Randomized Comparison of Two Vaginal Self-Sampling Methods for Human Papillomavirus Detection: Dry Swab versus FTA Cartridge.

Directory of Open Access Journals (Sweden)

Rosa Catarino

Full Text Available Human papillomavirus (HPV self-sampling (self-HPV is valuable in cervical cancer screening. HPV testing is usually performed on physician-collected cervical smears stored in liquid-based medium. Dry filters and swabs are an alternative. We evaluated the adequacy of self-HPV using two dry storage and transport devices, the FTA cartridge and swab.A total of 130 women performed two consecutive self-HPV samples. Randomization determined which of the two tests was performed first: self-HPV using dry swabs (s-DRY or vaginal specimen collection using a cytobrush applied to an FTA cartridge (s-FTA. After self-HPV, a physician collected a cervical sample using liquid-based medium (Dr-WET. HPV types were identified by real-time PCR. Agreement between collection methods was measured using the kappa statistic.HPV prevalence for high-risk types was 62.3% (95%CI: 53.7-70.2 detected by s-DRY, 56.2% (95%CI: 47.6-64.4 by Dr-WET, and 54.6% (95%CI: 46.1-62.9 by s-FTA. There was overall agreement of 70.8% between s-FTA and s-DRY samples (kappa = 0.34, and of 82.3% between self-HPV and Dr-WET samples (kappa = 0.56. Detection sensitivities for low-grade squamous intraepithelial lesion or worse (LSIL+ were: 64.0% (95%CI: 44.5-79.8 for s-FTA, 84.6% (95%CI: 66.5-93.9 for s-DRY, and 76.9% (95%CI: 58.0-89.0 for Dr-WET. The preferred self-collection method among patients was s-DRY (40.8% vs. 15.4%. Regarding costs, FTA card was five times more expensive than the swab (~5 US dollars (USD/per card vs. ~1 USD/per swab.Self-HPV using dry swabs is sensitive for detecting LSIL+ and less expensive than s-FTA.International Standard Randomized Controlled Trial Number (ISRCTN: 43310942.

StorageTek T10000 Data Cartridge

CERN Multimedia

This data cartridge works on several StorageTek systems. The goal is to provide cartridge compatibility across several system. It has been designed for space saving and ultra-high capacity tape. It permit to fulfill high-volume backup, archiving, and disaster recovery.

Comparison of the Usefulness of SPE Cartridges for the Determination of β-Blockers and β-Agonists (Basic Drugs in Environmental Aqueous Samples

Directory of Open Access Journals (Sweden)

Magda Caban

2015-01-01

Full Text Available Even though the methodology used for the determination of β-blockers and β-agonists in environmental samples is based mainly on solid-phase extraction (SPE and gas chromatography or liquid chromatography with mass spectrometric detection, the available literature data on the applied SPE procedures is rather sparse. In this paper such comparison is presented. Moreover, the usefulness of the eight SPE cartridges for the determination of five β-blockers (acebutolol, atenolol, metoprolol, nadolol, and propranolol and two β-agonists (salbutamol and terbutaline in environmental aqueous samples using GC techniques is tested. Among them, three (the trifunction sorbent Strata Screen C, the copolymers LiChrolut EN, and the functionalized copolymer Isolute ENV+ were used for the first time for this purpose. It was confirmed that polystyrene-divinylbenzene-N-vinylpyrrolidone copolymers (PS-DVB-VP, Strata-X, and Oasis HLB cartridges have a better potential than a cation-exchange sorbent for the extraction of the target drugs from environmental water samples. However, it should be stressed out that the direct application of the tested SPE conditions for the analysis of real environmental water samples is not possible, and such parameters, like volume of loading sample, appropriate solvents for washing and elution steps, and so forth, must be optimized again in order to achieve satisfactory recovery values for the target compounds.

Development of the reactor lithium ampoule device for research of spectral-luminescent characteristics of nuclear-excited plasma

Energy Technology Data Exchange (ETDEWEB)

Batyrbekov, E.G. [National Nuclear Center of RK, Kurchatov (Kazakhstan); Gordienko, Yu. N., E-mail: gordienko@nnc.kz [National Nuclear Center of RK, Kurchatov (Kazakhstan); Ponkratov, Yu. V. [National Nuclear Center of RK, Kurchatov (Kazakhstan); Khasenov, M.U. [PI “National Laboratory Astana”, Astana (Kazakhstan); Tazhibayeva, I.L.; Barsukov, N.I.; Kulsartov, T.V.; Zaurbekova, Zh. A.; Tulubayev, Ye. Yu.; Skakov, M.K. [National Nuclear Center of RK, Kurchatov (Kazakhstan)

2017-04-15

Highlights: • The development procedure of the ampoule device for experiments with nuclear-excited plasma under neutron irradiation is described. • The methods of nuclear reactions’ energy conversion into the energy of optical radiation of nuclear-excited plasma are presented. • A scheme of reactor experiments, the experimental facility and experimental device to carry out the reactor experiments are considered. - Abstract: This paper describes the development procedure of the reactor ampoule device to perform the experiments on study of spectral luminescence characteristics of nuclear-excited plasma formed by products of {sup 6}Li(n,α){sup 3}H reaction under neutron irradiation at the IVG.1 M research reactor. The methods of nuclear reactions’ energy conversion into the energy of optical radiation of nuclear-excited plasma are presented. A scheme of reactor experiments, the experimental facility and experimental device to carry out the reactor experiments are considered in paper. The designed ampoule device is totally meets the requirements of irradiation experiments on the IVG.1M reactor.

IBM 3480 tape cartridge

CERN Multimedia

1984-01-01

The 3480 tape format is a magnetic tape data storage format developed by IBM. The cartridge contains a single reel. IBM’s 3480 cartridge tape system sought to replace the traditional reels of magnetic tape in the computer center. Because of their speed, reliability, durability and low media cost, these tapes and tape drives are still in high demand. A hallmark of the genre is transferability. Tapes recorded with one tape drive are generally readable on another drive, even if the tape drives were built by different manufacturers.

Molecularly imprinted polymer cartridges coupled on-line with high performance liquid chromatography for simple and rapid analysis of dextromethorphan in human plasma samples.

Science.gov (United States)

Moein, Mohammad Mahdi; Javanbakht, Mehran; Akbari-Adergani, Behrouz

2011-04-01

In this paper, a novel method is described for automated determination of dextromethorphan in biological fluids using molecularly imprinted solid-phase extraction (MISPE) as a sample clean-up technique combined with high performance liquid chromatography (HPLC). The water-compatible molecularly imprinted polymers (MIPs) were prepared using methacrylic acid as functional monomer, ethylene glycol dimethacrylate as cross-linker, chloroform as porogen and dextromethorphan as template molecule. These imprinted polymers were used as solid-phase extraction sorbent for the extraction of dextromethorphan from human plasma samples. Various parameters affecting the extraction efficiency of the MIP cartridges were evaluated. The high selectivity of the sorbent coupled to the high performance liquid chromatographic system permitted a simple and rapid analysis of this drug in plasma samples with limits of detection (LOD) and quantification (LOQ) of 0.12 ng/mL and 0.35 ng/mL, respectively. The MIP selectivity was evaluated by analyzing of the dextromethorphan in presence of several substances with similar molecular structures and properties. Results from the HPLC analyses showed that the recoveries of dextromethorphan using MIP cartridges from human plasma samples in the range of 1-50 ng/mL were higher than 87%. Copyright © 2011 Elsevier B.V. All rights reserved.

The Isonzo front in the First World War: glass ampoules found in the vicinity of the village Kred.

Science.gov (United States)

Krbavcic, Ales

2015-01-01

To identify the contents of ampoules stored items at the WW I Kobarid Museum, Slovenia. Sources and methods: Analysis of ampoules from the Kobarid Museum using pharmacopoeial methods. The contents of the unlabelled ampoules were identified as calcium hypochlorite, a decontaminant for mustard gas (Yperite). The Isonzo front/Soška fronta was opened on May 24 1915 by the Kingdom of Italy according to a secret London Treaty. In exchange for the opening of this front, the Kingdom of Italy would be granted large tracts of territory in the wesster provinces of the Austro-Hungarian Empire and along the Adriatic coast. The ensuing trench-warfare during the eleven Isonzo battles ended with the 12th battle known as the Kobarid/Karfeit/Caporetto break-thru in October 1917. The joint German and Austro-Hungarian forces waged a massive gas-attack with dichloroarsine and phosgene, which was later disclosed as the horrifying overture to the general disordered retreat of the Italian troops to Piave. The possibility of a chemical attack was underestimated by the Italian high command as shown by the ineffective gas-masks issued to the troops. Hovewer, a recent find of ampoules with calcium hypochlorite at the village of Kred, now exhibited at the Kobarid WWI Museum, leads to the conclusion that the Italian IVth army's command, located in Kred, considered decontamination measures against Yperite necessary.

Do insulin cartridges really provide a lower risk of potential diabetes complications than traditional vials?

Science.gov (United States)

Al-Sharayri, Mohammad G; Aljbori, Tariq M; Migdadi, Qusai M; Al-Omoush, Marwa B; Jaarah, Ayman R

2014-09-01

Recently, many publicly funded healthcare organizations suffered from an economical crisis. This forced some organizations to utilize less costly alternatives where possible. Insulin cartridges and vials are examples. Many patients are questioning the difference between the two alternatives as they contain the same active ingredient. To find out if insulin cartridges really provide a lower risk of potential diabetes complications than traditional vials. A questionnaire was used to ask two random samples of diabetic patients about the development of some diabetes complications. The first sample (n = 41) consisted of patients using cartridges; the second sample (n = 40) consisted of patients using vials. Patients were randomly selected from the endocrine clinic and the out-patient pharmacy in Al-Hussein Hospital in King Hussein Medical Center in Amman- Jordan. 44% of respondents in the first sample did not suffer from any complication; on the other hand, the percentage was only 15% of respondents in the second sample. All respondents (100%) in the first sample suffered from only 2 complications or less; however, 25% of the respondents in the second sample suffered from 3 or more complications. Nephropathy complications, were slightly higher in the first sample; 22% compared to 15% in the second sample. On the other hand, all complications reported in the second sample were higher; 30% for neuropathy, 65% for retinopathy complications and 42.5% for extremities damage compared to only 9.7%, 7.3% and 26.8% respectively in the first sample. In general, respondents who were using cartridges reported a lesser incidence of diabetes complications. Although many organizations suffered from an economical crisis, the cost-effectiveness aspect should be taken into consideration when purchasing medical alternatives. This will provide higher quality of life for patients and eventually lower hidden and future costs for the organizations.

Rapid and sensitive determination of phenylurea herbicides in water in the presence of their anilines by extraction with a Carbopack cartridge followed by liquid chromatography.

Science.gov (United States)

Di Corcia, A; Marchetti, M

1991-03-22

A rapid and sensitive method for determining phenylurea herbicides in environmental aqueous samples in the presence of their anilines is described. The water sample is preconcentrated by passage at a flow-rate of ca. 150 ml/min through a 250-mg graphitized carbon black (Carbopack B) cartridge. After washing with 0.6 ml of methanol, the Carbopack B trap is connected with a cartridge containing a strong cation exchanger. Organics trapped by the Carbopack cartridge are eluted by passage of 6 ml of methylene chloride-methanol (95:5, v/v). Anilines and other basic compounds are quantitatively subtracted from the solvent system while flowing through the cation-exchange cartridge. After evaporation and redissolution, the sample is subjected to reversed-phase gradient elution high-performance liquid chromatography with UV detection at 250 nm. Recoveries of phenylureas added to water at levels between 30 and 3000 ng/l were higher than 92%. The limit of detection was about 1 ng/l, for a 2-1 sample. With respect to an octadecyl (C18)-bonded silica cartridge, the Carbopack B cartridge had a far better extraction efficiency for polar phenylureas.

Viability tests of LIPI-MC mould collection in ampoule of L-drying preservation after one year of storage at 5ºC

Directory of Open Access Journals (Sweden)

MUHAMMAD ILYAS

2007-01-01

Full Text Available A study on viability test of several LIPI-MC mould isolates in ampoule of L-drying preservation after one year storage at 5º C had been conducted. In this study, cell survival level of 34 ampoules number from eight mould generas and 17 species had been counted. The objective of this study was to observe the survival or viability level of several mould isolates in ampoule L-drying preservation after one year storage at 5º C. The measurement of viability level was based on the average of colony forming unit density (CFU/ml. The result showed that there were seven mould isolates have hingh viabilitiy, 18 isolates have medium viabilitiy, two isolates have low viability, and five isolates have lost its viability.

Adsorbent cartridge for the exhaust of diazo process machines

International Nuclear Information System (INIS)

Michlin, N.; Thies, E.J.

1982-01-01

A disposable cartridge filled with a chemical composition that acts as an adsorbent for ammonia vapor is adapted to be used in connection with a diazo process printing machine having a vacuum exhausted chamber. Exhaust from the chamber is passed through the cartridge to remove the noxious ammonia vapors and then is vented into the atmosphere. The cartridge is housed in an elongated rectangular cardboard box having three end flaps formed at each of its opposed open ends. Two opposed flaps of each set are formed with central holes and a plastic screen section adhered between these flaps to retain and allow access to the center section of the box which contains the adsorbent chemical. The center end flaps have knock-outs or tear strips that allow holes to be formed in their centers. These center end flaps cover the screens during shipment and when the cartridge is ready for use the center sections of these end flaps are knocked-out to allow the machine exhaust to be vented into and out of the cartridge

RPA using a multiplexed cartridge for low cost point of care diagnostics in the field.

Science.gov (United States)

Ereku, Luck Tosan; Mackay, Ruth E; Craw, Pascal; Naveenathayalan, Angel; Stead, Thomas; Branavan, Manorharanehru; Balachandran, Wamadeva

2018-04-15

A point of care device utilising Lab-on-a-Chip technologies that is applicable for biological pathogens was designed, fabricated and tested showing sample in to answer out capabilities. The purpose of the design was to develop a cartridge with the capability to perform nucleic acid extraction and purification from a sample using a chitosan membrane at an acidic pH. Waste was stored within the cartridge with the use of sodium polyacrylate to solidify or gelate the sample in a single chamber. Nucleic acid elution was conducted using the RPA amplification reagents (alkaline pH). Passive valves were used to regulate the fluid flow and a multiplexer was designed to distribute the fluid into six microchambers for amplification reactions. Cartridges were produced using soft lithography of silicone from 3D printed moulds, bonded to glass substrates. The isothermal technique, RPA is employed for amplification. This paper shows the results from two separate experiments: the first using the RPA control nucleic acid, the second showing successful amplification from Chlamydia Trachomatis. Endpoint analysis conducted for the RPA analysis was gel electrophoresis that showed 143 base pair DNA was amplified successfully for positive samples whilst negative samples did not show amplification. End point analysis for Chlamydia Trachomatis samples was fluorescence detection that showed successful detection of 1 copy/μL and 10 copies/μL spiked in a MES buffer. Crown Copyright © 2018. Published by Elsevier Inc. All rights reserved.

Criticality safety evaluation report for K Basin filter cartridges

International Nuclear Information System (INIS)

Schwinkendorf, K.N.

1995-01-01

A criticality safety evaluation of the K Basin filter cartridge assemblies has been completed to support operations without a criticality alarm system. The results show that for normal operation, the filter cartridge assembly is far below the safety limit of k eff = 0.95, which is applied to plutonium systems at the Hanford Site. During normal operating conditions, uranium, plutonium, and fission and corrosion products in solution are continually accumulating in the available void spaces inside the filter cartridge medium. Currently, filter cartridge assemblies are scheduled to be replaced at six month intervals in KE Basin, and at one year intervals in KW Basin. According to available plutonium concentration data for KE Basin and data for the U/Pu ratio, it will take many times the six-month replacement time for sufficient fissionable material accumulation to take place to exceed the safety limit of k eff = 0.95, especially given the conservative assumption that the presence of fission and corrosion products is ignored. Accumulation of sludge with a composition typical of that measured in the sand filter backwash pit will not lead to a k eff = 0.95 value. For off-normal scenarios, it would require at least two unlikely, independent, and concurrent events to take place before the k eff = 0.95 limit was exceeded. Contingencies considered include failure to replace the filter cartridge assemblies at the scheduled time resulting in additional buildup of fissionable material, the loss of geometry control from the filter cartridge assembly breaking apart and releasing the individual filter cartridges into an optimal configuration, and concentrations of plutonium at U/Pu ratios less than measured data for KE Basin, typically close to 400 according to extensive measurements in the sand filter backwash pit and plutonium production information

StorageTek T10000 Tape Cartridge

CERN Multimedia

1985-01-01

Oracle StorageTek T10000T2 cartridge has total capacity of 5 TB. It is actually manufactured by Fuji Film, uses Barium Ferrite (BaFe) particles technology data store, but is also equipped with RFID chip. There is over 1 km of tape inside of the cartridge with 3584 data tracks and it supports over 25000 load/unload cycles. The archival life is estimated to be around 30 years and uncorrected bit error rate is 10-19. CERN however usually migrates data to newer technologies roughly every 5 years in order to keep the footprint under control.

Rapid, efficient and selective preconcentration of benzo[a]pyrene (BaP) by molecularly imprinted composite cartridge and HPLC

Energy Technology Data Exchange (ETDEWEB)

Çorman, Mehmet Emin, E-mail: mecorman@sinop.edu.tr [Hacettepe University, Department of Chemistry, Ankara (Turkey); Sinop University, Department of Bioengineering, Sinop (Turkey); Armutcu, Canan [Hacettepe University, Department of Chemistry, Ankara (Turkey); Uzun, Lokman, E-mail: lokman@hacettepe.edu.tr [Hacettepe University, Department of Chemistry, Ankara (Turkey); Denizli, Adil [Hacettepe University, Department of Chemistry, Ankara (Turkey)

2017-01-01

In this study, cryogel-based molecularly imprinted composite cartridges were designed for the rapid, efficient, and selective preconcentration of benzo[a]pyrene (BaP) from water samples. First, a BaP-imprinted poly(2-hydroxyethyl methacrylate-N-methacryloyl-(L)-phenylalanine) composite cartridge was synthesized under semi-frozen conditions and characterized by scanning electron microscopy, elemental analysis, Fourier transform infrared spectroscopy, and swelling tests. After the optimization of preconcentration parameters, i.e., pH and initial BaP concentration, the selectivity and preconcentration efficiency, and reusability of these cartridges were also evaluated. In selectivity experiments, BaP imprinted composite cartridge exhibited binding capacities 3.09, 9.52, 8.87, and 8.77-fold higher than that of the non-imprinted composite cartridge in the presence of competitors, such as benzo[b]fluoranthene (BbF), benzo[k]fluoranthene (BkF), indeno[1,2,3-cd]pyrene (IcdP), and 1-naphthol, respectively. The method detection limit (MDL), relative standard deviation (RSD) and preconcentration efficiency (PE) of the synthesized composite cartridge were calculated as 24.86 μg/L, 1.60%, and 349.6%, respectively. - Highlights: • Cryogel based molecularly imprinted composite cartridges as solid-phase extraction sorbents • Combination unique structural features of cryogels with MIP • An excellent ability to recognize the BaP molecule even if single-run contact • Rapid, efficient, selective and cost-friendly PAH preconcentration • Hydrophobic interactions via N-methacryloyl-(L)-phenylalanine.

Alterations in a Unique Class of Cortical Chandelier Cell Axon Cartridges in Schizophrenia.

Science.gov (United States)

Rocco, Brad R; DeDionisio, Adam M; Lewis, David A; Fish, Kenneth N

2017-07-01

The axons of chandelier cells (ChCs) target the axon initial segment of pyramidal neurons, forming an array of boutons termed a cartridge. In schizophrenia, the density of cartridges detectable by gamma-aminobutyric acid (GABA) membrane transporter 1 immunoreactivity is lower, whereas the density of axon initial segments detectable by immunoreactivity for the α2 subunit of the GABA A receptor is higher in layers 2/superficial 3 of the prefrontal cortex. These findings were interpreted as compensatory responses to lower GABA levels in ChCs. However, we recently found that in schizophrenia, ChC cartridge boutons contain normal levels of the 67 kDa isoform of glutamic acid decarboxylase (GAD67) protein, the enzyme responsible for GABA synthesis in these boutons. To understand these findings we quantified the densities of ChC cartridges immunoreactive for vesicular GABA transporter (vGAT+), which is present in all cartridge boutons, and the subset of cartridges that contain calbindin (CB+). Prefrontal cortex tissue sections from 20 matched pairs of schizophrenia and unaffected comparison subjects were immunolabeled for vGAT, GAD67, and CB. The mean density of vGAT+/CB+ cartridges was 2.7-fold higher, exclusively in layer 2 of schizophrenia subjects, whereas the density of vGAT+/CB- cartridges did not differ between subject groups. Neither vGAT, CB, or GAD67 protein levels per ChC bouton nor the number of boutons per cartridge differed between subject groups. Our findings of a greater density of CB+ ChC cartridges in prefrontal cortex layer 2 from schizophrenia subjects suggests that the normal developmental pruning of these cartridges is blunted in the illness. Copyright © 2016 Society of Biological Psychiatry. Published by Elsevier Inc. All rights reserved.

Comparative analysis of ampoules and vials in sterile and conventional packaging as to microbial load and sterility test.

Science.gov (United States)

Freitas, Raphael Ribeiro de Aquino; Tardelli, Maria Angela

2016-05-24

To compare sterility and microbial (bacteria and fungi) load in the outer part of hyperbaric bupivacaine (Neocaína®) in ampoule and bupivacaine in vial, in conventional and sterile pack formulations. The sterile packs were divided into two groups: G1 (n=16) with ampoules and G2 (n=16) with vials. Conventional formulations were divided into two groups, being G3 (n=16) with ampoules and G4 (n=16) with vials. The ampoules and vials were opened and had their content drawn. The empty bottles were then placed in sterile plastic bags and sent for analysis of microbial load (bacteria and fungi) and sterility testing. Data were analyzed using the χ2 test with Yates correction, and 95% confidence interval. G1 and G2 showed no bacterial growth when compared to conventional groups (pgrupos, sendo que o G1 (n=16) continha as ampolas e o G2 (n=16), os frascos-ampola. As apresentações convencionais foram distribuídas em dois grupos, a saber G3 (n=16) com as ampolas e G4 (n=16) com os frascos-ampola. As ampolas e os frascos-ampolas eram abertos e tinham seu conteúdo aspirado. Os frascos vazios eram, então, acondicionados em sacos plásticos estéreis e enviados para análise quanto à carga microbiana (bactérias e fungos), bem como para o teste de esterilidade. Os dados foram analisados por meio do teste χ2 com correção Yates com intervalo de confiança de 95%. Os grupos G1 e G2 não apresentaram crescimento bacteriano quando comparado aos grupos convencionais (pgrupos. O uso de embalagens estéreis (sterile pack) diminui a carga microbiana dos frascos de envasamentos, o que diminuiria a chance de exposição a uma potencial contaminação da solução anestésica.

Thermal analysis with expendable cartridge

International Nuclear Information System (INIS)

Susaki, K.; Landgraf, F.J.G.

1981-01-01

The pratical method of thermal analysis with expendable cartridge and some aspects of its use are presented. The results of the method applied to the system Nb-Mn are presented together with data from microprobe. (Author) [pt

Evaluation and comparison of a national made dental cartridge with two foreign made

Directory of Open Access Journals (Sweden)

Mahmood Hashemi H

2006-06-01

Full Text Available Background and Aim: Several factories produce dental cartridge in the world. In Iran, Daroupakhsh company is responsible for this task. The aim of this study was evaluate some properties of daroupakhsh cartridge and compare them with two imported ones: Ecocaine (made in Italy and Septodont (made in France. Materials and Methods: In this experimental study, 70 healthy patients from maxillofacial clinic of Shariaty hospital were selected. After obtaining informed consent, 0.1 cc of each carpule was injected to the patients' frontal region and the extent of anesthesia was measured at different time intervals. Also the quality of injections was evaluated by 11 surgeons. The dimensions of the three cartridges were also measured and compared together. Data were analyzed by repeated measure ANOVA and Friedman with p<0.05 as the limit of significance. Results: There was no significant difference in extent and duration of anesthesia among the studied cartridges. Surgeons were equally satisfied of all three kinds of cartridges. All of the cartridges were aspirable. Conclusion: Based on the results of this study, the three studied cartridges had similar properties.

42 CFR 84.194 - Filters used with chemical cartridges; location; replacement.

Science.gov (United States)

2010-10-01

...; replacement. 84.194 Section 84.194 Public Health PUBLIC HEALTH SERVICE, DEPARTMENT OF HEALTH AND HUMAN...; replacement. (a) Particulate matter filters used in conjunction with a chemical cartridge shall be located on... replacement on the cartridge. ...

Hazard classification test of the cartridge, 120-mm, APFSDS-T, XM829

Energy Technology Data Exchange (ETDEWEB)

Hooker, C.D.; Hadlock, D.E.; Mishima, J.; Gilchrist, R.L.

1983-11-01

Research was conducted to determine the behavior of the ammunition XM829 when subjected to detonation of an adjacent XM829 cartridge, and a sustained hot fire. It was concluded that the functioning of an XM829 cartridge, in one shipping container, will not cause immediate functioning of XM829 cartridges in adjacent containers. However, if a fire results and is sustained, adjacent cartridges may ignite, resulting in some scattering of debris within a maximum radius of 40 feet. Further, the XM829 cartridge can be expected to remain in a kinetic controlled regime with vigorous oxidation occurring early in such a fire but dropping off as the temperature cools toward ambient. Mass balance analyses data indicated a recovery of at least 80% in the 1982 external heat; in the 1983 test, the recovery percentage was improved to approximately 100% of the original depleted uranium weight volume. Therefore, it may be concluded that a significant airborne release of the depleted uranium material did not occur.

Methods of viscosity measurements in sealed ampoules

Science.gov (United States)

Mazuruk, Konstantin

1999-07-01

Viscosity of semiconductors and metallic melts is usually measured by oscillating cup method. This method utilizes the melts contained in vacuum sealed silica ampoules, thus the problems related to volatility, contamination, and high temperature and pressure can be alleviate. In a typical design, the time required for a single measurement is of the order of one hour. In order to reduce this time to a minute range, a high resolution angular detection system is implemented in our design of the viscometer. Furthermore, an electromagnet generating a rotational magnetic field (RMF) is incorporated into the apparatus. This magnetic field can be used to remotely and nonintrusively measure the electrical conductivity of the melt. It can also be used to induce a well controlled rotational flow in the system. The transient behavior of this flow can potentially yield of the fluid. Based on RMF implementation, two novel viscometry methods are proposed in this work: a) the transient torque method, b) the resonance method. A unified theoretical approach to the three methods is presented along with the initial test result of the constructed apparatus. Advantages of each of the method are discussed.

Development of technology of handling with ampoule source of ionizing radiation

International Nuclear Information System (INIS)

Urenskij, N.A.; Boltovskij, S.A.; Ganzha, V.V.; Shuklin, G.S.

2000-01-01

It is reported that in Kazakhstan at different enterprises there are more than 80,000 ampoule source of ionizing radiation (ASIR) and about 20,000 of them should be disposed. In 1995 the first phase of depository for spent ASIR was putted into operation. The depository is placed on 'Baikal-1' stand complex. The first phase of depository consists of following buildings and equipment: 2 special equipped motorcar; temporary depository; special washing machine; radiation protected chamber, intermediate depository; lift crane with set of special grips; protective container; jackets; cassette-holders; constant depository. Design of the depository, its equipment, system of dosimetric control and qualified personnel provide the security of operation and exclude the environment contamination

The Imation 9840 Tape Cartridge

CERN Multimedia

It’s a 20 GB uncompressed center-load cartridge used in StorageTek T9840 tape drives. The tape is a Metal Particle (MP) tape suitable for use on all Oracle/Sun/StorageTek 9840 A, B, C and D drives. The 9840 tape has an archival life of 15-30 years.

Nanoparticle separation with a miniaturized asymmetrical flow field-flow fractionation cartridge

Science.gov (United States)

Müller, David; Cattaneo, Stefano; Meier, Florian; Welz, Roland; deMello, Andrew

2015-07-01

Asymmetrical Flow Field-Flow Fractionation (AF4) is a separation technique applicable to particles over a wide size range. Despite the many advantages of AF4, its adoption in routine particle analysis is somewhat limited by the large footprint of currently available separation cartridges, extended analysis times and significant solvent consumption. To address these issues, we describe the fabrication and characterization of miniaturized AF4 cartridges. Key features of the scale-down platform include simplified cartridge and reagent handling, reduced analysis costs and higher throughput capacities. The separation performance of the miniaturized cartridge is assessed using certified gold and silver nanoparticle standards. Analysis of gold nanoparticle populations indicates shorter analysis times and increased sensitivity compared to conventional AF4 separation schemes. Moreover, nanoparticulate titanium dioxide populations exhibiting broad size distributions are analyzed in a rapid and efficient manner. Finally, the repeatability and reproducibility of the miniaturized platform are investigated with respect to analysis time and separation efficiency.

Combining cationic and anionic mixed-mode sorbents in a single cartridge to extract basic and acidic pharmaceuticals simultaneously from environmental waters.

Science.gov (United States)

Salas, Daniela; Borrull, Francesc; Fontanals, Núria; Marcé, Rosa Maria

2018-01-01

The aim of the present study is to broaden the applications of mixed-mode ion-exchange solid-phase extraction sorbents to extract both basic and acidic compounds simultaneously by combining the sorbents in a single cartridge and developing a simplified extraction procedure. Four different cartridges containing negative and positive charges in the same configuration were evaluated and compared to extract a group of basic, neutral, and acidic pharmaceuticals selected as model compounds. After a thorough optimization of the extraction conditions, the four different cartridges showed to be capable of retaining basic and acidic pharmaceuticals simultaneously through ionic interactions, allowing the introduction of a washing step with 15 mL methanol to eliminate interferences retained by hydrophobic interactions. Using the best combined cartridge, a method was developed, validated, and further applied to environmental waters to demonstrate that the method is promising for the extraction of basic and acidic compounds from very complex samples.

Agreement for HPV genotyping detection between self-collected specimens on a FTA cartridge and clinician-collected specimens

Science.gov (United States)

Guan, YaoYao; Gravitt, Patti E.; Howard, Roslyn; Eby, Yolanda J.; Wang, Shaoming; Li, Belinda; Feng, Changyan; Qiao, You-Lin; Castle, Philip E.

2016-01-01

The current method of transporting self-collected cervicovaginal specimen for HPV DNA testing relies on liquid based medium, which is challenging and expensive to transport. A novel, dry storage and transportation device, Whatman indicating FTA™ Elute Cartridge, avoids some of the pitfalls of liquid-based medium. This method has been shown to be comparable to liquid-based collection medium, but relative performance of self-collected (SC) and clinician-collected (CC) samples onto FTA cards has not been reported. The objective of this study is to compare the analytic performance of self- and clinician-collected samples onto FTA cartridges for the detection of carcinogenic HPV using Linear Array. There was a 91% agreement, 69% positive agreement, and kappa of 0.75 between the clinician-collected and self-collected specimens for detection of any carcinogenic HPV genotype. When the HPV results were categorized hierarchically according to cervical cancer risk, there was no difference in the distribution of the HPV results for the clinician- and self-collected specimens (p = 0.7). This study concludes that FTA elute cartridge is a promising method of specimen transport for cervical cancer screening programs considering using self-collected specimen and HPV testing. Larger studies with clinical endpoints are now needed to assess the clinical performance. PMID:23370404

Inductively coupled plasma mass spectrometry study of the retention behavior of arsenic species on various solid phase extraction cartridges and its application in arsenic speciation

Energy Technology Data Exchange (ETDEWEB)

Yu Chunhai; Cai Qiantao E-mail: qtcai@cawt.sui.com.sg; Guo Zhongxian; Yang Zhaoguang; Khoo, Soo Beng

2003-07-18

Inductively coupled plasma mass spectrometry (ICP-MS) was used to investigate the retention behavior of arsenite, arsenate, monomethylarsonic acid (MMA), dimethylarsinic acid (DMA), arsenobetaine (AsB), arsenocholine (AsC), trimethylarsine oxide (TMAO) and tetramethylarsonium ion (TMAI) on various silica-based solid phase extraction (SPE) cartridges. A method for arsenic speciation is then developed on the basis of selective SPE separation of arsenic species and highly sensitive ICP-MS detection. Factors affecting the retention and elution of arsenic species were examined. Results showed that the retention of arsenic species depended on the chemical characteristics of arsenic species and the types of sorbent materials. Change of pH in the range of 2.0-9.0 did not show significant effects on the retention of DMA, AsB, AsC, TMAI and TMAO on an ethylbenzene sulfonic acid-based strong cation exchange (SCX-3) cartridge. pH also did not influence the retention of AsB, AsC, TMAI and TMAO on a mixed-mode (M-M) cartridge containing non-polar, strong cation exchange and strong anion exchange (SAX) functional groups. However, the retentions of As(V) and MMA on the SAX and the M-M cartridge changed with pH. As(V) and MMA were completely retained on the SAX cartridge and sequentially selectively eluted with 1.0 mol l{sup -1} acetic acid (for MMA). DMA, AsB, AsC, TMAI and TMAO were completely retained on the SCX-3 cartridge and sequentially selectively eluted with 1.0 mol l{sup -1} HNO{sub 3} (for DMA). As(V), MMA, AsB, AsC, TMAI and TMAO were completely retained on the M-M cartridge. As(III) was not retained on either cartridge and remained in solution. Arsenic species in solution and those eluted from the cartridges were subsequently determined by ICP-MS. A detection limit of 8 ng l{sup -1} arsenic in water sample was obtained. This method was successfully applied to arsenic speciation in various sources of water samples (drinking water, waste water, raw water, etc.) and US

42 CFR 84.1155 - Filters used with canisters and cartridges; location; replacement.

Science.gov (United States)

2010-10-01

...; location; replacement. 84.1155 Section 84.1155 Public Health PUBLIC HEALTH SERVICE, DEPARTMENT OF HEALTH... Efficiency Respirators and Combination Gas Masks § 84.1155 Filters used with canisters and cartridges; location; replacement. (a) Particulate matter filters used in conjunction with a canister or cartridge...

Agreement for HPV genotyping detection between self-collected specimens on a FTA cartridge and clinician-collected specimens.

Science.gov (United States)

Guan, Yaoyao; Gravitt, Patti E; Howard, Roslyn; Eby, Yolanda J; Wang, Shaoming; Li, Belinda; Feng, Changyan; Qiao, You-Lin; Castle, Philip E

2013-04-01

The current method of transporting self-collected cervicovaginal specimen for HPV DNA testing relies on liquid based medium, which is challenging and expensive to transport. A novel, dry storage and transportation device, Whatman indicating FTA™ Elute Cartridge, avoids some of the pitfalls of liquid-based medium. This method has been shown to be comparable to liquid-based collection medium, but relative performance of self-collected (SC) and clinician-collected (CC) samples onto FTA cards has not been reported. The objective of this study is to compare the analytic performance of self- and clinician-collected samples onto FTA cartridges for the detection of carcinogenic HPV using Linear Array. There was a 91% agreement, 69% positive agreement, and kappa of 0.75 between the clinician-collected and self-collected specimens for detection of any carcinogenic HPV genotype. When the HPV results were categorized hierarchically according to cervical cancer risk, there was no difference in the distribution of the HPV results for the clinician- and self-collected specimens (p=0.7). This study concludes that FTA elute cartridge is a promising method of specimen transport for cervical cancer screening programs considering using self-collected specimen and HPV testing. Larger studies with clinical endpoints are now needed to assess the clinical performance. Copyright © 2012 Elsevier B.V. All rights reserved.

Clinical evaluation of high-risk HPV detection on self-samples using the indicating FTA-elute solid-carrier cartridge.

Science.gov (United States)

Geraets, D T; van Baars, R; Alonso, I; Ordi, J; Torné, A; Melchers, W J G; Meijer, C J L M; Quint, W G V

2013-06-01

High-risk human papillomavirus (hrHPV) testing in cervical screening is usually performed on physician-taken cervical smears in liquid-based medium. However, solid-state specimen carriers allow easy, non-hazardous storage and transportation and might be suitable for self-collection by non-responders in screening and in low-resource settings. We evaluated the adequacy of self-collected cervicovaginal (c/v) samples using a Viba-brush stored on an Indicating FTA-elute cartridge (FTA-based self-sampling) for hrHPV testing in women referred to a gynecology clinic due to an abnormal smear. 182 women accepted to self-collect a c/v sample. After self-sampling, a physician obtained a conventional liquid-based cervical smear. Finally, women were examined by colposcopy and a biopsy was taken when clinically indicated. Self-samples required only simple DNA elution, and DNA was extracted from physician-obtained samples. Both samples were tested for 14 hrHPVs by GP5+/6+-EIA-LQ Test and SPF(10)-DEIA-LiPA(25). Both assays detected significantly more hrHPV in physician-collected specimens than in self-collected samples (75.3% and 67.6% by SPF(10); 63.3% and 53.3% by GP5+/6+, respectively). The combination of physician-collected specimen and GP5+/6+ testing demonstrated the optimal balance in sensitivity (98.0%) and specificity (48.1%) for CIN2+ detection in this referral population. A test system of FTA-based self-collection and SPF(10) hrHPV detection approached this sensitivity (95.9%) and specificity (42.9%). These results show that the clinical performance of hrHPV detection is determined by both the sample collection system and the test method. FTA-based self-collection with SPF(10) testing might be valuable when a liquid-based medium cannot be used, but requires further investigation in screening populations. Copyright © 2013 Elsevier B.V. All rights reserved.

Preparation of a New Adsorbent from Activated Carbon and Carbon Nanofiber (AC/CNF for Manufacturing Organic-Vacbpour Respirator Cartridge

Directory of Open Access Journals (Sweden)

Mehdi Jahangiri

2013-01-01

Full Text Available In this study a composite of activated carbon and carbon nanofiber (AC/CNF was prepared to improve the performance of activated carbon (AC for adsorption of volatile organic compounds (VOCs and its utilization for respirator cartridges. Activated carbon was impregnated with a nickel nitrate catalyst precursor and carbonnanofibers (CNF were deposited directly on the AC surface using catalytic chemical vapor deposition. Deposited CNFs on catalyst particles in AC micropores, were activated by CO2 to recover the surface area and micropores.Surface and textural characterizations of the prepared composites were investigated using Brunauer, Emmett andTeller’s (BET technique and electron microscopy respectively. Prepared composite adsorbent was tested forbenzene, toluene and xylene (BTX adsorption and then employed in an organic respirator cartridge in granularform. Adsorption studies were conducted by passing air samples through the adsorbents in a glass column at an adjustable flow rate. Finally, any adsorbed species not retained by the adsorbents in the column were trapped in a charcoal sorbent tube and analyzed by gas chromatography. CNFs with a very thin diameter of about 10-20 nmwere formed uniformly on the AC/CNF. The breakthrough time for cartridges prepared with CO2 activated AC/CNF was 117 minutes which are significantly longer than for those cartridges prepared with walnut shell- based activated carbon with the same weight of adsorbents. This study showed that a granular form CO2 activated AC/CNF composite could be a very effective alternate adsorbent for respirator cartridges due to its larger adsorption capacities and lower weight.

The reactor Phenix - cartridge rupture detection

International Nuclear Information System (INIS)

Graftieaux, J.

1967-01-01

This report defines the role of cartridge rupture detection in the reactor Phenix. It gives the possible methods, their probable performances, their advantages and disadvantages. The final form of the installation will be determined mainly by the degree of safety required, by the technical possibilities of the reactor design and by the operational flexibility wanted. (author) [fr

Determining Service Life of Respirator Cartridges Using a Simple and Practical Method: Case Study in a Car Manufacturing Industry

Directory of Open Access Journals (Sweden)

A.M Rashidi

2012-01-01

Full Text Available Background and aims: For ensuring about proper performance of air-purifying respirators in providing protection against workplace contaminants, it is necessary to change the respirator cartridges before the end of their service life. The aim of this study was determination of service life of organic vapor cartridges using a simple and practical method in a spray painting booth of a car manufacturing industry.   Methods: NIOSH MultiVapor software was used for estimating service life of respirator cartridges based on workplace conditions and cartridge specifications. Efficiency of determined service life was investigated using an apparatus for field testing of cartridges in the workplace.   Results: The results showed that existing schedule for changing the respirator cartridges is not effective and no longer provide adequate protection for sprayers against organic contaminants while working in a painting booth. It is necessary to change the cartridges before their estimated service life (every 4 hours.   Conclusion: NIOSH MultiVapor has acceptable efficiency for determining respirator cartridges service life and could be used as a simple and practical method in the workplace. Moreover, Service life estimated by this software was confirmed by cartridge field test apparatus.

CONSTRUCTION AND OPTIMISATION OF A CARTRIDGE FILTER ...

African Journals Online (AJOL)

a

1Department of Chemistry, Egerton University, P.O. Box 356, Njoro, Kenya .... the resident time in the filter, thus there is not enough time for F- to interact with the ... associated with creation of too much backpressure in the cartridge as well as ...

A longitudinal evaluation of performance of automated BCR-ABL1 quantitation using cartridge-based detection system.

Science.gov (United States)

Enjeti, Anoop; Granter, Neil; Ashraf, Asma; Fletcher, Linda; Branford, Susan; Rowlings, Philip; Dooley, Susan

2015-10-01

An automated cartridge-based detection system (GeneXpert; Cepheid) is being widely adopted in low throughput laboratories for monitoring BCR-ABL1 transcript in chronic myelogenous leukaemia. This Australian study evaluated the longitudinal performance specific characteristics of the automated system.The automated cartridge-based system was compared prospectively with the manual qRT-PCR-based reference method at SA Pathology, Adelaide, over a period of 2.5 years. A conversion factor determination was followed by four re-validations. Peripheral blood samples (n = 129) with international scale (IS) values within detectable range were selected for assessment. The mean bias, proportion of results within specified fold difference (2-, 3- and 5-fold), the concordance rate of major molecular remission (MMR) and concordance across a range of IS values on paired samples were evaluated.The initial conversion factor for the automated system was determined as 0.43. Except for the second re-validation, where a negative bias of 1.9-fold was detected, all other biases fell within desirable limits. A cartridge-specific conversion factor and efficiency value was introduced and the conversion factor was confirmed to be stable in subsequent re-validation cycles. Concordance with the reference method/laboratory at >0.1-≤10 IS was 78.2% and at ≤0.001 was 80%, compared to 86.8% in the >0.01-≤0.1 IS range. The overall and MMR concordance were 85.7% and 94% respectively, for samples that fell within ± 5-fold of the reference laboratory value over the entire period of study.Conversion factor and performance specific characteristics for the automated system were longitudinally stable in the clinically relevant range, following introduction by the manufacturer of lot specific efficiency values.

Batch fabrication of polymer microfluidic cartridges for QCM sensor packaging by direct bonding

Science.gov (United States)

Sandström, Niklas; Zandi Shafagh, Reza; Gylfason, Kristinn B.; Haraldsson, Tommy; van der Wijngaart, Wouter

2017-12-01

Quartz crystal microbalance (QCM) sensing is an established technique commonly used in laboratory based life-science applications. However, the relatively complex, multi-part design and multi-step fabrication and assembly of state-of-the-art QCM cartridges make them unsuited for disposable applications such as point-of-care (PoC) diagnostics. In this work, we present the uncomplicated manufacturing of QCMs in polymer microfluidic cartridges. Our novel approach comprises two key innovations: the batch reaction injection molding of microfluidic parts; and the integration of the cartridge components by direct, unassisted bonding. We demonstrate molding of batches of 12 off-stoichiometry thiol-ene epoxy polymer (OSTE+) polymer parts in a single molding cycle using an adapted reaction injection molding process; and the direct bonding of the OSTE+  parts to other OSTE+  substrates, to printed circuit boards, and to QCMs. The microfluidic QCM OSTE+  cartridges were successfully evaluated in terms of liquid sealing as well as electrical properties, and the sensor performance characteristics are on par with those of a commercially available QCM biosensor cartridge. The simplified manufacturing of QCM sensors with maintained performance potentializes novel application areas, e.g. as disposable devices in a point of care setting. Moreover, our results can be extended to simplifying the fabrication of other microfluidic devices with multiple heterogeneously integrated components.

Depository of ampoule ionizing radiation sources on the basis of stand complex Baikal-I. Operation experience and application perspectives

International Nuclear Information System (INIS)

Ganzha, V.V.; Boltovskij, S.A.; Kolbaenkov, A.N.; Meshin, M.M.; Nasonov, S.G.; Pivovarov, O.S.; Storozhenko, A.S.; Yakovlev, V.V.

2001-01-01

Depository of ampoule sources of ionizing radiation (ASIR) on the basis of stand complex Baikal-I was founded an put into operation in 1995. It is intended for prolonged storage of the spent ASIR from a different institutions of Kazakhstan. To the present time a more than 10000 spent ASIR with activity more than 2000 Ci were taken and placed for storage

The isolation of water-soluble radionuclides from deteriorating spent nuclear fuel in zeolite cartridge

International Nuclear Information System (INIS)

Hassan, N.M.; Thompson, M.C.

1996-01-01

A method of isolating water-soluble radionuclides leaching from deteriorating spent nuclear fuel by ion-exchange in zeolite cartridges has been studied. Design calculations of two zeolite cartridges to be incorporated in typical spent fuel storage bundle have been provided. Equilibrium exchange data obtained at several temperatures have shown that the maximum exchange capacity of total cesium in sodium titanium aluminosilicate was 114 mg/g zeolite and the capacity at 95% exchange for radioactive isotope Cs-137 was calculated as 55.2 mg/g zeolite. The kinetic data suggest that the rate of exchange of Cs + in sodium titanium aluminosilicate zeolite takes place by a fast initial exchange step followed by slow diffusion of cesium cations. Design calculations based on the equilibrium exchange data show that water-soluble radionuclides leaching from Mk 31 slugs can be isolated using two zeolite cartridges, each 3.7 inches in inside diameter and 2.5 inches in length. The cartridges are designed to isolate 95% of the Cs + leaching from the spent fuel storage bundle. The results from the thermal induced convective flow tests indicate that the system will provide necessary cooling to the spent fuel by convective currents while isolating the Cs + leaching from spent fuel storage bundle in the cartridges

Separation of V(V)-4-(2-pyridylazo)resorcinolato complex from a large excess reagent using an ODS cartridge for high-performance liquid chromatography.

Science.gov (United States)

Takahashi, Toru; Kaneko, Emiko; Yotsuyanagi, Takao

2006-12-01

A selective off-line preconcentration technique for the V(V) complex with 4-(2-pyridylazo)resorcinol has been developed and successfully applied to the determination of V(V) in an air-borne sample. The target complex was separated from excess reagent using an ODS cartridge and water as the eluent. The complex was then concentrated on another ODS cartridge using tetrabutylammonium bromide and eluted with methanol; the eluate was applied to a one-drop concentration/HPLC. A detection limit as low as (6.05 +/- 0.82)x 10(-11) M (5 ppt) was achieved.

Simplified quality control of radioactive seeds in sterile cartridge for prostate brachytherapy using an imaging plate and a collimator

International Nuclear Information System (INIS)

Saze, T.; Miyoshi, H.; Maezawa, H.; Kubota, M.; Furutani, S.; Nishitani, H.; Kawaguchi, Y.; Nakayama, S.; Ito, S.; Nishizawa, K.

2008-01-01

Image analyzer system and collimator has been successfully applied to calibrate simultaneously multiple 125 I seeds in a sterile cartridge. Seeds within the cartridge were placed on an imaging plate, and the imaging plate irradiated. To remove scatter radiation, and improve spatial resolution of seed images, this study used a specially designed collimator. The irradiated imaging plate was scanned using an image analyzer system, and radioactivity intensities of seed images were given in counts. Counts could be translated to profiles, and each seed within the cartridge was analyzed. It is observed that a good correlation between counts and total radioactivity of the seeds within the cartridge. Thus, using a least-squares line, it was possible to calibrate a seed with unknown apparent activity. By analyzing the profiles, it was possible not only to detect a mis calibrated seed in the cartridge from its relative difference in counts, but also to identify its position in the cartridge. Using an imaging analyzer system, all seeds in a cartridge could be calibrated in a sterile environment. (author)

Characterization of the water filters cartridges from the iea-r1 reactor using the Monte Carlo method

International Nuclear Information System (INIS)

Costa, Priscila; Potiens Junior, Ademar J.

2015-01-01

Filter cartridges are part of the primary water treatment system of the IEA-R1 Research Reactor and, when saturated, they are replaced and become radioactive waste. The IEA-R1 is located at the Nuclear and Energy Research Institute (IPEN), in Sao Paulo, Brazil. The primary characterization is the main step of the radioactive waste management in which the physical, chemical and radiological properties are determined. It is a very important step because the information obtained in this moment enables the choice of the appropriate management process and the definition of final disposal options. In this paper, it is presented a non-destructive method for primary characterization, using the Monte Carlo method associated with the gamma spectrometry. Gamma spectrometry allows the identification of radionuclides and their activity values. The detection efficiency is an important parameter, which is related to the photon energy, detector geometry and the matrix of the sample to be analyzed. Due to the difficult to obtain a standard source with the same geometry of the filter cartridge, another technique is necessary to calibrate the detector. The technique described in this paper uses the Monte Carlo method for primary characterization of the IEA-R1 filter cartridges. (author)

Validation of a cartridge method for the quality control determination of 99Tcm-HMPAO

International Nuclear Information System (INIS)

Pandos, G.; Penglis, S.; Tsopelas, C.; Royal Adelaide Hospital, Adelaide, SA

1999-01-01

Full text: The manufacturer's method for assessing the radiochemical purity (RCP) of ±-HMPAO requires the use of three solvent types on two different stationary phases, and is time-consuming (∼ 15 min) in consideration of the short shelf-life (30 min). An impetus to develop a rapid quality control procedure for this product has led to the use of a single strip Whatman 17 chromatography system using ethyl acetate as the developing solvent. This popular Whatman paper system was previously validates against the manufacturer's method. We have developed a new method to successfully determine the % RCP of ±-HMPAO, which employs a disposable, inexpensive and reusable Amprep C-18 cartridge with normal saline as a non-organic mobile phase. The Whatman paper system separates the primary lipophilic 99 Tc m -HMPAO complex from 99 Tc m O-2, 99 Tc m O 4 and secondary 99 Tc m -HMPAO complex at the origin. By comparison, the lipophilic portion was retained on the cartridge and the hydrophilic impurities were found in saline eluent with the cartridge method. Whatman 17 paper system results showed 95.1 ± I.7% 99 Tc m -HMPAO after 5 min and the cartridge method gave 95.5 ± 1.5% 99 Tc m -HMPAO (n = 8) after 3 min. The % 99 Tc m O 2 levels in 99 Tc m -HMPAO were insignificant. When a failed kit was assessed for RCP at 2.5 h post-reconstitution, the Whatman paper system and the cartridge method correlated well, resulting in 63.1 ± 2.7% and 62.9±2.1% 99 Tc m -HMPAO (n=3) respectively. Although the cartridge method may slightly overestimate the % RCP of 99 Tc m -HMPAO, it was found to be simple, rapid and reliable for the quality control analysis of routine 99 Tc m -HMPAO preparations

Sensitivity analysis overlaps of friction elements in cartridge seals

Directory of Open Access Journals (Sweden)

Žmindák Milan

2018-01-01

Full Text Available Cartridge seals are self-contained units consisting of a shaft sleeve, seals, and gland plate. The applications of mechanical seals are numerous. The most common example of application is in bearing production for automobile industry. This paper deals with the sensitivity analysis of overlaps friction elements in cartridge seal and their influence on the friction torque sealing and compressive force. Furthermore, it describes materials for the manufacture of sealings, approaches usually used to solution of hyperelastic materials by FEM and short introduction into the topic wheel bearings. The practical part contains one of the approach for measurement friction torque, which results were used to specifying the methodology and precision of FEM calculation realized by software ANSYS WORKBENCH. This part also contains the sensitivity analysis of overlaps friction elements.

Optimal stapler cartridge selection according to the thickness of the pancreas in distal pancreatectomy.

Science.gov (United States)

Kim, Hongbeom; Jang, Jin-Young; Son, Donghee; Lee, Seungyeoun; Han, Youngmin; Shin, Yong Chan; Kim, Jae Ri; Kwon, Wooil; Kim, Sun-Whe

2016-08-01

Stapling is a popular method for stump closure in distal pancreatectomy (DP). However, research on which cartridges are suitable for different pancreatic thickness is lacking. To identify the optimal stapler cartridge choice in DP according to pancreatic thickness.From November 2011 to April 2015, data were prospectively collected from 217 consecutive patients who underwent DP with 3-layer endoscopic staple closure in Seoul National University Hospital, Korea. Postoperative pancreatic fistula (POPF) was graded according to International Study Group on Pancreatic Fistula definitions. Staplers were grouped based on closed length (CL) (Group I: CL ≤ 1.5 mm, II: 1.5 mm 17 mm. With pancreatic thickness <12 mm, the POPF rate was lowest with Group II (I: 50%, II: 27.6%, III: 69.2%, P = 0.035).The optimal stapler cartridges with pancreatic thickness <12 mm were those in Group II (Gold, CL: 1.8 mm). There was no suitable cartridge for thicker pancreases. Further studies are necessary to reduce POPF in thick pancreases.

Magazine Influence on Cartridge Case Ejection Patterns with Glock Pistols.

Science.gov (United States)

Kerkhoff, Wim; Alberink, Ivo; Mattijssen, Erwin J A T

2018-01-01

In this study, the cartridge case ejection patterns of six different Glock model pistols (one specimen per model) were compared under three conditions: firing with a loaded magazine, an empty magazine, and without magazine. The distances, covered by the ejected cartridge cases given these three conditions, were compared for each of the six models. A significant difference was found between the groups of data for each of the tested specimens. This indicates that it is important that, to reconstruct a shooting scene incident based on the ejection patterns of a pistol, test shots are fired with the same pistol type and under the correct magazine condition. © 2017 American Academy of Forensic Sciences.

Change in muzzle velocity due to freezing and water immersion of .22, long rifle, K.F. cartridges.

Science.gov (United States)

Jauhari, M; Chatterjee, S M; Ghosh, P K

1975-01-01

A study of change in muzzle velocity due to freezing and water immersion of .22, long rifle, K. F. cartridges has been presented. A statistical criterion has been formulated to ascertain whether or not a cartridge undergoes a change in muzzle velocity due to a particular treatment. The muzzle velocity data of .22, long rifle, K. F. cartridges, obtained by an electronic timer before and after the various treatments, have been analyzed in the light of this criterion. These cartridges have generally been found to suffer considerable loss in muzzle velocity when immersed in water for three weeks and also when immersed in water for three days and simultaneously cooled to 0 degrees C. The forensic significance of this loss in muzzle velocity has been discussed.

Comparison of a gel column blood typing method and a point-of-care cartridge for dog erythrocyte antigen 1.1.

Science.gov (United States)

Blois, Shauna L; Richardson, Danielle M; Abrams-Ogg, Anthony C G

2013-01-01

Blood typing for the presence of Dog Erythrocyte Antigen (DEA) 1.1 is recommended in all donor and recipient dogs prior to transfusion of blood products. The objective of this study was to determine if a point-of-care DEA 1.1 blood typing cartridge could be used in place of the gel column typing method. Detection of DEA 1.1 was performed using a laboratory-based gel column method and a point-of-care cartridge. A convenience sample of 30 healthy blood donors, 13 dogs with immune-mediated hemolytic anemia (IMHA) (3 of which had concurrent immune-mediated thrombocytopenia [IMT]), and 44 dogs with other diseases was included in the study. Agreement was observed between the tests for normal dogs and dogs with nonimmune-mediated disease in 74/74 cases. Two dogs in the IMHA group had indeterminate gel column blood typing results; 1 dog in this group had a negative gel column test result but a positive cartridge test result. There was good agreement between the 2 methods for normal dogs and dogs with nonimmune-mediated disease. Blood typing methods in dogs with IMHA should be further investigated. © Veterinary Emergency and Critical Care Society 2013.

Synthesis of O-(2-[18F]fluoroethyl)-L-tyrosine based on a cartridge purification method

International Nuclear Information System (INIS)

Mueller, Dirk; Klette, Ingo; Kalb, Fabrizia; Baum, Richard P.

2011-01-01

Introduction: O-(2-[ 18 F]fluoroethyl)-L-tyrosine (FET) is widely used as a positron emission tomography tracer for brain tumors. Usually, a high-performance liquid chromatography (HPLC) purification at the end of the two-step synthesis is applied. In this work, we report an automatic radiosynthesis of FET with a purification procedure based on standard cartridges. Methods: O-(2-[ 18 F]fluoroethyl)-L-tyrosine was prepared by [ 18 F]fluoroethylation of L-tyrosine by a two-step synthesis using a modified [ 11 C]methionine module (Nuclear Interface). In the first reaction step, we synthesized [ 18 F]fluoroethyltosylate starting from [ 18 F]fluoride. After a purification step, L-tyrosine was [ 18 F]fluoroethylated with [ 18 F]fluoroethyltosylate. The final reaction mixture was purified by means of solid phase extraction. The FET was trapped on an SCX cartridge, eluted with saline solution and trapped again on an HRX cartridge. For a second purification step, the FET was eluted from the HRX cartridge with ammonium acetate buffer and collected on two SCX cartridges followed by a washing step with water. The final product was eluted with saline solution and neutralised with 450 μl NaHCO 3 solution (8.4%). Results: The synthesis was finished after 50 min and delivered the FET in a range of 3-16 GBq. The synthesis typically yielded 41% (21 experiments) of FET (d.c.) without an HPLC purification step. The radiochemical purity ranged between 97% and 100%. Conclusion: We present a radiosynthesis of FET where the usually used HPLC purification procedure has been substituted by a purification step based on standard cartridges. This method is useful for automatic modules without an expensive HPLC purification unit and for the routine production of FET.

Microfluidic cartridges for automated, point-of-care blood cell counting

CSIR Research Space (South Africa)

Smith, Suzanne

2016-11-01

Full Text Available Disposable, low-cost microfluidic cartridges for automated blood cell counting applications are presented in this article. The need for point-of-care medical diagnostic tools is evident, particularly in low-resource and rural settings, and a full...

[Effectiveness of FTA Elute® indicating cartridge in combination with hybrid capture 2 for cervical cancer screening].

Science.gov (United States)

Chen, Feng; Zhang, Xi; Wang, Shaoming; Hu, Shangying; Chen, Wen; Zhao, Fanghui; He, Wei; Zhang, Yuqing; Qiao, Youlin

2015-02-01

To evaluate the effectiveness of FTA Elute® Cartridge (GE healthcare, Kent, UK) in combination with hybrid capture 2 (HC2) testing for cervical cancer screening. From May to June 2012, 412 women aged 25 to 65 years in Jiangxi Tonggu were enrolled in the study. We used pathological outcome as the gold standard, and the accuracy of the FTA card in combination with HC2 testing was investigated from both physician- and self-sampling, respectively. Physician sampling using the FTA card in combination with HC2 testing showed a comparable sensitivity (12/13) with the liquid based medium, but a higher specificity 69.5% (266/383) vs (77.8%, 298/383) (P FTA card in combination with HC2 testing with liquid based medium was 10/13 vs 8/13(P = 0.625) and (62.3%, 238/382) vs (75.7%, 289/382) (P FTA and liquid-based sampling medium was 86.1% (340/395) and 79.5% (314/395). For physician-collected samples used for HC2 testing to detect CIN2+, the accuracy of the FTA card was superior to that of the liquid-based medium (area under the receiver operating characteristic curve (AUC) = 0.898, 95%CI:0.838-0.958). FTA Elute® cartridge in combination with HC2 testing is a promising method of specimen transport for cervical cancer screening programs with a good precision.With further optimization, it could become an effective method for cervical cancer screening in various economic levels of areas.

Time since discharge of 9mm cartridges by headspace analysis, part 1: Comprehensive optimisation and validation of a headspace sorptive extraction (HSSE) method.

Science.gov (United States)

Gallidabino, M; Romolo, F S; Weyermann, C

2017-03-01

Estimating the time since discharge of spent cartridges can be a valuable tool in the forensic investigation of firearm-related crimes. To reach this aim, it was previously proposed that the decrease of volatile organic compounds released during discharge is monitored over time using non-destructive headspace extraction techniques. While promising results were obtained for large-calibre cartridges (e.g., shotgun shells), handgun calibres yielded unsatisfying results. In addition to the natural complexity of the specimen itself, these can also be attributed to some selective choices in the methods development. Thus, the present series of paper aimed to more systematically evaluate the potential of headspace analysis to estimate the time since discharge of cartridges through the use of more comprehensive analytical and interpretative techniques. Specifically, in this first part, a method based on headspace sorptive extraction (HSSE) was comprehensively optimised and validated, as the latter recently proved to be a more efficient alternative than previous approaches. For this purpose, 29 volatile organic compounds were preliminary selected on the basis of previous works. A multivariate statistical approach based on design of experiments (DOE) was used to optimise variables potentially involved in interaction effects. Introduction of deuterated analogues in sampling vials was also investigated as strategy to account for analytical variations. Analysis was carried out by selected ion mode, gas chromatography coupled to mass spectrometry (GC-MS). Results showed good chromatographic resolution as well as detection limits and peak area repeatability. Application to 9mm spent cartridges confirmed that the use of co-extracted internal standards allowed for improved reproducibility of the measured signals. The validated method will be applied in the second part of this work to estimate the time since discharge of 9mm spent cartridges using multivariate models. Copyright �

Combustible Cartridge Cases: Current Status and Future Prospects

Science.gov (United States)

1992-08-01

and presents new models of combustible cartridge case burning . Following a summary of experimental data, it concludes with proposals for further...UNCLASSIFIED UNCLASSIFIED UNCLASSIFIED SAR NSN 7540-01-280-5500 Standard Form 298 (Rev 2-89) Precribed by ANSI Std Z39-19 IWFENTIONALLY LEFT BLANK...7 3.3 In-Depth Burning Model ........................................ 7 3.3.1 M odel A ................................................ 9 3.3.2

Characterization of cartridge filters from the IEA-R1 Nuclear Reactor

International Nuclear Information System (INIS)

2015-01-01

The management of radioactive waste ensures safety to human health and the environment nowadays and for the future, without overwhelming the upcoming generations. The primary characterization of radioactive waste is one of the main steps in the management of radioactive waste. This step permits to choose the best treatment for the radioactive waste before forwarding it to its final disposal. The aim of the present work is the primary characterization of cartridge filters from the IEA-R1 nuclear reactor utilizing gamma-ray spectrometry, and the method of Monte Carlo for calibration. The IEA-R1 is located in the Nuclear and Energy Research Institute (IPEN - CNEN) in the city of Sao Paulo, Brazil. Cartridge filters are used for purification of the cooling water that is pumped through the core of the pool type nuclear research reactors. Once worn out, these filters are replaced and then become radioactive waste. Determination of the radioactive inventory is of paramount importance in the management of such radioactive waste, and one of the main methods for doing so is the gamma-ray spectrometry, which can identify and quantify high energy photon emitters. The technique chosen for the characterization of radioactive waste in the present work is the gamma-ray spectrometry with High purity Germanium (HPGe) detectors. From the energy identified in the experimental spectrum, three radioisotopes were identified in the cartridge filter: 108m Ag, 110m Ag, 60 Co. For the estimated activity of the filter, the calibration in efficiency was made utilizing the MCNP4C code of the Monte Carlo method. Such method was chosen because there is no standard source available in the same geometry of the cartridge filter, therefore a simulation had to be developed in order to reach a calibration equation, necessary to estimate the activity of the radioactive waste. The results presented an activity value in the order of MBq for all radioisotopes. (authors)

Characterization of cartridge filters from the IEA-R1 Nuclear Reactor

Energy Technology Data Exchange (ETDEWEB)

NONE

2015-07-01

The management of radioactive waste ensures safety to human health and the environment nowadays and for the future, without overwhelming the upcoming generations. The primary characterization of radioactive waste is one of the main steps in the management of radioactive waste. This step permits to choose the best treatment for the radioactive waste before forwarding it to its final disposal. The aim of the present work is the primary characterization of cartridge filters from the IEA-R1 nuclear reactor utilizing gamma-ray spectrometry, and the method of Monte Carlo for calibration. The IEA-R1 is located in the Nuclear and Energy Research Institute (IPEN - CNEN) in the city of Sao Paulo, Brazil. Cartridge filters are used for purification of the cooling water that is pumped through the core of the pool type nuclear research reactors. Once worn out, these filters are replaced and then become radioactive waste. Determination of the radioactive inventory is of paramount importance in the management of such radioactive waste, and one of the main methods for doing so is the gamma-ray spectrometry, which can identify and quantify high energy photon emitters. The technique chosen for the characterization of radioactive waste in the present work is the gamma-ray spectrometry with High purity Germanium (HPGe) detectors. From the energy identified in the experimental spectrum, three radioisotopes were identified in the cartridge filter: {sup 108m}Ag, {sup 110m}Ag, {sup 60}Co. For the estimated activity of the filter, the calibration in efficiency was made utilizing the MCNP4C code of the Monte Carlo method. Such method was chosen because there is no standard source available in the same geometry of the cartridge filter, therefore a simulation had to be developed in order to reach a calibration equation, necessary to estimate the activity of the radioactive waste. The results presented an activity value in the order of MBq for all radioisotopes. (authors)

Identifying persistent and characteristic features in firearm tool marks on cartridge cases

Science.gov (United States)

Ott, Daniel; Soons, Johannes; Thompson, Robert; Song, John

2017-12-01

Recent concerns about subjectivity in forensic firearm identification have motivated the development of algorithms to compare firearm tool marks that are imparted on ammunition and to generate quantitative measures of similarity. In this paper, we describe an algorithm that identifies impressed tool marks on a cartridge case that are both consistent between firings and contribute strongly to a surface similarity metric. The result is a representation of the tool mark topography that emphasizes both significant and persistent features across firings. This characteristic surface map is useful for understanding the variability and persistence of the tool marks created by a firearm and can provide improved discrimination between the comparison scores of samples fired from the same firearm and the scores of samples fired from different firearms. The algorithm also provides a convenient method for visualizing areas of similarity that may be useful in providing quantitative support for visual comparisons by trained examiners.

Bubble Jet agent release cartridge for chemical single cell stimulation.

Science.gov (United States)

Wangler, N; Welsche, M; Blazek, M; Blessing, M; Vervliet-Scheebaum, M; Reski, R; Müller, C; Reinecke, H; Steigert, J; Roth, G; Zengerle, R; Paust, N

2013-02-01

We present a new method for the distinct specific chemical stimulation of single cells and small cell clusters within their natural environment. By single-drop release of chemical agents with droplets in size of typical cell diameters (d agent release cartridge with integrated fluidic structures and integrated agent reservoirs are shown, tested, and compared in this publication. The single channel setup features a fluidic structure fabricated by anisotropic etching of silicon. To allow for simultaneous release of different agents even though maintaining the same device size, the second type comprises a double channel fluidic structure, fabricated by photolithographic patterning of TMMF. Dispensed droplet volumes are V = 15 pl and V = 10 pl for the silicon and the TMMF based setups, respectively. Utilizing the agent release cartridges, the application in biological assays was demonstrated by hormone-stimulated premature bud formation in Physcomitrella patens and the individual staining of one single L 929 cell within a confluent grown cell culture.

Computer-Aided-Design of the Hydraulic System of Three-Dimensional Cartridge Valve Blocks (Selected Articles)

Science.gov (United States)

1991-03-21

sectional representation of the spatial figure can be correctly determined. 6 The AutoLisp language system in the AutoCAD software provides the most...softwares are developed on the 32-bit machines and little progress has been reported for the 16-bit machines. Even the AutoCAD is a two-ard-a-half... AutoCAD software as the basis, developed the design package of 3-D cartridge valve blocks on IM PC/AT. To realize the 3-D displaying of cartridge valves

Unsuitability of using the DNPH-coated solid sorbent cartridge for determination of airborne unsaturated carbonyls

Science.gov (United States)

Ho, Steven Sai Hang; Ho, K. F.; Liu, W. D.; Lee, S. C.; Dai, W. T.; Cao, J. J.; Ip, H. S. S.

2011-01-01

Measurements of aldehydes and ketones are typically conducted by derivatization using sorbent cartridges coated with 2,4-dinitrophenylhydrazine (DNPH). The collected samples are eluted with acetonitrile and analyzed by high-pressure liquid chromatography coupled with an ultra-violet detector (HPLC/UV). This paper intends to examine artifacts about its suitability in identification of unsaturated carbonyls. Kinetic tests for acrolein, crotonaldehyde, methacrolein and methyl vinyl ketone (MVK) showed formations of carbonyl-DNP-hydrazone during sampling, which could further react with DNPH, resulting in undesired UV absorption products [e.g., carbonyl-DNP-hydrazone-DNPH (dimer) and 2(carbonyl-DNP-hydrazone)-DNPH (trimer)]. The dimerization and trimerization occurred for acrolein and MVK whereas only dimerization for crotonaldehyde and methacrolein. The polymerization products undoubtedly affect the integrity of the chromatogram, leading to misidentification and inaccurate quantification. Whether precautions taken during sampling and/or sample treatment could avoid or minimize this artifact has not been thoughtfully investigated. More often, such artifacts are usually overlooked by scientists when the data are reported.

Motion-Based pH Sensing Based on the Cartridge-Case-like Micromotor.

Science.gov (United States)

Su, Yajun; Ge, Ya; Liu, Limei; Zhang, Lina; Liu, Mei; Sun, Yunyu; Zhang, Hui; Dong, Bin

2016-02-17

In this paper, we report a novel cartridge-case-like micromotor. The micromotor, which is fabricated by the template synthesis method, consists of a gelatin shell with platinum nanoparticles decorating its inner surface. Intriguingly, the resulting cartridge-case-like structure exhibits a pH-dependent "open and close" feature, which originates from the pH responsiveness of the gelatin material. On the basis of the catalytic activity of the platinum nanoparticle inside the gelatin shell, the resulting cartridge-case-like structure is capable of moving autonomously in the aqueous solution containing the hydrogen peroxide fuel. More interestingly, we find out that the micromotor can be utilized as a motion-based pH sensor over the whole pH range. The moving velocity of the micromotor increases monotonically with the increase of pH of the analyte solution. Three different factors are considered to be responsible for the proportional relation between the motion speed and pH of the analyte solution: the peroxidase-like and oxidase-like catalytic behavior of the platinum nanoparticle at low and high pH, the volumetric decomposition of the hydrogen peroxide under the basic condition and the pH-dependent catalytic activity of the platinum nanoparticle caused by the swelling/deswelling behavior of the gelatin material. The current work highlights the impact of the material properties on the motion behavior of a micromotor, thus paving the way toward its application in the motion-based sensing field.

On-cartridge derivatisation using matrix solid phase dispersion for the determination of cyclamate in foods

International Nuclear Information System (INIS)

Li, Jianjun; Liu, Yun; Liu, Qianping; Hui, Junfeng; Liu, Yangzi

2017-01-01

A novel method for determination of sodium cyclamate in foods was developed. In this method, a syringe was loaded with the homogeneous mixture of the sample, KMnO 4 powder and silica dispersant and used as a matrix solid phase dispersion (MSPD) reactor. As the reactor was infiltrated with small amounts of concentrated HCl, cyclamate was converted to 2-chlorocyclohexanone quickly and effectively within 5 min and determined by HPLC on a reversed-phase column using UV detection at a wavelength of 310 nm. Comparing with the traditional derivatisation in solution, the better clean-up was provided using on-cartridge derivatisation of MSPD, and much time, labor, and expense were saved. The results showed good linearity (r 2  = 0.9998) over the concentration range of 1–500 mg/L. The limit of detection (LOD) and limits of quantification (LOQ) of the cyclamate were 0.3 mg/L and 1 mg/L respectively. The recoveries ranged from 91.6% to 101.3% with the relative standard deviations (RSDs) in the range of 2.5%–4.3%. - Highlights: • A novel method was developed for the determination of cyclamate in foods. • On cartridge derivatisation, using matrix solid phase dispersion, was developed. • A new derivatisation reaction for cyclamate conversion to 2-chlorocyclohexanone was developed. • The method was rapid, simple, inexpensive, effective.

Development of a method for rapid and simultaneous monitoring of particulate and dissolved radiocesium in water with nonwoven fabric cartridge filters

International Nuclear Information System (INIS)

Hideki Tsuji; Tetsuo Yasutaka; Yoshihiko Kondo; Yasukazu Suzuki

2014-01-01

A method for the rapid and simultaneous monitoring of particulate and dissolved 137 Cs concentration in water was developed. This method uses pleated polypropylene nonwoven fabric filter to collect particulate radiocesium, and nonwoven fabric impregnated with Prussian blue (PB) to absorb dissolved radiocesium. The fabric was placed into cylindrical plastic cartridges (SS-cartridge and PB-cartridge). Traditional monitoring methods, such as evaporative concentration, often require time for pre-processing. However, this method described requires much less pre-processing time before the detection. Experiments conducted with simulated river water demonstrated that almost all of the suspended solids weight was collected in the SS-cartridge, and that more than 92 % of dissolved 137 Cs was absorbed onto the two PB-cartridges by 2.5 L/min flow rate when the range of the pH was 6-8. This device was applied to monitor Abukuma River water at two locations and the results were compared with those obtained using the filtrating and evaporative concentration method. The suspended solids concentration in river water, calculated by weight gain of the SS-cartridge and by sediment weight after filtration with a 0.45-μm membrane filter, agreed well. The radioactivity of the particulate and dissolved 137 Cs also agreed well in one of the two replications of this method. In addition, the required time for pre-processing was reduced by 60 times that by filtrating and evaporative concentration method. This method can separately collect and concentrate particulate and dissolved radiocesium rapidly and simultaneously in the field. (author)

Community Laboratory Testing for Cryptosporidium: Multicenter Study Retesting Public Health Surveillance Stool Samples Positive for Cryptosporidium by Rapid Cartridge Assay with Direct Fluorescent Antibody Testing.

