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作 者:孙有娥 李一辰 程春艳 赵丽娟 金小龙 SUN Youe;LI Yichen;CHENG Chunyan;ZHAO Lijuan;JING Xiaolong(Chizhou City Institute of Product Quality Supervision&Inspection,Chizhou 247000,China)
机构地区:[1]池州市产品质量监督检验所,安徽池州247000
出 处:《化学分析计量》2018年第6期91-94,共4页Chemical Analysis And Meterage
摘 要:建立测汞仪固体直接进样测定土壤中总汞的检测方法。样品经风干后除去石子和动植物残体等异物,研压过125μm尼龙筛后,采用直接进样测汞技术,在优化的仪器条件下测定。优化的仪器工作条件:载气(氧气)压力为100 kPa,流量为350 mL/min;输入压力为150 kPa;出口压力为7 kPa;输出压力为8 kPa;干燥温度为300℃,干燥时间为30 s;催化温度为600℃,催化时间为60 s;分解温度为800℃,分解时间为150 s;汞齐温度为600℃,汞齐时间为30 s。方法的线性范围为0~3 000 ng/g,线性相关系数为0.999 7,检出限为0.06 ng/g。测定结果的相对标准偏差小于2.0%(n=6),采用该方法测定土壤标准物质,测定值与标准值一致。该方法稳定可靠、操作简单高效、准确、重复性好,可用于土壤中汞的分析。A method for determination of total mercury in soil by mercury analyzer–solid direct injection was established.The sample was air-dried to remove foreign matter such as stones and animal and plant residues,and after being pressed through a 125μm nylon sieve,it was measured by direct injection mercury measurement technique under optimized instrument conditions.Instrument working conditions:carrier gas(oxidation)pressure was 100 kPa,flow rate was 350 mL/min,input pressure was 150 kPa,outlet pressure was 7 kPa,output pressure was 8 kPa;drying temperature was 300℃for 30 seconds,catalytic temperature 600℃for 60 seconds;the decomposition temperature was 800℃for 150 seconds,and the amalgam temperature was 600℃for 30 seconds.The linear range of this method was 0–3 000 ng/g,the correlation coefficient was 0.999 7,the detection limit was 0.06 ng/g,and the relative standard deviation was less than 2.0%(n=6).The soil standard substance was determined by this method,and the measured value was consistent with the standard value.The method is stable and reliable,simple,efficient,accurate and reproducible,it can be used for the analysis of total mercury in soil.
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