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Use of thermal ionization isotope dilution mass spectrometry (TI-IDMS) as an oligo-element method for the determination of photographically relevant trace elements in AgCl emulsions

Frank Vanhaecke UGent, J Diemer, KG Heumann, Luc Moens UGent and Richard Dams UGent (1998) FRESENIUS JOURNAL OF ANALYTICAL CHEMISTRY. 362(7-8). p.553-557
abstract
Thermal ionization isotope dilution mass spectrometry (TI-IDMS) was used as an oligo-element method for the determination of Cr, Cd and Pb in photographic AgCl emulsions. After addition of an appropriate amount of isotopically enriched spikes (Cr-53, Cd-116 and Pb-206) to the solid samples, the latter were completely dissolved in NH, solution, permitting isotopic exchange to take place. Thereafter, AgCl was selectively removed by precipitation, whereby ultrasonic treatment was used to enhance the recovery of the elements of interest. Despite the use of concentrated HNO3 and H2O2 during further sample processing, preliminary experiments indicated the presence of a substantial remainder of the organic matrix (gelatine). Hence, the analytes of interest were isolated by means of electrolytic deposition on Pt electrodes. Subsequently, the deposits were dissolved from the Pt electrodes using a mixture of concentrated HNO3 and H2O2 and the solutions evaporated to dryness. The solid residues were taken up in diluted HNO3 and loaded onto Re filaments. In order to improve the ionization yield, prior to the sample, a silicagel suspension containing AlCl3 was loaded onto the filament and after sample loading, both H3BO3 (for Cr and Pb) and H3PO4 (for Cd and Pb) were added as further ionization aids. Finally, the isotope ratios of interest (Cr-52/Cr-53, Cd-114/Cd-116 and Pb-206/Pb-208) were determined using thermal ionization mass spectrometry, whereby all three analyte elements were vaporized from the same filament. The limits of detection obtained using this procedure range from 0.4 ng (for Cd) to 4 ng (for Pb). Four different AgCl emulsions were analyzed. For Cr, the concentration found was quite similar for all emulsions analyzed, as it varied between similar to 40 and similar to 100 ng/g only. For Cd, very low values were found for all samples analyzed (less than or equal to 3 ng/g). Finally, for Pb a much larger variation from similar to 10 ng/g up to similar to 5.5 mu g/g was observed. For the sample with the highest Pb content, an excellent agreement could be established between the results obtained using quadrupole-based ICP-IDMS and those using TI-IDMS. For the determination of Cr by means of quadrupole-based ICP-IDMS, an instrument equipped with a ShieldTorch system was used to avoid spectral overlap of the Cr-52(+) and (ArC+)-Ar-40-C-12 ion signals. Also in this case, the results obtained are in very good agreement with those obtained using TI-IDMS. The comparison between TI-IDMS and ICP-IDMS also made clear that sample inhomogeneity limits the between-sample precision attainable.
Please use this url to cite or link to this publication:
author
organization
year
type
journalArticle (original)
publication status
published
subject
keyword
TH, HEAVY-METALS
journal title
FRESENIUS JOURNAL OF ANALYTICAL CHEMISTRY
Fresenius J. Anal. Chem.
volume
362
issue
7-8
pages
553 - 557
Web of Science type
Article
Web of Science id
000077577600001
ISSN
0937-0633
DOI
10.1007/s002160051123
language
English
UGent publication?