Directory of Open Access Journals (Sweden)

Dawn M Roellig

Full Text Available Cryptosporidium is a common cause of sporadic diarrheal disease and outbreaks in the United States. Increasingly, immunochromatography-based rapid cartridge assays (RCAs are providing community laboratories with a quick cryptosporidiosis diagnostic method. In the current study, the Centers for Disease Control and Prevention (CDC, the Association of Public Health Laboratories (APHL, and four state health departments evaluated RCA-positive samples obtained during routine Cryptosporidium testing. All samples underwent "head to head" re-testing using both RCA and direct fluorescence assay (DFA. Community level results from three sites indicated that 54.4% (166/305 of Meridian ImmunoCard STAT! positives and 87.0% (67/77 of Remel Xpect positives were confirmed by DFA. When samples were retested by RCA at state laboratories and compared with DFA, 83.3% (155/186 of Meridian ImmunoCard STAT! positives and 95.2% (60/63 of Remel Xpect positives were confirmed. The percentage of confirmed community results varied by site: Minnesota, 39.0%; New York, 63.9%; and Wisconsin, 72.1%. The percentage of confirmed community results decreased with patient age; 12.5% of community positive tests could be confirmed by DFA for patients 60 years of age or older. The percentage of confirmed results did not differ significantly by sex, storage temperature, time between sample collection and testing, or season. Findings from this study demonstrate a lower confirmation rate of community RCA positives when compared to RCA positives identified at state laboratories. Elucidating the causes of decreased test performance in order to improve overall community laboratory performance of these tests is critical for understanding the epidemiology of cryptosporidiosis in the United States (US.

Characteristics of a cartridge NEG (St101 Zr-Al)

International Nuclear Information System (INIS)

Hisamatsu, Hiromi; Shimamoto, Masayuki; Kanazawa, Ken-ichi; Ishimaru, Hajime

1990-01-01

The report addresses the application of a non-evaporable getter (NEG) pump to an accelerator (storage ring). Tests are performed to determine major characteristics of the non-evaporable getter pump in an effort to provide a method for its efficient use. Test results show that with an St101 cartridge NEG pump, it is possible to produce an ultrahigh vacuum in a system with a surface area of about 10 4 cm 2 through baking at 410K for two hours. Once activated at 1000K, a NEG pump recovers a pumping performance in a subsequent test run at 723K, though the pumping speed decreases by several tens of percent. The St-101 cartridge type NEG pump is at least 2 Pam 3 in pumping capacity for carbon monoxide. The pumping speed decreases with an increasing amount of occluded carbon monoxide. Upon activation, most of the occluded carbon monoxide diffuses into the pump while only little of it is released into the gas phase. Its diffusion through the surface of the NEG pump can occur even at room temperature, indicating that if a leak takes place, the pump would absorb the gas continuously. Thus, if a leak occurs during activation, the pump would occlude a large amount of gas and therefore, activation should be carried out with careful checking for a leak. (N.K.)

On-cartridge derivatisation using matrix solid phase dispersion for the determination of cyclamate in foods

Energy Technology Data Exchange (ETDEWEB)

Li, Jianjun, E-mail: bootan12@126.com [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, Northwest University, Xi' an 710069 (China); National Engineering Research Center for Miniaturized Detection Systems, Xi' an 710069 (China); Liu, Yun [College of Food Engineering and Nutritional Science, Shaanxi Normal University, Xi' an 710062 (China); Liu, Qianping [National Engineering Research Center for Miniaturized Detection Systems, Xi' an 710069 (China); Hui, Junfeng [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, Northwest University, Xi' an 710069 (China); Liu, Yangzi [National Engineering Research Center for Miniaturized Detection Systems, Xi' an 710069 (China)

2017-06-15

A novel method for determination of sodium cyclamate in foods was developed. In this method, a syringe was loaded with the homogeneous mixture of the sample, KMnO{sub 4} powder and silica dispersant and used as a matrix solid phase dispersion (MSPD) reactor. As the reactor was infiltrated with small amounts of concentrated HCl, cyclamate was converted to 2-chlorocyclohexanone quickly and effectively within 5 min and determined by HPLC on a reversed-phase column using UV detection at a wavelength of 310 nm. Comparing with the traditional derivatisation in solution, the better clean-up was provided using on-cartridge derivatisation of MSPD, and much time, labor, and expense were saved. The results showed good linearity (r{sup 2} = 0.9998) over the concentration range of 1–500 mg/L. The limit of detection (LOD) and limits of quantification (LOQ) of the cyclamate were 0.3 mg/L and 1 mg/L respectively. The recoveries ranged from 91.6% to 101.3% with the relative standard deviations (RSDs) in the range of 2.5%–4.3%. - Highlights: • A novel method was developed for the determination of cyclamate in foods. • On cartridge derivatisation, using matrix solid phase dispersion, was developed. • A new derivatisation reaction for cyclamate conversion to 2-chlorocyclohexanone was developed. • The method was rapid, simple, inexpensive, effective.

EPA Region 8, Memo on Desktop Printer Ink Cartridges Policy & Voluntary Printer Turn-in

Science.gov (United States)

This memo requests EPA Region 8 users to voluntarily turn-in their desktop printers and notifies users of the Region 8 policy to not provide maintenance or ink and toner cartridges for desktop printers.

Positive detection of exfoliated colon cancer cells on linear stapler cartridges was associated with depth of tumor invasion and preoperative bowel preparation in colon cancer.

Science.gov (United States)

Ikehara, Kishiko; Endo, Shungo; Kumamoto, Kensuke; Hidaka, Eiji; Ishida, Fumio; Tanaka, Jun-Ichi; Kudo, Shin-Ei

2016-08-31

The aim of this study was to investigate exfoliated cancer cells (ECCs) on linear stapler cartridges used for anastomotic sites in colon cancer. We prospectively analyzed ECCs on linear stapler cartridges used for anastomosis in 100 colon cancer patients who underwent colectomy. Having completed the functional end-to-end anastomosis, the linear stapler cartridges were irrigated with saline, which was collected for cytological examination and cytological diagnoses were made by board-certified pathologists based on Papanicolaou staining. The detection rate of ECCs on the linear stapler cartridges was 20 %. Positive detection of ECCs was significantly associated with depth of tumor invasion (p = 0.012) and preoperative bowel preparation (p = 0.003). There were no marked differences between ECC-positive and ECC-negative groups in terms of the operation methods, tumor location, histopathological classification, and surgical margins. Since ECCs were identified on the cartridge of the linear stapler used for anastomosis, preoperative mechanical bowel preparation using polyethylene glycol solution and cleansing at anastomotic sites using tumoricidal agents before anastomosis may be necessary to decrease ECCs in advanced colon cancer.

Environmental impacts and resource losses of incinerating misplaced household special wastes (WEEE, batteries, ink cartridges and cables)

DEFF Research Database (Denmark)

Bigum, Marianne Kristine Kjærgaard; Damgaard, Anders; Scheutz, Charlotte

2017-01-01

The contribution of misplaced special waste (sWEEE, lamps, CRT, batteries, ink cartridges and cables) to environmental impacts from incineration of residual household waste was quantified through life cycle assessment (LCA)-modelling. Misplaced special waste was quantified to constitute less than 1...... and batteries. However as shown by sensitivity analysis, lack of good data on the transfer of rare and hazardous metals to the flue gas in the incineration process should receive further investigation before the environmental impacts from misplaced incinerated special waste can fully be concluded upon. Although...... special waste (sWEEE, lamps, CRT, batteries, ink cartridges, and cables)....

Behavioral response and pain perception to computer controlled local anesthetic delivery system and cartridge syringe

Directory of Open Access Journals (Sweden)

T D Yogesh Kumar

2015-01-01

Full Text Available Aim: The present study evaluated and compared the pain perception, behavioral response, physiological parameters, and the role of topical anesthetic administration during local anesthetic administration with cartridge syringe and computer controlled local anesthetic delivery system (CCLAD. Design: A randomized controlled crossover study was carried out with 120 children aged 7-11 years. They were randomly divided into Group A: Receiving injection with CCLAD during first visit; Group B: Receiving injection with cartridge syringe during first visit. They were further subdivided into three subgroups based on the topical application used: (a 20% benzocaine; (b pressure with cotton applicator; (c no topical application. Pulse rate and blood pressure were recorded before and during injection procedure. Objective evaluation of disruptive behavior and subjective evaluation of pain were done using face legs activity cry consolability scale and modified facial image scale, respectively. The washout period between the two visits was 1-week. Results: Injections with CCLAD produced significantly lesser pain response, disruptive behavior (P < 0.001, and pulse rate (P < 0.05 when compared to cartridge syringe injections. Application of benzocaine produced lesser pain response and disruptive behavior when compared to the other two subgroups, although the result was not significant. Conclusion: Usage of techniques which enhance behavioral response in children like injections with CCLAD can be considered as a possible step toward achieving a pain-free pediatric dental practice.

Influence Factors Regarding the Effectiveness of Automated Ballistic Comparison on 0.38 Special Caliber Bullets and Cartridge Cases.

Science.gov (United States)

Dos Santos, Lehi Sudy; Vieira Muterlle, Palloma

2018-03-01

Factors influencing effectiveness of automated comparisons, test-fired bullets, and cartridge cases from 0.38 Special revolvers were logged into the Evofinder ® Ballistic ID System. Tests were performed as follows: First test correlated test-fires of the same type, second test compared different types of ammunition components, third test replicated the second test in a larger database, and fourth test replicated the third test with students having no previous firearm identification experience. System effectiveness with projectiles in the first test was 0.89. With cartridge cases, effectiveness was 0.79 with combined results, but analysis of separate results by breech face and firing pin revealed low effectiveness by breech face (0.40). In the second, third, and fourth tests, effectiveness with projectiles were 0.61, 0.51, and 0.44. In addition, these tests had effectiveness with cartridge cases equivalent to 0.55, 0.43, and 0.44. Results are useful to establish routine protocols, system improvements, or comparative assessment of other electronic systems. © 2018 American Academy of Forensic Sciences.

A patterned abrasion caused by the impact of a cartridge case may simulate an atypical muzzle imprint mark.

Science.gov (United States)

Kramer, Lena; Nadjem, Hadi; Glardon, Matthieu; Kneubuehl, Beat P; Pollak, Stefan; Große Perdekamp, Markus; Pircher, Rebecca

2016-05-01

In contact shots, the muzzle imprint is an informative finding associated with the entrance wound. It typically mirrors the constructional components being in line with the muzzle or just behind. Under special conditions, other patterned skin marks located near a gunshot entrance wound may give the impression to be part of the muzzle imprint. A potential mechanism causing a patterned pressure abrasion in close proximity to the bullet entrance site is demonstrated on the basis of a suicidal shot to the temple. The skin lesion in question appeared as a ring-shaped excoriation with a diameter corresponding to that of the cartridge case. Two hypotheses concerning the causative mechanism were investigated by test shots: - After being ejected, the cartridge case ricocheted inside a confined space (car cabin in the particular case) and secondarily hit the skin near the gunshot entrance wound. - The ejection of the cartridge case failed so that the case became stuck in the ejection port and its mouth contacted the skin when the body collapsed after being hit.

Analysis of large soil samples for actinides

Science.gov (United States)

Maxwell, III; Sherrod, L [Aiken, SC

2009-03-24

A method of analyzing relatively large soil samples for actinides by employing a separation process that includes cerium fluoride precipitation for removing the soil matrix and precipitates plutonium, americium, and curium with cerium and hydrofluoric acid followed by separating these actinides using chromatography cartridges.

Development and Preliminary Assessment of Hemoperfusion Cartridge with Tannic Acid for Toxic Proteins' Precipitation: An In Vitro Model

Directory of Open Access Journals (Sweden)

Valquíria Miwa Hanai Yoshida

2016-09-01

Full Text Available Charcoal hemoperfusion (CHP is one of the extracorporeal removal techniques that are used to remove toxins from the body. CHP generally is considered the preferred method for extracorporeal extraction of several toxins—toxins that are adsorbed by activated charcoal. Assessments of the tannic acid's protective effects on ophidian poisoning are associated with the toxic proteins' precipitation by tannic acid. The challenge in treating a snakebite lies in removing the injected poison with minimal damage to blood constituent proteins. An alternative is CHP, and this investigation proposed to develop a column for hemoperfuser cartridge, combining charcoal granules trapped between layers of polymeric material conjugated to tannic acid, using an in vitro model scaled to the Wistar rat, which can be tested in an animal model. The cartridge was evaluated using the 22 full factorial design, in duplicate, as a method to study the effects of granulated-charcoal size and tannic acid concentration on the hematologic profile (platelet and leukocyte counts and biochemical profile (total serum protein and albumin dosages of sheep blood. The results demonstrate that charcoal in hemoperfuser cartridge: (1 decreases the serum in sheep blood volume, as consequence, (2 increases the serum proteins' concentration, and (iii exerts slight influence on albumin. The inclusion of tannic acid in hemoperfuser column precipitates some of serum proteins and albumin, decreasing their concentrations in the plasma serum. In conclusion, based on these effects we can suggest the use of 0.02 g tannic acid concentration and 8–20 mesh granulated charcoal in hemoperfuser cartridge for precipitating toxic proteins from snake venoms.

Safety limits of half-mask cartridge respirators for organic solvent vapors

International Nuclear Information System (INIS)

Anon.

1975-01-01

Recent studies of the effective service life (safety limits) for typical half-mask cartridge respirators have shown these devices to be unsuitable for certain organic vapors, e.g., methanol, methylamine, vinyl chloride, and dichloromethane, because the effective service life is too short. For these vapors other forms of protection such as air-supplied respirators are recommended. The experimentally determined service life for many vapors is shorter--sometimes significantly shorter--than predicted by adsorption theory

Coagulation measurement from whole blood using vibrating optical fiber in a disposable cartridge.

Science.gov (United States)

Yaraş, Yusuf Samet; Gündüz, Ali Bars; Sağlam, Gökhan; Ölçer, Selim; Civitçi, Fehmi; Baris, İbrahim; Yaralioğlu, Göksenin; Urey, Hakan

2017-11-01

In clinics, blood coagulation time measurements are performed using mechanical measurements with blood plasma. Such measurements are challenging to do in a lab-on-a-chip (LoC) system using a small volume of whole blood. Existing LoC systems use indirect measurement principles employing optical or electrochemical methods. We developed an LoC system using mechanical measurements with a small volume of whole blood without requiring sample preparation. The measurement is performed in a microfluidic channel where two fibers are placed inline with a small gap in between. The first fiber operates near its mechanical resonance using remote magnetic actuation and immersed in the sample. The second fiber is a pick-up fiber acting as an optical sensor. The microfluidic channel is engineered innovatively such that the blood does not block the gap between the vibrating fiber and the pick-up fiber, resulting in high signal-to-noise ratio optical output. The control plasma test results matched well with the plasma manufacturer's datasheet. Activated-partial-thromboplastin-time tests were successfully performed also with human whole blood samples, and the method is proven to be effective. Simplicity of the cartridge design and cost of readily available materials enable a low-cost point-of-care device for blood coagulation measurements. (2017) COPYRIGHT Society of Photo-Optical Instrumentation Engineers (SPIE).

Sugar microanalysis by HPLC with benzoylation: improvement via introduction of a C-8 cartridge and a high efficiency ODS column.

Science.gov (United States)

Miyagi, Michiko; Yokoyama, Hirokazu; Hibi, Toshifumi

2007-07-01

An HPLC protocol for sugar microanalysis based on the formation of ultraviolet-absorbing benzoyl chloride derivatives was improved. Here, samples were prepared with a C-8 cartridge and analyzed with a high efficiency ODS column, in which porous spherical silica particles 3 microm in diameter were packed. These devices allowed us to simultaneously quantify multiple sugars and sugar alcohols up to 10 ng/ml and to provide satisfactory separations of some sugars, such as fructose and myo-inositol and sorbitol and mannitol. This protocol, which does not require special apparatuses, should become a powerful tool in sugar research.

Integration of an Optical Ring Resonator Biosensor into a Self-Contained Microfluidic Cartridge with Active, Single-Shot Micropumps

Directory of Open Access Journals (Sweden)

Sascha Geidel

2016-09-01

Full Text Available While there have been huge advances in the field of biosensors during the last decade, their integration into a microfluidic environment avoiding external tubing and pumping is still neglected. Herein, we show a new microfluidic design that integrates multiple reservoirs for reagent storage and single-use electrochemical pumps for time-controlled delivery of the liquids. The cartridge has been tested and validated with a silicon nitride-based photonic biosensor incorporating multiple optical ring resonators as sensing elements and an immunoassay as a potential target application. Based on experimental results obtained with a demonstration model, subcomponents were designed and existing protocols were adapted. The newly-designed microfluidic cartridges and photonic sensors were separately characterized on a technical basis and performed well. Afterwards, the sensor was functionalized for a protein detection. The microfluidic cartridge was loaded with the necessary assay reagents. The integrated pumps were programmed to drive the single process steps of an immunoassay. The prototype worked selectively, but only with a low sensitivity. Further work must be carried out to optimize biofunctionalization of the optical ring resonators and to have a more suitable flow velocity progression to enhance the system’s reproducibility.

3D-Printed Paper Spray Ionization Cartridge with Integrated Desolvation Feature and Ion Optics

NARCIS (Netherlands)

Salentijn, G Ij; Oleschuk, R D; Verpoorte, E

2017-01-01

In this work we present the application of 3D-printing for the miniaturization and functionalization of an ion source for (portable) mass spectrometry (MS). Two versions of a 3D-printed cartridge for paper spray ionization (PSI) are demonstrated, assessed, and compared. We first focus on the use of

Hydrogen Car Cartridges: A New Strategy for Hydrogen Storage, Delivering and Refueling

Energy Technology Data Exchange (ETDEWEB)

Prosini, Pier Paolo

2007-07-01

The purpose of the project is to introduce a sustainable model in the automotive field, guarantying the Kyoto agreements. The aim of the project is to develop an innovative hydrogen tank able to power an hydrogen fuel cell car with the same performance of liquid fuelled cars. Most of the system performance are expected to satisfy the Department of Energy (DOE) goals for 2015. The hydrogen releasing system is based on solid NaBH4 which is hydrolyzed with water or steam to obtain hydrogen. Sodium borate is obtained as by-product and it has to be recycled. Pure and humidified hydrogen, ready to be utilized in a fuel cell, is obtained by a simple and sure way. Hydrogen is produced only when it is requested and therefore there is never pressurized hydrogen or hydrogen overproduction The system works at atmospheric pressure avoiding the problems related to handling and storing pressurized gas. The car fuelling could be performed in area like the present service stations. The used cartridges can be removed and substituted by new cartridges. Contemporarily a water tank should be refilled. To improve the total energetic yield it was also proposed a NaBH4 regeneration process directly starting from the products of hydrolysis. (auth)

Fluid Creep Effects on Near-Wall Solute Transport for Non-Isothermal Ampoules

Science.gov (United States)

Papadopoulos, Dimitrios; Rosner, Daniel E.

1996-01-01

There is a growing practical and theoretical interest in developing accurate macroscopic modelling for flows arising in chemical or physical vapor transport (VT) crystal growth experiments, including those conducted in reduced gravity environments. Rosner was the first person to point out that previously neglected rarefield gas dynamics phenomena (Stefan and bouyancy-driven flows) become rather important sources of convection. In particular, the combination of rarefaction and strong gradients of temperature (and/or concentration) tangential to the side-walls of the ampoule induces convective flows known as thermal (and concentration) 'creep' respectively. His order-of-magnitude estimates revealed that thermal creep effects can be non-negligible even at normal gravitational levels. On the macroscopic level, the bulk fluid mechanics can be adequately described by the familiar macroscopic equations as long as the boundary conditions are modified to account for the integrated effect of kinetic boundary layers adjacent to solid boundaries. Motivated by the growing importance of these phenomena, we have embarked on a series of computational studies to elucidate these fundamental creep-induced effects for a rarefied gas in simple, two-dimensional confined geometries. However, unlike previous related studies, we resort to a microscopic description of the gas, mathematically expressed by the Boltzmann integro-differential equation. We employ the direct simulation Monte Carlo (DSMC) method of Bird, the theoretical foundations and several practical applications. In the case of thermally induced flows, the no-time counter method of Bird is used, as implemented for a hard-sphere gas. The scheme has been also extended to account for realistic molecular interaction models, an extension necessary if the diffusion physics underlying concentration creep are to be captured.

Rapid monitoring particulate radiocesium with nonwoven fabric cartridge filter and application to field monitoring

International Nuclear Information System (INIS)

Tsuji, Hideki; Yasutaka, Tetsuo; Kondo, Yoshihiko; Kawashima, Shoji

2013-01-01

A method for rapid monitoring particulate radiocesium using a nonwoven fabric cartridge filter was developed, which needs no further preprocessing before served to a detector. By a performance test, more than 98% of suspended solid (SS) was collected. This method showed the same radioactivity measurement accuracy as filtration by membrane filter and more rapid extraction capability of SS. (author)

Development of SPE for recovery of polysaccharides and its application to the determination of monosaccharides composition of the polysaccharide sample of a lactobacillus KLB 58.

Science.gov (United States)

Baik, Yoon Suk; Cheong, Won Jo

2007-07-01

A new SPE cartridge has been prepared in this study to purify polysaccharides of high molecular weights. A porous nonpolar styrene-divinylbenzene copolymer phase (Hamilton PRP-1) was used to make the new cartridge. The cartridge was conditioned with methanol, water, and ACN in sequence, and the sample dissolved in a small amount of water was loaded. Impurities of low molecular weights were removed first by elution of 80:20 or 90:10 v/v% ACN/water, and polysaccharides were quantitatively recovered by elution of 50:50 v/v% ACN/water or pure water. The recovery of pure dextran 10000 was 90-95%. The SPE method was applied to purification of the polysaccharide sample of KLB58, a new lactobacillus discovered in Korea. The purified KLB 58 sample (weight recovery after SPE purification; 60%) was hydrolyzed for analysis of composition of monosaccharides. The hydrolysate was found to be composed primarily of fructose, glucose, galactose, rhamnose, mannose with small amounts of fucose and ribose.

The security management of spent filter cartridge in Qinshan phase 3 (heavy water reactor) nuclear power plant

International Nuclear Information System (INIS)

Xue Dahai

2005-01-01

Qinshan phase 3 nuclear power plant is the first CANDU plant that China fetched in from Canada, and both two units operate under well condition up to now. The radioactive wastes produced during the unit operation mainly include technical waste, spent resin, and spent filter cartridge. The spent filter cartridge is one important part both in the volume and radioactivity of the radioactive waste, and it is the important content of radioactive waste management. Different from PWR, part of high radioactive spent filter in CANDU unit comes from heavy water system such as moderator system. It has to be dried through blowing before replaced from the system. But this working procedure result the filtrate dreg become flexible, and it can bring on the risk of internal or external exposure. It is very important to pay high attention to control the contamination spread during spent filter inside transfer. (authors)

Forensic analysis of a smuggled HEU sample interdicted in Bulgaria

International Nuclear Information System (INIS)

Niemeyer, S.; Hutcheon, I.

2002-01-01

Full text: A sample of HEU was seized in Rousse, Bulgaria on May 29, 1999, at a border crossing between Bulgaria and Romania. A search of the suspect's vehicle uncovered a lead canister hidden in the car trunk. The initial examination of the contents by Bulgarian scientists indicated that the sample was indeed HEU, and subsequently arrangements were made for a U.S. team of nuclear forensics scientists from several national laboratories to conduct a thorough examination. This report gives a summary of the results. The HEU sample was contained in a glass ampoule that was embedded in a yellow wax, and in turn the wax filled the inside of the cylindrical lead container. A broad set of techniques was used to examine both nuclear and non-nuclear materials. Our general experimental approach has been previously described at meetings of the Nuclear Smuggling International Technical Working Group (ITWG), but this case represents the application of the most diverse set of nuclear forensic measurements for an actual seized sample. Analysis of the HEU itself included particle characterization, stoichiometry, impurity elements, residual nuclides, age-dating, and U and Pu isotopics. Measurements by XRD, SEM, and TEM show that sample is mostly U3O8, with minor amounts of two other phases. The powder is extremely fine-grained (160 nm mean) and quite uniform in size. Most grains (95%) are equidimensional, with the remainder rod-or plate-shaped. The U is 72.7% U-235 with a high U-236 abundance of 12.1%. The sample is reprocessed, reactor-irradiated material. The original U enrichment was 90% and the irradiation burned up about 50% of the initial U-235. Pu is present at a very low-level (3 ppb); the Pu-239 abundance is 82% with 240/239=0.12. Three fission products were detected at low levels, giving unambiguous evidence of fuel recycling. The total impurity content is about 600 ppmw (mostly S, Cl, Fe, and Br), which we interpret as indicating a batch processing operation because the

Characterization of filters cartridges from the water polishing system of IEA-R1 reactor: radiometric methods

International Nuclear Information System (INIS)

Tessaro, Ana Paula G.; Vicente, Roberto

2015-01-01

The acceptance of radioactive waste in a repository depends primarily on knowledge of the radioisotopic inventory of the material, according to regulations established by regulatory agencies. The primary characterization is also a fundamental action to determine further steps in the management of the radioactive wastes. The aim of this work is to report the development of non-destructive methods for primary characterization of filters cartridges discarded as radioactive waste. The filters cartridges are used in the water polishing system of the IEA-R1 reactor retaining the particles in suspension in the reactor cooling water. The IEA-R1 is a pool type reactor with a thermal power of 5 MW, moderated and cooled with light water. It is located in the Energy and Nuclear Research Institute (IPEN-CNEN), in São Paulo, Brazil. The cartridge filters become radioactive waste when they are saturated and do not meet the required flow for the proper operation of the water polishing system. The activities of gamma emitters present in the filters are determined using gamma spectrometry, dose rate measurements and the Point Kernel Method to correlate results from both measurements. For the primary characterization, one alternative method is the radiochemical analysis of slices taken from each filter, what presents the disadvantage of higher exposures personnel and contamination risks. Another alternative method is the calibration of the measurement geometry of a gamma spectrometer, which requires the production of a standard filter. Both methods are necessary but can not be used in operational routine of radioactive waste management owing to cost and complexity. The method described can be used to determine routinely the radioactive inventory of these filters and other radioactive wastes, avoiding the necessity of destructive radiochemical analysis, or the necessity of calibrating the geometry of measurement. (author)

Preparation and use of maize tassels' activated carbon for the adsorption of phenolic compounds in environmental waste water samples.

Science.gov (United States)

Olorundare, O F; Msagati, T A M; Krause, R W M; Okonkwo, J O; Mamba, B B

2015-04-01

The determination and remediation of three phenolic compounds bisphenol A (BPA), ortho-nitrophenol (o-NTP), parachlorophenol (PCP) in wastewater is reported. The analysis of these molecules in wastewater was done using gas chromatography (GC) × GC time-of-flight mass spectrometry while activated carbon derived from maize tassel was used as an adsorbent. During the experimental procedures, the effect of various parameters such as initial concentration, pH of sample solution, eluent volume, and sample volume on the removal efficiency with respect to the three phenolic compounds was studied. The results showed that maize tassel produced activated carbon (MTAC) cartridge packed solid-phase extraction (SPE) system was able to remove the phenolic compounds effectively (90.84-98.49%, 80.75-97.11%, and 78.27-97.08% for BPA, o-NTP, and PCP, respectively). The MTAC cartridge packed SPE sorbent performance was compared to commercially produced C18 SPE cartridges and found to be comparable. All the parameters investigated were found to have a notable influence on the adsorption efficiency of the phenolic compounds from wastewaters at different magnitudes.

Dielectric relaxation in glassy Se75In25−xPbx alloys

Indian Academy of Sciences (India)

to their atomic percentages and were sealed in quartz ampoules (length ~5 cm and internal dia. ~8 mm) in vacuum ... samples were taken out by breaking the quartz ampoules. The glassy nature of the ... measured with the help of a calibrated copper–constantan thermocouple mounted very near to the sample, which could ...

Analysis of mercury in environmental samples

International Nuclear Information System (INIS)

Schoester, F.S.

1992-01-01

The possibility to determine mercury in sub-ppm levels in biological samples has been studied through neutron activation analysis , using as standards aliquots of mercury nitrate solution, deposited on treated cellulose with thio acetamide and ammonia. Sample and standards were irradiated simultaneously in quartz ampoules during 8 hours at a flux of 5 x 10 13 n/cm 2 s and were counted in a hyper pure germanium detector after 4 weeks of decay. Corrections were made for the interference of 75 Se in the 279 keV photopeak used in the determination. The results obtained for the reference materials IAEA-H-8(horse kidney), IAEA-M A-A2(fish flesh) and IAEA-M A-A-1(cope pod homogenate) were (0.91±0.07), (0.56±0.02) and (0.17±0.02) ppm, versus certified values of (0.91±0.08), (0.47±0.02) and (0.28±0.01) ppm respectively. (EMR). 54 refs., 8 app

Double versus single cartridge of 4% articaine infiltration into the retro-molar area for lower third molar surgery.

Science.gov (United States)

Sawang, Kamonpun; Chaiyasamut, Teeranut; Kiattavornchareon, Sirichai; Pairuchvej, Verasak; Bhattarai, Bishwa Prakash; Wongsirichat, Natthamet

2017-06-01

There are no studies regarding 4% articaine infiltration injection into the retro-molar area for an impacted lower third molar (LITM) surgery. This study aimed to evaluate the efficacy of infiltration using 1.7 ml (single cartridge: SC) of 4% articaine versus 3.4 ml (double cartridges: DC) of 4% articaine with 1:100,000 epinephrine in LITM surgery. This study involved 30 healthy patients with symmetrical LITM. The patients were assigned to receive either a DC or SC of 4% articaine with 1:100,000 epinephrine as a local anesthetic for each operation. Onset, duration, profoundness, need for additional anesthetic administration, total volume of anesthetic used, vitality of the tooth, and pain score during operation were recorded. The DC of 4 % articaine had a significantly higher success rate (83.3%) than did the SC (53.3%; P molar region can be an alternative anesthetic for LITM surgery.

[Determination of metformin hydrochloride, melamine and dicyandiamide in metformin hydrochloride preparations by tandem dual solid phase extraction cartridges-high performance liquid chromatography-electrospray ionization multi-stage mass spectrometry].

Science.gov (United States)

Zhou, Yanfen; Wang, Fanghuan; Wang, Zelan; Zhan, Haijuan; Liu, Wanyi; Meng, Zhe

2018-02-08

A method for the confirmation and quantification of metformin hydrochloride and its relative substances melamine and dicyandiamide using tandem dual solid phase extraction (SPE) cartridges and high performance liquid chromatography-electrospray ionization multi-stage mass spectrometry (HPLC-ESI-MS n ) was developed. The samples were extracted with anhydrous ethanol containing 0.1% (v/v) acetic acid under ultrasound-assisted conditions. The extracts were concentrated and purified using Cleanert PCX and C18 tandem dual solid phase extraction cartridges, and eluted with 5% (v/v) ammonia methanol solution. The separation was performed on a Kromasil-C18 column (100 mm×4.6 mm, 3.5 μm) with gradient elution. The detection was performed in selected ion monitoring (SIM) mode using electrospray ionization multi-stage mass spectrometry. The external standard method was used for quantification. The extraction solvents, types of SPE cartridges and eluents were optimized by comparing the recoveries under different conditions. The results showed that the detector response of each target compound was linear in corresponding mass concentration ranges with the correlation coefficients ( r 2 ) ≥ 0.9992. The limits of detection (LODs) and the limits of quantification (LOQs) of the three analytes were 1.48-13.61 μg/kg and 5.96-45.67 μg/kg, respectively. The recoveries of the three analytes were 65.02%-118.33% spiked at low, medium and high levels. The relative standard deviations (RSDs) were no more than 13.41%. The method is reliable, easy, and has a better purification effect. The method can be applied to the routine analysis of metformin hydrochloride and its relative substances melamine and dicyandiamide in different preparations of metformin hydrochloride.

Sampling of tar from sewage sludge gasification using solid phase adsorption.

Science.gov (United States)

Ortiz González, Isabel; Pérez Pastor, Rosa Ma; Sánchez Hervás, José Ma

2012-06-01

Sewage sludge is a residue from wastewater treatment plants which is considered to be harmful to the environment and all living organisms. Gasification technology is a potential source of renewable energy that converts the sewage sludge into gases that can be used to generate energy or as raw material in chemical synthesis processes. But tar produced during gasification is one of the problems for the implementation of the gasification technology. Tar can condense on pipes and filters and may cause blockage and corrosion in the engines and turbines. Consequently, to minimize tar content in syngas, the ability to quantify tar levels in process streams is essential. The aim of this work was to develop an accurate tar sampling and analysis methodology using solid phase adsorption (SPA) in order to apply it to tar sampling from sewage sludge gasification gases. Four types of commercial SPA cartridges have been tested to determine the most suitable one for the sampling of individual tar compounds in such streams. Afterwards, the capacity, breakthrough volume and sample stability of the Supelclean™ ENVI-Carb/NH(2), which is identified as the most suitable, have been determined. Basically, no significant influences from water, H(2)S or NH(3) were detected. The cartridge was used in sampling real samples, and comparable results were obtained with the present and traditional methods.

Fast and Easy Drying Method for the Preparation of Activated [{sup 18}F]Fluoride Using Polymer Cartridge

Energy Technology Data Exchange (ETDEWEB)

Seo, Jai Woong [Inha University, Inchon (Korea, Republic of); Lee, Byoung Se; Chi, Dae Yoon [FutureChem Co., Ltd., Seoul (Korea, Republic of); Lee, Sang Ju [Sogang University, Seoul (Korea, Republic of); Oh, Seung Jun [Asan Medical Center, University of Ulsan College of Medicine, Seoul (Korea, Republic of)

2011-01-15

An efficient nucleophilic [{sup 18}F]fluorination has been studied to reduce byproducts and preparation time. Instead of conventional aqueous solution of K{sub 2}CO{sub 3}-K{sub 222}, several organic solution containing inert organic salts were used to release [{sup 18}F]fluoride ion and anion bases captured in the polymer cartridge, concluding that methanol solution is the best choice. Comparing to azeotropic drying process, one min was sufficient to remove methanol completely, resulting in about 10% radioactivity saving by reducing drying time. The polymer cartridge, Chromafix (PS-HCO{sub 3}) was pretreated with several anion bases to displace pre-loaded bicarbonate base. Phosphate bases showed better results than carbonate bases in terms of lower basicity. tert-Butanol solvent used as a reaction media played another critical role in nucleophilic [{sup 18}F]fluorination by suppressing eliminated side product. Consequent [{sup 18}F]fluorination under the present condition afforded fast preparation of reaction solution and high radiochemical yields (98% radio-TLC, 84% RCY) with 94% of precursor remained.

"1"4CO_2 processing using an improved and robust molecular sieve cartridge

International Nuclear Information System (INIS)

Wotte, Anja; Wordell-Dietrich, Patrick; Wacker, Lukas; Don, Axel; Rethemeyer, Janet

2017-01-01

Radiocarbon ("1"4C) analysis on CO_2 can provide valuable information on the carbon cycle as different carbon pools differ in their "1"4C signature. While fresh, biogenic carbon shows atmospheric "1"4C concentrations, fossil carbon is "1"4C free. As shown in previous studies, CO_2 can be collected for "1"4C analysis using molecular sieve cartridges (MSC). These devices have previously been made of plastic and glass, which can easily be damaged during transport. We thus constructed a robust MSC suitable for field application under tough conditions or in remote areas, which is entirely made of stainless steel. The new MSC should also be tight over several months to allow long sampling campaigns and transport times, which was proven by a one year storage test. The reliability of the "1"4CO_2 results obtained with the MSC was evaluated by detailed tests of different procedures to clean the molecular sieve (zeolite type 13X) and for the adsorption and desorption of CO_2 from the zeolite using a vacuum rig. We show that the "1"4CO_2 results are not affected by any contamination of modern or fossil origin, cross contamination from previous samples, and by carbon isotopic fractionation. In addition, we evaluated the direct CO_2 transfer from the MSC into the automatic graphitization equipment AGE with the subsequent "1"4C AMS analysis as graphite. This semi-automatic approach can be fully automated in the future, which would allow a high sample throughput. We obtained very promising, low blank values between 0.0018 and 0.0028 F"1"4C (equivalent to 50,800 and 47,200 yrs BP), which are within the analytical background and lower than results obtained in previous studies.

Rapid column extraction method for actinides and strontium in fish and other animal tissue samples

International Nuclear Information System (INIS)

Maxwell III, S.L.; Faison, D.M.

2008-01-01

The analysis of actinides and radiostrontium in animal tissue samples is very important for environmental monitoring. There is a need to measure actinide isotopes and strontium with very low detection limits in animal tissue samples, including fish, deer, hogs, beef and shellfish. A new, rapid separation method has been developed that allows the measurement of plutonium, neptunium, uranium, americium, curium and strontium isotopes in large animal tissue samples (100-200 g) with high chemical recoveries and effective removal of matrix interferences. This method uses stacked TEVA Resin R , TRU Resin R and DGA Resin R cartridges from Eichrom Technologies (Darien, IL, USA) that allows the rapid separation of plutonium (Pu), neptunium (Np), uranium (U), americium (Am), and curium (Cm) using a single multi-stage column combined with alphaspectrometry. Strontium is collected on Sr Resin R from Eichrom Technologies (Darien, IL, USA). After acid digestion and furnace heating of the animal tissue samples, the actinides and 89/90 Sr are separated using column extraction chromatography. This method has been shown to be effective over a wide range of animal tissue matrices. Vacuum box cartridge technology with rapid flow rates is used to minimize sample preparation time. (author)

Characterization of primary coolant purification system samples for assay of spent ion exchanger radionuclide inventor

International Nuclear Information System (INIS)

Sajin Prasad, S.; Pant, Amar; Sharma, Ranjit; Pal, Sanjit

2018-01-01

The primary coolant system water of a research reactor contains various fission and activation products and the water is circulated continuously through ion exchange resin cartridges, to reduce the radioactive ionic impurity present in it. The coolant purification system comprises of an ion exchange cooler, two micro filters, and a battery of six ion exchanger beds, associated valves, piping and instrumentation (Heavy water System Operating manual, 2014). The spent cartridge is finally disposed off as active solid waste which contains predominantly long lived fission and activation products. The heavy water coolant is also used to cool the structural assemblies after passing through primary heat exchanger and a metallic strainer, which accumulates the fission and activation products. When there is a reduction of coolant flow through these strainers, they are removed for cleaning and decontamination. This paper describes the characterization of ion exchange resin samples and liquid effluent generated during ultra sonic decontamination of strainer. The results obtained can be used as a methodology for the assay of the spent ion exchanger cartridges radionuclide inventory, during its disposal

Permanent disposal of radioactive particulate waste in cartridge containing ferromagnetic material

International Nuclear Information System (INIS)

Troy, M.

1986-01-01

This patent describes a cartridge for permanent disposal of solid radioactive particulate waste, comprising; a liquid impervious casing having an upper end cover, a lower end cover and a side wall extending between the covers, the casing enclosing a waste storage region; ferromagnetic fibrous material defining a waste retaining matrix and filling a major portion of the waste storage region; means defining an inlet conduit extending through the upper end cover and axially of the casing through the waste storage region, and opening into the waste storage region in the vicinity of the lower and end cover; and means defining first and second outlet conduits extending through the upper end cover and opening into the waste storage region in the vicinity of the upper end cover

Enhancement of the 1985 Browns Ferry exercise through the use of spiked samples

International Nuclear Information System (INIS)

McNees, J.L.

1987-01-01

The use of spiked environmental samples has proven to be a beneficial part of nuclear power plant exercises. Milk, soil, and air sampling cartridges can easily be spiked with realistic concentrations of radionuclide without violating Nuclear Regulatory Commission regulations or policy and with no significant radiation hazard to exercise participants. Analysis and reporting of data from realistic samples significantly improves motivation, attitude, moral, and overall preparedness of the individuals participating in that phase of the exercise

Analysis of {sup 210}Pb in water samples with plastic scintillation resins

Energy Technology Data Exchange (ETDEWEB)

Lluch, E.; Barrera, J. [Department of Analytical Chemistry, University of Barcelona, Martí i Franqués, 1-11, E-08028, Barcelona (Spain); Tarancón, A., E-mail: alex.tarancon@ub.edu [Department of Analytical Chemistry, University of Barcelona, Martí i Franqués, 1-11, E-08028, Barcelona (Spain); Bagán, H. [Department of Pure and Applied Biochemistry, Lund University, Getingevägen 60, Hus II, 22100 SE, Lund (Sweden); García, J.F. [Department of Analytical Chemistry, University of Barcelona, Martí i Franqués, 1-11, E-08028, Barcelona (Spain)

2016-10-12

{sup 210}Pb is a radioactive lead isotope present in the environment as member of the {sup 238}U decay chain. Since it is a relatively long-lived radionuclide (T{sub 1/2} = 22.2 years), its analysis is of interest in radiation protection and the geochronology of sediments and artwork. Here, we present a method for analysing {sup 210}Pb using plastic scintillation resins (PSresins) packaged in solid-phase extraction columns (SPE cartridge). The advantages of this method are its selectivity, the low limit of detection, as well as reductions in the amount of time and reagents required for analysis and the quantity of waste generated. The PSresins used in this study were composed of a selective extractant (4′,4″(5″)-Di-tert-butyldicyclohexano-18-crown-6 in 1-octanol) covering the surface of plastic scintillation microspheres. Once the amount of extractant (1:1/4) and medium of separation (2 M HNO{sub 3}) were optimised, PSresins in SPE cartridges were calibrated with a standard solution of {sup 210}Pb. {sup 210}Pb could be fully separated from its daughters, {sup 210}Bi and {sup 210}Po, with a recovery value of 91(3)% and detection efficiency of 44(3)%. Three spiked water samples (one underground and two river water samples) were analysed in triplicates with deviations lower than 10%, demonstrating the validity of the PS resin method for {sup 210}Pb analysis. - Highlights: • A plastic scintillation resin for selective analysis of {sup 210}Pb has been developed. • A commercial SPE cartridge has been use for separation and scintillation counting. • {sup 210}Pb separation from {sup 210}Bi and {sup 210}Po is achieved with a 91(3)% of recovery. • The method is valid for analysis of {sup 210}Pb in river water samples.

Comparison between a commercial solid-phase extraction cartridge and a home-made silver containing charcoal column: purification of Mo-99 from I-131 and Te-121

International Nuclear Information System (INIS)

Dias, Carla Roberta; Teodoro, Rodrigo; Osso Junior, Joao

2011-01-01

Among the radioisotopes used for medical application in Nuclear Medicine, 99m Tc, readily available from the elution of 99 Mo/ 99m Tc generators, is the most used, responsible for more than eighty percent of the total applications. These generators use the 99 Mo radioisotope that is produced in nuclear reactors and IPEN imports all the 99 Mo used in Brazil, mainly from Canada (Nordion). Due to the increasing needs of the Nuclear Medicine in Brazil and the world shortage of 99 Mo observed since 2008, IPEN decided to construct a new research reactor named Brazilian Multipurpose Reactor (BMR) as well as to develop the production of 99 Mo through the route of 235 U fission using a CINTICHEM modified separation process. The 99 Mo obtained from this process contains some contaminants and need to be purified. The aim of this work is to compare the preliminary results of the purification step of the solution containing 99 Mo and the contaminants, 131 I and 121 Te in the silver containing charcoal column and a solid-phase extraction cartridge. The purification process of 99 Mo coming from fission LEU foils was performed by adsorption chromatography using a home-made activated charcoal containing silver column (AC-Ag) and a commercial solid-phase extraction cartridge (OnGuard II Ag). High yields of 99 Mo elution and high retention of 131 I were achieved in the AC-Ag column and silver cartridge but 121 Te was more retained in the cartridge than in the AC-Ag column. (author)

Characterization of filter cartridges from the IEA-R1 reactor by radiochemical method

International Nuclear Information System (INIS)

Geraldo, Bianca; Vicente, Roberto; Ferreira, Robson J.; Goes, Marcos M.; Marumo, Julio T.

2015-01-01

The filter cartridges used in water purification system of research nuclear reactor IEA-R1 are considered radioactive wastes after their useful life. The characterization of these wastes is one of the stages of management, which aims to identify and quantify the radionuclides present, including those known as 'difficult to measure' (DTM) radionuclides. Establish a radiochemical analysis methodology for this type of waste is a difficult job, not only by the application of these techniques, but also by the amount of radionuclides that should be analyzed. In the waste produced in a nuclear reactor, the most important radionuclides are fission products, activation products and transuranic elements. Since these radionuclides emit gamma radiation not measurable in its decay process and consequently are difficult to measure, their concentrations can be estimated by indirect methods such as scale factors. This method is used to evaluate the DTM concentration, which is represented by alpha and beta nuclides using the correlation between them and the radionuclide key, a gamma emitter. The objective of this work is to describe a radiochemical analysis methodology for gamma emitter nuclides, present in the filter cartridges, evaluating the activity and concentrations by destructive assays. At the same time, two studies have been performed by non-destructive assays, the first one based on dose rates and the point kernel method to correlate the results and the second one based on calibration efficiency with Monte Carlo method. These studies belong to the radioactive waste characterization program that has been conducted at the Waste Management Laboratory of Nuclear and Energy Research Institute, IPEN-CNEN/SP. (author)

Characterization of filter cartridges from the IEA-R1 reactor by radiochemical method

Energy Technology Data Exchange (ETDEWEB)

Geraldo, Bianca; Vicente, Roberto; Ferreira, Robson J.; Goes, Marcos M.; Marumo, Julio T., E-mail: bgeraldo@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

2015-07-01

The filter cartridges used in water purification system of research nuclear reactor IEA-R1 are considered radioactive wastes after their useful life. The characterization of these wastes is one of the stages of management, which aims to identify and quantify the radionuclides present, including those known as 'difficult to measure' (DTM) radionuclides. Establish a radiochemical analysis methodology for this type of waste is a difficult job, not only by the application of these techniques, but also by the amount of radionuclides that should be analyzed. In the waste produced in a nuclear reactor, the most important radionuclides are fission products, activation products and transuranic elements. Since these radionuclides emit gamma radiation not measurable in its decay process and consequently are difficult to measure, their concentrations can be estimated by indirect methods such as scale factors. This method is used to evaluate the DTM concentration, which is represented by alpha and beta nuclides using the correlation between them and the radionuclide key, a gamma emitter. The objective of this work is to describe a radiochemical analysis methodology for gamma emitter nuclides, present in the filter cartridges, evaluating the activity and concentrations by destructive assays. At the same time, two studies have been performed by non-destructive assays, the first one based on dose rates and the point kernel method to correlate the results and the second one based on calibration efficiency with Monte Carlo method. These studies belong to the radioactive waste characterization program that has been conducted at the Waste Management Laboratory of Nuclear and Energy Research Institute, IPEN-CNEN/SP. (author)

{sup 14}CO{sub 2} processing using an improved and robust molecular sieve cartridge

Energy Technology Data Exchange (ETDEWEB)

Wotte, Anja, E-mail: Anja.Wotte@uni-koeln.de [Institute of Geology and Mineralogy, University of Cologne, Cologne (Germany); Wordell-Dietrich, Patrick [Thünen Institute of Climate-Smart Agriculture, Braunschweig (Germany); Wacker, Lukas [Ion Beam Physics, ETH Zurich, Zurich (Switzerland); Don, Axel [Thünen Institute of Climate-Smart Agriculture, Braunschweig (Germany); Rethemeyer, Janet [Institute of Geology and Mineralogy, University of Cologne, Cologne (Germany)

2017-06-01

Radiocarbon ({sup 14}C) analysis on CO{sub 2} can provide valuable information on the carbon cycle as different carbon pools differ in their {sup 14}C signature. While fresh, biogenic carbon shows atmospheric {sup 14}C concentrations, fossil carbon is {sup 14}C free. As shown in previous studies, CO{sub 2} can be collected for {sup 14}C analysis using molecular sieve cartridges (MSC). These devices have previously been made of plastic and glass, which can easily be damaged during transport. We thus constructed a robust MSC suitable for field application under tough conditions or in remote areas, which is entirely made of stainless steel. The new MSC should also be tight over several months to allow long sampling campaigns and transport times, which was proven by a one year storage test. The reliability of the {sup 14}CO{sub 2} results obtained with the MSC was evaluated by detailed tests of different procedures to clean the molecular sieve (zeolite type 13X) and for the adsorption and desorption of CO{sub 2} from the zeolite using a vacuum rig. We show that the {sup 14}CO{sub 2} results are not affected by any contamination of modern or fossil origin, cross contamination from previous samples, and by carbon isotopic fractionation. In addition, we evaluated the direct CO{sub 2} transfer from the MSC into the automatic graphitization equipment AGE with the subsequent {sup 14}C AMS analysis as graphite. This semi-automatic approach can be fully automated in the future, which would allow a high sample throughput. We obtained very promising, low blank values between 0.0018 and 0.0028 F{sup 14}C (equivalent to 50,800 and 47,200 yrs BP), which are within the analytical background and lower than results obtained in previous studies.

Ways of increasing of efficiency of the use of chemical gazogene cartridges at the mining of facing raw material

OpenAIRE

Кальчук, Сергій Володимирович; Лукащук, Олександр Вікторович

2016-01-01

The analysis and theoretical generalizations of influencing of the known methods of separation to the stone on the array of breeds is executed. Certain backlogs of increase of the OIR use of chemical gazogene cartridges. Offered ways of determination of optimum parameters of most effective their applications on the deposits of facing stone.

Towards a Mobile Ecogenomic sensor: the Third Generation Environmental Sample Processor (3G-ESP).

Science.gov (United States)

Birch, J. M.; Pargett, D.; Jensen, S.; Roman, B.; Preston, C. M.; Ussler, W.; Yamahara, K.; Marin, R., III; Hobson, B.; Zhang, Y.; Ryan, J. P.; Scholin, C. A.

2016-02-01

Researchers are increasingly using one or more autonomous platforms to characterize ocean processes that change in both space and time. Conceptually, studying processes that change quickly both spatially and temporally seems relatively straightforward. One needs to sample in many locations synoptically over time, or follow a coherent water mass and sample it repeatedly. However, implementing either approach presents many challenges. For example, acquiring samples over days to weeks far from shore, without human intervention, requires multiple systems to work together seamlessly, and the level of autonomy, navigation and communications needed to conduct the work exposes the complexity of these requirements. We are addressing these challenges by developing a new generation of robotic systems that are primarily aimed at studies of microbial-mediated processes. As a step towards realizing this new capability, we have taken lessons learned from our second-generation Environmental Sample Processor (2G-ESP), a robotic microbiology "lab-in-a-can" and have re-engineered the system for use on a Tethys-class Long Range AUV (LRAUV). The new instrument is called the third-generation ESP (3G-ESP), and its integration with the LRAUV provides mobility and a persistent presence not seen before in microbial oceanography. The 3G-ESP autonomously filters a water sample and then either preserves that material for eventual return to a laboratory, or processes the sample in real-time for further downstream molecular analytical analyses. The 3G ESP modularizes hardware needed for the collection and preparation of a sample from subsequent molecular analyses by the use of self-contained "cartridges". Cartridges currently come in two forms: one for the preservation of a sample, and the other for onboard homogenization and handoff for downstream processing via one or more analytical devices. The 3G-ESP is designed as a stand-alone instrument, and thus could be deployed on a variety of

Direct preparation of a graphene oxide modified monolith in a glass syringe as a solid-phase extraction cartridge for the extraction of quaternary ammonium alkaloids from Chinese patent medicine.

Science.gov (United States)

Liang, Xiaojing; Wang, Licheng; Wang, Shuai; Li, Yijing; Guo, Yong

2017-11-01

Packed cartridges have been widely used in solid-phase extraction. However, there are still some drawbacks, such as they are blocked easily and the method is time-consuming. In view of the advantages of monoliths, a monolithic extraction material has been directly synthesized in a glass syringe without any gap between the monolith and syringe inner wall. The monolithic syringe was modified with graphene oxide by loading graphene oxide dispersion onto it. The content of graphene oxide and the surface topography of the monolith have been evaluated by elemental analysis and scanning electron microscopy, respectively, which confirmed the successful modification. This prepared graphene oxide-modified monolithic syringe was directly used as a traditional solid-phase extraction cartridge. As expected, it shows good permeability and excellent capability for the extraction of quaternary ammonium alkaloids. The sample loading velocity (1-6 mL/min) does not affect the recovery. Under the optimal conditions, good linearities (R = 0.9992-0.9998) were obtained for five quaternary ammonium alkaloids, and the limits of detection and quantification were 0.5-1 and 1-2 μg/L, respectively. The proposed method was successfully applied for the analysis of quaternary ammonium alkaloids in Chinese patent medicine. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Observation of Meyer–Neldel rule in thermally activated Poole ...

Indian Academy of Sciences (India)

to their atomic percentages and were sealed in a quartz ampoule (length ~5 cm and internal dia. ~8 mm) in a ... The quenched sample was taken out by breaking the quartz ampoules. The glassy nature of the ... and the temperature measured by a calibrated copper–constantan thermocouple mounted very near to the films.

Domestic Preparedness: Phase 2 Sarin Vapor Challenge and Corn Oil Protection Factor (PF) Testing of Commercial Powered Air Purifying Respirator (PAPR) Systems and Cartridges

National Research Council Canada - National Science Library

Campbell, Lee E; Lins, Ray; Pappas, Alex G

2002-01-01

.... Results indicate that cartridges provide complete penetration resistance against 200 mg/m3 GB challenge concentrations for 60 minutes, but that unacceptably high levels of GB vapor and corn oil...

Simultaneous determination of paracetamol, 4-Aminophenol, 4-Chloroacetanilid, Benzyl alcohol,Benzaldehyde and EDTA by HPLC methodin paracetamol injection ampoule

Directory of Open Access Journals (Sweden)

Ali Merrikhi Khosroshahi

2016-06-01

Full Text Available Paracetamol that is known as acetaminophen have the most consume as an analgesic and antipyretic drug in the world. That is formulated in single compound or mixture at many forms such as tablets, syrups, suspensions and drops. The last form is intravenous injections. Paracetamol derived from 4-minophenol which is synthesized by acylated the P-acetaminophenol and acetic anhydride. 4-aminophenol is the main impurity at manufacturing of paracetamol which could produce by hydrolysis during storage or synthesis under normal conditions (temperature, pH, etc.. Also, 4-chloroacetanilid may be observed as an impurity in the raw material of paracetamol synthesis. Benzyl alcohol is a preservative that used in Paracetamol for injection. It will be very important if there are analytical techniques to measuring paracetamol and its degradation products accurately and easily. Undoubtedly the most important and widely used, separation technique is chromatography. There are several reports about separation and quantitative determination of paracetamol lonely or simultaneous determination of paracetamol and 4-aminophenol. In this paper investigated simultaneous determination of paracetamol, 4-aminophenol, 4-chloroacetanilid, benzyl alcohol, benzaldehyde, and EDTA in paracetamol for injection ampoules by high performance liquid chromatography. By changing the ratio of mixing methanol and acetonitrile as mobile phase at the wavelength of 215 nm and pH=3 separation of all compounds were completely done.

Minimization of the blank values in the neutron activation analysis of biological samples considering the whole procedure

International Nuclear Information System (INIS)

Lux, F.; Bereznai, T.; Trebert Haeberlin, S.

1987-01-01

During the determination of trace element contents of animal tissue by neutron activation analysis in the course of structure-activity relationship studies on platinum containing cancer drugs and wound healing the authors tried to minimize the blank values that are caused by different sources of contamination during surgery, sampling and the activation analysis procedure. The following topics were investigated: abrasions from scalpels made of stainless steel, titanium or quartz, the type of surgery, the surface contaminations of the quartz ampoules, etc. The measures to be taken to reduce tha blank values are described. (author) 19 refs.; 4 tables

Temperature measurement of the reactor materials samples irradiated in the fuel channels of the RA reactor - Annex 16

International Nuclear Information System (INIS)

Nikolic, M.; Djalovic, M.

1964-01-01

Reactor materials as graphite, stainless steel, magnox, zirconium alloys, etc. were exposed to fast neutron flux inside the fuel elements specially adapted for this purpose. Samples in the form ampoules were placed in capsules inside the fuel channels and cooled by heavy water which cools the fuel elements. In order to monitor the samples temperature 42 thermocouples were placed in the samples. That was necessary for reactor safety reasons and for further interpretation of measured results. Temperature monitoring was done continuously by multichannel milivoltmeters. This paper describes the technique of introducing the thermocouples, compensation instruments, control of the cold ends and adaptation of the instruments for precision (0.5%) temperature measurement in the range 30 deg - 130 deg C; 30 deg - 280 deg C and 30 deg - 80 deg C [sr

Thermal enhancement cartridge heater modified (TECH Mod) tritium hydride bed development, Part 1 - Design and fabrication

Energy Technology Data Exchange (ETDEWEB)

Klein, J.E.; Estochen, E.G. [Savannah River National Laboratory, Aiken, SC (United States)

2015-03-15

The Savannah River Site (SRS) tritium facilities have used first generation (Gen1) LaNi{sub 4.25}Al{sub 0.75} (LANA0.75) metal hydride storage beds for tritium absorption, storage, and desorption. The Gen1 design utilizes hot and cold nitrogen supplies to thermally cycle these beds. Second and third generation (Gen2 and Gen3) storage bed designs include heat conducting foam and divider plates to spatially fix the hydride within the bed. For thermal cycling, the Gen2 and Gen3 beds utilize internal electric heaters and glovebox atmosphere flow over the bed inside the bed external jacket for cooling. The currently installed Gen1 beds require replacement due to tritium aging effects on the LANA0.75 material, and cannot be replaced with Gen2 or Gen3 beds due to different designs of these beds. At the end of service life, Gen1 bed desorption efficiencies are limited by the upper temperature of hot nitrogen supply. To increase end-of-life desorption efficiency, the Gen1 bed design was modified, and a Thermal Enhancement Cartridge Heater Modified (TECH Mod) bed was developed. Internal electric cartridge heaters in the new design to improve end-of-life desorption, and also permit in-bed tritium accountability (IBA) calibration measurements to be made without the use of process tritium. Additional enhancements implemented into the TECH Mod design are also discussed. (authors)

Minimization of the blank values in the neutron activation analysis of biological samples considering the whole procedure

International Nuclear Information System (INIS)

Lux, F.; Bereznai, T.; Haeberlin, T.H.

1986-01-01

In our determination of trace element contents of animal tissue by neutron activation analysis in the course of structure-activity relationship studies on platinum containing cancer drugs and wound healing we have tried to minimize the blank values that are caused by different sources of contamination during surgery, sampling and the activation analysis procedure. The following topics have been investigated: the abrasions from scalpels made of stainless steel, titanium or quartz; the type of surgery; the homogenisation of the samples before irradiation by use of a ball milll; the surface contaminations of the quartz ampoules that pass into the digestion solution of the irradiated samples. The appropriate measures taken in order to reduce the blank values are described. The results of analyses performed under these conditions indicate the effectiveness of the given measures, especially shown by the low values obtained for the chromium contents of the analysed muscle samples. (author)

Measurement of stable isotope ratio of organic carbon in water samples

International Nuclear Information System (INIS)

Fujii, Toshihiro; Otsuki, Akira

1977-01-01

A new method for the measurement of stable isotope ratios was investigated and applied to organic carbon's isotope ratio measurements in water samples. A few river water samples from Tsuchiura city were tested. After the wet oxidation of organic carbons to carbon dioxide in a sealed ampoule, the isotope ratios were determined with the gas chromatograph-quadrupole mass spectrometer combined with a total organic carbon analyser, under the dynamic conditions. The GC-MS had been equipped with the multiple ion detector-digital integrator system. The ion intensities at m/e 44 and 45 were simultaneously measured at a switching rate of 1 ms. The measurements with carbon dioxide acquired from sodium carbonate (53 μg) gave the isotope ratios with the variation coefficient of 0.62%. However, the variation coefficients obtained from organic carbons in natural water samples were 2 to 3 times as high as that from sodium carbonate. This method is simple and rapid and may be applied to various fields especially in biology and medicine. (auth.)

Determining the effect of cartridge case coatings on GSR using post-fire priming cup residue.

Science.gov (United States)

Terry, Molly; Fookes, Barry; Bridge, Candice M

2017-07-01

Ammunition is typically composed of a lead-based priming mixture which contributes to the characteristics most commonly used for the identification of gunshot residue (GSR). Due to the health risks often associated with lead, the use of lead-free primers in ammunitions is becoming more popular. Thus, the presence of GSR is becoming more difficult to discern based on the traditional means, i.e. the presence of lead (Pb), barium (Ba), and antimony (Sb). While research has been conducted on the differences between lead-based and lead-free muzzle discharge residue, few have researched other components of ammunition which may lead to other means of characterizing GSR. This research, therefore, covers that gap by focusing on the priming cup present in ammunition and the residue which may originate from it, that can contribute to muzzle discharge residue. In this study, a lead-based and a lead-free ammunition from four different manufacturers were chosen. The cartridges were fired using a Glock 17, 9mm Parabellum, collected post-fire, and subsequently de-primed resulting in the removal of the anvil. The GSR present on the anvils and cups was analyzed using scanning electron microscopy coupled with energy dispersive x-ray spectrometry (SEM-EDX). The data was then processed using unit vector analysis for normalization and analyzed using principal component analysis (PCA) and linear discriminant analysis (LDA). This data was then used to determine the components of the cartridge case which contribute to GSR and develop a method of characterization between lead-free and lead-based ammunition. Such a method will improve the detection of GSR by strengthening the criteria of identification. Copyright © 2017 Elsevier B.V. All rights reserved.

Recent advances in column switching sample preparation in bioanalysis.

Science.gov (United States)

Kataoka, Hiroyuki; Saito, Keita

2012-04-01

Column switching techniques, using two or more stationary phase columns, are useful for trace enrichment and online automated sample preparation. Target fractions from the first column are transferred online to a second column with different properties for further separation. Column switching techniques can be used to determine the analytes in a complex matrix by direct sample injection or by simple sample treatment. Online column switching sample preparation is usually performed in combination with HPLC or capillary electrophoresis. SPE or turbulent flow chromatography using a cartridge column and in-tube solid-phase microextraction using a capillary column have been developed for convenient column switching sample preparation. Furthermore, various micro-/nano-sample preparation devices using new polymer-coating materials have been developed to improve extraction efficiency. This review describes current developments and future trends in novel column switching sample preparation in bioanalysis, focusing on innovative column switching techniques using new extraction devices and materials.

A Modified Electrostatic Adsorption Apparatus for Latent Fingerprint Development on Unfired Cartridge Cases.

Science.gov (United States)

Xu, Jingyang; Zhang, Ziyuan; Zheng, Xiaochun; Bond, John W

2017-05-01

Visualization of latent fingerprints on metallic surfaces by the method of applying electrostatic charging and adsorption is considered as a promising chemical-free method, which has the merit of nondestruction, and is considered to be effective for some difficult situations such as aged fingerprint deposits or those exposed to environmental extremes. In fact, a portable electrostatic generator can be easily accessible in a local forensic technology laboratory, which is already widely used in the visualization of footwear impressions. In this study, a modified version of this electrostatic apparatus is proposed for latent fingerprint development and has shown great potential in visualizing fingerprints on metallic surfaces such as cartridge cases. Results indicate that this experimental arrangement can successfully develop aged latent fingerprints on metal surfaces, and we demonstrate its effectiveness compared with existing conventional fingerprint recovery methods. © 2016 American Academy of Forensic Sciences.

Intelligent front-end sample preparation tool using acoustic streaming.

Energy Technology Data Exchange (ETDEWEB)

Cooley, Erika J.; McClain, Jaime L.; Murton, Jaclyn K.; Edwards, Thayne L.; Achyuthan, Komandoor E.; Branch, Darren W.; Clem, Paul Gilbert; Anderson, John Mueller; James, Conrad D.; Smith, Gennifer; Kotulski, Joseph Daniel

2009-09-01

We have successfully developed a nucleic acid extraction system based on a microacoustic lysis array coupled to an integrated nucleic acid extraction system all on a single cartridge. The microacoustic lysing array is based on 36{sup o} Y cut lithium niobate, which couples bulk acoustic waves (BAW) into the microchannels. The microchannels were fabricated using Mylar laminates and fused silica to form acoustic-fluidic interface cartridges. The transducer array consists of four active elements directed for cell lysis and one optional BAW element for mixing on the cartridge. The lysis system was modeled using one dimensional (1D) transmission line and two dimensional (2D) FEM models. For input powers required to lyse cells, the flow rate dictated the temperature change across the lysing region. From the computational models, a flow rate of 10 {micro}L/min produced a temperature rise of 23.2 C and only 6.7 C when flowing at 60 {micro}L/min. The measured temperature changes were 5 C less than the model. The computational models also permitted optimization of the acoustic coupling to the microchannel region and revealed the potential impact of thermal effects if not controlled. Using E. coli, we achieved a lysing efficacy of 49.9 {+-} 29.92 % based on a cell viability assay with a 757.2 % increase in ATP release within 20 seconds of acoustic exposure. A bench-top lysing system required 15-20 minutes operating up to 58 Watts to achieve the same level of cell lysis. We demonstrate that active mixing on the cartridge was critical to maximize binding and release of nucleic acid to the magnetic beads. Using a sol-gel silica bead matrix filled microchannel the extraction efficacy was 40%. The cartridge based magnetic bead system had an extraction efficiency of 19.2%. For an electric field based method that used Nafion films, a nucleic acid extraction efficiency of 66.3 % was achieved at 6 volts DC. For the flow rates we tested (10-50 {micro}L/min), the nucleic acid extraction

A faster sample preparation method for determination of polonium-210 in fish

International Nuclear Information System (INIS)

Sadi, B.B.; Jing Chen; Kochermin, Vera; Godwin Tung; Sorina Chiorean

2016-01-01

In order to facilitate Health Canada’s study on background radiation levels in country foods, an in-house radio-analytical method has been developed for determination of polonium-210 ( 210 Po) in fish samples. The method was validated by measurement of 210 Po in a certified reference material. It was also evaluated by comparing 210 Po concentrations in a number of fish samples by another method. The in-house method offers faster sample dissolution using an automated digestion system compared to currently used wet-ashing on a hot plate. It also utilizes pre-packed Sr-resin® cartridges for rapid and reproducible separation of 210 Po versus time-consuming manually packed Sr-resin® columns. (author)

Evaluating the effect of sample type on American alligator (Alligator mississippiensis) analyte values in a point-of-care blood analyser.

Science.gov (United States)

Hamilton, Matthew T; Finger, John W; Winzeler, Megan E; Tuberville, Tracey D

2016-01-01

The assessment of wildlife health has been enhanced by the ability of point-of-care (POC) blood analysers to provide biochemical analyses of non-domesticated animals in the field. However, environmental limitations (e.g. temperature, atmospheric humidity and rain) and lack of reference values may inhibit researchers from using such a device with certain wildlife species. Evaluating the use of alternative sample types, such as plasma, in a POC device may afford researchers the opportunity to delay sample analysis and the ability to use banked samples. In this study, we examined fresh whole blood, fresh plasma and frozen plasma (sample type) pH, partial pressure of carbon dioxide (PCO2), bicarbonate (HCO3 (-)), total carbon dioxide (TCO2), base excess (BE), partial pressure of oxygen (PO2), oxygen saturation (sO2) and lactate concentrations in 23 juvenile American alligators (Alligator mississippiensis) using an i-STAT CG4+ cartridge. Our results indicate that sample type had no effect on lactate concentration values (F 2,65 = 0.37, P = 0.963), suggesting that the i-STAT analyser can be used reliably to quantify lactate concentrations in fresh and frozen plasma samples. In contrast, the other seven blood parameters measured by the CG4+ cartridge were significantly affected by sample type. Lastly, we were able to collect blood samples from all alligators within 2 min of capture to establish preliminary reference ranges for juvenile alligators based on values obtained using fresh whole blood.

Thermal enhancement cartridge heater modified tritium hydride bed development, Part 2 - Experimental validation of key conceptual design features

Energy Technology Data Exchange (ETDEWEB)

Heroux, K.J.; Morgan, G.A. [Savannah River Laboratory, Aiken, SC (United States)

2015-03-15

The Thermal Enhancement Cartridge Heater Modified (TECH Mod) tritium hydride bed is an interim replacement for the first generation (Gen1) process hydride beds currently in service in the Savannah River Site (SRS) Tritium Facilities. 3 new features are implemented in the TECH Mod hydride bed prototype: internal electric cartridge heaters, porous divider plates, and copper foam discs. These modifications will enhance bed performance and reduce costs by improving bed activation and installation processes, in-bed accountability measurements, end-of-life bed removal, and He-3 recovery. A full-scale hydride bed test station was constructed at the Savannah River National Laboratory (SRNL) in order to evaluate the performance of the prototype TECH Mod hydride bed. Controlled hydrogen (H{sub 2}) absorption/ desorption experiments were conducted to validate that the conceptual design changes have no adverse effects on the gas transfer kinetics or H{sub 2} storage/release properties compared to those of the Gen1 bed. Inert gas expansions before, during, and after H{sub 2} flow tests were used to monitor changes in gas transfer rates with repeated hydriding/de-hydriding of the hydride material. The gas flow rates significantly decreased after initial hydriding of the material; however, minimal changes were observed after repeated cycling. The data presented herein confirm that the TECH Mod hydride bed would be a suitable replacement for the Gen1 bed with the added enhancements expected from the advanced design features. (authors)

Rapid purification of radioiodinated peptides with Sep-Pak reversed phase cartridges and HPLC

International Nuclear Information System (INIS)

Miller, J.J.; Schultz, G.S.; Levy, R.S.

1984-01-01

A simple, rapid method is described for the purification of radioiodinated peptides for use in radioimmuno- and in radioreceptor assays. Iodinated reaction mixtures are applied directly onto Sep-Pak disposable, reversed phase cartridges equilibrated with phosphate buffer. Unreacted 125-iodide and other non-peptide reaction components are eluted with buffer. The peptide fraction is then eluted with 70% buffer:30% acetonitrile. The peptide fraction is further purified by reversed phase high pressure liquid chromatography to separate the native peptide and the mono- and diiodo-derivatives. In this study the method is used to prepare 125-iodide-labeled monoiodo-leucine enkephalin and monoiodo-angiotensin II, which are free of the parent peptides and diiodo-derivatives and are of maximum obtainable specific radioactivity. The usefulness of these labeled peptides in radioimmuno- and radioreceptor assays is demonstrated by their binding to specific antibodies and receptors, respectively. (author)

A new screening method for amphetamine and methamphetamine using dansyl chloride derivatization and cartridge fluorescence.

Science.gov (United States)

Yamada, H; Ikeda-Wada, S; Oguri, K

1998-07-01

A new screening method for amphetamines was developed. It consists of derivatization with dansyl chloride, extraction of the derivative using a Sep-Pak C18 or a Bond Elut C18, solid phase extraction columns, and visualization of the fluorescence of the cartridge. A control test using drug-free urine showed no fluorescence. Amphetamine, methamphetamine and the methylenedioxy derivatives exhibited strong fluorescence, while related compounds, such as N-ethylamphetamine and fenetylline, were negative or weakly positive. The disadvantage of the present method is that it is a multi-step procedure and 20-30 min is required for screening. However, since it has a different specificity from the widely used immunochemical technique, it is suggested to be a useful screen for amphetamines.

