey, A J; Garcia-Contreras, L

2014-01-01

CPZEN-45 is a new drug candidate being considered for the treatment of tuberculosis (TB). The aim of this study was to develop and validate a reverse-phase high-performance liquid chromatographic (HPLC) method suitable to determine CPZEN-45 concentrations in biological samples. CPZEN-45 was extracted from biological fluids and tissues (plasma, lung and spleen from guinea pig) by sequential extraction with acetonitrile and quantified by a Waters HPLC Alliance System coupled with a ZORBAX Bonus-RP column, guard column and UV detection at 263nm. The mobile phase was 20:80 acetonitrile:ultrapure-water with 0.05% TFA. The CPZEN-45 peak was eluted at 5.1min with no interference from the inherent peaks of plasma, bronchoalveolar lavage (BAL), lung or spleen tissues. Recovery of CPZEN-45 from biological samples was >96% of the spiked amount. The limit of detection was 0.05μg/ml and the limit of quantitation was 0.29μg/ml which was more than 5 and 21 times lower than the reported minimal inhibitory concentration of CPZEN-45 (MIC=1.56μg/ml for Mycobacterium tuberculosis and 6.25μg/ml for MDR-TB, respectively). Thus, HPLC method was deemed reliable, sensitive, reproducible and accurate for the determination of CPZEN-45 concentrations in plasma, BAL, lung and spleen tissues. Therefore, this method was used in subsequent studies in the guinea pig model to determine the disposition of CPZEN-45 after administration of solutions by the IV and SC routes. Copyright © 2013 Elsevier B.V. All rights reserved.

Modeling Aquatic Toxicity through Chromatographic Systems.

Science.gov (United States)

Fernández-Pumarega, Alejandro; Amézqueta, Susana; Farré, Sandra; Muñoz-Pascual, Laura; Abraham, Michael H; Fuguet, Elisabet; Rosés, Martí

2017-08-01

Environmental risk assessment requires information about the toxicity of the growing number of chemical products coming from different origins that can contaminate water and become toxicants to aquatic species or other living beings via the trophic chain. Direct toxicity measurements using sensitive aquatic species can be carried out but they may become expensive and ethically questionable. Literature refers to the use of chromatographic measurements that correlate to the toxic effect of a compound over a specific aquatic species as an alternative to get toxicity information. In this work, we have studied the similarity in the response of the toxicity to different species and we have selected eight representative aquatic species (including tadpoles, fish, water fleas, protozoan, and bacteria) with known nonspecific toxicity to chemical substances. Next, we have selected four chromatographic systems offering good perspectives for surrogation of the eight selected aquatic systems, and thus prediction of toxicity from the chromatographic measurement. Then toxicity has been correlated to the chromatographic retention factor. Satisfactory correlation results have been obtained to emulate toxicity in five of the selected aquatic species through some of the chromatographic systems. Other aquatic species with similar characteristics to these five representative ones could also be emulated by using the same chromatographic systems. The final aim of this study is to model chemical products toxicity to aquatic species by means of chromatographic systems to reduce in vivo testing.

Measurement uncertainty of liquid chromatographic analyses visualized by Ishikawa diagrams.

Science.gov (United States)

Meyer, Veronika R

2003-09-01

Ishikawa, or cause-and-effect diagrams, help to visualize the parameters that influence a chromatographic analysis. Therefore, they facilitate the set up of the uncertainty budget of the analysis, which can then be expressed in mathematical form. If the uncertainty is calculated as the Gaussian sum of all uncertainty parameters, it is necessary to quantitate them all, a task that is usually not practical. The other possible approach is to use the intermediate precision as a base for the uncertainty calculation. In this case, it is at least necessary to consider the uncertainty of the purity of the reference material in addition to the precision data. The Ishikawa diagram is then very simple, and so is the uncertainty calculation. This advantage is given by the loss of information about the parameters that influence the measurement uncertainty.

Estimations of temperature deviations in chromatographic columns using isenthalpic plots. I. Theory for isocratic systems.

Science.gov (United States)

Tarafder, Abhijit; Iraneta, Pamela; Guiochon, Georges; Kaczmarski, Krzysztof; Poe, Donald P

2014-10-31

We propose to use constant enthalpy or isenthalpic diagrams as a tool to estimate the extent of the temperature variations caused by the mobile phase pressure drop along a chromatographic column, e.g. of its cooling in supercritical fluid and its heating in ultra-performance liquid chromatography. Temperature strongly affects chromatographic phenomena. Any of its variations inside the column, whether intended or not, can lead to significant changes in separation performance. Although instruments use column ovens in order to keep constant the column temperature, operating conditions leading to a high pressure drop may cause significant variations of the column temperature, both in the axial and the radial directions, from the set value. Different ways of measuring these temperature variations are available but they are too inconvenient to be employed in many practical situations. In contrast, the thermodynamic plot-based method that we describe here can easily be used with only a ruler and a pencil. They should be helpful in developing methods or in analyzing results in analytical laboratories. Although the most effective application area for this approach should be SFC (supercritical fluid chromatography), it can be applied to any chromatographic conditions in which temperature variations take place along the column due to the pressure drop, e.g. in ultra-high pressure liquid chromatography (UHPLC). The method proposed here is applicable to isocractic conditions only. Copyright © 2014 Elsevier B.V. All rights reserved.

High energy-density liquid rocket fuel performance

Science.gov (United States)

Rapp, Douglas C.

1990-01-01

A fuel performance database of liquid hydrocarbons and aluminum-hydrocarbon fuels was compiled using engine parametrics from the Space Transportation Engine Program as a baseline. Propellant performance parameters are introduced. General hydrocarbon fuel performance trends are discussed with respect to hydrogen-to-carbon ratio and heat of formation. Aluminum-hydrocarbon fuel performance is discussed with respect to aluminum metal loading. Hydrocarbon and aluminum-hydrocarbon fuel performance is presented with respect to fuel density, specific impulse and propellant density specific impulse.

The counterintuitive role of extra-column volume in the determination of column efficiency and scaling of chromatographic processes

NARCIS (Netherlands)

Schultze-Jena, A.; Boon, M.A.; Bussmann, P.J.Th.; Janssen, A.E.M.; Padt, van der A.

2017-01-01

In industrial liquid separation processes chromatography often has a key function in the optimization of yield and purity. For the design of an industrial system, chromatographic processes are generally simulated using mathematical models, tested and optimized at laboratory level, and then scaled

The counterintuitive role of extra-column volume in the determination of column efficiency and scaling of chromatographic processes

NARCIS (Netherlands)

Schultze-Jena, A.; Boon, M.A.; Bussmann, P.J.T.; Janssen, A.E.M.; Padt, A. van der

2017-01-01

In industrial liquid separation processes chromatography often has a key function in the optimization of yield and purity. For the design of an industrial system, chromatographic processes are generally simulated using mathematical models, tested and optimized at laboratory level, and then scaled up

Monitoring for 99Tc in borehole waters using an extraction chromatographic resin

International Nuclear Information System (INIS)

Davis, T.M.; Nelson, D.M.; Thompson, E.G.

1993-01-01

A technique using an extraction chromatographic resin for the analysis of 99 Tc in borehole waters is presented. The method involves one pass of the sample through two resins, a rinse of the resins, then counting of one of the resins by liquid scintillation counting. The technique is intended to be used as a screening method of 99 Tc. The procedure employs commercially available materials, generates little waste and requires very little operator time

Investigation of Underground Hydrocarbon Leakage using Ground Penetrating Radar

Science.gov (United States)

Srigutomo, Wahyu; Trimadona; Agustine, Eleonora

2016-08-01

Ground Penetrating Radar (GPR) survey was carried out in several petroleum plants to investigate hydrocarbon contamination beneath the surface. The hydrocarbon spills are generally recognized as Light Non-Aqueous Phase Liquids (LNAPL) if the plume of leakage is distributed in the capillary fringe above the water table and as Dense Non-Aqueous Phase Liquids (DNAPL) if it is below the water table. GPR antennas of 200 MHz and 400 MHz were deployed to obtain clear radargrams until 4 m deep. In general, the interpreted radargram sections indicate the presence of surface concrete layer, the compacted silty soill followed by sand layer and the original clayey soil as well as the water table. The presence of hydrocarbon plumes are identified as shadow zones (radar velocity and intensity contrasts) in the radargram that blur the layering pattern with different intensity of reflected signal. Based on our results, the characteristic of the shadow zones in the radargram is controlled by several factors: types of hydrocarbon (fresh or bio-degraded), water moisture in the soil, and clay content which contribute variation in electrical conductivity and dielectric constants of the soil.

Assessment of plant-derived hydrocarbons. Final report

Energy Technology Data Exchange (ETDEWEB)

McFadden, K.; Nelson, S.H.

1981-09-30

A number of hydrocarbon producing plants are evaluated as possible sources of rubber, liquid fuels, and industrial lubricants. The plants considered are Euphorbia lathyris or gopher plant, milkweeds, guayule, rabbit brush, jojoba, and meadow foam. (ACR)

Instrumental liquid chromatography: a practical manual on high-performance liquid chromatographic methods

National Research Council Canada - National Science Library

Parris, N. A

1976-01-01

Available texts on liquid chromatography have tended to emphasize the developments in the theoretical understanding of the technique and methodology or to list numerous applications, complete with experimental details...

Methods for reformation of gaseous hydrocarbons using electrical discharge

KAUST Repository

Cha, Min Suk

2017-02-16

Methods for the reformation of gaseous hydrocarbons are provided. The methods can include forming a bubble containing the gaseous hydrocarbon in a liquid. The bubble can be generated to pass in a gap between a pair of electrodes, whereby an electrical discharge is generated in the bubble at the gap between the electrodes. The electrodes can be a metal or metal alloy with a high melting point so they can sustain high voltages of up to about 200 kilovolts. The gaseous hydrocarbon can be combined with an additive gas such as molecular oxygen or carbon dioxide. The reformation of the gaseous hydrocarbon can produce mixtures containing one or more of H2, CO, H2O, CO2, and a lower hydrocarbon such as ethane or ethylene. The reformation of the gaseous hydrocarbon can produce low amounts of CO2 and H2O, e.g. about 15 mol-% or less.

Methods for reformation of gaseous hydrocarbons using electrical discharge

KAUST Repository

Cha, Min; Zhang, Xuming

2017-01-01

Methods for the reformation of gaseous hydrocarbons are provided. The methods can include forming a bubble containing the gaseous hydrocarbon in a liquid. The bubble can be generated to pass in a gap between a pair of electrodes, whereby an electrical discharge is generated in the bubble at the gap between the electrodes. The electrodes can be a metal or metal alloy with a high melting point so they can sustain high voltages of up to about 200 kilovolts. The gaseous hydrocarbon can be combined with an additive gas such as molecular oxygen or carbon dioxide. The reformation of the gaseous hydrocarbon can produce mixtures containing one or more of H2, CO, H2O, CO2, and a lower hydrocarbon such as ethane or ethylene. The reformation of the gaseous hydrocarbon can produce low amounts of CO2 and H2O, e.g. about 15 mol-% or less.

Continuous process for converting hydrocarbons, etc

Energy Technology Data Exchange (ETDEWEB)

1934-05-01

A continuous process is disclosed for converting hydrocarbons, liquid, semi-liquid, and solid, of all origins and kinds, into incondensable gases, without carbon deposits, characterized by the fact that an intimate mixture of the material and superheated steam before cracking is passed through a contact mass. The contact mass consists of all metals, metal alloys, and mineral salts which, at the reaction temperature, are fused and do not react with the water vapor or gaseous products.

Monolithic columns with organic sorbent based on poly-1-vinylimidazole for high performance liquid chromatography

Science.gov (United States)

Patrushev, Y. V.; Sidelnikov, V. N.; Yudina, Y. S.

2017-03-01

Monolithic chromatographic columns for HPLC with sorbent based on 1-vinylimidazole are prepared. It is shown that changing the 1-vinylimidazole content in the initial solution allows us to change the polarity of columns. An example of aromatic hydrocarbons separation is presented.

Detection system for a gas chromatograph. [. cap alpha. -methylnaphthalene,. beta. -methylnapthalene

Science.gov (United States)

Hayes, J.M.; Small, G.J.

1982-04-26

A method and apparatus are described for the quantitative analysis of vaporizable compounds, and in particular of polycyclic aromatic hydrocarbons which may be induced to fluoresce. The sample to be analyzed is injected into a gas chromatography column and is eluted through a narrow orifice into a vacuum chamber. The free expansion of the eluted sample into the vacuum chamber creates a supersonic molecular beam in which the sample molecules are cooled to the extent that the excited vibrational and rotational levels are substantially depopulated. The cooled molecules, when induced to fluoresce by laser excitation, give greatly simplified spectra suitable for analytical purposes. The laser induced fluorimetry provides great selectivity, and the gas chromatograph provides quantitative transfer of the sample to the molecular beam. 3 figures, 2 tables.

Preparing valuable hydrocarbons by hydrogenation

Energy Technology Data Exchange (ETDEWEB)

Pier, M

1930-08-22

A process is described for the preparation of valuable hydrocarbons by treatment of carbonaceous materials, like coal, tars, minerals oils, and their distillation and conversion products, and for refining of liquid hydrocarbon mixture obtained at raised temperature and under pressure, preferably in the presence of catalysts, by the use of hydrogen-containing gases, purified and obtained by distilling solid combustibles, characterized by the purification of the hydrogen-containing gases being accomplished for the purpose of practically complete removal of the oxygen by heating at ordinary or higher pressure in the presence of a catalyst containing silver and oxides of metals of group VI of the periodic system.

Post-synthetic modification of MIL-101(Cr) with pyridine for high-performance liquid chromatographic separation of tocopherols.

Science.gov (United States)

Yang, Fang; Yang, Cheng-Xiong; Yan, Xiu-Ping

2015-05-01

Effective separation of tocopherols is challenging and significant due to their structural similarity and important biological role. Here we report the post-synthetic modification of metal-organic framework (MOF) MIL-101(Cr) with pyridine for high-performance liquid chromatographic (HPLC) separation of tocopherols. Baseline separation of four tocopherols was achieved on a pyridine-grafted MIL-101(Cr) packed column within 10 min using hexane/isopropanol (96:4, v/v) as the mobile phase at a flow rate of 0.5 mL min(-1). The pyridine-grafted MIL-101(Cr) packed column gave high column efficiency (85,000 plates m(-1) for δ-tocopherol) and good precision (0.2-0.3% for retention time, 1.8-3.4% for peak area, 2.6-2.7% for peak height), and also offered much better performance than unmodified MIL-101(Cr) and commercial amino-bonded silica packed column for HPLC separation of tocopherols. The results not only show the promising application of pyridine-grafted MIL-101(Cr) as a novel stationary phase for HPLC separation of tocopherols, but also reveal a facile post-modification of MOFs to expand the application of MOFs in separation sciences. Copyright © 2015 Elsevier B.V. All rights reserved.

HPLC-PFD determination of priority pollutant PAHs in water, sediment, and semipermeable membrane devices

Science.gov (United States)

Williamson, K.S.; Petty, J.D.; Huckins, J.N.; Lebo, J.A.; Kaiser, E.M.

2002-01-01

High performance liquid chromatography coupled with programmable fluorescence detection was employed for the determination of 15 priority pollutant polycyclic aromatic hydrocarbons (PPPAHs) in water, sediment, and semipermeable membrane devices (SPMDs). Chromatographic separation using this analytical method facilitates selectivity, sensitivity (ppt levels), and can serve as a non-destructive technique for subsequent analysis by other chromatographic and spectroscopic techniques. Extraction and sample cleanup procedures were also developed for water, sediment, and SPMDs using various chromatographic and wet chemical methods. The focus of this publication is to examine the enrichment techniques and the analytical methodologies used in the isolation, characterization, and quantitation of 15 PPPAHs in different sample matrices.

Assessment of the chromatographic lipophilicity of eight cephalosporins on different stationary phases.

Science.gov (United States)

Dąbrowska, Monika; Starek, Małgorzata; Komsta, Łukasz; Szafrański, Przemysław; Stasiewicz-Urban, Anna; Opoka, Włodzimierz

2017-04-01

The retention behaviors were investigated for a series of eight cephalosporins in thin-layer chromatography (TLC) using stationary phases of RP-2, RP-8, RP-18, NH 2 , DIOL, and CN chemically bonded silica gel. Additionally, various binary mobile phases (water/methanol and water/acetone) were used in different volume proportions. The retention behavior of the analyzed molecules was defined by R M0 constant. In addition, reversed phase high performance liquid chromatography (RP-HPLC) was performed in lipophilicity studies by using immobilized artificial membrane (IAM) stationary phase. Obtained chromatographic data (R M0 and logk' IAM ) were correlated with the lipophilicity, expressed as values of the log calculated (logP calc ) and experimental (logP exp(shake-flask) ) partition coefficient. Principal component analysis (PCA) was applied in order to obtain an overview of similarity or dissimilarity among the analyzed compounds. Hierarchical cluster analysis (HCA) was performed to compare the separation characteristics of the applied stationary phases. This study was undertaken to identify the best chromatographic system and chromatographic data processing method to enable the prediction of logP values. A comprehensive chromatographic investigation into the retention of the analyzed cephalosporins revealed a similar behavior on RP-18, RP-8 and CN stationary phases. The weak correlations obtained between experimental and certain computed lipophilicity indices revealed that R M0 and PC1/RM are relevant lipophilicity parameters and the RP-8, CN and RP-18 plates are appropriate stationary phases for lipophilicity investigation, whereas computational approaches still cannot fully replace experimentation. Copyright © 2017 Elsevier B.V. All rights reserved.

Chromatographic and electrophoretic approaches in ink analysis.

Science.gov (United States)

Zlotnick, J A; Smith, F P

1999-10-15

Inks are manufactured from a wide variety of substances that exhibit very different chemical behaviors. Inks designed for use in different writing instruments or printing methods have quite dissimilar components. Since the 1950s chromatographic and electrophoretic methods have played important roles in the analysis of inks, where compositional information may have bearing on the investigation of counterfeiting, fraud, forgery, and other crimes. Techniques such as paper chromatography and electrophoresis, thin-layer chromatography, high-performance liquid chromatography, gas chromatography, gel electrophoresis, and the relatively new technique of capillary electrophoresis have all been explored as possible avenues for the separation of components of inks. This paper reviews the components of different types of inks and applications of the above separation methods are reviewed.

Liquid phase chromatography on microchips

DEFF Research Database (Denmark)

Kutter, Jörg Peter

2012-01-01

explosive development of, in particular, chromatographic separation systems on microchips, has, however, slowed down in recent years. This review takes a closer, critical look at how liquid phase chromatography has been implemented in miniaturized formats over the past several years, what is important...

Method for the conversion of hydrocarbon charges

Energy Technology Data Exchange (ETDEWEB)

Whittam, T V

1976-11-11

The basis of the invention is the application of defined zeolites as catalysts to hydrocarbon conversion processes such as reformation, isomerization, dehydrocyclization, and cracking. By charging the zeolite carrier masses with 0.001 to 5% metal of the 8th group of the periodic system, preferably noble metals, a wide region of applications for the catalysts is achieved. A method for the isomerization of an alkyl benzene (or mixture of alkyl benzenes) in the liquid or gas phase under suitable temperature, pressure and flow-rate conditions, as well as in the presence of a cyclic hydrocarbon, is described as preferential model form of the invention; furthermore, a method for the reformation of a hydrocarbon fraction boiling in the gasoline or benzene boiling region and a method for the hydrocracking of hydrocarbon charge (e.g. naphtha, kerosine, gas oils) are given. Types of performance of the methods are explained using various examples.

New high performance liquid chromatographic method for simultaneous determination of diclofenac and meloxicam in oral formulation of liposomes and human plasma

International Nuclear Information System (INIS)

Madni, A.; Ahmad, M.; Usman, M.; Zubair, M.M.; Shoiab, H.M.; Khan, S.A.; Qureshi, M.S.

2010-01-01

A new, easy and consistent reversed-phase high-performance liquid chromatographic method with diode array detection has been developed and validated for the simultaneous determination of diclofenac potassium (DP) and meloxicam (MLX) in liposome, marketed brands and human plasma. Microextraction method based on liquid-liquid extraction principal was used to extract drug from plasma matrix. The optimized mobile phase was used in the molar ratio of 20:20:60 (v/v/v) mixture of acetonitrile, methanol and 20 x 10/sup -3/ M potassium dihydrogen phosphate buffer (pH 3.7), pumped at an optimized flow rate of 1.0 mL.min/sup -1/. The linearity was performed in the concentration range of 15 ng.mL/sup -1/ to 10 mu g.mL/sup -1/ with gamma/sup 2/ of 0.9989 +- 0.13 and 0.9979 +- 0.11 (n = 6) for DP and MLX, respectively. The assay was repeatable at concentration levels of 10 ng.mL/sup -1/, 1 mu g.mL/sup -1/ and 10 mu g.mL/sup -1/ with coefficient of variation of 0.168 - 0.603% for 10 ng.mL-1 (DP), 15 ng.mL/sup -/1 (MLX) and 1 mu g.mL/sup -1/ and 10 mu g.mL/sup -1/ for DP and MLX. The LOD values were 3 and 5 ng.mL/sup -1/, while values of LOQ were 10 and 15 ng.mL/sup =11, for DP and MLX. The present method is applicable in routine quality control operations, advanced drug delivery formulations (Liposomes) and in human Plasma samples for pharmacokinetics and bioequivalence studies. (author)

A novel strategy for the determination of polycyclic aromatic hydrocarbon monohydroxylated metabolites in urine using ultra-high-performance liquid chromatography with tandem mass spectrometry.

