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研究了不同温度以及HNO_3、HNO_3/H_2O_2、HNO_3/HF和HNO_3/HF+H_3BO_3 4种酸对飞灰微波消解效果和元素分析的影响。以NIST-1633b为飞灰标准物质。建立了用HNO_3/HF(9mL+1mL)分解0.05g飞灰,再加入10mL 4%(ρ)的H_3BO_3中和过量HF及氟化物沉淀的两步微波消解方法。并利用ICP-OES检测了Al、Ca、Fe、Mg、K、Na、S、Si和Ti等9种矿物元素,元素回收率在92%-105%之间;利用ICP-MS检测了V、Cr、Mn、Co、Ni、Cu、Zn、As、Se、Sr、Cs、Ba、Eu和Pb等14种重金属元素,元素回收率在83%-109%之间。各元素检测的RSD均小于3%。
Effects of different temperatures and HNO 3, HNO 3 / H 2 O 2, HNO 3 / HF and HNO 3 / HF + H 3 BO 3 acids on microwave digestion and elemental analysis of fly ash were studied. NIST-1633b as fly ash standard material. A two-step microwave digestion method was developed to decompose 0.05g fly ash with HNO3 / HF (9mL + 1mL) and then add 10mL of 4% (ρ) H_3BO_3 to neutralize excess HF and fluoride precipitation. Nine mineral elements such as Al, Ca, Fe, Mg, K, Na, S, Si and Ti were detected by ICP-OES. The recoveries of elements were between 92% and 105% 14 kinds of heavy metal elements such as Cr, Mn, Co, Ni, Cu, Zn, As, Se, Sr, Cs, Ba, Eu and Pb, with the recoveries of 83% -109%. The RSDs of each element were less than 3%.