Polyethylene (PE) based proton exchange membrane for use in fuel cell

International Nuclear Information System (INIS)

Moraes, Gilberto de Oliveira

2008-01-01

The irradiation - induced graft of styrene onto polyethylene (PE) in a Cobalt-60 source was carried out using direct (simultaneous) and indirect (preirradiation and peroxidation) methods at room temperature. The dose applied in both cases varied from 0,5 to 80 kGy; In the direct method, the films were immersed in a solution of styrene: methanol (30:70 v/v) and 30% of sulfuric acid(additive) in glass ampoules of 40 ml under inert atmosphere, and then irradiated. After irradiation process, the samples were kept in solution for 8 hours and taken off the ampoules, dried in oven at 60 deg C for another 8 hour period until constant weight. In pre-irradiation method, the samples were irradiated in dry and sealed ampoules, under inert atmosphere. The solution was then added to the samples, and after 8 hours, taken off, dried, sealed and weighted. In peroxidation method, the difference was not inert atmosphere but atmosphere of air (0 2 ).For each samples it was calculated the degree of grafting (DOG). The samples that showed some DOG were sulfonated, characterized (DSC, TGA and infrared) and the ion exchange capacity (IEC) was calculated. The samples processed by indirect method presented no DOG at all. The samples processed by direct method present grafting (best result was 80 kGy). These samples, after sulfonated, presented ion exchange properties. (author)

Development of solid materials for UF₆ sampling: FY16 Annual Report

Energy Technology Data Exchange (ETDEWEB)

Smith, Nicholas [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Savina, Joseph [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Hebden, Andrew [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division

2016-10-31

A handheld implementation of the ABACC-developed Cristallini method, which captures uranium hexafluoride samples as an inert salt, was organized in FY17 and succeeded in demonstrating the handheld sampler concept with reactive hexafluoride gases. The Cristallini method relies on the use of a hydrated substrate to react the incoming hexafluoride resulting in the formation of a stable uranyl fluoride salt. The Cristallini method has been demonstrated as a facility modification installed near the sampling tap of a gas centrifuge enrichment plant. While very successful in reducing the hazards of uranium hexafluoride sample, the method still takes a considerable amount of time and can only be used in facilities where the apparatus has been installed; this arrangement generally prohibits the sampling of filled cylinders that have already exited the facility and have been deposited in the on-site tank storage yard. The handheld unit under development will allow the use of the Cristallini method at facilities that have not been converted as well as tanks in the storage yard. The handheld system utilizes an active vacuum system, rather than a passive vacuum system in the facility setup, to drive the uranium hexafluoride onto the adsorbing media. The handheld unit will be battery operated for fully autonomous operation and will include onboard pressure sensing and flushing capability. To date, the system concept of operations was demonstrated with tungsten hexafluoride that showed the active vacuum pump with multiple cartridges of adsorbing media was viable. Concurrently, the hardened prototype system was developed and tested; removable sample cartridges were developed (the only non-COTS component to date); and preparations were made for uranium tests and a domestic field test.

Rapid and simple detection of foot-and-mouth disease virus: Evaluation of a cartridge-based molecular detection system for use in basic laboratories.

Science.gov (United States)

Goller, K V; Dill, V; Madi, M; Martin, P; Van der Stede, Y; Vandenberge, V; Haas, B; Van Borm, S; Koenen, F; Kasanga, C J; Ndusilo, N; Beer, M; Liu, L; Mioulet, V; Armson, B; King, D P; Fowler, V L

2018-04-01

Highly contagious transboundary animal diseases such as foot-and-mouth disease (FMD) are major threats to the productivity of farm animals. To limit the impact of outbreaks and to take efficient steps towards a timely control and eradication of the disease, rapid and reliable diagnostic systems are of utmost importance. Confirmatory diagnostic assays are typically performed by experienced operators in specialized laboratories, and access to this capability is often limited in the developing countries with the highest disease burden. Advances in molecular technologies allow implementation of modern and reliable techniques for quick and simple pathogen detection either in basic laboratories or even at the pen-side. Here, we report on a study to evaluate a fully automated cartridge-based real-time RT-PCR diagnostic system (Enigma MiniLab ® ) for the detection of FMD virus (FMDV). The modular system integrates both nucleic acid extraction and downstream real-time RT-PCR (rRT-PCR). The analytical sensitivity of this assay was determined using serially diluted culture grown FMDV, and the performance of the assay was evaluated using a selected range of FMDV positive and negative clinical samples of bovine, porcine and ovine origin. The robustness of the assay was evaluated in an international inter-laboratory proficiency test and by deployment into an African laboratory. It was demonstrated that the system is easy to use and can detect FMDV with high sensitivity and specificity, roughly on par with standard laboratory methods. This cartridge-based automated real-time RT-PCR system for the detection of FMDV represents a reliable and easy to use diagnostic tool for the early and rapid disease detection of acutely infected animals even in remote areas. This type of system could be easily deployed for routine surveillance within endemic regions such as Africa or could alternatively be used in the developed world. © 2017 The Authors. Transboundary and Emerging Diseases

Simultaneous analysis of multiple classes of antimicrobials in environmental water samples using SPE coupled with UHPLC-ESI-MS/MS and isotope dilution.

Science.gov (United States)

Tran, Ngoc Han; Chen, Hongjie; Do, Thanh Van; Reinhard, Martin; Ngo, Huu Hao; He, Yiliang; Gin, Karina Yew-Hoong

2016-10-01

A robust and sensitive analytical method was developed for the simultaneous analysis of 21 target antimicrobials in different environmental water samples. Both single SPE and tandem SPE cartridge systems were investigated to simultaneously extract multiple classes of antimicrobials. Experimental results showed that good extraction efficiencies (84.5-105.6%) were observed for the vast majority of the target analytes when extraction was performed using the tandem SPE cartridge (SB+HR-X) system under an extraction pH of 3.0. HPLC-MS/MS parameters were optimized for simultaneous analysis of all the target analytes in a single injection. Quantification of target antimicrobials in water samples was accomplished using 15 isotopically labeled internal standards (ILISs), which allowed the efficient compensation of the losses of target analytes during sample preparation and correction of matrix effects during UHPLC-MS/MS as well as instrument fluctuations in MS/MS signal intensity. Method quantification limit (MQL) for most target analytes based on SPE was below 5ng/L for surface waters, 10ng/L for treated wastewater effluents, and 15ng/L for raw wastewater. The method was successfully applied to detect and quantify the occurrence of the target analytes in raw influent, treated effluent and surface water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

A comparative study of the density of defect states in bulk samples ...

Indian Academy of Sciences (India)

1. Introduction. Numerous potential applications of chalcogenide glasses are proposed in the civil, medi- cal and military areas [1–6]. ... rapidly by removing the ampoule from the furnace and dropping it to ice-cooled water. 2.2 Preparation of pellets and thin films. The glassy alloys of Se90Sb10 thus prepared are ground to a ...

SERS as an analytical tool in environmental science: The detection of sulfamethoxazole in the nanomolar range by applying a microfluidic cartridge setup.

Science.gov (United States)

Patze, Sophie; Huebner, Uwe; Liebold, Falk; Weber, Karina; Cialla-May, Dana; Popp, Juergen

2017-01-01

Sulfamethoxazole (SMX) is a commonly applied antibiotic for treating urinary tract infections; however, allergic reactions and skin eczema are known side effects that are observed for all sulfonamides. Today, this molecule is present in drinking and surface water sources. The allowed concentration in tap water is 2·10 -7  mol L -1 . SMX could unintentionally be ingested by healthy people when drinking contaminated tap water, representing unnecessary drug intake. To assess the quality of tap water, fast, specific and sensitive detection methods are required, in which consequence measures for improving the purification of water might be initiated in the short term. Herein, the quantitative detection of SMX down to environmentally and physiologically relevant concentrations in the nanomolar range by employing surface-enhanced Raman spectroscopy (SERS) and a microfluidic cartridge system is presented. By applying surface-water samples as matrices, the detection of SMX down to 2.2·10 -9  mol L -1 is achieved, which illustrates the great potential of our proposed method in environmental science. Copyright © 2016 Elsevier B.V. All rights reserved.

CSER 95-014: Criticality storage category for K Basin spent cartridge filters in ECOROK casks at central waste complex

International Nuclear Information System (INIS)

Miller, E.M.

1996-01-01

This CSER justifies storing K Basin spent cartridge filters in ECOROK 25-11 casks with liners under the limits in an existing criticality prevention specification, CPS-SW-149-00002, Rev./Mod. B-1, because the worst case fissionable material inventory is less then 1/2 the CPS limit and the cask is larger than allowed containers, the cask and liner have adequate iron content to meet the CPS requirements, and the cask concrete walls are thick enough to isolate the fissionable contents of each cask from neutron interaction with fissionable material external to each cask

Are extracted materials truly representative of original samples? Impact of C18 extraction on CDOM optical and chemical properties

Directory of Open Access Journals (Sweden)

Andrea A Andrew

2016-02-01

Full Text Available Some properties of dissolved organic matter (DOM and chromophoric dissolved organic matter (CDOM can be easily measured directly on whole waters, while others require sample concentration and removal of natural salts. To increase CDOM content and eliminate salts, solid phase extraction is often employed. Biases following extraction and elution are inevitable, thus raising the question of how truly representative the extracted material is of the original. In this context, we investigated the wavelength dependence of extraction efficiency for C18 cartridges with respect to CDOM optical properties using samples obtained from the Middle Atlantic Bight (MAB and the Equatorial Atlantic Ocean (EAO. Further, we compared the optical changes of C18 extracts and the corresponding whole water following chemical reduction with sodium borohydride (NaBH4.C18 cartridges preferentially extracted long-wavelength absorbing/emitting material for samples impacted by riverine input. Extraction efficiency overall decreased with offshore distance away from riverine input. Spectral slopes of C18-OM samples were also almost always lower than those of their corresponding CDOM samples supporting the preferential extraction of higher molecular weight absorbing material. The wavelength dependence of the optical properties (absorption, fluorescence emission and quantum yield of the original water samples and their corresponding extracted material were very similar. C18 extracts and corresponding water samples further exhibited comparable optical changes following NaBH4 reduction, thus suggesting a similarity in nature (structure of the optically active extracted material, independent of geographical locale. Altogether, these data suggested a strong similarity between C18 extracts and corresponding whole waters, thus indicating that extracts are representative of the CDOM content of original waters.

Are Extracted Materials Truly Representative of Original Samples? Impact of C18 Extraction on CDOM Optical and Chemical Properties.

Science.gov (United States)

Andrew, Andrea A; Del Vecchio, Rossana; Zhang, Yi; Subramaniam, Ajit; Blough, Neil V

2016-01-01

Some properties of dissolved organic matter (DOM) and chromophoric dissolved organic matter (CDOM) can be easily measured directly on whole waters, while others require sample concentration and removal of natural salts. To increase CDOM content and eliminate salts, solid phase extraction (SPE) is often employed. Biases following extraction and elution are inevitable, thus raising the question of how truly representative the extracted material is of the original. In this context, we investigated the wavelength dependence of extraction efficiency for C18 cartridges with respect to CDOM optical properties using samples obtained from the Middle Atlantic Bight (MAB) and the Equatorial Atlantic Ocean (EAO). Further, we compared the optical changes of C18 extracts and the corresponding whole water following chemical reduction with sodium borohydride (NaBH4). C18 cartridges preferentially extracted long-wavelength absorbing/emitting material for samples impacted by riverine input. Extraction efficiency overall decreased with offshore distance away from riverine input. Spectral slopes of C18-OM samples were also almost always lower than those of their corresponding CDOM samples supporting the preferential extraction of higher molecular weight absorbing material. The wavelength dependence of the optical properties (absorption, fluorescence emission, and quantum yield) of the original water samples and their corresponding extracted material were very similar. C18 extracts and corresponding water samples further exhibited comparable optical changes following NaBH4 reduction, thus suggesting a similarity in nature (structure) of the optically active extracted material, independent of geographical locale. Altogether, these data suggested a strong similarity between C18 extracts and corresponding whole waters, thus indicating that extracts are representative of the CDOM content of original waters.

Are extracted materials truly representative of original samples? Impact of C18 extraction on CDOM optical and chemical properties

Science.gov (United States)

Andrew, Andrea; Del Vecchio, Rossana; Zhang, Yi; Subramaniam, Ajit; Blough, Neil

2016-02-01

Some properties of dissolved organic matter (DOM) and chromophoric dissolved organic matter (CDOM) can be easily measured directly on whole waters, while others require sample concentration and removal of natural salts. To increase CDOM content and eliminate salts, solid phase extraction is often employed. Biases following extraction and elution are inevitable, thus raising the question of how truly representative the extracted material is of the original. In this context, we investigated the wavelength dependence of extraction efficiency for C18 cartridges with respect to CDOM optical properties using samples obtained from the Middle Atlantic Bight (MAB) and the Equatorial Atlantic Ocean (EAO). Further, we compared the optical changes of C18 extracts and the corresponding whole water following chemical reduction with sodium borohydride (NaBH4). C18 cartridges preferentially extracted long-wavelength absorbing/emitting material for samples impacted by riverine input. Extraction efficiency overall decreased with offshore distance away from riverine input. Spectral slopes of C18-OM samples were also almost always lower than those of their corresponding CDOM samples supporting the preferential extraction of higher molecular weight absorbing material. The wavelength dependence of the optical properties (absorption, fluorescence emission and quantum yield) of the original water samples and their corresponding extracted material were very similar. C18 extracts and corresponding water samples further exhibited comparable optical changes following NaBH4 reduction, thus suggesting a similarity in nature (structure) of the optically active extracted material, independent of geographical locale. Altogether, these data suggested a strong similarity between C18 extracts and corresponding whole waters, thus indicating that extracts are representative of the CDOM content of original waters.

Development of an Analytical Protocol for Determination of Cyanide in Human Biological Samples Based on Application of Ion Chromatography with Pulsed Amperometric Detection

OpenAIRE

Jaszczak, Ewa; Ruman, Marek; Narkowicz, Sylwia; Namieśnik, Jacek; Polkowska, Żaneta

2017-01-01

A simple and accurate ion chromatography (IC) method with pulsed amperometric detection (PAD) was proposed for the determination of cyanide ion in urine, sweat, and saliva samples. The sample pretreatment relies on alkaline digestion and application of Dionex OnGuard II H cartridge. Under the optimized conditions, the method showed good linearity in the range of 1–100 μg/L for urine, 5–100 μg/L for saliva, and 3–100 μg/L for sweat samples with determination coefficients (R) > 0.992. Low detec...

Multi-chamber nucleic acid amplification and detection device

Science.gov (United States)

Dugan, Lawrence

2017-10-25

A nucleic acid amplification and detection device includes an amplification cartridge with a plurality of reaction chambers for containing an amplification reagent and a visual detection reagent, and a plurality of optically transparent view ports for viewing inside the reaction chambers. The cartridge also includes a sample receiving port which is adapted to receive a fluid sample and fluidically connected to distribute the fluid sample to the reaction chamber, and in one embodiment, a plunger is carried by the cartridge for occluding fluidic communication to the reaction chambers. The device also includes a heating apparatus having a heating element which is activated by controller to generate heat when a trigger event is detected. The heating apparatus includes a cartridge-mounting section which positioned a cartridge in thermal communication with the heating element so that visual changes to the contents of the reaction chambers are viewable through the view ports.

Method of Promoting Single Crystal Growth During Melt Growth of Semiconductors

Science.gov (United States)

Su, Ching-Hua (Inventor)

2013-01-01

The method of the invention promotes single crystal growth during fabrication of melt growth semiconductors. A growth ampoule and its tip have a semiconductor source material placed therein. The growth ampoule is placed in a first thermal environment that raises the temperature of the semiconductor source material to its liquidus temperature. The growth ampoule is then transitioned to a second thermal environment that causes the semiconductor source material in the growth ampoule's tip to attain a temperature that is below the semiconductor source material's solidus temperature. The growth ampoule so-transitioned is then mechanically perturbed to induce single crystal growth at the growth ampoule's tip.

14CO2 analysis of soil gas: Evaluation of sample size limits and sampling devices

Science.gov (United States)

Wotte, Anja; Wischhöfer, Philipp; Wacker, Lukas; Rethemeyer, Janet

2017-12-01

Radiocarbon (14C) analysis of CO2 respired from soils or sediments is a valuable tool to identify different carbon sources. The collection and processing of the CO2, however, is challenging and prone to contamination. We thus continuously improve our handling procedures and present a refined method for the collection of even small amounts of CO2 in molecular sieve cartridges (MSCs) for accelerator mass spectrometry 14C analysis. Using a modified vacuum rig and an improved desorption procedure, we were able to increase the CO2 recovery from the MSC (95%) as well as the sample throughput compared to our previous study. By processing series of different sample size, we show that our MSCs can be used for CO2 samples of as small as 50 μg C. The contamination by exogenous carbon determined in these laboratory tests, was less than 2.0 μg C from fossil and less than 3.0 μg C from modern sources. Additionally, we tested two sampling devices for the collection of CO2 samples released from soils or sediments, including a respiration chamber and a depth sampler, which are connected to the MSC. We obtained a very promising, low process blank for the entire CO2 sampling and purification procedure of ∼0.004 F14C (equal to 44,000 yrs BP) and ∼0.003 F14C (equal to 47,000 yrs BP). In contrast to previous studies, we observed no isotopic fractionation towards lighter δ13C values during the passive sampling with the depth samplers.

Forensic analysis of high explosives residues in post-blast water samples employing solid phase extraction for analyte pro-concentration

International Nuclear Information System (INIS)

Umi Kalsom Ahmad; Rajendran, Sumathy; Ling, Lee Woan

2008-01-01

Nitro aromatic, nitramine and nitrate ester compounds are a major group of high order explosive or better known as military explosives. Octahydro-1,3,5,7-tetrazocine (HMX), 1,3,5-hexahydro-1,3,5-trinitro triazine (RDX), 2,4,6-trinitro-toluene (TNT), pentaerythritol tetranitrate (PETN) and 2,4-dinitrotoluene (2,4-DNT) are secondary high explosives classified as most commonly used explosives components. There is an increasing demand for pre-concentration of these compounds in water samples as the sensitivity achieved by instrumental analytical methods for these high explosives residues are the main drawback in the application at trace levels for forensic analysis. Hence, a simple cartridge solid phase extraction (SPE) procedure was optimized as the off-line extraction and pre-concentration method to enhance the detection limit of high explosive residues using micellar electrokinetic chromatography (MEKC) and gas chromatography with electron-capture detection (GC-ECD) methods. The SPE cartridges utilized LiChrolut EN as the SPE adsorbent. By emplying pre-concentration using SPE, the detection limits of the target analytes in water sample were lowered by more than 1000 times with good percentage recovery (>87%) for MEKC method and lowered by 120 times with more than 2 % percentage recovery for GC-ECD methods. In order to test the feasibility of the developed method to real cases, post-blast water samples were analyzed. The post-blast water samples which were collected from Baling Bom training range, Ulu Kinta, Perak contained RDX and PETN in the range of 0.05 - 0.17 ppm and 0.0124 - 0.0390 ppm respectively. (author)

Rapid determination of actinides in seawater samples

International Nuclear Information System (INIS)

Maxwell, S.L.; Culligan, B.K.; Hutchison, J.B.; Utsey, R.C.; McAlister, D.R.

2014-01-01

A new rapid method for the determination of actinides in seawater samples has been developed at the Savannah River National Laboratory. The actinides can be measured by alpha spectrometry or inductively-coupled plasma mass spectrometry. The new method employs novel pre-concentration steps to collect the actinide isotopes quickly from 80 L or more of seawater. Actinides are co-precipitated using an iron hydroxide co-precipitation step enhanced with Ti +3 reductant, followed by lanthanum fluoride co-precipitation. Stacked TEVA Resin and TRU Resin cartridges are used to rapidly separate Pu, U, and Np isotopes from seawater samples. TEVA Resin and DGA Resin were used to separate and measure Pu, Am and Cm isotopes in seawater volumes up to 80 L. This robust method is ideal for emergency seawater samples following a radiological incident. It can also be used, however, for the routine analysis of seawater samples for oceanographic studies to enhance efficiency and productivity. In contrast, many current methods to determine actinides in seawater can take 1-2 weeks and provide chemical yields of ∼30-60 %. This new sample preparation method can be performed in 4-8 h with tracer yields of ∼85-95 %. By employing a rapid, robust sample preparation method with high chemical yields, less seawater is needed to achieve lower or comparable detection limits for actinide isotopes with less time and effort. (author)

Improvements of the sensitivity of burst cartridge detection; Amelioration du seuil de detection des ruptures de gaine

Energy Technology Data Exchange (ETDEWEB)

Vasnier, F [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

1967-07-01

I - Special tests for improving the sensitivity of burst cartridge detection equipment in power reactors II - Scintillator purge-flow tests using aged gas in the B.C.D. /E.D.F. 2 Summary. - The first part of this report describes the tests carried out on fission product detectors by a process in which gas is continuously injected in front of the scintillator. Using this system, the background is reduced and perturbations caused by pneumatic switches on the prospecting circuits are eliminated. The quality of the signals thus obtained permits better processing of the data and thus leads to a possible improvement in the sensitivity of burst cartridge detection. The second part gives results of tests carried out with both fresh and aged gases, the economic advantage of the latter being that it permits recycling through the reactor. Reduction of the background is less pronounced but the advantage of the stable signals is conserved. (author) [French] I - Essais speciaux pour ameliorer le seuil de detection des installations de D.R.G. des reacteurs de puissance II- Essais de balayage sous scintillateur avec gaz vieilli a la D.R.G. /E.D.F. 2 Sommaire. - La premiere partie de ce rapport decrit les essais effectues sur les detecteurs de produits de fission par un procede d'injection continue de gaz sous le scintillateur. Grace a ce systeme on obtient une reduction du bruit de fond et l'elimination des perturbations causees par les commutations pneumatiques des circuits de prospection. La qualite des signaux obtenus ainsi permet un meilleur traitement des informations d'ou une amelioration possible du seuil de detection des ruptures de gaines. La seconde partie donne les resultats d'essais effectues avec du gaz propre et vieilli, l'utilisation de ce dernier presentant l'avantage economique d'etre recycle du reacteur. La reduction du bruit de fond est moins importante mais on conserve l'avantage de la stabilisation des signaux. (auteur)

Microfluidic impact printer with interchangeable cartridges for versatile non-contact multiplexed micropatterning.

Science.gov (United States)

Ding, Yuzhe; Huang, Eric; Lam, Kit S; Pan, Tingrui

2013-05-21

Biopatterning has been increasingly used for well-defined cellular microenvironment, patterned surface topology, and guided biological cues; however, it meets challenges on biocompatibility, thermal and chemical sensitivity, as well as limited availability of reagents. In this paper, we aim at combining the desired features from non-contact inkjet printing and dot-matrix impact printing to establish a versatile multiplexed micropatterning platform, referred to as Microfluidic Impact Printer (MI-Printer), for emerging biomedical applications. Using this platform, we can achieve the distinct features of no cross-contamination, sub-microliter ink loading with a minimal dead volume, high-throughput printing, biocompatible non-contact processing, sequential patterning with self-alignment, wide adaptability for complex media (e.g., cell suspension or colloidal solutions), interchangeable/disposable cartridge design, and simple assembly and configuration, all highly desirable towards laboratory-based research and development. Specifically, the printing resolution of the MI-printer platform has been experimentally characterized and theoretically analysed. Optimal printing resolution of 80 μm has been repeatedly obtained. Furthermore, two useful functions of the MI-printer, multiplexed printing and combinatorial printing, have been experimentally demonstrated with less than 10 μm misalignment. Moreover, molecular and biological patterning, utilizing the multiplexed and combinatorial printing, has been implemented to illustrate the utility of this versatile printing technique for emerging biomedical applications.

Presentation of the Nuclear Material Metrology Laboratory (LAMMAN)

International Nuclear Information System (INIS)

Arpigny, S.; Biscarrat, C.; Ruas, A.; Viallesoubranne, C.; Hanssens, A.; Roche, C.

2008-01-01

The EQRAIN Uranium or Plutonium programmes (Evaluation of the Quality of Analysis Results in the Nuclear Industry) have led to the creation of round-robins, which require reference solutions of uranyl nitrate or of plutonium nitrate to be made available. The samples are fabricated and packaged, and their benchmark values determined, by the Nuclear Material Metrology Laboratory in the Atalante facility. All the operations are carried out by highly precise weighing, including correction for air buoyancy. In order to guarantee the preservation of reference samples, a laser-sealing apparatus is used to condition the final solutions in ampoules. Random tests to check the concentration of uranium or plutonium are carried out on a certain number of ampoules after the sealing step. The analysis are performed on a photo-gravimetric analysis line (in glove box for Pu) based on the titanium potentiometric analysis method. The ampoules are then packaged and delivered to the participating laboratories. The French nuclear laboratories participating in the EQRAIN programs belong to the Cea and to the AREVA Group, with activities covering the entire fuel cycle. They have been joined by new participants from European, Japanese and South American laboratories

Presentation of the Nuclear Material Metrology Laboratory (LAMMAN)

Energy Technology Data Exchange (ETDEWEB)

Arpigny, S.; Biscarrat, C.; Ruas, A.; Viallesoubranne, C. [CEA/DEN/DRCP/SE2A/LAMM, Marcoule, BP 17171, 30207 Bagnols sur Ceze (France); Hanssens, A.; Roche, C. [CEA/DEN/DRCP/CETAMA Marcoule, BP 17171, 30207 Bagnols sur Ceze (France)

2008-07-01

The EQRAIN Uranium or Plutonium programmes (Evaluation of the Quality of Analysis Results in the Nuclear Industry) have led to the creation of round-robins, which require reference solutions of uranyl nitrate or of plutonium nitrate to be made available. The samples are fabricated and packaged, and their benchmark values determined, by the Nuclear Material Metrology Laboratory in the Atalante facility. All the operations are carried out by highly precise weighing, including correction for air buoyancy. In order to guarantee the preservation of reference samples, a laser-sealing apparatus is used to condition the final solutions in ampoules. Random tests to check the concentration of uranium or plutonium are carried out on a certain number of ampoules after the sealing step. The analysis are performed on a photo-gravimetric analysis line (in glove box for Pu) based on the titanium potentiometric analysis method. The ampoules are then packaged and delivered to the participating laboratories. The French nuclear laboratories participating in the EQRAIN programs belong to the Cea and to the AREVA Group, with activities covering the entire fuel cycle. They have been joined by new participants from European, Japanese and South American laboratories.

Identification of chemical contamination in an aqueous sample using liquid chromatography with mass spectrometry during 2nd NATO mixed samples laboratory exercise

International Nuclear Information System (INIS)

Grolmusova, K.; Tkac, M.

2010-01-01

Biological and radiological screening was conducted to determine the type of biological and radiological contamination for a sample and the reference sample. Biological screening confirmed the presence of biological contamination. Radiological screening confirmed the presence of 235 U. Preliminary chemical screening military confirmed the presence of volatile chemicals (chemical warfare agents, CWA), but refute the presence of non-volatile CWA and their degradation products and precursors (1,2,3 directory Organization for the Prohibition of Chemical Weapons, OPCW). To carry out further analysis it was necessary to adjust the aqueous sample so that it minimizes the possibility of radiological contamination, while maintaining chemical contamination. To remove 235 U from the water sample for selective extraction of chemical contamination SCX cartridges (strong cation exchange) by solid phase extraction were used. To identify chemical contamination (from the list of substances 1, 2, 3 OPCW) GC-MS and LC-MS were used. LC-ESI-MS analysis has demonstrated the presence of unknown substance designated as Chemical A in an aqueous sample. LC-ESI-MS chromatograms of the reference sample, water sample and standard were compared. Unknown substance was identified on the basis of the correlation of retention times and MS spectra of unknown substance Chemical A and standard such as triethanolamine (TEA, a breakdown product of nitrogen mustard - HN 3 fabric from the list 3B17Y OPCW).

Determination of submicrogram-per-liter concentrations of caffeine in surface water and groundwater samples by solid-phase extraction and liquid chromatography

Science.gov (United States)

Burkhardt, M.R.; Soliven, P.P.; Werner, S.L.; Vaught, D.G.

1999-01-01

A method for determining submicrogram-per-liter concentrations of caffeine in surface water and groundwater samples has been developed. Caffeine is extracted from a 1 L water sample with a 0.5 g graphitized carbon-based solid-phase cartridge, eluted with methylene chloride-methanol (80 + 20, v/v), and analyzed by liquid chromatography with photodiode-array detection. The single-operator method detection limit for organic-free water samples was 0.02 ??g/L. Mean recoveries and relative standard deviations were 93 ?? 13% for organicfree water samples fortified at 0.04 ??g/L and 84 ?? 4% for laboratory reagent spikes fortified at 0.5 ??g/L. Environmental concentrations of caffeine ranged from 0.003 to 1.44 ??g/L in surface water samples and from 0.01 to 0.08 ??g/L in groundwater samples.

Sample preparation of sewage sludge and soil samples for the determination of polycyclic aromatic hydrocarbons based on one-pot microwave-assisted saponification and extraction

Energy Technology Data Exchange (ETDEWEB)

Pena, M.T.; Pensado, Luis; Casais, M.C.; Mejuto, M.C.; Cela, Rafael [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia. Instituto de Investigacion y Analisis Alimentario, Santiago de Compostela (Spain)

2007-04-15

A microwave-assisted sample preparation (MASP) procedure was developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) in sewage sludge and soil samples. The procedure involved the simultaneous microwave-assisted extraction of PAHs with n-hexane and the hydrolysis of samples with methanolic potassium hydroxide. Because of the complex nature of the samples, the extracts were submitted to further cleaning with silica and Florisil solid-phase extraction cartridges connected in series. Naphthalene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benz[a]anthracene, chrysene, benzo[e]pyrene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenz[a,h]anthracene, benzo[g,h,i]perylene, and indeno[1,2,3-cd]pyrene, were considered in the study. Quantification limits obtained for all of these compounds (between 0.4 and 14.8 {mu}g kg{sup -1} dry mass) were well below of the limits recommended in the USA and EU. Overall recovery values ranged from 60 to 100%, with most losses being due to evaporation in the solvent exchange stages of the procedure, although excellent extraction recoveries were obtained. Validation of the accuracy was carried out with BCR-088 (sewage sludge) and BCR-524 (contaminated industrial soil) reference materials. (orig.)

Sample preparation of sewage sludge and soil samples for the determination of polycyclic aromatic hydrocarbons based on one-pot microwave-assisted saponification and extraction.

Science.gov (United States)

Pena, M Teresa; Pensado, Luis; Casais, M Carmen; Mejuto, M Carmen; Cela, Rafael

2007-04-01

A microwave-assisted sample preparation (MASP) procedure was developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) in sewage sludge and soil samples. The procedure involved the simultaneous microwave-assisted extraction of PAHs with n-hexane and the hydrolysis of samples with methanolic potassium hydroxide. Because of the complex nature of the samples, the extracts were submitted to further cleaning with silica and Florisil solid-phase extraction cartridges connected in series. Naphthalene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benz[a]anthracene, chrysene, benzo[e]pyrene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenz[a,h]anthracene, benzo[g,h,i]perylene, and indeno[1,2,3-cd]pyrene, were considered in the study. Quantification limits obtained for all of these compounds (between 0.4 and 14.8 microg kg(-1) dry mass) were well below of the limits recommended in the USA and EU. Overall recovery values ranged from 60 to 100%, with most losses being due to evaporation in the solvent exchange stages of the procedure, although excellent extraction recoveries were obtained. Validation of the accuracy was carried out with BCR-088 (sewage sludge) and BCR-524 (contaminated industrial soil) reference materials.

Comparison between sampling and analytical methods in characterization of pollutants in biogas.

Science.gov (United States)

Mariné, Sílvia; Pedrouzo, Marta; Marcé, Rosa Maria; Fonseca, Ignacio; Borrull, Francesc

2012-10-15

Different sampling methods involving the collection of biogas by Tedlar bags or adsorption tubes, and different GC-MS injection systems, loop injection or cold trap injection (with bags or by tube desorption), were compared to establish the best method to determine the minority compounds in biogas from sewage treatment plants (STPs). A study of parameters is included, such as the stability of compounds in Tedlar bags or cartridges and the adsorption effect of some less volatile compounds in the thermal desorption system (TD). The optimized methods allowed to determine most compounds at low mgm(-3) levels. Among them, maximum values of D5 (4.84 mg m(-3)), decane (95-118 mg m(-3)) and H(2)S (2223 mg m(-3)) were found in biogas samples. Copyright © 2012 Elsevier B.V. All rights reserved.

The NOSAMS sample preparation laboratory in the next millenium: Progress after the WOCE program

International Nuclear Information System (INIS)

Gagnon, Alan R.; McNichol, Ann P.; Donoghue, Joanne C.; Stuart, Dana R.; Reden, Karl von

2000-01-01

Since 1991, the primary charge of the National Ocean Sciences AMS (NOSAMS) facility at the Woods Hole Oceanographic Institution has been to supply high throughput, high precision AMS 14 C analyses for seawater samples collected as part of the World Ocean Circulation Experiment (WOCE). Approximately 13,000 samples taken as part of WOCE should be fully analyzed by the end of Y2K. Additional sample sources and techniques must be identified and incorporated if NOSAMS is to continue in its present operation mode. A trend in AMS today is the ability to routinely process and analyze radiocarbon samples that contain tiny amounts ( 14 C analysis has been recognized as a major facility goal. The installation of a new 134-position MC-SNICS ion source, which utilizes a smaller graphite target cartridge than presently used, is one step towards realizing this goal. New preparation systems constructed in the sample preparation laboratory (SPL) include an automated bank of 10 small-volume graphite reactors, an automated system to process organic carbon samples, and a multi-dimensional preparative capillary gas chromatograph (PCGC)

Activation analysis of rare-earth elements in opium and cannabis samples

International Nuclear Information System (INIS)

Henke, G.

1977-01-01

Rare-earth concentrations in 65 Opium, Cannabis and Cannabis resin samples seized from various parts of the world were determined by destructive NAA. Because of the greater concentrations of Ca, P, K, Fe, Na and Si in plant materials, rare-earth elements were isolated after neutron irradiation and determined by gamma-spectrometry. The main steps of the method are: Preashing of 1 g Cannabis resin, 2.5 g Cannabis or 7.5 g Opium, respectively, in quartz ampoules (5 h, 500 deg C). Neutron irradiation, 24 h at 5x10 13 n cm -2 sec -1 . Cooling period 2-3 days. After addition of 0.1 μCi 139 Ce and rare-earth carriers wet ashing of irradiated samples with H 2 SO 4 /HNO 3 , followed by alternate addition of HNO 3 and H 2 O 2 (30%). Precipitation and removal of silicates, precipitation of fluorides, precipitation of hydroxides. Dissolution of hydroxides in HCl. Extraction with di-(2-ethylhexyl)phosphate (DEHP)/toluene and twice back-extraction of rare earths, gamma-spectrometry of HCl phase. Due to sample activity and half-life of nuclides, three measurements were made on each sample: 2 days (for La, Sm, Gd, Ho, Er, Yb); 14 days (for Nd, Lu) and 30 days after irradiation (for Ce, Eu, Tb). Great variations in absolute element concentrations, but only small significant differences of rare earth concentration ratios were found, indicating inconsiderable biogeochemical fractionation. The mean values of these ratios correspond to the relative abundances of the rare earths in the upper continental earth's crust. (T.G.)

A method to eliminate wetting during the homogenization of HgCdTe

Science.gov (United States)

Su, Ching-Hua; Lehoczky, S. L.; Szofran, F. R.

1986-01-01

Adhesion of HgCdTe samples to fused silica ampoule walls, or 'wetting', during the homogenization process was eliminated by adopting a slower heating rate. The idea is to decrease Cd activity in the sample so as to reduce the rate of reaction between Cd and the silica wall.

A Method for Multiple Mycotoxin Analysis in Wines by Solid Phase Extraction and Multifunctional Cartridge Purification, and Ultra-High-Performance Liquid Chromatography Coupled to Tandem Mass Spectrometry

Science.gov (United States)

Tamura, Masayoshi; Takahashi, Ayumi; Uyama, Atsuo; Mochizuki, Naoki

2012-01-01

An analytical method using two solid phase extractions and ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) was developed for the identification and quantification of 14 mycotoxins (patulin, deoxynivalenol, aflatoxins B1, B2, G1, G2, M1, T-2 toxin, HT-2 toxin, zearalenone, fumonisins B1, B2, B3, and ochratoxin A) in domestic and imported wines. Mycotoxins were purified with an Oasis HLB cartridge, followed by a MultiSepTM #229 Ochra. As a result, sufficient removal of the pigments and highly polar matrices from the red wines was achieved. UHPLC conditions were optimized, and 14 mycotoxins were separated in a total of 13 min. Determinations performed using this method produced high correlation coefficients for the 14 mycotoxins (R > 0.990) and recovery rates ranging from 76 to 105% with good repeatability (relative standard deviation RSD < 12%). Twenty-seven samples of domestic and imported wines were analyzed using this method. Although ochratoxin A (OTA) and fumonisins (FMs) were detected in several samples, the FM levels were less than limits of quantification (LOQs) (1 μg/L), and even the largest of the OTA levels was below the EU regulatory level (2 μg/L). These results suggest that the health risk posed to consumers from the wines available in Japan is relatively low. PMID:22822458

A simple and rapid in situ preconcentration method for the determination of phosphate in environmental waters by use of solid-phase extraction, and its applications to brackish lake waters.

Science.gov (United States)

Okumura, M; Tong, L; Fujinaga, K; Seike, Y

2001-05-01

A simple and rapid in situ preconcentration method for the determination of phosphate in environmental waters has been developed for field analysis. This method is based on solid-phase extraction on a zirconium-loaded Sep-Pack Accell CM cartridge (Zr-SP) and is applicable to studies in which sampling is performed by use of a graduated syringe to prevent contamination and to ensure easy operation at sampling sites. The Zr-SP cartridge was prepared by passing 0.1 mol L(-1) zirconium solution through a Sep-Pak Accell CM cartridge, packed with cation exchange sorbent based on a silica matrix. The adsorption of phosphate and its desorption depend only on the pH of the solution. A water sample containing phosphate was adjusted to pH 2 and passed through the Zr-SP cartridge to collect it. The retained phosphate was quantitatively eluted with 0.5 mol L(-1) sodium hydroxide solution. The phosphate retained in the Zr-SP cartridge was stable for at least one month. The established preconcentration method was successfully applied to brackish lake waters to investigate seasonal changes in the distribution and behavior of phosphate in a brackish lake.

Identification of chemical contamination in an aqueous sample using liquid chromatography with mass spectrometry during 2nd NATO mixed samples laboratory exercise

International Nuclear Information System (INIS)

Grolmusova, K.; Tkac, M.

2010-01-01

Biological and radiological screening was conducted on a sample and reference sample to determine the type of biological and radiological contamination. Biological screening confirmed the presence of biological contamination. Radiological screening confirmed the presence of 235 U. Preliminary chemical military screening confirmed the presence of volatile chemicals (chemical warfare agents, CWA), but refute the presence of non-volatile CWA and their degradation products and precursors (1,2,3 directory Organization for the Prohibition of Chemical Weapons, OPCW). To carry out further analysis it was necessary to adjust aqueous sample so that it minimizes the possibility of radiological contamination, while maintaining chemical contamination. To remove of 235 U from the water sample for selective extraction of chemical contamination by solid phase extraction (solid phase extraction - SPE) using SCX (strong cation exchange) cartridges were used. To identify chemical contamination (from the list of substances 1, 2, 3 OPCW) GC-MS and LC-MS were used. LC-ESI-MS analysis has demonstrated the presence of an unknown substance designated as Chemical A in an aqueous sample. LC-ESI-MS chromatograms of the reference sample, water sample and standard were compared. Unknown substance has been identified on the basis of the correlation of retention times and MS spectra of unknown substances - chemical A and standard such as triethanolamine (TEA, a breakdown product of nitrogen mustard - HN 3 fabric from the list 3B17Y OPCW).

Method of analysis and quality-assurance practices for determination of pesticides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry at the U.S. Geological Survey California District Organic Chemistry Laboratory, 1996-99

Science.gov (United States)

Crepeau, Kathryn L.; Baker, Lucian M.; Kuivila, Kathryn

2000-01-01

A method of analysis and quality-assurance practices were developed to study the fate and transport of pesticides in the San Francisco Bay-Estuary by the U.S. Geological Survey. Water samples were filtered to remove suspended-particulate matter and pumped through C-8 solid-phase extraction cartridges to extract the pesticides. The cartridges were dried with carbon dioxide and the pesticides were eluted with three cartridge volumes of hexane:diethyl ether (1:1) solution. The eluants were analyzed using capillary-column gas chromatography/mass spectrometry in full-scan mode. Method detection limits for pesticides ranged from 0.002 to 0.025 microgram per liter for 1-liter samples. Recoveries ranged from 44 to 140 percent for 25 pesticides in samples of organic-free reagent water and Sacramento-San Joaquin Delta and Suisun Bay water fortified at 0.05 and 0.50 microgram per liter. The estimated holding time for pesticides after extraction on C-8 solid-phase extraction cartridges ranged from 10 to 257 days.

Luminescence properties of Eu2+- and Ce3+-doped CaAl2S4 and application in white LEDs

International Nuclear Information System (INIS)

Yu Ruijin; Wang Jing; Zhang Jianhui; Yuan Haibin; Su Qiang

2008-01-01

The Eu 2+ - and Ce 3+ -doped CaAl 2 S 4 phosphors were comparatively synthesized by conventional solid-state reaction and the evacuated sealed quartz ampoule. The X-ray diffraction (XRD) patterns show that the sample with better crystalline quality was prepared by the evacuated sealed quartz ampoule, resulting in the enhancement of the emission intensity of Eu 2+ ion by a factor of 1.7. The intensive green LEDs were also fabricated by combining CaAl 2 S 4 :Eu 2+ with near-ultraviolet InGaN chips (λ em =395 nm). The dependence of as-fabricated green LEDs on forward-bias currents shows that it presents good chromaticity stability and luminance saturation, indicating that CaAl 2 S 4 :Eu 2+ is a promising green-emitting phosphor for a near-UV InGaN-based LED. In addition, the optical properties of CaAl 2 S 4 :Ce 3+ were systematically investigated by means of diffuse reflectance, photoluminescence excitation and emission, concentrating quenching and the decay curve. - Graphical abstract: The Eu 2+ - and Ce 3+ -doped CaAl 2 S 4 phosphors were comparatively synthesized by two methods. The emission intensity of Eu 2+ ion in sample synthesized by the evacuated sealed quartz ampoule method is by a factor of 1.7 as strong as that of Eu 2+ ion in sample prepared by the conventional solid-state reaction method

The NOSAMS sample preparation laboratory in the next millenium: Progress after the WOCE program

Energy Technology Data Exchange (ETDEWEB)

Gagnon, Alan R. E-mail: agagnon@whoi.edu; McNichol, Ann P.; Donoghue, Joanne C.; Stuart, Dana R.; Reden, Karl von

2000-10-01

Since 1991, the primary charge of the National Ocean Sciences AMS (NOSAMS) facility at the Woods Hole Oceanographic Institution has been to supply high throughput, high precision AMS {sup 14}C analyses for seawater samples collected as part of the World Ocean Circulation Experiment (WOCE). Approximately 13,000 samples taken as part of WOCE should be fully analyzed by the end of Y2K. Additional sample sources and techniques must be identified and incorporated if NOSAMS is to continue in its present operation mode. A trend in AMS today is the ability to routinely process and analyze radiocarbon samples that contain tiny amounts (<100 {mu}g) of carbon. The capability to mass-produce small samples for {sup 14}C analysis has been recognized as a major facility goal. The installation of a new 134-position MC-SNICS ion source, which utilizes a smaller graphite target cartridge than presently used, is one step towards realizing this goal. New preparation systems constructed in the sample preparation laboratory (SPL) include an automated bank of 10 small-volume graphite reactors, an automated system to process organic carbon samples, and a multi-dimensional preparative capillary gas chromatograph (PCGC)

Passive sampling of selected pesticides in aquatic environment using polar organic chemical integrative samplers.

Science.gov (United States)

Thomatou, Alphanna-Akrivi; Zacharias, Ierotheos; Hela, Dimitra; Konstantinou, Ioannis

2011-08-01

Polar chemical integrative samplers (POCIS) were examined for their sampling efficiency of 12 pesticides and one metabolite commonly detected in surface waters. Laboratory-based calibration experiments of POCISs were conducted. The determined passive sampling rates were applied for the monitoring of pesticides levels in Lake Amvrakia, Western Greece. Spot sampling was also performed for comparison purposes. Calibration experiments were performed on the basis of static renewal exposure of POCIS under stirred conditions for different time periods of up to 28 days. The analytical procedures were based on the coupling of POCIS and solid phase extraction by Oasis HLB cartridges with gas chromatography-mass spectrometry. The recovery of the target pesticides from the POCIS was generally >79% with relative standard deviation (RSD) monitoring campaign using both passive and spot sampling whereas higher concentrations were measured by spot sampling in most cases. Passive sampling by POCIS provides a useful tool for the monitoring of pesticides in aquatic systems since integrative sampling at rates sufficient for analytical quantitation of ambient levels was observed. Calibration data are in demand for a greater number of compounds in order to extend the use in environmental monitoring.

Adrenaline in cardiac arrest: Prefilled syringes are faster.

Science.gov (United States)

Helm, Claire; Gillett, Mark

2015-08-01

Standard ampoules and prefilled syringes of adrenaline are widely available in Australasian EDs for use in cardiac arrest. We hypothesise that prefilled syringes can be administered more rapidly and accurately when compared with the two available standard ampoules. This is a triple arm superiority study comparing the time to i.v. administration and accuracy of dosing of three currently available preparations of adrenaline. In their standard packaging, prefilled syringes were on average more than 12 s faster to administer than the 1 mL 1:1000 ampoules and more than 16 s faster than the 10 mL 1:10,000 ampoules (P adrenaline utilising a Minijet (CSL Limited, Parkville, Victoria, Australia) is faster than using adrenaline in glass ampoules presented in their plastic packaging. Removing the plastic packaging from the 1 mL (1 mg) ampoule might result in more rapid administration similar to the Minijet. Resuscitation personnel requiring rapid access to adrenaline should consider storing it as either Minijets or ampoules devoid of packaging. These results might be extrapolatable to other clinical scenarios, including pre-hospital and anaesthesia, where other drugs are required for rapid use. © 2015 Australasian College for Emergency Medicine and Australasian Society for Emergency Medicine.

Investigation of solid phase sorbents for the pre- concentration of pads from aqueous medium and their quantitation by high performance liquid chromatography-UV detection

International Nuclear Information System (INIS)

Waqar, F.; Jan, S.; Muhammad, B.; Ahmad, S.; Riaz, M.; Akram, N.

2005-01-01

A solid phase extraction method was optimized for the pre-concentration of polyaromatic hydrocarbons (PAHs) in water samples. Graphite powder and Lab scale locally synthesized styrene divinylbenzene (SDVB) Copolymer were used as sorbents for the extraction of PAHs and compared with commercially used C18 solid phase extraction cartridge (SPE). Various parameters were optimized to evaluate the extraction efficiencies, the best results were obtained by proper conditioning of extraction cartridges and desorption with suitable solvent. Percentage recoveries were enhanced by rinsing the sample bottles with acetonitrile and combining the rinse with the sample extract. Quantitative analysis was performed by High performance Liquid chromatography (HPLC) with UV detection. Many other parameters, including optimization of mobile phase, selection of HPLC Columns, sample-loading flow rate on extraction cartridge and weight of sorbent were performed to get optimal results. Percent recoveries obtained with synthesized copolymer were comparable with commercial cartridge, while graphite powder showed excellent retention but very poor recoveries. Obtained recoveries of selected PAHs were ranged from 80-87% with relative standard deviation <6%. Developed method was applied for the analysis of drinking water samples(author)

Reduction of Defects in Germanium-Silicon

Science.gov (United States)

2003-01-01

Crystals grown without contact with a container have far superior quality to otherwise similar crystals grown in direct contact with a container. In addition to float-zone processing, detached- Bridgman growth is a promising tool to improve crystal quality, without the limitations of float zoning or the defects introduced by normal Bridgman growth. Goals of this project include the development of the detached Bridgman process to be reproducible and well understood and to quantitatively compare the defect and impurity levels in crystals grown by these three methods. Germanium (Ge) and germanium-silicon (Ge-Si) alloys are being used. At MSFC, we are responsible for the detached Bridgman experiments intended to differentiate among proposed mechanisms of detachment, and to confirm or refine our understanding of detachment. Because the contact angle is critical to determining the conditions for detachment, the sessile drop method was used to measure the contact angles as a function of temperature and composition for a large number of substrates made of potential ampoule materials. Growth experiments have used pyrolytic boron nitride (pBN) and fused silica ampoules with the majority of the detached results occurring predictably in the pBN. Etch pit density (EPD) measurements of normal and detached Bridgman-grown Ge samples show a two order of magnitude improvement in the detached-grown samples. The nature and extent of detachment is determined by using profilometry in conjunction with optical and electron microscopy. The stability of detachment has been analyzed, and an empirical model for the conditions necessary to achieve sufficient stability to maintain detached growth for extended periods has been developed. We have investigated the effects on detachment of ampoule material, pressure difference above and below the melt, and Si concentration; samples that are nearly completely detached can be grown repeatedly in pBN. Current work is concentrated on developing a

Analytical method for the determination of atrazine and its dealkylated chlorotriazine metabolites in water using SPE sample preparation and GC-MSD analysis.

Science.gov (United States)

Huang, Sung-Ben; Stanton, Jeffrey S; Lin, Yi; Yokley, Robert A

2003-12-03

A method is reported for the determination of atrazine and its dealkylated chlorotriazine metabolites in ground, surface, and deionized water. Water samples are adjusted to pH 3-4 prior to loading onto two SPE cartridges in series: C-18 and C-18/cation exchange mixed-mode polymeric phases. The analytes are eluted from each of the two cartridges separately, and the pooled and concentrated fraction is analyzed using gas chromatography-mass selective detection in the selected ion monitoring mode. The lower limit of method validation is 0.10 micrograms/L (ppb) for 2-chloro-4-(ethylamino)-6-(isopropylamino)-s-triazine (atrazine), 2-amino-4-chloro-6-(isopropylamino)-s-triazine (G-30033, deethylatrazine), 2-amino-4-chloro-6-(ethylamino)-s-triazine (G-28279, deisopropylatrazine), and 2,4-diamino-6-chloro-s-triazine (G-28273, didealkyatrazine). The overall mean procedural recoveries (and standard deviations) are 96 (6.9), 96 (5.5), 95 (6.8), and 100% (10%) for atrazine, G-30033, G-28279, and G-28273, respectively (n = 49). The method validation study was conducted under U.S. EPA FIFRA Good Laboratory Practice Guidelines 40 CFR 160. The reported procedure accounts for residues of G-28273 in water.

Method to determine trace elements in water samples by neutron activation analysis

International Nuclear Information System (INIS)

Kueppers, G.; Erdtmann, G.

1981-05-01

For the determination of trace elements in water by neutron activation analysis irradiation porcedures and chemical separation procedures have been developed. Irradiation in melted quarz glass ampoules in the presence of a platinum wire (for recombination of the oxyhydrogen gas produced by radiolysis) proved successfull with different variants of the irradiation methods, as long irradiation periods without pressure build-up could be achieved. Possible falsifications of the analysis results were investigated in detail (losses by absorption on vessel walls etc.). The irradiated samples can be measured directly with a gamma ray spectrometer and from the radionuclides found the trace element contents may be calculated. More sensitive determinations are possible if the radionuclides are chemically separated. Procedures for removing the matrix activities, for the separation of the radionuclides in groups of elements and for the isolation of single elements have been developed. For especially sensitive determination of some elements selective separation procedures for antimony, cadmium, selenium, mercury and uranium have been developed. The analytical procedures described have been applied to trace element determinations in river water, glacier ice and water solutions from technical processes. (orig./RB) [de

Construction of a mutagenesis cartridge for poliovirus genome-linked viral protein: isolation and characterization of viable and nonviable mutants

International Nuclear Information System (INIS)

Kuhn, R.J.; Tada, H.; Ypma-Wong, M.F.; Dunn, J.J.; Semler, B.L.; Wimmer, E.

1988-01-01

By following a strategy of genetic analysis of poliovirus, the authors have constructed a synthetic mutagenesis cartridge spanning the genome-linked viral protein coding region and flanking cleavage sites in an infectious cDNA clone of the type I (Mahoney) genome. The insertion of new restriction sites within the infectious clone has allowed them to replace the wild-type sequences with short complementary pairs of synthetic oligonucleotides containing various mutations. A set of mutations have been made that create methionine codons within the genome-linked viral protein region. The resulting viruses have growth characteristics similar to wild type. Experiments that led to an alteration of the tyrosine residue responsible for the linkage to RNA have resulted in nonviable virus. In one mutant, proteolytic processing assayed in vitro appeared unimpaired by the mutation. They suggest that the position of the tyrosine residue is important for genome-linked viral protein function(s)

Development of a calibration system for airborne "1"3"1I monitoring devices

International Nuclear Information System (INIS)

Zhao, C.; Tang, F.; He, L.; Xu, Y.; Lu, X.

2016-01-01

A prototype calibration system for airborne "1"3"1I monitoring devices was developed at the Shanghai Institute of Measurement and Testing Technology (SIMT). This system consists of a gaseous "1"3"1I_2 generator, an airborne storage chamber, an airborne iodine sampler, and an HPGe spectrometer. With this system, "1"3"1I reference samples in the form of charcoal filters and charcoal cartridges, with activities ranging from 100 to 10,000 Bq, were produced with overall relative standard uncertainties of 2.8% (for filter samples) and 3.5% (for cartridge samples); the activities range could be extended according to need. - Highlights: • Original calibration system for airborne "1"3"1I monitoring devices was developed. • Two types of "1"3"1I reference samples was prepared. • The activity of the produced "1"3"1I reference sample could be easily controlled. • The influence of uneven distribution of "1"3"1I in cartridge samples was considered.

A rapid high-performance liquid-chromatographic method for simultaneously determining the concentrations of TFM and Bayer 73 in water during lampricide treatments

Science.gov (United States)

Dawson, V.K.

1982-01-01

The high-performance liquid-chromatography (HPLC) procedure requires only minutes per sample, is specific, and is relatively sensitive (limit of detection 18 disposable cartridge. The cartridge adsorbs and retains both the lampricides and the internal standard. The quantitative elution of the three chemicals from the cartridge with a small volume of methanol effectively concentrates the sample and provides sample cleanup. The methanol extract is then analyzed directly by HPLC on an MCH 10 reverse phase column by using a methanol:0.01 mol/L acetate buffer (87:13, v:v) as the mobile phase at 2 mL/min and detected by ultraviolet spectrophotometry at 330 (or 254) nm. A microprocessor data system further facilitates the procedure by quantifying off-scale peaks and yielding results directly in units of concentration (mg/L).

Quantitative method of viral pollution determination for large volume of water using ferric hydroxide gel impregnated on the surface of glassfibre cartridge

Directory of Open Access Journals (Sweden)

Akira Homma

1974-01-01

Full Text Available Quantitative method of viral pollution determination for large volume of water using ferric hydroxide gel impregnated on the surface of glassfibre cartridge filter. The use of ferric hydroxide gel, impregnated on the surface of glassfibre cartridge filter enable us to recover 62.5% of virus (Poliomylitis type I, Lsc strain exsogeneously added to 400 liters of tap-water. The virus concentrator system consists of four cartridge filters, in which the three first one are clarifiers, where the contaminants are removed physically, without significant virus loss at this stage. The last cartridge filter is impregnated with ferric hydroxide gel, where the virus is adsorbed. After the required volume of water has been processed, the last filter is removed from the system and the viruses are recovered from the gel, using 1 liter of glycine/NaOH buffer, at pH 11. Immediately the eluate is clarified through series of cellulose acetate membranes mounted in a 142mm Millipore filter. For the second step of virus concentration, HC1 1N is added slowly to the eluate to achieve pH 3.5-4. MgC1, is added to give a final concentration of 0.05M and the viruses are readsorbed on a 0.45 , porosity (HA cellulose acetate membrane, mounted in a 90 mm Millipore filter. The viruses are recovered using the same eluent plus 10% of fetal calf serum, to a final volume of 3 ml. In this way, it was possible to concentrate virus from 400 liters of tap-water, into 1 liter in the first stage of virus concentration and just to 3 ml of final volume in a second step. The efficiency, simplicity and low operational cost, provded by the method, make it feasible to study viral pollution of recreational and tap-water sources.Relata-se o emprego de um concentrador portátil, o qual se mostrou capaz de recuperar 62,5% dos vírus (Polio I, amostra Lsc experimentalmente dispersos em 400 litros de água, os quais foram reduzidos a 3 ml. O sistema concentrador de vírus é composto de quatro

Simple system for isothermal DNA amplification coupled to lateral flow detection.

Directory of Open Access Journals (Sweden)

Kristina Roskos

Full Text Available Infectious disease diagnosis in point-of-care settings can be greatly improved through integrated, automated nucleic acid testing devices. We have developed an early prototype for a low-cost system which executes isothermal DNA amplification coupled to nucleic acid lateral flow (NALF detection in a mesofluidic cartridge attached to a portable instrument. Fluid handling inside the cartridge is facilitated through one-way passive valves, flexible pouches, and electrolysis-driven pumps, which promotes a compact and inexpensive instrument design. The closed-system disposable prevents workspace amplicon contamination. The cartridge design is based on standard scalable manufacturing techniques such as injection molding. Nucleic acid amplification occurs in a two-layer pouch that enables efficient heat transfer. We have demonstrated as proof of principle the amplification and detection of Mycobacterium tuberculosis (M.tb genomic DNA in the cartridge, using either Loop Mediated Amplification (LAMP or the Exponential Amplification Reaction (EXPAR, both coupled to NALF detection. We envision that a refined version of this cartridge, including upstream sample preparation coupled to amplification and detection, will enable fully-automated sample-in to answer-out infectious disease diagnosis in primary care settings of low-resource countries with high disease burden.

Intercomparison campaign of Contracted Partner Institutes 1997

International Nuclear Information System (INIS)

Reinen, H.A.J.M.; Tijsmans, M.H.; Van Tuinen, S.T.; Overwater, R.M.W.; Aldenkamp, F.J.

1998-01-01

The Dutch National Plan for Nuclear Emergency Planning and Response (EPR) is trained frequently. Intercomparison campaigns and exercises are part of this training for the Contracted Partner Institutes (CPI). The results of an intercomparison campaign in 1997 for the CPI are reported. Two carbon cartridges, one contaminated homogeneously and one inhomogeneously with 131 I, and a water sample contaminated with 134 Cs and 137 Cs were analysed by means of gamma spectroscopy. The results had to be faxed to RIVM within the time limits prescribed in the emergency protocols for CPI, i.e. 2 hours for the cartridges and 24 hours for the water sample. Most CPI reported in time. The results for the inhomogeneously contaminated cartridge are within 25% from the accepted reference value (ARV). For the homogeneously contaminated cartridge the results are within 40% from the ARV. In reality, the contamination of the cartridge will have an exponential profile, with most of the activity in the first few millimeters. In this situation results can be expected to be within 20% from the true value. The results for the water sample are within 5% from the ARV. Although most CPI have applied corrections for coincidence summing for 134 Cs there is still a systematic error of 4% for this nuclide. In regard of the requirements for measurements during emergency situations, the results of this intercomparison campaign are satisfactory

Exploitation of FTA cartridges for the sampling, long-term storage, and DNA-based analyses of plant-parasitic nematodes.

Science.gov (United States)

Marek, Martin; Zouhar, Miloslav; Douda, Ondřej; Maňasová, Marie; Ryšánek, Pavel

2014-03-01

The use of DNA-based analyses in molecular plant nematology research has dramatically increased over recent decades. Therefore, the development and adaptation of simple, robust, and cost-effective DNA purification procedures are required to address these contemporary challenges. The solid-phase-based approach developed by Flinders Technology Associates (FTA) has been shown to be a powerful technology for the preparation of DNA from different biological materials, including blood, saliva, plant tissues, and various human and plant microbial pathogens. In this work, we demonstrate, for the first time, that this FTA-based technology is a valuable, low-cost, and time-saving approach for the sampling, long-term archiving, and molecular analysis of plant-parasitic nematodes. Despite the complex structure and anatomical organization of the multicellular bodies of nematodes, we report the successful and reliable DNA-based analysis of nematode high-copy and low-copy genes using the FTA technology. This was achieved by applying nematodes to the FTA cards either in the form of a suspension of individuals, as intact or pestle-crushed nematodes, or by the direct mechanical printing of nematode-infested plant tissues. We further demonstrate that the FTA method is also suitable for the so-called "one-nematode-assay", in which the target DNA is typically analyzed from a single individual nematode. More surprisingly, a time-course experiment showed that nematode DNA can be detected specifically in the FTA-captured samples many years after initial sampling occurs. Collectively, our data clearly demonstrate the applicability and the robustness of this FTA-based approach for molecular research and diagnostics concerning phytonematodes; this research includes economically important species such as the stem nematode (Ditylenchus dipsaci), the sugar beet nematode (Heterodera schachtii), and the Northern root-knot nematode (Meloidogyne hapla).

Arsenic Sulfide Nanowire Formation on Fused Quartz Surfaces

Energy Technology Data Exchange (ETDEWEB)

Olmstead, J.; Riley, B.J.; Johnson, B.R.; Sundaram, S.K.

2005-01-01

Arsenic sulfide (AsxSy) nanowires were synthesized by an evaporation-condensation process in evacuated fused quartz ampoules. During the deposition process, a thin, colored film of AsxSy was deposited along the upper, cooler portion of the ampoule. The ampoule was sectioned and the deposited film analyzed using scanning electron microscopy (SEM) to characterize and semi-quantitatively evaluate the microstructural features of the deposited film. A variety of microstructures were observed that ranged from a continuous thin film (warmer portion of the ampoule), to isolated micron- and nano-scale droplets (in the intermediate portion), as well as nanowires (colder portion of the ampoule). Experiments were conducted to evaluate the effects of ampoule cleaning methods (e.g. modify surface chemistry) and quantity of source material on nanowire formation. The evolution of these microstructures in the thin film was determined to be a function of initial pressure, substrate temperature, substrate surface treatment, and initial volume of As2S3 glass. In a set of two experiments where the initial pressure, substrate thermal gradient, and surface treatment were the same, the initial quantity of As2S3 glass per internal ampoule volume was doubled from one test to the other. The results showed that AsxSy nanowires were only formed in the test with the greater initial quantity of As2S3 per internal ampoule volume. The growth data for variation in diameter (e.g. nanowire or droplet) as a function of substrate temperature was fit to an exponential trendline with the form y = Aekx, where y is the structure diameter, A = 1.25×10-3, k = 3.96×10-2, and x is the temperature with correlation coefficient, R2 = 0.979, indicating a thermally-activated process.

Development of an Analytical Protocol for Determination of Cyanide in Human Biological Samples Based on Application of Ion Chromatography with Pulsed Amperometric Detection

Directory of Open Access Journals (Sweden)

Ewa Jaszczak

2017-01-01

Full Text Available A simple and accurate ion chromatography (IC method with pulsed amperometric detection (PAD was proposed for the determination of cyanide ion in urine, sweat, and saliva samples. The sample pretreatment relies on alkaline digestion and application of Dionex OnGuard II H cartridge. Under the optimized conditions, the method showed good linearity in the range of 1–100 μg/L for urine, 5–100 μg/L for saliva, and 3–100 μg/L for sweat samples with determination coefficients (R>0.992. Low detection limits (LODs in the range of 1.8 μg/L, 5.1 μg/L, and 5.8 μg/L for urine, saliva, and sweat samples, respectively, and good repeatability (CV < 3%, n=3 were obtained. The proposed method has been successfully applied to the analysis of human biological samples.

Development of an Analytical Protocol for Determination of Cyanide in Human Biological Samples Based on Application of Ion Chromatography with Pulsed Amperometric Detection.

Science.gov (United States)

Jaszczak, Ewa; Ruman, Marek; Narkowicz, Sylwia; Namieśnik, Jacek; Polkowska, Żaneta

2017-01-01

A simple and accurate ion chromatography (IC) method with pulsed amperometric detection (PAD) was proposed for the determination of cyanide ion in urine, sweat, and saliva samples. The sample pretreatment relies on alkaline digestion and application of Dionex OnGuard II H cartridge. Under the optimized conditions, the method showed good linearity in the range of 1-100  μ g/L for urine, 5-100  μ g/L for saliva, and 3-100  μ g/L for sweat samples with determination coefficients ( R ) > 0.992. Low detection limits (LODs) in the range of 1.8  μ g/L, 5.1  μ g/L, and 5.8  μ g/L for urine, saliva, and sweat samples, respectively, and good repeatability (CV < 3%, n = 3) were obtained. The proposed method has been successfully applied to the analysis of human biological samples.

Activation analysis of rare-earth elements in opium and cannabis samples. [Neutron reactions

Energy Technology Data Exchange (ETDEWEB)

Henke, G [Muenster Univ. (Germany, F.R.). Inst. fuer Pharmazeutische Chemie

1977-01-01

Rare-earth concentrations in 65 Opium, Cannabis and Cannabis resin samples seized from various parts of the world were determined by destructive NAA. Because of the greater concentrations of Ca, P, K, Fe, Na and Si in plant materials, rare-earth elements were isolated after neutron irradiation and determined by gamma-spectrometry. The main steps of the method are: Preashing of 1 g Cannabis resin, 2.5 g Cannabis, or 7.5 g Opium, respectively, in quartz ampoules (5 h, 500 deg C). Neutron irradiation, 24 h at 5x10/sup 13/n cm/sup -2/sec/sup -1/. Cooling period 2-3 days. After addition of 0.1 ..mu..Ci /sup 139/Ce and rare-earth carriers wet ashing of irradiated samples with H/sub 2/SO/sub 4//HNO/sub 3/, followed by alternate addition of HNO/sub 3/ and H/sub 2/O/sub 2/ (30%). Precipitation and removal of silicates, precipitation of fluorides, precipitation of hydroxides. Dissolution of hydroxides in HCl. Extraction with di-(2-ethylhexyl)phosphate (DEHP)/toluene and twice back-extraction of rare earths, gamma-spectrometry of HCl phase. Due to sample activity and half-life of nuclides, three measurements were made on each sample: 2 days (for La, Sm, Gd, Ho, Er, Yb); 14 days (for Nd, Lu) and 30 days after irradiation (for Ce, Eu, Tb). Great variations in absolute element concentrations, but only small significant differences of rare earth concentration ratios were found, indicating inconsiderable biogeochemical fractionation. The mean values of these ratios correspond to the relative abundances of the rare earths in the upper continental earth's crust.

An in-line clean system for the solid-phase extraction of emerging contaminants in natural waters

OpenAIRE

Sodré, Fernando F.; Locatelli, Marco Antonio F.; Jardim, Wilson F.

2010-01-01

A solid-phase in-line extraction system for water samples containing low levels of emerging contaminants is described. The system was specially developed for large volume samples (up to 4 L) using commercial solid-phase extraction (SPE) cartridges. Four sets containing PTFE-made connectors, brass adapters and ball valves were used to fit SPE cartridges and sample bottles to a 4-port manifold attached to a 20 L carboy. A lab-made vacuum device was connected to the manifold cap. The apparatus i...

Sistema limpo em linha para extração em fase sólida de contaminantes emergentes em águas naturais

OpenAIRE

Sodré,Fernando F.; Locatelli,Marco Antonio F.; Jardim,Wilson F.

2010-01-01

A solid-phase in-line extraction system for water samples containing low levels of emerging contaminants is described. The system was specially developed for large volume samples (up to 4 L) using commercial solid-phase extraction (SPE) cartridges. Four sets containing PTFE-made connectors, brass adapters and ball valves were used to fit SPE cartridges and sample bottles to a 4-port manifold attached to a 20 L carboy. A lab-made vacuum device was connected to the manifold cap. The apparatus i...

Limitations of amorphous content quantification by isothermal calorimetry using saturated salt solutions to control relative humidity: alternative methods.

Science.gov (United States)

Khalef, Nawel; Pinal, Rodolfo; Bakri, Aziz

2010-04-01

Despite the high sensitivity of isothermal calorimetry (IC), reported measurements of amorphous content by this technique show significant variability even for the same compound. An investigation into the reasons behind such variability is presented using amorphous lactose and salbutamol sulfate as model compounds. An analysis was carried out on the heat evolved as a result of the exchange of water vapor between the solid sample during crystallization and the saline solution reservoir. The use of saturated salt solutions as means of control of the vapor pressure of water within sealed ampoules bears inherent limitations that lead in turn to the variability associated with the IC technique. We present an alternative IC method, based on an open cell configuration that effectively addresses the limitations encountered with the sealed ampoule system. The proposed approach yields an integral whose value is proportional to the amorphous content in the sample, thus enabling reliable and consistent quantifications. 2009 Wiley-Liss, Inc. and the American Pharmacists Association

What Can we learn from Raman spectroscopy and model calculations on room temperature ionic liquids?

OpenAIRE

Berg, Rolf W.

2006-01-01

Traditionally ionic liquids involve inorganic hygroscopic substances that need to be contained under protective atmospheres, e.g. in sealed ampoules. Experimental methods to study the chemistry inside closed ampoules are limited, and one popular technique has been and still is Raman scattering because the laser light easily passes through the glassy ampoule wall. The method is of course equally valuable for non-hygroscopic substances and mixtures and “green liquids”. Raman spectra - though ch...

Solidification of eutectic system alloys in space (M-19)

Science.gov (United States)

Ohno, Atsumi

1993-01-01

cast by the Ohno Continuous Casting Process and they show the unidirectionally solidified structure. Each flight and ground sample was made of these same rods. The dimensions of all samples are 4.5 mm in diameter and 23.5 mm in length. Each sample is put in a graphite capsule and then vacuum sealed in a double silica ampoule. Then the ampoule is put in the tantalum cartridge and sealed by electron beam welding. For onbard experiments, a Continuous Heating Furnance (CHF) will be used for melting and solidifying samples under microgravity conditions. Six flight samples will be used. Four samples are hypo-eutectic and two are hyper-eutectic alloys. The surface of the two hypo-eutectic alloy samples are covered with aluminum oxide film to prevent Marangoni convection expected under microgravity conditions. Each sample will be heated to 700 C and held at that temperature for 5 min. After that the samples will be allowed to cool to 500 C in the furnace and they will be taken out of the furnace for He gas cooling. The heating and cooling diagrams for the flight experiments are shown. After collecting the flight samples, the solidified structures of the samples will be examined and the mechanisms of eutectic solidification under microgravity conditions will be determined. It is likely that successful flight experiment results will lead to production of high quality eutectic alloys and eutectic composite materials in space.

Process for obtaining oxygen doped zinc telluride monocrystals and scintillator crystals obtained by this process

International Nuclear Information System (INIS)

Schneider, Maurice; Moreau, Roland; D'Haenen, J.-P.; Merenda, Pierre.

1976-01-01

A process is described for obtaining oxygen doped zinc telluride monocrystals, for use as scintillator crystals for ionising radiation detectors. The following operations are carried out in succession: one or several zinc telluride crystals are introduced into a silica ampoule together with a ternary mixture of zinc tellurium and oxygen, as an oxide or hydroxide of these elements; the ampoule is pumped down to a high vacuum and sealed; the sealed ampoule containing the mixture and monocrystals is placed in a kiln and brought to a uniform temperature sufficient to make the mixture three-phased, depending on its composition; the zinc telluride crystalline compound remains solid; the ampoule is then tempered to bring it quickly back to ambient temperature [fr

Analysis of intraosseous samples in endotoxemic shock--an experimental study in the anaesthetised pig.

Science.gov (United States)

Strandberg, G; Larsson, A; Lipcsey, M; Berglund, L; Eriksson, M

2014-03-01

Intraosseous (IO) access is used in emergency situations to allow rapid initiation of treatment. IO access is also sometimes used for blood sampling, although data on accuracy of such sampling in critical illness are limited. There is also a potential risk that bone marrow fragments in IO samples may damage laboratory equipment. It is ethically questionable to perform a simultaneous comparison between IO and arterial/venous sampling in critically ill humans. We have, thus, studied the analytical performance of IO sampling in a porcine septic shock model using a cartridge-based analyser. Eight pigs with endotoxin-induced septic shock were sampled hourly for 6 h, and analysed for blood gases, acid base status, haemoglobin, glucose and lactate using point of care instruments. Samples were taken from three IO cannulae (tibia bilaterally, one with infusion, and humerus), one arterial and one venous. An interaction test was used to assess changes in agreement between methods over time. Bland–Altman plots were constructed to study bias between methods. There were, to a varying extent, differences between IO and arterial/venous levels for all studied variables, but agreement did not change significantly during the experiment. A general finding was a large dispersion of differences between methods. IO sample values should be treated with caution in this setting but may add useful information to the clinical picture. The tibia or humerus may be used for sampling. IO infusion decreases agreement, thus sampling during infusion should be avoided.

Multi-class multi-residue analysis of veterinary drugs in meat using enhanced matrix removal lipid cleanup and liquid chromatography-tandem mass spectrometry.

Science.gov (United States)

Zhao, Limian; Lucas, Derick; Long, David; Richter, Bruce; Stevens, Joan

2018-05-11

This study presents the development and validation of a quantitation method for the analysis of multi-class, multi-residue veterinary drugs using lipid removal cleanup cartridges, enhanced matrix removal lipid (EMR-Lipid), for different meat matrices by liquid chromatography tandem mass spectrometry detection. Meat samples were extracted using a two-step solid-liquid extraction followed by pass-through sample cleanup. The method was optimized based on the buffer and solvent composition, solvent additive additions, and EMR-Lipid cartridge cleanup. The developed method was then validated in five meat matrices, porcine muscle, bovine muscle, bovine liver, bovine kidney and chicken liver to evaluate the method performance characteristics, such as absolute recoveries and precision at three spiking levels, calibration curve linearity, limit of quantitation (LOQ) and matrix effect. The results showed that >90% of veterinary drug analytes achieved satisfactory recovery results of 60-120%. Over 97% analytes achieved excellent reproducibility results (relative standard deviation (RSD) meat matrices. The matrix co-extractive removal efficiency by weight provided by EMR-lipid cartridge cleanup was 42-58% in samples. The post column infusion study showed that the matrix ion suppression was reduced for samples with the EMR-Lipid cartridge cleanup. The reduced matrix ion suppression effect was also confirmed with 30%) for all tested veterinary drugs in all of meat matrices. The results showed that the two-step solid-liquid extraction provides efficient extraction for the entire spectrum of veterinary drugs, including the difficult classes such as tetracyclines, beta-lactams etc. EMR-Lipid cartridges after extraction provided efficient sample cleanup with easy streamlined protocol and minimal impacts on analytes recovery, improving method reliability and consistency. Copyright © 2018 Elsevier B.V. All rights reserved.

