CORRECTION OF ANALYTICAL RESULTS FOR RECOVERY: DETERMINATION OF PAHsIN AMBIENT AIR, SOIL, AND DIESEL EMISSION CONTROL SAMPLES BY ISOTOPE DILUTION GAS CHROMATOGRAPHY-MASS SPECTROMETRY

2006 ◽  
Vol 26 (5) ◽  
pp. 313-329 ◽  
Author(s):  
Andrzej Wnorowski ◽  
Mylaine Tardif ◽  
David Harnish ◽  
Gary Poole ◽  
Chung H. Chiu
1989 ◽  
Vol 72 (2) ◽  
pp. 349-354 ◽  
Author(s):  
Lee Q Huang

Abstract A multiresidue method was developed for the simultaneous determination of low parts per billion (ppb) concentrations of the herbicides alachlor, metolachlor, atrazine, and simazine in water and soil using isotope dilution gas chromatography/mass spectrometry (GC/MS). Known amounts of 15N,13C-alachlor and 2H5-atrazine were added to each sample as internal standards. The samples were then prepared by a solid phase extraction with no further cleanup. A high resolution GC/low resolution MS system with data acquisition in selected ion monitoring mode was used to quantitate herbicides in the extract. The limit of detection was 0.05 ppb for water and 0.5 ppb for soil. Accuracy greater than 80% and precision better than 4% was demonstrated with spiked samples.


1994 ◽  
Vol 40 (8) ◽  
pp. 1494-1502 ◽  
Author(s):  
S K Aggarwal ◽  
M Kinter ◽  
D A Herold

Abstract A stable isotope dilution gas chromatography-mass spectrometry (GC-MS) method is described for the determination of lead (Pb) in urine and whole blood. The use of lithium bis(trifluoroethyl)dithiocarbamate Pb(FDEDTC) as a chelating agent showed strong memory effect, restricting the range of Pb isotope ratios that can be measured in unknown samples. To overcome this carryover problem, we further derivatized the Pb(FDEDTC)2 chelate with 4-fluorophenyl magnesium bromide to form Pb(FC6H4)4. The sequential analyses of solutions of natural Pb and enriched 204Pb with Pb(FC6H4)4 chelate by GC-MS demonstrated no observable memory effect. Precision and accuracy of Pb isotope ratio measurements with Pb(FC6H4)4 were established, and the isotope dilution GC-MS method was validated by determining Pb concentrations in urine standards from the National Institute of Standards and Technology, urine and blood reference materials from the New York State Department of Health, and blood Pb survey samples from the College of American Pathologists.


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