Czech Academy of Sciences Publication Activity Database

Lanková, D.; Urbancová, K.; Šrám, Radim; Hajslová, J.; Pulkrabová, J.

2016-01-01

Roč. 408, č. 10 (2016), s. 2515-2525 ISSN 1618-2642 R&D Projects: GA ČR(CZ) GA13-13458S Institutional support: RVO:68378041 Keywords : monohydroxylated metabolites of polycyclic aromatic hydrocarbons * SRM 3673 * tandem mass spectrometry * ultra-high-performance liquid chromatography * urine Subject RIV: DN - Health Impact of the Environment Quality Impact factor: 3.431, year: 2016

Atmospheric chlorinated polycyclic aromatic hydrocarbons in East Asia.

Science.gov (United States)

Kakimoto, Kensaku; Nagayoshi, Haruna; Konishi, Yoshimasa; Kajimura, Keiji; Ohura, Takeshi; Hayakawa, Kazuichi; Toriba, Akira

2014-09-01

This study estimates atmospheric concentrations of chlorinated polycyclic aromatic hydrocarbons (ClPAHs) and polycyclic aromatic hydrocarbons (PAHs) in East Asia using a Gas Chromatograph with High Resolution Mass Spectrometer (GC-HRMS). ClPAHs are ubiquitously generated from PAHs through substitution, and some ClPAHs show higher aryl hydrocarbon receptor (AhR)-mediated activities than their parent PAHs. Atmospheric particles were collected using a high-volume air sampler equipped with a quartz-fiber filter. We determined the ClPAH concentrations of atmospheric particles collected in Japan (Sapporo, Sagamihara, Kanazawa, and Kitakyushu), Korea (Busan), and China (Beijing). The concentrations of ClPAHs were highest in the winter Beijing sample, where the total mean concentration was approximately 15-70 times higher than in the winter samples from Japan and Korea. The concentrations of Σ19ClPAHs and Σ9PAHs were significantly correlated in the Kanazawa and the Busan samples. This indicates that within those cities ClPAHs and PAHs share the same origin, implying direct chlorination of parent PAHs. Toxic equivalent concentrations (TEQs) of the total ClPAHs and PAHs were lowest in Kanazawa in the summer, reaching 1.18 and 2610fg-TEQm(-3) respectively, and highest in Beijing in the winter, reaching 627 and 4240000fg-TEQm(-3) respectively. Copyright © 2014 Elsevier Ltd. All rights reserved.

In-syringe dispersive liquid-liquid microextraction with liquid chromatographic determination of synthetic pyrethroids in surface water

Directory of Open Access Journals (Sweden)

Saeed S. Albaseer

2012-03-01

Full Text Available An indigenously fabricated in laboratory glass syringe was used for in-syringe dispersive liquid-liquid microextraction (is-DLLME and preconcentration of synthetic pyrethroids (SPs from surface waters suitable for their determination by high performance liquid chromatography. In contrast to classical DLLME, is-DLLME allows the use of lighter-than-water organic solvents and the analysis of environmental contaminants’ samples without prior filtration, which is of great importance due to the high affinity of pyrethroids to adsorb to solid particulates present in environmental samples. The effects of various parameters on the extraction efficiency were evaluated and optimized systemically using one-factor-at-a-time method (OFAT and statistically using full factorial design (24. Three SPs (viz.; cypermethrin, resmethrin and permethrin were analyzed. The method showed good accuracy with RSD% in the range of of 4.8–6.9%. The method detection limits of the three pesticides ranged from 0.14 to 0.16 ng mL-1. The proposed method was applied for the determination of synthetic pyrethroids in lake water

Characterization of polycyclic aromatic hydrocarbons (PAH's) present in sampled cooked food

International Nuclear Information System (INIS)

Palm Naa-Dedei, L.M.

2010-07-01

The study was conducted to determine the levels of Polycyclic Aromatic Hydrocarbons in the following traditionally prepared food: smoked and grilled Scomba japonicus, grilled meat (khebab) and bread sampled from some Ghanaian markets. By way of preparation of traditional food, some food comes into direct contact with smoke or extremely high temperature which are potential sources of Polycyclic Aromatic Hydrocarbon generation. Levels of 20 individual Polycyclic Aromatic Hydrocarbons including acenaphthene, acenaphtyelene, anthanthrene, anthracene, benz(a)anthracene, benzo(a)pyrene, benzo(b)fluoranthene, benzo(e)pyrene, benzo(ghi)perylene, benzo(j)fluoranthene, benzo(k)fluoranthene, chrysene, cyclopenta(cd)pyrene, dibenzo(ah)anthracene, fluoranthene, fluorene, indeno(1,2,3-cd)pyrene, naphthalene, phenanthrene and pyrene were determined in 11 smoked and 5 grilled fish, 4 grilled pieces of meat and 3 loaves of baked bread using gas chromatographic techniques with flame ionization detector. Benzo(a)pyrene, which is one of the few PAH for which a legal limit exists in different types of food matrices and other high molecular weight PAHs suspected to be carcinogenic have been detected in high concentrations in most samples. Bread samples gave mean polycyclic aromatic hydrocarbon concentrations of up to 20.39 μg/kg while khebab samples gave mean polycyclicaromatic hydrocarbon concentrations of up to 67.61 μg/kg. There was positive correlation of 0.987 between levels of polycyclic aromatic hydrocarbon concentrations in khebab samples from locations Osu and Atomic down. There was a positive correlation in the concentrations of the high molecular weight PAHs in all smoked fishes from four locations with values between 0.954 and 0.999 for the correlation between any two groups. The polycyclic aromatic hydrocarbon concentration determined in smoked fish samples deceased in terms of location according to the order Winneba > Madina > Chorkor > Ada.

Alkylsulfate-based ionic liquids in the liquid–liquid extraction of aromatic hydrocarbons

International Nuclear Information System (INIS)

García, Silvia; Larriba, Marcos; García, Julián; Torrecilla, José S.; Rodríguez, Francisco

2012-01-01

Highlights: ► Values of α 2,1 for the four R-SO 4 ionic liquids are higher than those of sulfolane. ► Values of D 2 for all the ionic liquids are lower than those of sulfolane. ► Values of D 2 for [emim][C 2 H 5 SO 4 ] are the highest among the R-SO 4 ionic liquids. - Abstract: The (liquid + liquid) equilibrium data (LLE) for the extraction of toluene from heptane with different ionic liquids (ILs) based on the alkylsulfate anion (R-SO 4 ) was determined at T = 313.2 K and atmospheric pressure. The effect of more complex R-SO 4 anions on capacity of extraction and selectivity in the liquid–liquid extraction of toluene from heptane was studied. The ternary systems were formed by {heptane + toluene + 1,3-dimethylimidazolium methylsulfate ([mmim][CH 3 SO 4 ]), 1-ethyl-3-methylimidazolium hydrogensulfate ([emim][HSO 4 ]), 1-ethyl-3-methylimidazolium methylsulfate ([emim][CH 3 SO 4 ]), or 1-ethyl-3-methylimidazolium ethylsulfate ([emim][C 2 H 5 SO 4 ])}. The degree of quality of the experimental LLE data was ascertained by applying the Othmer–Tobias correlation. The phase diagrams for the ternary systems were plotted, and the tie lines correlated with the NRTL model compare satisfactorily with the experimental data.

Precolumn derivatization followed by liquid chromatographic separation and determination of tramiprosate in rat plasma by fluorescence detector: application to pharmacokinetics.

Science.gov (United States)

Rao, R Nageswara; Maurya, Pawan K; Shinde, Dhananjay D; Khalid, Sara

2011-05-15

Alzheimer disease (AD) is characterized pathologically by extracellular amyloid deposits composed of amyloid β (Aβ) protein. A simple and rapid method using HPLC with fluorescence detector was developed and validated for determination of tramiprosate in rat plasma. Pre-column derivatization of the deproteinized rat plasma was carried out using o-phthaldialdehyde (OPA) as a fluorescent reagent in presence of 3-mercaptopropionic acid. The liquid chromatographic separation was achieved on a Kromasil C18 column using methanol:acetonitrile: 20 mM phosphate buffer pH 7.5 (8.0:17.5:74.5 v/v/v) as a mobile phase in an isocratic elution mode. The eluents were monitored by a fluorescence detector set at 330 and 450 nm of excitation and emission wavelength respectively. Vigabatrin was used as an internal standard. The method was linear within the range 30.0-1000.0 ng/mL. Design of experiments (DOE) was used to evaluate the robustness of the method. The developed method was applied to study the pharmacokinetics of tramiprosate in rats. Copyright © 2011. Published by Elsevier B.V.

Trace determinations of individual organic pollutants - 25 years of research at the Swiss Federal Institute for Environmental Science and Technology (EAWAG)

Energy Technology Data Exchange (ETDEWEB)

Giger, W. [Swiss Federal Inst. for Environmental Science and Technology (EAWAG), Duebendorf (Switzerland)

1997-12-01

An overview is given on analytical developments and applications for the determination of organic trace pollutants which have been performed at EAWAG since 1972. Gas and liquid chromatographic methods are of crucial importance. The presented examples include environmental hydrocarbons, semivolatile compounds and detergent-derived chemicals. (author) 4 figs., 1 tab., 6 refs.

Principles of qualitative analysis in the chromatographic context.

Science.gov (United States)

Valcárcel, M; Cárdenas, S; Simonet, B M; Carrillo-Carrión, C

2007-07-27

This article presents the state of the art of qualitative analysis in the framework of the chromatographic analysis. After establishing the differences between two main classes of qualitative analysis (analyte identification and sample classification/qualification) the particularities of instrumental qualitative analysis are commented on. Qualitative chromatographic analysis for sample classification/qualification through the so-called chromatographic fingerprint (for complex samples) or the volatiles profile (through the direct coupling headspace-mass spectrometry using the chromatograph as interface) is discussed. Next, more technical exposition of the qualitative chromatographic information is presented supported by a variety of representative examples.

Multiple-channel ultra-violet absorbance detector for two-dimensional chromatographic separations.

Science.gov (United States)

Lynch, Kyle B; Yang, Yu; Ren, Jiangtao; Liu, Shaorong

2018-05-01

In recent years, much research has gone into developing online comprehensive two-dimensional liquid chromatographic systems allowing for high peak capacities in comparable separation times to that of one-dimensional liquid chromatographic systems. However, the speed requirements in the second dimension (2nd-D) still remain one challenge for complex biological samples due to the current configuration of two column/two detector systems. Utilization of multiple 2nd-D columns can mitigate this challenge. To adapt this approach, we need a multiple channel detector. Here we develop a versatile multichannel ultraviolet (UV) light absorbance detector that is capable of simultaneously monitoring separations in 12 columns. The detector consists of a deuterium lighthouse, a flow cell assembly (a 13-channel flow cell fitted with a 13-photodiode-detection system), and a data acquisition and monitoring terminal. Through the use of a custom high optical quality furcated fiber to improve light transmission, precise machining of a flow cell to reduce background stray light through precision alignment, and sensitive electronic circuitry to reduce electronic noise through an active low pass filter, the background noise level is measured in the tens of µAU. We obtain a linear dynamic range of close to three orders of magnitude. Compared to a commercialized multichannel UV light absorbance detector like the Waters 2488 UV/Vis, our device provides an increase in channel detection while residing within the same noise region and linear range. Copyright © 2018 Elsevier B.V. All rights reserved.

Automation of an ion chromatograph for precipitation analysis with computerized data reduction

Science.gov (United States)

Hedley, Arthur G.; Fishman, Marvin J.

1982-01-01

Interconnection of an ion chromatograph, an autosampler, and a computing integrator to form an analytical system for simultaneous determination of fluoride, chloride, orthophosphate, bromide, nitrate, and sulfate in precipitation samples is described. Computer programs provided with the integrator are modified to implement ionchromatographic data reduction and data storage. The liquid-flow scheme for the ion chromatograph is changed by addition of a second suppressor column for greater analytical capacity. An additional vave enables selection of either suppressor column for analysis, as the other column is regenerated and stabilized with concentrated eluent.Minimum limits of detection and quantitation for each anion are calculated; these limits are a function of suppressor exhaustion. Precision for replicate analyses of six precipitation samples for fluoride, chloride, orthophosphate, nitrate, and sulfate ranged from 0.003 to 0.027 milligrams per liter. To determine accuracy of results, the same samples were spiked with known concentrations of the above mentioned anions. Average recovery was 108 percent.

Liquid chromatographic determination of para-toluenesulfonamide in edible fillet tissues from three species of fish

Science.gov (United States)

Meinertz, J.R.; Schmidt, L.J.; Stehly, G.R.; Gingerich, W.H.

1999-01-01

Chloramine-T (N-sodium-N-chloro-p-toluene-sulfonamide) is a candidate therapeutic drug for treating bacterial gill disease, a predominant disease of a variety of fish species. Research has been initiated to obtain the U.S. Food and Drug Administration's (FDA) approval for the use of chloramine-T on a variety of fish species. An attribute of a therapeutic aquaculture drug that must be characterized before the FDA approves its use is depletion of the drug's marker residue (the drug's parent compound or metabolite of highest concentration in an edible tissue). Para-Toluenesulfonamide (p-TSA) is the primary degradation product and marker residue for chloramine-T in rainbow trout. To conduct residue depletion studies for chloramine-T in fish, a robust analytical method sensitive and specific for p-TSA residues in edible fillet tissue from a variety of fish was required. Homogenized fillet tissues from rainbow trout (Oncorhynchus mykiss), walleye (Stizostedion vitreum), and channel catfish (Ictalurus punctatus) were fortified at nominal p-TSA concentrations of 17, 67, 200, 333, and 1000 ng/g. Samples were analyzed by isocratic reversed-phase liquid chromatography (LC) with absorbance detection at 226 nm. Mean recoveries of p-TSA ranged from 77 to 93.17%; relative standard deviations ranged from 1.5 to 14%; method quantitation limits ranged from 13 to 18 ng/g; and method detection limits ranged from 3.8 to 5.2 ng/g. The LC parameters produced p-TSA peaks without coelution of endogenous compounds and excluded chromatographic interference from at least 20 chemicals and drugs of potential use in aquaculture.

Biotransformation of the polycyclic aromatic hydrocarbon pyrene by the marine polychaete Nereis virens

DEFF Research Database (Denmark)

Jørgensen, Anne; Giessing, Anders M. B.; Rasmussen, Lene Juel

2005-01-01

In vivo and in vitro biotransformation of the polycyclic aromatic hydrocarbon (PAH) pyrene was investigated in the marine polychaete Nereis virens. Assays were designed to characterize phase I and II enzymes isolated from gut tissue. High-pressure liquid chromatography measurement of 1-hydroxypyr......In vivo and in vitro biotransformation of the polycyclic aromatic hydrocarbon (PAH) pyrene was investigated in the marine polychaete Nereis virens. Assays were designed to characterize phase I and II enzymes isolated from gut tissue. High-pressure liquid chromatography measurement of 1...

UPLC and LC-MS studies on degradation behavior of irinotecan hydrochloride and development of a validated stability-indicating ultra-performance liquid chromatographic method for determination of irinotecan hydrochloride and its impurities in pharmaceutical dosage forms.

Science.gov (United States)

Kumar, Navneet; Sangeetha, Dhanaraj; Reddy, Sunil P

2012-10-01

The objective of the current investigation was to study the degradation behavior of irinotecan hydrochloride under different International Conference on Harmonization (ICH) recommended stress conditions using ultra-performance liquid chromatography and liquid chromatography-mass spectrometry and to establish a validated stability-indicating reverse-phase ultra-performance liquid chromatographic method for the quantitative determination of irinotecan hydrochloride and its seven impurities and degradation products in pharmaceutical dosage forms. Irinotecan hydrochloride was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. Irinotecan hydrochloride was found to degrade significantly in oxidative and base hydrolysis and photolytic degradation conditions. The degradation products were well resolved from the main peak and its impurities, thus proving the stability-indicating power of the method. Chromatographic separation was achieved on a Waters Acquity BEH C8 (100 × 2.1 mm) 1.7-µm column with a mobile phase containing a gradient mixture of solvent A (0.02M KH(2)PO(4) buffer, pH 3.4) and solvent B (a mixture of acetonitrile and methanol in the ratio of 62:38 v/v). The mobile phase was delivered at a flow rate of 0.3 mL/min with ultraviolet detection at 220 nm. The run time was 8 min, within which irinotecan and its seven impurities and degradation products were satisfactorily separated. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision and robustness. This method was also suitable for the assay determination of irinotecan hydrochloride in pharmaceutical dosage forms.

Chromatographic Separations of Enantiomers and Underivatized Oligosaccharides

Energy Technology Data Exchange (ETDEWEB)

Liu, Ying [Iowa State Univ., Ames, IA (United States)

2004-01-01

My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic

Chromatographic Separations of Enantiomers and Underivatized Oligosaccharides

International Nuclear Information System (INIS)

Ying Liu

2004-01-01

My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic

Detection and identification of radiation induced hydrocarbons in meets with the use of gas chromatography as one of methods for the detection of irradiated food

International Nuclear Information System (INIS)

Lehner, K.; Stachowicz, W.

2000-01-01

Results of the determination of the content of radiation induced hydrocarbons in meat samples (chicken, pork, beef) as well as proportion between the concentration of individual hydrocarbons in relation to the content of fatty acids in a given product are presented. The measurements have been done with the use of a Perkin Elmer model 8700 gas chromatograph equipped with a FID detector. The present study is a preliminary work on the implementation of a routine method for the detection of irradiation in foods that contain fats. (author)

Versatile ligands for high-performance liquid chromatography: An overview of ionic liquid-functionalized stationary phases.

Science.gov (United States)

Zhang, Mingliang; Mallik, Abul K; Takafuji, Makoto; Ihara, Hirotaka; Qiu, Hongdeng

2015-08-05

Ionic liquids (ILs), a class of unique substances composed purely by cation and anions, are renowned for their fascinating physical and chemical properties, such as negligible volatility, high dissolution power, high thermal stability, tunable structure and miscibility. They are enjoying ever-growing applications in a great diversity of disciplines. IL-modified silica, transforming the merits of ILs into chromatographic advantages, has endowed the development of high-performance liquid chromatography (HPLC) stationary phase with considerable vitality. In the last decade, IL-functionalized silica stationary phases have evolved into a series of branches to accommodate to different HPLC modes. An up-to-date overview of IL-immobilized stationary phases is presented in this review, and divided into five parts according to application mode, i.e., ion-exchange, normal-phase, reversed-phase, hydrophilic interaction and chiral recognition. Specific attention is channeled to synthetic strategies, chromatographic behavior and separation performance of IL-functionalized silica stationary phases. Copyright © 2015 Elsevier B.V. All rights reserved.

Hydrocarbon contamination of coastal sediments from the Sfax area (Tunisia), Mediterranean Sea.

Science.gov (United States)

Louati, A; Elleuch, B; Kallel, M; Saliot, A; Dagaut, J; Oudot, J

2001-06-01

The coastal area off the city of Sfax (730,000 inhabitants), well-known for fisheries and industrial activities, receives high inputs of organic matter mostly anthropogenic. Eighteen stations were selected in the vicinity of the direct discharge of industrial sewage effluents in the sea in order to study the spatial distribution of the organic contamination. Surface sediments sampled in the shallow shelf were analysed for hydrocarbons by Fourier transform infrared spectroscopy, gas chromatography and gas chromatography/mass spectrometry. Total hydrocarbon distributions revealed high contamination as compared to other coastal Mediterranean sites, with an average concentration of 1865 ppm/dry weight sediment. Gas chromatographic distribution patterns, values of unresolved mixture/n-alkane ratio and distributions of steranes and hopanes confirmed a petroleum contamination of the Arabian light crude oil type. Biogenic compounds were also identified with a series of short-chain carbon-numbered n-alkenes in the carbon range 16-24.

