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1.
NARL (the Australian National Analytical Reference Laboratory) is preparing a pureed tomato reference material spiked with residue concentrations of a range of pesticide chemicals relevant to the Australian horticultural industry. Traceable certified pesticide concentration values will be established using both isotope dilution mass spectrometry primary methods (developed within NARL) and measurements carried out by a number of experienced laboratories. As far as we are aware, there is no other similar CRM available anywhere in the world. The need for such a material is evident from the results of interlaboratory proficiency studies conducted by NARL among Australian and Asia-Pacific residue testing laboratories. Many participants are experiencing difficulties with the analysis of pesticide residues in fruit and vegetables at concentrations of regulatory significance. Chemicals such as methamidophos (an organophosphorus pesticide widely used on tomato crops) are causing particular problems. In a pilot study, a number of units of control (unspiked tomato) and the candidate reference material were prepared and packaged into lacquered steel cans which were sealed and sterilised by immersion in boiling water. Accelerated stability testing of the packaged material was conducted using isochronous measurement. All of the pesticides showed some degree of degradation after 4 weeks of storage at 50?°C, and after 168 days of storage at room temperature. However, all appeared to be stable after 168 days of freezer storage. Homogeneity testing involved duplicate test portions taken from every 50th unit of reference material. An experimental protocol was devised with the aim of minimising the analytical variability and assuring the quality of the data generated. There is some degree of inhomogeneity in the prepared material and a small fill trend is also indicated. Potential improvements to the spiking and preparation procedure have been identified and it is planned to prepare a second batch of both control and spiked material for further homogeneity trials and for certification of the pesticide concentrations. 相似文献
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The International Atomic Energy Agency maintains a database of internationally available certified reference materials (CRM) of natural matrices. This database is periodically updated, and presently documents nearly 25,000 measurands in 1700 materials. The organic constituents are classified in five major groups of analytes – aliphatic and aromatic hydrocarbons (A), chlorinated hydrocarbons (B), pesticides (C), organometallic compounds (D) and other organic constituents (nutrients, etc.) (E). The matrices include natural materials such as body fluids, food products, soils, and sediments, terrestrial (e.g. plants), and anthropogenic products (e.g. dust, fly ash). These five organic groups of analytes encompass more than 2000 measurands for 420 different analytes in 230 materials. Of these measurands, 1682 (68%) are certified, and 768 (32%) are provided as informational values. Within each major group of analytes, measurands reported as informational values accounted for: A (35%); B (35%); C (26%); D (10%), and E (22%). The high proportion of informational values (i.e. non-certified values) for A, B, and C, compares well with a similar but undesirable situation faced in the nineteen-seventies in the inorganic area when simultaneous multielement techniques became available. In the case of D and E, it appears that mostly targeted analytes are measured, leading to a cohesive certification profile. Although the IAEA database is not equally comprehensive for all groups of analytes cited above, it can still serve as an useful indicator of the status of organic constituents in RMs. 相似文献
