The determination of zinc in standard reference materials by isotope dilution and atomic absorption analysis

1971 ◽  
Vol 8 (1) ◽  
pp. 25-32 ◽  
Author(s):  
K.J.R. Rosman ◽  
P.M. Jeffery
1972 ◽  
Vol 55 (6) ◽  
pp. 1339-1344
Author(s):  
Theodore C Rains ◽  
Oscar Menis

Abstract In a study of the flameless atomic absorption method for the determination of nanogram amounts of mercury in organic materials, the technique was improved to provide greater precision and accuracy. The loss of mercury during the digestion of organic materials with nitric, sulfuric, and perchloric acids is prevented by controlled heating and a packed refluxing column. The reduction and absorption system was simplified by using a heated absorption cell which alleviates the interference of volatile vapors. This method has been applied to the determination of mercury in NBS Standard Reference Materials of orchard leaves, liver, and coal, and the results were compared with results obtained with 2 other analytical methods.


2012 ◽  
Vol 95 (4) ◽  
pp. 1189-1194 ◽  
Author(s):  
Stig Valdersnes ◽  
Amund Maage ◽  
Daniel Fliegel ◽  
Kåre Julshamn

Abstract Currently, there is no legal limit for methyl mercury (MeHg) in food; thus, no standardized method for the determination of MeHg in seafood exists within the European jurisdiction. In anticipation of a future legislative limit an inductively coupled plasma isotope dilution mass spectrometry (GC-ICP-ID-MS) method was developed in collaboration with the European Standardization Organization (CEN). The method comprises spiking the tissue sample with Me201Hg, followed by decomposition with tetramethylammonium hydroxide, pH adjustment and derivatization with sodium tetraethylborate, and finally organic extraction of the derivatized MeHg in a hexane phase. Subsequently, the sample is analyzed via GC-ICP-MS and the result calculated using the ID equation. The working range of the method was 0.0005–1.321 mg/kg MeHg in marine tissue, with an internal reproducibility (RSD) of 12–1%. The method was validated based on statistical measures, such as the z-scores, using the commercially available reference materials from National Institute of Standards and Technology Standard Reference Material (NIST SRM) 1566b, NIST SRM 2977 and National Research Council of Canada (NRCC) TORT 2, NRCC, DORM 3, NRCC DOLT 4, and European Reference Material (ERM) CE 464. Z-scores for all standard reference materials, except for NIST SRM 1566b, were better than |1.5|. The wide range of marine tissues used during the validation ensures that the method will be applicable for measuring of MeHg in seafood matrixes of all kinds.


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