Determination of As(III) and total inorganic As in water samples using an on-line solid phase extraction and flow injection hydride generation atomic absorption spectrometry

International Nuclear Information System (INIS)

Sigrist, Mirna; Albertengo, Antonela; Beldomenico, Horacio; Tudino, Mabel

2011-01-01

A simple and robust on-line sequential injection system based on solid phase extraction (SPE) coupled to a flow injection hydride generation atomic absorption spectrometer (FI-HGAAS) with a heated quartz tube atomizer (QTA) was developed and optimized for the determination of As(III) in groundwater without any kind of sample pretreatment. The method was based on the selective retention of inorganic As(V) that was carried out by passing the filtered original sample through a cartridge containing a chloride-form strong anion exchanger. Thus the most toxic form, inorganic As(III), was determined fast and directly by AsH 3 generation using 3.5 mol L -1 HCl as carrier solution and 0.35% (m/v) NaBH 4 in 0.025% NaOH as the reductant. Since the uptake of As(V) should be interfered by several anions of natural occurrence in waters, the effect of Cl - , SO 4 2- , NO 3 - , HPO 4 2- , HCO 3 - on retention was evaluated and discussed. The total soluble inorganic arsenic concentration was determined on aliquots of filtered samples acidified with concentrated HCl and pre-reduced with 5% KI-5% C 6 H 8 O 6 solution. The concentration of As(V) was calculated by difference between the total soluble inorganic arsenic and As(III) concentrations. Detection limits (LODs) of 0.5 μg L -1 and 0.6 μg L -1 for As(III) and inorganic total As, respectively, were obtained for a 500 μL sample volume. The obtained limits of detection allowed testing the water quality according to the national and international regulations. The analytical recovery for water samples spiked with As(III) ranged between 98% and 106%. The sampling throughput for As(III) determination was 60 samples h -1 . The device for groundwater sampling was especially designed for the authors. Metallic components were avoided and the contact between the sample and the atmospheric oxygen was carried to a minimum. On-field arsenic species separation was performed through the employ of a serial connection of membrane filters and

A Fully Automated Radiosynthesis of [18F]Fluoroethyl-Diprenorphine on a Single Module by Use of SPE Cartridges for Preparation of High Quality 2-[18F]Fluoroethyl Tosylate

Directory of Open Access Journals (Sweden)

Gjermund Henriksen

2013-06-01

Full Text Available We have developed a new method for automated production of 2-[18F]fluoroethyl tosylate ([18F]FETos that enables 18F-alkylation to provide PET tracers with high chemical purity. The method is based on the removal of excess ethylene glycol bistosylate precursor by precipitation and subsequent filtration and purification of the filtrate by means of solid phase extraction cartridges (SPE. The method is integrated to a single synthesis module and thereby provides the advantage over previous methods of not requiring HPLC purification, as demonstrated by the full radiosynthesis of the potent opioid receptor PET tracer [18F]fluoroethyldiprenorphine.

Primary Dendrite Arm Spacing and Trunk Diameter in Al-7-Weight-Percentage Si Alloy Directionally Solidified Aboard the International Space Station

Science.gov (United States)

Ghods, M.; Tewari, S. N.; Lauer, M.; Poirier, D. R.; Grugel, R. N.

2016-01-01

Under a NASA-ESA collaborative research project, three Al-7-weight-percentage Si samples (MICAST-6, MICAST-7 and MICAST 2-12) were directionally solidified aboard the International Space Station to determine the effect of mitigating convection on the primary dendrite array. The samples were approximately 25 centimeters in length with a diameter of 7.8 millimeter-diameter cylinders that were machined from [100] oriented terrestrially grown dendritic Al-7Si samples and inserted into alumina ampoules within the Sample Cartridge Assembly (SCA) inserts of the Low Gradient Furnace (LGF). The feed rods were partially remelted in space and directionally solidified to effect the [100] dendrite-orientation. MICAST-6 was grown at 5 microns per second for 3.75 centimeters and then at 50 microns per second for its remaining 11.2 centimeters of its length. MICAST-7 was grown at 20 microns per second for 8.5 centimeters and then at 10 microns per second for 9 centimeters of its remaining length. MICAST2-12 was grown at 40 microns per second for 11 centimeters. The thermal gradient at the liquidus temperature varied from 22 to 14 degrees Kelvin per centimeter during growth of MICAST-6, from 26 to 24 degrees Kelvin per centimeter for MICAST-7 and from 33 to 31 degrees Kelvin per centimeter for MICAST2-12. Microstructures on the transverse sections along the sample length were analyzed to determine nearest-neighbor spacing of the primary dendrite arms and trunk diameters of the primary dendrite-arrays. This was done along the lengths where steady-state growth prevailed and also during the transients associated with the speed-changes. The observed nearest-neighbor spacings during steady-state growth of the MICAST samples show a very good agreement with predictions from the Hunt-Lu primary spacing model for diffusion controlled growth. The observed primary dendrite trunk diameters during steady-state growth of these samples also agree with predictions from a coarsening-based model

Applied Sciences Department (R&D) Patents; a Compilation

Science.gov (United States)

1978-12-28

References Cited the first ampoule so that the two ampoules can he bro- UNITED STATES PATENTS ken simultaneously, and, upon mixing of the chemilu...Che-V222/541 miluminescent material and the other ampoule con-.tains an activator material. The almpoules can be bro-(561 References Cited ken by...Eaminer.-Robe" F. Stshl Aimmweys- Edgar J. broere. Ii. H Loach . and Paul S. isat `PYROTECHNCIGNALING ID E 1cER IT4 COMtPiOm WA!Eft EACTII’tIGN11M 4

Investigation of Filtration Membranes from the Dairy Protein Industry for Residual Fouling Using Infrared Spectroscopy and Chemometrics

DEFF Research Database (Denmark)

Jensen, Jannie Krog

the reversible fouling can be removed/cleaned. The aim of this thesis is to investigate the residual fouling that is deposited on ultrafiltration and microfiltration membranes after usage. The membrane surfaces are investigated using infrared spectroscopy with an attenuated reflectance sampling unit...... and this is thesis work highlights the strengths and weaknesses of using infrared spectroscopy to investigate residual fouling on membranes and in particular the challenges with the infrared penetration depth when layering in the samples occurs. Real size production membrane cartridges at different stages of use...... microfiltration membrane cartridges were investigated with Attenuated- Total-Reflection Fourier-Transform-Infrared (ATR FT-IR) to map the residual fouling on both types of cartridges. The height of the characteristic amide peaks from proteins were used to determine the relative concentrations. The first...

Isolation of dissolved organic matter from permafrost soil and freshwater environments of the Kolyma River basin, east Siberia, for high resolution structural analysis

Science.gov (United States)

Dubinenkov, I. V.; Perminova, I. V.; Bulygina, E. B.; Holmes, R. M.; Davydov, S.; Mann, P. J.; Vonk, J.; Zimov, S. A.

2010-12-01

The Arctic and Subarctic ecosystems are known to be the most vulnerable with respect to climate change. Hence, research on carbon cycling in the Arctic region is very important for understanding the current climatic trends and their consequences. The Kolyma River watershed is one of the Arctic Ocean’s largest. It is dominated by continuous permafrost which is underlain with rich organic soils susceptible to increased fluvial transport. The thaw of permafrost enhanced due to global warming might provide additional large source of organic carbon to the Kolyma River and to the Arctic Ocean as a whole. For estimating the contribution of this source to the total pool of organic carbon, specific structural features of permafrost dissolved organic matter (DOM) as opposed to the waterborne DOM of the Kolyma River should be identified and monitored. The objective of this work was to isolate a representive set of the DOM samples from permafrost soil and freshwater environments of the Kolyma River basin suitable for further structural analysis using high resolution Fourier Transform Ion Cyclotron Resonance Mass Spectroscopy (FTICR-MS) and 1H NMR spectroscopy. The isolation protocol of DOM used in this study has been developed by Dittmar et al, 2008 for sampling marine DOM for NMR studies. It is based on the solid phase extraction of DOM from seawater using PPL Varian Bond Elute cartridges Those cartridges were shown to possess the highest efficiency in DOM isolation from marine water. Prior to discharge through the cartridge, a water sample was filtered through 0.45 μm filter for separation of particulate matter and acidified to pH 2 using HCl. About 50mg of DOM could be sequestered from aqueous phase using one cartridge. Sorption extent was monitored by measurements of DOC concentration and UV-vis spectra at the inlet and outlet of the cartridge. It was determined that from 60 to 65% of the total DOC could be extracted from the tested samples of freshwater. As a result

Solid-phase extraction of carotenoids.

Science.gov (United States)

Shen, Yao; Hu, Yumin; Huang, Ke; Yin, Shi'an; Chen, Bo; Yao, Shouzhuo

2009-07-24

In this work, solid-phase extraction (SPE) trapping performance of lutein and beta-carotene, which were used as the model molecules of carotenoids, was investigated. The absorption, elution, and enrichment of carotenoids on SPE cartridges with four different sorbents, i.e. C(30), C(18), diol, and silica, were compared respectively with the help of frontal analysis technique. The high retentions of both lutein and beta-carotene were achieved on the C(18) and C(30) cartridges. The diol and silica cartridges only had good retention for lutein. The optimized SPE method for sample pretreatment for the carotenoids analysis was obtained after the investigation of trapping performance. The method was applied successfully to the analysis of biological sample, i.e. serum and human breast milk. The recovery, accuracy, and precision of SPE method comparing with those of traditional liquid-liquid extraction (LLE) method for the sample pretreatment for the analysis of carotenoids owned a number of advantages such as rapid, no chloroform used, and accurate versus LLE.

Detached phenomenon: Its effect on the crystal quality of Ga{sub (1−x)}In{sub x}Sb bulk crystal grown by the VDS technique

Energy Technology Data Exchange (ETDEWEB)

Gadkari, Dattatray, E-mail: db.gadkari@gmail.com [Department of Physics, Mithibai College, Mumbai 400056 (India)

2013-05-15

Vertical directional solidification (VDS) technique is used on the combined growth principals of the conventional methods since 1994, which leads to the detached growth. For evaluation of the detached growth, five bulk ingots of indium doped gallium–antimonide GaSb:In (In = 0.5, 0.25, 0.15) have been grown – without the seed, without contact to the ampoule wall, without coating and without external pressure. The gap is attributed to compensate the differential thermal dilatation that is grown with the reduced diameter than the diameter of the ampoule. VDS experiments have been proved that the sum of the contact angle and growth angle is large enough to allow detachment without any additional pressure difference under the melt to offset hydrostatic pressure. A meniscus forms at the bottom of the melt, the capillarity effect establishes due to which spontaneous gap could be created by the melt free surface, thus no thermal shear stress and thermo-mechanical stresses at the interface. Detached grown bulk GaSb:In crystals showed superior crystal quality with the highest physical properties and mobility than the crystals grown ever. The axial and radial composition profile of the grown GaSb:In ingots showed variation ≤10%. From the conical region, dislocation density decreases in the growth direction and reaches less than 10{sup 3} cm{sup −2}. - Highlights: ► Detachment: without seed, without ampoule contact, without coating, without external pressure. ► Detached ingot growth samples showed the highest physical properties and the carrier mobility. ► Initial to final transition: in detached growth, dislocations decreases and less than 10{sup 3} cm{sup −2}. ► Detached samples: Raman spectrum shows only TO phonon (110) direction of single orientation. ► Detached ingot: FTIR shows highest transmissions % but decreases on increase doping in samples.

Sistema limpo em linha para extração em fase sólida de contaminantes emergentes em águas naturais An in-line clean system for the solid-phase extraction of emerging contaminants in natural waters

Directory of Open Access Journals (Sweden)

Fernando F. Sodré

2010-01-01

Full Text Available A solid-phase in-line extraction system for water samples containing low levels of emerging contaminants is described. The system was specially developed for large volume samples (up to 4 L using commercial solid-phase extraction (SPE cartridges. Four sets containing PTFE-made connectors, brass adapters and ball valves were used to fit SPE cartridges and sample bottles to a 4-port manifold attached to a 20 L carboy. A lab-made vacuum device was connected to the manifold cap. The apparatus is robust and less expensive than the typical available system. Its also provides less experimental handling, avoiding cross contamination and sample losses.

What Can we learn from Raman spectroscopy and model calculations on room temperature ionic liquids?

DEFF Research Database (Denmark)

Berg, Rolf W.

2006-01-01

Traditionally ionic liquids involve inorganic hygroscopic substances that need to be contained under protective atmospheres, e.g. in sealed ampoules. Experimental methods to study the chemistry inside closed ampoules are limited, and one popular technique has been and still is Raman scattering be...

Penetrating chest trauma caused by a blank cartridge actuated rubber ball projectile: case presentation and ballistic investigation of an uncommon weapon type.

Science.gov (United States)

Frank, Matthias; Peters, Dieter; Klemm, Wolfram; Grossjohann, Rico; Ekkernkamp, Axel; Bockholdt, Britta; Seifert, Julia

2017-09-01

Recently, an increasing number of an uncommon weapon type based on a caliber 6-mm Flobert blank cartridge actuated revolver which discharges 10-mm-diameter rubber ball projectiles has been confiscated by police authorities following criminal offenses. A recent trauma case presenting with a penetrating chest injury occasioned an investigation into the basic ballistic parameters of this type of weapon. Kinetic energy E of the test projectiles was calculated between 5.8 and 12.5 J. Energy density ED of the test projectiles was close to or higher than the threshold energy density of human skin. It can be concluded that penetrating skin injuries due to free-flying rubber ball projectiles discharged at close range cannot be ruled out. However, in case of a contact shot, the main injury potential of this weapon type must be attributed to the high energy density of the muzzle gas jet which may, similar to well-known gas or alarm weapons, cause life-threatening or even lethal injuries.

Interface Shape and Convection During Solidification and Melting of Succinonitrile

Science.gov (United States)

Degroh, Henry C., III; Lindstrom, Tiffany

1994-01-01

An experimental study was conducted of the crystal growth of succinonitrile during solidification, melting, and no-growth conditions using a horizontal Bridgman furnace and square glass ampoule. For use as input boundary conditions to numerical codes, thermal profiles on the outside of the ampoule at five locations around its periphery were measured along the ampoule's length. Temperatures inside the ampoule were also measured. The shapes of the s/l interface in various two dimensional planes were quantitatively determined. Though interfaces were nondendritic and noncellular, they were not flat, but were highly curved and symmetric in only one unique longitudinal y-z plane (at x=O). The shapes of the interface were dominated by the primary longitudinal flow cell characteristic of shallow cavity flow in horizontal Bridgman; this flow cell was driven by the imposed furnace temperature gradient and caused a 'radical' thermal gradient such that the upper half of the ampoule was hotter than the bottom half. We believe that due to the strong convection, the release of latent heat does not significantly influence the thermal conditions near the interface. We hope that the interface shape and thermal data presented in this paper can be used to optimize crystal growth processes and validate numerical models.

Determination of carbonyl compounds in air by HPLC

International Nuclear Information System (INIS)

Garcia, S.; Perez, R.M.; Campos, A.; Gonzalez, D.

1995-09-01

A method for the determination of seven carbonyl compounds in air is presented. The procedure involve sampling of air by a Sep-Pak cartridge impregnated with 2,4-dinitrophenylhydrazine. Elution was done with 3 mL of acetonitrile and the eluate was diluted to 5 mL. The analysis was done by HPLC with UV detection and external standard method quantification. It has been achieved relative standard deviations about 5% and detection limits of 80 ng/cartridge for formaldehyde, acetaldehyde and acetone+acrolein. Three different types of samples (rural, urban, petrol emission) were successfully analyzed

Trace determination of 10 beta-lactam antibiotics in environmental and food samples by capillary liquid chromatography.

Science.gov (United States)

Bailón-Pérez, M I; García-Campaña, A M; del Olmo-Iruela, M; Gámiz-Gracia, L; Cruces-Blanco, C

2009-11-20

A sensitive and reliable method using capillary HPLC with UV-diode array detection (DAD) has been developed and validated for the trace determination of residues of 10 beta-lactam antibiotics of human and veterinary use, in milk, chicken meat and environmental water samples. The analytes included ampicillin, amoxicillin, penicillin V, penicillin G, cloxacillin, oxacillin, dicloxacillin, nafcillin, piperacillin and clavulanic acid. Legal levels are regulated by the EU Council regulation 2377/90 in animal edible tissues for these compounds. For food analysis, a solid-phase extraction (SPE) procedure consisting in a tandem of Oasis HLB and Alumina N cartridges was applied for off-line preconcentration and cleanup. For water analysis, the first step was only necessary. The limits of detection for the studied compounds were between 0.04-0.06 microg l(-1) for water samples and 0.80-1.40 microg l(-1) (or microg kg(-1)) in the case of foods derived from animals. Average recoveries for fortified samples at different concentration levels ranged between 82.9% and 98.2%, with relative standard deviations (RSDs) lower than 9%. The method showed the advantages of capillary HPLC for the detection of these widely applied antibiotics in different samples at very low concentration levels.

Rapid and automated on-line solid phase extraction HPLC-MS/MS with peak focusing for the determination of ochratoxin A in wine samples.

Science.gov (United States)

Campone, Luca; Piccinelli, Anna Lisa; Celano, Rita; Pagano, Imma; Russo, Mariateresa; Rastrelli, Luca

2018-04-01

This study reports a fast and automated analytical procedure based on an on-line SPE-HPLC-MS/MS method for the automatic pre-concentration, clean up and sensitive determination of OTA in wine. The amount of OTA contained in 100μL of sample (pH≅5.5) was retained and concentrated on an Oasis MAX SPE cartridge. After a washing step to remove matrix interferents, the analyte was eluted in back-flush mode and the eluent from the SPE column was diluted through a mixing Tee, using an aqueous solution before the chromatographic separation achieved on a monolithic column. The developed method has been validated according to EU regulation N. 519/2014 and applied for the analysis of 41 red and 17 white wines. The developed method features minimal sample handling, low solvent consumption, high sample throughput, low analysis cost and provides an accurate and highly selective results. Copyright © 2017 Elsevier Ltd. All rights reserved.

Extending laboratory automation to the wards: effect of an innovative pneumatic tube system on diagnostic samples and transport time.

Science.gov (United States)

Suchsland, Juliane; Winter, Theresa; Greiser, Anne; Streichert, Thomas; Otto, Benjamin; Mayerle, Julia; Runge, Sören; Kallner, Anders; Nauck, Matthias; Petersmann, Astrid

2017-02-01

The innovative pneumatic tube system (iPTS) transports one sample at a time without the use of cartridges and allows rapid sending of samples directly into the bulk loader of a laboratory automation system (LAS). We investigated effects of the iPTS on samples and turn-around time (TAT). During transport, a mini data logger recorded the accelerations in three dimensions and reported them in arbitrary area under the curve (AUC) units. In addition representative quantities of clinical chemistry, hematology and coagulation were measured and compared in 20 blood sample pairs transported by iPTS and courier. Samples transported by iPTS were brought to the laboratory (300 m) within 30 s without adverse effects on the samples. The information retrieved from the data logger showed a median AUC of 7 and 310 arbitrary units for courier and iPTS transport, respectively. This is considerably below the reported limit for noticeable hemolysis of 500 arbitrary units. iPTS reduces TAT by reducing the hands-on time and a fast transport. No differences in the measurement results were found for any of the investigated 36 analytes between courier and iPTS transport. Based on these findings the iPTS was cleared for clinical use in our hospital.

Determination of As(III) and total inorganic As in water samples using an on-line solid phase extraction and flow injection hydride generation atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Sigrist, Mirna, E-mail: msigrist@fiq.unl.edu.ar [Laboratorio Central, Facultad de Ingenieria Quimica, Universidad Nacional del Litoral, Santiago del Estero 2654-Piso 6, (3000) Santa Fe (Argentina); Albertengo, Antonela; Beldomenico, Horacio [Laboratorio Central, Facultad de Ingenieria Quimica, Universidad Nacional del Litoral, Santiago del Estero 2654-Piso 6, (3000) Santa Fe (Argentina); Tudino, Mabel [Laboratorio de Analisis de Trazas, Departamento de Quimica Inorganica, Analitica y Quimica Fisica/INQUIMAE, Facultad de Ciencias Exactas y Naturales, Pabellon II, Ciudad Universitaria (1428), Buenos Aires (Argentina)

2011-04-15

A simple and robust on-line sequential injection system based on solid phase extraction (SPE) coupled to a flow injection hydride generation atomic absorption spectrometer (FI-HGAAS) with a heated quartz tube atomizer (QTA) was developed and optimized for the determination of As(III) in groundwater without any kind of sample pretreatment. The method was based on the selective retention of inorganic As(V) that was carried out by passing the filtered original sample through a cartridge containing a chloride-form strong anion exchanger. Thus the most toxic form, inorganic As(III), was determined fast and directly by AsH{sub 3} generation using 3.5 mol L{sup -1} HCl as carrier solution and 0.35% (m/v) NaBH{sub 4} in 0.025% NaOH as the reductant. Since the uptake of As(V) should be interfered by several anions of natural occurrence in waters, the effect of Cl{sup -}, SO{sub 4}{sup 2-}, NO{sub 3}{sup -}, HPO{sub 4}{sup 2-}, HCO{sub 3}{sup -} on retention was evaluated and discussed. The total soluble inorganic arsenic concentration was determined on aliquots of filtered samples acidified with concentrated HCl and pre-reduced with 5% KI-5% C{sub 6}H{sub 8}O{sub 6} solution. The concentration of As(V) was calculated by difference between the total soluble inorganic arsenic and As(III) concentrations. Detection limits (LODs) of 0.5 {mu}g L{sup -1} and 0.6 {mu}g L{sup -1} for As(III) and inorganic total As, respectively, were obtained for a 500 {mu}L sample volume. The obtained limits of detection allowed testing the water quality according to the national and international regulations. The analytical recovery for water samples spiked with As(III) ranged between 98% and 106%. The sampling throughput for As(III) determination was 60 samples h{sup -1}. The device for groundwater sampling was especially designed for the authors. Metallic components were avoided and the contact between the sample and the atmospheric oxygen was carried to a minimum. On-field arsenic species

A simple and selective method for determination of phthalate biomarkers in vegetable samples by high pressure liquid chromatography-electrospray ionization-tandem mass spectrometry.

Science.gov (United States)

Zhou, Xi; Cui, Kunyan; Zeng, Feng; Li, Shoucong; Zeng, Zunxiang

2016-06-01

In the present study, solid-phase extraction cartridges including silica reversed-phase Isolute C18, polymeric reversed-phase Oasis HLB and mixed-mode anion-exchange Oasis MAX, and liquid-liquid extractions with ethyl acetate, n-hexane, dichloromethane and its mixtures were compared for clean-up of phthalate monoesters from vegetable samples. Best recoveries and minimised matrix effects were achieved using ethyl acetate/n-hexane liquid-liquid extraction for these target compounds. A simple and selective method, based on sample preparation by ultrasonic extraction and liquid-liquid extraction clean-up, for the determination of phthalate monoesters in vegetable samples by liquid chromatography/electrospray ionisation-tandem mass spectrometry was developed. The method detection limits for phthalate monoesters ranged from 0.013 to 0.120 ng g(-1). Good linearity (r(2)>0.991) between MQLs and 1000× MQLs was achieved. The intra- and inter-day relative standard deviation values were less than 11.8%. The method was successfully used to determine phthalate monoester metabolites in the vegetable samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

Surface deposition measurements of the TMI-2 gross decontamination experiment

International Nuclear Information System (INIS)

McIssac, C.V.; Hetzer, D.C.

1982-01-01

In order to measure the effectiveness of the gross decontamination experiment (principally a water spray technique) performed in the TMI-2 reactor building, the Technical Information and Examination Program's Radiation and Environment personnel made surface activity measurements before and after the experiment. In conjunction with surface sampling, thermoluminescent dosimeter (TLD) and gamma spectrometry measurements were also performed to distinguish between radiation fields and contamination. The surface sampler used to collect samples from external surfaces within the reactor building is a milling tool having four major components: a 1.27-cm constant-speed drill; a drill support assembly that allows setting sample penetration depth; filter cartridges for intake air purification and sample collection; and an air pump that forces air across the surface being sampled and through the sample filter cartridge

Application of activated carbon fiber to a filter used for airborne radioiodine sampling

International Nuclear Information System (INIS)

Kato, Shohei; Murata, Mikio; Yoshikazu, Yoshida

1988-01-01

An airborne radioiodine sampling filter is required to have low pressure drop, mechanical strength enough to a practical use and high collection efficiency under high relative humidity(RH). To develop a filter to meet the requirements, the influences of impregnation amount of triethylenediamin(TEDA) on the collection efficiencies for methyl iodide and the reaction rates were investigated for several kinds of activated carbon fiber varied in specific surface area, pore diameter, etc. Silver silica gel(Sut Chemi, AC6120), silver zeolite(CTI Nuc., AgX Type III), silver alumina(Hitachi Co.) and granular activated charcoal were also examined for comparison. A new type filter made of activated carbon fiber (ACF filter) was developed based on the above experimental results. The ACF filter was examined for the pressure drop by the filter and collection efficiency for methyl iodide being compared with other types of filters such as an activated charcoal cartridge (ACC) and an activated charcoal filter paper (ACP)

Supercritical fluid extraction and ultra performance liquid chromatography of respiratory quinones for microbial community analysis in environmental and biological samples.

Science.gov (United States)

Hanif, Muhammad; Atsuta, Yoichi; Fujie, Koichi; Daimon, Hiroyuki

2012-03-05

Microbial community structure plays a significant role in environmental assessment and animal health management. The development of a superior analytical strategy for the characterization of microbial community structure is an ongoing challenge. In this study, we developed an effective supercritical fluid extraction (SFE) and ultra performance liquid chromatography (UPLC) method for the analysis of bacterial respiratory quinones (RQ) in environmental and biological samples. RQ profile analysis is one of the most widely used culture-independent tools for characterizing microbial community structure. A UPLC equipped with a photo diode array (PDA) detector was successfully applied to the simultaneous determination of ubiquinones (UQ) and menaquinones (MK) without tedious pretreatment. Supercritical carbon dioxide (scCO(2)) extraction with the solid-phase cartridge trap proved to be a more effective and rapid method for extracting respiratory quinones, compared to a conventional organic solvent extraction method. This methodology leads to a successful analytical procedure that involves a significant reduction in the complexity and sample preparation time. Application of the optimized methodology to characterize microbial communities based on the RQ profile was demonstrated for a variety of environmental samples (activated sludge, digested sludge, and compost) and biological samples (swine and Japanese quail feces).

Development and optimization of the determination of pharmaceuticals in water samples by SPE and HPLC with diode-array detection.

Science.gov (United States)

Pavlović, Dragana Mutavdžić; Ašperger, Danijela; Tolić, Dijana; Babić, Sandra

2013-09-01

This paper describes the development, optimization, and validation of a method for the determination of five pharmaceuticals from different therapeutic classes (antibiotics, anthelmintics, glucocorticoides) in water samples. Water samples were prepared using SPE and extracts were analyzed by HPLC with diode-array detection. The efficiency of 11 different SPE cartridges to extract the investigated compounds from water was tested in preliminary experiments. Then, the pH of the water sample, elution solvent, and sorbent mass were optimized. Except for optimization of the SPE procedure, selection of the optimal HPLC column with different stationary phases from different manufacturers has been performed. The developed method was validated using spring water samples spiked with appropriate concentrations of pharmaceuticals. Good linearity was obtained in the range of 2.4-200 μg/L, depending on the pharmaceutical with the correlation coefficients >0.9930 in all cases, except for ciprofloxacin (0.9866). Also, the method has revealed that low LODs (0.7-3.9 μg/L), good precision (intra- and interday) with RSD below 17% and recoveries above 98% for all pharmaceuticals. The method has been successfully applied to the analysis of production wastewater samples from the pharmaceutical industry. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Tandem Solid Phase Extraction for the Determination of Pharmaceuticals in Wastewater

International Nuclear Information System (INIS)

Licaberth Ismail; Rozita Osman; Norashikin Saim

2013-01-01

In this study, a simple and rapid tandem solid phase extraction (SPE) was developed for the analysis of seven pharmaceuticals (acetaminophen, caffeine, carbamazepine, diclofenac, naproxen, ibuprofen and metaprolol) in wastewater sample. The novel aspect of coupling SPE cartridge in tandem is the ability to simplify the SPE procedure (sample introduction step) as no single sorbent was able to retain and concentrate all selected compounds since these compounds are of different physicochemical properties. A tandem SPE cartridges using Oasis HLB and octadecyl bonded silica (C 18 ) was found to be efficient with the advantages of minimizing sample volume and reducing analysis time. Using this approach, carbamazepine, diclofenac, naproxen and metaprolol were trapped in the Oasis HLB while acetaminophen, caffeine and ibuprofen were trapped in the second cartridge (C 18 ). The instrumental limits of detection (LOD) ranged from 0.01 to 0.04 μg/ L and satisfactory recoveries were obtained between 76 % to 104 %. The calibration curves were linear from 0.1 to 5.0 μg/ mL, with correlation coefficients (R 2 ) in the range of 0.995 to 0.999. The developed method was applied to the analysis of pharmaceuticals in wastewater samples. The amount of pharmaceuticals detected in wastewater samples varied from 0.4 to 24.5 mg/ L. (author)

Determination of dimethyltryptamine and β-carbolines (ayahuasca alkaloids) in plasma samples by LC-MS/MS.

Science.gov (United States)

Oliveira, Carolina Dizioli Rodrigues; Okai, Guilherme Gonçalves; da Costa, José Luiz; de Almeida, Rafael Menck; Oliveira-Silva, Diogo; Yonamine, Mauricio

2012-07-01

Ayahuasca is a psychoactive plant beverage originally used by indigenous people throughout the Amazon Basin, long before its modern use by syncretic religious groups established in Brazil, the USA and European countries. The objective of this study was to develop a method for quantification of dimethyltryptamine and β-carbolines in human plasma samples. The analytes were extracted by means of C18 cartridges and injected into LC-MS/MS, operated in positive ion mode and multiple reaction monitoring. The LOQs obtained for all analytes were below 0.5 ng/ml. By using the weighted least squares linear regression, the accuracy of the analytical method was improved at the lower end of the calibration curve (from 0.5 to 100 ng/ml; r(2)> 0.98). The method proved to be simple, rapid and useful to estimate administered doses for further pharmacological and toxicological investigations of ayahuasca exposure.

Selective trace enrichment of chlorotriazine pesticides from natural waters and sediment samples using terbuthylazine molecularly imprinted polymers

Science.gov (United States)

Ferrer, I.; Lanza, F.; Tolokan, A.; Horvath, V.; Sellergren, B.; Horvai, G.; Barcelo, D.

2000-01-01

Two molecularly imprinted polymers were synthesized using either dichloromethane or toluene as the porogen and terbuthylazine as the template and were used as solid-phase extraction cartridges for the enrichment of six chlorotriazines (deisopropylatrazine, deethylatrazine, simazine, atrazine, propazine, and terbuthylazine) in natural water and sediment samples. The extracted samples were analyzed by liquid chromatography/diode array detection (LC/DAD). Several washing solvents, as well as different volumes, were tested for their ability to remove the matrix components nonspecifically adsorbed on the sorbents. This cleanup step was shown to be of prime importance to the successful extraction of the pesticides from the aqueous samples. The optimal analytical conditions were obtained when the MIP imprinted using dichloromethane was the sorbent, 2 mL of dichloromethane was used in the washing step, and the preconcentrated analytes were eluted with 8 mL of methanol. The recoveries were higher than 80% for all the chlorotriazines except for propazine (53%) when 50- or 100-mL groundwater samples, spiked at 1 ??g/L level, were analyzed. The limits of detection varied from 0.05 to 0.2 ??g/L when preconcentrating a 100-mL groundwater sample. Natural sediment samples from the Ebre Delta area (Tarragona, Spain) containing atrazine and deethylatrazine were Soxhlet extracted and analyzed by the methodology developed in this work. No significant interferences from the sample matrix were noticed, thus indicating good selectivity of the MIP sorbents used.

Determination of carbonyl compounds in air by HPLC

International Nuclear Information System (INIS)

Garcia, S.; Perez, R.M.; Campos, A.; Gonzalez, D.

1995-01-01

A method for the determination of seven carbonyl compounds in air is presented. The procedure involve sampling of air by a Sep-Pak Cartridge impregnated with 2,4-dinitrophenylhydrazine. Elution was done with 3 mL of acetonitrile and the eluate was diluted to 5 mL. The analysis was done by HPLC with UV detection and external standard method quantification. It has been achieved relative standard deviations about 5% and detection limits of 80 ng/cartridge for formaldehyde, acetaldehyde and acetoacetonitrile. Three different types of samples (rural, urban, petrol emission) were successfully analyzed. (Author) 12 refs

Determination of carbonyl compounds in air by HPLC; Determinacion de compuestos carbonilicos en aire por HPLC

Energy Technology Data Exchange (ETDEWEB)

Garcia, S; Perez, R M; Campos, A; Gonzalez, D

1995-07-01

A method for the determination of seven carbonyl compounds in air is presented. The procedure involve sampling of air by a Sep-Pak Cartridge impregnated with 2,4-dinitrophenylhydrazine. Elution was done with 3 mL of acetonitrile and the eluate was diluted to 5 mL. The analysis was done by HPLC with UV detection and external standard method quantification. It has been achieved relative standard deviations about 5% and detection limits of 80 ng/cartridge for formaldehyde, acetaldehyde and acetoacetonitrile. Three different types of samples (rural, urban, petrol emission) were successfully analyzed. (Author) 12 refs.

Analytical and pre-analytical performance characteristics of a novel cartridge-type blood gas analyzer for point-of-care and laboratory testing.

Science.gov (United States)

Oyaert, Matthijs; Van Maerken, Tom; Bridts, Silke; Van Loon, Silvi; Laverge, Heleen; Stove, Veronique

2018-03-01

Point-of-care blood gas test results may benefit therapeutic decision making by their immediate impact on patient care. We evaluated the (pre-)analytical performance of a novel cartridge-type blood gas analyzer, the GEM Premier 5000 (Werfen), for the determination of pH, partial carbon dioxide pressure (pCO 2 ), partial oxygen pressure (pO 2 ), sodium (Na + ), potassium (K + ), chloride (Cl - ), ionized calcium ( i Ca 2+ ), glucose, lactate, and total hemoglobin (tHb). Total imprecision was estimated according to the CLSI EP5-A2 protocol. The estimated total error was calculated based on the mean of the range claimed by the manufacturer. Based on the CLSI EP9-A2 evaluation protocol, a method comparison with the Siemens RapidPoint 500 and Abbott i-STAT CG8+ was performed. Obtained data were compared against preset quality specifications. Interference of potential pre-analytical confounders on co-oximetry and electrolyte concentrations were studied. The analytical performance was acceptable for all parameters tested. Method comparison demonstrated good agreement to the RapidPoint 500 and i-STAT CG8+, except for some parameters (RapidPoint 500: pCO 2 , K + , lactate and tHb; i-STAT CG8+: pO 2 , Na + , i Ca 2+ and tHb) for which significant differences between analyzers were recorded. No interference of lipemia or methylene blue on CO-oximetry results was found. On the contrary, significant interference for benzalkonium and hemolysis on electrolyte measurements were found, for which the user is notified by an interferent specific flag. Identification of sample errors from pre-analytical sources, such as interferences and automatic corrective actions, along with the analytical performance, ease of use and low maintenance time of the instrument, makes the evaluated instrument a suitable blood gas analyzer for both POCT and laboratory use. Copyright © 2018 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

Microfluidic system for the identification of bacterial pathogens causing urinary tract infections

Science.gov (United States)

Becker, Holger; Hlawatsch, Nadine; Haraldsson, Tommy; van der Wijngaart, Wouter; Lind, Anders; Malhotra-Kumar, Surbi; Turlej-Rogacka, Agata; Goossens, Herman

2015-03-01

Urinary tract infections (UTIs) are among the most common bacterial infections and pose a significant healthcare burden. The growing trend in antibiotic resistance makes it mandatory to develop diagnostic kits which allow not only the determination of a pathogen but also the antibiotic resistances. We have developed a microfluidic cartridge which takes a direct urine sample, extracts the DNA, performs an amplification using batch-PCR and flows the sample over a microarray which is printed into a microchannel for fluorescence detection. The cartridge is injection-molded out of COP and contains a set of two-component injection-molded rotary valves to switch between input and to isolate the PCR chamber during thermocycling. The hybridization probes were spotted directly onto a functionalized section of the outlet microchannel. We have been able to successfully perform PCR of E.coli in urine in this chip and perform a fluorescence detection of PCR products. An upgraded design of the cartridge contains the buffers and reagents in blisters stored on the chip.

Determination of proguanil and metabolites in small sample volumes of whole blood stored on filter paper by high-performance liquid chromatography.

Science.gov (United States)

Kolawole, J A; Taylor, R B; Moody, R R

1995-12-01

A method is reported for the determination of proguanil and its two metabolites cycloguanil and 4-chlorophenylbiguanide in whole blood and plasma samples obtained by thumbprick and stored dry on filter paper. The sample preparation involves liquid extraction from the filter paper and subsequent solid-phase extraction using C8 Bond-Elut cartridges. Separation and quantification is by a previously reported ion-pairing high-performance liquid chromatographic system with ODS Hypersil as stationary phase and an 50:50 acetonitrile-pH 2 phosphate buffer mobile phase containing 200 mM sodium dodecylsulphate as ion-pairing agent. The analytical characteristics of the method are reported. Representative concentrations are shown as a function of time from a human subject after ingestion of a single 200-mg dose of proguanil hydrochloride. Typical ranges of concentration detected by the proposed method in human subjects were proguanil 12-900 ng/ml, cycloguanil 16-44 ng/ml and 4-chlorophenylbiguanide 1.5-10 ng/ml in whole blood.

Radiography technique

Energy Technology Data Exchange (ETDEWEB)

Panaiotov, L N

1951-10-23

A new method of hollow articles radiography is presented enabling to eliminate shortcomings coupled with medical personnel irradiation when the ampoule incorporating radioactive substance is removed from the protective container and adjusted in the article. The method presented permits to transport the ampoule from the protective container immediately into the inner cavity of the article.

Device for sampling sodium from a circuit with a view to dosing its impurities (1963); Dispositif de prelevement de sodium sur un cuicuit en vue du dosage des impuretes (1063)

Energy Technology Data Exchange (ETDEWEB)

Sannier, J; Vingot, P [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

1963-07-01

The device described was developed with the two following essential conditions in mind: - absence of any pollution during the sampling operation and the transfer to the analysis apparatus; - simultaneous extraction of several samples, each one remaining representative of the sodium in the circuit. The sampling is therefore carried out completely in a vacuum in a Pyrex-glass apparatus, this limiting the sodium temperature to a maximum of 240 deg. C. The samples are in the form of bulbs sealed in vacuo containing 2 to 3 grams of sodium each. The analysis of the oxygen by the amalgamation technique, carried out on samples obtained by this method show a very satisfactory reproducibility for concentrations of under 20 ppm. (authors) [French] Le dispositif decrit a ete mis au point compte tenu des deux imperatifs essentiels suivants: - absence de toute pollution pendant les operations de prelevement et de transport vers l'appareil d'analyse; - obtention simultanee de plusieurs echantillons, chacun restant representatif du sodium du circuit. A cet effet, le prelevement est effectue entierement sous vide dans un appareillage en verre Pyrex, ce qui limite la temperature du sodium a 240 deg. C. Les echantillons se presentent sous la forme d'ampoules scellees sous vide et contenant chacune 2 a 3 grammes de sodium. L'analyse de l'oxygene par la technique d'amalgamation, effectuee sur des echantillons preleves par cette methode, revele une reproductibilite tres satisfaisante, dans le domaine des teneurs inferieures a 20 ppm. (auteurs)

Influence of Contact Angle, Growth Angle and Melt Surface Tension on Detached Solidification of InSb

Science.gov (United States)

Wang, Yazhen; Regel, Liya L.; Wilcox, William R.

2000-01-01

We extended the previous analysis of detached solidification of InSb based on the moving meniscus model. We found that for steady detached solidification to occur in a sealed ampoule in zero gravity, it is necessary for the growth angle to exceed a critical value, the contact angle for the melt on the ampoule wall to exceed a critical value, and the melt-gas surface tension to be below a critical value. These critical values would depend on the material properties and the growth parameters. For the conditions examined here, the sum of the growth angle and the contact angle must exceed approximately 130, which is significantly less than required if both ends of the ampoule are open.

Production of reference enteroviruses.

Science.gov (United States)

Kalter, S S; Rodriguez, A R; Armour, V

1968-10-01

Forty-five human enterovirus reagents of certified purity and quality were prepared for use as seed viruses and as immunizing antigens. One of the reagents was ampouled as "untreated" seed virus, whereas 14 were ampouled as "MgCl(2)-stabilized" reagents. The remaining 30 reagents were ampouled as "untreated" seed viruses and as "MgCl(2)-stabilized" reagents. Thirty of the reagents were propagated on primary African green monkey kidney cells, 3 on primary baboon kidney cells, 3 on primary rhesus monkey kidney cells, and the remaining 9 on human amnion cells. Forty-two of the viral antigens were concentrated for use in the production of high-titered specific antisera in large animals.

Optical band gap of Sn0⋅2Bi1⋅8Te3 thin films

Indian Academy of Sciences (India)

Unknown

tors, thermocouples, thermo coolers and IR sensors with the best figure of merit near room temperature (Roy et al. 1978; Jeon et al 1981; Rowe and Bandari 1981; Good- ... pressure used to seal the quartz ampoules containing the charge was of the order of 10–5 Pa. The sealed ampoule was kept in an alloy mixing furnace, ...

A numerical study of thermal conditions in the THM growth of HgTe

Science.gov (United States)

Martínez-Tomás, M. C.; Muñoz-Sanjosé, V.; Reig, C.

2002-09-01

A numerical simulation of the travelling heater method (THM) process in the growth of HgTe is carried out. The whole system (furnace, ampoule and charge) is taken into account in the frame of a quasi-steady-state model. The mass conservation condition for the solute in the liquid zone permits the determination of the rate of advance of the crystallisation isotherm as a function of the heater position. We claim to study the evolution of different magnitudes along the growth process, searching for the physical reasons which could be at the origin of defects in the form of thin layers observed in some growing experiences. To solve the governing equations of fluid flow, heat transfer and mass transport we have made use of a commercial code which can run in a PC. The simulation is made by using a three-level strategy, which allows the reduction of the computational effort. In the first level, heat transport is assumed to be by conduction, convection and radiation between the furnace and the ampoule, and by conduction through the ampoule wall, coating, solid and liquid zones. The temperature calculated at this level in the air/ampoule boundary is used as boundary condition for the second and third level. In these two levels the ampoule and its content are studied in detail. Convection in the liquid zone is considered at the second level and thermosolutal convection is finally included at the third level. The analysis of the incoming/outcoming heat flux per second through the ampoule for the whole system shows that the lower part of the ampoule exhibits some ineffectiveness for the heat evacuation at certain positions of the growth run, depending on thermal properties of the whole system and the particular material to be grown. As a consequence, the growth rate suffers a significant variation just for these positions of the heater. From these considerations a plausible interpretation has been proposed to understand the apparition of solvent inclusions in the form of thin

Solid-phase extraction of polar pesticides from environmental water samples on graphitized carbon and Empore-activated carbon disks and on-line coupling to octadecyl-bonded silica analytical columns.

Science.gov (United States)

Slobodník, J; Oztezkizan, O; Lingeman, H; Brinkman, U A

1996-10-25

The suitability of Empore-activated carbon disks (EACD), Envi-Carb graphitized carbon black (GCB) and CPP-50 graphitized carbon for the trace enrichment of polar pesticides from water samples was studied by means of off-line and on-line solid-phase extraction (SPE). In the off-line procedure, 0.5-2 l samples spiked with a test mixture of oxamyl, methomyl and aldicarb sulfoxide were enriched on EnviCarb SPE cartridges or 47 mm diameter EACD and eluted with dichloromethane-methanol. After evaporation, a sample was injected onto a C18-bonded silica column and analysed by liquid chromatography with ultraviolet (LC-UV) detection. EACD performed better than EnviCarb cartridges in terms of breakthrough volumes (> 2 l for all test analytes), reproducibility (R.S.D. of recoveries, 4-8%, n = 3) and sampling speed (100 ml/min); detection limits in drinking water were 0.05-0.16 microgram/l. In the on-line experiments, 4.6 mm diameter pieces cut from original EACD and stacked onto each other in a 9 mm long precolumn, and EnviCarb and CPP-50 packed in 10 x 2.0 mm I.D. precolumn, were tested, and 50-200 ml spiked water samples were preconcentrated. Because of the peak broadening caused by the strong sorption of the analytes on carbon, the carbon-packed precolumns were eluted by a separate stream of 0.1 ml/min acetonitrile which was mixed with the gradient LC eluent in front of the C18 analytical column. The final on-line procedure was also applied for the less polar propoxur, carbaryl and methiocarb. EnviCarb could not be used due to its poor pressure resistance. CPP-50 provided less peak broadening than EACD: peak widths were 0.1-0.3 min and R.S.D. of peak heights 4-14% (n = 3). In terms of analyte trapping efficiency on-line SPE-LC-UV with a CPP-50 precolumn also showed better performance than when Bondesil C18/OH or polymeric PLRP-S was used, but chromatographic resolution was similar. With the CPP-50-based system, detection limits of the test compounds were 0.05-1 microgram

Household hazardous waste data for the UK by direct sampling.

Science.gov (United States)

Slack, Rebecca J; Bonin, Michael; Gronow, Jan R; Van Santen, Anton; Voulvoulis, Nikolaos

2007-04-01

The amount of household hazardous waste (HHW) disposed of in the United Kingdom (UK) requires assessment. This paper describes a direct analysis study carried out in three areas in southeast England involving over 500 households. Each participating householder was provided with a special bin in which to place items corresponding to a list of HHW. The amount of waste collected was split into nine broad categories: batteries, home maintenance (DIY), vehicle upkeep, pesticides, pet care, pharmaceuticals, photographic chemicals, household cleaners, and printer cartridges. Over 1 T of waste was collected from the sample households over a 32-week period, which would correspond to an estimated 51,000 T if extrapolated to the UK population for the same period or over 7,000 T per month. Details of likely disposal routes adopted by householders were also sought, demonstrating the different pathways selected for different waste categories. Co-disposal with residual household waste dominated for waste batteries and veterinary medicines, hence avoiding classification as hazardous waste under new UK waste regulations. The information can be used to set a baseline for the management of HHW and provides information for an environmental risk assessment of the disposal of such wastes to landfill.

The determination of radiocaesium in sea and fresh waters

International Nuclear Information System (INIS)

Baker, C.W.

1975-10-01

The caesium is adsorbed on to a cartridge of silica gel impregnated with ammonium molybdophosphate from 50 litres of filtered water, adjusted to pH 2 with nitric acid. The cartridge is then placed in a well crystal detector and gamma counted. An additional separation step is required if zirconium-95/niobium-95 contamination has occurred, as shown by gamma spectrometric analysis of the cartridge. The measurement of caesium-137 and caesium-134 is by conventional γ-spectrometry. The output of the analysing system is ASCII paper tape, and a PDP-8 computer is used to convert this spectral information to activity of caesium-137 and -134 in pCi l -1 at the time of sample collection. (U.K.)

Preliminary results for the detection method of perfluoroalkyl substances (PFASs residues in pork

Directory of Open Access Journals (Sweden)

Shih-kuo Lin

2017-05-01

Full Text Available The perfluoroalkyl substances (PFASs residues, which come from environmental pollution, tend to accumulate in the food chain (EFSA, 2008; Guerranti et al., 2013. 17 chemicals of PFASs family were selected for this study. Fresh pork samples were extracted by Waters® WAX SPE (solid phase extraction cartridges. All extracted samples were analyzed by liquid chromatography tandem mass spectrometry (LC-MS/MS. The results of calibration curves of each PFAS were good, the R2 values ranging from 0.9901 to 0.9993. The Recoveries were in the range 80%-119%. The protocol of extraction by Waters® WAX SPE cartridge will be applied in future studies.

Lyophilization Cycle Design for Dual Chamber Cartridges and a Method for Online Process Control: The "DCC LyoMate" Procedure.

Science.gov (United States)

Korpus, Christoph; Friess, Wolfgang

2017-08-01

Freeze-drying process design is a challenging task that necessitates a profound understanding of the complex interrelation among critical process parameters (e.g., shelf temperature and chamber pressure), heat transfer characteristics of the involved materials (e.g., product containers and holder devices), and critical quality attributes of the product (e.g., collapse temperatures). The Dual Chamber Cartridge "(DCC) LyoMate" (from lyophilization and automated) is a manometric temperature measurement-based process control strategy that was developed within this study to streamline this complicated task. It was successfully applied using 5% sucrose formulations with 0.5 and 1 mL fill volumes. The system was further challenged using 2, 20, and 100 mg/mL monoclonal antibody formulations. The DCC LyoMate method did not only produce pharmaceutically acceptable cakes but was also able to maintain the desired product temperature irrespective of formulation and protein content. It enabled successful process design even at high protein concentrations and aided the design and online control of the lyophilization process for drying in DCCs within a single development run. Thus, it helps to reduce development cost and the DCC LyoMate can also be easily installed on every freeze-dryer capable of performing a manometric temperature measurement, without the need for hardware modification. Copyright © 2017 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Intemational collaborative study on the preparation of 1st international standard for rhTSH for bioassay

International Nuclear Information System (INIS)

Huang Ying; Shen Hongzheng; Yu Ting; Xu Ligen

2007-01-01

The history of the international collaborative studies on the preparation of standards of TSH for bioassay and immunoassay was reviewed. The result of collaborative study on the 1st international standard for thyroid-stimulating hormone, recombinant, human, for bioassay was reported in detail in this article. Based on the results of this collaborative study, it is proposed that the candidate standard be established as the international standard for rhTSH for bioassay, and be assigned an activity of 9.5 IU per ampoule. The national standard preparation of TSH for immunoassay was also reassayed, revealing the potency to be 0.557 mIU/ampoule, i.e. 92. 8% of the labelled value of 0.600mIU/ampoule, a reasonable consistency. (authors)

Supercritical Fluid Extraction and Ultra Performance Liquid Chromatography of Respiratory Quinones for Microbial Community Analysis in Environmental and Biological Samples

Directory of Open Access Journals (Sweden)

Koichi Fujie

2012-03-01

Full Text Available Microbial community structure plays a significant role in environmental assessment and animal health management. The development of a superior analytical strategy for the characterization of microbial community structure is an ongoing challenge. In this study, we developed an effective supercritical fluid extraction (SFE and ultra performance liquid chromatography (UPLC method for the analysis of bacterial respiratory quinones (RQ in environmental and biological samples. RQ profile analysis is one of the most widely used culture-independent tools for characterizing microbial community structure. A UPLC equipped with a photo diode array (PDA detector was successfully applied to the simultaneous determination of ubiquinones (UQ and menaquinones (MK without tedious pretreatment. Supercritical carbon dioxide (scCO2 extraction with the solid-phase cartridge trap proved to be a more effective and rapid method for extracting respiratory quinones, compared to a conventional organic solvent extraction method. This methodology leads to a successful analytical procedure that involves a significant reduction in the complexity and sample preparation time. Application of the optimized methodology to characterize microbial communities based on the RQ profile was demonstrated for a variety of environmental samples (activated sludge, digested sludge, and compost and biological samples (swine and Japanese quail feces.

Aerosol Sampling System for Collection of Capstone Depleted Uranium Particles in a High-Energy Environment

International Nuclear Information System (INIS)

Holmes, Thomas D.; Guilmette, Raymond A.; Cheng, Yung-Sung; Parkhurst, MaryAnn; Hoover, Mark D.

2009-01-01

The Capstone Depleted Uranium Aerosol Study was undertaken to obtain aerosol samples resulting from a kinetic-energy cartridge with a large-caliber depleted uranium (DU) penetrator striking an Abrams or Bradley test vehicle. The sampling strategy was designed to (1) optimize the performance of the samplers and maintain their integrity in the extreme environment created during perforation of an armored vehicle by a DU penetrator, (2) collect aerosols as a function of time post-impact, and (3) obtain size-classified samples for analysis of chemical composition, particle morphology, and solubility in lung fluid. This paper describes the experimental setup and sampling methodologies used to achieve these objectives. Custom-designed arrays of sampling heads were secured to the inside of the target in locations approximating the breathing zones of the vehicle commander, loader, gunner, and driver. Each array was designed to support nine filter cassettes and nine cascade impactors mounted with quick-disconnect fittings. Shielding and sampler placement strategies were used to minimize sampler loss caused by the penetrator impact and the resulting fragments of eroded penetrator and perforated armor. A cyclone train was used to collect larger quantities of DU aerosol for chemical composition and solubility. A moving filter sample was used to obtain semicontinuous samples for depleted uranium concentration determination. Control for the air samplers was provided by five remotely located valve control and pressure monitoring units located inside and around the test vehicle. These units were connected to a computer interface chassis and controlled using a customized LabVIEW engineering computer control program. The aerosol sampling arrays and control systems for the Capstone study provided the needed aerosol samples for physicochemical analysis, and the resultant data were used for risk assessment of exposure to DU aerosol

Application of two analytic techniques of sampling for the determination of aldehydes in air and in rain water in three areas of Costa Rica

International Nuclear Information System (INIS)

Vega Montero, D. I

2001-01-01

The aldehydes are of supreme interest in the quality of the air of Costa Rica; reason why it is very important to determine them qualitative and quantitatively. This study has as objectives the identification and quantification of aldehydes in samples of air and of rain water in three areas of Costa Rica, to compare two methods of taking of samples of air and to correlate the concentration of the aldehydes in the different points of taking of samples. The sampling one carries out in three located stations, in the Hill of the Piroclasticos (3 km. To the Northeast of the active crater of the Volcano Irazu), Escazu (it plants potabilizadora of water) and in Turrucares (facilities of the Rural Watch). The used sampling devices, denuders and cartridges, they were recovered with a breakup of 2,4-dinitrofenilhidrazina o'clock like absorbent reagent, which I form the corresponding hidrazonas in presence of the aldehydes. The identification and quantification of the aldehydes, one carries out by means of chromatography it liquidates of high resolution. The comparison among the concentrations of the aldehydes in air gathered by the two used sampling methods indicates that a significant difference exists among them, at a level of trust of 95% [es

In-Pile Assemblies for Investigation of Tritium Release from Li2TiO3 Lithium Ceramic

International Nuclear Information System (INIS)

Shestakov, V.; Tazhibayeva, I.; Kawamura, H.; Kenzhin, Y.; Kulsartov, T.; Chikhray, Y.; Kolbaenkov, A.; Arinkin, F.; Gizatulin, Sh.; Chakrov, P.

2005-01-01

The description of algorithm to design in-pipe experimental ampoule devices (IPAD) is presented here, including description of IPAD design for irradiation tests of highly enriched lithium ceramics at WWR-K reactor. The description of the system for registration of tritium release from ceramics during irradiation is presented as well. Typical curve of tritium release from the IPAD during irradiation under various temperatures of the samples is shown here

Ultra-high performance liquid chromatography tandem mass spectrometry for the determination of five glycopeptide antibiotics in food and biological samples using solid-phase extraction.

Science.gov (United States)

Deng, Fenfang; Yu, Hong; Pan, Xinhong; Hu, Guoyuan; Wang, Qiqin; Peng, Rongfei; Tan, Lei; Yang, Zhicong

2018-02-23

This paper demonstrated the development and validation of an ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method for simultaneous determination of five glycopeptide antibiotics in food and biological samples. The target glycopeptide antibiotics were isolated from the samples by solvent extraction, and the extracts were cleaned with a tandem solid-phase extraction step using mixed strong cation exchange and hydrophilic/lipophilic balance cartridges. Subsequently, the analytes were eluted with different solvents, and then quantified by UHPLC-MS/MS in the positive ionization mode with multiple reaction monitoring. Under optimal conditions, good linear correlations were obtained for the five glycopeptide antibiotics in the concentration range of 1.0 μg/L to 20.0 μg/L, and with linear correlation coefficients >0.998. Employing this method, the target glycopeptide antibiotics in food and biological samples were identified with a recovery of 83.0-102%, and a low quantitation limit of 1.0 μg/kg in food and 2.0 μg/L in biological samples with low matrix effects. Copyright © 2018 Elsevier B.V. All rights reserved.

Miniature acoustic wave lysis system and uses thereof

Science.gov (United States)

Branch, Darren W.; Vreeland, Erika Cooley; Smith, Gennifer Tanabe

2016-12-06

The present invention relates to an acoustic lysis system including a disposable cartridge that can be reversibly coupled to a platform having a small, high-frequency piezoelectric transducer array. In particular, the system releases viable DNA, RNA, and proteins from human or bacterial cells, without chemicals or additional processing, to enable high-speed sample preparation for clinical point-of-care medical diagnostics and use with nano/microfluidic cartridges. Also described herein are methods of making and using the system of the invention.

Some methods of detection of atmospheric contamination by iodine 131

International Nuclear Information System (INIS)

Billard, Francois; Chevalier, Gerard; Gaillard, Pierre; Pradel, Jacques

1964-01-01

Due to the extensive use of iodine, risks of contamination by iodine 131 are increasing. Moreover, the increase of reactor power requires venting installations equipped with efficient safety filters which must be tested. The authors thus report the study of iodine trapping in filters, and its atmospheric detection and measurement. They report studies and achievements in the field of measurement of atmospheric pollution, and tests performed on iodine trapping by activated coals. After having outlined key qualities of an apparatus for atmospheric control, the authors indicate the various sampling methods. They discuss the method and calibration for the measurement of radioactivity of filters and coal which have trapped iodine 131. They discuss measurement sensitivity. They report how the efficiency of coals has been checked. They describe the experimental installation, and report the tests of some detectors of atmospheric contamination: sampling cartridges full of activated coal, gas mask cartridge, continuous control apparatus ('coffee machine' type), and detector of gaseous iodine. Appendices indicate the calculation of error on a cartridge counting rate, iodine generation methods (discontinuous method, continuous method) [fr

Determination of neonicotinoid pesticides residues in agricultural samples by solid-phase extraction combined with liquid chromatography-tandem mass spectrometry.

Science.gov (United States)

Xie, Wen; Han, Chao; Qian, Yan; Ding, Huiying; Chen, Xiaomei; Xi, Junyang

2011-07-15

This work reports a new sensitive multi-residue liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for detection, confirmation and quantification of six neonicotinoid pesticides (dinotefuran, thiamethoxam, clothiandin, imidacloprid, acetamiprid and thiacloprid) in agricultural samples (chestnut, shallot, ginger and tea). Activated carbon and HLB solid-phase extraction cartridges were used for cleaning up the extracts. Analysis is performed by LC-MS/MS operated in the multiple reaction monitoring (MRM) mode, acquiring two specific precursor-product ion transitions per target compound. Quantification was carried by the internal standard method with D(4)-labeled imidacloprid. The method showed excellent linearity (R(2)≥0.9991) and precision (relative standard deviation, RSD≤8.6%) for all compounds. Limits of quantification (LOQs) were 0.01 mg kg(-1) for chestnut, shallot, ginger sample and 0.02 mg kg(-1) for tea sample. The average recoveries, measured at three concentrations levels (0.01 mg kg(-1), 0.02 mg kg(-1) and 0.1 mg kg(-1) for chestnut, shallot, ginger sample, 0.02 mg kg(-1), 0.04 mg kg(-1) and 0.2 mg kg(-1) for tea sample), were in the range 82.1-108.5%. The method was satisfactorily validated for the analysis of 150 agricultural samples (chestnut, shallot, ginger and tea). Imidacloprid and acetamiprid were detected at concentration levels ranging from 0.05 to 3.6 mg kg(-1). Copyright © 2011 Elsevier B.V. All rights reserved.

Field Deployable Method for Arsenic Speciation in Water.

Science.gov (United States)

Voice, Thomas C; Flores Del Pino, Lisveth V; Havezov, Ivan; Long, David T

2011-01-01

Contamination of drinking water supplies by arsenic is a world-wide problem. Total arsenic measurements are commonly used to investigate and regulate arsenic in water, but it is well understood that arsenic occurs in several chemical forms, and these exhibit different toxicities. It is problematic to use laboratory-based speciation techniques to assess exposure as it has been suggested that the distribution of species is not stable during transport in some types of samples. A method was developed in this study for the on-site speciation of the most toxic dissolved arsenic species: As (III), As (V), monomethylarsonic acid (MMA) and dimethylarsenic acid (DMA). Development criteria included ease of use under field conditions, applicable at levels of concern for drinking water, and analytical performance.The approach is based on selective retention of arsenic species on specific ion-exchange chromatography cartridges followed by selective elution and quantification using graphite furnace atomic absorption spectroscopy. Water samples can be delivered to a set of three cartridges using either syringes or peristaltic pumps. Species distribution is stable at this point, and the cartridges can be transported to the laboratory for elution and quantitative analysis. A set of ten replicate spiked samples of each compound, having concentrations between 1 and 60 µg/L, were analyzed. Arsenic recoveries ranged from 78-112 % and relative standard deviations were generally below 10%. Resolution between species was shown to be outstanding, with the only limitation being that the capacity for As (V) was limited to approximately 50 µg/L. This could be easily remedied by changes in either cartridge design, or the extraction procedure. Recoveries were similar for two spiked hard groundwater samples indicating that dissolved minerals are not likely to be problematic. These results suggest that this methodology can be use for analysis of the four primary arsenic species of concern in

New practical algorithm for modelling analyte recovery in bioanalytical reversed phase and mixed-mode solid phase extraction

NARCIS (Netherlands)

Hendriks, G.; Uges, D. R. A.; Franke, J. P.

2008-01-01

Solid phase extraction (SPE) is a widely used method for sample cleanup and sample concentration in bioanalytical sample preparation. A few methods to model the retention behaviour on SPE cartridges have been described previously but they are either not applicable to ionised species or are not

Detached Bridgman Growth of Germanium and Germanium-Silicon Alloy Crystals

Science.gov (United States)

Szofran, F. R.; Volz, M. P.; Schweizer, M.; Cobb, S. D.; Motakef, S.; Croell, A.; Dold, P.; Curreri, Peter A. (Technical Monitor)

2002-01-01

Earth based experiments on the science of detached crystal growth are being conducted on germanium and germanium-silicon alloys (2 at% Si average composition) in preparation for a series of experiments aboard the International Space Station (ISS). The purpose of the microgravity experiments includes differentiating among proposed mechanisms contributing to detachment, and confirming or refining our understanding of the detachment mechanism. Because large contact angle are critical to detachment, sessile drop measurements were used to determine the contact angles as a function of temperature and composition for a large number of substrates made of potential ampoule materials. Growth experiments have used pyrolytic boron nitride (pBN) and fused silica ampoules with the majority of the detached results occurring predictably in the pBN. The contact angles were 173 deg (Ge) and 165 deg (GeSi) for pBN. For fused silica, the contact angle decreases from 150 deg to an equilibrium value of 117 deg (Ge) or from 129 deg to an equilibrium value of 100 deg (GeSi) over the duration of the experiment. The nature and extent of detachment is determined by using profilometry in conjunction with optical and electron microscopy. The stability of detachment has been analyzed, and an empirical model for the conditions necessary to achieve sufficient stability to maintain detached growth for extended periods has been developed. Results in this presentation will show that we have established the effects on detachment of ampoule material, pressure difference above and below the melt, and silicon concentration; samples that are nearly completely detached can be grown repeatedly in pBN.

A comparison of surface topography characterization technologies for use in comparing spent bullet and cartridge case signatures

Energy Technology Data Exchange (ETDEWEB)

Batishko, C.R.; Hickman, B.J.; Cuta, F.M.

1992-11-01

The Pacific Northwest Laboratory was tasked by the US Department of Energy to provide technical assistance to the Federal Bureau of Investigation in evaluating and ranking technologies potentially useful in high-speed comparison of unique spent bullet and cartridge case surface signatures. Information sources included vendor input, current relevant literature, vendor phone contacts, other FBI resources, relevant PNL reports, and personal contact with numerous PNL technical staff. A comprehensive list of technologies was reduced to a list of 38 by grouping very similar methodologies, and further reduced to a short list of six by applying a set of five minimum functional requirements. A total of 14 primary criteria, many having secondary criteria, were subsequently used to evaluate each technology. The ranked short list results are reported and supported in this document, and their scores normalized to a hypothetical ideal system are as follows: (1) confocal microscopy 82.13; (2) laser dynamic focusing 72.04; (3)moire interferometry V70.94; (4)fringe field capacitance;(5)laser triangulation 66.18; (6)structured/sectioned light 65.55. Information available within the time/budget constraints which was used for the evaluation and ranking was not sufficiently detailed to evaluate specific implementations of the technologies. Each of the technologies in the short list was judged potentially capable of meeting the minimum requirements. Clever, novel engineering solutions resulting in a more cost-effective system, or a closer fit to the ``ideal system,`` could result in a reordering of the short list when actual technical proposals are evaluated. Therefore, it is recommended that a Request for Proposal not be limited to only the highest ranked technology, but include all six technologies in the short list.

Quality assurance and quality control in light stable isotope laboratories: A case study of Rio Grande, Texas, water samples

Science.gov (United States)

Coplen, T.B.; Qi, H.

2009-01-01

New isotope laboratories can achieve the goal of reporting the same isotopic composition within analytical uncertainty for the same material analysed decades apart by (1) writing their own acceptance testing procedures and putting them into their mass spectrometric or laser-based isotope-ratio equipment procurement contract, (2) requiring a manufacturer to demonstrate acceptable performance using all sample ports provided with the instrumentation, (3) for each medium to be analysed, prepare two local reference materials substantially different in isotopic composition to encompass the range in isotopic composition expected in the laboratory and calibrated them with isotopic reference materials available from the International Atomic Energy Agency (IAEA) or the US National Institute of Standards and Technology (NIST), (4) using the optimum storage containers (for water samples, sealing in glass ampoules that are sterilised after sealing is satisfactory), (5) interspersing among sample unknowns local laboratory isotopic reference materials daily (internationally distributed isotopic reference materials can be ordered at three-year intervals, and can be used for elemental analyser analyses and other analyses that consume less than 1 mg of material) - this process applies to H, C, N, O, and S isotope ratios, (6) calculating isotopic compositions of unknowns by normalising isotopic data to that of local reference materials, which have been calibrated to internationally distributed isotopic reference materials, (7) reporting results on scales normalised to internationally distributed isotopic reference materials (where they are available) and providing to sample submitters the isotopic compositions of internationally distributed isotopic reference materials of the same substance had they been analysed with unknowns, (8) providing an audit trail in the laboratory for analytical results - this trail commonly will be in electronic format and might include a laboratory

A New Solid Phase Extraction for the Determination of Anthocyanins in Grapes

Directory of Open Access Journals (Sweden)

Marta Ferreiro-González

2014-12-01

Full Text Available A method for the concentration and cleaning of red grape extracts prior to the determination of anthocyanins by UPLC-DAD has been developed. This method is of special interest in the determination of phenolic maturity as it allows the analysis of the anthocyanins present in grapes. Several different SPE cartridges were assessed, including both C-18- and vinylbenzene-based cartridges. C-18-based cartridges presented a very low retention for the glucosylated anthocyanidins while vinylbenzene-based cartridges showed excellent retention for these compounds. The optimized method involves the initial conditioning of the cartridge using 10 mL of methanol and 10 mL of water, followed by loading of up to 100 mL of red grape extract. Ten mL of water was used in the washing step and anthocyanins were subsequently eluted using 1.5 mL of acidified methanol at pH 2. This method simplifies the determination of individual anthocyanins as, on the one hand, it cleans the sample of interference and, on the other hand, it increases the concentration to up to 25:1.5. The developed method has been validated with a range of different grapes and it has also been tested as a means of determining the different anthocyanins in grapes with different levels of maturity.

Determination of a wide range of volatile organic compounds in ambient air using multisorbent adsorption/thermal desorption and gas chromatography/mass spectrometry

Science.gov (United States)

Pankow, J.F.; Luo, W.; Isabelle, L.M.; Bender, D.A.; Baker, R.J.

1998-01-01

Adsorption/thermal desorption with multisorbent air-sampling cartridges was developed for the determination of 87 method analytes including halogenated alkanes, halogenated alkenes, ethers, alcohols, nitriles, esters, ketones, aromatics, a disulfide, and a furan. The volatilities of the compounds ranged from that of dichlorofluoromethane (CFC12) to that of 1,2,3- trichlorobenzene. The eight most volatile compounds were determined using a 1.5-L air sample and a sample cartridge containing 50 mg of Carbotrap B and 280 mg of Carboxen 1000; the remaining 79 compounds were determined using a 5-L air sample and a cartridge containing 180 mg of Carbotrap B and 70 mg of Carboxen 1000. Analysis and detection were by gas chromatography/mass spectrometry. The minimum detectable level (MDL) concentration values ranged from 0.01 parts per billion by volume (ppbv) for chlorobenzene to 0.4 ppbv for bromomethane; most of the MDL values were in the range 0.02-0.06 ppbv. No breakthrough was detected with the prescribed sample volumes. Analyte stability on the cartridges was very good. Excellent recoveries were obtained with independent check standards. Travel spike recoveries ranged from 90 to 110% for 72 of the 87 compounds. The recoveries were less than 70% for bromomethane and chloroethene and for a few compounds such as methyl acetate that are subject to losses by hydrolysis; the lowest travel spike recovery was obtained for bromomethane (62%). Blank values for all compounds were either below detection or very low. Ambient atmospheric sampling was conducted in New Jersey from April to December, 1997. Three sites characterized by low, moderate, and high densities of urbanization/traffic were sampled. The median detected concentrations of the compounds were either similar at all three sites (as with the chlorofluorocarbon compounds) or increased with the density of urbanization/traffic (as with dichloromethane, MTBE, benzene, and toluene). For toluene, the median detected

Novel nanoporous sorbent for solid-phase extraction in petroleum fingerprinting

Science.gov (United States)

Alayande, S. Oluwagbemiga; Hlengilizwe, Nyoni; Dare, E. Olugbenga; Msagati, Titus A. M.; Akinlabi, A. Kehinde; Aiyedun, P. O.

2016-04-01

Sample preparation is crucial in the analysis of petroleum and its derivatives. In this study, developing affordable sorbent for petroleum fingerprinting analysis using polymer waste such expanded polystyrene was explored. The potential of electrospun expanded polystyrene (EPS) as a sorbent for the solid-phase extraction (SPE) technique was investigated, and its efficiency was compared with commercial cartridges such as alumina, silica and alumina/silica hybrid commercial for petroleum fingerprinting analysis. The chromatograms showed that the packed electrospun EPS fibre demonstrated excellent properties for SPE applications relative to the hybrid cartridges.

A versatile gas interface for routine radiocarbon analysis with a gas ion source

Energy Technology Data Exchange (ETDEWEB)

Wacker, L., E-mail: wacker@phys.ethz.ch [Laboratory of Ion Beam Physics, ETH Zurich, 8093 Zurich (Switzerland); Fahrni, S.M. [Department of Chemistry and Biochemistry, University of Bern, 3012 Berne (Switzerland); Oeschger Centre for Climate Change Research, University of Bern, 3012 Berne (Switzerland); Paul Scherrer Institute (PSI), 5232 Villigen (Switzerland); Hajdas, I. [Laboratory of Ion Beam Physics, ETH Zurich, 8093 Zurich (Switzerland); Molnar, M. [Laboratory of Ion Beam Physics, ETH Zurich, 8093 Zurich (Switzerland); Institute of Nuclear Research, Hungarian Academy of Sciences, 4026 Debrecen (Hungary); Synal, H.-A. [Laboratory of Ion Beam Physics, ETH Zurich, 8093 Zurich (Switzerland); Szidat, S. [Department of Chemistry and Biochemistry, University of Bern, 3012 Berne (Switzerland); Oeschger Centre for Climate Change Research, University of Bern, 3012 Berne (Switzerland); Zhang, Y.L. [Department of Chemistry and Biochemistry, University of Bern, 3012 Berne (Switzerland); Oeschger Centre for Climate Change Research, University of Bern, 3012 Berne (Switzerland); Paul Scherrer Institute (PSI), 5232 Villigen (Switzerland)

2013-01-15

In 2010 more than 600 radiocarbon samples were measured with the gas ion source at the MIni CArbon DAting System (MICADAS) at ETH Zurich and the number of measurements is rising quickly. While most samples contain less than 50 {mu}g C at present, the gas ion source is attractive as well for larger samples because the time-consuming graphitization is omitted. Additionally, modern samples are now measured down to 5 per-mill counting statistics in less than 30 min with the recently improved gas ion source. In the versatile gas handling system, a stepping-motor-driven syringe presses a mixture of helium and sample CO{sub 2} into the gas ion source, allowing continuous and stable measurements of different kinds of samples. CO{sub 2} can be provided in four different ways to the versatile gas interface. As a primary method, CO{sub 2} is delivered in glass or quartz ampoules. In this case, the CO{sub 2} is released in an automated ampoule cracker with 8 positions for individual samples. Secondly, OX-1 and blank gas in helium can be provided to the syringe by directly connecting gas bottles to the gas interface at the stage of the cracker. Thirdly, solid samples can be combusted in an elemental analyzer or in a thermo-optical OC/EC aerosol analyzer where the produced CO{sub 2} is transferred to the syringe via a zeolite trap for gas concentration. As a fourth method, CO{sub 2} is released from carbonates with phosphoric acid in septum-sealed vials and loaded onto the same trap used for the elemental analyzer. All four methods allow complete automation of the measurement, even though minor user input is presently still required. Details on the setup, versatility and applications of the gas handling system are given.

