Blakemore W M, Billedeau S M
J Assoc Off Anal Chem. 1981 Nov;64(6):1284-90.
Analytical procedures are described for the determination of arsenic, cadmium, calcium, copper, lead, mercury, selenium, and zinc in animal feed. Mercury is determined by digesting the feed sample in a mixture of concentrated nitric and sulfuric acids with vanadium pentoxide added as an oxidation catalyst, reducing with stannous chloride, and sweeping the elemental mercury into an absorption tube for measurement by atomic absorption (AA) spectrophotometry. Arsenic and selenium are determined simultaneously by digesting the sample with a mixture of concentrated nitric, sulfuric, and perchloric acids; the hydrides of arsenic and selenium, which are formed with the addition of sodium borohydride, are swept into an argon-hydrogen flame for analysis by AA. A low temperature ash is prepared and dissolved in IN HNO3 for the analysis of calcium, copper, and zinc by emission spectroscopy using the inductively coupled argon plasma source; the same solution is used for the determination of cadmium and lead by flameless AA. Animal feed spiked with 3 levels of each of the 8 elements gave recoveries that ranged from 80 to 107%.
介绍了测定动物饲料中砷、镉、钙、铜、铅、汞、硒和锌的分析方法。汞的测定方法是:将饲料样品在浓硝酸和浓硫酸的混合液中消化,并加入五氧化二钒作为氧化催化剂,用氯化亚锡还原,然后将元素汞吹扫到吸收管中,用原子吸收(AA)分光光度法进行测定。砷和硒的同时测定方法是:用浓硝酸、浓硫酸和高氯酸的混合液消化样品;加入硼氢化钠后形成的砷和硒的氢化物被吹扫到氩氢火焰中,用原子吸收法进行分析。制备低温灰分并将其溶解在1N硝酸中,使用电感耦合氩等离子体源通过发射光谱法分析钙、铜和锌;同样的溶液用于无火焰原子吸收法测定镉和铅。在动物饲料中添加8种元素中的每种元素的3个水平,回收率在80%至107%之间。