摘要
将微波消解技术与电感耦合等离子体质谱法相结合测定了煤炭中铅、镉、铬、砷、汞、铍6种元素.以硝酸和氢氟酸作为消解试剂,采用高压密闭微波消解仪及功率控制梯度消解模式,在190℃温度、38 bar压力,0.3 bar/s升压速率的条件下消解样品.样品消解完全后加入一定量硼酸,除去过量的氢氟酸以保护仪器.测定时,选择202 Hg、208 Pb、9 Be、75As、53Cr和114Cd作为测定同位素,同量异位素的干扰采用无干扰元素校正方式来消除,基体效应产生的信号漂移采用103 Rh作为内标进行校正.方法应用于SARM 19煤和GBW07430土壤有证标准物质的分析,测定值与认定值吻合,相对标准偏差（RSD,n=8）在1.5％～5.6％范围,回收率在88％～110％之间.
A method was developed for the determination of six elements in coal including lead, cadmi- um, chromium, arsenic, mercury and beryllium by inductively coupled plasma mass spectrometry with microwave digestion. The sample was digested with nitric acid and hydrofluoric acid as digestion rea- gents in a high-pressure closed micro-wave digestion instrument at power-controlled gradient mode at 190℃, 38 bar and 0. 3 bar/s. After digestion, a certain amount of boric acid was added to remove the excessive hydrofluoric acid and to protect the instrument. In the determination, ^202 Hg, ^208 Pb , ^9Be, ^75 As, ^53 Cr and ^114 Cd were selected as testing isotopes, and the interference from the isobars was elimi- nated by interference-free element correction method. ^103 Rh was used as the internal standard for cor- recting the signal drift caused by matrix effect. The proposed method had been applied to the analysis of SARM 19 coal and GBW07430 soil CRMs, whose results were consistent with the certified values. The relative standard deviations （RSDs, n=8） were 1.5%-5.6%, and the recoveries were 88%-110g.
出处
《冶金分析》
CAS
CSCD
北大核心
2014年第8期22-26,共5页
Metallurgical Analysis
关键词
煤炭
微波消解
电感耦合等离子体质谱法
铅
镉
铬
砷
汞
铍
coal
microwave digestion
inductively coupled plasma mass spectrometry
lead
cadmi-um
chromium
arsenic
mercury
beryllium