Screening of extremotolerant fungi for the bioremediation of hydrocarbon contaminated sites

Science.gov (United States)

Poyntner, Caroline; Blasi, Barbara; Prenafeta, Francesc; Sterflinger, Katja

2015-04-01

Bioremediation can be used to treat contaminated sites, by taking advantage of microorganisms which have the potential to degrade a wide range of contaminants. While research has been focused mainly on bacteria, the knowledge on other microorganisms, especially fungal communities, is still limited. However, the use of fungi may have advantages compared to bacteria. Extremophile fungi like the black yeasts can withstand high levels of environmental stress (e.g. range of pH, water availability and temperature, presence of toxic chemicals). Therefore they might be applicable in situations, where bacterial communities show limited performance. In order to identify fungi which are good candidates for bioremediation application, a selection of 163 fungal strains, mostly from the group of the black yeasts, was tested for their capability to degrade three different pollutants: hexadecane, toluene, and polychlorinated biphenyl 126, which were used as model compounds for aliphatic hydrocarbons, aromatic hydrocarbons and polychlorinated biphenyls. These chemicals are frequently found in sites contaminated by oil, gas and coal. The screening was based on a two-step selection approach. As a first step, a high throughput method was developed to screen the relatively large amount of fungal strains regarding their tolerance to the contaminants. A microtiter plate based method was developed for monitoring fungal growth in the presence of the selected contaminants photometrically with a Tecan reader. Twenty five strains out of 163, being species of the genera Cladophilaophora, Scedosporium and Exophiala, showed the ability to grow on at least 2 hydrocarbons, and are therefore the most promising candidates for further tests. In a second step, degradation of the contaminants was investigated in more detail for a subset of the screened fungi. This was done by closing the carbon balance in sealed liquid cultures in which the selected pollutant was introduce as the sole source of carbon

Liquid-Phase Electrical Discharges: Fundamental Mechanisms and Applications

Science.gov (United States)

Franclemont, Joshua

The increased demand in alternative energy in recent decades has generated significant interest in cleaner fuel sources including hydrogen and syngas (hydrogen and carbon monoxide). Hydrogen and syngas are both primarily produced through the steam reforming of hydrocarbons, specifically natural gas. Although other processes are known, the cheapest source of these fuels is currently through the heating of natural gas in the presence of steam and a catalyst. However, due to the emissions associated with the steam reforming of natural gas and the lack of low cost, efficient, and reliable onboard hydrogen storage technologies for fuel cell powered vehicles, attention has been focused on plasma-assisted reforming of hydrocarbons. Plasma processes can be implemented onboard and are able to directly reform liquid hydrocarbons and alcohols without external heating or catalysts. In addition to hydrogen and syngas, the plasma-assisted reforming of hydrocarbons and alcohols offers other desirable products such as C2 gases (ethane, ethylene, and acetylene), methanol and ethanol. The primary goal of this study is to investigate the fundamental chemical reactions occurring during plasma-assisted reforming of liquid hydrocarbons and alcohols using streamer-like pulsed electrical discharges. Due to the relatively unexplored field of chemical reactions in liquid plasmas, the focus of this study is on elucidating chemical pathways responsible for the formation of hydrogen, syngas, and other products during the direct reforming of liquid methanol, glycerol, and pentane as model species.

Quantitative Analysis of Matrine in Liquid Crystalline Nanoparticles by HPLC

Directory of Open Access Journals (Sweden)

Xinsheng Peng

2014-01-01

Full Text Available A reversed-phase high-performance liquid chromatographic method has been developed to quantitatively determine matrine in liquid crystal nanoparticles. The chromatographic method is carried out using an isocratic system. The mobile phase was composed of methanol-PBS(pH6.8-triethylamine (50 : 50 : 0.1% with a flow rate of 1 mL/min with SPD-20A UV/vis detector and the detection wavelength was at 220 nm. The linearity of matrine is in the range of 1.6 to 200.0 μg/mL. The regression equation is y=10706x-2959 (R2=1.0. The average recovery is 101.7%; RSD=2.22%  (n=9. This method provides a simple and accurate strategy to determine matrine in liquid crystalline nanoparticle.

Syngas Conversion to Gasoline-Range Hydrocarbons over Pd/ZnO/Al2O3 and ZSM-5 Composite Catalyst System

Energy Technology Data Exchange (ETDEWEB)

Dagle, Robert A.; Lizarazo Adarme, Jair A.; Lebarbier, Vanessa MC; Gray, Michel J.; White, James F.; King, David L.; Palo, Daniel R.

2014-07-01

A composite Pd/ZnO/Al2O3-HZSM-5 (Si/Al=40) catalytic system was evaluated for the synthesis of gasoline-range hydrocarbons directly from synthesis gas. Bifunctional catalyst comprising PdZn metal and acid sites present the required catalytically active sites necessary for the methanol synthesis, methanol dehydration, and methanol-to-gasoline reactions. This system provides a unique catalytic pathway for the production of liquid hydrocarbons directly from syngas. However, selectivity control is difficult and poses many challenges. The composite catalytic system was evaluated under various process conditions. Investigated were the effects of temperature (310-375oC), pressure (300-1000 psig), time-on-stream (50 hrs), and gas-hour space velocity (740-2970 hr-1), using a H2/CO molar syngas ratio of 2.0. By operating at the lower end of the temperature range investigated, liquid hydrocarbon formation was favored, as was decreased amounts of undesirable light hydrocarbons. However, lower operating temperatures also facilitated undesirable CO2 formation via the water-gas shift reaction. Higher operating pressures slightly favored liquid synthesis. Operating at relatively low pressures (e.g. 300 psig) was made possible, whereas for methanol synthesis alone higher pressure are usually required to achieve similar conversion levels (e.g. 1000 psig). Thermodynamic constraints on methanol synthesis are eased by pushing the equilibrium through hydrocarbon formation. Catalytic performance was also evaluated by altering Pd and Zn composition of the Pd/ZnO/Al2O3 catalyst. Of the catalysts and conditions tested, selectivity toward liquid hydrocarbon was highest when using a 5% Pd metal loading and Pd/Zn molar ratio of 0.25 and mixed with HZMS-5, operating at 310oC and 300 psig, CO conversion was 43 % and selectivity (carbon weight basis) to hydrocarbons was 49 wt. %. Of the hydrocarbon fraction, 44wt. % was in the C5-C12 liquid product range and consisted primarily of aromatic

Measurements of activity coefficients at infinite dilution of aliphatic and aromatic hydrocarbons, alcohols, thiophene, tetrahydrofuran, MTBE, and water in ionic liquid [BMIM][SCN] using GLC

International Nuclear Information System (INIS)

Domanska, Urszula; Laskowska, Marta

2009-01-01

The activity coefficients at infinite dilution, γ 13 ∞ for 32 solutes: alkanes, alken-1-es, alkyn-1-es, cycloalkanes, aromatic hydrocarbons, alcohols, thiophene, tetrahydrofuran, tert-butyl methyl ether, and water in the ionic liquid 1-butyl-3-methylimidazolium thiocyanate [BMIM][SCN] were determined by gas-liquid chromatography at the temperatures from 298.15 K to 368.15 K. The values of the partial molar excess enthalpies at infinite dilution ΔH 1 E,∞ were calculated from the experimental γ 13 ∞ values obtained over the temperature range. The selectivities for the hexane/benzene, cyclohexane/benzene, hexane/thiophene, and other separation problems were calculated from the γ 13 ∞ and compared to the other ionic liquids, N-methyl-2-pyrrolidinone, and sulfolane, taken from the recent literature. This work demonstrates that with chosen ionic liquid it is possible to separate different organic compounds with the highest selectivity, ever published

Plasma Reforming of Liquid Hydrocarbon Fuels in Non-Thermal Plasma-Liquid Systems

Science.gov (United States)

2010-04-30

channel with liquid wall in the microporous media under the ultrasound cavitations has shown the following: · The action of the ultrasound field in the...microporous liquid which has a very large ratio of the plasma-liquid contact surface to the plasma volume. As is known the ultrasonic (US) cavitation is a very...2) and it ran over a flat dielectric surface of the magnetostrictive transmitter (5) which produced ultrasonic (US) cavitations , so the discharge

UHPLC: The Greening Face of Liquid Chromatography.

Science.gov (United States)

Cielecka-Piontek, Judyta; Zalewski, Przemysław; Jelińska, Anna; Garbacki, Piotr

2013-01-01

Pharmaceutical analysis based on chromatographic separation is an important part of studies aimed at developing routine quality analysis of drugs. High-performance liquid chromatography (HPLC) is one of the main analytical techniques recommended for drug analysis. Although it meets many criteria vital for analysis, it is time-consuming and uses a relatively high amount of organic solvents compared to other analytical techniques. Recently, Ultra-high-performance liquid chromatography (UHPLC) has been frequently proposed as an alternative to HPLC, which means introducing an environment-friendly approach to drug analysis achieved by reducing the consumption of solvents. It also offers greater chromatographic resolution and higher sensitivity as well as requiring less time due to faster analysis. This review focuses on the basics of UHPLC, compares that technique with HPLC and discusses the possibilities of applying UHPLC for the analysis of different pharmaceuticals and biopharmaceuticals.

Direct coupling of a dense (supercritical) gas chromatograph to a mass spectrometer using a supersonic molecular beam interface

International Nuclear Information System (INIS)

Randall, L.G.; Wahrhaftig, A.L.

1981-01-01

A detecting mass spectrometer has been successfully coupled to a dense gas (supercritical fluid) chromatograph to produce an instrument (DGC/MS) that may be an alternative to high performance liquid chromatograph/mass spectrometer instruments (HPLC/MS) and gas chromatograph/mass spectrometer instruments (GC/MS) for analysis of involatile and/or thermally labile compounds. The mobile phase in DGC is a gas held at temperatures above the critical temperature and at pressures sufficient to obtain nearly liquid-like densities. DGC combines advantages of GC and HPLC: rapid separations, moderate operating temperatures, and analysis of involatile compounds. An advantage unique to DGC is the solvent power dependence upon pressure. While several groups have studied DGC, its development has been limited by the lack of a sensitive and selective detector. Hence, work has been directed towards the design and construction of a DGC/MS resulting in a trial instrument capable of chromatographic pressures of at least 300 atm and temperatures from 10 0 to 60 0 C. The DGC/MS coupling has been accomplished by the use of a supersonic molecular beam interface. This application of molecular beam formation appears to be unique in its requirements of a large pressure ratio (approx.10 8 ), low flow rates, and low final pressures. The authors outline characteristics of supersonic jets and molecular beams pertinent to the design of such an instrument. The interface which uses pumping speeds of 2400 and 1200 l/s in the beam forming chambers is described in detail, while the other components: the detecting mass spectrometer, the dense gas supply, and the DGC: are briefly described. Preliminary work with this instrument has established the feasibility of DGC/MS as an analytical technique and further development is recommended

Fundamentals of Delayed Coking Joint Industry Project

Energy Technology Data Exchange (ETDEWEB)

Volk Jr., Michael; Wisecarver, Keith D.; Sheppard, Charles M.

2003-02-07

The coking test facilities include three reactors (or cokers) and ten utilities. Experiments were conducted using the micro-coker, pilot-coker, and stirred-batch coker. Gas products were analyzed using an on-line gas chromatograph. Liquid properties were analyzed in-house using simulated distillation (HP 5880a), high temperature gas chromatography (6890a), detailed hydrocarbon analysis, and ASTM fractionation. Coke analyses as well as feedstock analyses and some additional liquid analyses (including elemental analyses) were done off-site.

Liquid fuels production from biomass. Final report

Energy Technology Data Exchange (ETDEWEB)

Levy, P. F.; Sanderson, J. E.; Ashare, E.; Wise, D. L.; Molyneaux, M. S.

1980-06-30

The current program to convert biomass into liquid hydrocarbon fuels is an extension of a previous program to ferment marine algae to acetic acid. In that study it was found that marine algae could be converted to higher aliphatic organic acids and that these acids could be readily removed from the fermentation broth by membrane or liquid-liquid extraction. It was then proposed to convert these higher organic acids via Kolbe electrolysis to aliphatic hydrocarbons, which may be used as a diesel fuel. The specific goals for the current porgram are: (1) establish conditions under which substrates other than marine algae may be converted in good yield to organic acids, here the primary task is methane suppression; (2) modify the current 300-liter fixed packed bed batch fermenter to operate in a continuous mode; (3) change from membrane extraction of organic acids to liquid-liquid extraction; (4) optimize the energy balance of the electrolytic oxidation process, the primary task is to reduce the working potential required for the electrolysis while maintaining an adequate current density; (5) scale the entire process up to match the output of the 300 liter fermenter; and (6) design pilot plant and commercial size plant (1000 tons/day) processes for converting biomass to liquid hydrocarbon fuels and perform an economic analysis for the 1000 ton/day design.

Alternative Hydrocarbon Propulsion for Nano / Micro Launch Vehicle, Phase I

Data.gov (United States)

National Aeronautics and Space Administration — The technical innovation proposed here is the application of an alternative hydrocarbon fuel – densified propylene, in combination with liquid oxygen (LOX) – that...

[Detection of monoamine neurotransmitters and its metabolites by high performance liquid chromatograph after pre-column derivatization of dansyl chloride column].

Science.gov (United States)

Huang, Xiao; Chen, Jia-wen; He, Li-ping; Kang, Xue-jun

2012-12-01

To develop a high performance liquid chromatography (HPLC) for detection of monoamine neurotransmitters and its metabolites after pre-column derivatization with dansyl chloride. The C(18) chromatograph column (150 mm×4.6 mm×5 µm) was selected for detection, and derived by dansyl chloride (10 mg/ml) under the condition of 50°C water bath by pH11 buffer solution. 20 µl acetic acid acetone solution (1.0 mol/L) was then mixed in for termination of the reaction. Then the solution was cooling to room temperature, 0.1 mol/L acetic acid zinc-acetonitrile-tetrahydrofuran solution was adopted for mobile phrase, with the volume ratio at 62:35:3. The flow rate was 1.0 ml/min between 0-10 min, 2.0 ml/min between 10-35 min. The ultraviolet detection wavelength was 286 nm. The above method separately detected monoamine neurotransmitters and its metabolites and evaluated the limit of detection, accurate degree and accuracy degree. The linear relations between each component was good in the range of 1 - 20 µg/ml (r = 0.999). The lowest detection limit of norepinephrine, dopamine, 5-hydroxytryptamine and the metabolites 3-methoxy-4-benzoglycols, homovanillic acid and 5-heteroauxin were separately 0.60, 0.80, 0.41, 0.21, 0.19 and 0.1 µg/ml; while the average recovery rates were between 78.5% - 95.9%, and the relative standard deviation (RSD) was 6.62%, 7.64%, 2.98%, 3.60%, 5.09% and 3.09%, respectively. In the process of selection and optimization of the chromatographic conditions, we observed the importance of metal ions to discretion, and discussed the temperature, pH of the buffer solution and dosage of dansyl chloride in derivation. Under the above conditions, the reaction was perfect, and the baseline of the detected materials thoroughly separated. The method to detect monoamine neurotransmitters and its metabolites by HPLC and pre-column derivatization with dansyl chloride was established; and this method could provide reference for the detection of polyamine by HPLC.

Insertion of liquid crystal molecules into hydrocarbon monolayers

Energy Technology Data Exchange (ETDEWEB)

Popov, Piotr, E-mail: ppopov@kent.edu; Mann, Elizabeth K. [Department of Physics, Kent State University, Kent, Ohio 44242 (United States); Lacks, Daniel J. [Department of Chemical Engineering, Case Western Reserve University, Cleveland, Ohio 44106 (United States); Jákli, Antal [Liquid Crystal Institute, Kent State University, Kent, Ohio 44242-0001 (United States)

2014-08-07

Atomistic molecular dynamics simulations were carried out to investigate the molecular mechanisms of vertical surface alignment of liquid crystals. We study the insertion of nCB (4-Cyano-4{sup ′}-n-biphenyl) molecules with n = 0,…,6 into a bent-core liquid crystal monolayer that was recently found to provide good vertical alignment for liquid crystals. The results suggest a complex-free energy landscape for the liquid crystal within the layer. The preferred insertion direction of the nCB molecules (core or tail first) varies with n, which can be explained by entropic considerations. The role of the dipole moments was found to be negligible. As vertical alignment is the leading form of present day liquid crystal displays (LCD), these results will help guide improvement of the LCD technology, as well as lend insight into the more general problem of insertion of biological and other molecules into lipid and surfactant layers.

Improved bioavailability and biodegradation of a model polyaromatic hydrocarbon by a biosurfactant producing bacterium of marine origin.

Science.gov (United States)

Das, Palashpriya; Mukherjee, Soumen; Sen, Ramkrishna

2008-07-01

Polyaromatic hydrocarbons (PAHs) are organic pollutants mostly derived from the processing and combustion of fossil fuels and cause human health hazards. In the present study a marine biosurfactant producing strain of Bacillus circulans was used to increase the bioavailability and consequent degradation of a model polyaromatic hydrocarbon, anthracene. Although the organism could not utilize anthracene as the sole carbon source, it showed better growth and biosurfactant production in an anthracene supplemented glycerol mineral salts medium (AGlyMSM) compared to a normal glycerol mineral salts medium (GlyMSM). The biosurfactant product showed high degree of emulsification of various hydrocarbons. Analysis by gas chromatography (GC), high performance thin layer chromatography (HPTLC) and Fourier transform infrared spectroscopy (FTIR) showed that the biosurfactant could effectively entrap and solubilize PAH. Thin layer chromatographic analysis showed that anthracene was utilized as a carbon substrate for the production of biosurfactant. Thus organic pollutant anthracene was metabolized and converted to biosurfactants facilitating its own bioremediation.

Polycyclic aromatic hydrocarbons (PAH) in Danish barbecued meat

DEFF Research Database (Denmark)

Duedahl-Olesen, Lene; Aaslyng, Margit Dall; Meinert, Lene

2015-01-01

Barbecuing is known to result in the formation of polycyclic aromatic hydrocarbons (PAHs). A validated method that employed pressurized liquid extraction (PLE), gel permeation chromatography (GPC) followed by solid phase extraction (SPE) on Silica and analytical determination by GC-MS was applied...

UHPLC: The Greening Face of Liquid Chromatography

OpenAIRE

Cielecka-Piontek, Judyta; Zalewski, Przemys?aw; Jeli?ska, Anna; Garbacki, Piotr

2013-01-01

Pharmaceutical analysis based on chromatographic separation is an important part of studies aimed at developing routine quality analysis of drugs. High-performance liquid chromatography (HPLC) is one of the main analytical techniques recommended for drug analysis. Although it meets many criteria vital for analysis, it is time-consuming and uses a relatively high amount of organic solvents compared to other analytical techniques. Recently, Ultra-high-performance liquid chromatography (UHPLC) h...

Condensation Mechanism of Hydrocarbon Field Formation.

Science.gov (United States)

Batalin, Oleg; Vafina, Nailya

2017-08-31

Petroleum geology explains how hydrocarbon fluids are generated, but there is a lack of understanding regarding how oil is expelled from source rocks and migrates to a reservoir. To clarify the process, the multi-layer Urengoy field in Western Siberia was investigated. Based on this example, we have identified an alternative mechanism of hydrocarbon field formation, in which oil and gas accumulations result from the phase separation of an upward hydrocarbon flow. There is evidence that the flow is generated by the gases released by secondary kerogen destruction. This study demonstrates that oil components are carried by the gas flow and that when the flow reaches a low-pressure zone, it condenses into a liquid with real oil properties. The transportation of oil components in the gas flow provides a natural explanation for the unresolved issues of petroleum geology concerning the migration process. The condensation mechanism can be considered as the main process of oil field formation.

Hydrocarbon source apportionment for the 1996 Paso del Norte Ozone Study.

Science.gov (United States)

Fujita, E M

2001-08-10

The 1996 Paso del Norte (PdN) ozone study was conducted to improve current understanding of the significant meteorological and air quality processes that lead to high concentrations of ozone in El Paso, Texas (USA) and Ciudad Juárez, Chihuahua (Mexico). Two-hour canister samples were collected five times daily at 05.00-07.00 h, 07.00-09.00 h, 09.00-11.00 h, 11.00-13.00 h, and 15.00-17.00 h MST during intensive study periods at one urban and one rural site on each side of the border. An automated gas chromatograph was operated at one site in central El Paso. Source profiles (the fractional chemical composition of emissions) from motor vehicles, gasoline, liquefied petroleum gas, and commercial natural gas were combined with source profiles from other studies for input to the Chemical Mass Balance (CMB) receptor model to apportion the measured non-methane hydrocarbons (NMHC) to sources. On-road vehicle emissions accounted for one-half to two-thirds of the NMHC in Ciudad Juárez and El Paso with the highest contributions occurring during the morning and afternoon commute periods. Emissions from diesel exhaust contributed approximately 2-3% of NMHC in Ciudad Juárez and less than 2% in El Paso. The average sum of liquid gasoline and gasoline vapor increased during the day in Ciudad Juárez from 2% at 06.00 h to approximately 12% at 16.00 h. Diurnal and day-of-the-week patterns in the liquid gasoline contributions are essentially identical to the corresponding patterns for motor vehicle exhaust, which suggest that a large fraction of the liquid gasoline contribution may be associated with tailpipe emissions rather than evaporative emissions from motor vehicles or industrial sources. Including the sum of the two sources put the upper limit for tailpipe contributions at 60-70% of NMHC.

A chromatographic objective function to characterise chromatograms with unknown compounds or without standards available.

Science.gov (United States)

Alvarez-Segura, T; Gómez-Díaz, A; Ortiz-Bolsico, C; Torres-Lapasió, J R; García-Alvarez-Coque, M C

2015-08-28

Getting useful chemical information from samples containing many compounds is still a challenge to analysts in liquid chromatography. The highest complexity corresponds to samples for which there is no prior knowledge about their chemical composition. Computer-based methodologies are currently considered as the most efficient tools to optimise the chromatographic resolution, and further finding the optimal separation conditions. However, most chromatographic objective functions (COFs) described in the literature to measure the resolution are based on mathematical models fitted with the information obtained from standards, and cannot be applied to samples with unknown compounds. In this work, a new COF based on the automatic measurement of the protruding part of the chromatographic peaks (or peak prominences) that indicates the number of perceptible peaks and global resolution, without the need of standards, is developed. The proposed COF was found satisfactory with regard to the peak purity criterion when applied to artificial peaks and simulated chromatograms of mixtures built using the information of standards. The approach was applied to mixtures of drugs containing unknown impurities and degradation products and to extracts of medicinal herbs, eluted with acetonitrile-water mixtures using isocratic and gradient elution. Copyright © 2015 Elsevier B.V. All rights reserved.