Evaporation rate in containers used for storing radioactive tracer solutions

International Nuclear Information System (INIS)

Gascon, J.L.

2002-01-01

In radiochemical analysis, the storage of a tracer solution is an important issue to bear in mind. The evaporation of the tracer solution depends on the type of container used for storing. Evaporation rate in four kinds of containers, i.e., flame-sealed glass ampoule, sealed glass flask, flame-sealed polyethylene ampoule and screw glass vial was studied. It is concluded that the evaporation rate depends on the system of closing. (author)

Determination of colloidal and dissolved silver in water samples using colorimetric solid-phase extraction.

Science.gov (United States)

Hill, April A; Lipert, Robert J; Porter, Marc D

2010-03-15

The increase in bacterial resistance to antibiotics has led to resurgence in the use of silver as a biocidal agent in applications ranging from washing machine additives to the drinking water treatment system on the International Space Station (ISS). However, growing concerns about the possible toxicity of colloidal silver to bacteria, aquatic organisms and humans have led to recently issued regulations by the US EPA and FDA regarding the usage of silver. As part of an ongoing project, we have developed a rapid, simple method for determining total silver, both ionic (silver(I)) and colloidal, in 0.1-1mg/L aqueous samples, which spans the ISS potable water target of 0.3-0.5mg/L (total silver) and meets the US EPA limit of 0.1mg/L in drinking water. The method is based on colorimetric solid-phase extraction (C-SPE) and involves the extraction of silver(I) from water samples by passage through a solid-phase membrane impregnated with the colorimetric reagent DMABR (5-[4-(dimethylamino)benzylidene]rhodanine). Silver(I) exhaustively reacts with impregnated DMABR to form a colored compound, which is quantified using a handheld diffuse reflectance spectrophotometer. Total silver is determined by first passing the sample through a cartridge containing Oxone, which exhaustively oxidizes colloidal silver to dissolved silver(I). The method, which takes less than 2 min to complete and requires only approximately 1 mL of sample, has been validated through a series of tests, including a comparison with the ICP-MS analysis of a water sample from ISS that contained both silver(I) and colloidal silver. Potential earth-bound applications are also briefly discussed. Copyright (c) 2009 Elsevier B.V. All rights reserved.

A comparison of surface topography characterization technologies for use in comparing spent bullet and cartridge case signatures

Energy Technology Data Exchange (ETDEWEB)

Batishko, C.R.; Hickman, B.J.; Cuta, F.M.

1992-11-01

The Pacific Northwest Laboratory was tasked by the US Department of Energy to provide technical assistance to the Federal Bureau of Investigation in evaluating and ranking technologies potentially useful in high-speed comparison of unique spent bullet and cartridge case surface signatures. Information sources included vendor input, current relevant literature, vendor phone contacts, other FBI resources, relevant PNL reports, and personal contact with numerous PNL technical staff. A comprehensive list of technologies was reduced to a list of 38 by grouping very similar methodologies, and further reduced to a short list of six by applying a set of five minimum functional requirements. A total of 14 primary criteria, many having secondary criteria, were subsequently used to evaluate each technology. The ranked short list results are reported and supported in this document, and their scores normalized to a hypothetical ideal system are as follows: (1) confocal microscopy 82.13; (2) laser dynamic focusing 72.04; (3)moire interferometry V70.94; (4)fringe field capacitance;(5)laser triangulation 66.18; (6)structured/sectioned light 65.55. Information available within the time/budget constraints which was used for the evaluation and ranking was not sufficiently detailed to evaluate specific implementations of the technologies. Each of the technologies in the short list was judged potentially capable of meeting the minimum requirements. Clever, novel engineering solutions resulting in a more cost-effective system, or a closer fit to the ideal system,'' could result in a reordering of the short list when actual technical proposals are evaluated. Therefore, it is recommended that a Request for Proposal not be limited to only the highest ranked technology, but include all six technologies in the short list.

Determination of trace elements in human blood serum and in the standard reference material ''Bovine Liver'' by instrumental neutron activation analysis

International Nuclear Information System (INIS)

Behne, D.; Juergensen, H.

1978-01-01

Ag, Br, Co, Cr, Cs, Fe, Na, Rb, Sb, Se and Zn were determined in biological materials by gamma-spectrometry of long-lived radionuclides after long-time irradiation with thermal neutrons. Blood was taken from a vein in the arm of the test person via an indwelling plastic cannula. The serum was separated from other blood components by centrifugation and stored at a temperature of -20 deg C. Ampoules of high purity silica quartz were chosen as irradiation containers. The vials were cleaned by etching with 40% hydrofluoric acid. For the analysis 300 μl of serum were taken. The ampoules were irradiated for 10 days at a thermal neutron flux density of 5.10 13 n.cm -2 .sec -1 . They were then cleaned by etching for 5 min with hydrofluoric acid. The gamma-ray spectra of the irradiated samples were measured twice. From the first spectra, which were obtained 10 days after irradiation, the concentrations of Br and Na were calculated. From the gamma-peaks after a decay time of 3 months Ag, Co, Cr, Cs, Fe, Rb, Sc, Se and Zn were determined. The accuracy and precision of the procedure were tested, using the standard reference material ''Bovine Liver'' and identical serum samples. In the case of blood serum the method proved to be suitable for the determination of Br, Cs, Fe, Na, Rb, Se and Zn. By analysing samples from several subjects information about element levels in human serum was obtained. (T.G.)

Microcalorimetric monitoring of grape withering

International Nuclear Information System (INIS)

Morozova, Ksenia; Romano, Andrea; Lonardi, Francesco; Ferrarini, Roberto; Biasioli, Franco; Scampicchio, Matteo

2016-01-01

Highlights: • Microcalorimetry was applied to monitor grape withering. • Heat flow was used to estimate rate of respiration. • Calorimetry was coupled with analysis of volatile compounds. • Data analysis showed three steps of withering. - Abstract: This work aimed at monitoring the metabolic activity of grapes during withering by microcalorimetry. Samples of Corvina grapes, a cultivar used in the production of Amarone wine, were dehydrated for about 120 days at an industrial scale plants (fruttaia). Single berries, sampled in the course of the withering process, were closed in ampoules and maintained at constant temperature. As biochemical events (i.e. berry respiration, microbial growth, etc.) are always accompanied by the production of heat (q), the heat-flow (dq/dt) emitted by berries enclosed in the ampoules was used to monitor their metabolic activity during withering, i.e. respiration. For each sampling time, the heat rate production of the berries at 298 K was monitored till a steady state signal was achieved (within 60 h). Such heat flow value was used as marker during the entire withering process (120 days). Its trend allowed to characterize the changes in the metabolic activity of the grape berries along the withering process. To understand the origin of such changes, the emission of volatile organic compounds (VOCs) were also measured by proton transfer mass spectrometry (PTR-MS). The use of microcalorimetry associated with the analysis of specific VOCs fragments offered a valuable information to describe the withering process.

Microcalorimetric monitoring of grape withering

Energy Technology Data Exchange (ETDEWEB)

Morozova, Ksenia; Romano, Andrea [Free University of Bozen-Bolzano, Faculty of Science and Technology, piazza Università 1, 39100 Bolzano (Italy); Lonardi, Francesco; Ferrarini, Roberto [PerfectWine s.r.l., Via della Pieve 70, 37029 S. Floriano (Italy); Biasioli, Franco [Department of Food Quality and Nutrition, Research and Innovation Centre, Fondazione Edmund Mach (FEM), Via E. Mach 1, 38010 San Michele all’Adige (Italy); Scampicchio, Matteo, E-mail: matteo.scampicchio@unibz.it [Free University of Bozen-Bolzano, Faculty of Science and Technology, piazza Università 1, 39100 Bolzano (Italy)

2016-04-20

Highlights: • Microcalorimetry was applied to monitor grape withering. • Heat flow was used to estimate rate of respiration. • Calorimetry was coupled with analysis of volatile compounds. • Data analysis showed three steps of withering. - Abstract: This work aimed at monitoring the metabolic activity of grapes during withering by microcalorimetry. Samples of Corvina grapes, a cultivar used in the production of Amarone wine, were dehydrated for about 120 days at an industrial scale plants (fruttaia). Single berries, sampled in the course of the withering process, were closed in ampoules and maintained at constant temperature. As biochemical events (i.e. berry respiration, microbial growth, etc.) are always accompanied by the production of heat (q), the heat-flow (dq/dt) emitted by berries enclosed in the ampoules was used to monitor their metabolic activity during withering, i.e. respiration. For each sampling time, the heat rate production of the berries at 298 K was monitored till a steady state signal was achieved (within 60 h). Such heat flow value was used as marker during the entire withering process (120 days). Its trend allowed to characterize the changes in the metabolic activity of the grape berries along the withering process. To understand the origin of such changes, the emission of volatile organic compounds (VOCs) were also measured by proton transfer mass spectrometry (PTR-MS). The use of microcalorimetry associated with the analysis of specific VOCs fragments offered a valuable information to describe the withering process.

Study of gunshot residues from Sintox® ammunition containing marking substances

Directory of Open Access Journals (Sweden)

Júlia Polovková

2015-12-01

Full Text Available Two types of factory marked Sintox® ammunition were investigated from the composition of gunshot residue particles (GSR and occurrence of marking substance points of view. The experiments were carried out with two cartridges of caliber 9 mm Luger (9 × 19 Parabellum of two producers (Ruag Ammotec, Switzerland and Men, Germany. The first cartridge (type Action 4, Ruag Ammotec contains gadolinium as a marking element, while the other cartridge (type PEP II, Men is marked with gallium in gunpowder. Scanning electron microscopy equipped with EDAX analyzer (SEM/EDX was used to detect and analyze the GSR particles in samples collected from the cartridges, barrels and shooter’s hands. Besides those, particles from the hit clothes placed at different shooting distances were collected and analyzed. The spreading of GSR cloud from the gun was observed using the high-speed camera. Results obtained clearly revealed that the way of ammunition production/construction and type of marking of ammunition can significantly influence the presence and detection reliability of marking elements in GSR. The detectability is affected also by the shooting distance.

Iodine removal adsorbent histories, aging and regeneration

International Nuclear Information System (INIS)

Hunt, J.R.; Rankovic, L.; Lubbers, R.; Kovach, J.L.

1976-01-01

The experience of efficiency changes with life under various test conditions is described. The adsorbents were periodically removed from both standby and continuously operating systems and tested under various test methods for residual iodine adsorption efficiency. Adsorbent from several conventional ''sampler'' cartridges versus the bulk adsorbent was also tested showing deficiency in the use of cartridge type sampling. Currently required test conditions were found inadequate to follow the aging of the adsorbent because pre-equilibration of the sample acts as a regenerant and the sample is not tested in the ''as is'' condition. The most stringent test was found to be the ambient temperature, high humidity test to follow the aging of the adsorbent. Several methods were evaluated to regenerate used adsorbents; of these high temperature steaming and partial reimpregnation were found to produce adsorbents with near identical properties of freshly prepared adsorbents

Sample to answer visualization pipeline for low-cost point-of-care blood cell counting

Science.gov (United States)

Smith, Suzanne; Naidoo, Thegaran; Davies, Emlyn; Fourie, Louis; Nxumalo, Zandile; Swart, Hein; Marais, Philip; Land, Kevin; Roux, Pieter

2015-03-01

We present a visualization pipeline from sample to answer for point-of-care blood cell counting applications. Effective and low-cost point-of-care medical diagnostic tests provide developing countries and rural communities with accessible healthcare solutions [1], and can be particularly beneficial for blood cell count tests, which are often the starting point in the process of diagnosing a patient [2]. The initial focus of this work is on total white and red blood cell counts, using a microfluidic cartridge [3] for sample processing. Analysis of the processed samples has been implemented by means of two main optical visualization systems developed in-house: 1) a fluidic operation analysis system using high speed video data to determine volumes, mixing efficiency and flow rates, and 2) a microscopy analysis system to investigate homogeneity and concentration of blood cells. Fluidic parameters were derived from the optical flow [4] as well as color-based segmentation of the different fluids using a hue-saturation-value (HSV) color space. Cell count estimates were obtained using automated microscopy analysis and were compared to a widely accepted manual method for cell counting using a hemocytometer [5]. The results using the first iteration microfluidic device [3] showed that the most simple - and thus low-cost - approach for microfluidic component implementation was not adequate as compared to techniques based on manual cell counting principles. An improved microfluidic design has been developed to incorporate enhanced mixing and metering components, which together with this work provides the foundation on which to successfully implement automated, rapid and low-cost blood cell counting tests.

Automated sample preparation using membrane microtiter extraction for bioanalytical mass spectrometry.

Science.gov (United States)

Janiszewski, J; Schneider, P; Hoffmaster, K; Swyden, M; Wells, D; Fouda, H

1997-01-01

The development and application of membrane solid phase extraction (SPE) in 96-well microtiter plate format is described for the automated analysis of drugs in biological fluids. The small bed volume of the membrane allows elution of the analyte in a very small solvent volume, permitting direct HPLC injection and negating the need for the time consuming solvent evaporation step. A programmable liquid handling station (Quadra 96) was modified to automate all SPE steps. To avoid drying of the SPE bed and to enhance the analytical precision a novel protocol for performing the condition, load and wash steps in rapid succession was utilized. A block of 96 samples can now be extracted in 10 min., about 30 times faster than manual solvent extraction or single cartridge SPE methods. This processing speed complements the high-throughput speed of contemporary high performance liquid chromatography mass spectrometry (HPLC/MS) analysis. The quantitative analysis of a test analyte (Ziprasidone) in plasma demonstrates the utility and throughput of membrane SPE in combination with HPLC/MS. The results obtained with the current automated procedure compare favorably with those obtained using solvent and traditional solid phase extraction methods. The method has been used for the analysis of numerous drug prototypes in biological fluids to support drug discovery efforts.

Determination of fluorine in fodder phosphates and phosphorite flour by fast neutron activation method

International Nuclear Information System (INIS)

Abashin, E.G.; Lisovskij, I.P.; Smakhtin, L.A.

1980-01-01

A neutron-activation method is suggested for determination of fluorine in fodder phosphates and phosphorite flour. Used as the source of fast neutrons was an NG-150M neutron generator with a maximum yield of 10 8 nxcm -2 xs -1 . Samples were irradiated in polyethylene ampoules using a pneumatic shuttle. Fluorine was determined with reference to the fluorine-18 isotope. The accuracy of determining fluorine in fodder phosphates and phosphorite flour is 1 to 4% (rel.) at a rate of not less than 10 samples per hour. The method is suitable for in-process testing of products

Determination of fluorine in fodder phosphates and phosphorite flour by fast neutron activation method

Energy Technology Data Exchange (ETDEWEB)

Abashin, E G; Lisovskii, I P; Smakhtin, L A

1980-01-01

A neutron-activation method is suggested for determination of fluorine in fodder phosphates and phosphorite flour. Used as the source of fast neutrons was an NG-150M neutron generator with a maximum yield of 10/sup 8/ nxcm/sup -2/xs/sup -1/. Samples were irradiated in polyethylene ampoules using a pneumatic shuttle. Fluorine was determined with reference to the fluorine-18 isotope. The accuracy of determining fluorine in fodder phosphates and phosphorite flour is 1 to 4% (rel.) at a rate of not less than 10 samples per hour. The method is suitable for in-process testing of products.

Award of two contracts for the renting of magnetic tape drives and tape libraries for LHC data storage and the purchase of the associated tape cartridges

CERN Document Server

2005-01-01

This document concerns the award of two contracts for the renting and possible subsequent purchase of magnetic tape drives and tape libraries for LHC data storage. The Finance Committee is invited to agree to the procedure described in section 3 of this document for the evaluation and possible subsequent purchase of tape drives and tape libraries for the storage of data from the LHC experiments. Subject to approval of this procedure, the Finance Committee is further invited to approve the negotiation of a contract for the renting of tape drives and tape libraries for evaluation purposes from IBM, for an amount of 579 707 Swiss francs, and from StorageTek, for an amount of 472 297 Swiss francs, during the period January 2006 â?" March 2007, plus the purchase of the associated tape cartridges for amounts of 202 500 Swiss francs and 284 748 Swiss francs respectively. The Finance Committee will be informed of the results of the evaluation by the end of 2006 and, subject to the outcome, will be invited to approve...

Development and validation of an UHPLC-MS/MS method for β2-agonists quantification in human urine and application to clinical samples.

Science.gov (United States)

Bozzolino, Cristina; Leporati, Marta; Gani, Federica; Ferrero, Cinzia; Vincenti, Marco

2018-02-20

A fast analytical method for the simultaneous detection of 24 β 2 -agonists in human urine was developed and validated. The method covers the therapeutic drugs most commonly administered, but also potentially abused β 2 -agonists. The procedure is based on enzymatic deconjugation with β-glucuronidase followed by SPE clean up using mixed-phase cartridges with both ion-exchange and lipophilic properties. Instrumental analysis conducted by UHPLC-MS/MS allowed high peak resolution and rapid chromatographic separation, with reduced time and costs. The method was fully validated according ISO 17025:2005 principles. The following parameters were determined for each analyte: specificity, selectivity, linearity, limit of detection, limit of quantification, precision, accuracy, matrix effect, recovery and carry-over. The method was tested on real samples obtained from patients subjected to clinical treatment under chronic or acute therapy with either formoterol, indacaterol, salbutamol, or salmeterol. The drugs were administered using pressurized metered dose inhalers. All β 2 -agonists administered to the patients were detected in the real samples. The method proved adequate to accurately measure the concentration of these analytes in the real samples. The observed analytical data are discussed with reference to the administered dose and the duration of the therapy. Copyright © 2017 Elsevier B.V. All rights reserved.

Molecularly imprinted solid-phase extraction of glutathione from urine samples

International Nuclear Information System (INIS)

Song, Renyuan; Hu, Xiaoling; Guan, Ping; Li, Ji; Zhao, Na; Wang, Qiaoli

2014-01-01

Molecularly imprinted polymer (MIP) particles for glutathione were synthesized through iniferter-controlled living radical precipitation polymerization (IRPP) under ultraviolet radiation at ambient temperature. Static adsorption, solid-phase extraction, and high-performance liquid chromatography were carried out to evaluate the adsorption properties and selective recognition characteristics of the polymers for glutathione and its structural analogs. The obtained IRPP-MIP particles exhibited a regularly spherical shape, rapid binding kinetics, high imprinting factor, and high selectivity compared with the MIP particles prepared using traditional free-radical precipitation polymerization. The selective separation and enrichment of glutathione from the mixture of glycyl-glycine and glutathione disulfide could be achieved on the IRPP-MIP cartridge. The recoveries of glutathione, glycyl-glycine, and glutathione disulfide were 95.6% ± 3.65%, 29.5% ± 1.26%, and 49.9% ± 1.71%, respectively. The detection limit (S/N = 3) of glutathione was 0.5 mg·L −1 . The relative standard deviations (RSDs) for 10 replicate detections of 50 mg·L −1 of glutathione were 5.76%, and the linear range of the calibration curve was 0.5 mg·L −1 to 200 mg·L −1 under optimized conditions. The proposed approach was successfully applied to determine glutathione in spiked human urine samples with recoveries of 90.24% to 96.20% and RSDs of 0.48% to 5.67%. - Highlights: • Imprinted polymer particles were prepared by IRPP at ambient temperature. • High imprinting factor, high selectivity, and rapid binding kinetics were achieved. • Selective solid-phase extraction of glutathione from human urine samples

A selective and simplified radioimmunoassay of 25-hydroxyvitamin D3

International Nuclear Information System (INIS)

Hummer, L.; Nilas, L.; Tjellesen, L.; Christiansen, C.

1984-01-01

A simple, non-chromatographic and selective assay for determination of 250 HD 3 in serum is described. The serum sample is deproteinated with acetonitrile and the supernatant purified over a small prepacked cartridge, Sep-pak. In the eluate from the cartridge, 250 HD 3 is measured by radioimmunoassay. The selectivity of the assay for 250 HD 3 is improved by adding vitamin D 2 to the antiserum; the assay is thus capable of measuring 250 HD 3 in serum samples containing up to a ratio of 250 HD 2 /250 HD 3 equal to 150. The simplicity, speed and the small amount of sample needed (0.5 ml) make this method suitable for use in a routine clinical laboratory. Because of its selectivity for 250 HD 3 the assay is a necessary prerequisite in the further investigation of metabolic discrimination between vitamins D 2 and D 3 . (author)

Proteoglycan from salmon nasal cartridge promotes in vitro wound healing of fibroblast monolayers via the CD44 receptor

International Nuclear Information System (INIS)

Ito, Gen; Kobayashi, Takeshi; Takeda, Yoshie; Sokabe, Masahiro

2015-01-01

Highlights: • Proteoglycan from salmon nasal cartridge (SNC-PG) promoted wound healing in fibroblast monolayers. • SNC-PG stimulated both cell proliferation and cell migration. • Interaction between chondroitin sulfate-units and CD44 is responsible for the effect. - Abstract: Proteoglycans (PGs) are involved in various cellular functions including cell growth, adhesion, and differentiation; however, their physiological roles are not fully understood. In this study, we examined the effect of PG purified from salmon nasal cartilage (SNC-PG) on wound closure using tissue-cultured cell monolayers, an in vitro wound-healing assay. The results indicated that SNC-PG significantly promoted wound closure in NIH/3T3 cell monolayers by stimulating both cell proliferation and cell migration. SNC-PG was effective in concentrations from 0.1 to 10 μg/ml, but showed much less effect at higher concentrations (100–1000 μg/ml). The effect of SNC-PG was abolished by chondroitinase ABC, indicating that chondroitin sulfates (CSs), a major component of glycosaminoglycans (GAGs) in SNC-PG, are crucial for the SNC-PG effect. Furthermore, chondroitin 6-sulfate (C-6-S), a major CS of SNC-PG GAGs, could partially reproduce the SNC-PG effect and partially inhibit the binding of SNC-PG to cells, suggesting that SNC-PG exerts its effect through an interaction between the GAGs in SNC-PG and the cell surface. Neutralization by anti-CD44 antibodies or CD44 knockdown abolished SNC-PG binding to the cells and the SNC-PG effect on wound closure. These results suggest that interactions between CS-rich GAG-chains of SNC-PG and CD44 on the cell surface are responsible for the SNC-PG effect on wound closure

Proteoglycan from salmon nasal cartridge promotes in vitro wound healing of fibroblast monolayers via the CD44 receptor

Energy Technology Data Exchange (ETDEWEB)

Ito, Gen; Kobayashi, Takeshi; Takeda, Yoshie [Department of Physiology, Nagoya University Graduate School of Medicine, Nagoya, Aichi 466-8550 (Japan); Sokabe, Masahiro, E-mail: msokabe@med.nagoya-u.ac.jp [Department of Physiology, Nagoya University Graduate School of Medicine, Nagoya, Aichi 466-8550 (Japan); Mechanobiology Laboratory, Nagoya University Graduate School of Medicine, Nagoya, Aichi 466-8550 (Japan); Mechanobiology Institute Singapore, National University of Singapore, Singapore 117411 (Singapore)

2015-01-16

Highlights: • Proteoglycan from salmon nasal cartridge (SNC-PG) promoted wound healing in fibroblast monolayers. • SNC-PG stimulated both cell proliferation and cell migration. • Interaction between chondroitin sulfate-units and CD44 is responsible for the effect. - Abstract: Proteoglycans (PGs) are involved in various cellular functions including cell growth, adhesion, and differentiation; however, their physiological roles are not fully understood. In this study, we examined the effect of PG purified from salmon nasal cartilage (SNC-PG) on wound closure using tissue-cultured cell monolayers, an in vitro wound-healing assay. The results indicated that SNC-PG significantly promoted wound closure in NIH/3T3 cell monolayers by stimulating both cell proliferation and cell migration. SNC-PG was effective in concentrations from 0.1 to 10 μg/ml, but showed much less effect at higher concentrations (100–1000 μg/ml). The effect of SNC-PG was abolished by chondroitinase ABC, indicating that chondroitin sulfates (CSs), a major component of glycosaminoglycans (GAGs) in SNC-PG, are crucial for the SNC-PG effect. Furthermore, chondroitin 6-sulfate (C-6-S), a major CS of SNC-PG GAGs, could partially reproduce the SNC-PG effect and partially inhibit the binding of SNC-PG to cells, suggesting that SNC-PG exerts its effect through an interaction between the GAGs in SNC-PG and the cell surface. Neutralization by anti-CD44 antibodies or CD44 knockdown abolished SNC-PG binding to the cells and the SNC-PG effect on wound closure. These results suggest that interactions between CS-rich GAG-chains of SNC-PG and CD44 on the cell surface are responsible for the SNC-PG effect on wound closure.

A pilot evaluation of whole blood finger-prick sampling for point-of-care HIV viral load measurement: the UNICORN study.

Science.gov (United States)

Fidler, Sarah; Lewis, Heather; Meyerowitz, Jodi; Kuldanek, Kristin; Thornhill, John; Muir, David; Bonnissent, Alice; Timson, Georgina; Frater, John

2017-10-20

There is a global need for HIV viral load point-of-care (PoC) assays to monitor patients receiving antiretroviral therapy. UNICORN was the first study of an off-label protocol using whole blood finger-prick samples tested with and without a simple three minute spin using a clinic-room microcentrifuge. Two PoC assays were evaluated in 40 HIV-positive participants, 20 with detectable and 20 with undetectable plasma viral load (pVL) (<20 copies/ml). Using 100 µl finger-prick blood samples, the Cepheid Xpert HIV-1 Viral Load and HIV-1 Qual cartridges were compared with laboratory pVL assessment (TaqMan, Roche). For participants with undetectable viraemia by TaqMan, there was poor concordance without centrifugation with the TaqMan platform with only 40% 'undetectable' using Xpert VL and 25% 'not detected' using the Qual assay. After a 3 minute spin, 100% of samples were undetectable using either assay, showing full concordance with the TaqMan assay. Defining a lower limit of detection of 1000 copies/ml when including a spin, there was 100% concordance with the TaqMan platform with strong correlation (rho 0.95 and 0.94; p < 0.0001 for both assays). When including a simple microcentrifugation step, finger-prick PoC testing was a quick and accurate approach for assessing HIV viraemia, with excellent concordance with validated laboratory approaches.

Experimental study of nitrogen oxides in the IRT-M reactor

International Nuclear Information System (INIS)

Brazovskij, I.I.; Doroshevich, V.N.; Gvozdev, A.A.; Nesterenko, V.B.; Trubnikov, V.P.

1982-01-01

A critical review of different approaches to the radiolysis study of nitrogen oxide under mixed radiation conditions of a nuclear reactor was presented. Loop reactor piant opereted following gas-liquid cycle. It was shown in the process of long experiment in the operating conditions that irreversible radiation-thermal decomposition of the coolant increases little with temperature and pressure and radioactivity of the coolant and thermophysical equipment was moderate. Numerous kinetic experiments were conducted on the ampoule plant wherein all coolant existed in the zone of ionizing radiation effect. Initial pressure in the ampoule plant was set in the range of 0.1-16 MPa, depending on conditions of the experiment, and temperature 200-500 deg C. Dosimetry of the ampoule was carried out by the radiolysis of nitrogen monoxide. The analysis of the radiolysis products was conducted utilizing gas chromatography method, coolant vapours were removed in the process of low-temperature condensation under - 70 deg C

Fluid Delivery System For Capillary Electrophoretic Applications.

Science.gov (United States)

Li, Qingbo; Liu, Changsheng; Kane, Thomas E.; Kernan, John R.; Sonnenschein, Bernard; Sharer, Michael V.

2002-04-23

An automated electrophoretic system is disclosed. The system employs a capillary cartridge having a plurality of capillary tubes. The cartridge has a first array of capillary ends projecting from one side of a plate. The first array of capillary ends are spaced apart in substantially the same manner as the wells of a microtitre tray of standard size. This allows one to simultaneously perform capillary electrophoresis on samples present in each of the wells of the tray. The system includes a stacked, dual carrousel arrangement to eliminate cross-contamination resulting from reuse of the same buffer tray on consecutive executions from electrophoresis. The system also has a gel delivery module containing a gel syringe/a stepper motor or a high pressure chamber with a pump to quickly and uniformly deliver gel through the capillary tubes. The system further includes a multi-wavelength beam generator to generate a laser beam which produces a beam with a wide range of wavelengths. An off-line capillary reconditioner thoroughly cleans a capillary cartridge to enable simultaneous execution of electrophoresis with another capillary cartridge. The streamlined nature of the off-line capillary reconditioner offers the advantage of increased system throughput with a minimal increase in system cost.

Automated Parallel Capillary Electrophoretic System

Science.gov (United States)

Li, Qingbo; Kane, Thomas E.; Liu, Changsheng; Sonnenschein, Bernard; Sharer, Michael V.; Kernan, John R.

2000-02-22

An automated electrophoretic system is disclosed. The system employs a capillary cartridge having a plurality of capillary tubes. The cartridge has a first array of capillary ends projecting from one side of a plate. The first array of capillary ends are spaced apart in substantially the same manner as the wells of a microtitre tray of standard size. This allows one to simultaneously perform capillary electrophoresis on samples present in each of the wells of the tray. The system includes a stacked, dual carousel arrangement to eliminate cross-contamination resulting from reuse of the same buffer tray on consecutive executions from electrophoresis. The system also has a gel delivery module containing a gel syringe/a stepper motor or a high pressure chamber with a pump to quickly and uniformly deliver gel through the capillary tubes. The system further includes a multi-wavelength beam generator to generate a laser beam which produces a beam with a wide range of wavelengths. An off-line capillary reconditioner thoroughly cleans a capillary cartridge to enable simultaneous execution of electrophoresis with another capillary cartridge. The streamlined nature of the off-line capillary reconditioner offers the advantage of increased system throughput with a minimal increase in system cost.

Motorized Positioning Apparatus Having Coaxial Carrousels.

Science.gov (United States)

Li, Qingbo; Kane, Thomas E.; Liu, Changsheng; Sonnenschein, Bernard; Sharer, Michael V.; Kernan, John R.

2002-04-02

An automated electrophoretic system is disclosed. The system employs a capillary cartridge having a plurality of capillary tubes. The cartridge has a first array of capillary ends projecting from one side of a plate. The first array of capillary ends are spaced apart in substantially the same manner as the wells of a microtitre tray of standard size. This allows one to simultaneously perform capillary electrophoresis on samples present in each of the wells of the tray. The system includes a stacked, dual carrousel arrangement to eliminate cross-contamination resulting from reuse of the same buffer tray on consecutive executions from electrophoresis. The system also has a gel delivery module containing a gel syringe/a stepper motor or a high pressure chamber with a pump to quickly and uniformly deliver gel through the capillary tubes. The system further includes a multi-wavelength beam generator to generate a laser beam which produces a beam with a wide range of wavelengths. An off-line capillary reconditioner thoroughly cleans a capillary cartridge to enable simultaneous execution of electrophoresis with another capillary cartridge. The streamlined nature of the off-line capillary reconditioner offers the advantage of increased system throughput with a minimal increase in system cost.

The Origin and Time Dependence of the Amount and Composition of Non-Constituent Gases Present in Crystal Growth Systems

Science.gov (United States)

Palosz, Witold

1998-01-01

Presence of different, non-constituent gases may be a critical factor in crystal growth systems. In Physical Vapor Transport processes the cras(es) can be used intentionally (to prevent excessively high, unstable growth conditions), or can evolve unintentionally during the course of the process (which may lead to undesired reduction in the -rowth rate). In melt growth, particularly under low gravity conditions (reduced hydrostatic pressure) the gas present in the system may contribute to formation of voids in the growing crystals and even to a separation of the crystal and the liquid phase [1]. On the other hand, some amount of gas may facilitate 'contactless' crystal growth particularly under reduced gravity conditions [2 - 6]. Different non-constituent gases may be present in growth ampoules, and their amount and composition may change during the crystallization process. Some gases can appear even in empty ampoules sealed originally under high vacuum: they may diffuse in from the outside, and/or desorb from the ampoule walls. Residual gases can also be generated by the source materials: even very high purity commercial elements and compounds may contain trace amounts of impurities, particularly oxides. The oxides may have low volatilities themselves but their reaction with other species, particularly carbon and hydrogen, may produce volatile compounds like water or carbon oxides. The non-constituent gases, either added initially to the system or evolved during the material processing, may diffuse out of the ampoule during the course of the experiment. Gases present outside (e.g. as a protective atmosphere or thermal conductor) may diffuse into the ampoule. In either case the growth conditions and the quality of the crystals may be affected. The problem is of a particular importance in sealed systems where the amount of the gases cannot be directly controlled. Therefore a reasonable knowledge and understanding of the origin, composition, magnitude, and change with

Lab-on-a-Chip: From Astrobiology to the International Space Station

Science.gov (United States)

Maule, Jake; Wainwright, Nor; Steele, Andrew; Gunter, Dan; Monaco, Lisa A.; Wells, Mark E.; Morris, Heather C.; Boudreaux, Mark E.

2008-01-01

The continual and long-term habitation of enclosed environments, such as Antarctic stations, nuclear submarines and space stations, raises unique engineering, medical and operational challenges. There is no easy way out and no easy way to get supplies in. This situation elevates the importance of monitoring technology that can rapidly detect events within the habitat that affect crew safety such as fire, release of toxic chemicals and hazardous microorganisms. Traditional methods to monitor microorganisms on the International Space Station (ISS) have consisted of culturing samples for 3-5 days and eventual sample return to Earth. To augment these culture methods with new, rapid molecular techniques, we developed the Lab-on-a-Chip Application Development - Portable Test System (LOCAD-PTS). The system consists of a hand-held spectrophotometer, a series of interchangeable cartridges and a surface sampling/dilution kit that enables crew to collect samples and detect a range of biological molecules, all within 15 minutes. LOCAD-PTS was launched to the ISS aboard Space Shuttle Discovery in December 2006, where it was operated for the first time during March-May 2007. The surfaces of five separate sites in the US Lab and Node 1 of ISS were analyzed for endotoxin, using cartridges that employ the Limulus Amebocyte Lysate (LAL) assay; results of these tests will be presented. LOCAD-PTS will remain permanently onboard ISS with new cartridges scheduled for launch in February and October of 2008 for the detection of fungi (Beta-glucan) and Gram-positive bacteria (lipoteichoic acid), respectively.

Optical studies on Sn, K, Hg{sub 2} I{sub 2}, and I{sub 2}-doped {alpha}-HgI{sub 2}

Energy Technology Data Exchange (ETDEWEB)

Gonzalez, M.; Ibarra, A.; Willmott, C.; Pascual, J. L.; Dieguez, E.

1997-07-01

The influence on the optical properties of {alpha}-mercuric iodide stoichiometric deviations have been investigated. The optical behaviour of samples doped with Sn (IV) and K were also studied. To prepare mercury-rich and iodide rich samples (non-stoichiometric compounds), vapour phase crystal growth was performed on a closed ampoule with a mercurous iodide or iodine atmosphere, respectively. Dopants were introduced through the vapour phase by means of Snl{sub 4} and KI vapours during crystal growth. A decrease in the energy gap is deduced from the optical absorption spectra taken on non-stoichiometric and doped samples. Photoluminescence was also performed as a function of temperature while samples were under uniaxial pressure. Differences between doped, non-stoichiometric and pure samples are observed on luminescence emission wavelength and intensity.

Microcalorimetric measurements of heat production in human erythrocytes. IV. Comparison between different calorimetric techniques, suspension media, and preparation methods.

Science.gov (United States)

Monti, M; Wadsö, I

1976-10-01

Heat production in human erythrocytes from healthy subjects has been measured under different experimental conditions. Simultaneous measurements were made on the same samples using different types of microcalorimeters: a static ampoule calorimeter, an air perfusion calorimeter, and a flow calorimeter. Obtained heat effect values for specified standard conditions, P degrees, were within uncertainty limits the same for the different calorimeters. Cells were suspended either in autologous plasma or in a phosphate buffer. P degrees values for buffer suspensions were significantly higher than those for plasma suspensions. Erythrocyte samples prepared by the column adsorption technique gave higher P degrees values than those obtained by a conventional centrifugation procedure.

System for portable nucleic acid testing in low resource settings

Science.gov (United States)

Lu, Hsiang-Wei; Roskos, Kristina; Hickerson, Anna I.; Carey, Thomas; Niemz, Angelika

2013-03-01

Our overall goal is to enable timely diagnosis of infectious diseases through nucleic acid testing at the point-of-care and in low resource settings, via a compact system that integrates nucleic acid sample preparation, isothermal DNA amplification, and nucleic acid lateral flow (NALF) detection. We herein present an interim milestone, the design of the amplification and detection subsystem, and the characterization of thermal and fluidic control and assay execution within this system. Using an earlier prototype of the amplification and detection unit, comprised of a disposable cartridge containing flexible pouches, passive valves, and electrolysis-driven pumps, in conjunction with a small heater, we have demonstrated successful execution of an established and clinically validated isothermal loop-mediated amplification (LAMP) reaction targeting Mycobacterium tuberculosis (M.tb) DNA, coupled to NALF detection. The refined design presented herein incorporates miniaturized and integrated electrolytic pumps, novel passive valves, overall design changes to facilitate integration with an upstream sample preparation unit, and a refined instrument design that automates pumping, heating, and timing. Nucleic acid amplification occurs in a two-layer pouch that facilitates fluid handling and appropriate thermal control. The disposable cartridge is manufactured using low-cost and scalable techniques and forms a closed system to prevent workplace contamination by amplicons. In a parallel effort, we are developing a sample preparation unit based on similar design principles, which performs mechanical lysis of mycobacteria and DNA extraction from liquefied and disinfected sputum. Our next step is to combine sample preparation, amplification, and detection in a final integrated cartridge and device, to enable fully automated sample-in to answer-out diagnosis of active tuberculosis in primary care facilities of low-resource and high-burden countries.

[Monitoring of the residue of fosthiazate in water samples using solid-phase extraction coupled with gas chromatography/mass spectrometry].

Science.gov (United States)

Zhu, Jing; Zhou, Xin; Fu, Chunmei; Liu, Sankang; Li, Zhangwan

2004-11-01

Solid-phase extraction (SPE) coupled with gas chromatography/mass spectrometry (GC/MS) was used to determine the fosthiazate residue in water samples. The water samples were first filtered through cellulose filters (0.45 microm pore size). A 100 mL volume of filtered water, in which 1 mL of methanol has been added, was then passed through a pre-conditioned 3 cm C18 cartridge at a flow-rate of 1.5 mL/min. Elution was performed by 1 mL of methanol. The eluant was finally dried under reduced pressure for solvent evaporation. The volume was quantitatively adjusted to 0.5 mL with methanol. The analysis was carried out on GC/MS. The mass spectrometer was operated in selected ion monitoring (SIM) mode. According to mass spectrum of fosthiazate, three selected ions at m/z of 126, 195, 283, respectively, were monitored for identification and quantification. High sensitivity and selectivity were achieved by using this method. The limit of detection for fosthiazate in water samples was determined to be 56.4 ng/L. The linearity was demonstrated over a wide range of concentrations covering from 0.282 to 141 microg/L. The recoveries were more than 85.5% and the relative standard deviations for the overall procedure were less than 4.42%. The fosthiazate residue was detected in the water samples from a pool near cropland where fosthiazate was used. The results demonstrate the suitability of the SPE-GC/MS approach for the analysis of fosthiazate in water.

Determination of 99Tc in fresh water using TRU resin by ICP-MS.

Science.gov (United States)

Guérin, Nicolas; Riopel, Remi; Kramer-Tremblay, Sheila; de Silva, Nimal; Cornett, Jack; Dai, Xiongxin

2017-10-02

Technetium-99 ( 99 Tc) determination at trace level by inductively coupled plasma mass spectrometry (ICP-MS) is challenging because there is no readily available appropriate Tc isotopic tracer. A new method using Re as a recovery tracer to determine 99 Tc in fresh water samples, which does not require any evaporation step, was developed. Tc(VII) and Re(VII) were pre-concentrated on a small anion exchange resin (AER) cartridge from one litre of water sample. They were then efficiently eluted from the AER using a potassium permanganate (KMnO 4 ) solution. After the reduction of KMnO 4 in 2 M sulfuric acid solution, the sample was passed through a small TRU resin cartridge. Tc(VII) and Re(VII) retained on the TRU resin were eluted using near boiling water, which can be directly used for the ICP-MS measurement. The results for method optimisation, validation and application were reported. Crown Copyright © 2017. Published by Elsevier B.V. All rights reserved.

Evaluation of {sup 131}I retention in several adsorbers

Energy Technology Data Exchange (ETDEWEB)

Catanoso, Marcela F.; Osso Junior, Joao Alberto, E-mail: marcela.forli@gmail.co, E-mail: jaosso@ipen.b [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil). Diretoria de Radiofarmacia

2011-07-01

Several iodine radioisotopes are used in nuclear medicine for treatment and diagnostic purposes. The radioisotope {sup 131}I is used both in diagnosis and therapy due to its physical characteristics of decay by {beta}{sup -} and its {gamma}-ray emissions suitable for diagnosis. It is routinely produced at IPEN through the irradiation of TeO{sub 2} targets in the IEA-R1m nuclear reactor. After the irradiation, the {sup 131}I is separated by dry distillation, where the targets are put in an oven, heated at 760 deg C for 2 hours and the {sup 131}I, volatile, is carried by an O{sub 2} gas stream. The aim of this work was to evaluate the retention and elution of {sup 131}I samples produced at IPEN in several adsorbers as part of a project aiming the purification of these radioisotopes, allowing the labeling of biomolecules. Samples of {sup 131}I were used for retention and elution studies with the following adsorbers: commercial cartridges, anionic resin columns and cationic resin column. The results showed that Ag cartridges and anionic resins Dowex 1X8, Dowex 3 and IRA 400 had a great iodine retention but no elution after using specific eluents. The QMA light, acid alumina, neutral alumina and cationic resin Dowex 50WX4 showed high retention and elution and QMA plus and cationic resin Dowex 50WX8 and Dowex 50WX12 had a good retention but lower elution. Regarding to the better retention and elution, Ag cartridges and resins showed a higher percentage of iodine retention but lower elution yield and QMA light, acid and neutral alumina cartridges showed better results. (author)

Interpretation of measurements made by oscillations of irradiated fuels in natural uranium, graphite-gas piles

International Nuclear Information System (INIS)

Laponche, Bernard; Luffin, Jean; Brunet, Max; Guerange, Jacques; Tonolli, Jacky

1969-06-01

When considering a pile operation, it is interesting to know the evolution of fuel quality with respect to irradiation, i.e. the variation of its fission rate and of its absorption rate. In order to experimentally obtain these features, a method is to introduce an irradiated cartridge into a critical reactor and to measure the induced effect on its reactivity and on the neutron density at the vicinity of the cartridge. An oscillation method presented in another document and based on a periodic introduction of fuel sample into a critical reactor allows, from the measurement of reactivity variation (global signal), and of the neutron density (local signal), effective macroscopic fission and absorption cross sections of this sample to be obtained. As previous studies revealed that the interpretation of the local signal was notably delicate, this information has been replaced by computed information, the fission rate, which is determined by means of the COREGRAF1 code. Thus, the remaining quantity to be obtained is the fuel absorption rate. The authors report studies performed on several sets of cartridges from different reactors, and with an irradiation range from about 700 to 4000 MWJ/T. In a first part, they describe the characteristics of the studied cartridges, their irradiation and measurement conditions, and the use of the evolution code. In a second part, they try to define the interpretation of oscillation-based measurements by using two methods, a first and fast one which gives an approximation of results, and a more elaborated second one which complies with measurement conditions. The last part presents and discusses the obtained results [fr

Evaluation of 131I retention in several adsorbers

International Nuclear Information System (INIS)

Catanoso, Marcela F.; Osso Junior, Joao Alberto

2011-01-01

Several iodine radioisotopes are used in nuclear medicine for treatment and diagnostic purposes. The radioisotope 131 I is used both in diagnosis and therapy due to its physical characteristics of decay by β - and its γ-ray emissions suitable for diagnosis. It is routinely produced at IPEN through the irradiation of TeO 2 targets in the IEA-R1m nuclear reactor. After the irradiation, the 131 I is separated by dry distillation, where the targets are put in an oven, heated at 760 deg C for 2 hours and the 131 I, volatile, is carried by an O 2 gas stream. The aim of this work was to evaluate the retention and elution of 131 I samples produced at IPEN in several adsorbers as part of a project aiming the purification of these radioisotopes, allowing the labeling of biomolecules. Samples of 131 I were used for retention and elution studies with the following adsorbers: commercial cartridges, anionic resin columns and cationic resin column. The results showed that Ag cartridges and anionic resins Dowex 1X8, Dowex 3 and IRA 400 had a great iodine retention but no elution after using specific eluents. The QMA light, acid alumina, neutral alumina and cationic resin Dowex 50WX4 showed high retention and elution and QMA plus and cationic resin Dowex 50WX8 and Dowex 50WX12 had a good retention but lower elution. Regarding to the better retention and elution, Ag cartridges and resins showed a higher percentage of iodine retention but lower elution yield and QMA light, acid and neutral alumina cartridges showed better results. (author)

Adsorption of various antimicrobial agents to endotoxin removal polymyxin-B immobilized fiber (Toraymyxin®). Part 2: Adsorption of two drugs to Toraymyxin PMX-20R cartridges.

Science.gov (United States)

Shimokawa, Ken-ichi; Takakuwa, Ryotaro; Wada, Yuko; Yamazaki, Noriko; Ishii, Fumiyoshi

2013-01-01

In our previous study, the degree of adsorption of 9 representative antimicrobial agents to Toraymyxin(®) PMX-F sheets was quantitatively evaluated. As a result, the adsorption rate was 22.1% for Linezolid in the presence of serum. Therefore, we investigated whether two types of antimicrobial agents (Ciprofroxacin and Linezolid) can be better adsorbed on PMX-F sheets. When the number of PMX-F sheets was increased in a step wise manner, specifically 2, 4, 6, 8 and 12, the adsorption rate increased linearly. In addition, the adsorption to polymyxin-B immobilized fiber (Toraymyxin(®) PMX-20R) cartridges, widely used to remove endotoxins from circulating blood in the treatment of sepsis, was quantitatively evaluated. As a result, in the presence of serum, Linezolid showed adsorption to PMX-20R, and the adsorption rate after 2h was 54.5%, and that after 4h was 65.8%. The results of this study suggest the necessity of monitoring blood antimicrobial concentration during treatment for sepsis with Linezolid, which showed adsorption to PMX-20R in an environment close to a clinical environment. Copyright © 2012 Elsevier B.V. All rights reserved.

Chiral Analysis of Methamphetamine in Oral Fluid Samples: A Method to Distinguish Licit from Illicit Drug Use.

Science.gov (United States)

Borg, Damon; Kolb, Elizabeth; Lantigua, Cindy; Stripp, Richard

2018-01-01

Methamphetamine (MAMP) is a popular illicit drug abused for its central nervous system stimulating effects. MAMP is also used therapeutically in the treatment of overeating disorders, narcolepsy, attention deficit disorder, in over-the-counter (OTC) products to ease nasal congestion. MAMP exists in two enantiomeric forms, dextrorotary (d-MAMP) or levorotary (l-MAMP). The compounds are similar in chemical structure, simply differing in the orientation of functional groups around the asymmetric carbon. In part because of the availability of l-MAMP in OTC nasal inhalers, forensic guidelines require a sample to contain greater than 20% d-MAMP to consider illicit drug use when interpreting results. Standard analytical methods readily detect MAMP in biological specimens but cannot resolve the enantiomeric composition of the sample. Specialized analytical techniques based on chiral separation of the enantiomers are required to differentiate d-MAMP from l-MAMP. Our laboratory sought to develop and validate a method for the analysis of oral fluid specimens for d/l-MAMP using a chiral derivatizing agent and traditional reverse phase liquid chromatography tandem mass spectrometry (LC-MS-MS). MAMP was extracted from dilute oral fluid samples using Strata-XC solid phase extraction (SPE) cartridges and derivatized with Marfey's reagent. Chromatographic separation was achieved using Zorbax Eclipse Plus C18 columns. Linearity, accuracy and precision, recovery, matrix effects and specificity of the method were all within acceptable criteria. Intraday accuracy ranged from 93.3 to 103.4% and precision 0.1 to 1.6%. Interday accuracy ranged from 90.0 to 103.4% and precision 3.8 to 11.6%. Finally, having previously tested positive for MAMP using non-chiral analysis, 256 de-identified authentic oral fluid samples were analyzed using this validated method. 98% of all samples tested positive for d-MAMP at greater than 20%.

Development and validation of an SPE HG-AAS method for determination of inorganic arsenic in samples of marine origin

Energy Technology Data Exchange (ETDEWEB)

Rasmussen, Rie R.; Larsen, Erik H.; Sloth, Jens J. [Technical University of Denmark, National Food Institute, Division of Food Chemistry, Soeborg (Denmark); Hedegaard, Rikke V. [Technical University of Denmark, National Food Institute, Division of Food Chemistry, Soeborg (Denmark); University of Copenhagen, Faculty of Life Sciences, Department of Food Science, Frederiksberg (Denmark)

2012-07-15

The present paper describes a novel method for the quantitative determination of inorganic arsenic (iAs) in food and feed of marine origin. The samples were subjected to microwave-assisted extraction using diluted hydrochloric acid and hydrogen peroxide, which solubilised the analytes and oxidised arsenite (As{sup III}) to arsenate (As{sup V}). Subsequently, a pH buffering of the sample extract at pH 6 enabled selective elution of As{sup V} from a strong anion exchange solid-phase extraction (SPE) cartridge. Hydride generation atomic absorption spectrometry (HG-AAS) was applied to quantify the concentration of iAs (sum of As{sup III} and As{sup V}) as the total arsenic (As) in the SPE eluate. The results of the in-house validation showed that mean recoveries of 101-104% were achieved for samples spiked with iAs at 0.5, 1.0 and 1.5 mg.kg{sup -1}, respectively. The limit of detection was 0.08 mg kg{sup -1}, and the repeatability (RSD{sub r}) and intra-laboratory reproducibility (RSD{sub IR}) were less than 8% and 13%, respectively, for samples containing 0.2 to 1.5 mg kg{sup -1} iAs. The trueness of the SPE HG-AAS method was verified by confirming results obtained by parallel analysis using high-performance liquid chromatography coupled to inductively coupled plasma mass spectrometry. It was demonstrated that the two sets of results were not significantly different (P < 0.05). The SPE HG-AAS method was applied to 20 marine food and feed samples, and concentrations of up to 0.14 mg kg{sup -1} of iAs were detected. (orig.)

A simplified radiometabolite analysis procedure for PET radioligands using a solid phase extraction with micellar medium

International Nuclear Information System (INIS)

Nakao, Ryuji; Halldin, Christer

2013-01-01

A solid phase extraction method has been developed for simple and high-speed direct determination of PET radioligands in plasma. Methods: This methodology makes use of a micellar medium and a solid-phase extraction cartridge for displacement of plasma protein bound radioligand and separation of PET radioligands from their radiometabolites without significant preparation. The plasma samples taken from monkey or human during PET measurements were mixed with a micellar eluent containing an anionic surfactant sodium dodecyl sulphate and loaded onto SPE cartridges. The amount of radioactivity corresponding to parent radioligand (retained on the cartridge) and its radioactive metabolites (eluted with micellar eluent) was measured. Results: Under the optimized conditions, excellent separation of target PET radioligands from their radiometabolites was achieved with a single elution and short run-time of 1 min. This method was successfully applied to study the metabolism for 11 C-labelled radioligands in human or monkey plasma. The amount of parent PET radioligands estimated by micellar solid phase extraction strongly corresponded with that determined by radio-LC. The improved throughput permitted the analysis of a large number of plasma samples (up to 13 samples per one PET study) for accurate estimation of metabolite-corrected input function during quantitative PET imaging studies. Conclusion: Solid phase extraction together with micellar medium is fast, sensitive and easy to use, and therefore it is an attractive alternative method to determine relative composition of PET radioligands in plasma

Surfactant-enhanced spectrofluorimetric determination of total aflatoxins from wheat samples after magnetic solid-phase extraction using modified Fe3O4 nanoparticles

Science.gov (United States)

Manafi, Mohammad Hanif; Allahyari, Mehdi; Pourghazi, Kamyar; Amoli-Diva, Mitra; Taherimaslak, Zohreh

2015-07-01

The extraction and preconcentration of total aflatoxins (including aflatoxin B1, B2, G1, and G2) using magnetic nanoparticles based solid phase extraction (MSPE) followed by surfactant-enhanced spectrofluorimetric detection was proposed. Ethylene glycol bis-mercaptoacetate modified silica coated Fe3O4 nanoparticles as an efficient antibody-free adsorbent was successfully applied to extract aflatoxins from wheat samples. High surface area and strong magnetization properties of magnetic nanoparticles were utilized to achieve high enrichment factor (97), and satisfactory recoveries (92-105%) using only 100 mg of the adsorbent. Furthermore, the fast separation time (less than 10 min) avoids many time-consuming cartridge loading or column-passing procedures accompany with the conventional SPE. In determination step, signal enhancement was performed by formation of Triton X-100 micelles around the analytes in 15% (v/v) acetonitrile-water which dramatically increase the sensitivity of the method. Main factors affecting the extraction efficiency and signal enhancement of the analytes including pH of sample solution, desorption conditions, extraction time, sample volume, adsorbent amount, surfactant concentration and volume and time of micelle formation were evaluated and optimized. Under the optimum conditions, wide linear range of 0.1-50 ng mL-1 with low detection limit of 0.03 ng mL-1 were obtained. The developed method was successfully applied to the extraction and preconcentration of aflatoxins in three commercially available wheat samples and the results were compared with the official AOAC method.

Rapid determination of glyphosate in cereal samples by means of pre-column derivatisation with 9-fluorenylmethyl chloroformate and coupled-column liquid chromatography with fluorescence detection.

Science.gov (United States)

Hogendoorn, E A; Ossendrijver, F M; Dijkman, E; Baumann, R A

1999-02-12

A rapid procedure for the determination of glyphosate in cereals has been developed. Convenient sample pretreatment is carried out by (i) a overnight standing extraction of 1.0 g homogenized sample with 20 ml of water, (ii) centrifugation of the samples, (iii) a passing of 2.5 ml of the clear layer through a 100 mg C18 solid-phase extraction cartridge and (iv) collection of the last 1.5 ml of the eluent into a calibrated tube. For the instrumental analysis, the efficient approach developed earlier for environmental water samples [J.V. Sancho, F. Hernández, F.J. LUpez, E.A. Hogendoorn, E. Dijkman, P. van Zoonen, J. Chromatogr. A, 737 (1996) 75] was successfully adopted for the determination of glyphosate in the obtained cereal extracts. The procedure includes a 15 min derivatisation step of the analyte with 9-fluorenylmethyl chloroformate and a 16 times dilution step prior to instrumental analysis employing coupled-column LC with fluorescence detection. The developed procedure has a sample throughput of more than 25 samples per day and a limit of quantification of 0.5 mg/kg. The method was validated by analyzing freshly spiked cereal samples and samples with aged residues at levels between 1.0 and 10 mg/kg. The overall recovery of the freshly spiked samples was 86% (n = 10) with a repeatability of 6.5% and a reproducibility of 9.5%. For samples with aged residues recoveries performed at different time intervals (range 80-150 days) did not differ significantly; the overall recovery (n = 10) was 74% with a repeatability and reproducibility of 14 and 20%, respectively.

Radioimmunoassay in microtiter plates

International Nuclear Information System (INIS)

Hirschberg, T.; Hirschberg, H.

1987-01-01

A radioimmunoassay was performed in the wells of casein-coated microplates employing 125 I-labelled sheep anti-human second antibody. The antigen-antibody complexes were thereafter dislodged from the well walls using detergent sodium dodecyl sulfate (SDS) and the entire contents of the wells were simultaneously absorbed into 48 cellulose acetate-absorbing cartridges. All 48 cartridges were transferred to counting vials and the radioactivity determined by standard gamma counting techniques. The particular advantage of the method described here is the ease with which the supernatants can be collected and transferred to counting vials with minimal handling of radioactive samples. 6 refs.; 1 figure; 1 table

Método colorimétrico para determinação de dióxido de nitrogênio atmosférico com preconcentração em coluna de c-18

Directory of Open Access Journals (Sweden)

Ugucione Cássia

2002-01-01

Full Text Available An alternative analytical method for nitrogen dioxide (NO2 in atmosphere was developed. The collection of NO2 is performed by a Sep-Pack C-18 cartridge impregnated with 11% (v/v of triethanolamine plus 3,6 % (v/v of ethylene glycol plus 25 % (v/v of acetone combined solution. When the impregnating is used, NO2 is collected with good repeatibility (CV = 3,3 %. The NO2 absorbed in the sampler was stripped from the sorbent with a methanol 5% (v/v aqueous solution and was determined by colorimetry as nitrite by using the Griess-Saltzman reagent. The detection limit of 1,4 ppb for 60 min sampling at 0,5 L min-1 flow rate was obtained. Preparation and conditioning procedures for TEA-C-18 cartridge, sampling flow rate, absorption capacity and interference of other species are discussed.

Development of a rapid LC-DAD/FLD method for the simultaneous determination of auxins and abscisic acid in plant extracts.

Science.gov (United States)

Bosco, Renato; Caser, Matteo; Vanara, Francesca; Scariot, Valentina

2013-11-20

Plant hormones play a crucial role in controlling plant growth and development. These groups of naturally occurring substances trigger physiological processes at very low concentrations, which mandate sensitive techniques for their quantitation. This paper describes a method to quantify endogenous (±)-2-cis-4-trans-abscisic acid, indole-3-acetic acid, indole-3-propionic acid, and indole-3-butyric acid. The method combines high-performance liquid chromatography (HPLC) with diode array and fluorescence detection in a single run. Hybrid tea rose 'Monferrato' matrices (leaves, petals, roots, seeds, androecium, gynoecium, and pollen) were used as references. Rose samples were separated and suspended in extracting methanol, after which (±)-2-cis-4-trans-abscisic acid and auxins were extracted by solvent extraction. Sample solutions were added first to cation solid phase extraction (SPE) cartridges and the eluates to anion SPE cartridges. The acidic hormones were bound to the last column and eluted with 5% phosphoric acid in methanol. Experimental results showed that this approach can be successfully applied to real samples and that sample preparation and total time for routine analysis can be greatly reduced.

Combining selection valve and mixing chamber for nanoflow gradient generation: Toward developing a liquid chromatography cartridge coupled with mass spectrometer for protein and peptide analysis.

Science.gov (United States)

Chen, Apeng; Lu, Joann J; Gu, Congying; Zhang, Min; Lynch, Kyle B; Liu, Shaorong

2015-08-05

Toward developing a micro HPLC cartridge, we have recently built a high-pressure electroosmotic pump (EOP). However, we do not recommend people to use this pump to deliver an organic solvent directly, because it often makes the pump rate unstable. We have experimented several approaches to address this issue, but none of them are satisfactory. Here, we develop an innovative approach to address this issue. We first create an abruption (a dead-volume) within a fluid conduit. We then utilize an EOP to withdraw, via a selection valve, a train of eluent solutions having decreasing eluting power into the fluid conduit. When these solutions are further aspirated through the dead-volume, these solutions are partially mixed, smoothening concentration transitions between two adjacent eluent solutions. As these solutions are pushed back, through the dead-volume again, a smooth gradient profile is formed. In this work, we characterize this scheme for gradient formation, and we incorporate this approach with a high-pressure EOP, a nanoliter injection valve, and a capillary column, yielding a micro HPLC system. We then couple this micro HPLC with an electrospray ionization - mass spectrometer for peptide and protein separations and identifications. Copyright © 2015 Elsevier B.V. All rights reserved.

Hexagonal boron nitride nanosheets as adsorbents for solid-phase extraction of polychlorinated biphenyls from water samples

Energy Technology Data Exchange (ETDEWEB)

Jia, Shiliang; Wang, Zhenhua; Ding, Ning [Key Laboratory for Applied Technology of Sophisticated Analytical Instruments, Shandong Academy of Sciences, Jinan, Shandong (China); Elaine Wong, Y.-L. [Department of Chemistry, The Chinese University of Hong Kong, Hong Kong Special Administrative Region (Hong Kong); Chen, Xiangfeng, E-mail: xiangfchensdas@163.com [Key Laboratory for Applied Technology of Sophisticated Analytical Instruments, Shandong Academy of Sciences, Jinan, Shandong (China); Department of Chemistry, The Chinese University of Hong Kong, Hong Kong Special Administrative Region (Hong Kong); Qiu, Guangyu [Department of Physics and Materials Science, City University of Hong Kong, Hong Kong Special Administrative Region (Hong Kong); Dominic Chan, T.-W., E-mail: twdchan@cuhk.edu.hk [Department of Chemistry, The Chinese University of Hong Kong, Hong Kong Special Administrative Region (Hong Kong)

2016-09-14

The adsorptive potential of hexagonal boron nitride nanosheets (h-BNNSs) for solid-phase extraction (SPE) of pollutants was investigated for the first time. Seven indicators of polychlorinated biphenyls (PCBs) were selected as target analytes. The adsorption of PCBs on the surface of the h-BNNSs in water was simulated by the density functional theory and molecular dynamics. The simulation results indicated that the PCBs are adsorbed on the surface by π–π, hydrophobic, and electrostatic interactions. The PCBs were extracted with an h-BNNS-packed SPE cartridge, and eluted by dichloromethane. Gas chromatography–tandem mass spectrometry working in the multiple reaction monitor mode was used for the sample quantification. The effect of extraction parameters, including the flow rate, pH value, breakthrough volume, and the ionic strength, were investigated. Under the optimal working conditions, the developed method showed low limits of detection (0.24–0.50 ng L{sup −1}; signal-to-noise ratio = 3:1), low limits of quantification (0.79–1.56 ng L{sup −1}; signal-to-noise ratio = 10:1), satisfactory linearity (r > 0.99) within the concentration range of 2–1000 ng L{sup −1}, and good precision (relative standard deviation < 12%). The PCBs concentration in environmental water samples was determined by the developed method. This results demonstrate that h-BNNSs have high analytical potential in the enrichment of pollutants. - Highlights: • The hexagonal boron nitride nanosheets were synthesized. • The nanosheets were used as adsorbent for solid-phase extraction. • The h-BN demonstrates remarkable adsorption of PCBs from water samples. • The method was successfully applied in determination of PCBs in water samples.

Neutron Activation analysis of waste water

International Nuclear Information System (INIS)

Hernandez H, V.

1997-01-01

An instrumental neutron activation analysis for the simultaneous determination of chlorine, bromine, sodium, manganese, cobalt, copper, chromium, zinc, nickel, antimony and iron in waste water is described. They were determined in waste water samples under normal conditions by non-destructive neutron activation simultaneously using a suitable monostandard method. Standardized water samples were used and irradiated in polyethylene ampoules at a neutron flux of 10 13 cm -2 s -1 for periods of 1 minute, 1 and 10 hours. A Ge hyperpure detector was used for your activity determination, with count times of 60, 180, 300 and 600 seconds. The obtained results show than the method can be utilized for the determination of this elements without realize anything previous treatment of the samples. (Author)

Neutron Activation analysis of waste water; Analisis de aguas residuales mediante activacion neutronica

Energy Technology Data Exchange (ETDEWEB)

Hernandez H, V

1997-12-01

An instrumental neutron activation analysis for the simultaneous determination of chlorine, bromine, sodium, manganese, cobalt, copper, chromium, zinc, nickel, antimony and iron in waste water is described. They were determined in waste water samples under normal conditions by non-destructive neutron activation simultaneously using a suitable monostandard method. Standardized water samples were used and irradiated in polyethylene ampoules at a neutron flux of 10{sup 13} cm{sup -2} s{sup -1} for periods of 1 minute, 1 and 10 hours. A Ge hyperpure detector was used for your activity determination, with count times of 60, 180, 300 and 600 seconds. The obtained results show than the method can be utilized for the determination of this elements without realize anything previous treatment of the samples. (Author).

A new method activation analysis of 131I in charcoal cartridge sampler

International Nuclear Information System (INIS)

Lai Caifeng; Xu Jiayun; Qin Jianguo; Wang Dalun

2011-01-01

Instead of the traditional method for measuring 1311 activation by calibrating the detecting efficiency, MCNP5 calculation and ill-posed equation solution were used in a new method for analysing 131 I activation and depth distribution in sample box. Because of no necessary to prepare for standard sample and calibrate the efficiency, it makes the survey of 131 I more quickly and accurately and is able to take into account the physics processes of 131 I in the sample box. (authors)

Successful therapeutic response of resistant cases of mucocutaneous leishmaniasis to a very low dose of antimony Resposta terapêutica bem sucedida de casos resistentes de leishmaniose mucocutânea a doses muito baixas de antimônio

Directory of Open Access Journals (Sweden)

Manoel Paes de Oliveira-Neto

2006-08-01

Full Text Available Two mucocutaneous leishmaniasis cases resistant to therapy are reported here. After the failure of initial therapies (antimony, amphotericin B and/or pentamidine patients received a low-dose schedule: one ampoule of meglumine antimoniate (405mg of pentavalent antimony [Sb v] by intramuscular injection, three times a week until complete healing of the lesions. One patient was cured with a total of 30 ampoules in 10 weeks and the other received 36 ampoules in 12 weeks. Both remain clinically cured after one year of follow-up.São relatados dois casos de leishmaniose mucocutânea resistentes ao tratamento. Depois das terapêuticas iniciais (antimônio, anfotericina B e/ou pentamidina, os pacientes receberam um esquema alternativo: uma ampola de antimoniato de meglumina (405mg de antimônio pentavalnte [Sb v] por via intramuscular, três vezes por semana até a cura completa das lesões. Um paciente recebeu um total de 30 ampolas durante 10 semanas e o outro, 36 ampolas durante 12 semanas. Ambos permanecem clinicamente curados até um ano após o tratamento.

Establishment of carcinoembryonic antigen working standard for immunoassay

International Nuclear Information System (INIS)

Xu Ligen; Sun Youxiang; Jiao Yan

2001-01-01

The author is to prepare the working standard of carcinoembryonic antigen (CEA) for immunoassay and determine its potency. CEA solution of 320 μg/L was prepared from purified CEA solution of 4.6 mg/L and 1% human albumin solution buffered with 50 mmol/L sodium phosphate, pH7.4. This solution was distributed in an aliquot of 0.5 mL (160 ng per ampoule) and lyophilized. The potency of CEA working standard, in terms of present standard of CEA RIA and IRMA kits made by Chinese manufacturers and in terms of 1st IRP CEA HUMAN 73/601 supplied by WHO, has been determined. Mean immunological potency of the working standard is 163 ng per ampoule with confident limit of 159-168 ng per ampoule at 95% probability level. Test of parallelism of dose-response curve for the working standard to that for 1st IRP CEA HUMAN 73/601 has been passed. CEA working standard is suitable to the kits standard for CEA radioimmunoassay and immunoradiometric assay

Meniscus Shapes in Detached Bridgman Growth

Science.gov (United States)

Volz, M. P.; Mazuruk, K

2010-01-01

In detached Bridgman crystal growth, most of the melt is in contact with the ampoule wall, but the crystal is separated from the wall by a small gap, typically 1-100 micrometers. A liquid free surface, or meniscus, bridges across this gap at the position of the melt-crystal interface. Meniscus shapes have been calculated for the case of detached Bridgman growth in cylindrical ampoules by solving the Young-Laplace equation. Key parameters affecting meniscus shapes are the growth angle, contact angle of the meniscus to the ampoule wall, the pressure differential across the meniscus, and the Bond number, a measure of the ratio of gravitational to capillary forces. In general, for specified values of growth and contact angles, solutions exist only over a finite range of pressure differentials. For intermediate values of the Bond number, there are multiple solutions to the Young-Laplace equations. There are also cases where, as a function of pressure differential, existence intervals alternate with intervals where no solutions exist. The implications of the meniscus shape calculations on meniscus stability are discussed.

The Use of a Mechanical Non-Penetrating Captive Bolt Device for the Euthanasia of Neonate Lambs.

Science.gov (United States)

Grist, Andrew; Lines, Jeff A; Knowles, Toby G; Mason, Charles W; Wotton, Stephen B

2018-04-02

A non-penetrating captive bolt device, powered by a 1-grain 0.22″ cartridge delivering a calculated kinetic energy of 47 Joules was tested as a euthanasia method on 200 neonate lambs (Ovis aries) of 4.464 kg (SD (Standard deviation) ± 1.056) mean dead weight, to assess effectiveness and shot position. Every lamb (n = 200) was effectively stunned when the weapon was applied powered by a brown, 1-grain cartridge but 10/200 (5%) of the lambs displayed rhythmic or agonal breathing and were subsequently euthanased using euthatal (Merial, UK, GTIN: 03661103015550). Evaluation of the method was conducted using behavioural indicators of brain dysfunction followed by post-mortem examination of the heads. A second trial was conducted using a higher velocity 1.25-grain cartridge and a specific shot position on 48 lambs (mean dead weight = 6.21 kg, SD ± 1.24) averaging 5 days old. One hundred percent of the lambs in the second trial were immediately stun-killed. Given this complete kill rate and the sample size of the study, the study provides a statistical 95% confidence interval of 92.6% to 100%. The use of the Accles & Shelvoke “CASH” Small Animal Tool (Birmingham, UK) can therefore be recommended for the euthanasia of neonate lambs with a 1.25-grain cartridge and a specific shooting position.

The Use of a Mechanical Non-Penetrating Captive Bolt Device for the Euthanasia of Neonate Lambs

Directory of Open Access Journals (Sweden)

Andrew Grist

2018-04-01

Full Text Available A non-penetrating captive bolt device, powered by a 1-grain 0.22″ cartridge delivering a calculated kinetic energy of 47 Joules was tested as a euthanasia method on 200 neonate lambs (Ovis aries of 4.464 kg (SD (Standard deviation ± 1.056 mean dead weight, to assess effectiveness and shot position. Every lamb (n = 200 was effectively stunned when the weapon was applied powered by a brown, 1-grain cartridge but 10/200 (5% of the lambs displayed rhythmic or agonal breathing and were subsequently euthanased using euthatal (Merial, UK, GTIN: 03661103015550. Evaluation of the method was conducted using behavioural indicators of brain dysfunction followed by post-mortem examination of the heads. A second trial was conducted using a higher velocity 1.25-grain cartridge and a specific shot position on 48 lambs (mean dead weight = 6.21 kg, SD ± 1.24 averaging 5 days old. One hundred percent of the lambs in the second trial were immediately stun-killed. Given this complete kill rate and the sample size of the study, the study provides a statistical 95% confidence interval of 92.6% to 100%. The use of the Accles & Shelvoke “CASH” Small Animal Tool (Birmingham, UK can therefore be recommended for the euthanasia of neonate lambs with a 1.25-grain cartridge and a specific shooting position.

Restricted access carbon nanotubes for direct extraction of cadmium from human serum samples followed by atomic absorption spectrometry analysis.

Science.gov (United States)

Barbosa, Adriano F; Barbosa, Valéria M P; Bettini, Jefferson; Luccas, Pedro O; Figueiredo, Eduardo C

2015-01-01

In this paper, we propose a new sorbent that is able to extract metal ions directly from untreated biological fluids, simultaneously excluding all proteins from these samples. The sorbent was obtained through the modification of carbon nanotubes (CNTs) with an external bovine serum albumin (BSA) layer, resulting in restricted access carbon nanotubes (RACNTs). The BSA layer was fixed through the interconnection between the amine groups of the BSA using glutaraldehyde as cross-linker. When a protein sample is percolated through a cartridge containing RACNTs and the sample pH is higher than the isoelectric point of the proteins, both proteins from the sample and the BSA layer are negatively ionized. Thus, an electrostatic repulsion prevents the interaction between the proteins from the sample on the RACNTs surface. At the same time, metal ions are adsorbed in the CNTs (core) after their passage through the chains of proteins. The Cd(2+) ion was selected for a proof-of-principle case to test the suitability of the RACNTs due to its toxicological relevance. RACNTs were able to extract Cd(2+) and exclude almost 100% of the proteins from the human serum samples in an online solid-phase extraction system coupled with thermospray flame furnace atomic absorption spectrometry. The limits of detection and quantification were 0.24 and 0.80 μg L(-1), respectively. The sampling frequency was 8.6h(-1), and the intra- and inter-day precisions at the 0.80, 15.0, and 30.0 μg L(-1) Cd(2+) levels were all lower than 10.1% (RSD). The recoveries obtained for human blood serum samples fortified with Cd(2+) ranged from 85.0% to 112.0%. The method was successfully applied to analyze Cd(2+) directly from six human blood serum samples without any pretreatment, and the observed concentrations ranged from

Airborne aldehydes in cabin-air of commercial aircraft: Measurement by HPLC with UV absorbance detection of 2,4-dinitrophenylhydrazones.

