Study on the Availability of Wet Chemical Digestion of Geo-electrochemical Polyurethane Foam Samples
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摘要: 灰化法和微波消解法作为地电化学泡塑样品的预处理方法适用于多数元素，但二者都存在局限性，如灰化法的高温加热过程会造成As、Hg等元素的损失影响测定结果，微波消解法则因用样量小（0.1 g），存在样品代表性和检出限方面的问题。湿法消解是一种传统的样品预处理方法，具有消解完全、元素损失量低、样品代表性好等优点，可以有效解决以上两种方法的不足。但因为加入高氯酸消解泡塑（有机物）样品过程中易爆炸和酸空白等问题，一直没有在泡塑样品的预处理中得到推广。本文选取内蒙古洛恪顿热液型铅锌多金属矿床一条地电化学勘查剖面，用20 mL硝酸+5 mL高氯酸和5 mL王水对泡塑样品（约0.5 g）进行预处理，氢化物发生原子荧光光谱法和高分辨电感耦合等离子体质谱法测定元素含量。结果表明：大多数元素的空白含量都比较低，地球化学剖面图上有良好的异常显示；湿法消解处理泡塑样品是可行的，分析泡塑样品主要使用这种预处理方法。
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关键词:
- 地电化学 /
- 泡塑样品 /
- 湿法消解 /
- 氢化物发生-原子荧光光谱法 /
- 高分辨电感耦合等离子体质谱法
Abstract: As the pretreatment methods in analyzing geo-electrochemical polyurethane foam samples, ashing and microwave digestion methods are suitable for determination of most elements. Both methods have their disadvantages. The ashing method may cause volatilization loss of some elements (e.g. Hg, As) under high temperature, whereas issues about sample representation and detection limit exist in the microwave digestion method because of the small amount of sample (0.1 g). Wet chemical digestion is a traditional pretreatment method, which is widely used in the pretreatment of various geochemical samples and has the advantages of complete digestion, low element loss and good sample representation. However, because of the problems of explosion and acid blank during digestion of polyurethane foam (organic) samples, this method has not been used in pretreatment of geo-electrochemical foam samples. For this study a geo-electrochemical exploration line in Luokedun hydrothermal lead-zinc polymetallic deposit in Inner Mongolia was selected as the research subject. 20 mL of Nitric acid, 5 mL of perchloric acid, and 5 mL of aqua regia were used to digest 0.5 g foam samples. The contents of some related elements were determined by High-resolution Inductively Coupled Plasma-Mass Spectrometry (HR-ICP-MS) and Atomic Fluorescence Spectrometry (AFS). Results show that contents of the foam blank are relatively low for most elements, and the geochemical profiles show good anomalies. It is suggested that wet digestion is feasible in the analysis of geo-electrochemical polyurethane foam samples, and could be used widely in the future. -
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表 1 样品分析重复测定监控结果
Table 1. Repeated measurement results of samples
元素 样品10 样品10重复测定
编号288001相对偏差
(%)样品25 样品25重复测定
编号288002相对偏差
(%)样品40 样品40重复测定
编号288003相对偏差
(%)Au 1.35 1.55 12.90 5.62 5.73 1.94 0.40 0.93 79.70 Ag 3.58 4.73 27.68 63.69 63.42 0.42 3.49 4.10 16.07 Al 38 40 5.13 85 88 3.47 188 215 13.40 As 64 59 8.13 80 77 3.82 134 134 0.00 Bi 5.88 5.53 6.13 7.04 6.68 5.25 18.81 19.63 4.27 Cd 12.72 13.77 7.93 4.42 4.38 0.91 23.01 26.61 14.51 Co 85 85 0.00 226 234 3.48 155 171 9.82 Cr 913 902 1.21 7496 7687 2.52 2083 2337 11.49 Cu 3358 3421 1.86 123925 126908 2.38 1688 2053 19.51 Fe 79 81 2.50 213 216 1.40 162 185 13.26 K 25.9 26.4 1.91 36.5 37.0 1.36 57.4 63.7 10.40 La 68 53 24.79 165 143 14.29 265 285 7.27 Mo 17.3 19.8 13.48 28.9 29.2 1.03 50.5 51.0 0.99 Ni 196 180 8.51 2196 2253 2.56 738 821 10.65 Pb 200 185 7.79 416 399 4.17 1612 1670 3.53 Sb 45 39 14.29 32 30 6.45 1065 1145 7.24 Se 23 25 8.33 23 24 4.26 50 43 15.05 Ti 5918 6234 5.20 7241 7532 3.94 9813 11069 12.03 U 26 25 3.92 45 43 4.55 79 82 3.73 Zn 3039 2991 1.59 6595 6680 1.28 5794 6446 10.65 注：K、Fe、Al含量的单位为μg，其余元素的单位为ng。 
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表 2 酸溶法处理内蒙古洛恪顿矿区电提取剖面样品测量数据统计结果
Table 2. Measurement data statistics of elements in samples from electric extraction profile of the Luokedun deposit in Inner Mongolia, pretreated with polyacid digestion
指标 Au Ag Al As Bi Cd Co Cr Cu Fe K La Mo Ni Pb Sb Se Ti U Zn 样品数 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 极大值 72.08 816.5 3.10 1.52 0.14 172.9 3.11 96.09 1588 3.24 0.87 4.64 0.73 69.9 12.12 8.01 0.38 222 1.72 84.54 极小值 1.44 6.39 0.28 0.27 0.04 25.25 0.60 5.17 2.67 0.42 0.19 0.52 0.14 1.44 1.59 0.20 0.18 38.1 0.11 14.63 平均值 7.51 42.17 0.85 0.65 0.06 55.92 0.99 15.06 52.6 0.90 0.34 1.57 0.26 6.22 2.98 1.15 0.25 70.3 0.44 31.87 中值 3.96 13.69 0.77 0.56 0.05 50.08 0.83 8.72 7.28 0.76 0.31 1.36 0.24 2.92 2.37 0.63 0.24 62.8 0.42 25.52 标准差 12.01 128.5 0.52 0.26 0.02 25.64 0.52 17.73 249.8 0.55 0.13 1.03 0.11 11.4 1.97 1.47 0.05 32.7 0.30 18.09 变异系数 1.60 3.05 0.61 0.40 0.34 0.46 0.52 1.18 4.75 0.61 0.38 0.66 0.42 1.83 0.66 1.28 0.19 0.47 0.68 0.57 泡塑空白 2.80 6.91 0.27 0.26 0.06 26.72 2.37 5.89 1.75 0.68 0.19 1.82 0.08 1.24 1.88 0.21 0.14 168 0.15 16.34 注：K、Fe、Al含量的单位为mg，Au、Ag、Cd含量的单位为ng，其余元素含量的单位为μg。
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