Discussion on Influence of Residues in Instruments on Detection of Selenium and Tellurium by Hydride Generation-Atomic Fluorescence Spectrometry
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摘要: 用氢化物发生-原子荧光光谱法(HG-AFS)分析地矿样品时，在仪器反应块、传输管路和原子化器上会有残留物生成，这些残留物中的某些成分积累到一定量时就会显著地影响硒和碲的测定。本文在分析HG-AFS法测定硒和碲干扰情况的基础上，用高纯物质配制的标准系列进行试验，避免了共存成分的影响。通过比较在仪器反应块、传输管路和原子化器更换前后标准系列的测定结果，表明仪器残留物会对硒、碲测定产生影响。对一些反应块、传输管路和原子化器的溶出物进行分析，发现钛、铜、砷、锑和铋会影响硒、碲的测定灵敏度和标准系列线性相关系数，这些元素也是文献中提到的共存成分中的干扰元素。通过更换仪器相应配件，克服了仪器残留物的影响，硒、碲的灵敏度有不同程度的提高，标准系列测试结果质量明显改善，线性相关系数均在0.9995以上。本研究认为对仪器残留物成分的分析是控制原子荧光光谱法干扰的一种有效手段。Abstract: Abstract: During the analyses of ore and rock samples by Hydride Generation-Atomic Fluorescence Spectrometry (HG-AFS), many residues were formed in the tubes in which the hydride was generated, transport channelled and atomized. If a certain amount of the residues accumulat, they can distinctively affect the detection sensitivity of Se and Te. Many coexisting ingredients in the samples have a large influence on the detection of Se and Te by HG-AFS. In this article, to avoid interference from these ingredients, the series of standard solutions prepared with highly pure material were used. The standard solutions were tested with used tubes and cleaned ones. Through comparison of the data of the standard solutions, it was demonstrated that the residues in the instrument affected the detection of Se and Te by making the detection sensibility lower and the linear correlation coefficient smaller. The residues were analyzed with Atomic Fluorescence Spectrometry, Atomic Absorption Spectroscopy and Inductively Coupled Plasma-Atomic Emission Spectrometry. On the basis of the analytical results of the residues, Ti, Cu, As, Sb and Bi have great effect on the detection sensitivity and the linear correlation coefficient of Se and Te. These elements are a part of the coexisting interferences mentioned in literatures. When the tubes were cleaned, the measured quality was remarkably improved with higher sensitivity, and the linear correlation coefficient was more than 0.9995. According to the data obtained in this study, indications are that the analysis of residue components in the tubes is one of the effective methods to control the interference of HG-AFS.
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表 1 断续流动程序
Table 1 The working program for the intermittent flow instrument
步骤 时间t/s 泵转速v/(r·min-1) 读数 1 3 0 No 2 8 100 No 3 3 0 No 4 13 120 Yes 
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表 2 灵敏度低时仪器反应块、传输管路和原子化器更换前后标准系列测试数据
Table 2 Analytical results of Se and Te in standard series before and after replacing of instrument response block, transmission pipeline and atomizer when the sensitivity was low
ρ(Se)/(ng·mL-1) 荧光强度 ρ(Te)/(ng·mL-1) 荧光强度 更换前 更换后 增加率/% 更换前 更换后 增加率/% 1 82.365 92.975 12.88 1 175.640 205.690 17.11 2 152.321 182.030 19.50 2 265.358 401.463 51.29 5 372.651 459.028 23.18 5 720.245 992.675 37.82 10 751.365 915.485 21.84 10 1285.254 1994.503 55.18 15 1123.327 1391.518 23.87 15 1998.841 2948.195 47.50 20 1573.325 1902.173 20.90 20 2742.874 3872.415 41.18 线性相关系数 0.9993 0.9998 线性相关系数 0.9990 0.9999
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表 3 线性相关性差时仪器反应块、传输管路和原子化器更换前后标准系列测试数据
Table 3 Analytical results of Se and Te in standard series before and after replacing of instrument response block, transmission pipeline and atomizer when the linear correlation was worse
ρ(Se)/(ng·mL-1) 荧光强度 ρ(Te)/(ng·mL-1) 荧光强度 更换前 更换后 增加率/% 更换前 更换后 增加率/% 1 89.985 76.963 -14.47 1 200.088 186.821 -6.63 2 172.248 159.100 -7.63 2 395.300 379.788 -3.92 5 369.958 425.095 14.90 5 961.860 971.610 1.01 10 668.210 791.025 18.38 10 1862.367 1884.795 1.20 15 1112.290 1228.135 10.41 15 2947.692 2860.188 -2.97 20 1585.245 1626.055 2.57 20 3681.087 3716.455 0.96 线性相关系数 0.9959 0.9998 线性相关系数 0.9989 0.9998
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表 4 仪器残留物测试结果
Table 4 Analytical results of elements in instrument residues
样品编号 管道名称 ρB/(ng·mL-1) V Mn Ti Cr Cu Zn Co Ni As Sb Bi Hg Se Te 1 反应块和传输管路 < 50 < 30 228 52 232 2381 < 50 < 50 20.5 7.1 15.88 3.043 24.78 13.30 1 原子化器 < 50 < 30 < 20 < 50 < 40 34 < 50 < 50 73.2 14.5 86.55 0.647 9.98 3.91 2 反应块和传输管路 < 50 < 30 35 55 62 622 < 50 110 49.1 5.2 1.32 1.820 9.87 6.47 2 原子化器 < 50 < 30 < 20 < 50 < 40 221 < 50 < 50 117.9 8.6 13.15 0.450 0.64 0.75 3 反应块和传输管路 < 50 63 69 140 67 1814 < 50 130 6.6 3.7 2.36 2.525 77.82 13.98 3 原子化器 < 50 34 < 20 < 50 < 40 42 < 50 < 50 40.3 7.4 13.77 0.458 1.09 0.61
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表 5 载流清洗残留物后测试结果
Table 5 Analytical results of Se and Te in standard solution tested with 10% of hydrochloric acid washing
载流清洗次数 ρB/(ng·mL-1) Se Te 2 16.8514 17.4243 15 16.7067 17.6382 30 16.1861 17.2532 60 17.5332 17.8798 90 17.8008 18.3455
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表 6 干扰物测试前后标准系列测试结果
Table 6 Analytical results of Se and Te in standard series tested before and after measurement of interferences
ρ(Se)/(ng·mL-1) 荧光强度 ρ(Te)/(ng·mL-1) 荧光强度 干扰物测试前 干扰物测试后 降低率/% 干扰物测试前 干扰物测试后 降低率/% 1 82.235 71.038 13.62 1 165.128 157.055 4.89 2 158.063 144.835 8.37 2 315.390 311.295 1.30 5 423.390 380.003 10.25 5 801.975 789.580 1.55 10 855.800 750.083 12.35 10 1634.078 1597.470 2.24 15 1254.800 1222.028 2.61 15 2420.140 2459.750 -1.64 20 1636.527 1574.875 3.77 20 3257.857 3193.655 1.97 线性相关系数 0.9997 0.9993 - 线性相关系数 1.0000 0.9998 -
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