Science.gov (United States)

Rosenberger, Wolfgang; Beckmann, Bibiana; Wrbitzky, Renate

2016-04-15

This paper presents the strategy and results of in-flight measurements of airborne aldehydes during normal operation and reported "smell events" on commercial aircraft. The aldehyde-measurement is a part of a large-scale study on cabin-air quality. The aims of this study were to describe cabin-air quality in general and to detect chemical abnormalities during the so-called "smell-events". Adsorption and derivatization of airborne aldehydes on 2,4-dinitrophenylhydrazine coated silica gel (DNPH-cartridge) was applied using tailor-made sampling kits. Samples were collected with battery supplied personal air sampling pumps during different flight phases. Furthermore, the influence of ozone was investigated by simultaneous sampling with and without ozone absorption unit (ozone converter) assembled to the DNPH-cartridges and found to be negligible. The method was validated for 14 aldehydes and found to be precise (RSD, 5.5-10.6%) and accurate (recovery, 98-103 %), with LOD levels being 0.3-0.6 μg/m(3). According to occupational exposure limits (OEL) or indoor air guidelines no unusual or noticeable aldehyde pollution was observed. In total, 353 aldehyde samples were taken from two types of aircraft. Formaldehyde (overall average 5.7 μg/m(3), overall median 4.9 μg/m(3), range 0.4-44 μg/m(3)), acetaldehyde (overall average 6.5 μg/m(3), overall median 4.6, range 0.3-90 μg/m(3)) and mostly very low concentrations of other aldehydes were measured on 108 flights. Simultaneous adsorption and derivatization of airborne aldehydes on DNPH-cartridges to the Schiff bases and their HPLC analysis with UV absorbance detection is a useful method to measure aldehydes in cabin-air of commercial aircraft. Copyright © 2015 Elsevier B.V. All rights reserved.

Pre-concentration of pesticide residues in environmental water samples using Silica nanoparticles and identification of residues By GC-MS method

OpenAIRE

Tentu. Nageswara Rao; A. Muralidhar Reddy; SNVS. Murthy; Prathipati Revathi; K. Suneel Kumar

2016-01-01

The silica nanoparticles prepared by stober’s mechanism by reaction of tetraethylorthosilicate (TEOS) with ammonia was tested for their adsorption capacity in the pre-concentration of residues of pesticides in water. The synthesized nanoparticles were characterized by Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM) and X-Ray Diffraction (XRD). The size of the silica nanoparticles were 50 to 250 nm. The solid phase extraction (SPE) cartridges were prepared by filling...

Radioimmunoassay of deoxynivalenol in wheat and corn

International Nuclear Information System (INIS)

Xu, Y.C.; Zhang, G.S.; Chu, F.S.

1986-01-01

With the availability of antibody against deoxynivalenol triacetate (DON-triacetate), a radioimmunoassay (RIA) for DON in wheat was developed. DON is extracted from the sample with acetonitrile-water defatted with hexane, and then reacted with acetic anhydride to form DON-triacetate. The reaction mixture is loaded onto a C-18 cartridge to remove excess reagents and impurities. Acetylated DON is eluted from the cartridge with 50% methanol in water, and then analyzed by radioimmunoassay utilizing antiserum against DON-triacetate and tritiated DON-triacetate. Overall recovery for DON added to wheat between 50 and 5000 ppb was 86% with a standard deviation of 7% and coefficient of variation of 8%. The limit of detection for DON was about 20 ppb. Analysis of 12 naturally contaminated wheat, corn, and mixed feed samples for DON revealed that RIA results agreed well with thin layer chromatographic analyses performed by other laboratories

Determination of seven bisphenol analogues in reed and Callitrichaceae by ultra performance liquid chromatography-tandem mass spectrometry.

Science.gov (United States)

Lu, Libin; Yang, Yunjia; Zhang, Jing; Shao, Bing

2014-03-15

An analytical procedure was developed to simultaneously determine bisphenol S, bisphenol F, bisphenol B, bisphenol A, bisphenol AF, tetrachlorobisphenol A, and tetrabromobisphenol A in reed and Callitrichaceae. Homogenized samples were extracted with acetonitrile and purified using an ENVI™-Carb cartridge followed by an NH2 cartridge. The analytes were separated and quantified by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The recoveries at three fortified levels in reed and Callitrichaceae were 57-108% and 68-106%, respectively, with relative standard deviations of no more than 15% (n=6). The method limits of quantification and detection for the seven bisphenol analogues were 0.005-0.500μg/kg and 0.002-0.150μg/kg, respectively. This method was used to analyze the seven compounds in ten reed and Callitrichaceae samples collected from Zhejiang, China. Copyright © 2014 Elsevier B.V. All rights reserved.

Determination of emamectin benzoate in medicated fish feed.

Science.gov (United States)

Farer, L J; Hayes, J; Rosen, J; Knight, P

1999-01-01

A method was developed to quantitate emamectin benzoate in fish feed at levels between 5 and 15 ppm. The active ingredient is extracted from 20 g medicated feed into aqueous-methanolic solvent by overnight shaking. A solid-phase extraction procedure using a 2 g C18 cartridge is then used to concentrate the active residue and remove interfering matrix components. The extracted drug and internal standard are eluted from the cartridge, evaporated to dryness, and reconstituted in methanol. A control feed sample and fortified control working standard are simultaneously prepared. Remaining interferences and sample analysis are further separated on a gradient liquid chromatographic system. Recovery of emamectin benzoate from fortified feeds ranged from 97 to 100%, with a coefficient of variation (CV) of 1.2%. Determination of emamectin benzoate in medicated feeds resulted in CVs ranging from 2.3 to 4.2% and recoveries of 88 to 98% of label claim.

Analysis Study of Stevioside and Rebaudioside A from Stevia rebaudiana Bertoni by Normal Phase SPE and RP-HPLC

Science.gov (United States)

Martono, Y.; Rohman, A.; Riyanto, S.; Martono, S.

2018-04-01

Solid Phase Extraction (SPE) method using silica as sorbent for stevioside and rebaudiosida A analysis in Stevia rebaudiana Bertoni leaf have not been performed. The aim of this study is to develop SPE method using silica as sorbent for Reverse Phase-High Performance Liquid Chromatography (RP-HPLC) analysis of stevioside and rebaudiosida A in S. rebaudiana leaf. The results of this study indicate that the optimal conditions for normal phase SPE (silica) are conditioned with 3.0 mL of hexane. The sample loading volume is 0.1 mL. Cartridge is eluted with 1.0 mL acetonitrile: water (80: 20, v/v) to separate both analytes. The cartridge is washed with chloroform and water of 0.3 mL respectively. The developed SPE sample preparation method meets the accuracy and precision test and can be used for the analysis of stevioside and rebaudioside A by RP-HPLC.

Temperature measurement of the reactor materials samples irradiated in the fuel channels of the RA reactor - Annex 16; Prilog 16 - Merenje temperature uzoraka reaktorskih materijala ozracivanih u gorivnim kanalima reaktora RA

Energy Technology Data Exchange (ETDEWEB)

Nikolic, M; Djalovic, M [Institute of Nuclear Sciences Boris Kidric, Reaktor RA, Vinca, Beograd (Serbia and Montenegro)

1964-12-15

Reactor materials as graphite, stainless steel, magnox, zirconium alloys, etc. were exposed to fast neutron flux inside the fuel elements specially adapted for this purpose. Samples in the form ampoules were placed in capsules inside the fuel channels and cooled by heavy water which cools the fuel elements. In order to monitor the samples temperature 42 thermocouples were placed in the samples. That was necessary for reactor safety reasons and for further interpretation of measured results. Temperature monitoring was done continuously by multichannel milivoltmeters. This paper describes the technique of introducing the thermocouples, compensation instruments, control of the cold ends and adaptation of the instruments for precision (0.5%) temperature measurement in the range 30 deg - 130 deg C; 30 deg - 280 deg C and 30 deg - 80 deg C. Ozracivanje uzoraka materijala za izgradnju reaktora kao sto su grafit, nerdjajuci celik, magnox, legure cirkonijuma, aluminijuma itd. vrseno je u fluksu brzih neutrona unutar samih gorivnih elemenata koji su specijalno adaptirani za ovu svrhu. Uzorci u vidu ampula smesteni su u kapsulu od aluminijuma i postavljeni unutar kanala gde su hladjeni cirkulacijom teske vode koja hladi same gorivne elemente. U cilju kontrole temperature uzoraka radi bezbednosti samog reaktora, kao i radi kasnije interpretacije rezultata ispitivanja radijacionog ostecenja materijala, ugradjeno je 42 termopara u uzorke. Kontrola temperature je vrsena kontinualno visekanalnim registratorima. U radu je prikazana tehnika izvodjenja termoparova, kompenzacionih vodova, kontrola hladnih krajeva i prilagodjenje instrumentacije za merenje i registraciju temperature sa tacnoscu 0,5% u opsezima 30 deg - 130 deg C; 30 deg - 280 deg C i 30 deg - 80 deg C (author)

Bottom loaded filter for radioactive liquids

International Nuclear Information System (INIS)

Wendland, W.G.

1980-01-01

A bottom loaded filter assembly for filtering radioactive liquids through a replaceable cartridge filter is disclosed. The filter assembly includes a lead-filled jacket enveloping a housing having a chamber therein for the filter cartridge. A track arrangement carries a hatch for sealing the chamber. A spacer plug supports the cartridge within guide means associated with the inlet conduit in the chamber. The plug and cartridge drop out of the chamber when the hatch is unbolted and move laterally of the chamber. During cartridge replacement, a new plug and cartridge are supported in the guide means by a spacer bar inserted across the track means under the chamber. The hatch is then slid under the chamber and bolted to the vessel, engaging an o-ring to seal the chamber

[Determination method of polysorbates in powdered soup by HPLC].

Science.gov (United States)

Takeda, Y; Abe, Y; Ishiwata, H; Yamada, T

2001-04-01

A method for qualitative and quantitative analyses of polysorbates in powdered soup by HPLC was studied. Polysorbates in samples were extracted with acetonitrile after rinsing with n-hexane to remove fats and oils. The extract was cleaned up using a Bond Elut silica gel cartridge (500 mg). The cartridge was washed with ethyl acetate and polysorbates were eluted with a small amount of acetonitrile-methanol (1:2) mixture. The eluate was treated with cobalt thiocyanate solution to form a blue complex with polysorbate. In order to determine polysorbate, the complex was subjected to HPLC with a GPC column, using a mixture of acetonitrile-water (95:5) as a mobile phase, with a detection wavelength of 620 nm. The recoveries of polysorbate 80 added to powdered soups were more than 75% and the determination limit was 0.04 mg/g. When the proposed method was applied to the determination of polysorbates in 16 commercial samples of powdered soup for instant noodles and seasoning consomme, no polysorbates were detected in any sample.

Development and validation of an automated unit for the extraction of radiocaesium from seawater

International Nuclear Information System (INIS)

Bokor, Ilonka; Sdraulig, Sandra; Jenkinson, Peter; Madamperuma, Janaka; Martin, Paul

2016-01-01

An automated unit was developed for the in-situ extraction of radiocaesium ( 137 Cs and 134 Cs) from large volumes of seawater to achieve very low detection limits. The unit was designed for monitoring of Australian ocean and coastal waters, including at ports visited by nuclear-powered warships. The unit is housed within a robust case, and is easily transported and operated. It contains four filter cartridges connected in series. The first two cartridges are used to remove any suspended material that may be present in the seawater, while the last two cartridges are coated with potassium copper hexacyanoferrate for caesium extraction. Once the extraction is completed the coated cartridges are ashed. The ash is transferred to a small petri dish for counting of 137 Cs and 134 Cs by high resolution gamma spectrometry for a minimum of 24 h. The extraction method was validated for the following criteria: selectivity, trueness, precision, linearity, limit of detection and traceability. The validation showed the unit to be fit for purpose with the method capable of achieving low detection limits required for environmental samples. The results for the environmental measurements in Australian seawater correlate well with those reported in the Worldwide Marine Radioactivity Study (WOMARS). The cost of preparation and running the system is low and waste generation is minimal. - Highlights: • Automated unit for in-situ extraction of 137 Cs and 134 Cs from 1000 L of seawater. • Unit is robust, and easily transported and operated. • Cs extraction uses cartridges coated with potassium copper hexacyanoferrate. • Validated for selectivity, trueness, precision, linearity, LOD and traceability. • System fit for purpose for monitoring of Australian coastal and ocean waters.

Bottom loaded filter for radioactive liquid

International Nuclear Information System (INIS)

Wendland, W.G.

1980-01-01

A specification is given for a bottom loaded filter assembly for filtering radioactive liquids through a replaceable cartridge filter, which includes a lead-filled jacket enveloping a housing having a chamber therein for the filter cartridge. A track arrangement carries a hatch for sealing the chamber. A spacer plug supports the cartridge within guide means associated with the inlet conduit in the chamber. The plug and cartridge drop out of the chamber when the hatch is unbolted and moved laterally of the chamber along the track. During cartridge replacement a new plug and cartridge are supported in the guide means by a spacer bar inserted across the track means under the chamber. The hatch is then slid under the chamber and bolted to a flange on the housing, engaging an O-ring to seal the chamber. (author)

Rapid purification of radiodinated glucagon with Sep-PakR reversed phase cartridges

International Nuclear Information System (INIS)

Borghi, V.C.; Nascimento, M.; Wajchenberg, B.L.

1989-01-01

A simple, rapid method is described for the purification of radioiodinated glucagon for use in radioimmunoassay. Samples of the radioiodinated hormone, before and after purification are analysed on polyacrylamide gel electrophoresis. The 125 I incorporation in these samples is also checked through thrichloroacetic acid precipitation. The usefulness of this labeled glucagon in radioimmunoassay is demonstrated by its biding to specific antibodies. (M.A.C.) [pt

Determination of Human-Health Pharmaceuticals in Filtered Water by Chemically Modified Styrene-Divinylbenzene Resin-Based Solid-Phase Extraction and High-Performance Liquid Chromatography/Mass Spectrometry

Science.gov (United States)

Furlong, Edward T.; Werner, Stephen L.; Anderson, Bruce D.; Cahill, Jeffery D.

2008-01-01

In 1999, the Methods Research and Development Program of the U.S. Geological Survey National Water Quality Laboratory began the process of developing a method designed to identify and quantify human-health pharmaceuticals in four filtered water-sample types: reagent water, ground water, surface water minimally affected by human contributions, and surface water that contains a substantial fraction of treated wastewater. Compounds derived from human pharmaceutical and personal-care product use, which enter the environment through wastewater discharge, are a newly emerging area of concern; this method was intended to fulfill the need for a highly sensitive and highly selective means to identify and quantify 14 commonly used human pharmaceuticals in filtered-water samples. The concentrations of 12 pharmaceuticals are reported without qualification; the concentrations of two pharmaceuticals are reported as estimates because long-term reagent-spike sample recoveries fall below acceptance criteria for reporting concentrations without qualification. The method uses a chemically modified styrene-divinylbenzene resin-based solid-phase extraction (SPE) cartridge for analyte isolation and concentration. For analyte detection and quantitation, an instrumental method was developed that used a high-performance liquid chromatography/mass spectrometry (HPLC/MS) system to separate the pharmaceuticals of interest from each other and coextracted material. Immediately following separation, the pharmaceuticals are ionized by electrospray ionization operated in the positive mode, and the positive ions produced are detected, identified, and quantified using a quadrupole mass spectrometer. In this method, 1-liter water samples are first filtered, either in the field or in the laboratory, using a 0.7-micrometer (um) nominal pore size glass-fiber filter to remove suspended solids. The filtered samples then are passed through cleaned and conditioned SPE cartridges at a rate of about 15

Adjustments Recommended in Fiscal Year 1982 Ammunition Procurement and Modernization Programs

Science.gov (United States)

1981-06-30

No comment 4.8 No comment Cartridge, 7.6 2-mm., all types Cartridge, .45 caliber ball 31.9 58.3 -0.8 2.9 Cartridge, 1.6 30-mm., TP...4.5 - 1.6 57.5 Inventory exceeds re- quirements for rifle grenade cartridge 2.8 No comment 77.1 No comment - Inventory exceeds re...quirements 10.7 Inventory exceeds re- quirements Premature buy Premature buy 4.5 No comment 38 APPENDIX I APPENDIX

A novel sample preparation procedure for effect-directed analysis of micro-contaminants of emerging concern in surface waters.

Science.gov (United States)

Osorio, Victoria; Schriks, Merijn; Vughs, Dennis; de Voogt, Pim; Kolkman, Annemieke

2018-08-15

A novel sample preparation procedure relying on Solid Phase Extraction (SPE) combining different sorbent materials on a sequential-based cartridge was optimized and validated for the enrichment of 117 widely diverse contaminants of emerging concern (CECs) from surface waters (SW) and further combined chemical and biological analysis on subsequent extracts. A liquid chromatography coupled to high resolution tandem mass spectrometry LC-(HR)MS/MS protocol was optimized and validated for the quantitative analysis of organic CECs in SW extracts. A battery of in vitro CALUX bioassays for the assessment of endocrine, metabolic and genotoxic interference and oxidative stress were performed on the same SW extracts. Satisfactory recoveries ([70-130]%) and precision ( 0.99) over three orders of magnitude. Instrumental limits of detection and method limits of quantification were of [1-96] pg injected and [0.1-58] ng/L, respectively; while corresponding intra-day and inter-day precision did not exceed 11% and 20%. The developed procedure was successfully applied for the combined chemical and toxicological assessment of SW intended for drinking water supply. Levels of compounds varied from < 10 ng/L to < 500 ng/L. Endocrine (i.e. estrogenic and anti-androgenic) and metabolic interference responses were observed. Given the demonstrated reliability of the validated sample preparation method, the authors propose its integration in an effect-directed analysis procedure for a proper evaluation of SW quality and hazard assessment of CECs. Copyright © 2018 Elsevier B.V. All rights reserved.

A liquid chromatography-tandem mass spectrometry method for simultaneous analysis of acrylamide and the precursors, asparagine and reducing sugars in bread

DEFF Research Database (Denmark)

Nielsen, N.J.; Granby, Kit; Hedegaard, Rikke Susanne Vingborg

2006-01-01

A LC-MS-MS method for simultaneous determination of acrylamide, asparagine, fructose, glucose and sucrose in bread was developed. The method is based on aqueous extraction by blending. After centrifugation the samples were cleaned up by solid phase extraction on C18 cartridges conditioned with 2 ...

Volatile organic compound measurements in the California/Mexico border region during SCOS97

International Nuclear Information System (INIS)

Zielinska, B.; Sagebiel, J.; Harshfield, G.; Pasek, R.

2001-01-01

Measurements of volatile organic compounds (VOC) were carried out in the California/Mexico border region during the Southern California Ozone Study in the summer of 1997 (SCOS97). Integrated 3-h samples were collected in Rosarito (south of Tijuana, Mexico) and in Mexicali during intensive operational periods (IOP), twice per IOP day. VOC were collected using stainless-steel 6-l canisters; carbonyl compounds were collected using 2,4-dinitrophenylhydrazine (DNPH) impregnated C18 SepPak cartridges. The canister samples were analyzed for speciated volatile hydrocarbons (C 2 -C 12 ), CO, CO 2 , CH 4 , methyl t-butyl ether (MTBE), and halogenated hydrocarbons. DNPH-impregnated cartridges were analyzed for 14 C 1 -C 7 carbonyl compounds. The concentrations of all species were higher at Mexicali than in Rosarito. A good correlation between total non-methane hydrocarbons (TNMHC), CO, and other pollutants associated with motor vehicle emissions observed for Mexicali indicates that the main source of TNMHC at this site is vehicular traffic

Absolute 22Na radioactivity measurement by gamma efficiency variation of 4πβ-γ coincidence method

International Nuclear Information System (INIS)

Hino, Yoshio; Kawada, Yasusi.

1994-01-01

The absolute radioactivity of 22 Na was obtained by gamma efficiency variation of 4πβ-γ coincidence method. Some other previous techniques, such as sum peak gate method based on the positron emission rate, relative measurement with calibrated ionization chambers, and gamma spectrometry with a HPGe detector, were also tried to ensure the present result. The results of these methods were in reasonable agreement with the present absolute measurement. The assayed source solution of this experiment was transferred to NBS type ampoules, and sealed ampoules were sent to the SIR (International Reference System) in BIPM, Taiwan and Indonesia for the international comparison. (author)

Feasibility and Environmental Implications of Using Waste Motor Oil as Alternative Supplemental Fuel in Contingency Prime Power Generation

Science.gov (United States)

2017-03-23

50 x Figure 19 - Baldwin Fuel/ Water Separator and Replacement Cartridge Filters ............... 51 Figure 20 - Waste Drained from...15ppm for ULSDa 20,000ppm Catalyst equipped engines will be damaged Sodium Content 0.5ppm maximum 10ppm Water & Sediment Not to exceed 0.05...for further sample collection parameters and number of samples collected for each type. To prevent contamination from sediment , water , or antifreeze

76 FR 70422 - Procurement List Additions

Science.gov (United States)

2011-11-14

..., Disinfectant Cleaner-Degreaser Cartridge Concentrate. NSN: 7930-00-NIB-0593--Refills, Multi-Purpose Cleaner, Cartridge Concentrate. NSN: 7930-00-NIB-0594--Starter Kit, Multi-Purpose Cleaner, Cartridge Concentrate. NPA..., Anniston, AL Service Type/Locations: Rubbish Removal and Recycling Service Department of the Treasury...

Incidence of missed inferior alveolar nerve blocks in vital asymptomatic subjects and in patients with symptomatic irreversible pulpitis.

Science.gov (United States)

Fowler, Sara; Reader, Al; Beck, Mike

2015-05-01

The purpose of this retrospective study was to determine the incidence of missed inferior alveolar nerve (IAN) blocks by using a 1- or 2-cartridge volume of 2% lidocaine with 1:100,000 epinephrine in vital asymptomatic teeth and in emergency patients with symptomatic irreversible pulpitis. As part of 37 studies, 3169 subjects/patients were evaluated for missed IAN blocks. The study included 2450 asymptomatic subjects and 719 emergency patients presenting with symptomatic irreversible pulpitis. Each subject or patient received either a 1- or 2-cartridge volume of 2% lidocaine with 1:100,000 epinephrine. A missed block was defined as no lip numbness at 15-20 minutes after the IAN block. The effect of anesthetic volume on the incidence of missed blocks was assessed by using mixed models logistic regression with individual studies as a random effect. The incidence of missed blocks for asymptomatic subjects was 6.3% for the 1-cartridge volume and 3.8% for the 2-cartridge volume. For patients presenting with irreversible pulpitis, the incidence of missed blocks was 7.7% for the 1-cartridge volume and 2.3% for the 2-cartridge volume. In both asymptomatic subjects and patients with irreversible pulpitis, the 2-cartridge volume was significantly (P = .0395) better than the 1-cartridge volume. There were no significant effects for pulpal diagnosis (P = .7523) or the pulpal diagnosis and anesthetic volume interaction (P = .3973). Concerning missed IAN blocks, we concluded that administration of a 2-cartridge volume was significantly better (P = .0395) than a 1-cartridge volume in both asymptomatic subjects and emergency patients presenting with irreversible pulpitis. Copyright © 2015 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.

Development of procedures for calculating stiffness and damping properties of elastomers in engineering applications. Part 4: Testing of elastomers under a rotating load. [resonance testing

Science.gov (United States)

Darlow, M. S.; Smalley, A. J.

1977-01-01

A test rig designed to measure stiffness and damping of elastomer cartridges under a rotating load excitation is described. The test rig employs rotating unbalance in a rotor which runs to 60,000 RPM as the excitation mechanism. A variable resonant mass is supported on elastomer elements and the dynamic characteristics are determined from measurements of input and output acceleration. Five different cartridges are considered: three of these are buttons cartridges having buttons located in pairs, with 120 between each pair. Two of the cartridges consist of 360 elastomer rings with rectangular cross-sections. Dynamic stiffness and damping are measured for each cartridge and compared with predictions at different frequencies and different strains.

NEW METHOD FOR DETERMINATION OF ACTINIDES AND STRONTIUM IN ANIMAL TISSUE

Energy Technology Data Exchange (ETDEWEB)

Maxwell, S; Jay Hutchison, J; Don Faison, D

2007-05-07

The analysis of actinides in animal tissue samples is very important for environmental monitoring. There is a need to measure actinide isotopes with very low detection limits in animal tissue samples, including fish, deer, hogs, beef and shellfish. A new, rapid actinide separation method has been developed and implemented that allows the measurement of plutonium, neptunium, uranium, americium, curium and strontium isotopes in large animal tissue samples (100-200 g) with high chemical recoveries and effective removal of matrix interferences. This method uses stacked TEVA Resin{reg_sign}, TRU Resin{reg_sign} and DGA-Resin{reg_sign} cartridges from Eichrom Technologies (Darien, IL, USA) that allows the rapid separation of plutonium (Pu), neptunium (Np), uranium (U), americium (Am), and curium (Cm) using a single multi-stage column combined with alpha spectrometry. Sr-90 is collected on Sr Resin{reg_sign} from Eichrom Technologies (Darien, IL, USA). After acid digestion and furnace heating of the animal tissue samples, the actinides and Sr-89/90 are separated using column extraction chromatography. This method has been shown to be effective over a wide range of animal tissue matrices. By using vacuum box cartridge technology with rapid flow rates, sample preparation time is minimized.

Monitoring of trace-levels of herbicides in the Cachoeira River in Bahia State, Brazil, by neutron activation analysis

International Nuclear Information System (INIS)

Severo, Maria Isabel; Oliveira, Eduardo; Caribe, Ana Cristina; Revel, Gilles; Oliveira, Arno Heeren

1995-01-01

A systematic study was undertaken in order to find out which of the most relevant elements can be determined in water normal conditions by non-destructive neutron activation and a suitable mono standard method. Standardized water from Cachoeira river and croustaceous samples were brought to dryness by freeze-drying and irradiated in quartz at a neutron flux of 10 14 cm -2 s -1 . Trace element contents in quartz ampoules from different origins were determined separately. The following elements were preliminarily identified: Cr, Co, Cu, Br, Sb, Cs, Ce, Nb, Au, Pa, Zn, La, Sm. (author). 10 refs., 2 tabs

Comparison of solid phase extraction, saponification and gel permeation chromatography for the clean-up of microwave-assisted biological extracts in the analysis of polycyclic aromatic hydrocarbons.

Science.gov (United States)

Navarro, P; Cortazar, E; Bartolomé, L; Deusto, M; Raposo, J C; Zuloaga, O; Arana, G; Etxebarria, N

2006-09-22

The feasibility of different clean-up procedures was studied for the determination of polycyclic aromatic hydrocarbons (PAHs) in biota samples such as oysters, mussels and fish liver. In this sense, once the samples were extracted--essentially with acetone and in a microwave system--and before they could be analysed by gas chromatography-mass spectrometry (GC-MS), three different approaches were studied for the clean-up step: solid phase extraction (SPE), microwave-assisted saponification (MAS) and gel permeation chromatography (GPC). The main aim of this work was to maximise the recoveries of PAHs and to minimise the presence of interfering compounds in the last extract. In the case of SPE, Florisil cartridges of 1, 2 and 5 g, and silica cartridges of 5 g were studied. In that case, and with oysters and mussels, microwave-assisted extraction and 5 g Florisil cartridges provided good results. In addition, the concentrations obtained for Standard Reference Material (SRM) NIST 2977 (mussel tissue) were in good agreement with the certified values. In the case of microwave-assisted saponification, the extracts were not as clean as those obtained with 5 g Florisil and this fact lead to overestimate the concentration of the heaviest PAHs. Finally, the cleanest extracts were obtained by GPC. The method was successfully applied to mussels, oysters and hake liver, and the results obtained for NIST 2977 (mussel tissue) were within the confidence interval of the certified reference material for most of the certified analytes.

Raman spectroscopy and capillary electrophoresis applied to forensic colour inkjet printer inks analysis.

Science.gov (United States)

Król, Małgorzata; Karoly, Agnes; Kościelniak, Paweł

2014-09-01

Forensic laboratories are increasingly engaged in the examination of fraudulent documents, and what is important, in many cases these are inkjet-printed documents. That is why systematic approaches to inkjet printer inks comparison and identification have been carried out by both non-destructive and destructive methods. In this study, micro-Raman spectroscopy and capillary electrophoresis (CE) were applied to the analysis of colour inkjet printer inks. Micro-Raman spectroscopy was used to study the chemical composition of colour inks in situ on a paper surface. It helps to characterize and differentiate inkjet inks, and can be used to create a spectra database of inks taken from different cartridge brands and cartridge numbers. Capillary electrophoresis in micellar electrophoretic capillary chromatography mode was applied to separate colour and colourless components of inks, enabling group identification of those components which occur in a sufficient concentration (giving intensive peaks). Finally, on the basis of the obtained results, differentiation of the analysed inks was performed. Twenty-three samples of inkjet printer inks were examined and the discriminating power (DP) values for both presented methods were established in the routine work of experts during the result interpretation step. DP was found to be 94.0% (Raman) and 95.6% (CE) when all the analysed ink samples were taken into account, and it was 96.7% (Raman) and 98.4% (CE), when only cartridges with different index numbers were considered. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Determination of Wastewater Compounds in Sediment and Soil by Pressurized Solvent Extraction, Solid-Phase Extraction, and Capillary-Column Gas Chromatography/Mass Spectrometry

Science.gov (United States)

Burkhardt, Mark R.; Zaugg, Steven D.; Smith, Steven G.; ReVello, Rhiannon C.

2006-01-01

A method for the determination of 61 compounds in environmental sediment and soil samples is described. The method was developed in response to increasing concern over the effects of endocrine-disrupting chemicals in wastewater and wastewater-impacted sediment on aquatic organisms. This method also may be used to evaluate the effects of combined sanitary and storm-sewer overflow on the water and sediment quality of urban streams. Method development focused on the determination of compounds that were chosen on the basis of their endocrine-disrupting potential or toxicity. These compounds include the alkylphenol ethoxylate nonionic surfactants and their degradates, food additives, fragrances, antioxidants, flame retardants, plasticizers, industrial solvents, disinfectants, fecal sterols, polycyclic aromatic hydrocarbons, and high-use domestic pesticides. Sediment and soil samples are extracted using a pressurized solvent extraction system. The compounds of interest are extracted from interfering matrix components by high-pressure water/isopropyl alcohol extraction. The compounds were isolated using disposable solid-phase extraction (SPE) cartridges containing chemically modified polystyrene-divinylbenzene resin. The cartridges were dried with nitrogen gas, and then sorbed compounds were eluted with methylene chloride (80 percent)-diethyl ether (20 percent) through Florisil/sodium sulfate SPE cartridge, and then determined by capillary-column gas chromatography/mass spectrometry. Recoveries in reagent-sand samples fortified at 4 to 72 micrograms averaged 76 percent ?13 percent relative standard deviation for all method compounds. Initial method reporting levels for single-component compounds ranged from 50 to 500 micrograms per kilogram. The concentrations of 20 out of 61 compounds initially will be reported as estimated with the 'E' remark code for one of three reasons: (1) unacceptably low-biased recovery (less than 60 percent) or highly variable method performance

Comparison between Different Extraction Methods for Determination of Primary Aromatic Amines in Food Simulant

Directory of Open Access Journals (Sweden)

Morteza Shahrestani

2018-01-01

Full Text Available The primary aromatic amines (PAAs are food contaminants which may exist in packaged food. Polyurethane (PU adhesives which are used in flexible packaging are the main source of PAAs. It is the unreacted diisocyanates which in fact migrate to foodstuff and then hydrolyze to PAAs. These PAAs include toluenediamines (TDAs and methylenedianilines (MDAs, and the selected PAAs were 2,4-TDA, 2,6-TDA, 4,4′-MDA, 2,4′-MDA, and 2,2′-MDA. PAAs have genotoxic, carcinogenic, and allergenic effects. In this study, extraction methods were applied on a 3% acetic acid as food simulant which was spiked with the PAAs under study. Extraction methods were liquid-liquid extraction (LLE, dispersive liquid-liquid microextraction (DLLME, and solid-phase extraction (SPE with C18 ec (octadecyl, HR-P (styrene/divinylbenzene, and SCX (strong cationic exchange cartridges. Extracted samples were detected and analyzed by HPLC-UV. In comparison between methods, recovery rate of SCX cartridge showed the best adsorption, up to 91% for polar PAAs (TDAs and MDAs. The interested PAAs are polar and relatively soluble in water, so a cartridge with cationic exchange properties has the best absorption and consequently the best recoveries.

Preparation and certification of a reference uranium

International Nuclear Information System (INIS)

Anon.

1979-06-01

The CEA Analysis Coordination has produced a reference uranium metal of guaranteed minimum uranium content. The metal was purified by electro-refining in fused salt baths and the dendrites obtained were cast in the form of an ingot by electron bombardment. The ingot was rolled and cut into pieces of mass between 0.5 g and 1.5 g, and each piece conditioned in a glass ampoule under primary vacuum. The total number of reference samples is about 4500. The uranium content was inferred from the impurity concentration determined by spark mass spectrometry and atomic or molecular adsorption spectrophotometry and from the gas concentration determined by specific methods. A certificate of guarantee gives instructions for the use of these reference samples [fr

Low-temperature synthesis of the infinite-layer compound LaNiO2 by soft-chemical techniques

International Nuclear Information System (INIS)

Takamatsu, Tomohisa; Kato, Masatsune; Noji, Takashi; Koike, Yoji

2010-01-01

Bulk samples of LaNiO 2 with the so-called infinite-layer structure have successfully been synthesized. First, polycrystalline samples of LaNiO 3 with the perovskite structure were prepared using molten KOH at a temperature of 400-450degC. Then, they were finely ground with a double stoichiometric excess of reductant CaH 2 and sealed in an evacuated Pyrex tube. The sealed ampoule was then heated at 300degC for 24 h. Powder X-ray diffraction analysis has revealed that the product obtained after removing the residual CaH 2 and the byproduct CaO is of almost single phase with tetragonal symmetry, indicating the formation of the infinite-layer compound LaNiO 2 . (author)

Online drug information platform for the public in Hong Kong-Review of local drug information use and needs.

Science.gov (United States)

Cheng, F W T; So, S W K; Fung, B W T; Hung, W H; Lee, V W Y

2018-06-01

In view of the popularity of Internet usage in Hong Kong, an interactive web-based drug information platform entitled "Ask My Pharmacist - Online University Led drug Enquiry Platform" (AMPOULE) was launched in 2009 to better serve the needs of drug information in Hong Kong. This paper aimed to evaluate the utility of AMPOULE in improving drug-related knowledge among the public and to reassess the needs of the general public in Hong Kong. All enquiries sent via AMPOULE were reviewed. Demographic data, nature of questions and types of drug class covered were analyzed. The workload of pharmacists was examined with respect to the preparation time needed for the enquiry, the lag days to reply and also the timing of enquiry recipient. 2122 enquiries were received from 2009 to 2017. Most enquirers were from Hong Kong (56.6%) and female gender (49.2%). 13% of the concerned subjects were aged over 61-year-old. The most frequent types of questions and medications covered were "Drug Ingredients and Indications" (28.0%) and Adverse Drug Reactions (26.8%) and "Cardiovascular Medication" (21.9%) respectively but these varied in different age groups or enquirer groups. The median time for preparation was 40.0 min (IQR: 25-65 min) while the median time lag was found to be 2.5 days (IQR: 1.0-5.0 days). The number of enquiries received was evenly distributed throughout the day except during 1:00 am to 9:00 am and 7:00 pm to 8:00 pm. AMPOULE has demonstrated that an online platform providing patient-oriented drug information service through the Internet is promising and further promotion is warranted. Current data suggested that the need of different age groups and enquirer groups are different and should therefore be individualized. Copyright © 2018 Elsevier B.V. All rights reserved.

Time dependent phase associations of iron and other trace elements elucidated by 234Th/238U inventories in tropical coastal waters

International Nuclear Information System (INIS)

Szymczak, R.; Zaw, M.

1999-01-01

In this study samples were collected in the Gulf of Papua region of PNG, on board the research vessel Franklin as apart of a multidisciplinary study of factors influencing the fate of terrestrial material entering the tropical coastal ocean. Samples for 234 Th were collected using a in situ large volume pump device (Challenger Oceanic) passing seawater (1000-2000 litres) through a series of cartridge filters in polycarbonate housings

Innovative Technology Development for Comprehensive Air Quality Characterization from Open Burning

Science.gov (United States)

2012-04-01

data acquisition computer with a Roots meter . Following sampling, the glass cartridge (sorbent) was removed from the Flyer, wrapped in clean aluminum...Determination Of Hydrogen Halide And Halogen Emissions From Stationary Sources Non- Isokinetic Method. U.S. EPA Method 3A, Carbon Monoxide. U.S...flowrate and concentration. HCl gas will be metered via a mass flow controller and will target concentrations seen in the field during sampling (ca. 20

Development of Micellar HPLC-UV Method for Determination of Pharmaceuticals in Water Samples

Directory of Open Access Journals (Sweden)

Danielle Cristina da Silva

2018-01-01

Full Text Available Method for extraction and determination of amoxicillin, caffeine, ciprofloxacin, norfloxacin, tetracycline, diclofenac, ibuprofen, nimesulide, levonorgestrel, and 17α-ethynylestradiol exploiting micellar liquid chromatography with PDA detector and solid-phase extraction was proposed. The usage of toxic solvents was low; the chromatographic separation of the medicaments was performed using a C18 column and mobile phases A and B containing 15.0% (v/v ethanol, 3.0% (m/v sodium dodecyl sulfate (SDS, and 0.02 mol·L−1 phosphate at pHs 7.0 and 8.0, respectively. The method is simple, selective, and fast, and the analytes were separated in 23.0 min. For extraction, 1000 mL of sample containing 2.0% (v/v ethanol and 0.002 mol·L−1 citric acid at pH 2.50 was loaded through a 1000 mg of C18 cartridge. The analytes were eluted using 3.0 mL of ethanol, which were evaporated and redissolved in 0.5 mL of mobile phase. Concentration factors better than 1200, except amoxicillin (224, were obtained. The analytical curves were linear (R2 better than 0.992; LOD and LOQ n=10 presented values in the range of 0.019–0.247 and 0.058–0.752 mg·L−1, respectively. Recoveries of 99% were obtained, and the results are in agreement with those obtained by the comparative methods.

Studies on the production of technetium-99m generators based on gel elution

International Nuclear Information System (INIS)

Castro, M.

1993-12-01

Technetium-99m generator based on Ti Mo elution has been carried out. The gel matrix was prepared by mixing non-irradiated molybdate with Titanium Chloride solution. Conditions of preparing and drying Ti Mo were evaluated as a function of elution yield. Thus, pH and water content were found highly critical for reproductiveness of the results. Non-elutable form of Tc-99m can be oxidized treating the target after irradiation with K 2 Cr 2 O 7 0.001M solution. During several experiments the columns were soaked with this oxidizing solution for one hour and afterwards the Ti Mo was washed with 150 ml physiological saline. Daily elutions were done with 10 ml of NaCl 0.9%. Cooling water reactor during irradiation quartz ampoules has been studied. To study this effect, one group of samples were irradiated in aluminium caps air-tight screw and another one was irradiated in drilled caps with six holes to permit water reactor recirculation around quartz ampoules. By combination K 2 Cr 2 O 7 target treatment and cooling Ti Mo during irradiation is possible to get yields of Tc-99m near to 76%. The radiochemical purity was > 99% and Al content < 10ppm , Cr < 0.05ppm , Mo <20ppm, Ti was no detected. Biological scans practiced in animals have been considered satisfactory. (author). 8 refs., 7 tabs., 3 figs

USGS48 Puerto Rico precipitation - A new isotopic reference material for δ2H and δ18O measurements of water

Science.gov (United States)

Qi, Haiping; Coplen, Tyler B.; Tarbox, Lauren V.; Lorenz, Jennifer M.; Scholl, Martha A.

2014-01-01

A new secondary isotopic reference material has been prepared from Puerto Rico precipitation, which was filtered, homogenised, loaded into glass ampoules, sealed with a torch, autoclaved to eliminate biological activity, and calibrated by dual-inlet isotope-ratio mass spectrometry. This isotopic reference material, designated as USGS48, is intended to be one of two isotopic reference waters for daily normalisation of stable hydrogen (δ2H) and stable oxygen (δ18O) isotopic analysis of water with a mass spectrometer or a laser absorption spectrometer. The δ2H and δ18O values of this reference water are−2.0±0.4 and−2.224±0.012 ‰, respectively, relative to Vienna Standard Mean Ocean Water on scales normalised such that the δ2H and δ18O values of Standard Light Antarctic Precipitation reference water are−428 and−55.5 ‰, respectively. Each uncertainty is an estimated expanded uncertainty (U=2uc) about the reference value that provides an interval that has about a 95 % probability of encompassing the true value. This isotopic reference water is available by the case of 144 glass ampoules containing 5 mL of water in each ampoule.

Development and validation of a solid-phase extraction method coupled to liquid chromatography with fluorescence detection for the determination of fluoroquinolone residues in powdered infant formulae. Application to the analysis of samples from the Spanish and Latin American market.

Science.gov (United States)

Rodriguez, E; Moreno-Bondi, M C; Marazuela, M D

2008-10-31

This paper describes a new method for the effective extraction, clean-up and chromatographic analysis of residues of four fluoroquinolones (ciprofloxacin, enrofloxacin, danofloxacin and sarafloxacin) in powdered infant formulae and follow-on preparations. Samples were reconstituted following the manufacturer's recommendations and treated with trichloroacetic acid in methanol 10% (w/v) for deproteinization. Two solid-phase extraction cartridges have been evaluated for sample clean-up and preconcentration, Strata Screen A and Strata X and the later provided the best recoveries for all the analytes tested. Chromatographic analysis has been carried out using a polar endcapped column (AQUA C(18)) and fluorescence detection, with lomefloxacin (LOME) as internal standard. Method validation has been performed according to European Commission Decision 2002/657/EC criteria, in terms of linearity, recovery, precision, specificity, decision limit (CC(alpha)) and detection capability (CC(beta)). Typical recoveries ranged between 70 and 110% at levels below and above the maximum residue limits of the target analytes in bovine milk, with an excellent intralab reproducibility (RSDsmarket, using LC-MS/MS as confirmatory technique.

Micro versus macro solid phase extraction for monitoring water contaminants: a preliminary study using trihalomethanes.

Science.gov (United States)

Alexandrou, Lydon D; Spencer, Michelle J S; Morrison, Paul D; Meehan, Barry J; Jones, Oliver A H

2015-04-15

Solid phase extraction is one of the most commonly used pre-concentration and cleanup steps in environmental science. However, traditional methods need electrically powered pumps, can use large volumes of solvent (if multiple samples are run), and require several hours to filter a sample. Additionally, if the cartridge is open to the air volatile compounds may be lost and sample integrity compromised. In contrast, micro cartridge based solid phase extraction can be completed in less than 2 min by hand, uses only microlitres of solvent and provides comparable concentration factors to established methods. It is also an enclosed system so volatile components are not lost. The sample can also be eluted directly into a detector (e.g. a mass spectrometer) if required. However, the technology is new and has not been much used for environmental analysis. In this study we compare traditional (macro) and the new micro solid phase extraction for the analysis of four common volatile trihalomethanes (trichloromethane, bromodichloromethane, dibromochloromethane and tribromomethane). The results demonstrate that micro solid phase extraction is faster and cheaper than traditional methods with similar recovery rates for the target compounds. This method shows potential for further development in a range of applications. Copyright © 2015 Elsevier B.V. All rights reserved.

Cleanup strategies and advantages in the determination of several therapeutic classes of pharmaceuticals in wastewater samples by SPE-LC-MS/MS.

Science.gov (United States)

Sousa, M A; Gonçalves, C; Cunha, E; Hajšlová, J; Alpendurada, M F

2011-01-01

This work describes the development and validation of an offline solid-phase extraction with simultaneous cleanup capability, followed by liquid chromatography-(electrospray ionisation)-ion trap mass spectrometry, enabling the concurrent determination of 23 pharmaceuticals of diverse chemical nature, among the most consumed in Portugal, in wastewater samples. Several cleanup strategies, exploiting the physical and chemical properties of the analytes vs. interferences, alongside with the use of internal standards, were assayed in order to minimise the influence of matrix components in the ionisation efficiency of target analytes. After testing all combinations of adsorbents (normal-phase, ion exchange and mixed composition) and elution solvents, the best results were achieved with the mixed-anion exchange Oasis MAX cartridges. They provided recovery rates generally higher than 60%. The precision of the method ranged from 2% to 18% and 4% to 19% (except for diclofenac (22%) and simvastatin (26%)) for intra- and inter-day analysis, respectively. Method detection limits varied between 1 and 20 ng L(-1), while method quantification limits were diclofenac and bezafibrate were detected in concentrations ranging from 1 to 20 μg L(-1), while gemfibrozil, simvastatin, ketoprofen, azithromycin, bisoprolol, lorazepam and paroxetine were quantified in levels below 1 μg L(-1). These WWTPs were given particular attention since they discharge their effluents into the Douro river, where water is extracted for the production of drinking water. Some sampling spots in this river were also analysed.

Photo-induced fluorescence of magnesium derivatives of tetracycline antibiotics in wastewater samples

International Nuclear Information System (INIS)

Pena, A.; Albert-Garcia, J.R.; Silva, L.J.G.; Lino, C.M.; Calatayud, J. Martinez

2010-01-01

An analytical strategy, for the determination of tetracyclines (TCs), based on a HPLC system coupled with a photo-reactor followed by post-column derivatization was developed. Higher fluorescence emission after coupling the resulting photo-fragments with magnesium ions was observed for the determination of minocycline (MC), epitetracycline (ETC), tetracycline (TC) and doxycycline (DC). The manifold included a HPLC system with a photo-reactor (PTFE tubing helically coiled around a low-pressure mercury lamp), a mixing T-piece and a fluorescence detector. The derivatization reagent was delivered at 0.5 mL min -1 by a pump. After HPLC separation using a gradient system with a mobile phase containing oxalic acid 0.02 M and acetonitrile, TCs were irradiated for 60 s, and the resulting photo-fragments were mixed with the post-column derivatization reagent, and the magnesium derivatives of TCs were detected by fluorimetry (λ exc 386 nm, λ em 500 nm). The results obtained showed a significant increase of sensitivity due to photodegration of TCs, 45.4%, 37.6% and 25.3% for MC, TC and ETC respectively. For DC an increase of only 1.5% was observed. The developed method was successfully applied to TCs determination in hospital and municipal wastewater samples using solid phase extraction with Oasis HLB cartridges. The LOQs were 0.25, 0.15, 01 and 0.25 μg L -1 for TC, ETC, MC and DC, respectively. The recovery values oscillated between 107.1% and 92.4% for fortification of 2.5 μg L -1 of each antibiotic.

Photo-induced fluorescence of magnesium derivatives of tetracycline antibiotics in wastewater samples

Energy Technology Data Exchange (ETDEWEB)

Pena, A., E-mail: apena@ff.uc.pt [Group of Health Surveillance, Center of Pharmaceutical Studies, Faculty of Pharmacy, University of Coimbra (Portugal); Albert-Garcia, J.R. [Department of Analytical Chemistry, Faculty of Chemistry, University of Valencia (Portugal); Silva, L.J.G.; Lino, C.M. [Group of Health Surveillance, Center of Pharmaceutical Studies, Faculty of Pharmacy, University of Coimbra (Portugal); Calatayud, J. Martinez [Department of Analytical Chemistry, Faculty of Chemistry, University of Valencia (Portugal)

2010-07-15

An analytical strategy, for the determination of tetracyclines (TCs), based on a HPLC system coupled with a photo-reactor followed by post-column derivatization was developed. Higher fluorescence emission after coupling the resulting photo-fragments with magnesium ions was observed for the determination of minocycline (MC), epitetracycline (ETC), tetracycline (TC) and doxycycline (DC). The manifold included a HPLC system with a photo-reactor (PTFE tubing helically coiled around a low-pressure mercury lamp), a mixing T-piece and a fluorescence detector. The derivatization reagent was delivered at 0.5 mL min{sup -1} by a pump. After HPLC separation using a gradient system with a mobile phase containing oxalic acid 0.02 M and acetonitrile, TCs were irradiated for 60 s, and the resulting photo-fragments were mixed with the post-column derivatization reagent, and the magnesium derivatives of TCs were detected by fluorimetry ({lambda}{sub exc} 386 nm, {lambda}{sub em} 500 nm). The results obtained showed a significant increase of sensitivity due to photodegration of TCs, 45.4%, 37.6% and 25.3% for MC, TC and ETC respectively. For DC an increase of only 1.5% was observed. The developed method was successfully applied to TCs determination in hospital and municipal wastewater samples using solid phase extraction with Oasis HLB cartridges. The LOQs were 0.25, 0.15, 01 and 0.25 {mu}g L{sup -1} for TC, ETC, MC and DC, respectively. The recovery values oscillated between 107.1% and 92.4% for fortification of 2.5 {mu}g L{sup -1} of each antibiotic.

Directional solidification of Al2-Cu-Al and Al3-Ni-Al eutectics during TEXUS rocket flight

Science.gov (United States)

Favier, J. J.; Degoer, J.

1984-01-01

One lamellar eutectic sample and one fiber-like eutectic sample were solidified directionally during the TEXUS-6 rocket flight. The microstructures and the results of the thermal analysis, obtained from the temperatures recorded on the cartridge skin, are compared. No appreciable modifications of the regularity of the eutectic structures were observed by passing from 1 g to 0.0001 g in these experiments. No steady state growth conditions were achieved in these experiments.

HPLC-DAD determination of imidacloprid in onion

OpenAIRE

Mandić Aljoša; Lazić Sanja; Inđić Dušanka

2003-01-01

Imidacloprid is an insecticide most commonly used on vegetables, potato sugar beet, fruit, cereal, maize and rice. Imidacloprid residue has been determined in spiked onion and in onion samples. Sample preparation consisted of dichlormethane extraction of imidacloprid from onion, followed by purification of the obtained extract on a LC-Florisil disposable cartridge. The HPLC-DAD method bas been developed on reversed-phase for separation of imidacloprid with a mixture of 0.01 M phosphate buffer...

An on-line coupling of nanofibrous extraction with column-switching high performance liquid chromatography - A case study on the determination of bisphenol A in environmental water samples.

Science.gov (United States)

Háková, Martina; Chocholoušová Havlíková, Lucie; Chvojka, Jiří; Solich, Petr; Šatínský, Dalibor

2018-02-01

Polyamide 6 nanofiber polymers were used as modern sorbents for on-line solid phase extraction (SPE) coupled with liquid chromatography. The on-line SPE system was tested for the determination of bisphenol A in river water samples. Polyamide nanofibers were prepared using needleless electrospinning, inserted into a mini-column cartridge (5 × 4.6mm) and coupled with HPLC. The effect of column packing and the amount of polyamide 6 on extraction efficiency was tested and the packing process was optimized. The proposed method was performed using a 50-µL sample injection followed by an on-line nanofibrous extraction procedure. The influence of the washing mobile phase on the retention of bisphenol A during the extraction procedure was evaluated. Ascentis ® Express C18 (10cm × 4.6mm) core-shell column was used as an analytical column. Fluorescence detection wavelengths (λ ex = 225nm and λ em = 320nm) were used for identification and quantification of Bisphenol A in river waters. The linearity was tested in the range from 2 to 500µgL -1 (using nine calibration points). The limits of detection and quantification were 0.6 and 2µgL -1 , respectively. The developed method was successfully used for the determination of bisphenol A in various samples of river waters in the Czech Republic (The Ohře, Labe, Nisa, Úpa, and Opava Rivers). Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of nanomolar chromate in drinking water with solid phase extraction and a portable spectrophotometer.

Science.gov (United States)

Ma, Jian; Yang, Bo; Byrne, Robert H

2012-06-15

Determination of chromate at low concentration levels in drinking water is an important analytical objective for both human health and environmental science. Here we report the use of solid phase extraction (SPE) in combination with a custom-made portable light-emitting diode (LED) spectrophotometer to achieve detection of chromate in the field at nanomolar levels. The measurement chemistry is based on a highly selective reaction between 1,5-diphenylcarbazide (DPC) and chromate under acidic conditions. The Cr-DPC complex formed in the reaction can be extracted on a commercial C18 SPE cartridge. Concentrated Cr-DPC is subsequently eluted with methanol and detected by spectrophotometry. Optimization of analytical conditions involved investigation of reagent compositions and concentrations, eluent type, flow rate (sample loading), sample volume, and stability of the SPE cartridge. Under optimized conditions, detection limits are on the order of 3 nM. Only 50 mL of sample is required for an analysis, and total analysis time is around 10 min. The targeted analytical range of 0-500 nM can be easily extended by changing the sample volume. Compared to previous SPE-based spectrophotometric methods, this analytical procedure offers the benefits of improved sensitivity, reduced sample consumption, shorter analysis time, greater operational convenience, and lower cost. Copyright © 2012 Elsevier B.V. All rights reserved.

Instrumental neutron activation analysis of hair for mercury determination in case of possible professional contamination. 1

International Nuclear Information System (INIS)

Dubinskaya, N.A.

1980-01-01

The results of neutron-activation determination of Hg in hair of the staff working with laboratory Hg-equipment are presented. The accuracy of the analysis has been tested including the possible Hg losses from phenol-formaldehyde resigns base standards in Al foils and from hair samples in polyethylene ampoules during their irradiation in water-filled nuclear reactor channel. The mean content of Hg in hair has been found to be 1.42+-0.42 (n=22) for the staff, and 1.05+-0.21 (n=10) μg for the controls. A staff group with a higher Hg content in hair (7.3+-3.0, n=10) has been singled out

Growth of methyl 2-(2,4-dinitrophenyl)aminopropanoate single crystals

Science.gov (United States)

Perigaud, A.; Nicolau, Y. F.

1986-12-01

Methyl 2-(2,4-dinitrophenyl)aminopropanoate single crystals, 1 cm in diameter and 7 cm in length have been grown by a travelling-heater-Bridgman method in polyethylene tubes introduced into glass ampoules, at a growth rate of 1.5-6 mm/day. The starting material was synthesised and purified by recrystallization from methanol and by vacuum evaporation to a purity of 99.994%. The period of growth, and hence the length of the crystal, is limited due to melt decomposition and polycondensation. The b-axis of the crystals is always oriented at about 72° to the ampoule axis. Good quality single crystals have been obtained giving a FWHM of the Cu Kα (040) rocking curve of about 1'.

Speciation analysis of tellurium by solid-phase extraction in the presence of ammonium pyrrolidine dithiocarbamate and inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Yu, Chunhai; Cai, Qiantao; Guo, Zhong-Xian; Yang, Zhaoguang [Centre for Advanced Water Technology, Innovation Centre (NTU), Singapore (Singapore); Khoo, Soo Beng [Department of Chemistry, National University of Singapore (Singapore)

2003-05-01

Under acidic conditions tellurium(IV) formed a complex with ammonium pyrrolidine dithiocarbamate (APDC). The tellurium(IV) complex was completely retained on a non-polar Isolute silica-based octadecyl (C{sub 18}) sorbent-containing solid-phase extraction (SPE) cartridge, while the uncomplexed Te(VI) passed through the cartridge and remained as a free species in the solution. Only partial Te(IV) was retained on the SPE cartridge for samples without addition of APDC. On the basis of different retention behaviours of the complexed Te(IV) and uncomplexed Te(VI), a simple and highly sensitive method is proposed for the determination of total tellurium and Te(VI) by SPE separation and inductively coupled plasma mass spectrometry (ICP-MS) detection. The Te(IV) concentration was calculated as the difference between total tellurium and Te(VI) concentrations. The detection limit (3{sigma}) is 3 ng L{sup -1} tellurium. Factors affecting the separation and detection of tellurium species were investigated. Coexisting ions did not show significant interferences with the Te(IV)-APDC complex retention and the subsequent ICP-MS detection of Te. The method has been successfully applied to the tellurium speciation analysis in waters with spiked recoveries for Te(IV) and Te(VI) of 86.0-108% and 87.1-97.4%, respectively. (orig.)

Sorptive capacities of lipids determined by passive dosing of non-polar organic chemicals

DEFF Research Database (Denmark)

Jahnke, Annika; Kierkegaard, Amelie; Bolinius, Damien

VMS), chlorobenzenes and polychlorinated biphenyls via a common headspace over an olive oil donor phase to transfer the same chemical activity into the samples; iii) sampling of EOM and olive oil controls at different time points; iv) purge-and-trap extraction of the model chemicals onto ENV+ SPE cartridges, elution...... and GC/MS analysis; v) characterization of the lipid composition in all samples via NMR. Our experiments demonstrate that the sorptive capacities of the EOM samples do not differ significantly from the olive oil controls if the EOM consists of neutral lipids only. However, the EOM samples show small...

Identification of alkyl dimethylbenzylammonium surfactants in water samples by solid-phase extraction followed by ion trap LC/MS and LC/MS/MS

Science.gov (United States)

Ferrer, I.; Furlong, E.T.

2001-01-01

A novel methodology was developed for the determination of alkyl (C12, C14, and C16) dimethylbenzylammonium chloride (benzalkonium chloride or BAC, Chemical Abstract Service number: 8001-54-5) in water samples. This method is based on solid-phase extraction (SPE) using polymeric cartridges, followed by high-performance liquid chromatography/ion trap mass spectrometry (LC/MS) and tandem mass spectrometry(MS/MS) detection, equipped with an electrospray interface in positive ion mode. Chromatographic separation was achieved for three BAC homologues by using a C18 column and a gradient of acetonitrile/10 millimolar aqueous ammonium formate. Total method recoveries were higher than 71% in different water matrices. The main ions observed by LC/MS were at mass-to-charge ratios (m/z) of 304, 332, and 360, which correspond to the molecular ions of the C12, C14, and C16 alkyl BAC, respectively. The unequivocal structural identification of these compounds in water samples was performed by LC/MS/MS after isolation and subsequent fragmentation of each molecular ion. The main fragmentation observed for the three different homologues corresponded to the loss of the toluyl group in the chemical structure, which leads to the fragment ions at m/z 212, 240, and 268 and a tropylium ion, characteristic of all homologues, at m/z 91. Detection limits for the methodology developed in this work were in the low nanogram-per-liter range. Concentration levels of BAC - ranging from 1.2 to 36.6 micrograms per liter - were found in surface-water samples collected downstream from different wastewater-treatment discharges, thus indicating its input and persistence through the wastewater-treatment process.

Development of analytical techniques for water and environmental samples (2)

Energy Technology Data Exchange (ETDEWEB)

Eum, Chul Hun; Jeon, Chi Wan; Jung, Kang Sup; Song, Kyung Sun; Kim, Sang Yeon [Korea Institute of Geology Mining and Materials, Taejon (Korea)

1998-12-01

The purpose of this study is to develop new analytical methods with good detection limit for toxic inorganic and organic compounds. The analyses of CN, organic acids, particulate materials in environmental samples have been done using several methods such as Ion Chromatography, SPE, SPME, GC/MS, GC/FID, SPLITT (split-flow thin cell fractionation) during the second year of this project. Advantage and disadvantage of several distillation method (by KS, JIS, EPA) for CN analysis in wastewater were investigated. As the results, we proposed new distillation apparatus for CN analysis, which was proved to be simpler, faster and to get better recovery than conventional apparatus. And ion chromatograph/pulsed amperometric detector (IC/PAD) system instead of colorimetry for CN detection was setup to solve matrix interference. And SPE(solid phase extraction) and SPME (solid phase micro extraction) as liquid-solid extraction technique were applied to the analysis of phenols in wastewater. Optimum experimental conditions and factors influencing analytical results were determined. From these results, It could be concluded that C{sub 18} cartridge and polystyrene-divinylbenzene disk in SPE method, polyacrylate fiber in SPME were proper solid phase adsorbent for phenol. Optimum conditions to analyze phenol derivatives simultaneously were established. Also, Continuous SPLITT (Split-flow thin cell) Fractionation (CSF) is a new preparative separation technique that is useful for fractionation of particulate and macromolecular materials. CSF is carried out in a thin ribbon-like channel equipped with two splitters at both inlet and outlet of the channel. In this work, we set up a new CSF system, and tested using polystyrene latex standard particles. And then we fractionated particles contained in air and underground water based on their sedimentation coefficients using CSF. (author). 27 refs., 13 tabs., 31 figs.

Routine plasma analysis for 2-[18F]fluorotyrosine by SAX-cartridges

International Nuclear Information System (INIS)

Kling, P.; Coenen, H.H.; Stoecklin, G.

1990-01-01

There is a great necessity for simple, reliable, and fast methods of plasma analysis. While HPLC is generally the most effective method, it is rather time consuming and expensive in a routine setting with numerous plasma samples. The authors have developed a new method for determination of the amino acid analogue 2-[ 18 F]fluorotyrosine using SAX columns (Adsorbex R SAX, 400 mg, Merck). The results obtained agree within 5% with those determined by reverse phase HPLC

Structural and optical properties of AgIn5S8

Science.gov (United States)

Rincón, Carlos A. Durante; Durán, Larissa T.; Medina, Josefa Estévez; Castro, Jaime A.; León, Máximo; Fermín, Jose R.

2017-12-01

Compounds of the chalcogenide family Ag-In-VI (VI = S, Se, Te) are interesting materials due to their stoichiometric stability and potential application in nonlinear optics and solar cells. A polycrystalline ingot of AgIn5S8, an ordered vacancy semiconductor, was prepared by direct fusion of the stoichiometric mixture of the elements in an evacuated quartz ampoule. The presence of a single phase with cubic structure was confirmed by X-ray powder diffraction at room temperature. The lattice parameter, a, was calculated, giving 10.821750 Å. Samples in evacuated quartz ampoules were used to perform Differential Thermal Analysis measurements, showing congruent melting at 1110∘C. Transmittance and reflectivity measurements were used to calculate the absorption coefficient α. From the plot of (αhν)2 versus hν, two direct transitions are observed at 1.25 eV and 1.88 eV. While the higher energy direct transition has been observed by other authors, the direct nature of the lower energy transition was confirmed from the fitting of the plot of the reflectivity versus 1/hν between 0.53 eV-1 (1.89 eV) and 0.55 eV-1 (1.82 eV), obtaining a value of 1.29 eV. The real refractive index n and the high-frequency dielectric constant 𝜀∞ were also obtained from the fit of the reflectivity, resulting to be 2.68 and 7.2, respectively.

Rapid extraction and quantitative detection of the herbicide diuron in surface water by a hapten-functionalized carbon nanotubes based electrochemical analyzer.

Science.gov (United States)

Sharma, Priyanka; Bhalla, Vijayender; Tuteja, Satish; Kukkar, Manil; Suri, C Raman

2012-05-21

A solid phase extraction micro-cartridge containing a non-polar polystyrene absorbent matrix was coupled with an electrochemical immunoassay analyzer (EIA) and used for the ultra-sensitive detection of the phenyl urea herbicide diuron in real samples. The EIA was fabricated by using carboxylated carbon nanotubes (CNTs) functionalized with a hapten molecule (an amine functionalized diuron derivative). Screen printed electrodes (SPE) were modified with these haptenized CNTs and specific in-house generated anti diuron antibodies were used for bio-interface development. The immunodetection was realized in a competitive electrochemical immunoassay format using alkaline phosphatase labeled secondary anti-IgG antibody. The addition of 1-naphthyl phosphate substrate resulted in the production of an electrochemically active product, 1-naphthol, which was monitored by using differential pulse voltammetry (DPV). The assay exhibited excellent sensitivity and specificity having a dynamic response range of 0.01 pg mL(-1) to 10 μg mL(-1) for diuron with a limit of detection of around 0.1 pg mL(-1) (n = 3) in standard water samples. The micro-cartridge coupled hapten-CNTs modified SPE provided an effective and efficient electrochemical immunoassay for the real-time monitoring of pesticides samples with a very high degree of sensitivity.

Meniscus effect in microgravity materials processing

Science.gov (United States)

1998-01-01

While the microgravity environment of orbit eliminates a number of effects that impede the formation of materials on Earth, the change can also cause new, unwanted effects. A mysterious phenomenon, known as detached solidification, apparently stems from a small hydrostatic force that turns out to be pervasive. The contact of the solid with the ampoule transfers stress to the growing crystal and causing unwanted dislocations and twins. William Wilcox and Liya Regel of Clarkson University theorize that the melt is in contact with the ampoule wall, while the solid is not, and the melt and solid are cornected by a meniscus. Their work is sponsored by NASA's Office of Biological and Physical Researcxh, and builds on earlier work by Dr. David Larson of the State University of New York at Stony Brook.

Decay-Accelerating Factor Mitigates Controlled Hemorrhage-Instigated Intestinal and Lung Tissue Damage and Hyperkalemia in Swine

Science.gov (United States)

2011-07-01

glucose , hematocrit (Hct), hemoglobin (Hb), sodium (Na+), potassium (K+), and ionized calcium (iCa2+) using i-STAT cartridges ( Abbott Laboratories...animals were observed for 200 minutes. Blood chemistry and physiological parameters were recorded. Tissue samples from lung and small intestine were...seemingly acceptable medical therapy and surgical intervention.4 The first physiologic response to severe blood loss is activation of the neuroendocrine

A neural network to improve dim-light vision? Dendritic fields of first-order interneurons in the nocturnal bee Megalopta genalis.

Science.gov (United States)

Greiner, Birgit; Ribi, Willi A; Warrant, Eric J

2005-11-01

Using the combined Golgi-electron microscopy technique, we have determined the three-dimensional dendritic fields of the short visual fibres (svf 1-3) and first-order interneurons or L-fibres (L1-4) within the first optic ganglion (lamina) of the nocturnal bee Megalopta genalis. Serial cross sections have revealed that the svf type 2 branches into one adjacent neural unit (cartridge) in layer A, the most distal of the three lamina layers A, B and C. All L-fibres, except L1-a, exhibit wide lateral branching into several neighbouring cartridges. L1-b shows a dendritic field of seven cartridges in layers A and C, dendrites of L2 target 13 cartridges in layer A, L3 branches over a total of 12 cartridges in layer A and three in layer C and L4 has the largest dendritic field size of 18 cartridges in layer C. The number of cartridges reached by the respective L-fibres is distinctly greater in the nocturnal bee than in the worker honeybee and is larger than could be estimated from our previous Golgi-light microscopy study. The extreme dorso-ventrally oriented dendritic field of L4 in M. genalis may, in addition to its potential role in spatial summation, be involved in edge detection. Thus, we have shown that the amount of lateral spreading present in the lamina provides the anatomical basis for the required spatial summation. Theoretical and future physiological work should further elucidate the roles that this lateral spreading plays to improve dim-light vision in nocturnal insects.

Determination of sodium in pharmaceuticals by neutron activation analysis

International Nuclear Information System (INIS)

Kanias, G.D.

1985-01-01

A simple, fast and accurate neutron activation analysis method for determination of Na in drugs concerning either active compound or total content was developed. The examined dosage forms consisted of 10 injectable ampoules and 10 bottles of oral solutions. The irradiation of samples and standards was carried out in the rotation system of the Reactor of Nuclear Research Center Democritos with maximal neutron flux of 2,9.10 13 n.cm -2 .sec -1 . Gamma-ray spectrometry of the irradiated samples and standards was accomplished with a coaxial Ge(Li) detector series Win 15 with an efficiency of 15% connected to an Ino-Tech 1024 channel analyser (Model IT 5200). The accuracy and precision of the method are found to be very high and therefore it could be established as an official one for the determination of sodium in parmaceuticals

Determination of quaternary ammonium compounds in seawater samples by solid-phase extraction and liquid chromatography-mass spectrometry.

Science.gov (United States)

Bassarab, P; Williams, D; Dean, J R; Ludkin, E; Perry, J J

2011-02-04

A method for the simultaneous determination of two biocidal quaternary ammonium compounds; didecyldimethylammonium chloride (didecyldimethyl quat) and dodecylbenzyldimethylammonium chloride (benzyl quat), in seawater by solid phase extraction (SPE) followed by liquid chromatography-mass spectrometry (LC-MS) was developed. The optimised procedure utilised off-line extraction of the analytes from seawater using polymeric (Strata-X) SPE cartridges. Recoveries ranged from 80 to 105%, with detection limits at the low parts-per-trillion (ng/l) level for both analytes. To demonstrate sensitivity, environmental concentrations were measured at three different locations along the North East coast of England with measured values in the range 120-270ng/l. Copyright © 2010 Elsevier B.V. All rights reserved.

Determination of decamethylcyclopentasiloxane in air using commercial solid phase extraction cartridges.

Science.gov (United States)

Kierkegaard, Amelie; McLachlan, Michael S

2010-05-21

Decamethylcyclopentasiloxane (D(5)), a high production volume chemical used in personal care products, has been designated for regulation in Canada and is under review in the EU because of concerns about its persistence and potential for bioaccumulation in the environment. D(5) is a volatile compound expected to be found primarily in air, but there is little information on atmospheric concentrations due to the lack of sensitive analytical methods. Here a simple and sensitive method to determine D(5) in ambient air is presented. The challenge in the environmental analysis of D(5) is avoiding contamination. Our method is based on the high trapping efficiency of the sorbent Isolute ENV+, combined with a comparably high sampling rate. A small amount of sorbent (10 mg) is eluted in a small volume of n-hexane (0.1-0.6 mL), which is injected onto a GC/MS system without further processing. The simplicity of the method enables the use of a field blank for every sample to trace contamination. The method provides low limits of quantification (approximately 0.3 ng/m(3)), good repeatability and limited breakthrough (approximately 1%). By lowering the limit of quantification compared to published work by almost two orders of magnitude, it became possible to quantify D(5) in ambient air at locations remote from strong point sources. The concentrations at a rural Swedish site ranged from 0.7 to 8 ng/m(3) over a period of 4 months. 2010 Elsevier B.V. All rights reserved.

Volatilizable Biogenic Organic Compounds (VBOCs with two dimensional Gas Chromatography-Time of Flight Mass Spectrometry (GC × GC-TOFMS: sampling methods, VBOC complexity, and chromatographic retention data

Directory of Open Access Journals (Sweden)

C. Chen

2012-02-01

Full Text Available Two dimensional gas chromatography (GC × GC with detection by time-of-flight mass spectrometry (TOFMS was applied in the rapid analysis of air samples containing highly complex mixtures of volatilizable biogenic organic compounds (VBOCs. VBOC analytical methodologies are briefly reviewed, and optimal conditions are discussed for sampling with both adsorption/thermal desorption (ATD cartridges and solid-phase microextraction (SPME fibers. Air samples containing VBOC emissions from leaves of two tree species (Cedrus atlantica and Calycolpus moritzianus were obtained by both ATD and SPME. The optimized gas chromatographic conditions utilized a 45 m, 0.25 mm I.D. low-polarity primary column (DB-VRX, 1.4 μm film and a 1.5 m, 0.25 mm I.D. polar secondary column (StabilwaxTM, 0.25 μm film. Excellent separation was achieved in a 36 min temperature programmed GC × GC chromatogram. Thousands of VBOC peaks were present in the sample chromatograms; hundreds of tentative identifications by NIST mass spectral matching are provided. Very few of the tentatively identified compounds are currently available as authentic standards. Minimum detection limit values for a 5 l ATD sample were 3.5 pptv (10 ng m−3 for isoprene, methyl vinyl ketone, and methacrolein, and ~1.5 pptv (~10 ng m−3 for monoterpenes and sesquiterpenes. Kovats-type chromatographic retention index values on the primary column and relative retention time values on the secondary column are provided for 21 standard compounds and for 417 tentatively identified VBOCs. 19 of the 21 authentic standard compounds were found in one of the Cedrus atlantica SPME samples. In addition, easily quantifiable levels of at least 13 sesquiterpenes were found in an ATD sample obtained from a branch enclosure of Calycolpus moritzianus. Overall, the results obtained via GC × GC-TOFMS highlight an extreme, and largely uncharacterized diversity of VBOCs, consistent with the hypothesis that sesquiterpenes and

Volatilizable Biogenic Organic Compounds (VBOCs) with two dimensional Gas Chromatography-Time of Flight Mass Spectrometry (GC × GC-TOFMS): sampling methods, VBOC complexity, and chromatographic retention data

Science.gov (United States)

Pankow, J. F.; Luo, W.; Melnychenko, A. N.; Barsanti, K. C.; Isabelle, L. M.; Chen, C.; Guenther, A. B.; Rosenstiel, T. N.