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The International Atomic Energy Agency maintains a database of internationally available certified reference materials (CRM) of natural matrices. This database is periodically updated, and presently documents nearly 25,000 measurands in 1,700 materials. The organic constituents are classified in five major groups of analytes aliphatic and aromatic hydrocarbons (A), chlorinated hydrocarbons (B), pesticides (C), organometallic compounds (D) and other organic constituents (nutrients, etc.) (E). The matrices include natural materials such as body fluids, food products, soils, and sediments, terrestrial (e.g. plants), and anthropogenic products (e.g. dust, fly ash). These five organic groups of analytes encompass more than 2000 measurands for 420 different analytes in 230 materials. Of these measurands, 1,682 (68%) are certified, and 768 (32%) are provided as informational values. Within each major group of analytes, measurands reported as informational values accounted for: A (35%); B (35%); C (26%); D (10%), and E (22%). The high proportion of informational values (i.e. non-certified values) for A, B, and C, compares well with a similar but undesirable situation faced in the nineteen-seventies in the inorganic area when simultaneous multielement techniques became available. In the case of D and E, it appears that mostly targeted analytes are measured, leading to a cohesive certification profile. Although the IAEA database is not equally comprehensive for all groups of analytes cited above, it can still serve as an useful indicator of the status of organic constituents in RMs. 相似文献
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The mass fractions of six organochlorine pesticides in a fish oil certified reference material (CRM) have been determined
using multiple methods of analysis. Fish oil was extracted from the filet of Tilapia fish collected from the River Nile, and
this CRM was recently issued by the National Institute of Standards (NIS). It can be used as natural matrix CRM for organochlorine
pesticides determination in fish and for marine environmental measurement purposes. The analytical methods used are described,
and the obtained results were combined to calculate the mass fractions of the six detected organochlorine pesticides and their
associated uncertainty values. It has been concluded that mass fractions of four pesticides are certified values. These are
1,1-(dichloroethylidene)bis[4-chlorobenzene](4,4′-DDE), 1,1-(2,2,-dichloroethylidene)bis[4-chlorobenzene] (4,4′-DDD), 1-chloro-2-[2,2,2-trichloro-1-(4-chlorophenyl)ethyl]benzene
(2,4′-DDT) and 1,1-(2,2,2-trichloroethylidene)bis[4-chlorobenzene] (4,4′-DDT). Meanwhile, mass fractions of two pesticides
were reference values. These are heptachlor and 1-chloro-2-[2,2-dichloro-1-(4-chlorophenyl)ethyl]benzene (2,4′-DDD). 相似文献
6.
Zeisler R Paul RL Oflaz Spatz R Yu LL Mann JL Kelly WR Lang BE Leigh SD Fagan J 《Analytical and bioanalytical chemistry》2011,399(1):509-517
A material containing single-wall carbon nanotubes (SWCNTs) with other carbon species, catalyst residues, and trace element
contaminants has been prepared by the National Institute of Standards and Technology for characterization and distribution
as Standard Reference Material SRM 2483 Carbon Nanotube Soot. Neutron activation analysis (NAA) and inductively coupled plasma
mass spectrometry (ICP–MS) were selected to characterize the elemental composition. Catalyst residues at percentage mass fraction
level were determined with independent NAA procedures and a number of trace elements, including selected rare earth elements,
were determined with NAA and ICP–MS procedures. The results of the investigated materials agreed well among the NAA and ICP–MS
procedures and good agreement of measured values with certified values was found in selected SRMs included in the analyses.
Based on this work mass fraction values for catalyst and trace elements were assigned to the candidate SRM. 相似文献
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Ilona Šperlingová Ludmila Dabrowská Vladimír Stránský Šárka Dušková Jan Kučera Monika Tvrdíková Milon Tichy 《Analytical and bioanalytical chemistry》2010,397(2):433-438
Ethylene glycol monobutyl ether (EGBE), an industrial solvent, is absorbed by the body not only by inhalation but also by
dermal absorption (liquid or vapour). EGBE is metabolized to butoxyacetic acid (BAA). Pooled freeze-dried urine candidate
reference material (RM) was prepared from urine obtained from persons occupationally exposed to EGBE. This material has the
advantage of containing butoxyacetic acid in both the free and conjugated (glutamine and glycine) forms, as found in native
urine. In all GC method modifications used, acid hydrolysis was used to release BAA from its conjugated form. The amount of
butoxyacetic acid in homogeneity and stability testing was measured by GC after derivatisation with N-tert-butyldimethylsilyl-N-methyltrifluoroacetamide. Detection was by MS in EI mode, in the authors’ laboratory. For interlaboratory comparison of the
