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1.
Two new marine sediment standard reference materials (SRMs) for the determination of organic contaminants 总被引:3,自引:0,他引:3
Wise SA Poster DL Schantz MM Kucklick JR Sander LC Lopez de Alda M Schubert P Parris RM Porter BJ 《Analytical and bioanalytical chemistry》2004,378(5):1251-1264
Two new marine sediment standard reference materials (SRMs), SRM 1941b Organics in Marine Sediment and SRM 1944 New York/New Jersey Waterway Sediment, have been recently issued by the National Institute of Standards and Technology (NIST) for the determination of organic contaminants including polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyl (PCB) congeners, and chlorinated pesticides. Both sediment SRMs were analyzed using multiple analytical methods including gas chromatography/mass spectrometry (GC/MS) on columns with different selectivity, reversed-phase liquid chromatography with fluorescence detection (for PAHs only), and GC with electron capture detection (for PCBs and pesticides only). SRM 1941b has certified concentrations for 24 PAHs, 29 PCB congeners, and 7 pesticides, and SRM 1944 has certified concentrations for 24 PAHs, 29 PCB congeners, and 4 pesticides. Reference concentrations are also provided for an additional 58 (SRM 1941b) and 39 (SRM 1944) PAHs, PCB congeners, and pesticides. SRM 1944, which was collected from multiple sites within New York/New Jersey coastal waterways, has contaminant concentrations that are generally a factor of 10–20 greater than SRM 1941b, which was collected in the Baltimore (Maryland) harbor. These two SRMs represent the most extensively characterized marine sediment certified reference materials available for the determination of organic contaminants.Electronic Supplementary Material Supplementary material is available in the online version of this article at . A link in the frame on the left on that page takes you directly to the supplementary material. 相似文献
2.
Wise SA Poster DL Kucklick JR Keller JM Vanderpol SS Sander LC Schantz MM 《Analytical and bioanalytical chemistry》2006,386(4):1153-1190
For the past 25 years the National Institute of Standards and Technology (NIST) has developed certified reference materials
(CRMs), known as standard reference materials (SRMs), for determination of organic contaminants in environmental matrices.
Assignment of certified concentrations has usually been based on combining results from two or more independent analytical
methods. The first-generation environmental-matrix SRMs were issued with certified concentrations for a limited number (5
to 10) of polycyclic aromatic hydrocarbons (PAHs) and polychlorinated biphenyls (PCBs). Improvements in the analytical certification
approach significantly expanded the number and classes of contaminants determined. Environmental-matrix SRMs currently available
include air and diesel particulate matter, coal tar, marine and river sediment, mussel tissue, fish oil and tissue, and human
serum, with concentrations typically assigned for 50 to 90 organic contaminants, for example PAHs, nitro-substituted PAHs,
PCBs, chlorinated pesticides, and polybrominated diphenyl ethers (PBDEs).
Electronic supplementary material Supplementary material is available in the online version of this article at and is accessible for authorized users. 相似文献
3.
Bezabeh DZ Bamford HA Schantz MM Wise SA 《Analytical and bioanalytical chemistry》2003,375(3):381-388
Gas chromatography/mass spectrometry (GC/MS) with negative ion chemical ionization (NICI) detection was utilized for quantitative determination of nitrated polycyclic aromatic hydrocarbons (nitro-PAHs) in diesel particulate-related standard reference materials (SRMs). Prior to GC/MS analysis, isolation of the nitro-PAHs from the complex diesel particulate extract was accomplished using solid phase extraction (SPE) and normal-phase liquid chromatographic (LC) fractionation using an amino/cyano stationary phase. Concentrations of eight to ten mononitro-PAHs and three dinitropyrenes were determined in three diesel particulate-related SRMs: SRM 1650a Diesel Particulate Matter, SRM 1975 Diesel Particulate Extract, and SRM 2975 Diesel Particulate Matter (Industrial Forklift). The results from GC/MS NICI using two different columns (5% phenyl methylpolysiloxane and 50% phenyl methylpolysiloxane) were compared to each other and to results from two other laboratories for selected nitro-PAHs. 1-Nitropyrene was the most abundant nitro-PAHs in each of the diesel particulate SRMs (19.8+/-1.1 micro g g(-1) particle in SRM 1650a and 33.1+/-0.6 micro g g(-1) particle in SRM 2975). Three dinitropyrene isomers were measured in SRM 1975 at 0.5-1.4 micro g g(-1) extract and in SRM 2975 at 1-3 micro g g(-1) particle. 相似文献
4.
