0000000000328525
AUTHOR
Jürgen Diemer
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
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 (53Cr, 116Cd and 206Pb) to the solid samples, the latter were completely dissolved in NH3 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 o…
Bromide/bromate speciation by NTI-IDMS and ICP-MS coupled with ion exchange chromatography
Two different mass spectrometric methods, negative thermal ionization isotope dilution mass spectrometry (NTI-IDMS) and inductively coupled plasma mass spectrometry (ICP-MS), off-line and on-line coupled with anion exchange chromatography, have been developed for simultaneous bromide and bromate determinations in water samples. The detection limits of these methods are in the range of 0.03–0.09 μg/L using a 50 mL sample.The results are independent of the content of other anions, which could be demonstrated by the analyses of six mineral waters containing chloride and sulfate of up to 160 mg/L and 1500 mg/L, respectively. Bromide has been analyzed by the NTI-IDMS method in the range of 10–50…
Development of an ICP-IDMS method for accurate routine analyses of toxic heavy metals in polyolefins and comparison with results by TI-IDMS
An inductively coupled plasma isotope dilution mass spectrometric (ICP-IDMS) method was developed as a suitable method - with respect to its sensitivity, precision, accuracy, and time-consumption - for the analysis of toxic heavy metal traces (Pb, Cd, Cr, and Hg) in polyolefins. Results for Pb, Cd, and Cr were compared with those obtained by thermal ionization isotope dilution mass spectrometry (TI-IDMS), which was used as a reference method. Because of its high first ionization potential and its high volatility mercury could not be determined by TI-IDMS. A multi-element spike solution, containing isotopically enriched 206Pb, 116Cd, 53Cr, and 201Hg, was used for the isotope dilution step. D…
Determination of zirconium traces in polymers by ICP-IDMS - a powerful and fast method for routine testing of zirconium residues in polyolefins
Zirconium trace analyses play an important role for polyolefins produced by modern catalytic processes with zirconium metallocenes. A reliable and fast routine testing method by inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) was therefore developed, which allows the determination of zirconium in polymers down to the low ng/g level. With respect to its precision, accuracy, and time-consumption this method is suitable for routine testing of production processes. A spike solution, enriched in the stable isotope 91Zr, was prepared and used for the isotope dilution procedure, which has the advantage of being an internal “one point” calibration method. The polyolefin sam…