reference material GC methods with MS, FID, and ECD were used. Different extraction solvents (dichloromethane–isopropanol
2:1, ethyl acetate, or dichloromethane) and derivatisation reagents (trimethylsilyldiazomethane, N-tert-butyldimethylsilyl-N-methyltrifluoroacetamide) were used. Using ANOVA (at the statistical level α = 0.05) no changes were found in the concentration of butoxyacetic acid during fifteen month isochronous stability testing,
or in homogeneity testing. The uncertainty contributions were u
h = 8.8 mg L−1 and u
s = 6.5 mg L−1. The concentration of butoxyacetic acid in freeze-dried urine RM was evaluated from the results of eight laboratory data
sets within an interlaboratory comparison by use of the interactive statistical software IPECA. The contribution to total
uncertainty derived from interlaboratory comparison was u
i = 12.7 mg L−1. The reference value (c = 273 ± 33 mg L−1) is an unweighted arithmetic average of accepted results. The value is traceable to the pure butoxyacetic acid (98% w/w; Acros Organic #257760010) used as calibrant. The uncertainty given is combined expanded uncertainty derived from the results
from interlaboratory comparison, and from homogeneity and stability tests (k = 2). The reference material will be used to verify method performance in the biological monitoring of occupational exposure
to EGBE. 相似文献
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The production of certified reference materials (CRM) requires a comprehensive consideration of which analytes and materials
to select. The present study describes the pre-tests for the production of CRM for nitroimidazoles in plasma or muscle. By
means of a commutability study, four factors, namely matrix (plasma – muscle), species (turkey – pig), matrix condition (fresh
- lyophilized) and measurement technique (GC-NCI/MS-LC-MSMS) were checked for their usability. The results showed that the
matrices, matrix conditions, as well as the species analyzed did not produce any relevantly different measurement results.
Varying significantly and subject to a systematic error were those results which were determined by means of different measurement
techniques.
Presented at BERM-10, April 2006, Charleston, SC, USA 相似文献
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Zs. Szántó M. Hult U. Wätjen T. Altzitzoglou 《Journal of Radioanalytical and Nuclear Chemistry》2007,273(1):167-170
The paper presents the results of radiological investigation of several mushroom samples collected in the fall of 2004 in
different parts of Europe. The work was performed in order to support decision making to develop and produce a certified reference
material for quality assurance of radionuclide measurements in environmental samples. The levels of 137Cs in mushrooms varied widely ranging from 0.6 to 4300 Bq/kg on dry mass basis, while those of natural 40K were relatively constant. In one sample 60Co of unknown origin was detected (25±2 Bq/kg dry mass), while 90Sr concentrations were usually below the detection limit (<150 mBq/kg dry mass). 相似文献
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A carefully controlled interlaboratory comparison of analyses by size exclusion chromatography of a poly(vinyl acetate) whole polymer showed that compatible measurements could be made of the molar mass distribution. The characterized sample is available as a Community Bureau of Reference (BCR) test material. 相似文献
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Della W.M. Sin Pui-kwan ChanSamuel T.C. Cheung Yee-Lok WongSiu-kay Wong Chuen-shing MokYiu-chung Wong 《Analytica chimica acta》2012
This paper presents the preparation of a candidate certified reference material (CRM) of cypermethrin in green tea, GLHK-11-01a according to the requirements of ISO Guide 34 and 35. Certification of the material was performed using a newly developed isotope dilution mass spectrometry (IDMS) approach, with gas chromatography high resolution mass spectrometry (GC–HRMS) and gas chromatography–tandem mass spectrometry (GC–MS/MS). Statistical analysis (one-way ANOVA) showed excellent agreement of the analytical data sets generated from the two mass spectrometric detections. The characterization methods have also been satisfactorily applied in an Asia-Pacific Metrology Program (APMP) interlaboratory comparison study. Both the GC–HRIDMS and GC–IDMS/MS methods proved to be sufficiently reliable and accurate for certification purpose. The certified value of cypermethrin in dry mass fraction was 148 μg kg−1 and the associated expanded uncertainty was 14 μg kg−1. The uncertainty budget was evaluated from sample in homogeneity, long-term and short-term stability and variability in the characterization procedure. GLHK-11-01a is primarily developed to support the local and wider testing community on need basis in quality assurance work and in seeking accreditation. 相似文献
