ICP-AES测定工作场所空气中镉、铬、锰、镍、铅的干扰校正
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摘要
目的探讨电感耦合等离子体-原子发射光谱(ICP-AES)法测定工作场所空气中镉、铬、锰、镍、铅浓度时减少干扰的校正方法。方法分析ICP-AES法测定工作场所空气中镉、铬、锰、镍、铅的干扰来源,比较背景扣除和内标校正前后的测定结果;以干扰误差对干扰元素质量浓度进行线性回归,得到干扰因子表;采用背景扣除、内标校正和干扰因子法校正实际样品测定结果。结果未扣除背景的镉和铅测定结果与理论值相对偏差达219.5%和131.5%,而扣除背景后的测定值与理论值相对偏差均<10.0%;当溶液中总金属离子质量浓度>800.00 mg/L时,未加内标的测定结果与理论值相对偏差为-21.0%～-11.0%,内标校正后相对偏差均<10.0%。采用本方法校正焊接烟尘中的5种金属的质量浓度,镉干扰校正前、后质量浓度分别为3.90～32.50和1.20～7.10μg/L;镍干扰校正前、后质量浓度分别为111.00～1 220.00和99.00～1 120.00μg/L;铬、锰、铅干扰校正前、后质量浓度不变。结论 ICP-AES法测定工作场所空气中金属时采用背景扣除、内标校正、干扰因子表等方法进行干扰校正可较好地排除干扰,保证结果准确性。
Objective To explore the interference correction reduction method for the determination of cadmium(Cd), chromium(Cr), manganese(Mn), nickel(Ni) and lead(Pb) concentration in workplace air by inductively coupled plasma-atomic emission spectrometry(ICP-AES). Methods The interference sources in the determination of metals in workplace air with ICP-AES was analyzed. The results before and after the background correction or the internal standard calibration were compared. Linear regression is performed on the interference element mass concentration by interference error to obtain a table of interference factors. The measurement results of actual samples were corrected using background subtraction, internal standard correction, and interference factor method. Results The relative deviation of results and theoretical values without background subtraction were 219.5% and 131.5% for Cd and Pb, respectively. The relative deviation between the measured values and theoretical values was less than 10.0% after background subtraction. When the total metal ion concentration was >800.00 mg/L, the relative deviation between measured result and the theoretical values was-21.0%--11.0% without internal standard correction, and the absolute value of them were less than 10.0% after internal standard correction. The interference correction method was used to correct the concentration of Cd, Cr, Mn, Ni, Pb in welding smoke. The mass concentrations of Cd before and after interference correction were 3.90-32.50 and 1.20-7.10 μg/L, respectively. The mass concentrations of nickel before and after interference correction were 111.00-1 220.00 and 99.00-1 120.00 μg/L, respectively. The mass concentration of Cr,Mn and Pb remained unchanged before and after the interference correction. Conclusion The background correction, internal standard correction and interference factor table can eliminate the interference for determination of metals in workplace air by ICP-AES and ensure the accuracy of results.
Objective To explore the interference correction reduction method for the determination of cadmium(Cd), chromium(Cr), manganese(Mn), nickel(Ni) and lead(Pb) concentration in workplace air by inductively coupled plasma-atomic emission spectrometry(ICP-AES). Methods The interference sources in the determination of metals in workplace air with ICP-AES was analyzed. The results before and after the background correction or the internal standard calibration were compared. Linear regression is performed on the interference element mass concentration by interference error to obtain a table of interference factors. The measurement results of actual samples were corrected using background subtraction, internal standard correction, and interference factor method. Results The relative deviation of results and theoretical values without background subtraction were 219.5% and 131.5% for Cd and Pb, respectively. The relative deviation between the measured values and theoretical values was less than 10.0% after background subtraction. When the total metal ion concentration was >800.00 mg/L, the relative deviation between measured result and the theoretical values was-21.0%--11.0% without internal standard correction, and the absolute value of them were less than 10.0% after internal standard correction. The interference correction method was used to correct the concentration of Cd, Cr, Mn, Ni, Pb in welding smoke. The mass concentrations of Cd before and after interference correction were 3.90-32.50 and 1.20-7.10 μg/L, respectively. The mass concentrations of nickel before and after interference correction were 111.00-1 220.00 and 99.00-1 120.00 μg/L, respectively. The mass concentration of Cr,Mn and Pb remained unchanged before and after the interference correction. Conclusion The background correction, internal standard correction and interference factor table can eliminate the interference for determination of metals in workplace air by ICP-AES and ensure the accuracy of results.