Acrylamide analysis in food by liquid chromatographic and gas chromatographic methods.

Science.gov (United States)

Elbashir, Abdalla A; Omar, Mei M Ali; Ibrahim, Wan Aini Wan; Schmitz, Oliver J; Aboul-Enein, Hassan Y

2014-01-01

Acrylamide (AA) is a compound classified as carcinogenic to humans by the International Agency for Research on Cancer. It was first discovered to be present in certain heated processed food by the Swedish National Food Administration (SNFA) and University of Stockholm in early 2002. The major pathway for AA formation in food is the Maillard reaction between reducing sugar and the amino acid asparagine at high temperature. Since the discovery of AA's presence in food, many analytical methods have been developed for determination of AA contents in different food matrices. Also, several studies have been conducted to develop extraction procedures for AA from difficult food matrices. AA is a small, highly polar molecule, which makes its extraction and analysis challenging. Many articles and reviews have been published dealing with AA in food. The aim of the review is to discuss AA formation in food, the factors affecting AA formation and removal, AA exposure assessment, AA extraction and cleanup from food samples, and analytical methods used in AA determination, such as high-performance liquid chromatography (HPLC) and gas chromatography (GC). Special attention is given to sample extraction and cleanup procedures and analytical techniques used for AA determination.

Comparison of the composition between coal-liquid naphtha and petroleum gasoline

Energy Technology Data Exchange (ETDEWEB)

Miki, Y.; Sugimoto, Y.; Ono, S.; Machida, M. [National Chemical Laboratory for Industry, Tsukuba (Japan)

1997-08-01

Compositional characterization was performed using a gas chromatography-mass spectrometry-atomic emission detector technique on coal-liquid raw naphtha, coal-liquid refined naphtha, coal-liquid reformate and commercial petroleum gasoline. The chemical composition of these oils are divided into five groups: chain hydrocarbons, monocyclic hydrocarbons, bicyclic hydrocarbons, oxygen-containing compounds and other compounds (containing unidentified compounds). Compared to petroleum gasoline, the coal-liquid raw naphtha contains higher concentrations of straight paraffins, cycloparaffins, cycloolefins, bicycloparaffins and oxygen-containing compounds, and contains lower concentrations of brached paraffins and monocyclic aromatic compounds. Phenols and ketones are the major components of oxygen-containing compounds. The total concentration of paraffins and cycloparaffins increased after refining. The hydrogenation of olefins and the hydrodeoxygenation of oxygen-containing compounds are suggested to proceed during the refining process. The reforming treatment increased the concentrations of branched paraffins and monocyclic aromatic compounds; this suggests that coal-liquid reformat could be used as a major blending substance with petroleum gasoline.

Distribution of trichloroethylene and selected aliphatic and aromatic hydrocarbons between ''weathered'' and ''unweathered'' fuel mixtures and groundwater: Equilibrium and kinetic considerations

International Nuclear Information System (INIS)

Doucette, W.J.; Dupont, R.R.

1995-01-01

The distribution of trichloroethylene and several aliphatic and aromatic fuel components between 46 weathered and 11 unweathered fuel mixtures and groundwater was investigated using a slow stirring method. The weathered fuel mixtures were obtained from several contaminated field sites. Both unlabeled and 14C-labeled test compounds were used in the distribution experiments. Analyses of the test compound concentrations over time was performed by gas chromatograph or liquid scintillation counting. The time required to reach equilibrium varied from about 24 to 72 hours. Generally, the greater the hydrophobicity of the test compounds the longer time that was required to reach equilibrium. It was also observed that the fuel/water distribution coefficients were generally larger for the weathered fuels than those measured for the unweathered fuels, in some cases by a factor of 100. The weathered fuel mixtures obtained from the field site were depleted of the more water soluble compounds over time and became significantly more enriched in long chain aliphatic hydrocarbons. The ability of several models to describe the observed distribution behavior was examined

Batch-to-batch quality consistency evaluation of botanical drug products using multivariate statistical analysis of the chromatographic fingerprint.

Science.gov (United States)

Xiong, Haoshu; Yu, Lawrence X; Qu, Haibin

2013-06-01

Botanical drug products have batch-to-batch quality variability due to botanical raw materials and the current manufacturing process. The rational evaluation and control of product quality consistency are essential to ensure the efficacy and safety. Chromatographic fingerprinting is an important and widely used tool to characterize the chemical composition of botanical drug products. Multivariate statistical analysis has showed its efficacy and applicability in the quality evaluation of many kinds of industrial products. In this paper, the combined use of multivariate statistical analysis and chromatographic fingerprinting is presented here to evaluate batch-to-batch quality consistency of botanical drug products. A typical botanical drug product in China, Shenmai injection, was selected as the example to demonstrate the feasibility of this approach. The high-performance liquid chromatographic fingerprint data of historical batches were collected from a traditional Chinese medicine manufacturing factory. Characteristic peaks were weighted by their variability among production batches. A principal component analysis model was established after outliers were modified or removed. Multivariate (Hotelling T(2) and DModX) control charts were finally successfully applied to evaluate the quality consistency. The results suggest useful applications for a combination of multivariate statistical analysis with chromatographic fingerprinting in batch-to-batch quality consistency evaluation for the manufacture of botanical drug products.

Ambient aromatic hydrocarbon measurements at Welgegund, South Africa

Energy Technology Data Exchange (ETDEWEB)

Jaars, K.; Beukes, J. P.; van Zyl, P. G.; Venter, A. D.; Josipovic, M.; Pienaar, J. J.; Vakkari, Ville; Aaltonen, H.; Laakso, H.; Kulmala, M.; Tiitta, P.; Guenther, Alex B.; Hellen, H.; Laakso, L.; Hakola, H.

2014-07-11

Aromatic hydrocarbons are associated with direct adverse human health effects and can have negative impacts on ecosystems due to their toxicity, as well as indirect negative effects through the formation of tropospheric ozone and secondary organic aerosol that affect human health, crop production and regional climate. Measurements were conducted at the Welgegund measurement station (South Africa) that is considered to be a regionally representative background site. However, the site is occasionally impacted by plumes from major anthropogenic source regions in the interior of South Africa, which include the western Bushveld Igneous Complex (e.g. platinum, base metal and ferrochrome smelters), the eastern Bushveld Igneous Complex (platinum and ferrochrome smelters), the Johannesburg-Pretoria metropolitan conurbation (>10 million people), the Vaal Triangle (e.g. petrochemical and industries), the Mpumalanga Highveld (e.g. coal-fired power plants and petrochemical industry) and also a region of anti-cyclonic recirculation of air mass over the interior of South Africa. The aromatic hydrocarbon measurements were conducted with an automated sampler on Tenax-TA and Carbopack-B adsorbent tubes with heated inlet for one year. Samples were collected twice a week for two hours during daytime and two hours 1 during night-time. A thermal desorption unit, connected to a gas chromatograph and a mass 2 selective detector was used for sample preparation and analysis. Results indicated that the 3 monthly median total aromatic hydrocarbon concentrations ranged between 0.01 to 3.1 ppb. 4 Benzene levels did not exceed local air quality standards. Toluene was the most abundant 5 species, with an annual median concentration of 0.63 ppb. No statistically significant 6 differences in the concentrations measured during daytime and night-time were found and no distinct seasonal patterns were observed. Air mass back trajectory analysis proved that the lack of seasonal cycles could be

Application of sunflower stalk-carbon nitride nanosheets as a green sorbent in the solid-phase extraction of polycyclic aromatic hydrocarbons followed by high-performance liquid chromatography.

Science.gov (United States)

Marzi Khosrowshahi, Elnaz; Razmi, Habib

2018-02-08

A green biocomposite of sunflower stalks and graphitic carbon nitride nanosheets has been applied as a solid-phase extraction adsorbent for sample preparation of five polycyclic aromatic hydrocarbons in different solutions using high-performance liquid chromatography with ultraviolet detection. Before the modification, sunflower stalks exhibited relatively low adsorption to the polycyclic aromatic hydrocarbons extraction. The modified sunflower stalks showed increased adsorption to the analytes extraction due to the increase in surface and existence of a π-π interaction between the analytes and graphitic carbon nitride nanosheets on the surface. Under the optimal conditions, the limits of detection and quantification for five polycyclic aromatic hydrocarbons compounds could reach 0.4-32 and 1.2-95 ng/L, respectively. The method accuracy was evaluated using recovery measurements in spiked real samples and good recoveries from 71 to 115% with relative standard deviations of polycyclic aromatic hydrocarbons determination in various samples-well water, tap water, soil, vegetable, and barbequed meat (kebab)-with analytes contents ranging from 0.065 to 13.3 μg/L. The prepared green composite as a new sorbent has some advantages including ease of preparation, low cost, and good reusability. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Chromatographic Monoliths for High-Throughput Immunoaffinity Isolation of Transferrin from Human Plasma

Directory of Open Access Journals (Sweden)

Irena Trbojević-Akmačić

2016-06-01

Full Text Available Changes in protein glycosylation are related to different diseases and have a potential as diagnostic and prognostic disease biomarkers. Transferrin (Tf glycosylation changes are common marker for congenital disorders of glycosylation. However, biological interindividual variability of Tf N-glycosylation and genes involved in glycosylation regulation are not known. Therefore, high-throughput Tf isolation method and large scale glycosylation studies are needed in order to address these questions. Due to their unique chromatographic properties, the use of chromatographic monoliths enables very fast analysis cycle, thus significantly increasing sample preparation throughput. Here, we are describing characterization of novel immunoaffinity-based monolithic columns in a 96-well plate format for specific high-throughput purification of human Tf from blood plasma. We optimized the isolation and glycan preparation procedure for subsequent ultra performance liquid chromatography (UPLC analysis of Tf N-glycosylation and managed to increase the sensitivity for approximately three times compared to initial experimental conditions, with very good reproducibility. This work is licensed under a Creative Commons Attribution 4.0 International License.

Evaluation and application of a mixed-mode chromatographic stationary phase in two-dimensional liquid chromatography for the separation of traditional Chinese medicine.

Science.gov (United States)

Wei, Zhishen; Fu, Qing; Cai, Jianfeng; Huan, Liyun; Zhao, Jianchao; Shi, Hui; Jin, Yu; Liang, Xinmiao

2016-06-01

In this study, two mixed-mode chromatography stationary phases (C8SAX and C8SCX) were evaluated and used to establish a two-dimensional liquid chromatography system for the separation of traditional Chinese medicine. The chromatographic properties of the mixed-mode columns were systematically evaluated by comparing with other three columns of C8, strong anion exchanger, and strong cation exchanger. The result showed that C8SAX and C8SCX had a mixed-mode retention mechanism including electrostatic interaction and hydrophobic interaction. Especially, they were suitable for separating acidic and/or basic compounds and their separation selectivities could be easily adjusted by changing pH value. Then, several off-line 2D-LC systems based on the C8SAX in the first dimension and C8SAX, C8SCX, or C8 columns in the second dimension were developed to analyze a traditional Chinese medicine-Uncaria rhynchophylla. The two-dimensional liquid chromatography system of C8SAX (pH 3.0) × C8SAX (pH 6.0) exhibited the most effective peak distribution. Finally, fractions of U. rhynchophylla prepared from the first dimension were successfully separated on the C8SAX column with a gradient pH. Thus, the mixed-mode stationary phase could provide a platform to separate the traditional Chinese medicine in practical applications. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Chromatographic hydrogen isotope separation

International Nuclear Information System (INIS)

Aldridge, F.T.

1983-01-01

Intermetallic compounds with the CaCu5 type of crystal structure, particularly LaNiCo and CaNi5, exhibit high separation factors and fast equilibrium times and therefore are useful for packing a chromatographic hydrogen isotope separation column. The addition of an inert metal to dilute the hydride improves performance of the column. A large scale multi-stage chromatographic separation process run as a secondary process off a hydrogen feedstream from an industrial plant which uses large volumes of hydrogen can produce large quantities of heavy water at an effective cost for use in heavy water reactors

Chromatographic hydrogen isotope separation

International Nuclear Information System (INIS)

Aldridge, F.T.

1981-01-01

Intermetallic compounds with the CaCu5 type of crystal structure , particularly LaNiCo and CaNi5, exhibit high separation factors and fast equilibrium times and therefore are useful for packing a chromatographic hydrogen isotope separation colum. The addition of an inert metal to dilute the hydride improves performance of the column. A large scale mutli-stage chromatographic separation process run as a secondary process off a hydrogen feedstream from an industrial plant which uses large volumes of hydrogen can produce large quantities of heavy water at an effective cost for use in heavy water reactors

Development and validation of a reversed phase liquid chromatographic method for analysis of oxytetracycline and related impurities.

Science.gov (United States)

Kahsay, Getu; Shraim, Fairouz; Villatte, Philippe; Rotger, Jacques; Cassus-Coussère, Céline; Van Schepdael, Ann; Hoogmartens, Jos; Adams, Erwin

2013-03-05

A simple, robust and fast high-performance liquid chromatographic method is described for the analysis of oxytetracycline and its related impurities. The principal peak and impurities are all baseline separated in 20 min using an Inertsil C₈ (150 mm × 4.6 mm, 5 μm) column kept at 50 °C. The mobile phase consists of a gradient mixture of mobile phases A (0.05% trifluoroacetic acid in water) and B (acetonitrile-methanol-tetrahydrofuran, 80:15:5, v/v/v) pumped at a flow rate of 1.3 ml/min. UV detection was performed at 254 nm. The developed method was validated for its robustness, sensitivity, precision and linearity in the range from limit of quantification (LOQ) to 120%. The limits of detection (LOD) and LOQ were found to be 0.08 μg/ml and 0.32 μg/ml, respectively. This method allows the separation of oxytetracycline from all known and 5 unknown impurities, which is better than previously reported in the literature. Moreover, the simple mobile phase composition devoid of non-volatile buffers made the method suitable to interface with mass spectrometry for further characterization of unknown impurities. The developed method has been applied for determination of related substances in oxytetracycline bulk samples available from four manufacturers. The validation results demonstrate that the method is reliable for quantification of oxytetracycline and its impurities. Copyright © 2012 Elsevier B.V. All rights reserved.

Solvent extraction of aromatics from middle distillates: equilibria prediction method by group contribution

Energy Technology Data Exchange (ETDEWEB)

Rahman, M.; Mikitenko, P.; Asselineau, L.

1984-01-01

A method of calculating liquid-liquid aromatics extraction of a middle distillate is described. The group contribution models of the ASOG and UNIFAC type are investigated. Four vapor liquid equilibrium (VLE), two solid-liquid equilibrium (SLE), three binary and six ternary liquid-liquid equilibrium (LLE) have been measured. The parameters of the models are based mainly on the data of the systems having 10-20 carbon number. VLE, SLE, and infinite dilution activity coefficient data (17-245/sup 0/C) have been used for calculating interaction parameters between hydrocarbon groups and LLE data (20-80/sup 0/C) for interaction parameters of dimethylformamide-hydrocarbon groups. Middle distillate representation is based on mass spectrometric and gas chromatographic analysis and on limited data of middle distillate-DMF liquid-liquid equilibrium. It is shown that the performance of ASOG and UNIFAC models are sufficiently valid in representation of data base and in extraction calculations. Considering the predictive character and the rapidity of its application this method can be useful in the preliminary study of extraction processes. 34 references, 2 figures, 10 tables.

Ambient aromatic hydrocarbon measurements at Welgegund, South Africa

Science.gov (United States)

Jaars, K.; Beukes, J. P.; van Zyl, P. G.; Venter, A. D.; Josipovic, M.; Pienaar, J. J.; Vakkari, V.; Aaltonen, H.; Laakso, H.; Kulmala, M.; Tiitta, P.; Guenther, A.; Hellén, H.; Laakso, L.; Hakola, H.

2014-07-01

Aromatic hydrocarbons are associated with direct adverse human health effects and can have negative impacts on ecosystems due to their toxicity, as well as indirect negative effects through the formation of tropospheric ozone and secondary organic aerosol, which affect human health, crop production and regional climate. Measurements of aromatic hydrocarbons were conducted at the Welgegund measurement station (South Africa), which is considered to be a regionally representative background site. However, the site is occasionally impacted by plumes from major anthropogenic source regions in the interior of South Africa, which include the western Bushveld Igneous Complex (e.g. platinum, base metal and ferrochrome smelters), the eastern Bushveld Igneous Complex (platinum and ferrochrome smelters), the Johannesburg-Pretoria metropolitan conurbation (> 10 million people), the Vaal Triangle (e.g. petrochemical and pyrometallurgical industries), the Mpumalanga Highveld (e.g. coal-fired power plants and petrochemical industry) and also a region of anticyclonic recirculation of air mass over the interior of South Africa. The aromatic hydrocarbon measurements were conducted with an automated sampler on Tenax-TA and Carbopack-B adsorbent tubes with heated inlet for 1 year. Samples were collected twice a week for 2 h during daytime and 2 h during night-time. A thermal desorption unit, connected to a gas chromatograph and a mass selective detector was used for sample preparation and analysis. Results indicated that the monthly median (mean) total aromatic hydrocarbon concentrations ranged between 0.01 (0.011) and 3.1 (3.2) ppb. Benzene levels did not exceed the local air quality standard limit, i.e. annual mean of 1.6 ppb. Toluene was the most abundant compound, with an annual median (mean) concentration of 0.63 (0.89) ppb. No statistically significant differences in the concentrations measured during daytime and night-time were found, and no distinct seasonal patterns were

Resolution of RNA using high-performance liquid chromatography

NARCIS (Netherlands)

Mclaughlin, L.W.; Bischoff, Rainer

1987-01-01

High-performance liquid chromatographic techniques can be very effective for the resolution and isolation of nucleic acids. The characteristic ionic (phosphodiesters) and hydrophobic (nucleobases) properties of RNAs can be exploited for their separation. In this respect anion-exchange and

Chromatographic assay of degradation products of tributyl phosphate

International Nuclear Information System (INIS)

Tripathi, S.C.; Ramanujam, A.; Nadkarni, M.N.; Rao, K.A.; Bandyopadhyay, C.

1985-01-01

Gas-liquid chromatography (GLC) and thin-layer chromatographic (TLC) procedures have been developed for the estimation of monobutyl phosphoric acid (H 2 MBP) and dibutyl phosphoric acid (HDBP) present in tributyl phosphate (TBP). Less than one microgram of H 2 MBP and HDBP is visually detected on TLC plate made of silicagel-cellulose (1:1). HDBP as separated by TLC has been quantitatively estimated in the range of 40-260 μg using an indirect spectrophotometric method. GLC method using 10 percent (W/W) XE-60 column can be effectively used for the simultaneous determination of 0.25 percent W/V H 2 MBP and HDBP present in 30 percent TBP-n-dodecane. The sensitivity may be enhanced 100 fold by careful column conditioning and judicious control of operational parameters. (author)

Optimization of the gas chromatographic separations

International Nuclear Information System (INIS)

Gasco Sanchez, L.

1973-01-01

A review and a critical study on the optimization of the gas chromatographic separations are made. After dealing with the fundamental gas chromatographic equations, some methods of expressing column performances are discussed: performance indices, performance parameters, resolution and effective plate number per unit time. This is completed with a comparative study on performances of various types of columns. Moreover, optimization methods for operating chromatographic conditions are extensively dealt with: as resolution optimization, separation time, and normalization techniques for the time of analysis in order to achieve the maximum resolution at constant time. Finally, some others non operating parameters such as: selectivity of stationary phases, column preparation and optimization methods by means of computers are studied. (Author) 68 refs

Application of Ionic Liquids in High Performance Reversed-Phase Chromatography

Directory of Open Access Journals (Sweden)

Wentao Bi

2009-06-01

Full Text Available Ionic liquids, considered “green” chemicals, are widely used in many areas of analytical chemistry due to their unique properties. Recently, ionic liquids have been used as a kind of novel additive in separation and combined with silica to synthesize new stationary phase as separation media. This review will focus on the properties and mechanisms of ionic liquids and their potential applications as mobile phase modifier and surface-bonded stationary phase in reversed-phase high performance liquid chromatography (RP-HPLC. Ionic liquids demonstrate advantages and potential in chromatographic field.

A Small-Scale Low-Cost Gas Chromatograph

Science.gov (United States)

Gros, Natasa; Vrtacnik, Margareta

2005-01-01

The design and application of a small-scale portable gas chromatograph for learning of the basic concepts of chromatography is described. The apparatus consists of two basic separable units, which includes a chromatographic unit and an electronic unit.

Chromatographic determination of the rate and extent of absorption of air pollutants by sea water

International Nuclear Information System (INIS)

Nikolakaki, S.; Vassilakos, C.; Katsanos, N.A.