Margarete S. Nocun Michele M. Schantz 《Analytical and bioanalytical chemistry》2013,405(16):5583-5593
Oxygenated polycyclic aromatic hydrocarbons (oxy-PAHs) have recently received much attention in discussions regarding the negative impacts of particulate matter (PM) on human health and the environment. The National Institute of Standards and Technology provides several environmental matrix standard reference materials (SRMs) with certified and reference values for polycyclic aromatic hydrocarbons (PAHs) and nitrated PAHs. In this study, the concentrations of oxygenated PAHs are determined in three air PM SRMs (1649b, 1648a, and 2786) and three diesel PM SRMs (1650b, 2975, and 1975) using two independent gas chromatography–mass spectrometry methods. Concentrations of oxy-PAHs were at the milligrams per kilogram level with higher overall concentrations in diesel PM (up to 50 mg/kg for 9,10-anthraquinone). One of the highest oxy-PAH concentrations (up to 5 mg/kg) measured in the air particulate SRMs was for 7,12-benz[a]anthracenquinone. These results suggest that oxygenated PAHs should not be neglected in the analysis of PM as their concentrations can be as high as those of some PAHs and are one to two orders of magnitude higher than those for nitro-PAHs. 相似文献
5.
Stapleton HM Keller JM Schantz MM Kucklick JR Leigh SD Wise SA 《Analytical and bioanalytical chemistry》2007,387(7):2365-2379
Standard reference materials (SRMs) are valuable tools in developing and validating analytical methods to improve quality
assurance standards. The National Institute of Standards and Technology (NIST) has a long history of providing environmental
SRMs with certified concentrations of organic and inorganic contaminants. Here we report on new certified and reference concentrations
for 27 polybrominated diphenyl ether (PBDE) congeners in seven different SRMs: cod-liver oil, whale blubber, fish tissue (two
materials), mussel tissue and sediment (two materials). PBDEs were measured in these SRMs, with the lowest concentrations
measured in mussel tissue (SRM 1974b) and the highest in sediment collected from the New York/New Jersey Waterway (SRM 1944).
Comparing the relative PBDE congener concentrations within the samples, we found the biota SRMs contained primarily tetrabrominated
and pentabrominated diphenyl ethers, whereas the sediment SRMs contained primarily decabromodiphenyl ether (BDE 209). The
cod-liver oil (SRM 1588b) and whale blubber (SRM 1945) materials were also found to contain measurable concentrations of two
methoxylated PBDEs (MeO-BDEs). Certified and reference concentrations are reported for 12 PBDE congeners measured in the biota
SRMs and reference values are available for two MeO-BDEs. Results from a sediment interlaboratory comparison PBDE exercise
are available for the two sediment SRMs (1941b and 1944). 相似文献
6.
Trifa M. Ahmed Christoffer Bergvall Magnus Åberg Roger Westerholm 《Analytical and bioanalytical chemistry》2015,407(2):427-438
The objective of this study was to develop a novel analytical chemistry method, comprised of a coupled high-performance liquid chromatography–gas chromatography/mass spectrometry system (LC–GC/MS) with low detection limits and high selectivity, for the identification and determination of oxygenated polycyclic aromatic hydrocarbons (OPAHs) and polycyclic aromatic hydrocarbons (PAHs) in urban air and diesel particulate matter. The linear range of the four OPAHs, which include 9,10-anthraquinone, 4H-cyclopenta[def]phenanthrene-4-one, benzanthrone, and 7,12-benz[a]anthraquinone, was 0.7 pg–43.3 ng with limits of detection (LODs) and limits of quantification (LOQs) on the order of 0.2–0.8 and 0.7–1.3 pg, respectively. The LODs in this study are generally lower than values reported in the literature, which can be explained by using large-volume injection. The recoveries of the OPAHs spiked onto glass fiber filters using two different pressurized liquid extraction (PLE) methods were in the ranges of 84–107 and 67–110 %, respectively. The analytical protocols were validated using the following National Institute of Standards and Technology standard reference materials: SRM 1649a (Urban Dust), SRM 1650b (Diesel Particulate Matter), and SRM 2975 (Diesel Particulate Matter, Industrial Forklift). The measured mass fractions of the OPAHs in the standard reference materials (SRMs) in this present study are higher than the values from the literature, except for benzanthrone in SRM 1649a (Urban Dust). In addition to the OPAHs, 44 PAHs could be detected and quantified from the same particulate extract used in this protocol. Using data from the literature and applying a two-sided t test at the 5 % level using Bonferroni correction, significant differences were found between the tested PLE methods for individual PAHs. However, the measured mass fractions of the PAHs were comparable, similar to, or higher than those previously reported in the literature. 相似文献
7.
We have assessed and compared the extraction recoveries of polycyclic aromatic hydrocarbons (PAHs) with molecular weights
of 252, 276, 278, 300 and 302 from diesel particulate matter (PM) and urban air particles using ultrasonically assisted extraction
and accelerated solvent extraction methods, and evaluated the effects of sample and treatment parameters. The results show
that accelerated solvent extraction can extract PAHs more efficiently from diesel PM than ultrasonically assisted extraction.
