Microwave heated vapor-phase digestion method for biological sample materials

A microwave heated, vapor-phase nitric acid-hydrogen peroxide digestion method for pulverized, biological sample materials was developed. Sample masses up to 200 mg were digested using calibrated quartz inserts inside first generation type, low-pressure, Teflon-PFA microwave vessels. In the first st...

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Bibliographic Details
Published in:Fresenius' journal of analytical chemistry 2001-01, Vol.369 (1), p.107-112
Main Authors: EILOLA, K, PERÄMÄKI, P
Format: Article
Language:English
Subjects:
Analytical chemistry
Animals
Cattle
Chemistry
Dogfish
Esocidae
Exact sciences and technology
Hydrogen Peroxide - chemistry
Indicators and Reagents
Liver - chemistry
Metals - analysis
Microwaves
nitric acid
Nitric Oxide - chemistry
Spectrometric and optical methods
Spectrophotometry, Atomic
Zea mays - chemistry
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Summary:A microwave heated, vapor-phase nitric acid-hydrogen peroxide digestion method for pulverized, biological sample materials was developed. Sample masses up to 200 mg were digested using calibrated quartz inserts inside first generation type, low-pressure, Teflon-PFA microwave vessels. In the first step, samples were digested in the vapor-phase for 80 min using a progressive heating pattern. Three mL of 70% nitric acid and 0.5 mL of 30% hydrogen peroxide were used as digestion reagents. In the second step, the small residue left after first step digestion was dissolved in 1.4% nitric acid or additionally with 0.5% hydrofluoric acid by heating for 15 min. The digestion method was optimized using pike (Esox lucius) muscle as a test material. The method was further optimized using three certified reference materials. Ca, Cu, Fe, Mg and Zn were determined from NIST-SRM 1577a bovine liver by ICP-AES. Cr and Ni were determined from NIST-SRM 8433 corn bran and NRCC DOLT-2 dogfish liver by GFAAS. For all elements the values obtained were close or within certified limits. Spike recoveries were between 96 to 107%. Digestion efficiency ranged from 91 to 99%.
ISSN:0937-0633
1432-1130
DOI:10.1007/s002160000611