1994-01-01

A simple chromatographic method is developed to determine the rate constant for expulsion of an air pollutant from water or its diffusion parameter in the liquid, the rate constant for chemical reaction of the pollutant with water, its mass transfer coefficient in the liquid, and the partition coefficient between liquid water and air. From these physicochemical parameters, the absorption rate by sea water and, therefore, the depletion rate of a polluting substance from the air can be calculated, together with the equilibrium state of this absorption. The method has been applied to nitrogen dioxide being absorbed by triple-distilled water and by sea water, at various temperatures. From the temperature variation of the reaction rate constant and of the partition coefficient, the activation energy for the reaction and the differential heat of solution were determined. (orig.)

Chromatographic fingerprint analysis of yohimbe bark and related dietary supplements using UHPLC/UV/MS.

Science.gov (United States)

Sun, Jianghao; Chen, Pei

2012-03-05

A practical ultra high-performance liquid chromatography (UHPLC) method was developed for fingerprint analysis of and determination of yohimbine in yohimbe barks and related dietary supplements. Good separation was achieved using a Waters Acquity BEH C(18) column with gradient elution using 0.1% (v/v) aqueous ammonium hydroxide and 0.1% ammonium hydroxide in methanol as the mobile phases. The study is the first reported chromatographic method that separates corynanthine from yohimbine in yohimbe bark extract. The chromatographic fingerprint analysis was applied to the analysis of 18 yohimbe commercial dietary supplement samples. Quantitation of yohimbine, the traditional method for analysis of yohimbe barks, were also performed to evaluate the results of the fingerprint analysis. Wide variability was observed in fingerprints and yohimbine content among yohimbe dietary supplement samples. For most of the dietary supplements, the yohimbine content was not consistent with the label claims. Copyright © 2011. Published by Elsevier B.V.

Chromatographic Determination of Toluene and its Metabolites in Urine for Toluene Exposure - A Review

International Nuclear Information System (INIS)

Mohamad Raizul Zinalibdin; Abdul Rahim Yacob; Mohd Marsin Sanagi

2016-01-01

The determinations of toluene and their metabolites in biological samples such as urine and blood allow the estimation of the degree of exposure to this chemical. Chromatographic methods and preliminary methods are now universally employed for this purpose. Preliminary color test methods are well established for qualitative determination of toluene and its metabolites. Mobile test kits using color test methods are a vast tool for screening urine samples but chromatographic methods are still needed for confirmation and quantitative analysis. Gas chromatography (GC) methods are well-adapted for the determination of toluene metabolite in urine, but these methods often require several pretreatment steps. Meanwhile, high performance liquid chromatography (HPLC) is becoming a powerful tool for the accurate and easy determination of toluene metabolites considering its decisive advantages for routine monitoring. Furthermore, recent development in HPLC could widen the usefulness of this method to solve the most complex analytical problems that could be encountered during the measurement. (author)

Warping methods for spectroscopic and chromatographic signal alignment: A tutorial

Energy Technology Data Exchange (ETDEWEB)

Bloemberg, Tom G., E-mail: T.Bloemberg@science.ru.nl [Radboud University Nijmegen, Institute for Molecules and Materials, Heyendaalseweg 135, 6525 AJ Nijmegen (Netherlands); Radboud University Nijmegen, Education Institute for Molecular Sciences, Heyendaalseweg 135, 6525 AJ Nijmegen (Netherlands); Gerretzen, Jan; Lunshof, Anton [Radboud University Nijmegen, Institute for Molecules and Materials, Heyendaalseweg 135, 6525 AJ Nijmegen (Netherlands); Wehrens, Ron [Centre for Research and Innovation, Fondazione Edmund Mach, Via E. Mach, 1, 38010 San Michele all’Adige, TN (Italy); Buydens, Lutgarde M.C. [Radboud University Nijmegen, Institute for Molecules and Materials, Heyendaalseweg 135, 6525 AJ Nijmegen (Netherlands)

2013-06-05

Highlights: •The concepts of warping and alignment are introduced. •The most important warping methods are critically reviewed and explained. •Reference selection, evaluation and place of warping in preprocessing are discussed. •Some pitfalls, especially for LC–MS and similar data, are addressed. •Examples are provided, together with programming scripts to rework and extend them. -- Abstract: Warping methods are an important class of methods that can correct for misalignments in (a.o.) chemical measurements. Their use in preprocessing of chromatographic, spectroscopic and spectrometric data has grown rapidly over the last decade. This tutorial review aims to give a critical introduction to the most important warping methods, the place of warping in preprocessing and current views on the related matters of reference selection, optimization, and evaluation. Some pitfalls in warping, notably for liquid chromatography–mass spectrometry (LC–MS) data and similar, will be discussed. Examples will be given of the application of a number of freely available warping methods to a nuclear magnetic resonance (NMR) spectroscopic dataset and a chromatographic dataset. As part of the Supporting Information, we provide a number of programming scripts in Matlab and R, allowing the reader to work the extended examples in detail and to reproduce the figures in this paper.

New chromatographic method for separating Omeprazole from its degradation components and the quantitatively determining it in its pharmaceutical products

International Nuclear Information System (INIS)

Touma, M.; Rajab, A.; Seuleiman, M.

2007-01-01

New chromatographic method for Quantitative Determination of Omeprazole in its Pharmaceutical Products was produced. Omeprazole and its degradation components were well separated in same chromatogram by using high perfume liquid chromatography (HPLC). The new analytical method has been validated by these characteristic tests (accuracy, precision, range, linearity, specificity/selectivity, limit of detection (LOD) and limit of quantitative (LOQ) ).(author)

New chromatographic Methods for Separation of Lansoprazole from its Degradation Components and The Quantitative Determination in its Pharmaceutical Products

International Nuclear Information System (INIS)

Touma, M.; Rajab, A.

2009-01-01

New chromatographic method was found for Quantitative Determination of Lansoprazole in its pharmaceutical products. Lansoprazole and its degradation components were well separated in same chromatogram by using high perfume liquid chromatography (HPLC). The new analytical method has been validated by these characteristic tests (accuracy, precision, range, linearity, specificity/selectivity, limit of detection (LOD) and limit of quantitative (LOQ)). (author)

Task 8: Evaluation of hydrocarbon potential

International Nuclear Information System (INIS)

Cashman, P.H.; Trexler, J.H. Jr.

1994-01-01

Our studies focus on the stratigraphy of Late Devonian to early Pennsylvanian rocks at the NTS, because these are the best potential hydrocarbon source rocks in the vicinity of Yucca Mountain. In the last year, our stratigraphic studies have broadened to include the regional context for both the Chainman and the Eleana formations. New age data based on biostratigraphy constrain the age ranges of both Chainman and Eleana; accurate and reliable ages are essential for regional correlation and for regional paleogeographic reconstructions. Source rock analyses throughout the Chainman establish whether these rocks contained adequate organic material to generate hydrocarbons. Maturation analyses of samples from the Chainman determine whether the temperature history has been suitable for the generation of liquid hydrocarbons. Structural studies are aimed at defining the deformation histories and present position of the different packages of Devonian - Pennsylvanian rocks. This report summarizes new results of our structural, stratigraphic and hydrocarbon source rock potential studies at the Nevada Test Site and vicinity. Stratigraphy is considered first, with the Chainman Shale and Eleana Formation discussed separately. New biostratigraphic results are included in this section. New results from our structural studies are summarized next, followed by source rock and maturation analyses of the Chainman Shale. Directions for future work are included where appropriate

[Research on the application of grey system theory in the pattern recognition for chromatographic fingerprints of traditional Chinese medicine].

Science.gov (United States)

Wei, Hang; Lin, Li; Zhang, Yuan; Wang, Lianjing; Chen, Qinqun

2013-02-01

A model based on grey system theory was proposed for pattern recognition in chromatographic fingerprints (CF) of traditional Chinese medicine (TCM). The grey relational grade among the data series of each testing CF and the ideal CF was obtained by entropy and norm respectively, then the principle of "maximal matching degree" was introduced to make judgments, so as to achieve the purpose of variety identification and quality evaluation. A satisfactory result in the high performance liquid chromatographic (HPLC) analysis of 56 batches of different varieties of Exocarpium Citrus Grandis was achieved with this model. The errors in the chromatographic fingerprint analysis caused by traditional similarity method or grey correlation method were overcome, as the samples of Citrus grandis 'Tomentosa' and Citrus grandis (L.) Osbeck were correctly distinguished in the experiment. Furthermore in the study on the variety identification of Citrus grandis 'Tomentosa', the recognition rates were up to 92.85%, although the types and the contents of the chemical compositions of the samples were very close. At the same time, the model had the merits of low computation complexity and easy operation by computer programming. The research indicated that the grey system theory has good applicability to pattern recognition in the chromatographic fingerprints of TCM.

Analysis of TPH and Aliphatic and Aromatic Hydrocarbons Fractions in Environmental Interest Matrices

International Nuclear Information System (INIS)

Pindado, O.; Perez, R. M.; Garcia, S.

2014-01-01

Analytical methods to analyze TPH and several aliphatic and aromatic fractions present in soil and groundwater samples contaminated by hydrocarbons are showed. As a part of BIOXISOIL project, analyzing these parameters is fundamental and indispensable to know the initial contamination level, design an adequate method to decontaminate it and eventually assess decontamination accomplished. Analysis of both matrices involve different extraction stages such as microwave radiation, clean up steps based on solid phase extraction and finally a chromatograph analysis with flame ion detector. Analytical procedures have showed satisfactory analytical quality parameters and have been validated against several certified reference materials. (Author)

Use of liquid chromatography for measuring atmospheric sulfur dioxide and nitrogen oxide

Energy Technology Data Exchange (ETDEWEB)

Benova, E

1973-02-01

A literature search to ascertain the applicability of liquid chromatography to the analysis of atmospheric sulfur dioxide and various oxides of nitrogen is reported. Simple or enriched samples can be analyzed. Plastic bags are recommended for preparation of simple samples; and a table of 18 plastic materials, their manufacturers, and pollutants to which they are inert is provided. Enriched samples can be prepared in chromatographic columns by adsorption methods. Tables are provided listing carriers, stationary phase materials, temperatures, carrier liquids (helium or nitrogen), column dimensions, and other data recommended for chromatographic tests of SO/sub 2/ and NOx. Because of its reactivity and tendency to polymerize, sulfur trioxide should be reduced to SO/sub 2/ prior to analysis.

High performance liquid chromatography of substituted aromatics with the metal-organic framework MIL-100(Fe): Mechanism analysis and model-based prediction.

Science.gov (United States)

Qin, Weiwei; Silvestre, Martin Eduardo; Li, Yongli; Franzreb, Matthias

2016-02-05

Metal-organic framework (MOF) MIL-100(Fe) with well-defined thickness was homogenously coated onto the outer surface of magnetic microparticles via a liquid-phase epitaxy method. The as-synthesized MIL-100(Fe) was used as stationary phase for high-performance liquid chromatography (HPLC) and separations of two groups of mixed aromatic hydrocarbons (toluene, styrene and p-xylene; acetanilide, 2-nirtoaniline and 1-naphthylamine) using methanol/water as mobile phase were performed to evaluate its performance. Increasing water content of the mobile phase composition can greatly improve the separations on the expense of a longer elution time. Stepwise elution significantly shortens the elution time of acetanilide, 2-nirtoaniline and 1-naphthylamine mixtures, while still achieving a baseline separation. Combining the experimental results and in-depth modeling using a recently developed chromatographic software (ChromX), adsorption equilibrium parameters, including the affinities and maximum capacities, for each analyte toward the MIL-100(Fe) are obtained. In addition, the pore diffusivity of aromatic hydrocarbons within MIL-100(Fe) was determined to be 5×10(-12)m(2)s(-1). While the affinities of MIL-100(Fe) toward the analyte molecules differs much, the maximum capacities of the analytes are in a narrow range with q*MOFmax,toluene=3.55molL(-1), q*MOFmax,styrene or p-xylene=3.53molL(-1), and q*MOFmax,anilines=3.12molL(-1) corresponding to approximately 842 toluene and 838 styrene or p-xylene, and 740 aniline molecules per MIL-100(Fe) unit cell, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

Sample preparation for liquid chromatographic analysis of phytochemicals in biological fluids.

Science.gov (United States)

Oh, Ju-Hee; Lee, Young-Joo

2014-01-01

Natural products have been used traditionally for the treatment and prevention of diseases for thousands of years and are nowadays consumed as dietary supplements and herbal medicine. To ensure the safe and effective use of these herbal products, information about bioavailability of active compounds in plasma or target tissues should be provided via validated analytical methods combined with appropriate sampling methods. To provide comprehensive and abridged information about sample preparation methods for the quantification of phytochemicals in biological samples using liquid chromatography analysis. Sample pre-treatment procedures used in analytical methods for in vivo pharmacokinetic studies of natural compounds or herbal medicines were reviewed. These were categorised according to the biological matrices (plasma, bile, urine, faeces and tissues) and sample clean-up processes (protein precipitation, liquid-liquid extraction and solid-phase extraction). Although various kinds of sample pre-treatment methods have been developed, liquid-liquid extraction is still widely used and solid-phase extraction is becoming increasingly popular because of its efficiency for extensive clean up of complex matrix samples. However, protein precipitation is still favoured due to its simplicity. Sample treatment for phytochemical analysis in biological fluids is an indispensable and critical step to obtain high quality results. This step could dominate the overall analytical process because both the duration of the process as well as the reliability of the data depend in large part on its efficiency. Thus, special attention should be given to the choice of a proper sample treatment method that targets analytes and their biomatrix. Copyright © 2013 John Wiley & Sons, Ltd.

[Advances of poly (ionic liquid) materials in separation science].

Science.gov (United States)

Liu, Cuicui; Guo, Ting; Su, Rina; Gu, Yuchen; Deng, Qiliang

2015-11-01

Ionic liquids, as novel ionization reagents, possess beneficial characteristics including good solubility, conductivity, thermal stability, biocompatibility, low volatility and non-flammability. Ionic liquids are attracting a mass of attention of analytical chemists. Poly (ionic liquid) materials have common performances of ionic liquids and polymers, and have been successfully applied in separation science area. In this paper, we discuss the interaction mechanisms between the poly(ionic liquid) materials and analytes including hydrophobic/hydrophilic interactions, hydrogen bond, ion exchange, π-π stacking and electrostatic interactions, and summarize the application advances of the poly(ionic liquid) materials in solid phase extraction, chromatographic separation and capillary electrophoresis. At last, we describe the future prospect of poly(ionic liquid) materials.

Direct production of fractionated and upgraded hydrocarbon fuels from biomass

Science.gov (United States)

Felix, Larry G.; Linck, Martin B.; Marker, Terry L.; Roberts, Michael J.

2014-08-26

Multistage processing of biomass to produce at least two separate fungible fuel streams, one dominated by gasoline boiling-point range liquids and the other by diesel boiling-point range liquids. The processing involves hydrotreating the biomass to produce a hydrotreatment product including a deoxygenated hydrocarbon product of gasoline and diesel boiling materials, followed by separating each of the gasoline and diesel boiling materials from the hydrotreatment product and each other.

The use of chromatographic indexes to study the biodegradation of crude oil in cold/icy seawater

International Nuclear Information System (INIS)

Siron, R.; Pelletier, E.

1993-01-01

A group of five protected mesocosms (3.5 m 3 each) was used to study the biodegradation of dispersed crude oil in cold and icy seawater. A wide range of oil concentrations was tested over four experiments lasting two weeks to six months. Various oil treatments were studied with respect to the natural bacterial degradation: chemically dispersed and untreated crude oil; and oil adsorbed on, and released from, an immersed substrate. The study was concerned with oil accommodated in the water column, accumulated in surface (sheens and emulsions), and collected in sediment traps. The oil biodegradation was assessed by means of the following gas chromatographic indexes: C17/pristane; C18/phytane; n-alkanes/isoprenoids; pristane/phytane; naphthalene/phenanthrene; 2-methyl naphthalene/1-methyl naphthalene; and methylnaphthalenes/total substituted naphthalenes. A combined index of biodegradation defined from the most significant hydrocarbon ratios is proposed to evaluate the overall biodegradation of dissolved compounds and oil droplets, involving both aliphatic and aromatic hydrocarbons. Coupled with mesocosm facilities, this approach appears very convenient to determine the potential degradability of crude oils by natural indigenous microflora. 26 refs., 11 figs., 2 tabs

Quantification of isomerically summed hydrocarbon contributions to crude oil by carbon number, double bond equivalent, and aromaticity using gas chromatography with tunable vacuum ultraviolet ionization.

Science.gov (United States)

Nowak, Jeremy A; Weber, Robert J; Goldstein, Allen H

2018-03-12

The ability to structurally characterize and isomerically quantify crude oil hydrocarbons relevant to refined fuels such as motor oil, diesel, and gasoline represents an extreme challenge for chromatographic and mass spectrometric techniques. This work incorporates two-dimensional gas chromatography coupled to a tunable vacuum ultraviolet soft photoionization source, the Chemical Dynamics Beamline 9.0.2 of the Advanced Light Source at the Lawrence Berkeley National Laboratory, with a time-of-flight mass spectrometer (GC × GC-VUV-TOF) to directly characterize and isomerically sum the contributions of aromatic and aliphatic species to hydrocarbon classes of four crude oils. When the VUV beam is tuned to 10.5 ± 0.2 eV, both aromatic and aliphatic crude oil hydrocarbons are ionized to reveal the complete chemical abundance of C 9 -C 30 hydrocarbons. When the VUV beam is tuned to 9.0 ± 0.2 eV only aromatic hydrocarbons are ionized, allowing separation of the aliphatic and aromatic fractions of the crude oil hydrocarbon chemical classes in an efficient manner while maintaining isomeric quantification. This technique provides an effective tool to determine the isomerically summed aromatic and aliphatic hydrocarbon compositions of crude oil, providing information that goes beyond typical GC × GC separations of the most dominant hydrocarbon isomers.

Problems of selectivity in liquid-phase oxidation

Energy Technology Data Exchange (ETDEWEB)

Emanuel, N M

1978-07-01

Based on a kinetic analysis of a generalized scheme for radical-chain process and on published experimental results, factors determining the selectivities of various liquid-phase oxidations of organic compounds are examined, including the kinetic chain length, molecular and chain decomposition of products, and competing routes in the initiated oxidation or autoxidation of hydrocarbons to peroxides. Also discussed are selective inhibition of undesirable routes in chain reactions, e.g., styrene and acetaldehyde co-oxidation; activation of molecular oxygen by variable-valence metal compounds used as homogeneous catalysts; modeling of fermentative processes by oxidation of hydrocarbons in complex catalytic systems, e.g., hydroxylation of alkanes, epoxidation or carbonylation of olefins, or oxidation of alcohols and ketones to acids; and the mechanisms of heterogeneous catalysis in liquid-phase reactions, e.g., oxidation of alkylaromatic hydrocarbons to peroxides and co-oxidation of propylene and acetaldehyde.

Sample preparation for large-scale bioanalytical studies based on liquid chromatographic techniques.

Science.gov (United States)

Medvedovici, Andrei; Bacalum, Elena; David, Victor

2018-01-01

Quality of the analytical data obtained for large-scale and long term bioanalytical studies based on liquid chromatography depends on a number of experimental factors including the choice of sample preparation method. This review discusses this tedious part of bioanalytical studies, applied to large-scale samples and using liquid chromatography coupled with different detector types as core analytical technique. The main sample preparation methods included in this paper are protein precipitation, liquid-liquid extraction, solid-phase extraction, derivatization and their versions. They are discussed by analytical performances, fields of applications, advantages and disadvantages. The cited literature covers mainly the analytical achievements during the last decade, although several previous papers became more valuable in time and they are included in this review. Copyright © 2017 John Wiley & Sons, Ltd.

Probabilistic peak detection for first-order chromatographic data.

Science.gov (United States)

Lopatka, M; Vivó-Truyols, G; Sjerps, M J

2014-03-19

We present a novel algorithm for probabilistic peak detection in first-order chromatographic data. Unlike conventional methods that deliver a binary answer pertaining to the expected presence or absence of a chromatographic peak, our method calculates the probability of a point being affected by such a peak. The algorithm makes use of chromatographic information (i.e. the expected width of a single peak and the standard deviation of baseline noise). As prior information of the existence of a peak in a chromatographic run, we make use of the statistical overlap theory. We formulate an exhaustive set of mutually exclusive hypotheses concerning presence or absence of different peak configurations. These models are evaluated by fitting a segment of chromatographic data by least-squares. The evaluation of these competing hypotheses can be performed as a Bayesian inferential task. We outline the potential advantages of adopting this approach for peak detection and provide several examples of both improved performance and increased flexibility afforded by our approach. Copyright © 2014 Elsevier B.V. All rights reserved.

Validation of a high-performance liquid chromatographic method with UV detection for the determination of ethopabate residues in poultry liver.

