Determination of high molecular weight PBDE by isotopic dilution in ECNI-MS

J. Björklund, P. Tollbäck, C. Östman
2003 | 61 (163-166)

Polybrominated diphenyl ethers (PBDEs) are widely used as additive flame-retardants in different types of appliances1. The increasing number of reports on the occurrence of PBDE in various environmental compartments such as air, sediment and biota raise concern about these compounds as global environmental contaminants2. In recent years the use of the technical decaBDE mixture, which contains up to about 98 % BDE-209, has increased, most likely due to pending regulations concerning the industrial use of PBDEs with a lower degree of bromination2. However, in an interlaboratory study by de Boer et al. it was concluded that the determination of BDE-209, decabromodiphenyl ether, is not under control for many of the laboratories3. The separation and detection of PBDE is most commonly performed using gas chromatography (GC) with mass spectrometric detection (MS)4. High resolution MS (HRMS) operated in electron ionization (EI) mode offers a good sensitivity and the possibility to use 13C-labeled standards for an accurate and precise determination of the BDE congeners utilizing isotopic dilution5. For low resolution MS (LRMS) the most sensitive operational mode is electron capture negative ion (ECNI) monitoring the [79Br] and [81Br] fragments. Generally this mode provides little structural information about the compounds compared to EI6. In this paper we propose 13C-labeled BDE-209 as an internal surrogate standard and its application for quantification by isotopic dilution in LRMS ECNI.

Multiply charged ions in electrospray ionization mass spectrometry of humic substances

Alsberg, T.; Persson, L.; Strandell, M. & Odham
2003

9th Nordic IHSS Symposium on Abundance and functions of natural organic matter species in soil and w

Distribution of PCBs between water and particulate organic carbon in the surface water of the open Baltic Sea.

Sobek, A.
2003 | Dep of Geo and Geochem, SU

Seafloor Imaging and Toxicity: Assessment of Risk caused by buried waste (SITAR) : Lethal biotoxicity analysis from background, reference and an ammunition dump site : Deliverable 6

Åkerman, G.; Hansson, T.; Tjärnlund, U.; Grunder, K.; Sundberg, H.; Balk, L.
2003 | SU (1-15)

This document has the purpose of reporting the first results obtained thorugh biotoxicity analysis of the bottom samples gathered at the refence, control and test sites of the SITAR project. The biotoxicity analysis is carried out by nanoinjection of bottom sample fractions at different concentration levels in fertilized fish eggs. The percentage of abnormous evolution of the fish embryos is taken as a relative measure of biotoxicity. Depending on the stage in time of the various observations, these can be grouped in lethal and sub-lethal toxicity indicators. Since the availability of the results is dictated by the pace at which the animals develop, in this report only the lethal toxicity indicators are reported, since these are the only ones available at this early stage. It is remarked though that, for bioaccumulation assessment, sub-lethal indicators may represent the most important indicators. The sub-lethal indicators will be available in a different report at a later stage in the project.

The report describes the sample collection procedure as well as the data analysis procedure. Results this far from the lethal toxicity indicators suggests very low or no release of toxicants from this particular investigated dumpsite located in the outer areas of Stockholm archipelago. Further analysis of biomarker will reject or confirm this preliminary risk evaluation.

Freezing thresholds and cirrus cloud formation mechanisms inferred from in situ measurements of relative humidity

Haag, W; Karcher, B; Ström, J; Minikin, A; Lohmann, U; Ovarlez, J; Stohl, A
2003 | Atmos. Chem. Phys. | 3 (1791-1806)

Effects of forest fire and fire-fighting operations on water chemistry in Tyresta National Park, Stockholm, Sweden

Eriksson, H.; Edberg, F.; Borg, H.
2003 | J. Phys. IV | 107 (427-430)

Critical loads and limits of heavy metals in ecosystems: Some Swedish contributions to European modelling efforts. United Nations UN/ECE-CLRTAP-ICPMM, 22 p. (http://www.icpmapping.org)

Meili, M.; Åkerblom, S.; Bringmark, L.; Johansson, K.; Munthe, J.
2003

http://www.oekodata.com/pub/mapping/workshops/ws_berlin/sweden.pdf

Scavenging efficiencies of aerosol particles in marine stratocumulus and cumulus clouds

Glantz, P.; Noone, K. J. and Osborne
2003 | Q. J. R. Meteorol. Soc | 129 (1329-1350)

Feasibility of an on-line restricted access material/liquid chromatography/tandem mass spectrometry method in the rapid and sensitive determination of organophosphorus triesters in human blood plasma

N. Amini, , C. Crescenzi
2003 | J. Chromatogr. B | 795(2) (245-256)

A rapid on-line solid phase extraction/liquid chromatography/tandem mass spectrometry (SPE/LC/MS/MS) method using restricted access material (RAM) was developed for the simultaneous determination of eight organophosphorus triesters in untreated human blood plasma. In a process involving column-switching techniques, the analytes were enriched on the RAM column, separated using a C-18 analytical column and detected with LC/MS. Tandem mass spectrometry was used to characterize and quantify the analytes. To elucidate the fragmentation pathway of a number of the analytes, MS3 experiments using an ion trap mass spectrometer were performed. The matrix effects associated with using APCI and ESI interfaces were investigated. The recoveries obtained were in the range 60–92% (R.S.D.

Automated Rotary Valve Injection for Polybrominated Diphenyl Ethers in Gas Chromatography

J. Björklund, P. Tollbäck, E. Dyremark, C. Östman
2003 | J Sep Sci | 26 (594-600)

A simple, automated rotary valve injector for gas chromatography was constructed and evaluated for injection of polybrominated diphenyl ethers with molecular weights ranging from 485 to 949 Dalton. These congeners, particularly those with nine and ten bromine substituents, constitute a severe problem when a split/splitless vaporizing injector is used for gas chromatographic determination of polybrominated diphenyl ethers. Volumes up to 50 L were injected without the need for a solvent vapor exit. Discrimination of the high molecular weight brominated diphenyl ether congeners with seven to ten bromine substituents is strongly reduced. The injector exhibits both high reproducibility and low carry-over effects. Average relative standard deviation of the absolute peak area was less than 3.5% and for the carryover it was less than 0.4%. An important observation is that the electron capture detector response factors remained constant independent of injection volume, allowing large volume injection to decrease sample concentration detection limits, which is an important feature regarding determination of high molecular weight polybrominated diphenyl ethers. A further advantage is that the rotary valve large volume injector facilitates on-line coupling of various clean-up systems to the gas chromatograph.

Provningsjämförelse 2003-1: Närsalter; NH4N, NKj, NO23N, NO2N, NO3N, Ntot, PO4P, Ptot.

Lagerman, B.; Sköld, E.
2003 | ITM, SU | ISBN: ISSN 1103-341

The presence of a ‘new’ flame retardant, decabromodiphenyl ethane, in environmental samples

Kierkegaard, A.; Björklund, J.
2003 | Organohalogen Compd. | 61 (183-186)

Dioxin 2003

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