姚晶,任 蓉,樊 婷,苏春燕,汪海峰.原子荧光光谱法同测粮食中砷汞总量的条件选择及干扰控制[J].中国无机分析化学,2019,9(4):1-7.
原子荧光光谱法同测粮食中砷汞总量的条件选择及干扰控制
Selection of working conditions and interference control for simultaneous trace analysis the content of As and Hg in grain by AFS
投稿时间:2019-02-19  修订日期:2019-04-01
DOI:10.3969/j.issn.2095-1035.2019.04.001
中文关键词:  原子荧光光谱法      条件选择  干扰控制
英文关键词:atomic fluorescence spectroscopy (AFS)  As  Hg  conditions optimized  interference control
基金项目:
              
作者单位
姚晶 苏州市吴中区粮油质量监测中心
任 蓉 苏州市吴中区粮油质量监测中心,江苏 苏州 215156
樊 婷 苏州市吴中区粮油质量监测中心,江苏 苏州 215156
苏春燕 苏州市吴中区粮油质量监测中心,江苏 苏州 215156
汪海峰 南京财经大学食品科学与工程学院,南京 210003
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中文摘要:
      为了原子荧光光谱仪有更好的测试稳定性和灵敏度,保证测试结果的精密度和准确度,本文 优化了原子荧光光谱仪的原子化高度、负高压、灯电流和载气流量等4个主要工作条件,并对仪器产生干扰的因素环境温度、光源稳定性、试剂进行了研究,通过回收率实验进行了验证。结果显示,在原子化高度10mm,负高压270V、灯电流60mA、Hg灯电流15mA、载气流量300mL/min的工作条件下,控制环境温度应控制在20~25℃、至少预热30min、首选HCl作为反应用酸,浓度应不低于5%(V/V),还原剂浓度应在15-20 g /L,结果显示,在此条件下,As的检出限为0.0247 ng/mL,RSD为0.370%,线性回归系数r=0.9999;Hg检出限为0.0015 ng/mL ,RSD为0.437%,线性回归系数r=0.9999,仪器检测稳定性好,灵敏度高,各项指标均优于标准规定,且检测结果精密度高、准确性好。
英文摘要:
      In order to ensure better test stability and sensitivity of the atomic fluorescence spectrometer(AFS)and ensure the precision and accuracy of test results., the stability and sensitivity of AFS with working conditions such as atomization height, negative high voltage, lamp current and carrier gas flow rate were investigated and optimized. The interference factors, such as ambient temperature, light source stability and reagent, were studied were studied, then the experiment was carried out by recovery experiments with three levels. The best working conditions were atomization height 10mm , negative high voltage 270V, As lamp current 60mA, Hg lamp current 15mA, carrier gas flow rate 300mL/min precision. In 20 ~ 25 ℃, preheated at least 30 min, the preferred not less than 5% (V/V) HCl as reaction with acid, and 15 to 20 g/L reducing agent concentration, the results were showed the test results were better than the national standards. Than the standard, indexes of the AFS had better stability, higher sensitivity, and the test result had high precision and accuracy.
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