Science.gov (United States)

Granja, Rodrigo H M M; Niño, Alfredo M Montes; Zucchetti, Roberto A M; Niño, Rosario E Montes; Salerno, Alessandro G

2008-01-01

Ethopabate is frequently used in the prophylaxis and treatment of coccidiosis in poultry. Residues of this drug in food present a potential risk to consumers. A simple, rapid, and sensitive column high-performance liquid chromatographic (HPLC) method with UV detection for determination of ethopabate in poultry liver is presented. The drug is extracted with acetonitrile. After evaporation, the residue is dissolved with an acetone-hexane mixture and cleaned up by solid-phase extraction using Florisil columns. The analyte is then eluted with methanol. LC analysis is carried out on a C18 5 microm Gemini column, 15 cm x 4.6 mm. Ethopabate is quantified by means of UV detection at 270 nm. Parameters such as decision limit, detection capability, precision, recovery, ruggedness, and measurement uncertainty were calculated according to method validation guidelines provided in 2002/657/EC and ISO/IEC 17025:2005. Decision limit and detection capability were determined to be 2 and 3 microg/kg, respectively. Average recoveries from poultry samples fortified with 10, 15, and 20 microg/kg levels of ethopabate were 100-105%. A complete statistical analysis was performed on the results obtained, including an estimation of the method uncertainty. The method is to be implemented into Brazil's residue monitoring and control program for ethopabate.

Incorporating high-pressure electroosmotic pump and a nano-flow gradient generator into a miniaturized liquid chromatographic system for peptide analysis.

Science.gov (United States)

Chen, Apeng; Lynch, Kyle B; Wang, Xiaochun; Lu, Joann J; Gu, Congying; Liu, Shaorong

2014-09-24

We integrate a high-pressure electroosmotic pump (EOP), a nanoflow gradient generator, and a capillary column into a miniaturized liquid chromatographic system that can be directly coupled with a mass spectrometer for proteomic analysis. We have recently developed a low-cost high-pressure EOP capable of generating pressure of tens of thousands psi, ideal for uses in miniaturized HPLC. The pump worked smoothly when it was used for isocratic elutions. When it was used for gradient elutions, generating reproducible gradient profiles was challenging; because the pump rate fluctuated when the pump was used to pump high-content organic solvents. This presents an issue for separating proteins/peptides since high-content organic solvents are often utilized. In this work, we solve this problem by incorporating our high-pressure EOP with a nano-flow gradient generator so that the EOP needs only to pump an aqueous solution. With this combination, we develop a capillary-based nano-HPLC system capable of performing nano-flow gradient elution; the pump rate is stable, and the gradient profiles are reproducible and can be conveniently tuned. To demonstrate its utility, we couple it with either a UV absorbance detector or a mass spectrometer for peptide separations. Copyright © 2014. Published by Elsevier B.V.

Synthetic transformation into liquid hydrocarbons of organic liquids

Energy Technology Data Exchange (ETDEWEB)

Rousseau, F P.A.

1918-09-09

The transformation is obtained by a pyrogenation descending in a closed vessel instead of recourse to distillation ascending as is usually done, the material poor in hydrogen being hydrogenated by a contribution from the gas during the pyrogenation; synthesis with the vapors from the treated material will also be realized. As a first product there is obtained an analogue of naphtha or crude gasoline containing in the liquid state all the bodies composing the material pyrogenated. This first product is purified and rectified by successive distillation, acidulation, washing, etc., according to methods in use for refining petroleum obtained from the ground.

Thermodynamic and kinetic characterization of polycyclic aromatic hydrocarbons in reversed-phase liquid chromatography.

Science.gov (United States)

Howerton, Samuel B; McGuffin, Victoria L

2003-07-15

The retention of six polycyclic aromatic hydrocarbons (PAHs) was characterized by reversed-phase liquid chromatography. The PAHs were detected by laser-induced fluorescence at four points along an optically transparent capillary column. The profiles were characterized in space and time using an exponentially modified Gaussian equation. The resulting parameters were used to calculate the retention factors, as well as the concomitant changes in molar enthalpy and molar volume, for each PAH on monomeric (2.7 micromol/m2) and polymeric (5.4 micromol/m2) octadecylsilica. The changes in molar enthalpy become more exothermic as ring number increases and as annelation structure becomes less condensed. The changes in molar volume become more negative as ring number increases for the planar PAHs, but are positive for the nonplanar solutes. In addition, the rate constants, as well as the concomitant activation enthalpy and activation volume, are calculated for the first time. The kinetic data demonstrate that many of the PAHs exhibit very fast transitions between the mobile and stationary phases. The transition state is very high in energy, and the activation enthalpies and volumes become greater as ring number increases and as annelation structure becomes less condensed. The changes in thermodynamic and kinetic behavior are much more pronounced for the polymeric phase than for the monomeric phase.

A case study of the intrinsic bioremediation of petroleum hydrocarbons

Energy Technology Data Exchange (ETDEWEB)

Barker, G.W.; Raterman, K.T.; Fisher, J.B.; Corgan, J.M. [and others

1995-12-31

Condensate liquids have been found to contaminate soil and groundwater at two gas production sites in the Denver Basin operated by Amoco Production Co. These sites have been closely monitored since July 1993 to determine whether intrinsic aerobic or anaerobic bioremediation of hydrocarbons occurs at a sufficient rate and to an adequate endpoint to support a no-intervention decision. Groundwater monitoring and analysis of soil cores suggest that intrinsic bioremediation is occurring at these sites by multiple pathways including aerobic oxidation, Fe{sup 3+} reduction, and sulfate reduction. In laboratory experiments the addition of gas condensate hydrocarbons to saturated soil from the gas production site stimulated sulfate reduction under anaerobic and oxygen-limiting conditions, and nitrate and Fe{sup 3+} reduction under oxygen-limiting conditions, compared to biotic controls that lacked hydrocarbon and sterile controls. The sulfate reduction corresponded to a reduction in the amount of toluene relative to other hydrocarbons. These results confirmed that subsurface soils at the gas production site have the potential for intrinsic bioremediation of hydrocarbons.

Liquid chromatography with luminol-based electrochemiluminescence detection determination of histamine

NARCIS (Netherlands)

Steijger, O.M.; Kamminga, D.A.; Brummelhuis, A.; Lingeman, H.

1998-01-01

The liquid chromatographic determination of histamine was achieved by precolumn derivatization with N-(4-aminobutyl)-N-ethylisoluminol isothiocyanate and electrochemiluminescence detection. Detection was carried out using postcolumn on-line electrochemical reagent generation and oxidation of the

On the use of ionic liquids as mobile phase additives in high-performance liquid chromatography. A review.

Science.gov (United States)

García-Alvarez-Coque, M C; Ruiz-Angel, M J; Berthod, A; Carda-Broch, S

2015-07-09

The popularity of ionic liquids (ILs) has grown during the last decades in several analytical separation techniques. Consequently, the number of reports devoted to the applications of ILs is still increasing. This review is focused on the use of ILs (mainly imidazolium-based associated to chloride and tetrafluoroborate) as mobile phase additives in high-performance liquid chromatography (HPLC). In this approach, ILs just function as salts, but keep several kinds of intermolecular interactions, which are useful for chromatographic separations. Both cation and anion can be adsorbed on the stationary phase, creating a bilayer. This gives rise to hydrophobic, electrostatic and other specific interactions with the stationary phase and solutes, which modify the retention behaviour and peak shape. This review updates the advances in this field, with emphasis on topics not always deeply considered in the literature, such as the mechanisms of retention, the estimation of the suppressing potency of silanols, modelling and optimisation of the chromatographic performance, and the comparison with other additives traditionally used to avoid the silanol problem. Copyright © 2015 Elsevier B.V. All rights reserved.

Identification and quantification of flavonoids in human urine samples by column switching liquid chromatography coupled to atmospheric pressure chemical ionization mass spectrometry

DEFF Research Database (Denmark)

Nielsen, Salka E.; Freese, R.; Cornett, C.

2000-01-01

A rapid and sensitive high-performance liquid chromatographic mass spectrometric (HPLC-MS) method is described for the determination and quantification of 12 dietary flavonoid glycosides and aglycons in human urine samples. Chromatographic separation of the analytes of interest was achieved...

Process for preparing hydrocarbons

Energy Technology Data Exchange (ETDEWEB)

Krauch, C; Anther, E; Pier, M

1926-04-07

A process is described for the conversion of coal of all kinds, wood, oil, shale, as well as other carbonaceous materials into liquid hydrocarbons in two steps, characterized by treatment of the coal and so forth with a stream of hydrogen or hydrogen-containing gases at raised temperatures and raised pressures and producing a tarry product which, after separation of the ashlike residue, is converted by a further treatment, in the presence of catalysts, with hydrogen or hydrogen-containing gases at raised temperature and pressure, largely into low-boiling products.

Chromatographic Techniques for Rare Earth Elements Analysis

Science.gov (United States)

Chen, Beibei; He, Man; Zhang, Huashan; Jiang, Zucheng; Hu, Bin

2017-04-01

The present capability of rare earth element (REE) analysis has been achieved by the development of two instrumental techniques. The efficiency of spectroscopic methods was extraordinarily improved for the detection and determination of REE traces in various materials. On the other hand, the determination of REEs very often depends on the preconcentration and separation of REEs, and chromatographic techniques are very powerful tools for the separation of REEs. By coupling with sensitive detectors, many ambitious analytical tasks can be fulfilled. Liquid chromatography is the most widely used technique. Different combinations of stationary phases and mobile phases could be used in ion exchange chromatography, ion chromatography, ion-pair reverse-phase chromatography and some other techniques. The application of gas chromatography is limited because only volatile compounds of REEs can be separated. Thin-layer and paper chromatography are techniques that cannot be directly coupled with suitable detectors, which limit their applications. For special demands, separations can be performed by capillary electrophoresis, which has very high separation efficiency.

A simple subcritical chromatographic test for an extended ODS high performance liquid chromatography column classification.

Science.gov (United States)

Lesellier, Eric; Tchapla, Alain

2005-12-23

This paper describes a new test designed in subcritical fluid chromatography (SFC) to compare the commercial C18 stationary phase properties. This test provides, from a single analysis of carotenoid pigments, the absolute hydrophobicity, the silanol activity and the steric separation factor of the ODS stationary phases. Both the choice of the analytical conditions and the validation of the information obtained from the chromatographic measurements are detailed. Correlations of the carotenoid test results with results obtained from other tests (Tanaka, Engelhard, Sander and Wise) performed both in SFC and HPLC are discussed. Two separation factors, calculated from the retention of carotenoid pigments used as probe, allowed to draw a first classification diagram. Columns, which present identical chromatographic behaviors are located in the same area on this diagram. This location can be related to the stationary phase properties: endcapping treatments, bonding density, linkage functionality, specific area or silica pore diameter. From the first classification, eight groups of columns are distinguished. One group of polymer coated silica, three groups of polymeric octadecyl phases, depending on the pore size and the endcapping treatment, and four groups of monomeric stationary phases. An additional classification of the four monomeric groups allows the comparison of these stationary phases inside each group by using the total hydrophobicity. One hundred and twenty-nine columns were analysed by this simple and rapid test, which allows a comparison of columns with the aim of helping along their choice in HPLC.

Conversion of associated natural gas to liquid hydrocarbons. Final report, June 1, 1995--January 31, 1997

Energy Technology Data Exchange (ETDEWEB)

NONE

1997-12-31

The original concept envisioned for the use of Fischer-Tropsch processing (FTP) of United States associated natural gas in this study was to provide a way of utilizing gas which could not be brought to market because a pipeline was not available or for which there was no local use. Conversion of gas by FTP could provide a means of utilizing offshore associated gas which would not require installation of a pipeline or re-injection. The premium quality F-T hydrocarbons produced by conversion of the gas can be transported in the same way as the crude oil or in combination (blended) with it, eliminating the need for a separate gas transport system. FTP will produce a synthetic crude oil, thus increasing the effective size of the resource. The two conventional approaches currently used in US territory for handling of natural gas associated with crude petroleum production are re-injection and pipelining. Conversion of natural gas to a liquid product which can be transported to shore by tanker can be accomplished by FTP to produce hydrocarbons, or by conversion to chemical products such as methanol or ammonia, or by cryogenic liquefaction (LNG). This study considers FTP and briefly compares it to methanol and LNG. The Energy International Corporation cobalt catalyst, ratio adjusted, slurry bubble column F-T process was used as the basis for the study and the comparisons. An offshore F-T plant can best be accommodated by an FPSO (Floating Production, Storage, Offloading vessel) based on a converted surplus tanker, such as have been frequently used around the world recently. Other structure types used in deep water (platforms) are more expensive and cannot handle the required load.

Buffer-Free High Performance Liquid Chromatography Method for ...

African Journals Online (AJOL)

Purpose: To develop and validate a simple, economical and reproducible high performance liquid chromatographic (HPLC) method for the determination of theophylline in pharmaceutical dosage forms. Method: Caffeine was used as the internal standard and reversed phase C-18 column was used to elute the drug and ...

Determination of marker pteridins and biopterin reduced forms, tetrahydrobiopterin and dihydrobiopterin, in human urine, using a post-column photoinduced fluorescence liquid chromatographic derivatization method

International Nuclear Information System (INIS)

Canada-Canada, Florentina; Espinosa-Mansilla, Anunciacion; Munoz de la Pena, Arsenio; Mancha de Llanos, Alicia

2009-01-01

A liquid chromatographic method for the simultaneous analysis of marker pteridins and biopterin reduced forms, in urine samples is proposed. A Zorbax Eclipse XDB-C18 column was used for the chromatographic separation, using a 98/2 (v/v), citrate buffer (pH 5.5)-acetonitrile mobile phase, in isocratic mode. A post-column photoderivatization was carried out with an on-line photoreactor, located between a diode array detector (DAD) and a fast scanning fluorescence detector (FSFD). Neopterin (NEO), biopterin (BIO), pterin (PT) and dihydrobiopterin (BH2) were determined by measuring native fluorescence, using the photoreactor in OFF-mode, and tetrahydrobiopterin (BH4) was determined by measuring of the induced fluorescence of the generated photoproducts, using the photoreactor in ON-mode. In addition, Creatinine (CREA), as a reference of metabolites excrection in urine, was simultaneously determined using the DAD detector. Detection limits were 0.2, 13.0, 0.3, 0.3 and 3.5 ng mL -1 , for NEO, BH2, BIO, PT and BH4, respectively, and 0.4 μg mL -1 for CREA. Ratio values for NEO/CREA, PT/CREA, BH4/CREA, BH2/CREA, NEO/BIO and BIO total /CREA, in urine samples, of healthy children and adults, phenylketonuric children and infected mononucleosis children, are reported. A comparative study, about the mean values obtained for each of the compounds, by the present procedure and by the classical iodine oxidation method (Fukushimas method), has been performed, in urine samples belonging to healthy volunteers. The values obtained were BH4/CREA: 0.41, BH2/CREA: 0.31 and BIO total /CREA: 0.73, by the proposed method, and BH4/CREA: 0.35, BH2/CREA: 0.20 and BIO total /CREA: 0.48, by iodine oxidation method.

Determination of marker pteridins and biopterin reduced forms, tetrahydrobiopterin and dihydrobiopterin, in human urine, using a post-column photoinduced fluorescence liquid chromatographic derivatization method

Energy Technology Data Exchange (ETDEWEB)

Canada-Canada, Florentina, E-mail: floricanada@gmail.com [Department of Analytical Chemistry, University of Extremadura, 06071 Badajoz (Spain); Espinosa-Mansilla, Anunciacion; Munoz de la Pena, Arsenio; Mancha de Llanos, Alicia [Department of Analytical Chemistry, University of Extremadura, 06071 Badajoz (Spain)

2009-08-19

A liquid chromatographic method for the simultaneous analysis of marker pteridins and biopterin reduced forms, in urine samples is proposed. A Zorbax Eclipse XDB-C18 column was used for the chromatographic separation, using a 98/2 (v/v), citrate buffer (pH 5.5)-acetonitrile mobile phase, in isocratic mode. A post-column photoderivatization was carried out with an on-line photoreactor, located between a diode array detector (DAD) and a fast scanning fluorescence detector (FSFD). Neopterin (NEO), biopterin (BIO), pterin (PT) and dihydrobiopterin (BH2) were determined by measuring native fluorescence, using the photoreactor in OFF-mode, and tetrahydrobiopterin (BH4) was determined by measuring of the induced fluorescence of the generated photoproducts, using the photoreactor in ON-mode. In addition, Creatinine (CREA), as a reference of metabolites excrection in urine, was simultaneously determined using the DAD detector. Detection limits were 0.2, 13.0, 0.3, 0.3 and 3.5 ng mL{sup -1}, for NEO, BH2, BIO, PT and BH4, respectively, and 0.4 {mu}g mL{sup -1} for CREA. Ratio values for NEO/CREA, PT/CREA, BH4/CREA, BH2/CREA, NEO/BIO and BIO{sub total}/CREA, in urine samples, of healthy children and adults, phenylketonuric children and infected mononucleosis children, are reported. A comparative study, about the mean values obtained for each of the compounds, by the present procedure and by the classical iodine oxidation method (Fukushimas method), has been performed, in urine samples belonging to healthy volunteers. The values obtained were BH4/CREA: 0.41, BH2/CREA: 0.31 and BIO{sub total}/CREA: 0.73, by the proposed method, and BH4/CREA: 0.35, BH2/CREA: 0.20 and BIO{sub total}/CREA: 0.48, by iodine oxidation method.

Single component, reversible ionic liquids for energy applications

Energy Technology Data Exchange (ETDEWEB)

Vittoria Blasucci; Ryan Hart; Veronica Llopis Mestre; Dominique Julia Hahne; Melissa Burlager; Hillary Huttenhower; Beng Joo Reginald Thio; Pamela Pollet; Charles L. Liotta; Charles A. Eckert [Georgia Institute of Technology, Atlanta, GA (United States). Chemical & Biomolecular Engineering

2010-06-15

Single component, reversible ionic liquids have excellent potential as novel solvents for a variety of energy applications. Our energy industry is faced with many new challenges including increased energy consumption, depleting oil reserves, and increased environmental awareness. We report the use of reversible ionic liquids to solve two energy challenges: extraction of hydrocarbons from contaminated crude oil and carbon capture from power plant flue gas streams. Our reversible solvents are derived from silylated amine molecular liquids which react with carbon dioxide reversibly to form ionic liquids. Here we compare the properties of various silylated amine precursors and their corresponding ionic liquids. We show how the property changes are advantageous in the two aforementioned energy applications. In the case of hydrocarbon purification, we take advantage of the polarity switch between precursor and ionic liquid to enable separations. In carbon capture, our solvents act as dual physical and chemical capture agents for carbon dioxide. Finally, we show the potential economics of scale-up for both processes. 20 refs., 1 fig., 3 tabs.

Evaluation of the suitability of chromatographic systems to predict human skin permeation of neutral compounds.

Science.gov (United States)

Hidalgo-Rodríguez, Marta; Soriano-Meseguer, Sara; Fuguet, Elisabet; Ràfols, Clara; Rosés, Martí

2013-12-18

Several chromatographic systems (three systems of high-performance liquid chromatography and two micellar electrokinetic chromatography systems) besides the reference octanol-water partition system are evaluated by a systematic procedure previously proposed in order to know their ability to model human skin permeation. The precision achieved when skin-water permeability coefficients are correlated against chromatographic retention factors is predicted within the framework of the solvation parameter model. It consists in estimating the contribution of error due to the biological and chromatographic data, as well as the error coming from the dissimilarity between the human skin permeation and the chromatographic systems. Both predictions and experimental tests show that all correlations are greatly affected by the considerable uncertainty of the skin permeability data and the error associated to the dissimilarity between the systems. Correlations with much better predictive abilities are achieved when the volume of the solute is used as additional variable, which illustrates the main roles of both lipophilicity and size of the solute to penetrate through the skin. In this way, the considered systems are able to give precise estimations of human skin permeability coefficients. In particular, the HPLC systems with common C18 columns provide the best performances in emulating the permeation of neutral compounds from aqueous solution through the human skin. As a result, a methodology based on easy, fast, and economical HPLC measurements in a common C18 column has been developed. After a validation based on training and test sets, the method has been applied with good results to the estimation of skin permeation of several hormones and pesticides. Copyright © 2013 Elsevier B.V. All rights reserved.

High-performance liquid chromatographic radioenzymatic assay for plasma catecyholamines

International Nuclear Information System (INIS)

Klaniecki, T.S.; Corder, C.N.; McDonald, R.H. Jr.; Feldman, J.A.

1977-01-01

A new assay method for plasma catecholamimes (CA) requiring only 50 μl has been developed, which uses high performance liquid chromatography (HPLC). The norepinephrine (NE), dopamine (D), and epinephrine (E) compounds found in plasma are radioactively o-methylated with S-[methyl- 3 H]-adenosyl-L-methionine ( 3 H-SAM) 3 H-SAM by the reaction of catechol-o-methyl transferase (COMT). The reaction is terminated and a standard mixture of nonradioactive o-methylated analogues of NE, D, and E is added to act as a carrier. Following separation by HPLC, the D,L-normetanephrine (NMN), 3-methoxy-4-hydroxyphenylethyl-amine or 3-methoxytyramine (3-MOT), and metanephrine (MN) radioactive peaks are collected which represent NE, D, and E, respectively. Then MNM and MN are oxidized to vanillin, and 3-MOT is acetylated. The products are subsequently separated by solvent extraction. This is necessary in order to avoid high radioactive blanks and to allow quantitation of the radioactivity by liquid scintillation spectrometry. The mean supine levels of NE, D, and E in normal subjects were respectively 182, 33, and 87 pg/ml of plasma. Similar assays on patients with pheochromocytoma revealed 797, 80, and 470 pg/ml

Determination of heavy polycyclic aromatic hydrocarbons by non-aqueous reversed phase liquid chromatography: Application and limitation in refining streams.