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A. R. Bleise B. Smodiš D. Glavic-Cindro R. M. Parr 《Journal of Radioanalytical and Nuclear Chemistry》2001,248(1):205-209
The International Atomic Energy Agency (IAEA) maintains a database of biological and environmental reference materials of natural origin (human and animal tissues, foods, plants, soils, sediments, etc.) for trace elements, radionuclides, stable isotopes, organic contaminants and other related measurands. The purpose is to help analysts to select reference materials for quality assurance purposes that match as closely as possible (i.e., with respect to matrix type and concentrations of the measurands of interest) the real samples that are to be analyzed. Former versions of this database were prepared in co-operation with the United Nations Environment Programme (UNEP), and provided as hardcopies free of charge. The latest version was from 1995. More recently the database has been updated by the IAEA so that it now contains more than 22,500 values (mass fraction or concentration) for 660 different measurands and 1,705 reference materials developed by 56 producers from 22 countries. This paper gives an overview of the structure and content of the database and of the two ways it may be browsed. Emphasis is given to reference materials that are intended to verifying analysis for radioanalytical measurements. The database is soon accessible on-line, cost-free, via the internet. 相似文献
15.
An effective process for the purification of folic acid candidate reference material with preparative high-performance liquid chromatography (Pre-HPLC) was developed in this study. During the process of experimental operation, parameters including the influences of mobile phase, flow rate, and injection volume on the purity and yield were investigated, and the optimized conditions were as follows: the mobile phase was acetonitrile and water in a gradient mode with flow rate of 16?mL/min and injection volume of 2.0?mL at concentration of 10?mg/mL. Under the conditions, the purity and yield of folic acid product were up to 99.4% and 21.0%, respectively, whereas the purity of folic acid raw material was 95.2%. The purified folic acid product was characterized by LC–MS, HPLC, Karl Fischer coulometer, and quantitative nuclear magnetic resonance (qNMR). Results proved that the main component of the product was folic acid and the purities determined by HPLC and qNMR were consistent. Two impurities including N-(4-aminobenzoyl)-L-glutamic acid and pteroic acid were further quantified by LC–MS. Compared with the recrystallization approach, the purity of folic acid obtained by Pre-HPLC increased from 98.2% to 99.4%. 相似文献
16.
R. Brennecke 《Fresenius' Journal of Analytical Chemistry》1991,339(6):399-401
Summary The use of extraction columns is a simple and effective clean-up technique which avoids emulsions, yields cleaner extracts and high recoveries, and saves effort, solvent and time. It can be recommended to all residue laboratories. 相似文献
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A batch of sulphydryl cotton microcolumns was prepared and charged with a mixed Hg standard solution (methyl-, ethyl- and inorganic Hg, 10 g l–1 as Hg, 3 ml) and stored at 4 °C in a light-tight box. At regular time intervals over a 4 month period microcolumns were removed and Hg species were quantified by gas chromatography microwave-induced plasma atomic emission spectrometry (after elution, extraction and derivatization steps). It was found that analyte recoveries for methyl- and inorganic Hg were quantitative over the 4 month period while ethyl-Hg species appeared to be stable for up to 2 months. 相似文献
20.
P. A. Sitnikov A. V. Kuchin A. G. Belykh I. N. Vaseneva Yu. I. Ryabkov 《Polymer Science Series D》2011,4(4):281-283
The conditions for preparing epoxy composite material in which rock containing analcime and montmorillonite serves as a filler
have been investigated. The introduction of filler in amounts of up to 1 wt % has increased strength characteristics and thermal
stability of the material by 20–25%. 相似文献