引文
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[10] 严倩琳.微波消解ICP-AES法测定70钛铁中硅、铝、锰、镍、钒、钼、铬、磷、铜[J].现代冶金,2017,45(2):1-4
[11] PEREIRA L S, PEDROTTI M F, MICELI T M, et al. Determination of elemental impurities in poly(vinyl chloride) by inductively coupled plasma optical emission spectrometry[J]. Talanta,2016,152:371-377.
[12] 马超,孟策,张彩霞,等.电感耦合等离子体发射光谱法测定右旋糖酐铁中重金属元素时的基体效应和内标校正方法研究[J].药物评价研究,2017,40(8):1098-1102.
[13] 何海洋,董学林,于晓琪,等.内标校正-电感耦合等离子体发射光谱法测定磷矿石中的磷[J].岩矿测试,2017,36(2):117-123.
[14] VUDAGANDLA S, NADAVALA S K, VUMMITI D, et al. Determination of boron, phosphorus, and molybdenum content in biosludge samples by microwave plasma atomic emission spectrometry (MP-AES)[J]. Appl Sci,2017,7(3):264.
[2] 龚燕,凌霞.工作场所空气中钾钠含量的ICP-AES同时测定法[J].职业与健康,2014,30(8):1063-1065.
[3] 潘巧裕,张子群,张爱华,等.电感耦合等离子体-质谱法测定工作场所空气中铬、铁、镍、锡、铅[J].中国职业医学,2014,41(3):341-343.
[4] 张爱华,董明,李娟,等.电感耦合等离子体-质谱在职业卫生检测中应用[J].中国职业医学,2014,41(1):56-60
[5] 中华人民共和国国家卫生和计划生育委员会.工作场所空气有毒物质测定第33部分:金属及其化合物:GBZ/T 300.33—2017[S].北京:中国标准出版社,2017.
[6] National Institute Occupational Safety Health. NIOSH manual of analytical methods (NMAM):ELEMENTS by ICP (Nitric/Perchloric Acid Ashing) 7300[EB/OL].(2003-03-15)[2018-12-18]. https://www.cdc.gov/niosh/docs/2003-154/pdfs/7300.pdf.
[7] Occupational Safety and Health Administration. Sampling and analytical methods: metal and metalloid particulates in workplace atmospheres (ICP Analysis) ID-125G[EB/OL].(2000-09)[2018-12-18]. https://www.osha.gov/dts/sltc/methods/inorganic/id125g/id125g.pdf.
[8] 方卫,胡洁,赵云昆,等.ICP-AES测定汽车催化剂中Pt、Rd、Rh的干扰研究[J].分析试验室,2009,28(5):86-90.
[9] 中华人民共和国卫生部.工作场所空气中有害物质监测的采样规范:GBZ 159—2004[S].北京:人民卫生出版社,2006.
[10] 严倩琳.微波消解ICP-AES法测定70钛铁中硅、铝、锰、镍、钒、钼、铬、磷、铜[J].现代冶金,2017,45(2):1-4
[11] PEREIRA L S, PEDROTTI M F, MICELI T M, et al. Determination of elemental impurities in poly(vinyl chloride) by inductively coupled plasma optical emission spectrometry[J]. Talanta,2016,152:371-377.
[12] 马超,孟策,张彩霞,等.电感耦合等离子体发射光谱法测定右旋糖酐铁中重金属元素时的基体效应和内标校正方法研究[J].药物评价研究,2017,40(8):1098-1102.
[13] 何海洋,董学林,于晓琪,等.内标校正-电感耦合等离子体发射光谱法测定磷矿石中的磷[J].岩矿测试,2017,36(2):117-123.
[14] VUDAGANDLA S, NADAVALA S K, VUMMITI D, et al. Determination of boron, phosphorus, and molybdenum content in biosludge samples by microwave plasma atomic emission spectrometry (MP-AES)[J]. Appl Sci,2017,7(3):264.