They also show that PAHs are more difficult to extract from diesel PM than from urban air particles. Using toluene and maximum
instrumental settings (200 °C, 3,000 psi and five extraction cycles) with 30-min static extraction times > 85% of the analytes
were estimated to be extracted from the diesel particles, but four extraction cycles with just 5-min static extraction times
under these conditions seem to be sufficient to extract > 95% of the analytes from the urban air particles. The accelerated
solvent extraction method was validated using the Standard Reference Materials (SRM) 1649a, Urban Dust, and SRM 2975 and SRM
1650a, Diesel Particulate Matter, from the US National Institute of Standards and Technology (NIST). PAH concentrations determined
by on-line high-performance liquid chromatography–gas chromatography–mass spectrometry (HPLC-GC-MS) following the developed
accelerated solvent extraction method were generally higher than the certified and reference NIST values and concentrations
reported in the literature (e.g. the estimated concentration of benzo[a]pyrene in SRM 2975 was 15-fold higher than the NIST-certified value), probably because the extraction recoveries were higher
than in previous studies. The developed accelerated solvent extraction method was used to analyse high molecular (HMW) weight
PAHs (MW > 302) in the investigated SRMs, and more than 170 (SRM 1649a), 80 (SRM 1650b) and 60 (SRM 2975) potential high molecular
weight PAHs were tentatively identified in them, with molecular weights (depending on the SRM sample analysed) of 316, 326,
328, 340, 342, 350, 352, 366, 374 and 376. This is, to our knowledge, the first study to tentatively report PAHs with molecular
weights of 316, 326, 328, 342, 350, 352, 366 and 376 in diesel particulate matter. GC-MS chromatograms obtained in selected
ion monitoring mode (extracted ions for the abovementioned m/z) and full-scan mass spectra of tentatively identified high molecular weight PAHs are shown in the Electronic supplementary material.
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users. 相似文献
8.
An extremely simple and sensitive method was developed for determination of nitrated polycyclic aromatic hydrocarbons (nitro-PAHs; mono-nitro-PAHs and dinitropyrenes) in diesel exhaust particles (DEPs) by gas chromatography-negative ion chemical ionisation tandem mass spectrometry (GC/NCI/MS/MS). We used two types of column in GC/NCI/MS/MS analysis. A polar column was used for determination of mono-nitro-PAHs, and a non-polar column was used for determination of dinitropyrenes and mono-nitro-PAHs except nitrofluoranthenes. The proposed method requires no clean-up procedure. The limits of detection ranged from 0.01 to 0.09 pg for all compounds tested. The applicability of the method to DEP samples was validated using diesel particulate standard reference materials (SRMs). Although DEPs contain complex matrices, all compounds could be detected easily in SRM2975 (diesel particulate matter) and SRM1975 (diesel particulate extract) without a clean-up procedure. The RSDs were less than 5% for all compounds examined. The quantitative results for SRMs exhibited good agreement with the available data in the literature. These results indicate that the proposed GC/NCI/MS/MS method is useful for determination of nitro-PAHs in DEP samples. 相似文献
9.
Stacy S. Vander Pol John R. Kucklick Stefan D. Leigh Barbara J. Porter Michele M. Schantz 《Analytical and bioanalytical chemistry》2010,397(2):483-492
Toxaphene is a complex technical mixture that has been found ubiquitously in the environment but has caused issues for analysis,
especially of individual congeners. This paper reports the elution order of 26 major toxaphene congeners on three gas chromatographic
columns. The three different stationary phases generally had similar elution orders for the toxaphene congeners, but fewer
co-elutions occurred on a low-bleed, low-polarity column. These congeners (except for two that co-eluted and were not added
to the calibration mixture) were examined in air particulate matter standard reference materials (SRMs), 1648a, 1649a, and
1649b as well as SRM 3067 toxaphene in methanol for assignment of reference values. SRM 3067 had mass fractions an order of
magnitude greater than the air particulate SRMs, which ranged from 0.568 ± 0.018 ng g−1 dry mass (B9-2006 in SRM 1648a) to 12.9 ± 0.20 ng g−1 dry mass (B9-715 (P 58) in SRM 1649a). The three air particulate SRMs all had different mass fractions and proportions of
congeners relative to the sum of the toxaphene congeners. SRM 3067 may be useful as a technical mixture toxaphene congener
calibrant. SRMs 1648a and 1649b will serve as reference materials for the analysis of 21 (three congeners were not included
due to values below the detection limit or a potential polychlorinated biphenyl co-elution) toxaphene congeners in atmospheric
particulate samples. 相似文献
10.
Zeisler R Murphy KE Becker DA Davis WC Kelly WR Long SE Sieber JR 《Analytical and bioanalytical chemistry》2006,386(4):1137-1151
NIST has developed an extensive collection of environmental SRMs, starting with fuel and biologically related materials in the late 1960s and now encompassing all sectors of environmental research. Advances in analytical methodology, including multi-element isotope-dilution mass spectrometry (IDMS) and expanded instrumental neutron-activation analysis (INAA) capabilities, enable value assignment based on fewer but better-characterized independent analytical techniques. The special advantages of IDMS for determination of S and Hg and for multi-element characterization of small-sample air particulate matter (SRM 2783) by IDMS and INAA are emphasized. Developments in materials production include the issuance of fresh-frozen biological materials and of jet-milled natural-matrix materials with improved homogeneity, including highly homogeneous air particulate matter and sediment SRMs for small-sample analytical techniques. 相似文献