2012-02-01

Two dimensional gas chromatography (GC × GC) with detection by time-of-flight mass spectrometry (TOFMS) was applied in the rapid analysis of air samples containing highly complex mixtures of volatilizable biogenic organic compounds (VBOCs). VBOC analytical methodologies are briefly reviewed, and optimal conditions are discussed for sampling with both adsorption/thermal desorption (ATD) cartridges and solid-phase microextraction (SPME) fibers. Air samples containing VBOC emissions from leaves of two tree species (Cedrus atlantica and Calycolpus moritzianus) were obtained by both ATD and SPME. The optimized gas chromatographic conditions utilized a 45 m, 0.25 mm I.D. low-polarity primary column (DB-VRX, 1.4 μm film) and a 1.5 m, 0.25 mm I.D. polar secondary column (StabilwaxTM, 0.25 μm film). Excellent separation was achieved in a 36 min temperature programmed GC × GC chromatogram. Thousands of VBOC peaks were present in the sample chromatograms; hundreds of tentative identifications by NIST mass spectral matching are provided. Very few of the tentatively identified compounds are currently available as authentic standards. Minimum detection limit values for a 5 l ATD sample were 3.5 pptv (10 ng m-3) for isoprene, methyl vinyl ketone, and methacrolein, and ~1.5 pptv (~10 ng m-3) for monoterpenes and sesquiterpenes. Kovats-type chromatographic retention index values on the primary column and relative retention time values on the secondary column are provided for 21 standard compounds and for 417 tentatively identified VBOCs. 19 of the 21 authentic standard compounds were found in one of the Cedrus atlantica SPME samples. In addition, easily quantifiable levels of at least 13 sesquiterpenes were found in an ATD sample obtained from a branch enclosure of Calycolpus moritzianus. Overall, the results obtained via GC × GC-TOFMS highlight an extreme, and largely uncharacterized diversity of VBOCs, consistent with the hypothesis that sesquiterpenes and other compounds

GdCuMg with ZrNiAl-type structure. An 82.2 K ferromagnet

Energy Technology Data Exchange (ETDEWEB)

Stein, Sebastian; Heletta, Lukas; Poettgen, Rainer [Muenster Univ. (Germany). Inst. fuer Anorganische und Analytische Chemie

2017-08-01

GdCuMg has been synthesized by induction-melting of the elements in a sealed niobium ampoule followed by annealing in a muffle furnace. The sample was studied by powder and single crystal X-ray diffraction: ZrNiAl type, P anti 62m (a=749.2(4), c=403.3(1) pm), wR2=0.0242, 315 F{sup 2} values and 15 variables. Temperature dependent magnetic susceptibility measurements have revealed an experimental magnetic moment of 8.54(1) μ{sub B} per Gd atom. GdCuMg orders ferromagnetically below T{sub C}=82.2(5) K and based on the magnetization isotherms it can be classified as a soft ferromagnet.

Radiation grafting of pH and thermosensitive N-isopropylacrylamide and acrylic acid onto PTFE films by two-steps process

International Nuclear Information System (INIS)

Bucio, E.; Burillo, G.

2007-01-01

Polytetrafluoroethylene (PTFE) was grafted (g) with acrylic acid (AAc) by γ-ray pre-irradiation method to get PTFE-g-AAc films, then N-isopropylacrylamide (NIPAAm) was grafted onto PTFE-g-AAc films with γ-ray to get (PTFE-g-AAc)-g-NIPAAm. PTFE films were irradiated in air at a dose rate of 3.0 kGy h -1 and different radiation dose. The irradiated films were placed in glass ampoules, which contained aqueous solutions with different monomer concentration (AAc), and then they were heated at different temperatures and reaction time. NIPAAm onto PTFE-g-AAc was carried out with the same procedure with monomer concentration of 1 mol L -1 . The thermosensitivity of the samples was defined and calculated as the ratio of the grafted samples swelling at 28 and 35 o C, and pH sensitivity defined as the ratio of the grafted samples swelling at pH 2 and 8

Integrated passive flux measurement in groundwater: design and performance of iFLUX samplers

Science.gov (United States)

Verreydt, Goedele; Razaei, Meisam; Meire, Patrick; Van Keer, Ilse; Bronders, Jan; Seuntjens, Piet

2017-04-01

monitor speed and direction of flow and 3 cartridges to monitor different sources of pollution - VOC's, heavy metals and nutrients. The modular design enables to sample several types of pollution at the same time. The principles and the design of the iFLUX technology will be presented, together with the results from performance and sensitivity analysis for different field scenarios and several field cases.

Preparation and stability study of ampouled polycyclic aromatic hydrocarbon solutions

NARCIS (Netherlands)

Vaessen; H.A.M.G.; Kamp; C.G. van de; Jekel; A.A.

1986-01-01

De stabiliteit van geampulleerde acetonitril- en tolueenoplossingen van zeven polycyclische aromatische koolwaterstoffen (PAK) werd bestudeerd gedurende een jaar. Beide oplossingen waren qua PAK- samenstelling en gehalte identiek en bereid uit een moederoplossing. Voor en vlak na het ampulleren

Automated Microfluidic Platform for Serial Polymerase Chain Reaction and High-Resolution Melting Analysis.

Science.gov (United States)

Cao, Weidong; Bean, Brian; Corey, Scott; Coursey, Johnathan S; Hasson, Kenton C; Inoue, Hiroshi; Isano, Taisuke; Kanderian, Sami; Lane, Ben; Liang, Hongye; Murphy, Brian; Owen, Greg; Shinoda, Nobuhiko; Zeng, Shulin; Knight, Ivor T

2016-06-01

We report the development of an automated genetic analyzer for human sample testing based on microfluidic rapid polymerase chain reaction (PCR) with high-resolution melting analysis (HRMA). The integrated DNA microfluidic cartridge was used on a platform designed with a robotic pipettor system that works by sequentially picking up different test solutions from a 384-well plate, mixing them in the tips, and delivering mixed fluids to the DNA cartridge. A novel image feedback flow control system based on a Canon 5D Mark II digital camera was developed for controlling fluid movement through a complex microfluidic branching network without the use of valves. The same camera was used for measuring the high-resolution melt curve of DNA amplicons that were generated in the microfluidic chip. Owing to fast heating and cooling as well as sensitive temperature measurement in the microfluidic channels, the time frame for PCR and HRMA was dramatically reduced from hours to minutes. Preliminary testing results demonstrated that rapid serial PCR and HRMA are possible while still achieving high data quality that is suitable for human sample testing. © 2015 Society for Laboratory Automation and Screening.

Simultaneous HPLC-F analysis of three recent antiepileptic drugs in human plasma.

Science.gov (United States)

Mercolini, Laura; Mandrioli, Roberto; Amore, Mario; Raggi, Maria Augusta

2010-09-21

An original high-performance liquid chromatographic method with fluorescence detection is presented for the simultaneous determination of the three antiepileptic drugs gabapentin, vigabatrin and topiramate in human plasma. After pre-column derivatisation with dansyl chloride, the analytes were separated on a Hydro-RP column with a mobile phase composed of phosphate buffer (55%) and acetonitrile (45%) and detected at lambda(em)=500 nm, exciting at 300 nm. An original pre-treatment procedure on biological samples, based on solid-phase extraction with MCX cartridges for gabapentin and vigabatrin, and with Plexa cartridges for topiramate, gave high extraction yields (>91%), satisfactory precision (RSDvigabatrin and in the 1.0-50.0 microg mL(-1) range for topiramate, with limits of detection (LODs) between 0.1 and 0.3 microg mL(-1). After validation, the method was successfully applied to some plasma samples from patients undergoing therapy with one or more of these drugs. Accuracy results were satisfactory (recovery >91%). Therefore, the method seems to be suitable for the therapeutic drug monitoring (TDM) of patients treated with gabapentin, vigabatrin and topiramate. Copyright 2010 Elsevier B.V. All rights reserved.

Extraction tools for identification of chemical contaminants in estuarine and coastal waters to determine toxic pressure on primary producers.

Science.gov (United States)

Booij, Petra; Sjollema, Sascha B; Leonards, Pim E G; de Voogt, Pim; Stroomberg, Gerard J; Vethaak, A Dick; Lamoree, Marja H

2013-09-01

The extent to which chemical stressors affect primary producers in estuarine and coastal waters is largely unknown. However, given the large number of legacy pollutants and chemicals of emerging concern present in the environment, this is an important and relevant issue that requires further study. The purpose of our study was to extract and identify compounds which are inhibitors of photosystem II activity in microalgae from estuarine and coastal waters. Field sampling was conducted in the Western Scheldt estuary (Hansweert, The Netherlands). We compared four different commonly used extraction methods: passive sampling with silicone rubber sheets, polar organic integrative samplers (POCIS) and spot water sampling using two different solid phase extraction (SPE) cartridges. Toxic effects of extracts prepared from spot water samples and passive samplers were determined in the Pulse Amplitude Modulation (PAM) fluorometry bioassay. With target chemical analysis using LC-MS and GC-MS, a set of PAHs, PCBs and pesticides was determined in field samples. These compound classes are listed as priority substances for the marine environment by the OSPAR convention. In addition, recovery experiments with both SPE cartridges were performed to evaluate the extraction suitability of these methods. Passive sampling using silicone rubber sheets and POCIS can be applied to determine compounds with different structures and polarities for further identification and determination of toxic pressure on primary producers. The added value of SPE lies in its suitability for quantitative analysis; calibration of passive samplers still needs further investigation for quantification of field concentrations of contaminants. Copyright © 2013 Elsevier Ltd. All rights reserved.

Comparison of techniques for the determination of conversion during suspension polymerization reactions

Directory of Open Access Journals (Sweden)

J. C. Santos

2008-06-01

Full Text Available The determination of conversion during suspension polymerization reactions is not an easy task due to the heterogeneity of the reaction medium and the tendency of particles to agglomerate rapidly when stirring is stopped. Usually, bulk polymerization in ampoules is employed to study the kinetics of suspension polymerization reactions. In this work, a comparison of different techniques for the determination of conversion during suspension polymerization reactions is presented. Results showed a good agreement between the conversion obtained by gravimetry during styrene suspension polymerization and on-line conversion monitoring data using fiber-optic based Raman Spectroscopy. Nevertheless, the polymerization rate of styrene bulk polymerization carried out in ampoules was higher than the real reaction rate of styrene suspension polymerization due to slightly higher reaction temperatures. Simulation results using the experimental temperature data in a mathematical model confirmed these results.

Analysis of nitrosamines in water by automated SPE and isotope dilution GC/HRMS Occurrence in the different steps of a drinking water treatment plant, and in chlorinated samples from a reservoir and a sewage treatment plant effluent.

Science.gov (United States)

Planas, Carles; Palacios, Oscar; Ventura, Francesc; Rivera, Josep; Caixach, Josep

2008-08-15

A method based on automated solid-phase extraction (SPE) and isotope dilution gas chromatography/high resolution mass spectrometry (GC/HRMS) has been developed for the analysis of nine nitrosamines in water samples. The combination of automated SPE and GC/HRMS for the analysis of nitrosamines has not been reported previously. The method shows as advantages the selectivity and sensitivity of GC/HRMS analysis and the high efficiency of automated SPE with coconut charcoal EPA 521 cartridges. Low method detection limits (MDLs) were achieved, along with a greater facility of the procedure and less dependence on the operator with regard to the methods based on manual SPE. Quality requirements for isotope dilution-based methods were accomplished for most analysed nitrosamines, regarding to trueness (80-120%), method precision (water samples (16 samples from a drinking water treatment plant {DWTP}, 2 chlorinated samples from a sewage treatment plant {STP} effluent, and 1 chlorinated sample from a reservoir) were analysed. Concentrations of nitrosamines in the STP effluent were 309.4 and 730.2 ng/L, being higher when higher doses of chlorine were applied. N-Nitrosodimethylamine (NDMA) and N-nitrosodiethylamine (NDEA) were the main compounds identified in the STP effluent, and NDEA was detected above 200 ng/L, regulatory level for NDMA in effluents stated in Ontario (Canada). Lower concentrations of nitrosamines were found in the reservoir (20.3 ng/L) and in the DWTP samples (n.d. -28.6 ng/L). NDMA and NDEA were respectively found in the reservoir and in treated and highly chlorinated DWTP samples at concentrations above 10 ng/L (guide value established in different countries). The highest concentrations of nitrosamines were found after chlorination and ozonation processes (ozonated, treated and highly chlorinated water) in DWTP samples.

Semi-field assessment of the BG-Malaria trap for monitoring the African malaria vector, Anopheles arabiensis.

Directory of Open Access Journals (Sweden)

Elis P A Batista

Full Text Available Odour-baited technologies are increasingly considered for effective monitoring of mosquito populations and for the evaluation of vector control interventions. The BG-Malaria trap (BGM, which is an upside-down variant of the widely used BG-Sentinel trap (BGS, has been demonstrated to be effective to sample the Brazilian malaria vector, Anopheles darlingi. We evaluated the BGM as an improved method for sampling the African malaria vectors, Anopheles arabiensis. Experiments were conducted inside a large semi-field cage to compare trapping efficiencies of BGM and BGS traps, both baited with the synthetic attractant, Ifakara blend, supplemented with CO2. We then compared BGMs baited with either of four synthetic mosquito lures, Ifakara blend, Mbita blend, BG-lure or CO2, and an unbaited BGM. Lastly, we compared BGMs baited with the Ifakara blend dispensed via either nylon strips, BG cartridges (attractant-infused microcapsules encased in cylindrical plastic cartridge or BG sachets (attractant-infused microcapsules encased in plastic sachets. All tests were conducted between 6P.M. and 7A.M., with 200-600 laboratory-reared An. arabiensis released nightly in the test chamber. The median number of An. arabiensis caught by the BGM per night was 83, IQR:(73.5-97.75, demonstrating clear superiority over BGS (median catch = 32.5 (25.25-37.5. Compared to unbaited controls, BGMs baited with Mbita blend caught most mosquitoes (45 (29.5-70.25, followed by BGMs baited with CO2 (42.5 (27.5-64, Ifakara blend (31 (9.25-41.25 and BG lure (16 (4-22. BGM caught 51 (29.5-72.25 mosquitoes/night, when the attractants were dispensed using BG-Cartridges, compared to BG-Sachet (29.5 (24.75-40.5, and nylon strips (27 (19.25-38.25, in all cases being significantly superior to unbaited controls (p < 000.1. The findings demonstrate potential of the BGM as a sampling tool for African malaria vectors over the standard BGS trap. Its efficacy can be optimized by selecting

Simple and fast analysis of tetrabromobisphenol A, hexabromocyclododecane isomers, and polybrominated diphenyl ethers in serum using solid-phase extraction or QuEChERS extraction followed by tandem mass spectrometry coupled to HPLC and GC.

Science.gov (United States)

Li, Jian; Chen, Tian; Wang, Yuwei; Shi, Zhixiong; Zhou, Xianqing; Sun, Zhiwei; Wang, Dejun; Wu, Yongning

2017-02-01

Two simplified sample preparation procedures for simultaneous extraction and clean-up of tetrabromobisphenol A, α-, β-, and γ-hexabromocyclododecane and polybrominated diphenyl ethers in human serum were developed and validated. The first procedure was based on solid-phase extraction. Sample extraction, purification, and lipid removal were carried out directly on an Oasis HLB cartridge. The second procedure was a quick, easy, cheap, effective, rugged, and safe-based approach using octadecyl-modified silica particles as a sorbent. After sample extraction and cleanup, tetrabromobisphenol A/hexabromocyclododecane was separated from polybrominated diphenyl ethers by using a Si-based cartridge. Tetrabromobisphenol A and hexabromocyclododecane were then detected by high-performance liquid chromatography coupled to tandem mass spectrometry, while polybrominated diphenyl ethers were detected by gas chromatography coupled to tandem mass spectrometry. The results of the spike recovery test using fetal bovine serum showed that the average recoveries of the analytes ranged from 87.3 to 115.3% with relative standard deviations equal to or lower than 13.4 %. Limits of detection of the analytes were in the range of 0.4-19 pg/mL except for decabromodiphenyl ether. The developed method was successfully applied to routine analysis of human serum samples from occupational workers and the general population. Extremely high serum polybrominated diphenyl ethers levels up to 3.32 × 10 4 ng/g lipid weight were found in occupational workers. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A new technique for the deposition of standard solutions in total reflection X-ray fluorescence spectrometry (TXRF) using pico-droplets generated by inkjet printers and its applicability for aerosol analysis with SR-TXRF

International Nuclear Information System (INIS)

Fittschen, U.E.A.; Hauschild, S.; Amberger, M.A.; Lammel, G.; Streli, C.; Foerster, S.; Wobrauschek, P.; Jokubonis, C.; Pepponi, G.; Falkenberg, G.; Broekaert, J.A.C.

2006-01-01

A new technique for the deposition of standard solutions on particulate aerosol samples using pico-droplets for elemental determinations with total reflection X-ray fluorescence spectrometry (TXRF) is described. It enables short analysis times without influencing the sample structure and avoids time consuming scanning of the sample with the exciting beam in SR-TXRF analysis. Droplets of picoliter volume (∼ 5-130 pL) were generated with commercially available and slightly modified inkjet printers operated with popular image processing software. The size of the dried droplets on surfaces of different polarity namely silicone coated and untreated quartz reflectors, was determined for five different printer types and ten different cartridge types. The results show that droplets generated by inkjet printers are between 50 and 200 μm in diameter (corresponding to volumes of 5 to 130 pL) depending on the cartridge type, which is smaller than the width of the synchrotron beam used in the experiments (< 1 mm at an energy of 17 keV at the beamline L at HASYLAB, Hamburg). The precision of the printing of a certain amount of a single element standard solution was found to be comparable to aliquoting with micropipettes in TXRF, where for 2.5 ng of cobalt relative standard deviations of 12% are found. However, it could be shown that the printing of simple patterns is possible, which is important when structured samples have to be analysed

Chemical transport of niobium(V) oxide and of lithium niobate with sulphur

International Nuclear Information System (INIS)

Schaefer, H.

1988-01-01

Niobium(V) oxide is transported by means of sulphur (calculated for 10 bar at 1223 K) from 1273 → 1173 K. The same applies for lithium niobate. Similar experiments of lithium oxide lead to turbidity of the quartz ampoule. (author)

Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory - Determination of Wastewater Compounds by Polystyrene-Divinylbenzene Solid-Phase Extraction and Capillary-Column Gas Chromatography/Mass Spectrometry

Science.gov (United States)

Zaugg, Steven D.; Smith, Steven G.; Schroeder, Michael P.; Barber, Larry B.; Burkhardt, Mark R.

2002-01-01

A method for the determination of 67 compounds typically found in domestic and industrial wastewater is described. The method was developed in response to increasing concern over the impact of endocrine-disrupting chemicals in wastewater on aquatic organisms. This method also may be useful for evaluating the impact of combined sanitary and storm-sewer overflow on the water quality of urban streams. The method focuses on the determination of compounds that are an indicator of wastewater or that have been chosen on the basis of their endocrine-disrupting potential or toxicity. These compounds include the alkylphenol ethoxylate nonionic surfactants and their degradates, food additives, fragrances, antioxidants, flame retardants, plasticizers, industrial solvents, disinfectants, fecal sterols, polycyclicaromatic hydrocarbons, and high-use domestic pesticides. Water samples are filtered to remove suspended particulate matter and then are extracted by vacuum through disposable solid-phase cartridges that contain polystyrene-divinylbenzene resin. Cartridges are dried with nitrogen gas, and then sorbed compounds are eluted with dichloromethane-diethyl ether (4:1) and determined by capillary-column gas chromatography/mass spectrometry. Recoveries in reagent-water samples fortified at 4 micrograms per liter averaged 74 percent ? 7 percent relative standard deviation for all method compounds. Initial method detection limits for single-component compounds (excluding hormones and sterols) averaged 0.15 microgram per liter. Samples are preserved by filtration, the addition of 60 grams NaCl, and storage at 4 degrees Celsius. The laboratory has established a sample-holding time (prior to sample extraction) of 14 days from the date of sample collection until a statistically accepted method can be used to determine the effectiveness of these sample-preservation procedures.

Subduction factory in an ampoule: Experiments on sediment-peridotite interaction under temperature gradient conditions

Science.gov (United States)

Woodland, A. B.; Bulatov, V. K.; Brey, G. P.; Girnis, A. V.; Höfer, H. E.; Gerdes, A.

2018-02-01

To better understand processes above subducted oceanic slabs, we have undertaken experiments with juxtaposed sediment and peridotite layers at pressures of 7.5 and 10.5 GPa at a controlled temperature gradient from ∼100 to ∼500 °C per a sample length of ∼3 mm. The sediment starting material contains H2O (6.9 wt%) and CO2 (5.9 wt%) and has a major-element composition similar to GLOSS (Plank and Langmuir, 1998) doped with trace elements at 10-100 ppm levels. Several experiments were conducted with ∼0.5 wt% Cl or F. The peridotite layer is composed of natural olivine (66 wt%), orthopyroxene (27 wt%) and garnet (7 wt%) mixed with ∼15 wt% graphite. Several experimental configurations were investigated, but the "basic" setup has the sediment layer at the bottom in the cold zone (400-1200 °C) overlain by peridotite at 900-1500 °C. The temperature distribution was determined by two thermocouples and orthopyroxene-garnet thermometry. Features common to many experiments are (1) the development of multiple layers of various lithologies and a pool of hydrous silicate or carbonate-silicate melt in the hottest part of the capsule; (2) replacement of olivine by orthopyroxene in the metaperidotite; (3) preservation and growth of garnet and local development of magnesite in the metaperidotite layer; (4) enrichment in garnet within the metasediment layer at the contact with the metaperidotite; (5) formation of a clinopyroxene-garnet assemblage at the bottom (the coldest part); (6) presence of K-bearing phases (phlogopite or phengite) and carbonates in the metasediment layer only at temperatures Ca are largely retained in the coldest part of the metasediment layer in clinopyroxene, Ca-rich garnet and aragonite. The melt is a product of interaction between partial melt or fluid from the sediment and peridotite. It has a silico-carbonatite composition with variable SiO2, MgO, FeO and CaO contents and low Al2O3. The addition of Cl has almost no effect on element

Automated measurement of 224Ra and 226Ra in water

International Nuclear Information System (INIS)

Dimova, N.; Burnett, W.C.; Horwitz, E.P.; Lane-Smith, D.

2007-01-01

We present a new simple approach for automated, non-destructive measurement of the alpha-emitting radium isotopes ( 223 Ra, 224 Ra, and 226 Ra) in water based on the emanation of their respective radon daughters ( 219 Rn, 220 Rn, and 222 Rn). The method combines the high adsorption uptake of MnO 2 Resin for radium (K d =2.4x10 4 ml/g) over a wide pH range with the simplicity of the activity registration using a commercial radon-in-air analyzer (RAD7, DURRIDGE Company, Inc). Radium is first adsorbed onto the MnO 2 Resin by passing a water sample through the resin packed in a gas-tight glass cartridge. The same cartridge is then connected to the radon analyzer via a simple tubing system to circulate air through the resin and a drying system. The efficiency of the proposed system is determined by running standards prepared in the same manner. Our results indicate that the efficiency for 226 Ra is >22% if both 218 Po and 214 Po counts are collected. This is comparable with typical efficiencies for alpha spectrometry but with much less sample preparation. We estimate that an MDA of 0.8 pCi/L for 226 Ra may be obtained with this new approach using a 1 L water sample and less than 4 h of counting

Development and characterization of a novel plug and play liquid chromatography-mass spectrometry (LC-MS) source that automates connections between the capillary trap, column, and emitter.

Science.gov (United States)

Bereman, Michael S; Hsieh, Edward J; Corso, Thomas N; Van Pelt, Colleen K; Maccoss, Michael J

2013-06-01

We report the development and characterization of a novel, vendor-neutral ultra-high pressure-compatible (~10,000 p.s.i.) LC-MS source. This device is the first to make automated connections with user-packed capillary traps, columns, and capillary emitters. The source uses plastic rectangular inserts (referred to here as cartridges) where individual components (i.e. trap, column, or emitter) can be exchanged independent of one another in a plug and play manner. Automated robotic connections are made between the three cartridges using linear translation powered by stepper motors to axially compress each cartridge by applying a well controlled constant compression force to each commercial LC fitting. The user has the versatility to tailor the separation (e.g. the length of the column, type of stationary phase, and mode of separation) to the experimental design of interest in a cost-effective manner. The source is described in detail, and several experiments are performed to evaluate the robustness of both the system and the exchange of the individual trap and emitter cartridges. The standard deviation in the retention time of four targeted peptides from a standard digest interlaced with a soluble Caenorhabditis elegans lysate ranged between 3.1 and 5.3 s over 3 days of analyses. Exchange of the emitter cartridge was found to have an insignificant effect on the abundance of various peptides. In addition, the trap cartridge can be replaced with minimal effects on retention time (<20 s).

Evaluation of the FTA carrier device for human papillomavirus testing in developing countries.

Science.gov (United States)

Gonzalez, Paula; Cortes, Bernal; Quint, Wim; Kreimer, Aimée R; Porras, Carolina; Rodríguez, Ana Cecilia; Jimenez, Silvia; Herrero, Rolando; Struijk, Linda; Hildesheim, Allan; Melchers, Willem

2012-12-01

Liquid-based methods for the collection, transportation, and storage of cervical cells are cumbersome and expensive and involve laborious DNA extraction. An FTA cartridge is a solid carrier device, easier to handle and allowing simple DNA elution for human papillomavirus (HPV) testing. HPV-DNA results from cervical specimens collected in PreservCyt medium (Hologic, Inc.) and the indicating FTA elute cartridge were compared in an area where transportation and storage may affect the performance of the test. Cervical cells from 319 young adult women enrolled in the Costa Rica Vaccine Trial were collected by a nurse using a Cervex brush (Roberts), which was placed on the FTA cartridge and subsequently rinsed in 20 ml of PreservCyt medium. Two 0.5-ml PreservCyt aliquots were frozen for HPV-PCR testing; the FTA cartridges were kept at room temperature. HPV-DNA detection and typing was performed using SPF(10) PCR/DEIA (DNA enzyme immunoassay detection of amplimers)/LiPA(25) system. The percent agreement, agreement among positives, and kappas were estimated. Positivity was higher for FTA compared to PreservCyt specimens (54.5% versus 45.8%, P FTA collection for HPV testing. HPV-DNA detection from FTA cartridges is broadly comparable to detection from PC medium. The higher HPV detection observed for FTA-collected specimens should be explored further. FTA cartridges could provide a simpler and more cost-effective method for cervical cell collection, storage, and transportation for HPV-DNA detection in research settings in developing countries.

SPE-GC/FTD determination of N-methyl-2-pyrrolidone and its metabolites in urine.

Science.gov (United States)

Kubota, Ryuichi; Endo, Yoko; Takeuchi, Akito; Inoue, Yoshinori; Ogata, Hiroko; Ogawa, Masanori; Nakagawa, Tomoo; Onda, Nobuhiko; Endo, Ginji

2007-07-01

An analytical method using a combination of solid-phase extraction (SPE) and gas chromatography with a flame thermionic detector (GC/FTD) was developed for determination of N-methyl-2-pyrrolidone (NMP), N-methylsuccinimide (MSI), and 2-hydroxy-N-methylsuccinimide (2-HMSI) in human urine. The SPE cartridge of poly(divinylbenzene/hydroxymethacrylate) used was directly loaded with urine sample, followed by elution with methyl isobutyl ketone (MIBK) and subsequent centrifugation, and the supernatant was injected into the capillary GC using a DB1701. This method allowed efficient separation of NMP, MSI, and 2-HMSI, which were nearly free of interference by other GC peaks arising from urine. Recoveries of NMP, MSI, and 2-HMSI from the SPE cartridge were about 98, 101, and 67%, respectively, with limits of detection of 0.04, 0.02, and 0.06 mg/L, respectively, which met the regulatory requirements. The present method was used for assay in biological monitoring of workers exposed to NMP in their occupational environment.

Simultaneous determination of kasugamycin and validamycin-A residues in cereals by consecutive solid-phase extraction combined with liquid chromatography-tandem mass spectrometry.

Science.gov (United States)

Zhang, Hong; Wang, Chenchen; Li, Huidong; Nie, Yan; Fang, Liping; Chen, Zilei

2018-03-01

Two polar aminoglycosides, kasugamycin and validamycin-A, were determined in cereals (brown rice, wheat and corn) by high-performance liquid chromatography-tandem mass spectrometry. The analytes were extracted from samples using methanol and water (70:30, v/v) at pH 5.5, purified using both a hydrophilic-hydrophobic-balanced cartridge and a strong cation-exchange cartridge, and then analysed using multiple reaction monitoring in positive electrospray ionisation mode with a special ReproSil 100 C 18 high-performance liquid chromatography column. This newly proposed method yielded good sensitivity and excellent chromatographic performance. The limits of quantification for kasugamycin and validamycin-A were 4.1 µg/kg and 1.0 µg/kg, respectively. The recoveries for both compounds at three fortification levels (4, 100 and 500 µg/kg for kasugamycin; 1, 10 and 100 µg/kg for validamycin-A) ranged from 75% to 110%, and the relative standard deviations were below 15%.

3D Printing and Assay Development for Point-of-Care Applications

Science.gov (United States)

Jagadeesh, Shreesha

Existing centralized labs do not serve patients adequately in remote areas. To enable universal timely healthcare, there is a need to develop low cost, portable systems that can diagnose multiple disease (Point-of-Care (POC) devices). Future POC diagnostics can be more multi-functional if medical device vendors can develop interoperability standards. This thesis developed the following medical diagnostic modules: Plasma from 25 microl blood was extracted through a filter membrane to demonstrate a 3D printed sample preparation module. Sepsis biomarker, C - reactive protein, was quantified through adsorption on nylon beads to demonstrate bead-based assay suitable for 3D printed disposable cartridge module. Finally, a modular fluorescent detection kit was built using 3D printed parts to detect CD4 cells in a disposable cartridge from ChipCare Corp. Due to the modularity enabled by 3D printing technique, the developed units can be easily adapted to detect other diseases.

Liquid chromatographic-diode-array detection multiresidue determination of rice herbicides in drinking and paddy-field water.

Science.gov (United States)

Roehrs, Rafael; Zanella, Renato; Pizzuti, Ionara; Adaime, Martha B; Pareja, Lucía; Niell, Silvina; Cesio, María V; Heinzen, Horacio

2009-01-01

A sensitive, rapid, and simple multiresidue method for the simultaneous determination of six postemergence herbicides currently used in rice cultivation--metsulfuron methyl, bensulfuron methyl, pyrazosulfuron ethyl, bentazone, bispyribac sodium, and cyhalofop butyl--in drinking and paddy-field water is presented. Water samples were extracted with solid-phase extraction cartridges. Final determination was made by LC with diode-array detection. The extraction efficiencies of C18 and HLB cartridges were compared. The average recovery obtained for these compounds for the lowest spiked level (0.1 microg/L) varied from 70 to 122% for C18 and 75-119% for HLB, with RSDs of 11 and 8.3%, respectively. The method had good linearity, and the lower detection limit for the pesticides studied varied from 0.03 to 0.04 microg/L. The proposed method was also tested in paddy-field water, with recovery studies giving good results with low RSDs at 1.0 microg/L.

IVGEN Post Flight Analysis

Science.gov (United States)

Mcquillen, John; Brown, Dan; Hussey, Sam; Zoldak, John

2014-01-01

consumption. Samples were generated and shipped to an FDA facility however, testing determined that the samples failed the TOC specification with most likely due to leaching from the sample container. Shelf life testing is examining packaging techniques and periodic testing of samples of DI cartridges that are capped and sealed in hermetic packages. Periodic testing of the purified water output will be conducted at six month intervals.

Fungos aeróbios no intestino grosso de borregos e de ovelhas criados em pastagens tropicais

Directory of Open Access Journals (Sweden)

C.E.S. Freitas

2012-02-01

Full Text Available Fungi populations were evaluated in large intestine from sheep raised in the North of Minas Gerais, Brazil. The samples were from 39 Santa Inês crossbred ewes and 30 lambs raised on Tanzania grass (Panicum maximum cv. Tanzania, both supplemented with mineral mixtures. The clinical specimens were directly collected from rectal ampoule with sterile swabs. The development of fungal mycelium was observed in all lamb samples and positive cultures were observed in 34 ewe specimens (87.2%. After microculture of 40 colonies from lambs, 34 isolates of the genus Aspergillus, three of Paecilomyces spp., one Acremonium sp., and one Trichoderma sp. were identified. Out of the 39 isolates from ewes, 15 Paecilomyces spp., 11 Aspergillus spp., 11 Malbranchea spp., and one Onychocola sp. were identified. The results showed the predominance of the genus Aspergillus in the lambs, while the genus Paecilomyces, Malbranchea, and Aspergillus were predominant, in ewes.

Leak test method for radioactive material packagings without pressure valve connections

International Nuclear Information System (INIS)

Johnson, S.F.; Stenbaeck, A.

1976-01-01

A leak test method has been developed at Studsvik which provides the possibility of testing Type B packagings unequipped with valves for evacuation or pressurizing. Even large packagings with pressure valve connections can be leak tested by this method. The method is a pressure test method. The test gas comprises a mixture of helium and nitrogen or helium and air. Excess pressure in a valveless packaging is achieved by vaporization of liquid nitrogen. All parts of the packaging or package where leaks might be expected are covered by plastic sheet. Samples of the gas accumulated under the plastic sheets are taken using evacuated glass ampoules which are initially sealed off to a breakable point. The gas samples are measured with a He-mass spectrometer. The sensitivity of this method of leak testing is, in practice, of the order of 10 -7 atmcm 3 s -1 . (author)

Capturing [11C]CO2 for use in aqueous applications

International Nuclear Information System (INIS)

Vandehey, Nicholas T.; O’Neil, James P.

2014-01-01

We present a simple method for trapping [ 11 C]CO 2 gas and releasing it into a buffered solution using an ion-exchange cartridge. Sodium hydroxide cartridges captured >99% of [ 11 C]CO 2 following NaOH activation. A sodium bicarbonate solution eluted >99% of trapped radioactivity. Trapping [ 11 C]CO 2 directly in small volumes of several solutions was less effective than cartridge methods. The recommended methods allow for fast and simple production of highly concentrated carbon-11 containing aqueous solutions for use in filling phantoms, calibrating detectors, or (bio)geochemical experiments. - Highlights: • An ion exchange resin can trap [ 11 C]CO 2 gas and release it with saturated bicarbonate. • Elution from cartridge requires as little as 300 µL volume, with eluant at pH=10. • SPE trap-and-release provided better results than trapping in solution

Evaluation of the i-STAT Portable Clinical Analyzer for point-of-care blood testing in the intensive care units of a university children's hospital.

Science.gov (United States)

Papadea, Christine; Foster, Joyce; Grant, Sharon; Ballard, Sandra A; Cate, John C; Southgate, W Michael; Purohit, Dilip M

2002-01-01

We evaluated the analytical performance of the i-STAT Portable Clinical Analyzer (PCA), a point-of-care testing system consisting of a hand-held analyzer and single-use cartridges that measure different panels of electrolytes, metabolites, blood gases, and hematocrit in 65-100 microl of blood. Our objective was to determine whether PCA measurements at the bedside of patients in the neonatal and pediatric intensive care units of the MUSC Children's Hospital would be as reliable as those performed by the clinical laboratory's primary methods (Radiometer ABL 725 blood gas analyzer; Vitros 750 chemistry analyzer; and Coulter STKS hematology analyzer). Four cartridge types: (a) EC8+ (sodium; potassium; chloride; urea; glucose; pH; blood gases [PO2; pCO2]), (b) EC6+ (sodium; potassium; ionized calcium; glucose; hematocrit; pH), (c) G3+ (pH; PO2; pCO2), and (d) creatinine, were assessed for reproducibility, linearity, and method comparisons using aqueous samples, blood samples supplemented with several analytes, and -225 blood samples from patients. Reproducibility (CV) was good ( or < 3 mo) showed that agreement between the PCA and the primary methods was clinically acceptable. After the PCA was implemented for clinical testing, the observation of discrepant results of creatinine concentrations in neonatal blood samples that would have affected clinical management led to a second creatinine comparison study (59 additional samples) and to our eventual discontinuation of the PCA creatinine assay. This problem notwithstanding, the successful implementation of the PCA is attributed to careful analytical evaluations and ongoing communication with the clinical staff.

Directional Solidification of Pure Succinonitrile and a Succinonitrile-Acetone Alloy

Science.gov (United States)

Simpson, James E.; deGroh, Henry C., III; Garimella, Suresh V.

2000-01-01

An experimental study of the horizontal Bridgman growth of pure succinonitrile (SCN) and of a succinonitrile-1.0 mol% acetone alloy (SCN-1.0 mol.% ACE) has been performed. Experiments involving both a stationary thermal field (no-growth case) and a translating thermal field (growth case) were conducted. Growth rates of 2 and 40 micrometers/sec were investigated. For the pure SCN experiments, the velocity field in the melt was estimated using video images of seed particles in the melt. Observations of the seed particles indicate that a primary longitudinal convective cell is formed. The maximum velocity of two different particles which traveled along similar paths was the same and equal to 1.49 +/- 0.01 mm/s. The general accuracy of velocity measurements is estimated to be +/-0.08 mm/s, though the data shows consistency to within +/- 0.02 mm/s. The shape of the solid/liquid interface was also quantitatively determined. The solid/liquid interface was stable (non-dendritic and non-cellular) but not flat: rather it was significantly distorted by the influence of connection in the melt and, for the growth case, by the moving temperature boundary conditions along the ampoule. It was found that the interface shape and position were highly dependent on the alignment of the ampoule in the apparatus. Consequently, the ampoule was carefully aligned for all experiments. The values for front location agree with those determined in previous experiments. For the alloy experiments, the solid/liquid interface was determined to be unstable at growth rates greater than 2.8 micrometers/sec, but stable for the cases of no-growth and growth at 2 micrometers/sec. When compared to the shape of the pure SCN interface, the alloy interface forms closer to the cold zone, indicating that the melting temperature decreased due to the alloying element. Extensive temperature measurements were performed on the outside of the ampoule containing pure SCN. The resulting thermal profiles are presented

Graft-copolymerization of styrene on polypropylene in the solid phase

NARCIS (Netherlands)

Beenen, W.; VanderWal, D.; Janssen, L.P.B.M.; Buijtenhuijs, A.; Hogt, A.H.; Wal, Douwe J. v.d.

The graft-copolymerization of styrene on PP in the solid phase has been studied under various reaction conditions using a radical initiator. Polymerization kinetics were investigated by DSC experiments and reactions in glass ampoules. The conversion rate and grafting efficiency of styrene appeared

Application of cation-exchange solid-phase extraction for the analysis of amino alcohols from water and human plasma for verification of Chemical Weapons Convention.

Science.gov (United States)

Kanaujia, Pankaj K; Tak, Vijay; Pardasani, Deepak; Gupta, A K; Dubey, D K

2008-03-28

The analysis of nitrogen containing amino alcohols, which are the precursors and degradation products of nitrogen mustards and nerve agent VX, constitutes an important aspect for verifying the compliance to the CWC (Chemical Weapons Convention). This work devotes on the development of solid-phase extraction method using silica- and polymer-based SCX (strong cation-exchange) and MCX (mixed-mode strong cation-exchange) cartridges for N,N-dialkylaminoethane-2-ols and alkyl N,N-diethanolamines, from water. The extracted analytes were analyzed by GC-MS (gas chromatography-mass spectrometry) in the full scan and selected ion monitoring modes. The extraction efficiencies of SCX and MCX cartridges were compared, and results revealed that SCX performed better. Extraction parameters, such as loading capacity, extraction solvent, its volume, and washing solvent were optimized. Best recoveries were obtained using 2 mL methanol containing 10% NH(4)OH and limits of detection could be achieved up to 5 x 10(-3) microg mL(-1) in the selected ion monitoring mode and 0.01 microg mL(-1) in full scan mode. The method was successfully employed for the detection and identification of amino alcohol present in water sample sent by Organization for Prohibition of Chemical Weapons (OPCW) in the official proficiency tests. The method was also applied to extract the analytes from human plasma. The SCX cartridge showed good recoveries of amino alcohols from human plasma after protein precipitation.

Assessment of an automated capillary system for Plasmodium vivax microsatellite genotyping.

Science.gov (United States)

Manrique, Paulo; Hoshi, Mari; Fasabi, Manuel; Nolasco, Oscar; Yori, Pablo; Calderón, Martiza; Gilman, Robert H; Kosek, Margaret N; Vinetz, Joseph M; Gamboa, Dionicia

2015-08-21

Several platforms have been used to generate the primary data for microsatellite analysis of malaria parasite genotypes. Each has relative advantages but share a limitation of being time- and cost-intensive. A commercially available automated capillary gel cartridge system was assessed in the microsatellite analysis of Plasmodium vivax diversity in the Peruvian Amazon. The reproducibility and accuracy of a commercially-available automated capillary system, QIAxcel, was assessed using a sequenced PCR product of 227 base pairs. This product was measured 42 times, then 27 P. vivax samples from Peruvian Amazon subjects were analyzed with this instrument using five informative microsatellites. Results from the QIAxcel system were compared with a Sanger-type sequencing machine, the ABI PRISM(®) 3100 Genetic Analyzer. Significant differences were seen between the sequenced amplicons and the results from the QIAxcel instrument. Different runs, plates and cartridges yielded significantly different results. Additionally, allele size decreased with each run by 0.045, or 1 bp, every three plates. QIAxcel and ABI PRISM systems differed in giving different values than those obtained by ABI PRISM, and too many (i.e. inaccurate) alleles per locus were also seen with the automated instrument. While P. vivax diversity could generally be estimated using an automated capillary gel cartridge system, the data demonstrate that this system is not sufficiently precise for reliably identifying parasite strains via microsatellite analysis. This conclusion reached after systematic analysis was due both to inadequate precision and poor reproducibility in measuring PCR product size.

Clinical evaluation of high-risk HPV detection on self-samples using the indicating FTA-elute solid-carrier cartridge

NARCIS (Netherlands)

Geraets, D.T.; Baars, R. van; Alonso, I.; Ordi, J.; Torne, A.; Melchers, W.J.G.; Meijer, C.J.W.; Quint, W.G.V.

2013-01-01

BACKGROUND: High-risk human papillomavirus (hrHPV) testing in cervical screening is usually performed on physician-taken cervical smears in liquid-based medium. However, solid-state specimen carriers allow easy, non-hazardous storage and transportation and might be suitable for self-collection by

Apparatus for filtering radioactive fluids

International Nuclear Information System (INIS)

Gischel, E.H.

1975-01-01

Apparatus is provided for filtering radioactive particles from the cooling and/or auxiliary process water of a nuclear reactor, or nuclear fuel processing plant, or other installations wherein radioactive fluid systems are known to exist. The apparatus affords disposal of the captured particles in a manner which minimizes the exposure of operating personnel to radioactivity. The apparatus comprises a housing adapted to contain a removable filter cartridge assembly, a valve normally closing the lower end of the housing, an upwardly-open shipping cask located below the valve, and an elongated operating rod assembly projecting upwardly from the filter cartridge assembly and through the upper end of the housing to enable a workman to dismount the filter cartridge assembly from its housing and to lower the filter cartridge assembly through the valve and into the cask from a remote location above the housing. (U.S.)

Evaluation of ultrasound-assisted extraction as sample pre-treatment for quantitative determination of rare earth elements in marine biological tissues by inductively coupled plasma-mass spectrometry

International Nuclear Information System (INIS)

Costas, M.; Lavilla, I.; Gil, S.; Pena, F.; Calle, I.; Cabaleiro, N. de la; Bendicho, C.

2010-01-01

In this work, the determination of rare earth elements (REEs), i.e. Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu in marine biological tissues by inductively coupled-mass spectrometry (ICP-MS) after a sample preparation method based on ultrasound-assisted extraction (UAE) is described. The suitability of the extracts for ICP-MS measurements was evaluated. For that, studies were focused on the following issues: (i) use of clean up of extracts with a C18 cartridge for non-polar solid phase extraction; (ii) use of different internal standards; (iii) signal drift caused by changes in the nebulization efficiency and salt deposition on the cones during the analysis. The signal drift produced by direct introduction of biological extracts in the instrument was evaluated using a calibration verification standard for bracketing (standard-sample bracketing, SSB) and cumulative sum (CUSUM) control charts. Parameters influencing extraction such as extractant composition, mass-to-volume ratio, particle size, sonication time and sonication amplitude were optimized. Diluted single acids (HNO 3 and HCl) and mixtures (HNO 3 + HCl) were evaluated for improving the extraction efficiency. Quantitative recoveries for REEs were achieved using 5 mL of 3% (v/v) HNO 3 + 2% (v/v) HCl, particle size <200 μm, 3 min of sonication time and 50% of sonication amplitude. Precision, expressed as relative standard deviation from three independent extractions, ranged from 0.1 to 8%. In general, LODs were improved by a factor of 5 in comparison with those obtained after microwave-assisted digestion (MAD). The accuracy of the method was evaluated using the CRM BCR-668 (mussel tissue). Different seafood samples of common consumption were analyzed by ICP-MS after UAE and MAD.

76 FR 57719 - Procurement List; Proposed Additions

Science.gov (United States)

2011-09-16

... proposed for addition to the Procurement List for production by the nonprofit agencies listed: Products NSN: 7930-00-NIB-0583--Refills, Bathroom Cleaner and Deodorizer, Cartridge Concentrate. NSN: 7930-00-NIB-0584--Starter Kit, Bathroom Cleaner and Deodorizer, Cartridge Concentrate. NSN: 7930-00-NIB-0585...

76 FR 35744 - Amendments to National Emission Standards for Hazardous Air Pollutants for Area Sources: Plating...

Science.gov (United States)

2011-06-20

... Metal Valve and Pipe Fitting Manufacturing; 332999, All Other Miscellaneous Fabricated Metal Product... spraying operation and exhaust them to a water curtain, or a cartridge, fabric, or HEPA filter... from the thermal spraying operation and exhaust them to a cartridge, fabric, or HEPA filter...

Study on the extraction, purification and quantification of jasmonic acid, abscisic acid and indole-3-acetic acid in plants.

Science.gov (United States)

Zhang, Feng Juan; Jin, You Ju; Xu, Xing You; Lu, Rong Chun; Chen, Hua Jun

2008-01-01

Jasmonic acid (JA), abscisic acid (ABA) and indole-3-acetic acid (IAA) are important plant hormones. Plant hormones are difficult to analyse because they occur in small concentrations and other substances in the plant interfere with their detection. To develop a new, inexpensive procedure for the rapid extraction and purification of IAA, ABA and JA from various plant species. Samples were prepared by extraction of plant tissues with methanol and ethyl acetate. Then the extracts were further purified and enriched with C(18) cartridges. The final extracts were derivatised with diazomethane and then measured by GC-MS. The results of the new methodology were compared with those of the Creelman and Mullet procedure. Sequential elution of the assimilates from the C(18 )cartridges revealed that IAA and ABA eluted in 40% methanol, while JA subsequently eluted in 60% methanol. The new plant hormone extraction and purification procedure produced results that were comparable to those obtained with the Creelman and Mullet's procedure. This new procedure requires only 0.5 g leaf samples to quantify these compounds with high reliability and can simultaneously determine the concentrations of the three plant hormones. A simple, inexpensive method was developed for determining endogenous IAA, ABA and JA concentrations in plant tissue.

Irradiation of lithium aluminate and tritium extraction

International Nuclear Information System (INIS)

Roth, E.; Abassin, J.J.; Botter, F.; Briec, M.; Chenebault, P.; Masson, M.; Rasneur, B.; Roux, N.

1984-12-01

After preselection of the preparation procedures, following short irradiations, γ LiAl0 2 samples submitted to 2.10 19 fast neutrons cm -2 and 1.5 10 20 thermal neutrons cm -2 fluences experienced no apparent damage. Post-irradiation tritium extraction from samples irradiated to 2.10 17 neutrons/cm 2 in quartz ampoules produced mostly tritiated water. When in-pile experiments are performed the sample container material influences greatly the measured ratio of tritium gas to tritiated water - Stainless steel capsules yield more T 2 gas than quartz capsules probably because of a reduction process. Difficulties in interpretation arise from adsoption of tritiated water on the measuring lines. Both experiments showed that much faster extraction rates are obtained from small grain size samples than from large ones at the same open porosity. If diffusion in the grains controls the extraction rates, apparent D values vary from 10 -16 to 1.5 10 -15 cm 2 S -1 in the temperature range explored. Around 500 0 C small grain samples reached equilibrium tritium concentration of a few mCi in 4 hours. Such values are suitable for a blanket concept

Sample size estimation and sampling techniques for selecting a representative sample

Directory of Open Access Journals (Sweden)

Aamir Omair

2014-01-01

Full Text Available Introduction: The purpose of this article is to provide a general understanding of the concepts of sampling as applied to health-related research. Sample Size Estimation: It is important to select a representative sample in quantitative research in order to be able to generalize the results to the target population. The sample should be of the required sample size and must be selected using an appropriate probability sampling technique. There are many hidden biases which can adversely affect the outcome of the study. Important factors to consider for estimating the sample size include the size of the study population, confidence level, expected proportion of the outcome variable (for categorical variables/standard deviation of the outcome variable (for numerical variables, and the required precision (margin of accuracy from the study. The more the precision required, the greater is the required sample size. Sampling Techniques: The probability sampling techniques applied for health related research include simple random sampling, systematic random sampling, stratified random sampling, cluster sampling, and multistage sampling. These are more recommended than the nonprobability sampling techniques, because the results of the study can be generalized to the target population.

76 FR 57913 - Amendments to National Emission Standards for Hazardous Air Pollutants for Area Sources: Plating...

Science.gov (United States)

2011-09-19

... Fixture Fitting and Trim Manufacturing; Other Metal Valve and Pipe Fitting Manufacturing; 332999, All... thermal spraying operation and exhaust them to a water curtain, or a cartridge, fabric, or HEPA filter... from the thermal spraying operation and exhaust them to a cartridge, fabric, or HEPA filter...

Activation analysis of copper in foodstuffs after their partial destruction

International Nuclear Information System (INIS)

Jiranek, V.; Bludovsky, R.

1978-01-01

The samples analyzed (0.1 to 0.8 g) and the standards were irradiated for 24 hours with thermal neutrons (2x10 12 n/cm 2 s), the ampoules were opened 2 hours after irradiation, 1 mg of non-active Cu carrier was added and the samples were mineralized for about 15 to 20 mins at 600 degC. The ash was leached with 5 ml of hot 10% HCl and following neutralization with ammonia and dilution with 20 ml of 10 -3 M HCl, 10 ml of an α-benzoineoxime (2 g), pyridine (100 ml) and chloroform (900 ml) mixture was extracted at pH>=2. The extract was used for measuring radioactivity (6 hours after irradiation) and for spectrophotometric determination of the separation yield by the reverse IDA method (600 nm). The least measurable amount was 10 -9 g, the standard deviation +-3.5%, the simultaneous processing of 20 samples took about 3 hours. With this method the results have higher values than with nonradiometric procedures burdened with a systematic error due to Cu losses. (M.K.)

Development of a gas chromatography-mass spectrometry method for the determination of pesticides in gaseous and particulate phases in the atmosphere.

Science.gov (United States)

Borrás, E; Sánchez, P; Muñoz, A; Tortajada-Genaro, L A

2011-08-05

A reliable multi-residue method for determining gaseous and particulate phase pesticides in atmospheric samples has been developed. This method, based on full scan gas chromatography-mass spectrometry (GC-MS), allowed the proper determination of sixteen relevant pesticides, in a wide range of concentrations and without the influence of interferences. The pesticides were benfluralin, bitertanol, buprofezin, chlorfenvinphos, chlorpyrifos, chlorpyrifos-methyl, ethalfluralin, fenthion, lindane, malathion, methidathion, propachlor, propanil, pyriproxifen, tebuconazol and trifluralin. Comparisons of two types of sampling filters (quartz and glass fibre) and four types of solid-phase cartridges (XAD-2, XAD-4, Florisil and Orbo-49P) showed that the most suitable supports were glass fibre filter for particulate pesticides and XAD-2 and XAD-4 cartridges for gaseous pesticides (>95% recovery). Evaluations of elution solvents for ultrasonic-assisted extraction demonstrated that isooctane is better than ethylacetate, dichloromethane, methanol or a mixture of acetone:hexane (1:1). Recovery assays and the standard addition method were performed to validate the proposed methodology. Moreover, large simulator chamber experiments allowed the best study of the gas-particle partitioning of pesticides for testing the sampling efficiency for the validation of an analytical multiresidue method for pesticides in air. Satisfactory analytical parameters were obtained, with a repeatability of 5±1%, a reproducibility of 13±3% and detection limits of 0.05-0.18 pg m(-3) for the particulate phase and 26-88 pg m(-3) for the gaseous phase. Finally, the methodology was successfully applied to rural and agricultural samples in the Mediterranean area. Copyright © 2011 Elsevier B.V. All rights reserved.

Experimental verification of agreement between thermal and real time visual melt-solid interface positions in vertical Bridgman grown germanium

Science.gov (United States)

Barber, P. G.; Fripp, A. L.; Debnam, W. J.; Woodell, G.; Berry, R. F.; Simchick, R. T.

1996-03-01

Measurements of the liquid-solid interface position during crystal growth were made by observing the discontinuity of the temperature gradient with movable thermocouples in a centerline, quartz capillary placed inside a sealed quartz ampoule of germanium in a vertical Bridgman furnace. Simultaneously, in situ, real time visual observations, using X-ray imaging technology, determined the position of the melt-solid interface. The radiographically detected interface position was several millimeters from the thermal interface position and the direction of displacement depended upon the direction of thermocouple insertion. Minimization of this spurious heat flow was achieved by using an unclad thermocouple that had each of its two wire leads entering the capillary from different ends of the furnace. Using this configuration the visual interface coincided with the thermal interface. Such observations show the utility of using in situ, real time visualization to record the melt-solid interface shape and position during crystal growth; and they suggest improvements in furnace and ampoule designs for use in high thermal gradients.

Determination of the Wetting Angle of Germanium and Germanium-Silicon Melts on Different Substrate Materials

Science.gov (United States)

Kaiser, Natalie; Croell, Arne; Szofran, F. R.; Cobb. S. D.; Dold, P.; Benz, K. W.

1999-01-01

During Bridgman growth of semiconductors detachment of the crystal and the melt meniscus has occasionally been observed, mainly under microgravity (microg) conditions. An important factor for detached growth is the wetting angle of the melt with the crucible material. High contact angles are more likely to result in detachment of the growing crystal from the ampoule wall. In order to achieve detached growth of germanium (Ge) and germanium-silicon (GeSi) crystals under 1g and microg conditions, sessile drop measurements were performed to determine the most suitable ampoule material as well as temperature dependence of the surface tension for GeSi. Sapphire, fused quartz, glassy carbon, graphite, SiC, pyrolytic Boron Nitride (pBN), AIN, and diamond were used as substrates. Furthermore, different cleaning procedures and surface treatments (etching, sandblasting, etc.) of the same substrate material and their effect on the wetting behavior were studied during these experiments. pBN and AIN substrates exhibited the highest contact angles with values around 170 deg.

Quantitative estimation of diphtheria and tetanus toxoids. 4. Toxoids as international reference materials defining Lf-units for diphtheria and tetanus toxoids.

Science.gov (United States)

Lyng, J

1990-01-01

The Lf-unit, which is used in the control of diphtheria and tetanus toxoid production and in some countries also to follow immunization of horses for production of antitoxins, has hitherto been defined by means of antitoxin preparations. A diphtheria toxoid and a tetanus toxoid preparation, both freeze-dried, were examined in an international collaborative study for their suitability to serve as reference reagents in the flocculation tests and for defining the Lf-units. It was shown that flocculation tests using the reference toxoids are very reproducible and reliable and the WHO Expert Committee on Biological Standardization established: the toxoid called DIFT as the International Reference Reagent of Diphtheria Toxoid for Flocculation Test with a defined content of 900 Lf-units of diphtheria toxoid per ampoule; and the toxoid called TEFT as the International Reference Reagent of Tetanus Toxoid for Flocculation Test with a defined content of 1000 Lf-units of diphtheria toxoid per ampoule.

PAT-1 safety analysis report addendum.

Energy Technology Data Exchange (ETDEWEB)

Weiner, Ruth F.; Schmale, David T.; Kalan, Robert J.; Akin, Lili A.; Miller, David Russell; Knorovsky, Gerald Albert; Yoshimura, Richard Hiroyuki; Lopez, Carlos; Harding, David Cameron; Jones, Perry L.; Morrow, Charles W.

2010-09-01

The Plutonium Air Transportable Package, Model PAT-1, is certified under Title 10, Code of Federal Regulations Part 71 by the U.S. Nuclear Regulatory Commission (NRC) per Certificate of Compliance (CoC) USA/0361B(U)F-96 (currently Revision 9). The purpose of this SAR Addendum is to incorporate plutonium (Pu) metal as a new payload for the PAT-1 package. The Pu metal is packed in an inner container (designated the T-Ampoule) that replaces the PC-1 inner container. The documentation and results from analysis contained in this addendum demonstrate that the replacement of the PC-1 and associated packaging material with the T-Ampoule and associated packaging with the addition of the plutonium metal content are not significant with respect to the design, operating characteristics, or safe performance of the containment system and prevention of criticality when the package is subjected to the tests specified in 10 CFR 71.71, 71.73 and 71.74.

A Modern Apparatus for Performing Flash Chromatography: An Experiment for the Organic Laboratory

Science.gov (United States)

Naumiec, Gregory R.; Del Padre, Angela N.; Hooper, Matthew M.; Germaine, Alison St.; DeBoef, Brenton

2013-01-01

A modern apparatus for performing flash chromatography using commercially available, prepacked silica cartridges has been developed. The key advantage of this system, when compared to traditional flash chromatography, is its use of commercially available silica cartridges, which obviates the need for students to handle silica gel. The apparatus…

Analysis of urinary neurotransmitters by capillary electrophoresis: Sensitivity enhancement using field-amplified sample injection and molecular imprinted polymer solid phase extraction

International Nuclear Information System (INIS)

Claude, Berengere; Nehme, Reine; Morin, Philippe

2011-01-01

of the FASI/CE-UV method.Therefore, a solid phase extraction (SPE) on a dedicated imprinted polymer (MIP) was developed to extract specific neurotransmitters, catecholamines, metanephrines and indolamines, from urine. Matrix salts were thus discarded after sample extraction on AFFINIMIP TM Catecholamine and Metanephrine (100 mg) cartridge. Therefore, lower limits of quantification were determined in artificial urine (46 nmol L -1 for DA, 11 nmol L -1 for 3-MT and 6 nmol L -1 for 5-HT).The application of this protocol MIP-SPE/FASI-CE-UV analysis of neurotransmitters in human urine gave rise to electropherograms with a very good base line and signal to noise ratios above 15.

Analysis of urinary neurotransmitters by capillary electrophoresis: Sensitivity enhancement using field-amplified sample injection and molecular imprinted polymer solid phase extraction

Energy Technology Data Exchange (ETDEWEB)

Claude, Berengere, E-mail: berengere.claude@univ-orleans.fr [Institut de Chimie Organique et Analytique, CNRS FR 2708 UMR 6005, Universite d' Orleans, 45067 Orleans (France); Nehme, Reine; Morin, Philippe [Institut de Chimie Organique et Analytique, CNRS FR 2708 UMR 6005, Universite d' Orleans, 45067 Orleans (France)

2011-08-12

neurotransmitters in urine, the presence of salts in the matrix greatly reduces the sensitivity of the FASI/CE-UV method.Therefore, a solid phase extraction (SPE) on a dedicated imprinted polymer (MIP) was developed to extract specific neurotransmitters, catecholamines, metanephrines and indolamines, from urine. Matrix salts were thus discarded after sample extraction on AFFINIMIP{sup TM} Catecholamine and Metanephrine (100 mg) cartridge. Therefore, lower limits of quantification were determined in artificial urine (46 nmol L{sup -1} for DA, 11 nmol L{sup -1} for 3-MT and 6 nmol L{sup -1} for 5-HT).The application of this protocol MIP-SPE/FASI-CE-UV analysis of neurotransmitters in human urine gave rise to electropherograms with a very good base line and signal to noise ratios above 15.

Matrix solid-phase dispersion on column clean-up/pre-concentration as a novel approach for fast isolation of abuse drugs from human hair.

Science.gov (United States)

Míguez-Framil, Martha; Moreda-Piñeiro, Antonio; Bermejo-Barrera, Pilar; Alvarez-Freire, Iván; Tabernero, María Jesús; Bermejo, Ana María

2010-10-08

A simple and fast sample pre-treatment method based on matrix solid-phase dispersion (MSPD) for isolating cocaine, benzoylecgonine (BZE), codeine, morphine and 6-monoacethylmorphine (6-MAM) from human hair has been developed. The MSPD approach consisted of using alumina (1.80 g) as a dispersing agent and 0.6M hydrochloric acid (4 mL) as an extracting solvent. For a fixed hair sample mass of 0.050 g, the alumina mass to sample mass ratio obtained was 36. A previously conditioned Oasis HLB cartridge (2 mL methanol, plus 2 mL ultrapure water, plus 1 mL of 0.2M/0.2M sodium hydroxide/boric acid buffer solution at pH 9.2) was attached to the end of the MSPD syringe for on column clean-up of the hydrochloric acid extract and for transferring the target compounds to a suitable solvent for gas chromatography (GC) analysis. Therefore, the adsorbed analytes were directly eluted from the Oasis HLB cartridges with 2 mL of 2% acetic acid in methanol before concentration by N(2) stream evaporation and dry extract derivatization with N-methyl-tert-butylsilyltrifluoroacetamide (BSTFA) and chlorotrimethylsilane (TMCS). The optimization/evaluation of all the factors affecting the MSPD and on column clean-up procedures has led to a fast sample treatment, and analytes extraction and pre-concentration can be finished in approximately 30 min. The developed method has been applied to eight hair samples from poli-drug abusers and measured analyte concentrations have been found to be statistically similar (95% confidence interval) to those obtained after a conventional enzymatic hydrolysis method (Pronase E). Copyright © 2010. Published by Elsevier B.V.

Dual solid-phase and stir bar sorptive extraction combined with gas chromatography-mass spectrometry analysis provides a suitable tool for assaying limonene-derived mint aroma compounds in red wine.

Science.gov (United States)

Picard, Magali; Franc, Céline; de Revel, Gilles; Marchand, Stéphanie

2018-02-25

A novel analytical method was developed for quantitative determination of eight limonene-derived monoterpenes responsible for the mint aroma in red wine. As these aromatic compounds are present at trace levels, a new dual extraction approach was proposed, combining solid-phase extraction (SPE) and stir bar sorptive extraction (SBSE), followed by gas chromatography-mass spectrometry analysis. The various parameters affecting the efficiency of extracting the analytes from wine samples in both the SPE and SBSE steps were first investigated, to determine the best compromise for the simultaneous analysis of the compounds studied. Following preliminary optimization of the dilution factor, phase ratio, and methanol content in the SBSE sample, cartridge sorbent mass, type of solvent, elution volume, and wine sample volume in the pre-concentration SPE step were studied. Highest response values were obtained when a 90 mL wine sample was extracted on a 500 mg SPE C18 cartridge and eluted with 1.5 mL methanol. The wine extract was then diluted in 10 mL water to obtain a final methanol content of 15% before the SBSE step. Good linearity, repeatability, reproducibility, accuracy and the required low detection and quantification limits were obtained under the conditions described, making this SPE-SBSE combination a suitable, powerful tool for routine analysis of the selected limonene-derived mint aroma compounds in large series of wine samples. Finally, the validated method was applied to 15 commercial red Bordeaux wines, aged from 3 to 23 years. Most of the compounds studied, present within the ng.L -1 range, were easily quantified for the first time in wine. Copyright © 2017 Elsevier B.V. All rights reserved.

Simultaneous determination of residues of emamectin and its metabolites, and milbemectin, ivermectin, and abamectin in crops by liquid chromatography with fluorescence detection.

Science.gov (United States)

Yoshii, K; Kaihara, A; Tsumura, Y; Ishimitsu, S; Tonogai, Y

2001-01-01

A liquid chromatographic (LC) method was developed for the determination of emamectin and its metabolites (8,9-Z-isomer, N-demethylated, N-formylated, and N-methylformylated emamectin) in various crops. The analytes were extracted with acetone, cleaned up on cartridge columns (C18 and NH2), derivatized with trifluoroacetic anhydride and 1-methylimidazole, and determined by LC with fluorescence detection. Because radish inhibited the formation of the fluorescent derivatives, an additional Bond Elut PRS cartridge was used in the cleanup of Japanese radish samples. During sample preparation, N-formylated emamectin partially degraded to emamectin B1b and emamectin B1a, and the 8,9-Z-isomer partially degraded to N-demethylated emamectin. Therefore, emamectin and its metabolites were determined as total emamectin, i.e., their sum was estimated as emamectin benzoate. Their recoveries from most crops were approximately 80-110% with the developed method. The detection limits for the analytes in vegetables were 0.1-0.3 parts per trillion (ppt). The results for these compounds were confirmed by LC/mass spectrometry (LC/MS; electrospray ionization mode). Because the fluorescent derivative of emamectin was undetectable by LC/MS, the results for the analyte were confirmed by using a sample solution without derivatization. Limits of detection by LC/MS were similar to the fluorescence detection limits, 0.1-0.3 ppt in vegetables. In addition to the emamectins, milbemectin, ivermectin, and abamectin were also determined by the developed method.

Preconcentration of plutonium radionuclides from natural waters

International Nuclear Information System (INIS)

Wong, K.M.; Nioshkin, V.E.; Jokela, T.A.

1978-02-01

A large volume water sampler using manganese dioxide impregnated cartridges for the in situ separation of plutonium in sea water and ground water was studied. Plutonium concentrations obtained by this technique are compared with a radiochemical coprecipitation method. Consistent results were obtained between the two methods for water samples from the Pacific Ocean and Enewetak lagoon. Different results were noted from samples collected in the Enewetak reef and ground water stations. Using this preconcentration technique and the coprecipitation method it was shown that the physical-chemical characteristics of Pu in Enewetak reef and ground water are different from the lagoon and open ocean

Automated solid-phase extraction of herbicides from water for gas chromatographic-mass spectrometric analysis

Science.gov (United States)

Meyer, M.T.; Mills, M.S.; Thurman, E.M.

1993-01-01

An automated solid-phase extraction (SPE) method was developed for the pre-concentration of chloroacetanilide and triazine herbicides, and two triazine metabolites from 100-ml water samples. Breakthrough experiments for the C18 SPE cartridge show that the two triazine metabolites are not fully retained and that increasing flow-rate decreases their retention. Standard curve r2 values of 0.998-1.000 for each compound were consistently obtained and a quantitation level of 0.05 ??g/l was achieved for each compound tested. More than 10,000 surface and ground water samples have been analyzed by this method.

Snubber assembly for a control rod drive

International Nuclear Information System (INIS)

1976-01-01

A snubber cartridge assembly is described which is mounted to the nozzle of a control rod drive mechanism to insure that it will be located within the liquid filled section of a nuclear reactor vessel whenever the control rod drive is assembled thereto. The snubber assembly includes a piston-mounted proximate to the control rod connecting end of the control rod drive leadscrew to allow the piston to travel within the liquid filled snubber cartridge and controllable exhaust the liquid during a 'scram' condition. The snubber cartridge provides three separate areas of increasing resistance to piston travel to insure a speedy but safe 'scram' of the control rod into the reactor

Snubber assembly for a control rod drive

International Nuclear Information System (INIS)

Matthews, J.C.

1978-01-01

A snubber cartridge assembly is mounted to the nozzle of a control rod drive mechanism to insure that the snubber assembly will be located within the liquid filled section of a nuclear reactor vessel whenever the control rod drive is assembled thereto. The snubber assembly includes a piston mounted proximate to the control rod connecting end of the control rod drive leadscrew to allow the piston to travel within the liquid filled snubber cartridge and controllably exhaust liquid therefrom during a ''scram'' condition. The snubber cartridge provides three separate areas of increasing resistance to piston travel to insure a speedy but safe ''scram'' of the control rod into the reactor

Development of a radiochemical method for analyzing radon gas in uranium mine atmospheres: covering the period February 3, 1975--March 31, 1976

Energy Technology Data Exchange (ETDEWEB)

Stein, L.; Shearer, J.A.; Hohorst, F.A.; Markun, F.

1977-01-14

A simplified radiochemical method has been developed for quantitatively analyzing radon gas in underground uranium mines. In this method, a measured volume of air is drawn by a pump through a drying tube and a cartridge containing dioxygenyl hexafluoroantimonate reagent. Radon is captured as a nonvolatile product. After radioactive equilibrium has been established between radon and its short-lived daughters (approximately 4 hours), the gamma-emission of the cartridge is measured with a scintillation counter. The amount of radon is then calculated from the gamma-emission rate. The effect of cartridge geometry, reagent load, and air flow rate upon collection efficiency and counting efficiency is reported.

Development of a radiochemical method for analyzing radon gas in uranium mine atmospheres: covering the period February 3, 1975--March 31, 1976

International Nuclear Information System (INIS)

Stein, L.; Shearer, J.A.; Hohorst, F.A.; Markun, F.

1977-01-01

A simplified radiochemical method has been developed for quantitatively analyzing radon gas in underground uranium mines. In this method, a measured volume of air is drawn by a pump through a drying tube and a cartridge containing dioxygenyl hexafluoroantimonate reagent. Radon is captured as a nonvolatile product. After radioactive equilibrium has been established between radon and its short-lived daughters (approximately 4 hours), the gamma-emission of the cartridge is measured with a scintillation counter. The amount of radon is then calculated from the gamma-emission rate. The effect of cartridge geometry, reagent load, and air flow rate upon collection efficiency and counting efficiency is reported

original articles

African Journals Online (AJOL)

prevention of postpartum haemorrhage. Potential side-effects, however, need to be quantified. Objective. ... Postpartum blood loss irl the first hour was measured by collection irl a special flat plastic bedpan. Setting. ... to use intramuscular Syntometrine 1 ampoule or oxytocin. 10 ill, or in more severe cases an intravenous ...

Bulletin of Materials Science | Indian Academy of Sciences

Indian Academy of Sciences (India)

Many antimonide (Sb) crystals of 8 mm to 18 mm diameter were grown by optimized growth parameters. The forced convection and absence of conducting support to ampoule showed improvement in crystal quality of as grown ingots. Crystals showed preferred orientation and self-seeding. Results on interface shape and ...

How to prevent and treat an allergic crisis

African Journals Online (AJOL)

of appropriate discharge medications, instructions and follow-up. Before discharge the following strategies for the prevention and treatment of anaphylaxis should be implemented: • Medical care. • Provision of self-injectable adrenaline from an auto-injector is a preferable option to self-injectable adrenaline from an ampoule ...

Study of methodologies for quality control of 99Mo used in 99Mo/99mTc generators

International Nuclear Information System (INIS)

Said, Daphne de Souza

2016-01-01

99m Tc is the most used radionuclide in nuclear medicine. In Brazil, the 99 Mo/ 99m Tc generators are exclusively produced by Radiopharmacy Center at IPEN-CNEN/ SP, by importing 99 Mo from different suppliers. 99 Mo (t 1/2 = 66 h) is a fission product of 235 U and it can have radionuclidic impurities that are prejudicial for human health. For safe use of generators, it is necessary to perform the evaluation of 99 Mo by quality control tests in order to assess if 99 Mo complies with the specifications. The European Pharmacopoeia (EP) presents a monograph for evaluation of the quality of the [ 99 Mo] solution as sodium molybdate,that is used as raw material for 99 Mo/ 99m Tc generators production, including specification parameters (identification, radiochemical purity and radionuclidic purity), analysis methods and limits. However, it has been observed difficulties on the execution and implementation of these methods by the generators producers, with a few literature about this subject, probably due to complexity of the proposed methods. In this work, many quality control parameters of 99 Mo described in the EP monograph were evaluated. Separation methods for 99M o from its radionuclidic impurities by solid phase extraction (SPE) and TLC were studied. After SPE separation, the quantification of metals by ICP-OES to evaluate the percentage of retention of Mo and the percentage of recovery of Ru, Te and Sr using different types of cartridges were proposed, replacing radiotracers use. It was observed that the specific type of SPE cartridge recommended by the EP for separation of 99 Mo presented low recoveries for Ru, compared to other available anion exchange SPE cartridges. 99 Mo samples from different worldwide suppliers were analyzed. It was observed that quantification of 103 Ru in 99 Mo samples with decay time higher than 4 weeks is possible. An alternative method for separation of 131 I from 99 Mo showed promising results by TLC. The quantification of beta and

Studies on the ageing of a magnesium-strontium nitrate pyrotechnic composition using isothermal microcalorimetry and thermal analysis techniques

International Nuclear Information System (INIS)

Tuukkanen, I.; Brown, S.D.; Charsley, E.L.; Goodall, S.J.; Rooney, J.J.; Griffiths, T.T.; Lemmetyinen, H.

2004-01-01

The ageing behaviour of a pyrotechnic composition containing equal parts by mass of magnesium and strontium nitrate has been followed by isothermal microcalorimetry. The measurements were carried out on the samples at 50 deg. C and 65% relative humidity in air using closed ampoules. The results have been compared to those obtained for magnesium powder under the same conditions. Following an initial induction period, the pyrotechnic compositions reacted at a much faster rate than magnesium powder alone. The main reaction products were found to be magnesium hydroxide and strontium nitrite; the amounts formed have been correlated with the cumulative heats of ageing. In addition, the influence of the ageing process on the pyrotechnic reaction has been studied by high temperature differential scanning calorimetry (DSC) and by modulated temperature DSC

A highly rationalized procedure of neutron activation analysis for routine applications in dairy science

International Nuclear Information System (INIS)

Heine, K.; Wiechen, A.