Science.gov (United States)

Panda, Saroj K; Muller, Hendrik; Al-Qunaysi, Thunayyan A; Koseoglu, Omer R

2018-01-19

The heavy polycyclic aromatic hydrocarbons (HPAHs) cause detrimental effects to hydrocracker operations by deactivating the catalysts and depositing in the downstream of the reactor/ exchangers. Therefore, it is essential to continuously monitor the accumulation of HPAHs in a hydrocracker unit. To accurately measure the concentration of HPAHs, the development of a fast and reliable analytical method is inevitable. In this work, an analytical method based on non-aqueous reversed phase chromatography in combination with high resolution Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) was developed. As a first step, five different types of stationary phases were evaluated for the separation of HPAHs in non-aqueous mode and the best suited phase was further used for the fractionation of HPAHs in a fractionator bottom sample obtained from a refinery hydrocracker unit. The eight major fractions or peaks obtained from the separation were further characterized by UV spectroscopy and FT-ICR MS and the compounds in the fractions were tentatively confirmed as benzoperylene, coronene, methylcoronene, naphthenocoronene, benzocoronene, dibenzoperylene, naphthocoronene and ovalene. The developed liquid chromatography method can be easily adapted in a refinery laboratory for the quantitation of HPAHs in hydrocracking products. The method was further tested to check the interference of sulfur aromatics and/or large alkylated aromatic hydrocarbons on the determination of HPAHs in hydrocracking products. Copyright © 2017 Elsevier B.V. All rights reserved.

Development of new process network for gas chromatograph and analyzers connected with SCADA system and Digital Control Computers at Cernavoda NPP Unit 1

International Nuclear Information System (INIS)

Deneanu, Cornel; Popa Nemoiu, Dragos; Nica, Dana; Bucur, Cosmin

2007-01-01

The continuous monitoring of gas mixture concentrations (deuterium/ hydrogen/oxygen/nitrogen) accumulated in 'Moderator Cover Gas', 'Liquid Control Zone' and 'Heat Transport D 2 O Storage Tank Cover Gas', as well as the continuous monitoring of Heavy Water into Light Water concentration in 'Boilers Steam', 'Boilers Blown Down', 'Moderator heat exchangers', and 'Recirculated Water System', sensing any leaks of Cernavoda NPP U1 led to requirement of developing a new process network for gas chromatograph and analyzers connected to the SCADA system and Digital Control Computers of Cernavoda NPP Unit 1. In 2005 it was designed and implemented the process network for gas chromatograph which connected the gas chromatograph equipment to the SCADA system and Digital Control Computers of the Cernavoda NPP Unit 1. Later this process network for gas chromatograph has been extended to connect the AE13 and AE14 Fourier Transform Infrared (FTIR) analyzers with either. The Gas Chromatograph equipment measures with best accuracy the mixture gases (deuterium/ hydrogen/oxygen/nitrogen) concentration. The Fourier Transform Infrared (FTIR) AE13 and AE14 Analyzers measure the Heavy Water into Light Water concentration in Boilers Steam, Boilers BlownDown, Moderator heat exchangers, and Recirculated Water System, monitoring and signaling any leaks. The Gas Chromatograph equipment and Fourier Transform Infrared (FTIR) AE13 and AE14 Analyzers use the new OPC (Object Link Embedded for Process Control) technologies available in ABB's VistaNet network for interoperability with automation equipment. This new process network has interconnected the ABB chromatograph and Fourier Transform Infrared analyzers with plant Digital Control Computers using new technology. The result was an increased reliability and capability for inspection and improved system safety

High Performance Liquid Chromatographic Analysis of Almotriptan Malate in Bulk and Tablets

Directory of Open Access Journals (Sweden)

Chandra Bala Sekaran

2013-02-01

Full Text Available Purpose: A simple RP-HPLC method has been developed and validated for the determination of almotriptan malate (ATM in bulk and tablets. Methods: Chromatographic separation of ATM was achieved by using a Thermo Scientific C18 column. A Mobile phase containing a mixture of methanol, water and acetic acid (4:8:0.1 v/v was pumped at the flow rate of 1 mL/min. Detection was performed at 227 nm. According to ICH guidelines, the method was validated. Results: The calibration curve was linear in the concentration range 5–60 μg/mL for the ATM with regression coefficient 0.9999. The method was precise with RSD <1.2%. Excellent recoveries of 99.60 - 100.80% proved the accuracy of the method. The limits of detection and quantification were found to be 0.025 and 0.075 μg/mL, respectively. Conclusion: The method was successfully applied for the quantification of ATM in tablets with acceptable accuracy and precision.

Gas-liquid chromatography measurements of activity coefficients at infinite dilution of various organic solutes and water in tri-iso-butylmethylphosphonium tosylate ionic liquid

International Nuclear Information System (INIS)

Domanska, Urszula; Paduszynski, Kamil

2010-01-01

Activity coefficients at infinite dilution (γ 13 ∞ ) of 33 different solutes (including alkanes, cycloalkanes, alkenes, alkynes, benzene, alkylbenzenes, water, alcohols, MTBE, thiophene and THF) in the ionic liquid tri-iso-butylmethylphosphonium tosylate have been determined by using the GLC method and have been reported over the temperature range (298.15 to 368.15) K. The partial molar excess enthalpies of mixing at infinite dilution have been determined based on temperature dependence of γ 13 ∞ . Selectivity and capacity at infinite dilution has been also calculated for exemplary separation processes in systems n-hexane/benzene and n-hexane/thiophene, to evaluate if the studied ionic liquid is capable to be a good entrainer for these processes, e.g. in the liquid-liquid extraction. The obtained results are promising however the ionic liquid studied shows a lower selectivity than some of imidazolium-based ionic liquids. To our best knowledge, the results indicate that tri-iso-butylmethylphosphonium tosylate is the best for the separation problem of aliphatic hydrocarbons from aromatic hydrocarbons among all of the studied quaternary phosphonium-based ionic liquids.

Fundamentals of Hydrocarbon Upgrading to Liquid Fuels and Commodity Chemicals over Catalytic Metallic Nanoparticles

Science.gov (United States)

Chen, Tao

Promising new technologies for biomass conversion into fuels and chemical feedstocks rely on the production of bio-oils, which need to be upgraded in order to remove oxygen-containing hydrocarbons and water. A high oxygen concentration makes bio-oils acidic and corrosive, unstable during storage, and less energetically valuable per unit weight than petroleum-derived hydrocarbons. Although there are efficient processes for the production of bio-oils, there are no efficient technologies for their upgrading. Current technologies utilize traditional petroleum refining catalysts, which are not optimized for biomass processing. New upgrading technologies are, therefore, urgently needed for development of sustainable energy resources. Development of such new technologies, however, is severely hindered by a lack of fundamental understanding of how oxygen and oxygen-containing hydrocarbons derived from biomass interact with promising noble-metal catalysts. In this study, kinetic reaction measurements, catalyst characterization and quantum chemical calculations using density functional theory were combined for determining adsorption modes and reaction mechanisms of hydrocarbons in the presence of oxygen on surfaces of catalytic noble-metal nanoparticles. The results were used for developing improved catalyst formulations and optimization of reaction conditions. The addition of molybdenum to platinum catalysts was shown to improve catalytic activity, stability, and selectivity in hydrodeoxygenation of acetic acid, which served as a model biomass compound. The fundamental results that describe interactions of oxygen and hydrocarbons with noble-metal catalysts were extended to other reactions and fields of study: evaluation of the reaction mechanism for hydrogen peroxide decomposition, development of improved hydrogenation catalysts and determination of adsorption modes of a spectroscopic probe molecule.

Source rock hydrocarbons. Present status

International Nuclear Information System (INIS)

Vially, R.; Maisonnier, G.; Rouaud, T.

2013-01-01

This report first presents the characteristics of conventional oil and gas system, and the classification of liquid and gaseous non conventional hydrocarbons, with the peculiar case of coal-bed methane. The authors then describe how source rock hydrocarbons are produced: production of shale oils and gases (horizontal drilling, hydraulic fracturing, exploitation) and of coal-bed methane and coal mine methane. In the next part, they address and discuss the environmental impact of source rock hydrocarbon production: installation footprint, water resource management, drilling fluids, fracturing fluids composition, toxicity and recycling, air pollution, induced seismicity, pollutions from other exploitation and production activities. They propose an overview of the exploitation and production of source rock gas, coal-bed gas and other non conventional gases in the world. They describe the current development and discuss their economic impacts: world oil context and trends in the USA, in Canada and other countries, impacts on the North American market, on the world oil industry, on refining industries, on the world oil balance. They analyse the economic impacts of non conventional gases: development potential, stakes for the world gas trade, consequence for gas prices, development opportunities for oil companies and for the transport sector, impact on CO 2 emissions, macro-economic impact in the case of the USA

Qualitative and quantitative analysis of light hydrocarbons produced by radiation degradation of N, N-dimethyl hydroxylamine

International Nuclear Information System (INIS)

Wang Jinhua; Bao Borong; Wu Minghong; Sun Xilian; Zhang Xianye; Hu Jingxin; Ye Guoan

2004-01-01

This paper reports the qualitative and quantitative analysis of light hydrocarbons produced by radiation degradation of N, N-dimethyl hydroxylamine. These analyses were performed on the gas chromatograph, in which porous layer open tubular column coated with aluminum oxide and flame-ionization detector are used. For the doses between 10 and 1000 kGy, the light hydrocarbons produced by radiation degradation of N,N-dimethyl hydroxylamine are methane, ethane, ethene, propane, propene and n-butane. When the concentration of N,N-dimethyl hydroxylamine is 0.2 mol/L, the volume fraction of methane is (9.996-247.5) x 10 -6 , the volume fraction of ethane, propane and n-butane is lower and that of ethene and propene is much lower. With the increase of dose the volume fraction of methane is increased but the volume fraction of ethane, ethene, propane, propene and n-butane is not obviously changed. (authors)

Solid-Phase Extraction Combined with High Performance Liquid ...

African Journals Online (AJOL)

Methods: Solid-phase extraction method was employed for the extraction of the estrogen from milk and high performance liquid chromatography-diode array detector (HPLC-DAD) was used for the determination of estrogen. Results: Optimal chromatographic conditions were achieved on an Eclipse XDB-C18 column at a ...

Determination of the ionisation potential of certain hydrocarbons in the liquid phase

International Nuclear Information System (INIS)

Casanovas, J.; Grob, R.; Brunet, G.; Sabattier, R.; Guelfucci, J.P.; Blanc, D.

1978-01-01

The first results obtained are presented on the determination of the ionisation potential of four alkanes (n-hexane, n-pentane, cyclopentane and trimethyl-2,2,4 pentane) in the liquid phase. In the gaseous phase, the ionisation potential values of these hydrocarbons are respectively 10.18 eV for n-hexane, 10.35 eV for n-pentane, 10.53 eV for cyclopentane and 9.86 eV for trimethyl-2,2,4 pentane. Consequently rare gas resonance lamps (krypton and Xenon) were made, sealed and excited by an ultra-high frequency wave, which emit photons in the energy field concerned, i.e. from 8.5 eV to 11eV. The energy of the photons emitted by these lamps is respectively 8.44 eV (100%) and 9.57 eV (2%) for xenon and 10.03 eV (100%) and 10.64 eV (5%) for krypton. From the extent of the induced ionisation currents and particularly the value of the ratio of the currents induced by the photons of the krypton and xenon lamps, a minimum value of the ionisation potential drop can be deduced compared with the gas phase of 0.61 eV for n-hexane, 0.78 eV for n-pentane, 0.96 eV for cyclopentane and a maximum value of 1.42 eV for trimethyl-2,2,4 pentane [fr

Surfactant-enhanced recovery of dissolved hydrocarbons at petroleum production facilities

International Nuclear Information System (INIS)

Freeman, J.T.; Mayes, M.; Wassmuth, F.; Taylor, K.; Rae, W.; Kuipers, F.

1997-01-01

The feasibility and cost effectiveness of surfactant-enhanced pumping to reduce source concentrations of petroleum hydrocarbons from contaminated soils was discussed. Light non-aqueous phase liquids (LNAPL) hydrocarbons are present beneath many petroleum production processing facilities in western Canada. Complete removal of LNAPLs from geologic materials is difficult and expensive. Treatment technologies include costly ex-situ methods such as excavation and in-situ methods such as physical extraction by soil venting and pumping, bioremediation, and combination methods such as bioventing, bioslurping or air sparging. Surfactant-aided pumping can reduce source hydrocarbon concentrations when used in conjunction with traditional pump and treat, or deep well injection. This study involved the selection of an appropriate surfactant from a wide variety of commercially available products. A site contaminated by hydrocarbons in Turner Valley, Alberta, was used for field scale testing. One of the major problems was quantifying the increase in the dissolved hydrocarbon concentrations in the recovered water once a surfactant was added. From the 30 surfactants screened in a series of washing and oil solubilization tests, two surfactants, Brij 97 and Tween 80, were selected for further evaluation. Increased hydrocarbon recovery was observed within 10 days of the introduction of the first surfactant. 2 refs., 7 figs

Etude d'équations d'état en vue de représenter les propriétés PVT et les équilibres liquide-vapeur d'hydrocarbures Equations of State for Representing Pvt Properties and Vapor-Liquid Equilibria of Hydrocarbons

Directory of Open Access Journals (Sweden)

Neau E.

2006-11-01

Full Text Available Une étude comparative de plusieurs équations d'état issues de la théorie de van der Waals a été effectuée dans le but de sélectionner des modèles capables de calculer les propriétés PVT d'hydrocarbures dans un large domaine de pression et température. 34 hydrocarbures de différentes tailles et structures ont été sélectionnés. Les données expérimentales d'équilibres liquide-vapeur (pressions de vapeur, volumes des liquides et les propriétés PVT de fluides comprimés ont été systématiquement comparées avec des résultats obtenus au moyen de différentes équations d'état. Il est apparu que seules les équations d'état complexes (notamment l'équation COR sont en mesure de représenter correctement les propriétés volumétriques dans un large domaine de température et de pression, le voisinage du point critique inclu. A comparative study of several equations of state (EOS derived from the van der Waals theory was performed. The aim was to select the models able to represent PVT properties of hydrocarbons in large pressure and temperature ranges. 34 hydrocarbons of various sizes and structures were selected. Experimental data of vapor liquid equilibria (vapor pressures and liquid volumes and PVT properties of compressed fluids were systematically compared with results obtained using selected EOS. It was shown that only the complex EOS (especially the COR equation are able to represent volumetric properties in wide temperature and presssure ranges, the critical region included.

Liquid chromatographic-tandem mass spectrometric method for the simultaneous determination of alkylphenols polyethoxylates, alkylphenoxy carboxylates and alkylphenols in wastewater and surface-water.

Science.gov (United States)

Ciofi, L; Ancillotti, C; Chiuminatto, U; Fibbi, D; Checchini, L; Orlandini, S; Del Bubba, M

2014-10-03

Four different pellicular stationary phases (i.e. octadecylsilane, octasilane, Phenyl-Hexyl and pentafluorophenyl) were investigated for the chromatographic resolution of alkylphenols (APs), alkylphenols polyethoxylates (APnEOs) and alkylphenoxy carboxylates (APECs) using mixtures of water and organic solvents (i.e. methanol, acetonitrile and tetrahydrofuran) as eluents, in order to obtain their determination by a single LC-MS/MS run. In fact, alkylphenols and alkylphenoxy carboxylates must be analysed in negative ion mode, whereas alkylphenols polyethoxylates undergo ionisation only in positive ion mode, and therefore, two distinct LC-MS/MS analysis are commonly adopted. The best resolution among the aforementioned target analytes was achieved on the pentafluorophenyl column, eluting with an acidified water-acetonitrile-tetrahydrofuran mixture and using the post column addition of an ammonia solution in methanol for the detection of positively ionisable compounds. Under these optimized chromatographic conditions the investigated compounds were determined via a single chromatographic run, with only one polarity switch, in 15min, achieving the following instrumental detection limits: 600pg for AP1EOs, 0.8-14pg for AP2EOs, 10.4-150pg for APs and 4.4-4.8pg for APECs. The chromatographic method was coupled with solid-phase extraction and clean-up procedures and successfully applied to the analysis of wastewater and surface water samples, highlighting mean concentration ranging from 6ng/L for 4-t-OP1EC to 1434ng/L for 4-NP1121EC, depending on the sample analysed. Copyright © 2014 Elsevier B.V. All rights reserved.

Fuel gas production by microwave plasma in liquid

International Nuclear Information System (INIS)

Nomura, Shinfuku; Toyota, Hiromichi; Tawara, Michinaga; Yamashita, Hiroshi; Matsumoto, Kenya

2006-01-01

We propose to apply plasma in liquid to replace gas-phase plasma because we expect much higher reaction rates for the chemical deposition of plasma in liquid than for chemical vapor deposition. A reactor for producing microwave plasma in a liquid could produce plasma in hydrocarbon liquids and waste oils. Generated gases consist of up to 81% hydrogen by volume. We confirmed that fuel gases such as methane and ethylene can be produced by microwave plasma in liquid

The precise measurement of the (vapour + liquid) equilibrium properties for (CO2 + isobutane) binary mixtures

International Nuclear Information System (INIS)

Nagata, Y.; Mizutani, K.; Miyamoto, H.

2011-01-01

Recently, it has been suggested that natural working fluids, such as CO 2 , hydrocarbons, and their mixtures, could provide a long-term alternative to fluorocarbon refrigerants. (Vapour + liquid) equilibrium (VLE) data for these fluids are essential for the development of equations of state, and for industrial process such as separation and refinement. However, there are large inconsistencies among the available literature data for (CO 2 + isobutane) binary mixtures, and therefore provision of reliable and new measurements with expanded uncertainties is required. In this study, we determined precise VLE data using a new re-circulating type apparatus, which was mainly designed by Akico Co., Japan. An equilibrium cell with an inner volume of about 380 cm 3 and two optical windows was used to observe the phase behaviour. The cell had re-circulating loops and expansion loops that were immersed in a thermostatted liquid bath and air bath, respectively. After establishment of a steady state in these loops, the compositions of the samples were measured by a gas chromatograph (GL Science, GC-3200). The VLE data were measured for CO 2 /propane and CO 2 /isobutane binary mixtures within the temperature range from 300 K to 330 K and at pressures up to 7 MPa. These data were compared with the available literature data and with values predicted by thermodynamic property models.

Probabilistic peak detection for first-order chromatographic data

NARCIS (Netherlands)

Lopatka, M.; Vivó-Truyols, G.; Sjerps, M.J.

2014-01-01

We present a novel algorithm for probabilistic peak detection in first-order chromatographic data. Unlike conventional methods that deliver a binary answer pertaining to the expected presence or absence of a chromatographic peak, our method calculates the probability of a point being affected by

A New High-Performance Liquid Chromatographic Method for the Determination and Distribution of Linalool in Michelia alba

Directory of Open Access Journals (Sweden)

Hua-Bin Li

2010-07-01

Full Text Available A new high-performance liquid chromatographic method with photodiode array detection was established for the determination of linalool in the plant Michelia alba. Linalool was extracted from the plant sample with the aid of ultrasound, and was analyzed on a Waters RP C18 column (4.6 × 150 mm, 5 μm using an acetonitrile and water (55:45, v/v mobile phase at a flow rate of 1.0 mL/min. The column temperature was set at 25 ºC, and the detection wavelength was 210 nm. The linear range of the method was 5–200 μg/mL with a correlation coefficient of 0.9975. The recovery was 92–112%, and the relative standard deviation was 1.85% (n = 9. The present method has been used to study the distribution of linalool in the plant Michelia alba. The plant samples include flowers, leaves and tender twigs. Furthermore, leaves included samples in their tender, grown-up and fallen phases, and flowers included samples in their juvenile, middle and whitening phases. The concentrations of linalool in different parts of the plant were 0.21–0.65%, 1.63–4.89% and 0.43% for leaves, flowers and tender twigs, respectively. The results showed that all the plant materials contained relative high concentration of linalool, and juvenile phase flowers contained the highest concentration of linalool. Notably, the fallen leaves also contained high concentrations of linalool, which could be a potential resource of this compound. The results obtained are very helpful for the potential full utilization of this plant.

Separation of tungsten from molybdenum by liquid-liquid extraction and extraction chromatography using thiocyanate and a quarternary ammonium salt

International Nuclear Information System (INIS)

Yonezawa, C.; Onishi, H.

1977-01-01

Methods were developed for the separation of tungsten from molybdenum by liquid-liquid extraction and extraction chromatography using thiocyanate and a quaternary ammonium salt, Zephiramine. Tungsten was extracted into chloroform as an ion associate of tungsten(V)-thiocyanate complex and Zephiramine cation was retained on a column of Teflon powder coated with Zephiramine, but molybdenum(III) was neither extracted nor retained. The extraction chromatographic method was succesfully applied to the determination of trace amounts of tungsten in molybdenum by neutron activation analysis. The γ-ray spectrum, observed with the Ge(Li) detector, of tungsten fraction separated from irradiated molybdenum are shown. The peaks of 99 Mo, sup(99m)Tc, and sup(99m)Nb (produced by 92 Mo(n,p)sup(99m)Nb) were seen, but these nuclides did nit interfere with the determination of tungsten using a NaI(Tl) detector. The results of the neutron activation analysis of a sample of ammonium molybdate agreed quite well with that of the spectrophotometric determination after extraction chromatographic separation. (T.G.)