yes
classification
A1
copyright statement
I have transferred the copyright for this publication to the publisher
id
181117
handle
http://hdl.handle.net/1854/LU-181117
date created
2004-01-14 13:41:00
date last changed
2012-11-21 11:37:49
@article{181117,
  abstract     = {Thermal ionization isotope dilution mass spectrometry (TI-IDMS) was used as an oligo-element method for the determination of Cr, Cd and Pb in photographic AgCl emulsions. After addition of an appropriate amount of isotopically enriched spikes (Cr-53, Cd-116 and Pb-206) to the solid samples, the latter were completely dissolved in NH, solution, permitting isotopic exchange to take place. Thereafter, AgCl was selectively removed by precipitation, whereby ultrasonic treatment was used to enhance the recovery of the elements of interest. Despite the use of concentrated HNO3 and H2O2 during further sample processing, preliminary experiments indicated the presence of a substantial remainder of the organic matrix (gelatine). Hence, the analytes of interest were isolated by means of electrolytic deposition on Pt electrodes. Subsequently, the deposits were dissolved from the Pt electrodes using a mixture of concentrated HNO3 and H2O2 and the solutions evaporated to dryness. The solid residues were taken up in diluted HNO3 and loaded onto Re filaments. In order to improve the ionization yield, prior to the sample, a silicagel suspension containing AlCl3 was loaded onto the filament and after sample loading, both H3BO3 (for Cr and Pb) and H3PO4 (for Cd and Pb) were added as further ionization aids. Finally, the isotope ratios of interest (Cr-52/Cr-53, Cd-114/Cd-116 and Pb-206/Pb-208) were determined using thermal ionization mass spectrometry, whereby all three analyte elements were vaporized from the same filament. The limits of detection obtained using this procedure range from 0.4 ng (for Cd) to 4 ng (for Pb). Four different AgCl emulsions were analyzed. For Cr, the concentration found was quite similar for all emulsions analyzed, as it varied between similar to 40 and similar to 100 ng/g only. For Cd, very low values were found for all samples analyzed (less than or equal to 3 ng/g). Finally, for Pb a much larger variation from similar to 10 ng/g up to similar to 5.5 mu g/g was observed. For the sample with the highest Pb content, an excellent agreement could be established between the results obtained using quadrupole-based ICP-IDMS and those using TI-IDMS. For the determination of Cr by means of quadrupole-based ICP-IDMS, an instrument equipped with a ShieldTorch system was used to avoid spectral overlap of the Cr-52(+) and (ArC+)-Ar-40-C-12 ion signals. Also in this case, the results obtained are in very good agreement with those obtained using TI-IDMS. The comparison between TI-IDMS and ICP-IDMS also made clear that sample inhomogeneity limits the between-sample precision attainable.},
  author       = {Vanhaecke, Frank and Diemer, J and Heumann, KG and Moens, Luc and Dams, Richard},
  issn         = {0937-0633},
  journal      = {FRESENIUS JOURNAL OF ANALYTICAL CHEMISTRY},
  keyword      = {TH,HEAVY-METALS},
  language     = {eng},
  number       = {7-8},
  pages        = {553--557},
  title        = {Use of thermal ionization isotope dilution mass spectrometry (TI-IDMS) as an oligo-element method for the determination of photographically relevant trace elements in AgCl emulsions},
  url          = {http://dx.doi.org/10.1007/s002160051123},
  volume       = {362},
  year         = {1998},
}

Chicago
Vanhaecke, Frank, J Diemer, KG Heumann, Luc Moens, and Richard Dams. 1998. “Use of Thermal Ionization Isotope Dilution Mass Spectrometry (TI-IDMS) as an Oligo-element Method for the Determination of Photographically Relevant Trace Elements in AgCl Emulsions.” Fresenius Journal of Analytical Chemistry 362 (7-8): 553–557.
APA
Vanhaecke, Frank, Diemer, J., Heumann, K., Moens, L., & Dams, R. (1998). Use of thermal ionization isotope dilution mass spectrometry (TI-IDMS) as an oligo-element method for the determination of photographically relevant trace elements in AgCl emulsions. FRESENIUS JOURNAL OF ANALYTICAL CHEMISTRY, 362(7-8), 553–557.
Vancouver
1.
Vanhaecke F, Diemer J, Heumann K, Moens L, Dams R. Use of thermal ionization isotope dilution mass spectrometry (TI-IDMS) as an oligo-element method for the determination of photographically relevant trace elements in AgCl emulsions. FRESENIUS JOURNAL OF ANALYTICAL CHEMISTRY. 1998;362(7-8):553–7.
MLA
Vanhaecke, Frank, J Diemer, KG Heumann, et al. “Use of Thermal Ionization Isotope Dilution Mass Spectrometry (TI-IDMS) as an Oligo-element Method for the Determination of Photographically Relevant Trace Elements in AgCl Emulsions.” FRESENIUS JOURNAL OF ANALYTICAL CHEMISTRY 362.7-8 (1998): 553–557. Print.