1976-01-01

A rational procedure was developed for the multi-element analysis by neutron activation for applications in dairy science. The preparation of samples prior to irradiation consists of drying, weighing, and welding in quartz ampoules. The neutron flux, samples are exposed to during reactor irradiation , is determined by the mono-comparator technique for which the Co-content of a commercial aluminium foil was chosen as the flux monitor. Constancy of the Co-content and uncomplicated handling of the foil essentially simplify the determination of flux. The samples are irradiated for 72 h, dissolved in HNO 3 /H 2 SO 4 and measured in the liquid state after waiting times of 1-2, 4 and 8 weeks by a Ge(Li)-detector and a 4,096 channel spectrometer. The procedure was confirmed by investigations of the biological KALE standard and by participation in inter-comparisons of biological substances of the Analytical Quality Control Service of the IAEA for the analysis of the elements Na, Ca, Cr, Fe, Co, Zn, Se, Rb, and Cs. So a procedure was developed suitable for routine multi-element analysis of biologic samples by optimizing and rationalizing all analytical steps. (orig./MG) [de

49 CFR 176.84 - Other requirements for stowage and segregation for cargo vessels and passenger vessels.

Science.gov (United States)

2010-10-01

... persons on passenger vessels. 94 Plastic jerricans and plastic drums not permitted under deck. 95 Stow... Stowage category “04” for projectiles or cartridges for guns, cannons or mortars; Stowage category “08... projectiles or cartridges for guns, cannons or mortars; Stowage category “07” for other types; magazines must...

40 CFR 63.11511 - What definitions apply to this subpart?

Science.gov (United States)

2010-07-01

... detonation gun spraying. Water curtain means a type of control device that draws the exhaust stream through a... emissions points and then convey the captured gas stream to a control device, as part of a complete control..., plenums, and fans. Cartridge filter means a type of control device that uses perforated metal cartridges...

Data acquisition system for the Hamilton Standard W2 Electron Beam Welder

International Nuclear Information System (INIS)

Hopwood, J.

1979-06-01

A data acquisition system has been designed which will perform on-line weld-parameter sampling. It is a microprocessor-based program controller and calculator. The parameters sampled are beam current, accelerating voltage, focus-coil current, workpiece rpm, and filament voltage. Sampling in analog form occurs in pre-selected angular-rotation increments from 1 to 9 degrees. There are three data printout options: (A) all data displayed; (B) only out-of-tolerance values displayed; and (C) differences between nominal and sampled values in excess of preselected error bands displayed. A magnetic tape cartridge unit allows long-term data storage and easy retrieval. This report is a manual for system operation. It also describes the design--logic principles, circuitry, and programming--in detail

Data acquisition system for the Hamilton Standard W2 Electron Beam Welder

Energy Technology Data Exchange (ETDEWEB)

Hopwood, J.

1979-06-01

A data acquisition system has been designed which will perform on-line weld-parameter sampling. It is a microprocessor-based program controller and calculator. The parameters sampled are beam current, accelerating voltage, focus-coil current, workpiece rpm, and filament voltage. Sampling in analog form occurs in pre-selected angular-rotation increments from 1 to 9 degrees. There are three data printout options: (A) all data displayed; (B) only out-of-tolerance values displayed; and (C) differences between nominal and sampled values in excess of preselected error bands displayed. A magnetic tape cartridge unit allows long-term data storage and easy retrieval. This report is a manual for system operation. It also describes the design--logic principles, circuitry, and programming--in detail.

Determination of diacylhydrazines-type insect growth regulator JS-118 residues in cabbage and soil by high performance liquid chromatography with DAD detection.

Science.gov (United States)

Hu, J-Y; Deng, Z-B; Qin, D-M

2009-12-01

JS-118 is a diacylhydrazines-type insect growth regulator used extensively in China now. An analytical method for residues determination of JS-118 in cabbage and soil samples by high performance liquid chromatography with DAD detection was established and optimized. Primary secondary amine solid phase extraction cartridge was used for sample preparation. Mean recoveries for the analyte ranged from 96.6% to 107.0% with CV value less than 4.7%. The limit of quantification is 0.01 mg/kg. Direct confirmation of JS-118 residues in samples was realized by high performance liquid chromatography-mass spectrometry. The proposed method is simple, rapid and reliable to perform and could be utilized for monitoring of pesticides residues.

Uncovering the method of production and detection of synthetic acetic acid adulteration in vinegar by tandem use of 14C liquid scintillation counting and 13C/12C ratio mass spectrometry

International Nuclear Information System (INIS)

Wechner, Stefan; Voropaev, Andrey; Eichinger, Lorenz; Santos, Flora L.; Castaneda, Soledad; Racho, Michael; Pabroa, Preciosa Corazon; Morco, Ryan; Sucgang, Raymond J.

2010-01-01

Fraudulent adulteration and or misrepresentation had been a problem for commercial vinegar in the Philippines. Solutions of synthetic acetic acid mixed with colorants and flavour enhancers have been marketed as v inegar . Philippine regulations prohibit the sale of these vinegars produced by non-biogenic means as well as misrepresentation of the fine natural vinegars with cheaper version produced using lower value raw materials. The lack of reliable analytical tools however, has hampered the proper implementation of these laws. In this study, authentic vinegar samples were acquired, which were prepared by natural fermentation of : sugar cane, pineapple juice, and mango juice. Another type of cane vinegar was prepared by fermentation of cane sugar using acetator. Commercial vinegar samples, purchased from major supermarkets in the Philippines, were likewise obtained. Calcium acetate was produced by reaction of distilled vinegar samples with calcium carbonate, and subsequent drying of the resulting solution. Portions of the calcium acetate derived from the samples,were reacted with pyrophosphoric acid in a reflux and the glacial acetic acid was recovered by distillation under reduced pressure. The recovered glacial acetic acid were reconstituted to 90 % v/v. The acetic solutions were mixed with an Optiphase Hisafe Scintillant in vials. The C14 activities of the samples were measured in a 1414 Wallac Scintillation Counter and expressed as disintegrations per gram carbon or dpm/g C. Biogenic samples exhibit 12-15 dpm/g C activities, while synthetic samples show 0-2 dpm/g C activities. The remaining portions of the calcium acetate powder were placed in evacuated glass ampoules containing potassium peroxidisulfate and silver (1) permanganate. The samples inside the ampoules were oxidized to Carbon Dioxide, CO 2 gas, in a furnace. The CO 2 were then purified and bled to an Isotope Ratio mass spectrometer. 1 3C/ 1 2C ratios were determined and compared against a standard

Uncovering the method of production and detection of synthetic acetic acid adulteration in vinegar by tandem use of {sup 1}4C liquid scintillation counting and {sup 1}3C/{sup 1}2C ratio mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Wechner, Stefan; Voropaev, Andrey; Eichinger, Lorenz [HYDROISOTOP GmbHk Scweitenkirchen, Germany (Germany); Santos, Flora L; Castaneda, Soledad; Racho, Michael; Pabroa, Preciosa Corazon; Morco, Ryan; Sucgang, Raymond J [Philippine Nuclear Research Institute, Diliman, Quezon City (Philippines)

2010-07-01

Fraudulent adulteration and or misrepresentation had been a problem for commercial vinegar in the Philippines. Solutions of synthetic acetic acid mixed with colorants and flavour enhancers have been marketed as {sup v}inegar{sup .} Philippine regulations prohibit the sale of these vinegars produced by non-biogenic means as well as misrepresentation of the fine natural vinegars with cheaper version produced using lower value raw materials. The lack of reliable analytical tools however, has hampered the proper implementation of these laws. In this study, authentic vinegar samples were acquired, which were prepared by natural fermentation of : sugar cane, pineapple juice, and mango juice. Another type of cane vinegar was prepared by fermentation of cane sugar using acetator. Commercial vinegar samples, purchased from major supermarkets in the Philippines, were likewise obtained. Calcium acetate was produced by reaction of distilled vinegar samples with calcium carbonate, and subsequent drying of the resulting solution. Portions of the calcium acetate derived from the samples,were reacted with pyrophosphoric acid in a reflux and the glacial acetic acid was recovered by distillation under reduced pressure. The recovered glacial acetic acid were reconstituted to 90 % v/v. The acetic solutions were mixed with an Optiphase Hisafe Scintillant in vials. The C14 activities of the samples were measured in a 1414 Wallac Scintillation Counter and expressed as disintegrations per gram carbon or dpm/g C. Biogenic samples exhibit 12-15 dpm/g C activities, while synthetic samples show 0-2 dpm/g C activities. The remaining portions of the calcium acetate powder were placed in evacuated glass ampoules containing potassium peroxidisulfate and silver (1) permanganate. The samples inside the ampoules were oxidized to Carbon Dioxide, CO{sub 2} gas, in a furnace. The CO{sub 2} were then purified and bled to an Isotope Ratio mass spectrometer. {sup 1}3C/{sup 1}2C ratios were determined and

intravenous infusion of chlorimipramine (anafranil)

African Journals Online (AJOL)

the already extensive outpatient facilities at Johannesburg. Hospital as well as the Tara Neuro-Psychiatric Hospital for long-term therapy. Technique of Chlorimipramine Infusion. Initially 1 ampoule of chlorimipramine 25 mg in 250 mg of 5°~ dextrose saline was administered intravenously at the rate of 60 drops per minute.

Behaviours, thoughts and perceptions around mealtime insulin usage and wastage among people with type 1 and type 2 diabetes mellitus: A cross-sectional survey study.

Science.gov (United States)

Van Brunt, Kate; Pedersini, Riccardo; Rooney, Jillian; Corrigan, Sheila M

2017-04-01

People with diabetes who use mealtime insulin (MTI) were surveyed about insulin wastage and injection habits when insufficient insulin remains in a disposable prefilled pen/cartridge to administer a full dose in a single injection. Cross-sectional, online, self-reported survey of MTI usage/wastage behaviour in 400 adults with type 1 (n=120) or type 2 (n=280) diabetes mellitus administering >20units/day of MTI via 100units/ml prefilled pens/cartridges for ⩾1month, conducted in France, Germany, Italy and UK. Participants' mean±standard deviation age was 54.5±12.2years, body mass index was 29.9±7.2kg/m 2 and duration of MTI therapy was 8.6±7.8years. They administered 3.7±5.9 injections/day with meals, using 11.3±18.0 prefilled pens/cartridges per month. Overall, 63.5% split the dose across two prefilled pens/cartridges (i.e. administered two injections to obtain a full dose), 15.0% used just what remained in their current pen (i.e. took a lower-than-prescribed dose) and 36.3% discarded prefilled pens/cartridges still containing insulin (i.e. took full dose with new pen). The latter participants discarded a mean 5.5±8.2 prefilled pens/cartridges monthly still containing insulin, each containing 8.6±8.7 units of insulin. Participants who wasted insulin considered it frustrating, time-consuming and painful to inject twice. Patients taking >20units/day MTI can find transitions between insulin pens challenging. This study highlights the need to identify ways of improving transitions between pens to make transitions easier for insulin users, which could potentially improve adherence to prescribed doses and reduce waste. Copyright © 2016 Eli Lilly and Company. Published by Elsevier B.V. All rights reserved.

Anesthetic Efficacy of a Combination of 4% Prilocaine/2% Lidocaine with Epinephrine for the Inferior Alveolar Nerve Block: A Prospective, Randomized, Double-blind Study.

Science.gov (United States)

Cook, Olivia; Nusstein, John; Drum, Melissa; Fowler, Sara; Reader, Al; Draper, John

2018-05-01

Prilocaine plain has a high pH and concentration (4%), which could decrease the pain of injection and increase success. The purpose of this study was to compare pain associated with anesthetic solution deposition and the degree of pulpal anesthesia obtained with the combination of prilocaine and lidocaine versus a lidocaine and lidocaine combination when used for inferior alveolar nerve blocks (IANBs). One hundred eighteen asymptomatic subjects were randomly given a combination of 1 cartridge of 4% prilocaine plain plus 1 cartridge of 2% lidocaine with 1:100,000 epinephrine or a combination of 2 cartridges of 2% lidocaine with 1:100,000 epinephrine for the IANB at 2 separate appointments. Subjects rated the pain associated with anesthetic solution deposition of injection. Mandibular teeth were tested with an electric pulp tester every 4 minutes for 57 minutes. Anesthesia was considered successful when 2 consecutive 80 readings were obtained within 17 minutes and the 80 reading was continuously sustained for 57 minutes. Comparisons for anesthetic success were analyzed using the exact McNemar test, and pain ratings associated with anesthetic solution deposition were analyzed using multiple Wilcoxon matched pairs signed rank tests; both were adjusted using the step-down Bonferroni method of Holm. Four percent prilocaine plain was significantly less painful upon anesthetic solution deposition. Pulpal anesthetic success was not significantly different between the 2 combinations. The combination of 4% prilocaine plain plus 2% lidocaine with 1:100,000 epinephrine did not increase pulpal anesthetic success for IANBs compared with a combination of 2 cartridges of 2% lidocaine with 1:100,000 epinephrine. Pain associated with anesthetic solution deposition from the first cartridge of 4% prilocaine plain was significantly less when compared with the first cartridge of 2% lidocaine with 1:100,000 epinephrine. Copyright © 2018 American Association of Endodontists. Published

Prevalence of Ex Vivo High On-treatment Platelet Reactivity on Antiplatelet Therapy after Transient Ischemic Attack or Ischemic Stroke on the PFA-100(®) and VerifyNow(®).

LENUS (Irish Health Repository)

Kinsella, Justin A

2012-09-12

BACKGROUND: The prevalence of ex vivo high on-treatment platelet reactivity (HTPR) to commonly prescribed antiplatelet regimens after transient ischemic attack (TIA) or ischemic stroke is uncertain. METHODS: Platelet function inhibition was simultaneously assessed with modified light transmission aggregometry (VerifyNow; Accumetrics Inc, San Diego, CA) and with a moderately high shear stress platelet function analyzer (PFA-100; Siemens Medical Solutions USA, Inc, Malvern, PA) in a pilot, cross-sectional study of TIA or ischemic stroke patients. Patients were assessed on aspirin-dipyridamole combination therapy (n = 51) or clopidogrel monotherapy (n = 25). RESULTS: On the VerifyNow, HTPR on aspirin was identified in 4 of 51 patients (8%) on aspirin-dipyridamole combination therapy (≥550 aspirin reaction units on the aspirin cartridge). Eleven of 25 (44%) patients had HTPR on clopidogrel (≥194 P2Y12 reaction units on the P2Y12 cartridge). On the PFA-100, 21 of 51 patients (41%) on aspirin-dipyridamole combination therapy had HTPR on the collagen-epinephrine (C-EPI) cartridge. Twenty-three of 25 patients (92%) on clopidogrel had HTPR on the collagen-adenosine diphosphate (C-ADP) cartridge. The proportion of patients with antiplatelet HTPR was lower on the VerifyNow than PFA-100 in patients on both regimens (P < .001). CONCLUSIONS: The prevalence of ex vivo antiplatelet HTPR after TIA or ischemic stroke is markedly influenced by the method used to assess platelet reactivity. The PFA-100 C-ADP cartridge is not sensitive at detecting the antiplatelet effects of clopidogrel ex vivo. Larger prospective studies with the VerifyNow and with the PFA-100 C-EPI and recently released Innovance PFA P2Y cartridges (Siemens Medical Solutions USA, Inc) in addition to newer tests of platelet function are warranted to assess whether platelet function monitoring predicts clinical outcome in ischemic cerebrovascular disease.

Simplified pressure method for respirator fit testing.

Science.gov (United States)

Han, D; Xu, M; Foo, S; Pilacinski, W; Willeke, K

1991-08-01

A simplified pressure method has been developed for fit testing air-purifying respirators. In this method, the air-purifying cartridges are replaced by a pressure-sensing attachment and a valve. While wearers hold their breath, a small pump extracts air from the respirator cavity until a steady-state pressure is reached in 1 to 2 sec. The flow rate through the face seal leak is a unique function of this pressure, which is determined once for all respirators, regardless of the respirator's cavity volume or deformation because of pliability. The contaminant concentration inside the respirator depends on the degree of dilution by the flow through the cartridges. The cartridge flow varies among different brands and is measured once for each brand. The ratio of cartridge to leakflow is a measure of fit. This flow ratio has been measured on human subjects and has been compared to fit factors determined on the same subjects by means of photometric and particle count tests. The aerosol tests gave higher values of fit.

Apparatus for inspecting the quality of nuclear fuel rod ends

International Nuclear Information System (INIS)

Brashier, R.W.; Pfau, E.D.

1990-01-01

This patent describes an apparatus for inspecting the quality of both ends of nuclear fuel rods. It comprises: a housing including a pair of longitudinally separated slots for receiving X-ray downwardly therethrough from an external source and so as to define first and second longitudinally spaced apart operating positions, means for serially guiding nuclear fuel rods longitudinally through the housing and to a first rod position wherein the forward ends of the rods are aligned below the first operating position and to a second rod position wherein the rear ends of the rods are aligned below the second operating position, belt conveyor assembly means for serially advancing X-ray film cartridges longitudinally through the housing and below the rods, and so that each cartridge may be selectively aligned below the first and second operating positions; and table means supported by the conveyor frame for selectively lifting the film cartridges supported by the belts and so that the conveyor belts may be advanced while the film cartridges are held stationary

Percutaneous biopsy of malignant hepatic tumor in patients with bleeding tendency : usefulness of gelfoam plugging up the biopsy track

International Nuclear Information System (INIS)

Yoon, Hye Ran; Kwak, Byung Kook; Choi, Chi Hoon; Park, Yong Ok; Yang, Keun Myeong; Seo, Ja Young; Lee, Shin Hyung; Lee, Chang Joon; Shim, Hyung Jin

1998-01-01

To plug the biopsy site in eight patients with coagulopathy who had undergone percutaneous liver biopsy. To this end, gelfoam cartridge was used as a sealant. Materials and Methods: Using an 18G Tru-Cut-type disposable automated biopsy gun(Soo Ho Medi-tech, Seoul, Korea) and under US guidance, eight patients underwent percutaneous liver biopsy. After the gun had fired, the biopsy specimen in the inner stylet was retrieved while the outer cannula was held in place ; the cannula was then used to plug the biopsy tracks with gelfoam, using two or three cartridges. If bleeding occurred, this was controlled by the use of more gelfoam cartridges. Results:Diagnostic target tissue was obtained in seven of the eight patients(87.5%). Hepatocellular carcinoma was diagnosed in five cases and metastatic cancer in two. Profuse bleeding was observed in one patient(12.5%) and resolved by gelfoam plugging. Conclusion: We believe that in patients with coagulopathy who are required to undergo liver biopsy plugging the liver biopsy track with gelfoam cartridge is a simple, safe and useful method

Volatile organic compound analysis in wood combustion and meat cooking emissions

International Nuclear Information System (INIS)

Zielinska, B.; McDonald, J.

1999-01-01

Residential wood combustion and meat cooking emissions were each analyzed for volatile organic compounds (VOC). Emissions were diluted 60--100 times, cooled to ambient temperature, and allowed 80 seconds for condensation prior to collection with the aid of a DRI-constructed dilution stack sampler. Fireplace and wood-stove emissions testing was conducted at the DRI facilities. Wood type, wood moisture, burn rate, and fuel load were varied for different experiments. Meat emissions testing was conducted at the CE-CERT stationary emissions lab, University of California, Riverside. Meat type, fat content, and cooking appliance were changed in different tests. VOCs were collected using stainless-steel 6 L canisters and Tenax cartridges, whereas for carbonyl compound collection 2,4-dinitrophenylhydrazine (DNPH)-impregnated C 18 SepPack cartridges were used. Analysis of VOC collected with canisters and Tenax cartridges was conducted by Gas Chromatography/Mass Spectrometry (GC/MS) and by GC/FID/ECD (flame ionization detection/electron capture detection). DNPH-impregnated cartridges were analyzed for fourteen C 1 --C 7 carbonyl compounds, using the HPLC method. The results of these measurements are discussed

A simple method to compare firing pin marks using stereomicroscope and Microsoft office (Windows 8) tools.

Science.gov (United States)

Suresh, R

2017-08-01

Pertinent marks of fired cartridge cases such as firing pin, breech face, extractor, ejector, etc. are used for firearm identification. A non-standard semiautomatic pistol and four .22rim fire cartridges (head stamp KF) is used for known source comparison study. Two test fired cartridge cases are examined under stereomicroscope. The characteristic marks are captured by digital camera and comparative analysis of striation marks is done by using different tools available in the Microsoft word (Windows 8) of a computer system. The similarities of striation marks thus obtained are highly convincing to identify the firearm. In this paper, an effort has been made to study and compare the striation marks of two fired cartridge cases using stereomicroscope, digital camera and computer system. Comparison microscope is not used in this study. The method described in this study is simple, cost effective, transport to field study and can be equipped in a crime scene vehicle to facilitate immediate on spot examination. The findings may be highly helpful to the forensic community, law enforcement agencies and students. Copyright © 2017 Elsevier B.V. All rights reserved.

Basic hydrolysis of 1, 3, 4, 6-tetra-O-acetyl-2-[18F] fluoro-D-glucose on solid phase extraction

International Nuclear Information System (INIS)

Zhang Jinming; Tian Jiahe; He Yijie; Huan Dingcai; Liu Boli

2003-01-01

A new base hydrolysis method are used for 1, 3, 4, 6-tetra-O-acetyl-2-[ 18 F] fluoro-D-glucose on solid phase extraction. The labeled intermediate is trapped on an active C-18 solid phase extraction cartridge, and hydrolyzed in cartridge with 1 mL 2 mol/L NaOH at room temperature. The results show that there are over 99% of the labeled intermediate being turned into 18 F-FDG within 2 min. It is easy to get 18 F-FDG after neutralized with phosphate buffer, purified by C-18 and Alumina cartridge. The basic hydrolysis on solid extraction is a simple method for preparation of 18 F-FDG

Engineering evaluation of solids/liquids separation processes applicable to sludge treatment project

International Nuclear Information System (INIS)

Duncan, J.B.

1998-01-01

This engineering study looks at the solids/liquids separation unit operations after the acid dissolution of the K Basin sludge treatment. Unit operations considered were centrifugation, filtration (cartridge, cross flow, and high shear filtration) and gravity settling. The recommended unit operations for the solids/liquids separations are based upon the efficiency, complexity, and off-the-shelf availability and adaptability. The unit operations recommended were a Robatel DPC 900 centrifuge followed by a nuclearized 31WM cartridge filter. The Robatel DPC 900 has been successfully employed in the nuclear industry on a world wide scale. The 31WM cartridge filter has been employed for filtration campaigns in both the government and civilian nuclear arenas

Linear and/or curvilinear rail mount system

Science.gov (United States)

Thomas, Jackie D. (Inventor); Harris, Lawanna L. (Inventor)

2012-01-01

One or more linear and/or curvilinear mounting rails are coupled to a structure. Each mounting rail defines a channel and at least one cartridge assembly is engaged in the channel. Each cartridge assembly includes a housing that slides within the channel. The housing defines a curvilinearly-shaped recess longitudinally aligned with the channel when the housing is in engagement therewith. The cartridge assembly also includes a cleat fitted in the recess for sliding engagement therealong. The cleat can be coupled to a fastener that passes through the mounting rail and the housing when the housing is so-engaged in the channel. The cleat is positioned in the recess by a position of the fastener.

Apparatus for rendering at least a portion of a device inoperable and related methods

Energy Technology Data Exchange (ETDEWEB)

Daniels, Michael A.; Steffler, Eric D.; Hartenstein, Steven D.; Wallace, Ronald S.

2016-11-08

Apparatus for rendering at least a portion of a device inoperable may include a containment structure having a first compartment that is configured to receive a device therein and a movable member configured to receive a cartridge having reactant material therein. The movable member is configured to be inserted into the first compartment of the containment structure and to ignite the reactant material within the cartridge. Methods of rendering at least a portion of a device inoperable may include disposing the device into the first compartment of the containment structure, inserting the movable member into the first compartment of the containment structure, igniting the reactant material in the cartridge, and expelling molten metal onto the device.

Water reactive hydrogen fuel cell power system

Science.gov (United States)

Wallace, Andrew P; Melack, John M; Lefenfeld, Michael

2014-01-21

A water reactive hydrogen fueled power system includes devices and methods to combine reactant fuel materials and aqueous solutions to generate hydrogen. The generated hydrogen is converted in a fuel cell to provide electricity. The water reactive hydrogen fueled power system includes a fuel cell, a water feed tray, and a fuel cartridge to generate power for portable power electronics. The removable fuel cartridge is encompassed by the water feed tray and fuel cell. The water feed tray is refillable with water by a user. The water is then transferred from the water feed tray into a fuel cartridge to generate hydrogen for the fuel cell which then produces power for the user.

Electrospun UiO-66/polyacrylonitrile nanofibers as efficient sorbent for pipette tip solid phase extraction of phytohormones in vegetable samples.

Science.gov (United States)

Yan, Zhiming; Wu, Mei; Hu, Biqing; Yao, Minna; Zhang, Lan; Lu, Qiaomei; Pang, Jie

2018-03-23

In this work, metal-organic framework particles incorporated fibers (UiO-66/PAN nanofibers) were used as adsorbent in pipette tip solid phase extraction (PT-SPE) for the first time. The UiO-66/PAN nanofibers were fabricated by a facile electrospinning method and characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, X-ray diffraction and nitrogen adsorption-desorption experiments. The UiO-66/PAN nanofibers were applied to assemble a novel PT-SPE cartridge for determination of four phytohormones followed by high performance liquid chromatography (HPLC). Several experimental parameters such as kinds of UiO-66/PAN nanofibers, the amount of UiO-66/PAN nanofibers, the effect of solution pH, ionic strength and desorption conditions were intensively investigated. Under the optimal conditions, the linear ranges of the phytohormones were in the range of 0.06-60 ng/mL with correlation coefficients above 0.992. The limits of detection were between 0.01 ng/mL to 0.02 ng/mL. The interday and intraday precision (RSD) for three replicate extractions of the four phytohormones (15 ng/mL for each) was in the range of 1.5-5.6%. The established method was successfully applied for the determination of phytohormones in watermelon and mung bean sprouts samples. The results showed that the electrostatic interaction between the positively charged UiO-66 and anionic forms of phytohormones played an important role in the extraction of the phytohormones. Copyright © 2018 Elsevier B.V. All rights reserved.

On-line packed magnetic in-tube solid phase microextraction of acidic drugs such as naproxen and indomethacin by using Fe3O4@SiO2@layered double hydroxide nanoparticles with high anion exchange capacity.

Science.gov (United States)

Shamsayei, Maryam; Yamini, Yadollah; Asiabi, Hamid; Safari, Meysam

2018-02-22

The authors describe a 3-component nanoparticle system composed of a silica-coated magnetite (Fe 3 O 4 ) core and a layered double (Cu-Cr) hydroxide nanoplatelet shell. The sorbent has a high anion exchange capacity for extraction anionic species. A simple online system, referred to as "on-line packed magnetic-in-tube solid phase microextraction" was designed. The nanoparticles were placed in a stainless steel cartridge via dry packing. The cartridge was then applied to the preconcentration acidic drugs including naproxen and indomethacin from urine and plasma. Extraction and desorption times, pH values of the sample solution and flow rates of sample solution and eluent were optimized. Analytes were then quantified by HPLC with UV detection. Under optimal conditions, the limits of detection range from 70 to 800 ng L -1 , with linear responses from 0.1-500 μg L -1 (water samples), 0.6-500 μg L -1 (spiked urine), and 0.9-500 μg L -1 (spiked plasma). The inter- and intra-assay precisions (RSDs, for n = 5) are in the range of 2.2-5.4%, 2.8-4.9%, and 2.0-5.2% at concentration levels of 5, 25 and 50 μg L -1 , respectively. The method was applied to the analysis of the drugs in spiked human urine and plasma, and good results were achieved. Graphical abstract Fe 3 O 4 @SiO 2 @CuCr-LDH magnetic nanoparticles were synthesized and packed in to a stainless steel column. The column was applied to solid phase microextraction of acidic drugs from biological samples.

Calculation Of Aerosol Transport Efficiency For The Airborne Radioiodine Monitoring System - ''RIS125''

International Nuclear Information System (INIS)

Kravchik, T.; Levinson, L.; Mazor, Y.; Dolev, E.; German, U.

1999-01-01

Radioactive iodine is a typical fission product in nuclear power reactors. Of the many iodine isotopes that can be generated in nuclear reactors only four are considered as radiobiological significant. These are: 125 1 (T 1/2 =60 days), '1 31 I (T 1/2 =8d), 133 I (T 1/2 =21h) and I35 I (T 1/2 7h). The chemical forms that have been identified in heavy water reactors are I 2 (elemental), organic iodides (CH 3 I), Inorganic iodides (HOI, HI) and LiI. Radioiodine is, generally, released as a gas but can be adsorbed on air particulates to form radioiodine contained aerosols. Therefore. its monitoring has to include both gas and aerosol sampling. A new monitoring system, RIS (Radioactive iodine Sampler), has been developed at the NRCN to monitor radioactive iodine (gas and aerosol) on-line in workplaces. This system samples radioiodine at a 60 L/min rate through a transport line connected to a filter holder. The filter consists of a cartridge containing activated charcoal with TEDA for iodine gas adsorption with a membrane for aerosols' retention in from of it. The radioiodine filter cartridge (F and J product code: TE2C) has a diameter of 2 1/4 inch and height of 1 inch . The gas adsorbent is coconut shell carbon type activated charcoal with 5% (by weight) TEDA impregnation and has 30x50 mesh size. This paper presents the aerosols' sampling characteristics of the RIS system including their transport in the sampling line and filter holder. The adsorption of iodine gas on the transport system components is negligible

Comparison of various liquid chromatographic methods involving UV and atmospheric pressure chemical ionization mass spectrometric detection for the efficient trace analysis of phenylurea herbicides in various types of water samples.

Science.gov (United States)

van der Heeft, E; Dijkman, E; Baumann, R A; Hogendoorn, E A

2000-05-19

The performance of mass spectrometric (MS) detection and UV detection in combination with reversed-phase liquid chromatography without and with the use of coupled column RPLC (LC-LC) has been compared for the trace analysis of phenylurea herbicides in environmental waters. The selected samples of this comparative study originated from an inter-laboratory study. For both detection modes, a 50 mm x 4.6 mm I.D. column and a 100 mm x 4.6 mm I.D. column packed with 3 microm C18 were used as the first (C-1) and second (C-2) column, respectively. Atmospheric pressure chemical ionization mass spectrometry was performed on a magnetic sector instrument. The LC-LC-MS analysis was carried out on-line by means of direct large volume (11.7 ml) injection (LVI). The performance of both on-line (LVI, 4 ml of sample) and off-line LC-LC-UV (244 nm) analysis was investigated. The latter procedure consisted of a solid-phase extraction (SPE) of 250 ml of water sample on a 500 mg C18 cartridge. The comparative study showed that LC-LC-MS is more selective then LC-LC-UV and, in most cases, more sensitive. The LVI-LC-LC-MS approach combines direct quantification and confirmation of most of the analytes down to a level of 0.01 microg/l in water samples in less then 30 min. As regards LC-LC-UV, the off-line method appeared to be a more viable approach in comparison with the on-line procedure. This method allows the screening of phenylurea's in various types of water samples down to a level of at least 0.05 microg/l. On-line analysis with LVI provided marginal sensitivity (limits of detection of about 0.1 microg/l) and selectivity was sometimes less in case of surface water samples. Both the on-line LVI-LC-LC-MS method and the LC-LC-UV method using off-line SPE were validated by analysing a series of real-life reference samples. These samples were part of an inter-laboratory test and contained residues of herbicides ranging from 0.02 to 0.8 microg/l. Beside good correlation between the methods

An investigation into the factors that influence toolmark identifications on ammunition discharged from semi-automatic pistols recovered from car fires.

Science.gov (United States)

Collender, Mark A; Doherty, Kevin A J; Stanton, Kenneth T

2017-01-01

Following a shooting incident where a vehicle is used to convey the culprits to and from the scene, both the getaway car and the firearm are often deliberately burned in an attempt to destroy any forensic evidence which may be subsequently recovered. Here we investigate the factors that influence the ability to make toolmark identifications on ammunition discharged from pistols recovered from such car fires. This work was carried out by conducting a number of controlled furnace tests in conjunction with real car fire tests in which three 9mm semi-automatic pistols were burned. Comparisons between pre-burn and post burn test fired ammunition discharged from these pistols were then performed to establish if identifications were still possible. The surfaces of the furnace heated samples and car fire samples were examined following heating/burning to establish what factors had influenced their surface morphology. The primary influence on the surfaces of the furnace heated and car fire samples was the formation of oxide layers. The car fire samples were altered to a greater extent than the furnace heated samples. Identifications were still possible between pre- and post-burn discharged cartridge cases, but this was not the case for the discharged bullets. It is suggested that the reason for this is a difference between the types of firearms discharge-generated toolmarks impressed onto the base of cartridge cases compared to those striated along the surfaces of bullets. It was also found that the temperatures recorded in the front foot wells were considerably less than those recorded on top of the rear seats during the car fires. These factors should be assessed by forensic firearms examiners when performing casework involving pistols recovered from car fires. Copyright © 2016 The Chartered Society of Forensic Sciences. Published by Elsevier Ireland Ltd. All rights reserved.

PAH distribution and mass fluxes in the Three Gorges Reservoir after impoundment of the Three Gorges Dam.

Science.gov (United States)

Deyerling, Dominik; Wang, Jingxian; Hu, Wei; Westrich, Bernhard; Peng, Chengrong; Bi, Yonghong; Henkelmann, Bernhard; Schramm, Karl-Werner

2014-09-01

Mass fluxes of polycyclic aromatic hydrocarbons (PAHs) were calculated for the Three Gorges Reservoir (TGR) in China, based on concentration and discharge data from the Yangtze River. Virtual Organisms (VOs) have been applied during four campaigns in 2008, 2009 (twice) and 2011 at sampling sites distributed from Chongqing to Maoping. The total PAH mass fluxes ranged from 110 to 2,160 mg s(-1). Highest loads were determined at Chongqing with a decreasing trend towards Maoping in all four sampling campaigns. PAH remediation capacity of the TGR was found to be high as the mass flux reduced by more than half from upstream to downstream. Responsible processes are thought to be adsorption of PAH to suspended particles, dilution and degradation. Furthermore, the dependence of PAH concentration upon water depth was investigated at Maoping in front of the Three Gorges Dam. Although considerable differences could be revealed, there was no trend observable. Sampling of water with self-packed filter cartridges confirmed more homogenous PAH depth distribution. Moreover, PAH content of suspended particles was estimated from water concentrations gathered by VOs based on a water-particle separation model and subsequently compared to PAH concentration measured in water and in filter cartridges. It could be shown that the modeled data predicts the concentration caused by particle-bound PAHs to be about 6 times lower than PAHs dissolved in water. Besides, the model estimates the proportions of 5- and 6-ring PAHs being higher than in water phase. Copyright © 2014 Elsevier B.V. All rights reserved.

Study of interfacial phenomena of organo-chlorinated steam adsorption on a microporous adsorbent. Case of tri chloro-1,1,1 ethane on activated charcoal

International Nuclear Information System (INIS)

Escallon, S.

1991-06-01

This study involves the construction and the perfecting of a test system for evaluating the service life of organic vapor cartridges versus 1,1,1 -trichloroethane. Thermogravimetric measurements were carried on in order to suggest a field method to reactive these cartridges, using hot air flow system. Assessment of adsorption rate during experiment is measured with a new electrical method. (author)

IM-CRDS for the analysis of matrix-bound water isotopes: a streamlined (and updated) tool for ecohydrologists to probe small-scale variability in plants Yasuhara, S. (syasuhara@picarro.com)1,Carter, J.A. (jcarter@picarro.com)1, Dennis, K.J. (kdennis@picarro.com)1 1Picarro Inc., 3105 Patrick Henry Drive, Santa Clara, CA 95054

Science.gov (United States)

Yasuhara, S.

2013-12-01

The ability to measure the isotopic composition of matrix-bound water is valuable to many facets of earth and environmental sciences. For example, ecohydrologists use stable isotopes of oxygen and hydrogen in plant and soil water, in combination with measurements of atmospheric water vapor, surface water and precipitation, to estimate budgets of evapotranspiration. Likewise, water isotopes of oceanic water, brines and other waters with high total dissolved solids (TDS, e.g., juices) are relevant to studying large-scale oceanic circulation, small-scale mixing, groundwater contamination, the balance of evaporation to precipitation, and the provenance of food. Conventionally matrix-bound water has been extracted using cryogenic distillation, whereby water is distilled from the material in question (e.g., a leaf sample) by heating under vacuum and collecting the resultant water vapor using liquid nitrogen. The water can then be analyzed for its stable isotopic composition by a variety of methods, including isotope ratio mass spectrometry and laser techniques, such as Cavity Ring-Down Spectroscopy (CRDS). Here we present recent improvements in an alternative, and stream-lined, solution for integrated sample extraction and isotopic measurement using a Picarro Induction Module (IM) coupled to commercially-available CRDS analyzer from Picarro. This technique is also valuable for waters with high TDS, which can have detrimental effects on flash vaporization process, typically used for the introduction of water to Picarro CRDS water isotope analyzers. The IM works by inductively heating a sample held within a metal sample holder in a glass vial flushed with dry air. Tested samples include leaves, stems, twigs, calibration water, juices, and salt water. The heating process evolves water vapor which is then swept through the system at approximately 150 standard cubic centimeters per minute. The evolved water vapor passes through an activated charcoal cartridge for removal of

Impact of dexamethason

Directory of Open Access Journals (Sweden)

Zahra Basirat

2016-09-01

Full Text Available Objective: Infertile women with polycystic ovary (PCOs involve with anovulatory cycles. Various adjuvant treatments have been suggested to improve ovarian response in these patients. In this study, we aimed to evaluate the role of dexamethasone in the outcome of IVF/ICSI in PCOs infertile women. Study design: 129 PCOs infertile women undergone IVF/ICSI were enrolled for this single blind clinical trial study in 2012–2013. Setting: Fatemezahra Infertility and Reproductive Health Research Center, Babol University of Medical Sciences, Babol, Iran. Method: 43 patients who underwent IVF received dexamethasone (0.5 mg, 4 tab/day in the treatment group and 74 patients were considered as the placebo group. Main outcome measure: Pregnancy rate was compared between the two groups. In addition, number of dominant follicle, oocytes retrieved, embryos transferred, and number of gonadotropin ampoule were evaluated. Results: The pregnancy rate in the group receiving dexamethasone was 17.5% significantly higher versus 4.3% in the placebo group (P < 0.05. The mean number of embryos in the patients received dexamethasone was 6.7 ± 4.3, significantly greater than placebo which was 4.9 ± 4.9 (P < 0.05. The mean number of gonadotropin ampoules used in the group received dexamethasone was 3.5 ± 1.6, significantly lower versus the placebo which was 5.3 ± 2.5 (P < 0.05. The mean number of oocytes in the group received dexamethasone was 11.8 ± 8 and in the placebo group was 9.6 ± 5.8 that was not significant. Conclusion: Dexamethasone enhances embryos and pregnancy rate; in addition, it reduces gonadotropines ampoule used for stimulation, hence, and we recommend using of dexamethasone in women with PCOs undertreatment of IVF/ICSI.

Hydrogen Bonding in Ion-pair Molecules in Vapors over ionic liquids, studied by Raman Spectroscopy and ab initio Calculations

DEFF Research Database (Denmark)

Berg, Rolf W.

gaseous free state models. Some extreme examples are to be discussed: (1) The 1,1,3,3-tetramethyl-guanidinium chloride “molecule” [TMG-H-Cl] found [ref 1] to exist in gaseous state over its corresponding liquid in evacuated ampouls heated at ~225°C (Fig. 1); (2) the analogous bromide “molecule” [TMG...

Electronic Vapor Cigarette Battery Explosion Causing Shotgun-like Superficial Wounds and Contusion

Directory of Open Access Journals (Sweden)

Siri Shastry, MD

2016-03-01

Full Text Available INTRODUCTION Electronic vapor cigarettes (E-cigarettes were created in 2003 as an alternative to traditional tobacco cigarettes. E-cigarettes have been available in the United States since 2006.1 The typical E-cigarette consists of a cartridge that contains liquid, an atomizer that heats the liquid (i.e. acts as a vaporizer, as well as a battery. The liquid contained within the cartridge contains nicotine, propylene glycol and/ or glycerol as well as flavorings. The consumer uses an E-cigarette through either pushing a button or inhalation, which triggers heating and therefore aerosolizes the liquid within the cartridge, emulating cigarette “smoke.” The newest E-cigarettes are larger than nicotine cigarettes and employ stronger, rechargeable batteries as a power source.2,3

A morphological study of the sulfurisation of digenite to covellite using reflected polarised light microscopy

DEFF Research Database (Denmark)

Rask Møller Frøkiær, Heidi; Warner, Terence E.

2017-01-01

A series of copper rods were reacted with sulfur vapour in evacuated glass ampoules at ∼445 °C. Product materials were characterised by powder X-ray diffraction and reflected polarised light microscopy. Copper sulfurised rapidly to digenite, γ-Cu2-xS, under these conditions, whereas the subsequen...... of the covellite structure. Sulfurising a coil of copper wire at ∼445 °C is an effective method for synthesising covellite.......A series of copper rods were reacted with sulfur vapour in evacuated glass ampoules at ∼445 °C. Product materials were characterised by powder X-ray diffraction and reflected polarised light microscopy. Copper sulfurised rapidly to digenite, γ-Cu2-xS, under these conditions, whereas the subsequent...... − besides being a p-type metal − is ionically conducting at 445 °C, although considerably less so than digenite. We infer that the growth of platy covellite crystals and their radial alignment in the primary CuS layer are a consequence of copper ion mobility being restricted to the basal plane...

Laparoscopic ovarian cystectomy of endometriomas does not affect the ovarian response to gonadotropin stimulation.

Science.gov (United States)

Marconi, Guillermo; Vilela, Martín; Quintana, Ramiro; Sueldo, Carlos

2002-10-01

To evaluate the ovarian response cycles of IVF-ET in patients who previously underwent laparoscopic cystectomy for endometriomas. Retrospective study with prospective selection of participants and controls. Instituto de Ginecología y Fertilidad Buenos Aires, Argentina. Thirty-nine patients underwent an operation for ovarian endometriomas by atraumatic removal of the pseudocapsule with minimal bipolar cauterization of small bleeders and an IVF-ET cycle (group A) and 39 control patients of similar age underwent an IVF-ET cycle for tubal factor infertility (group B). Laparoscopic endometrioma cystectomy, IVF-ET cycle. E(2) levels, number of gonadotropin ampoules, follicles, oocytes retrieved, number and quality of embryos transferred, and clinical pregnancy rate. There were no differences in all the parameters studied (E(2) levels, number of follicles, oocytes retrieved, number and quality of embryos transferred, and clinical pregnancy rate) except for the number of gonadotropin ampoules needed for ovarian hyperstimulation, which was significantly higher in group A than in group B. Our results indicate that laparoscopic cystectomy for endometriomas is an appropriate treatment since it did not negatively affect the ovarian response for IVF-ET.

Occupational exposure to mineral oil metalworking fluid (MWFs) mist: Development of new methodologies for mist sampling and analysis. Results from an inter-laboratory comparison

International Nuclear Information System (INIS)

Huynh, C Khanh; Herrera, H; Parrat, J; Wolf, R; Perret, V

2009-01-01

Metalworking Fluids (MWFs) are largely used in the sector of undercutting, a large professional activity in Switzerland, in particular in the fine mechanic and watch making industry. France proposes a Permissible Exposure Limit (PEL) of 1 mg.m -3 of aerosol. The American Conference of Governmental Industrial Hygienists (ACGIH) sets its value at 5 mg.m -3 but a proposal to lower the standard ('intended changes') to 0.2 mg.m -3 of aerosol is pending since 2001. However, it has not become a recognized threshold limit value for exposure. Since 2003, the new Swiss PEL (MAK) recommendations would be 0.2 mg.m -3 of aerosol (oil with boiling point > 350 deg. C without additives) and/or 20 mg.m -3 of oil aerosol + vapour for medium or light oil. To evaluate evaporative losses of sampled oil, the German 'Berufsgenossenschaftliches Institut fuer Arbeitssicherheit' (BGIA) recommends the use of a XAD-2 cartridge behind the filter. The method seems to work perfectly for MWFs in a clean occupational atmosphere free from interference of light vapour cleaning solvent such as White Spirit. But, in real situation, machine shop atmosphere contaminated with traces of White Spirit, the BGIA method failed to estimate the MWFs levels (over-estimation). In this paper, we propose a new approach meant to measure both oil vapours and aerosols. Five inter-laboratory comparisons are discussed, based on the production of oil mist in an experimental chamber under controlled conditions.

Systematic sampling with errors in sample locations

DEFF Research Database (Denmark)

Ziegel, Johanna; Baddeley, Adrian; Dorph-Petersen, Karl-Anton

2010-01-01

analysis using point process methods. We then analyze three different models for the error process, calculate exact expressions for the variances, and derive asymptotic variances. Errors in the placement of sample points can lead to substantial inflation of the variance, dampening of zitterbewegung......Systematic sampling of points in continuous space is widely used in microscopy and spatial surveys. Classical theory provides asymptotic expressions for the variance of estimators based on systematic sampling as the grid spacing decreases. However, the classical theory assumes that the sample grid...... is exactly periodic; real physical sampling procedures may introduce errors in the placement of the sample points. This paper studies the effect of errors in sample positioning on the variance of estimators in the case of one-dimensional systematic sampling. First we sketch a general approach to variance...

[A comparison of convenience sampling and purposive sampling].

Science.gov (United States)

Suen, Lee-Jen Wu; Huang, Hui-Man; Lee, Hao-Hsien

2014-06-01

Convenience sampling and purposive sampling are two different sampling methods. This article first explains sampling terms such as target population, accessible population, simple random sampling, intended sample, actual sample, and statistical power analysis. These terms are then used to explain the difference between "convenience sampling" and purposive sampling." Convenience sampling is a non-probabilistic sampling technique applicable to qualitative or quantitative studies, although it is most frequently used in quantitative studies. In convenience samples, subjects more readily accessible to the researcher are more likely to be included. Thus, in quantitative studies, opportunity to participate is not equal for all qualified individuals in the target population and study results are not necessarily generalizable to this population. As in all quantitative studies, increasing the sample size increases the statistical power of the convenience sample. In contrast, purposive sampling is typically used in qualitative studies. Researchers who use this technique carefully select subjects based on study purpose with the expectation that each participant will provide unique and rich information of value to the study. As a result, members of the accessible population are not interchangeable and sample size is determined by data saturation not by statistical power analysis.

Respons Antibodi Sekunder Terhadap Penyakit Tetelo pada Ayam Petelur Pascavaksinasi Ulangan dengan Vaksin Tetelo Aktif (NEWCASTLE DISEASESECONDARY ANTIBODY RESPONSE AFTER REVACCINATION IN LAYER WITH THE ACTIVE ND VACCINE

Directory of Open Access Journals (Sweden)

Andika Budi Kurnianto

2016-11-01

Full Text Available Revaccination is required in order to preventNewcastle Disease (ND reccurence inlayers chickens. Oneof vaccine for ND revaccination is freeze-died ND active vaccine containing e” 106,5EID50. Revaccinationisdone to trigger a faster secondary antibody responses in layers and can achieve protective antibody titersagainst ND that can be monitored by a hemagglutinationinhibition (HI. The aim of this study was todetermine the ND secondary antibody responses in layers after revaccination with ND active vaccine.Antibody titer of 20 layers chickens of 20 week old were determined before revaccinations (week 0 andafter revaccinations (week 1 until week 9. The first vaccination was conducted using ND-IB (NewcastleDisease-Infectious Bronchitis at the age of 2 days through eye drops and subcutaneous injection at the ageof 5 days using a dose of 1 ampoule.Vaccination is repeated at the age of 20 weeks at a dose of 1 ½ ampoule through drinking water. Blood samples were collected on the wing vein (venous cutane ulnar and left for 5-10 minutes at room temperature.Sera were then collected and stored at -20oC until use. HI antibody titerwas determined by micro titeration system. The HI mean titers were analyzed by Duncan test. The studyresults showed that antibody titer before revaccination was3,47 HI log 2 and the HI titers after revaccinationwere 4,02; 5,22; 6,52; 7,85; 8,4; 8,6; 7,7; 5,92; dan 3,87 HI log 2 respectivelly at weeks 1, 2, 3, 4, 5, 6, 7, 8, and9.The NDV revaccination with ND active vaccine significantly (P <0.01 increased in antibody titer inlayers starting from week 1 to week 6, but decreased following week 7 to week-9. It can be concluded thatrevaccinantion with ND active vaccine increases the antibody titers in layer chickens.

Nicotine content of electronic cigarettes, its release in vapour and its consistency across batches: regulatory implications.

Science.gov (United States)

Goniewicz, Maciej L; Hajek, Peter; McRobbie, Hayden

2014-03-01

Electronic cigarettes (EC) may have a potential for public health benefit as a safer alternative to smoking, but questions have been raised about whether EC should be licensed as a medicine, with accurate labelling of nicotine content. This study determined the nicotine content of the cartridges of the most popular EC brands in the United Kingdom and the nicotine levels they deliver in the vapour, and estimated the safety and consistency of nicotine delivery across batches of the same product as a proxy for quality control for individual brands and within the industry. We studied five UK brands (six products) with high internet popularity. Two samples of each brand were purchased 4 weeks apart, and analysed for nicotine content in the cartridges and nicotine delivery in vapour. The nicotine content of cartridges within the same batch varied by up to 12% relative standard deviation (RSD) and the mean difference between different batches of the same brand ranged from 1% [95% confidence interval (CI) = -5 to 7%] to 20% (95% CI=14-25%) for five brands and 31% (95% CI=21-39%) for the sixth. The puffing schedule used in this study vaporized 10-81% of the nicotine present in the cartridges. The nicotine delivery from 300 puffs ranged from ∼2 mg to ∼15 mg and was not related significantly to the variation of nicotine content in e-liquid (r=0.06, P=0.92). None of the tested products allowed access to e-liquid or produced vapour nicotine concentrations as high as conventional cigarettes. There is very little risk of nicotine toxicity from major electronic cigarette (EC) brands in the United Kingdom. Variation in nicotine concentration in the vapour from a given brand is low. Nicotine concentration in e-liquid is not well related to nicotine in vapour. Other EC brands may be of lower quality and consumer protection regulation needs to be implemented, but in terms of accuracy of labelling of nicotine content and risks of nicotine overdose, regulation over and above

Labeling Lanreotide with 125I and 188Re. China

International Nuclear Information System (INIS)

Bai Hongsheng

2000-01-01

Lanreotide (D-β-Nal-Cys-Try-D-Trp-Lys-Val-Cys-Thr-NH2) is a new somatostatin analogue. It can bind to human somatostatin receptor (hSSTR) subtype 2 through 5 with high affinity and to hSSTR subtype 1 with low affinity. We investigate labeling condition, quality control and stability in vitro of 125 I-Lanreotide and 188 Re-lanreotide respectively. (A) Lanreotide is labeled with 125 I using Chloramine T. The effect of reaction condition (such as reaction time, pH value, Lanreotide amount, quantity of Chloramine T and reaction volume) on labeling yield is investigated in detail. (B) The labeling yield and radiochemical purity (RP) is measured with paper chromatography (PC) and Sep-Pak C 18 Cartridge. For PC method, 125 I-Lanreotide is spotted on the Whatman No.1 paper and developed in the mixture of CH 3 CH 2 CH 2 CH 2 OH and CH 3 CH 2 OH and NH 4 OH (v/v/v=5:2:1), the Rf value of every component in the mobile phase is given in table 1. For Sep-Pak C 18 Cartridge methods each cartridge is washed with 10 ml of ethanol followed by 10 ml of iso-CH 3 CH 2 CH 2 OH solution. Aliquots of 0.1 mI sample is loaded onto the cartridge, unbound peptide (sodium iodine-125) is eluted with 5 ml of 0.5mol/L sodium acetate solution, 125 I-Lanreotide is eluted with 5 mI of 95% aqueous ethanol solution. (C) The stability of 125 I-Lanreotide in vitro is investigated by labeling compound incubating for 48 hours at 37 deg. C in the 0.9% sodium chloride solution and RP is tested by PC at specific time intervals. (D) Lanreotide is labeled directly with 188 Re via the mixture of citrate and tartate using stannous chloride as reduced agent. The influence of reaction conditions such as pH, temperature, amount of stannous chloride, amount of Lanreotide and reaction time on labeling yield is investigated in detail. At the time, the stability in vitro quality control and animal test are evaluated

Update of the BIPM.RI(II)-K1.Tc-99m comparison of activity measurements for the radionuclide {sup 99m}Tc to include new results for the LNE-LNHB and the NPL

Energy Technology Data Exchange (ETDEWEB)

Michotte, C.; Courte, S.; Ratel, G. [Bureau International des Poids et Mesures (BIPM), 92 - Sevres (France); Moune, M. [LNE-LNHB, Laboratoire national de metrologie et d' essais-Laboratoire National Henri Becquerel, Gif sur Yvette (France); Johansson, L.; Keightley, J. [National Physical Laboratory (NPL), Middlesex (United Kingdom)

2010-12-15

In 2007 and 2008 respectively, the Laboratoire national de metrologie et d'essais -Laboratoire national Henri Becquerel (LNE-LNHB), France and the National Physical Laboratory (NPL), UK, submitted ampoules with between 10 MBq and 130 MBq activity of {sup 99m}Tc to the International Reference System (SIR), to update their results in the BIPM.RI(II)-K1.Tc-99m comparison. Together with the four other national metrology institutes (NMI) that are participants, thirteen samples have been submitted since 1983. The key comparison reference value (KCRV) has been recalculated to include the latest primary results of the PTB and the LNE-LNB as this makes the evaluation more robust. The degrees of equivalence between each equivalent activity measured in the SIR are given in the form of a matrix for all six NMIs. A graphical presentation is also given. (authors)

Multiple and high-throughput droplet reactions via combination of microsampling technique and microfluidic chip

KAUST Repository

Wu, Jinbo

2012-11-20

Microdroplets offer unique compartments for accommodating a large number of chemical and biological reactions in tiny volume with precise control. A major concern in droplet-based microfluidics is the difficulty to address droplets individually and achieve high throughput at the same time. Here, we have combined an improved cartridge sampling technique with a microfluidic chip to perform droplet screenings and aggressive reaction with minimal (nanoliter-scale) reagent consumption. The droplet composition, distance, volume (nanoliter to subnanoliter scale), number, and sequence could be precisely and digitally programmed through the improved sampling technique, while sample evaporation and cross-contamination are effectively eliminated. Our combined device provides a simple model to utilize multiple droplets for various reactions with low reagent consumption and high throughput. © 2012 American Chemical Society.

Comparison of iSTAT and EPOC Blood Analyzers

Science.gov (United States)

2017-10-25

gold standard laboratory testing to two POC devices—iSTAT and EPOC—with and without expired cartridges and conditioned cartridges. The study was...analysis across a range of environmental conditions and, in extreme circumstances, use beyond the expiration date. We compared gold standard laboratory...BE) extra cellular fluid, BE blood, sulfur dioxide, Hgb) to gold standard measurements conducted by the central laboratory. The study also compared

Hazard categorization of K Basin water filtration upgrade project

International Nuclear Information System (INIS)

Conn, K.R.

1995-01-01

This supporting document provides the hazards categorization for the K Basin Water Filtration Upgrade Project at K East. All activities associated with the project are less than Hazard Category 3, except for the handling of the ECO-ROK liners containing spent filter cartridges. All activities involving the handling of liners, containing spent cartridges, by monorail, forklift or mobile crane are classified as Hazard Category 3

Chapter 3. Determination of semivolatile organic compounds and polycyclic aromatic hydrocarbons in solids by gas chromatography/mass spectrometry

Science.gov (United States)

Zaugg, Steven D.; Burkhardt, Mark R.; Burbank, Teresa L.; Olson, Mary C.; Iverson, Jana L.; Schroeder, Michael P.

2006-01-01

A method for the determination of 38 polycyclic aromatic hydrocarbons (PAHs) and semivolatile organic compounds in solid samples is described. Samples are extracted using a pressurized solvent extraction system. The compounds of interest are extracted from the solid sample twice at 13,800 kilopascals; first at 120 degrees Celsius using a water/isopropyl alcohol mixture (50:50, volume-to-volume ratio), and then the sample is extracted at 200 degrees Celsius using a water/isopropyl alcohol mixture (80:20, volume-to-volume ratio). The compounds are isolated using disposable solid-phase extraction (SPE) cartridges containing divinylbenzene-vinylpyrrolidone copolymer resin. The cartridges are dried with nitrogen gas, and then sorbed compounds are eluted from the SPE material using a dichloromethane/diethyl ether mixture (80:20, volume-to-volume ratio) and passed through a sodium sulfate/Florisil SPE cartridge to remove residual water and to further clean up the extract. The concentrated extract is solvent exchanged into ethyl acetate and the solvent volume reduced to 0.5 milliliter. Internal standard compounds are added prior to analysis by capillary-column gas chromatography/mass spectrometry. Comparisons of PAH data for 28 sediment samples extracted by Soxhlet and the accelerated solvent extraction (ASE) method described in this report produced similar results. Extraction of PAH compounds from standard reference material using this method also compared favorably with Soxhlet extraction. The recoveries of PAHs less than molecular weight 202 (pyrene or fluoranthene) are higher by up to 20 percent using this ASE method, whereas the recoveries of PAHs greater than or equal to molecular weight 202 are equivalent. This ASE method of sample extraction of solids has advantages over conventional Soxhlet extraction by increasing automation of the extraction process, reducing extraction time, and using less solvent. Extract cleanup also is greatly simplified because SPE replaces

Pneumatic probe with laser interferometer

International Nuclear Information System (INIS)

Wilkens, P.H.

1978-01-01

Improvements to upgrade the accuracy of Rotacon probes by a complete redesign of probe to include a Michelson interferometer to replace the existing long-range capacity transducer are described. This has resulted in a compact and interchangeable probe cartridge with a 3 μin. resolution and accuracy; the cartridge can be installed and replaced in the Rotacon gauge with the minimum of realignment, which should reduce our dependence on operator skill. In addition, the stylus contact force can be reduced to 750 mg for the contacting types, but an alternative feature, which we are still developing, will use a gas jet cushion in place of the stylus to provide a noncontacting version of the same basic probe cartridge. This device is very sensitive to external vibration effects because it is virtually frictionless

Information sampling behavior with explicit sampling costs

Science.gov (United States)

Juni, Mordechai Z.; Gureckis, Todd M.; Maloney, Laurence T.

2015-01-01

The decision to gather information should take into account both the value of information and its accrual costs in time, energy and money. Here we explore how people balance the monetary costs and benefits of gathering additional information in a perceptual-motor estimation task. Participants were rewarded for touching a hidden circular target on a touch-screen display. The target’s center coincided with the mean of a circular Gaussian distribution from which participants could sample repeatedly. Each “cue” — sampled one at a time — was plotted as a dot on the display. Participants had to repeatedly decide, after sampling each cue, whether to stop sampling and attempt to touch the hidden target or continue sampling. Each additional cue increased the participants’ probability of successfully touching the hidden target but reduced their potential reward. Two experimental conditions differed in the initial reward associated with touching the hidden target and the fixed cost per cue. For each condition we computed the optimal number of cues that participants should sample, before taking action, to maximize expected gain. Contrary to recent claims that people gather less information than they objectively should before taking action, we found that participants over-sampled in one experimental condition, and did not significantly under- or over-sample in the other. Additionally, while the ideal observer model ignores the current sample dispersion, we found that participants used it to decide whether to stop sampling and take action or continue sampling, a possible consequence of imperfect learning of the underlying population dispersion across trials. PMID:27429991

Derivatization Ion Chromatography for the Determination of Monoethanolamine in Presence of Hydrazine in PHWR Steam-Water Circuits

Directory of Open Access Journals (Sweden)

Ayushi D.

2011-01-01

Full Text Available A simple, rapid and accurate method for the determination of monoethanolamine (MEA in PHWR steam-water circuits has been developed. MEA is added in the feed water to provide protection against corrosion while hydrazine is added to scavenge dissolved oxygen. The quantitative determination of MEA in presence of hydrazine was accomplished using derivatization ion chromatography with conductometric detection in nonsuppressed mode. A Metrosep cation 1-2 analytical column and a Metrosep cartridge were used for cation separation. A mixture of 4 mM tartaric acid, 20% acetone and 0.05 mM HNO3 was used as eluent. Acetone in the mobile phase leads to the formation of different derivatives with MEA and hydrazine. The interferences due Na+ and NH4 + were eliminated by adopting a simple pretreatment procedure employing OnGuard-H cartridge. The limit of detection limit of MEA was 0.1 μg mL−1 and the relative standard deviation was 2% for the overall method. The recovery of MEA added was in the range 95%–102%. The method was applied to the determination of MEA in steam generator water samples.

Samples and Sampling Protocols for Scientific Investigations | Joel ...

African Journals Online (AJOL)

... from sampling, through sample preparation, calibration to final measurement and reporting. This paper, therefore offers useful information on practical guidance on sampling protocols in line with best practice and international standards. Keywords: Sampling, sampling protocols, chain of custody, analysis, documentation ...

Simultaneous analysis of non-steroidal anti-inflammatory drugs and estrogenic hormones in water and wastewater samples using gas chromatography–mass spectrometry and gas chromatography with electron capture detection

International Nuclear Information System (INIS)

Migowska, Natalia; Caban, Magda; Stepnowski, Piotr; Kumirska, Jolanta

2012-01-01

Non-steroidal anti-inflammatory drugs are the group of pharmaceuticals that is most often found in the environment, whereas estrogenic hormones are considered to be potent endocrine disruptors. However, the fate and persistence of these compounds in the environment are still unclear. In this study we propose two approaches for determining these compounds in environmental water samples: GC–MS using time windows and operating in selected ion-monitoring mode (SIM) and, for the first time, gas chromatography with electron capture detection (GC–ECD). The identification criteria of both methods fulfilled the requirements of Directive 2002/657/EC. The use of time windows improved the sensitivity of GC–MS measurements. In GC–MS analysis the pharmaceuticals were determined as trimethylsilyl, in GC–ECD as pentafluoropropionyl derivatives. The influence of such parameters as the type of reagent, type of solvent, reaction time, reaction temperature and microwave irradiation in a household microwave oven on the efficacy of silylation was investigated. Derivatization using N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) and 1% trimethylchlorosilane (TMCS) in pyridine (1:1, v/v) for 30 min in 60 °C was found to be optimal. Optimization of the solid phase extraction procedure (SPE) confirmed that the application of Oasis HLB cartridges, the acidification of loading samples to pH 2 and the use of methanol as eluent gave the best absolute recoveries (ARs) of the target compounds. The following ARs of all the compounds were achieved: 58.2–106.8% in influent wastewater, 77.8–103.4% in effluent wastewater and 81.2–101.9% in surface water samples. Validation of the SPE–GC–MS method enables 13 pharmaceuticals to be determined with MDLs between 3.3 and 343.6 ng/L, depending on the analytes and matrices. GC–ECD analysis enables the determination of 6 pharmaceuticals in surface water samples with MDLs between 0.7 and 5.4 ng/L. The proposed methods were successfully

Determination of selected UV filters in indoor dust by matrix solid-phase dispersion and gas chromatography-tandem mass spectrometry.

Science.gov (United States)

Negreira, N; Rodríguez, I; Rubí, E; Cela, R

2009-07-31

A simple, inexpensive sample preparation procedure, based on the matrix solid-phase dispersion (MSPD) technique, for the determination of six UV filters: 2-ethylhexyl salicylate (EHS), 3,3,5-trimethylcyclohexyl salicylate (Homosalate, HMS), 3-(4-methylbenzylidene) camphor (4-MBC), isoamyl-p-methoxycinnamate (IAMC), 2-ethylhexyl-p-methoxycinnamate (EHMC) and octocrylene (OCR), in dust from indoor environments is presented and the influence of several operational parameters on the extraction performance discussed. Under the final working conditions, sieved samples (0.5 g) were mixed with the same amount of anhydrous sodium sulphate and dispersed with 2 g of octadecyl bonded silica (C18) in a mortar with a pestle. This blend was transferred to a polypropylene solid-phase extraction cartridge containing 2 g of activated silica, as the clean-up co-sorbent. The cartridge was first rinsed with 5 mL of n-hexane and the analytes were then recovered with 4 mL of acetonitrile. This extract was adjusted to 1 mL, filtered and the compounds were determined by gas chromatography combined with tandem mass spectrometry (GC-MS/MS). Recoveries for samples spiked at two different concentrations ranged between 77% and 99%, and the limits of quantification (LOQs) of the method between 10 and 40 ng g(-1). Analysis of settled dust from different indoor areas, including private flats, public buildings and vehicle cabins, showed that EHMC and OCR were ubiquitous in this matrix, with maximum concentrations of 15 and 41 microg g(-1), respectively. Both UV filters were also quantified in dust reference material SRM 2585 for first time. EHS, 4-MBC and IAMC were detected in some of the analyzed samples, although at lower concentrations than EHMC and OCR.

Development and Validation of HPLC Method for Determination of Crocetin, a constituent of Saffron, in Human Serum Samples

Directory of Open Access Journals (Sweden)

Amir Hooshang Mohammadpour

2013-01-01

Full Text Available Objective(s:The present study reports the development and validation of a sensitive and rapid extraction method beside high performance liquid chromatographic method for the determination of crocetin in human serum. Materials and Methods:The HPLC method was carried out by using a C18 reversed-phase column and a mobile phase composed of methanol/water/acetic acid (85:14.5:0.5 v/v/v at the flow rate of 0.8 ml/min. The UV detector was set at 423 nm and 13-cis retinoic acid was used as the internal standard. Serum samples were pretreated with solid-phase extraction using Bond Elut C18 (200mg cartridges or with direct precipitation using acetonitrile. Results:The calibration curves were linear over the range of 0.05-1.25 µg/ml for direct precipitation method and 0.5-5 µg/ml for solid-phase extraction. The mean recoveries of crocetin over a concentration range of 0.05-5 µg/ml serum for direct precipitation method and 0.5-5 µg/ml for solid-phase extraction were above 70 % and 60 %, respectively. The intraday coefficients of variation were 0.37- 2.6% for direct precipitation method and 0.64 - 5.43% for solid-phase extraction. The inter day coefficients of variation were 1.69 – 6.03% for direct precipitation method and 5.13-12.74% for solid-phase extraction, respectively. The lower limit of quantification for crocetin was 0.05 µg/ml for direct precipitation method and 0.5 µg/ml for solid-phase extraction. Conclusion: The validated direct precipitation method for HPLC satisfied all of the criteria that were necessary for a bioanalytical method and could reliably quantitate crocetin in human serum for future clinical pharmacokinetic study

Proteomic analysis of polypeptides captured from blood during extracorporeal albumin dialysis in patients with cholestasis and resistant pruritus.

Directory of Open Access Journals (Sweden)

Marina Gay

Full Text Available Albumin dialysis using the molecular adsorbent recirculating system (MARS is a new therapeutic approach for liver diseases. To gain insight into the mechanisms involved in albumin dialysis, we analyzed the peptides and proteins absorbed into the MARS strong anion exchange (SAX cartridges as a result of the treatment of patients with cholestasis and resistant pruritus. Proteins extracted from the SAX MARS cartridges after patient treatment were digested with two enzymes. The resulting peptides were analyzed by multidimensional liquid chromatography coupled to tandem mass spectrometry. We identified over 1,500 peptide sequences corresponding to 144 proteins. In addition to the proteins that are present in control albumin-derived samples, this collection includes 60 proteins that were specific to samples obtained after patient treatment. Five of these proteins (neutrophil defensin 1 [HNP-1], secreted Ly-6/uPAR-related protein 1 [SLURP1], serum amyloid A, fibrinogen alpha chain and pancreatic prohormone were confirmed to be removed by the dialysis procedure using targeted selected-reaction monitoring MS/MS. Furthermore, capture of HNP-1 and SLURP1 was also validated by Western blot. Interestingly, further analyses of SLURP1 in serum indicated that this protein was 3-fold higher in cholestatic patients than in controls. Proteins captured by MARS share certain structural and biological characteristics, and some of them have important biological functions. Therefore, their removal could be related either to therapeutic or possible adverse effects associated with albumin dialysis.

Solid-phase extraction clean-up of ciguatoxin-contaminated coral fish extracts for use in the mouse bioassay.

Science.gov (United States)

Wong, Chun Kwan; Hung, Patricia; Lee, Kellie L H; Kam, Kai Man

2009-02-01

Florisil solid-phase extraction (SPE) cartridges were used for purifying ciguatoxin (CTX)-contaminated coral fish extracts, with the aim of removing extracted lipid but retaining optimal level of CTXs in the purified fractions. The CTX-containing fraction (target fraction) in fish ether extract was isolated and purified by eluting through a commercially available Florisil cartridge with hexane-acetone-methanol solvent mixtures of increasing polarity (hexane-acetone (4:1, v/v) < acetone-methanol (7:3, v/v) < 100% methanol). Application of Florisil SPE using acetone-methanol (7:3, v/v) condition facilitated the separation of 4.2 +/- 0.4 mg (mean +/- standard error of the mean (SEM)) of purified target fraction from 20 mg ether extract with good retention of CTXs. The mouse bioassay was used to demonstrate that the average CTX recovery of the target fraction from CTX-spiked samples was 75.8% +/- 3.3%, which was significantly increased by 96.7% +/- 15% when compared with CTX recovery from ether extracts (44.8% +/- 5.2%) without performing SPE purification. Over 70% of non-target lipids were removed in which no CTX toxicity was found. Moreover, the target fractions of both CTX-spiked and naturally CTX-contaminated samples gave more prominent toxic responses of hypothermia and/or induced more rapid death of the mice. The use of acetone-methanol (7:3, v/v) condition in the elution could significantly improve overall recovery of CTXs, while minimizing the possible interferences of lipid matrix from co-extractants on mice.

The sorption-chromaticity determination of Fe(III in the waters of the galvanic production

Directory of Open Access Journals (Sweden)

P. T. Sukhanov

2017-01-01

Full Text Available Developed out express Sorption-colorimetric methods for the determination of iron in water, based on the sorption concentration of detecting component of the solution impregnated in the polyurethane foam, the formation on the surface of a colored compound and then its definition in the sorbent matrix by measuring color intensity or chromaticity characteristics. The first method is based on determining the agitation of the sample solution with a tablet impregnated with PPU known mass, from which the air bubbles are removed, the second dynamic – by sampling by suction solution in the analytical cartridge impregnated with PPU. Discoloration polyurethane indicates the presence of iron (III in water, and its content was determined by comparing the color intensity of foam tablets previously prepared color chart or chromaticity characteristics comparing analyte and standard solutions. The conditions of sorption-photometric analysis: the concentration of the photometric reagent impregnated in the foam, the degree of loading it impregnant, the phases of contact, the acidity of the environment. When using analytical cartridges lower limit of detection is 2 times higher, and the measurement error to 3.5% lower than with the tablets. The proposed test methods using polyurethane enable to carry out the analysis of wash water and the total flow of galvanizing plant before and after neutralization station “on the spot”, without the use of sophisticated instruments and highly skilled operator.

Sampling and chemical analysis in environmental samples around Nuclear Power Plants and some environmental samples

Energy Technology Data Exchange (ETDEWEB)

Cho, Yong Woo; Han, Man Jung; Cho, Seong Won; Cho, Hong Jun; Oh, Hyeon Kyun; Lee, Jeong Min; Chang, Jae Sook [KORTIC, Taejon (Korea, Republic of)

2002-12-15

Twelve kinds of environmental samples such as soil, seawater, underground water, etc. around Nuclear Power Plants(NPPs) were collected. Tritium chemical analysis was tried for the samples of rain water, pine-needle, air, seawater, underground water, chinese cabbage, a grain of rice and milk sampled around NPPs, and surface seawater and rain water sampled over the country. Strontium in the soil that sere sampled at 60 point of district in Korea were analyzed. Tritium were sampled at 60 point of district in Korea were analyzed. Tritium were analyzed in 21 samples of surface seawater around the Korea peninsular that were supplied from KFRDI(National Fisheries Research and Development Institute). Sampling and chemical analysis environmental samples around Kori, Woolsung, Youngkwang, Wooljin Npps and Taeduk science town for tritium and strontium analysis was managed according to plans. Succeed to KINS after all samples were tried.

Pierre Gy's sampling theory and sampling practice heterogeneity, sampling correctness, and statistical process control

CERN Document Server

Pitard, Francis F

1993-01-01

Pierre Gy's Sampling Theory and Sampling Practice, Second Edition is a concise, step-by-step guide for process variability management and methods. Updated and expanded, this new edition provides a comprehensive study of heterogeneity, covering the basic principles of sampling theory and its various applications. It presents many practical examples to allow readers to select appropriate sampling protocols and assess the validity of sampling protocols from others. The variability of dynamic process streams using variography is discussed to help bridge sampling theory with statistical process control. Many descriptions of good sampling devices, as well as descriptions of poor ones, are featured to educate readers on what to look for when purchasing sampling systems. The book uses its accessible, tutorial style to focus on professional selection and use of methods. The book will be a valuable guide for mineral processing engineers; metallurgists; geologists; miners; chemists; environmental scientists; and practit...

Systematic Sampling and Cluster Sampling of Packet Delays

OpenAIRE

Lindh, Thomas

2006-01-01

Based on experiences of a traffic flow performance meter this papersuggests and evaluates cluster sampling and systematic sampling as methods toestimate average packet delays. Systematic sampling facilitates for exampletime analysis, frequency analysis and jitter measurements. Cluster samplingwith repeated trains of periodically spaced sampling units separated by randomstarting periods, and systematic sampling are evaluated with respect to accuracyand precision. Packet delay traces have been ...

Synthesis of 14C-dehydrocorydaline chloride