Deashing of coal liquids with ceramic membrane microfiltration and diafiltration

Energy Technology Data Exchange (ETDEWEB)

Bishop, B.; Goldsmith, R. [CeraMem Corp., Waltham, MA (United States)

1995-12-31

Removal of mineral matter from liquid hydrocarbons derived from the direct liquefaction of coal is required for product acceptability. Current methods include critical solvent deashing (Rose{sup {reg_sign}} process from Kerr-McGee) and filtration (U.S. Filter leaf filter as used by British Coal). These methods produce ash reject streams containing up to 15% of the liquid hydrocarbon product. Consequently, CeraMem proposed the use of low cost, ceramic crossflow membranes for the filtration of coal liquids bottoms to remove mineral matter and subsequent diafiltration (analogous to cake washing in dead-ended filtration) for the removal of coal liquid from the solids stream. The use of these ceramic crossflow membranes overcomes the limitations of traditional polymeric crossflow membranes by having the ability to operate at elevated temperature and to withstand prolonged exposure to hydrocarbon and solvent media. In addition, CeraMem`s membrane filters are significantly less expensive than competitive ceramic membranes due to their unique construction. With these ceramic membrane filters, it may be possible to reduce the product losses associated with traditional deashing processes at an economically attractive cost. The performance of these ceramic membrane microfilters is discussed.

Water Pollution Studies on Baher El-Bakar Mouth Northeast Nile-Delta, Egypt

International Nuclear Information System (INIS)

Moustafa, Y.M.; Abd El-Hakem, M.; Abdallah, R.I.; Barakat, M.A.K.

2005-01-01

Environmental assessments of petroleum contaminants in the surface water at the north nile delta (Baher El-Bakar mouth) were investigated. Quantitative determinations of oil content show that the studied areas have values high enough to cause lethal toxicity to the surrounding environment gas chromatographic (GC) studies reveal that the origin of pollutants is mainly petroleum origin (petrogenic) mixed with biogenic hydrocarbons. The studied samples are either highly or very highly weathered indicating that they suffered from chronic oil pollution. It is generally advisable to support gas chromatographic evidence by other methods of analysis. Ultraviolet spectrophotometric (UV) studies reflect the presence of aromatic compounds. Their detection is a good criterion of oil pollution. High performance liquid chromatography (HPLC) is used to investigate the distribution of individual pol cyclic aromatic hydrocarbons in water samples. Data indicate that all samples are characterized by the presence of Dibenzo (a,h) anthracene. Microscopic examination is used to investigate the characteristics of the particulate matter associated with the water samples

Viscosity Prediction of Hydrocarbon Mixtures Based on the Friction Theory

DEFF Research Database (Denmark)

Zeberg-Mikkelsen, Claus Kjær; Cisneros, Sergio; Stenby, Erling Halfdan

2001-01-01

The application and capability of the friction theory (f-theory) for viscosity predictions of hydrocarbon fluids is further illustrated by predicting the viscosity of binary and ternary liquid mixtures composed of n-alkanes ranging from n-pentane to n-decane for wide ranges of temperature and from...

Analysis of hydrocarbons generated in coalbeds

Science.gov (United States)

Butala, Steven John M.

This dissertation describes kinetic calculations using literature data to predict formation rates and product yields of oil and gas at typical low-temperature conditions in coalbeds. These data indicate that gas formation rates from hydrocarbon thermolysis are too low to have generated commercial quantities of natural gas, assuming bulk first-order kinetics. Acid-mineral-catalyzed cracking, transition-metal-catalyzed hydrogenolysis of liquid hydrocarbons, and catalyzed CO2 hydrogenation form gas at high rates. The gaseous product compositions for these reactions are nearly the same as those for typical natural coalbed gases, while those from thermal and catalytic cracking are more representative of atypical coalbed gases. Three Argonne Premium Coals (Upper-Freeport, Pittsburgh #8 and Lewiston-Stockton) were extracted with benzene in both Soxhlet and elevated pressure extraction (EPE) systems. The extracts were compared on the basis of dry mass yield and hydrocarbon profiles obtained by gas chromatography/mass spectrometry. The dry mass yields for the Upper-Freeport coal gave consistent results by both methods, while the yields from the Pittsburgh #8 and Lewiston-Stockton coals were greater by the EPE method. EPE required ˜90 vol. % less solvent compared to Soxhlet extraction. Single-ion-chromatograms of the Soxhlet extracts all exhibited bimodal distributions, while those of the EPE extracts did not. Hydrocarbons analyzed from Greater Green River Basin samples indicate that the natural oils in the basin originated from the coal seams. Analysis of artificially produced oil indicates that hydrous pyrolysis mimics generation of C15+ n-alkanes, but significant variations were found in the branched alkane, low-molecular-weight n-alkanes, and high-molecular-weight aromatic hydrocarbon distributions.

Optimisation of chromatographic resolution using objective functions including both time and spectral information.

Science.gov (United States)

Torres-Lapasió, J R; Pous-Torres, S; Ortiz-Bolsico, C; García-Alvarez-Coque, M C

2015-01-16

The optimisation of the resolution in high-performance liquid chromatography is traditionally performed attending only to the time information. However, even in the optimal conditions, some peak pairs may remain unresolved. Such incomplete resolution can be still accomplished by deconvolution, which can be carried out with more guarantees of success by including spectral information. In this work, two-way chromatographic objective functions (COFs) that incorporate both time and spectral information were tested, based on the peak purity (analyte peak fraction free of overlapping) and the multivariate selectivity (figure of merit derived from the net analyte signal) concepts. These COFs are sensitive to situations where the components that coelute in a mixture show some spectral differences. Therefore, they are useful to find out experimental conditions where the spectrochromatograms can be recovered by deconvolution. Two-way multivariate selectivity yielded the best performance and was applied to the separation using diode-array detection of a mixture of 25 phenolic compounds, which remained unresolved in the chromatographic order using linear and multi-linear gradients of acetonitrile-water. Peak deconvolution was carried out using the combination of orthogonal projection approach and alternating least squares. Copyright © 2014 Elsevier B.V. All rights reserved.

Application of Analytical Quality by Design concept for bilastine and its degradation impurities determination by hydrophilic interaction liquid chromatographic method.

Science.gov (United States)

Terzić, Jelena; Popović, Igor; Stajić, Ana; Tumpa, Anja; Jančić-Stojanović, Biljana

2016-06-05

This paper deals with the development of hydrophilic interaction liquid chromatographic (HILIC) method for the analysis of bilastine and its degradation impurities following Analytical Quality by Design approach. It is the first time that the method for bilastine and its impurities is proposed. The main objective was to identify the conditions where an adequate separation in minimal analysis duration could be achieved within a robust region. Critical process parameters which have the most influence on method performance were defined as acetonitrile content in the mobile phase, pH of the aqueous phase and ammonium acetate concentration in the aqueous phase. Box-Behnken design was applied for establishing a relationship between critical process parameters and critical quality attributes. The defined mathematical models and Monte Carlo simulations were used to identify the design space. Fractional factorial design was applied for experimental robustness testing and the method is validated to verify the adequacy of selected optimal conditions: the analytical column Luna(®) HILIC (100mm×4.6mm, 5μm particle size); mobile phase consisted of acetonitrile-aqueous phase (50mM ammonium acetate, pH adjusted to 5.3 with glacial acetic acid) (90.5:9.5, v/v); column temperature 30°C, mobile phase flow rate 1mLmin(-1), wavelength of detection 275nm. Copyright © 2016 Elsevier B.V. All rights reserved.

Quantitative determination of 14C(-)-epicatechin and 14C-rutin on the Uncaria plant by a two-step heterogeneous thin-layer chromatographic-liquid scintillation counting procedure

International Nuclear Information System (INIS)

Das, N.P.; Law, K.H.

1987-01-01

A simple, rapid, precise and relatively inexpensive thin-layer chromatographic method coupled to heterogeneous liquid scintillation counting procedure was used for the quantitation of radioactivity of biologically synthesized ( 14 C) flavonoids and other phenolic plant constituents. The two flavonoids, namely ( 14 C) rutin and ( 14 C) (-) -epicatechin, extracted from the plant Uncaria elliptica Roxb were separated on plastic thin-layer plates coated with silica gel using the two solvent systems : acetonitrile-acetic acid-water (8.5:0.5:1.5) and ethyl acetate-acetic acid-water (3:1:3). The respective spots on the plates that corresponded to the two flavonoids were cut out and eluted with 3 ml aliquots of methanol followed by direct addition of scintillation flour. This method gave 99 +- 2 per cent of the total count indicating the excellent elution procedure. The results were reproducible and showed linearity over the range of 0 - 35000 dpm. The elution efficiency by several other organic solvents were also investigated. (author). 19 refs., 4 tables

Hydrogenation of rapeseed oil for production of liquid bio-chemicals

International Nuclear Information System (INIS)

Pinto, F.; Martins, S.; Gonçalves, M.; Costa, P.; Gulyurtlu, I.; Alves, A.; Mendes, B.

2013-01-01

Highlights: ► Production of renewable liquid hydrocarbons through rapeseed oil hydrogenation. ► Hydrogenation at lower temperature and lower hydrogen pressures. ► Test of a catalyst commonly employed in petrochemical industry. ► Improve of hydrogenation process viability by decreasing operational costs. ► Analysis of hydrogenated product applications as bio-chemicals. -- Abstract: The main objective of rapeseed oil hydrogenation tests was the production of liquid bio-chemicals to be used as renewable raw material for the production of several chemicals and in chemical synthesis to substitute petroleum derived stuff. As, hydrogenation of vegetable oils is already applied for the production of biofuels, the work done focused in producing aromatic compounds, due to their economic value. The effect of experimental conditions on rapeseed oil hydrogenation was studied, namely, reaction temperature and time with the aim of selecting the most favourable conditions to convert rapeseed oil into liquid valuable bio-chemicals. Rapeseed oil was hydrogenated at a hydrogen initial pressure of 1.10 MPa. Reaction temperature varied in the range from 200 °C to 400 °C, while reaction times between 6 and 180 min were tested. The performance of a commercial cobalt and molybdenum catalyst was also studied. The highest hydrocarbons yields were obtained at the highest temperature and reaction times tested. At a temperature of 400 °C and at the reaction time of 120 min hydrocarbons yield was about 92% in catalyst presence, while in the absence of the catalyst this value decreased to 85%. Hydrocarbons yield was even higher when the reaction time of 180 min was used in the presence of catalyst, as the yield of 97% was observed. At these conditions hydrocarbons formed had a high content of aromatic compounds, around 50%. For this reason, the viscosity values of hydrogenated oils were lower than that established by EN590, which together with hydrogenated liquids composition

Reduction of silanophilic interactions in liquid chromatography with the use of ionic liquids

Energy Technology Data Exchange (ETDEWEB)

MarszaII, MichaI Piotr [Department of Biopharmaceutics and Pharmacodynamics, Medical University of Gdansk, Gen. J. Hallera 107, 80-416 Gdansk (Poland); Baczek, Tomasz [Department of Biopharmaceutics and Pharmacodynamics, Medical University of Gdansk, Gen. J. Hallera 107, 80-416 Gdansk (Poland); Kaliszan, Roman [Department of Biopharmaceutics and Pharmacodynamics, Medical University of Gdansk, Gen. J. Hallera 107, 80-416 Gdansk (Poland)]. E-mail: roman.kaliszan@amg.gda.pl

2005-08-22

A suppression of silanophilic interactions by the selected ionic liquids added to the mobile phase in thin-layer chromatography (TLC) and high-performance liquid chromatography (HPLC) is reported. Acetonitrile was used as the eluent, alone or with various concentrations of water and phosphoric buffer pH 3. Selectivity of the normal (NP) and the reversed (RP) stationary phase material was examined using a series of proton-acceptor basic drugs analytes. The ionic liquids studied appeared to significantly affect analyte retention in NP-TLC, RP-TLC and RP-HPLC systems tested. Consequently, the increased separation selectivity was attained. Due to ionic liquid additives to eluent even analytes could be chromatographed, which were not eluted from the silica-based stationary phase materials with 100% of acetonitrile in the mobile phase. Addition of ionic liquid already in very small concentration (0.5%, v/v) could reduce the amount of acetonitrile used during the optimization of basic analytes separations in TLC and HPLC systems. Moreover, the influence of temperature on the separation of basic analytes was demonstrated and considered in practical HPLC method development.

Reduction of silanophilic interactions in liquid chromatography with the use of ionic liquids

International Nuclear Information System (INIS)

MarszaII, MichaI Piotr; Baczek, Tomasz; Kaliszan, Roman

2005-01-01

A suppression of silanophilic interactions by the selected ionic liquids added to the mobile phase in thin-layer chromatography (TLC) and high-performance liquid chromatography (HPLC) is reported. Acetonitrile was used as the eluent, alone or with various concentrations of water and phosphoric buffer pH 3. Selectivity of the normal (NP) and the reversed (RP) stationary phase material was examined using a series of proton-acceptor basic drugs analytes. The ionic liquids studied appeared to significantly affect analyte retention in NP-TLC, RP-TLC and RP-HPLC systems tested. Consequently, the increased separation selectivity was attained. Due to ionic liquid additives to eluent even analytes could be chromatographed, which were not eluted from the silica-based stationary phase materials with 100% of acetonitrile in the mobile phase. Addition of ionic liquid already in very small concentration (0.5%, v/v) could reduce the amount of acetonitrile used during the optimization of basic analytes separations in TLC and HPLC systems. Moreover, the influence of temperature on the separation of basic analytes was demonstrated and considered in practical HPLC method development

Chemometric approach for development, optimization, and validation of different chromatographic methods for separation of opium alkaloids.

Science.gov (United States)

Acevska, J; Stefkov, G; Petkovska, R; Kulevanova, S; Dimitrovska, A

2012-05-01

The excessive and continuously growing interest in the simultaneous determination of poppy alkaloids imposes the development and optimization of convenient high-throughput methods for the assessment of the qualitative and quantitative profile of alkaloids in poppy straw. Systematic optimization of two chromatographic methods (gas chromatography (GC)/flame ionization detector (FID)/mass spectrometry (MS) and reversed-phase (RP)-high-performance liquid chromatography (HPLC)/diode array detector (DAD)) for the separation of alkaloids from Papaver somniferum L. (Papaveraceae) was carried out. The effects of various conditions on the predefined chromatographic descriptors were investigated using chemometrics. A full factorial linear design of experiments for determining the relationship between chromatographic conditions and the retention behavior of the analytes was used. Central composite circumscribed design was utilized for the final method optimization. By conducting the optimization of the methods in very rational manner, a great deal of excessive and unproductive laboratory research work was avoided. The developed chromatographic methods were validated and compared in line with the resolving power, sensitivity, accuracy, speed, cost, ecological aspects, and compatibility with the poppy straw extraction procedure. The separation of the opium alkaloids using the GC/FID/MS method was achieved within 10 min, avoiding any derivatization step. This method has a stronger resolving power, shorter analysis time, better cost/effectiveness factor than the RP-HPLC/DAD method and is in line with the "green trend" of the analysis. The RP-HPLC/DAD method on the other hand displayed better sensitivity for all tested alkaloids. The proposed methods provide both fast screening and an accurate content assessment of the six alkaloids in the poppy samples obtained from the selection program of Papaver strains.

Bioavailability enhanced rhizosphere remediation of petroleum hydrocarbon contaminated soil

International Nuclear Information System (INIS)

Marchenko, A.; Vorobyov, A.; Zharikov, G.; Ermolenko, Z.; Dyadishchev, N.; Borovick, R.; Sokolov, M.; Ortega-Calvo, J.J.

2005-01-01

Aliphatic, aromatic and polycyclic aromatic oil hydrocarbons are structurally complicated man-caused pollutants that are constantly brought into biosphere. Oil production in Russia, so as all over the world, is connected with pollution of biotopes, ecosystems and agro-landscapes. Presently large funds are allocated either for oil leak prevention or for discharged oil gathering. At the same time, in spite of large necessity in technologies for efficient reconstruction of soil bio-productivity, reliable regional systems of their remediation in situ have not been developed yet. One such method is rhizosphere remediation, a biotechnology, based on the functioning of plant-microbial complexes. Little is known about bioavailability in phyto-remediation systems. Specific bioavailability-promoting mechanisms, operating in soil with hydrocarbon-degrading populations, may be responsible for increased rates of pollutant transformation (increased bacterial adherence to the pollutants, production of bio-surfactants by bacteria or by plants, possible role of chemotaxis). In the course of work collection of 42 chemo-tactically active bio-surfactant producing strain-degraders of petroleum hydrocarbons including polycyclic aromatic hydrocarbons (PAHs) was created. Two representative strains were selected for detailed chemotaxis studies with PAHs (naphthalene, phenanthrene, anthracene, and pyrene), bacterial lipopolysaccharide and root exudates from seven different plants. These strains are produce the bio-surfactants (rhamno-lipid). The chemotactic response was quantified with a capillary and densitometric chemotaxis assay. Surface tension of cultural liquid was measured after cultivation of strains in the presence of hexadecane or phenanthrene with the use of a ring tensiometer. Before measuring of surface tension microbial cells were collected from liquid culture by centrifugation. Total petroleum Hydrocarbons (TPH) in soil were analyzed by infra-red spectroscopy method. PAHs

Bioavailability enhanced rhizosphere remediation of petroleum hydrocarbon contaminated soil

Energy Technology Data Exchange (ETDEWEB)

Marchenko, A.; Vorobyov, A.; Zharikov, G.; Ermolenko, Z.; Dyadishchev, N.; Borovick, R.; Sokolov, M. [Research Centre for Toxicology and Hygienic Regulation of Biopreparations, Moscow region (Russian Federation); Ortega-Calvo, J.J. [Instituto de Recursos Naturales y Agrobiologia, CSIC, Sevilla (Spain)

2005-07-01

Aliphatic, aromatic and polycyclic aromatic oil hydrocarbons are structurally complicated man-caused pollutants that are constantly brought into biosphere. Oil production in Russia, so as all over the world, is connected with pollution of biotopes, ecosystems and agro-landscapes. Presently large funds are allocated either for oil leak prevention or for discharged oil gathering. At the same time, in spite of large necessity in technologies for efficient reconstruction of soil bio-productivity, reliable regional systems of their remediation in situ have not been developed yet. One such method is rhizosphere remediation, a biotechnology, based on the functioning of plant-microbial complexes. Little is known about bioavailability in phyto-remediation systems. Specific bioavailability-promoting mechanisms, operating in soil with hydrocarbon-degrading populations, may be responsible for increased rates of pollutant transformation (increased bacterial adherence to the pollutants, production of bio-surfactants by bacteria or by plants, possible role of chemotaxis). In the course of work collection of 42 chemo-tactically active bio-surfactant producing strain-degraders of petroleum hydrocarbons including polycyclic aromatic hydrocarbons (PAHs) was created. Two representative strains were selected for detailed chemotaxis studies with PAHs (naphthalene, phenanthrene, anthracene, and pyrene), bacterial lipopolysaccharide and root exudates from seven different plants. These strains are produce the bio-surfactants (rhamno-lipid). The chemotactic response was quantified with a capillary and densitometric chemotaxis assay. Surface tension of cultural liquid was measured after cultivation of strains in the presence of hexadecane or phenanthrene with the use of a ring tensiometer. Before measuring of surface tension microbial cells were collected from liquid culture by centrifugation. Total petroleum Hydrocarbons (TPH) in soil were analyzed by infra-red spectroscopy method. PAHs

Hydrocarbons and fuels analyses with the supersonic gas chromatography mass spectrometry--the novel concept of isomer abundance analysis.

Science.gov (United States)

Fialkov, Alexander B; Gordin, Alexander; Amirav, Aviv

2008-06-27

Hydrocarbon analysis with standard GC-MS is confronted by the limited range of volatile compounds amenable for analysis and by the similarity of electron ionization mass spectra for many compounds which show weak or no molecular ions for heavy hydrocarbons. The use of GC-MS with supersonic molecular beams (Supersonic GC-MS) significantly extends the range of heavy hydrocarbons that can be analyzed, and provides trustworthy enhanced molecular ion to all hydrocarbons. In addition, unique isomer mass spectral features are obtained in the ionization of vibrationally cold hydrocarbons. The availability of molecular ions for all hydrocarbons results in the ability to obtain unique chromatographic isomer distribution patterns that can serve as a new method for fuel characterization and identification. Examples of the applicability and use of this novel isomer abundance analysis (IAA) method to diesel fuel, kerosene and oil analyses are shown. It is suggested that in similarity to the "three ions method" for identification purposes, three isomer abundance patterns can serve for fuel characterization. The applications of the Supersonic GC-MS for engine motor oil analysis and transformer oil analysis are also demonstrated and discussed, including the capability to achieve fast 1-2s sampling without separation for oil and fuel fingerprinting. The relatively fast analysis of biodiesel is described, demonstrating the provision of molecular ions to heavy triglycerides. Isomer abundance analysis with the Supersonic GC-MS could find broad range of applications including petrochemicals and fuel analysis, arson analysis, environmental oil/fuel spill analysis, fuel adulteration analysis and motor oil analysis.