Determination of Gold Mobile Fraction in Deep-penetrating Geochemical Samples by ICP-MS with Pre-extraction
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摘要: 金的地球化学勘查基于金的准确测定，地球化学样品中金含量通常处于ng/g水平，需先进行分离富集，再采用电感耦合等离子体质谱法（ICP-MS）或石墨炉原子吸收光谱法（GFAAS）进行测定。当前，隐伏矿床勘查是地球化学探测技术的发展前沿，金活动态提取技术是寻找隐伏金矿的有效手段之一。相比于全量分析，金的活动态含量更低，需要解决选择性提取、高效预富集与准确测定等一系列难题。本文采用柠檬酸铵与土壤中黏土矿物及次生矿物作用促使吸附和可交换组分的金进入提取液，以硫脲和硫代硫酸钠络合金使活动态金向提取液中扩散，达到选择性提取的目的，建立了提取液中金的预富集及ICP-MS测定方法。实验确定的分析条件为：采用5g/L柠檬酸铵-2g/L硫脲-5g/L硫代硫酸钠为提取剂，提取时间24h，在酸性硫脲介质下用活性炭富集金，金吸附率可达89.6%~109.2%，灰化解吸温度为650~700℃。本方法检出限为0.05ng/g，相对标准偏差（RSD）为9.4%~10.2%，加标回收率为91.2%~93.4%。与已报道的硫酸铁-硫脲-硫代硫酸钠溶液提取再GFAAS测定的方法相比，本方法具有检出限低、测试线性范围宽、测试速度快的优势；应用于森林覆盖区黑龙江东安金矿区地球化学探测试验，金活动态异常与隐伏金矿位置一致。要点
(1)采用柠檬酸铵-硫脲-硫代硫酸钠专用提取剂提取土壤活动态金。
(2)发展了金活动态提取液硫脲介质下活性炭富集方法。
(3)金活动态提取、测定技术成功应用于森林沼泽景观区隐伏金矿探测试验。
Highlights(1) The extraction of gold mobile fraction in soil with a special extractant of ammonium citrate-thiourea-sodium thiosulfate.
(2) The method using an active carbon preconcentration of gold mobile fraction in a thiourea medium was developed.
(3) The extraction and determination technology for gold mobile fraction was successfully applied to the detection test of hidden gold deposits in a forest swamp landscape area.
Abstract:BACKGROUNDThe geochemical exploration for gold deposits is based on the accurate determination of gold. The content of gold in geochemical samples is usually at the level of ng/g, which needs to be preconcentrated before determination by inductively coupled plasma-mass spectrometry (ICP-MS) or graphite furnace absorption spectroscopy (GFAAS). At present, the exploration of buried deposits is the frontier of geochemical exploration technology and the extraction of gold mobile fraction is one of the most effective approaches to find concealed gold deposits. Compared with whole rock gold analysis, the gold mobile fraction content is much lower, which requires specific leaching, efficient preconcentration and accurate determination.OBJECTIVESTo selectively extract gold mobile fraction and find surface secondary anomaly information for exploring concealed ore bodies.METHODSExperiments were carried out on the extraction agent and determination of gold mobile fraction by ICP-MS. Ammonium citrate was used to promote the disassociation of the adsorption of exchangeable form gold from the surface of clay minerals and secondary minerals in the soil. The complexation of thiourea and sodium thiosulfate was applied to diffuse the extracted gold into the solution to achieve the purpose of selective extraction. The procedure for gold preconcentration from extraction solution and the ICP-MS determination method were established.RESULTSThe experiments determined that the extractant was composed of 5g/L ammonium citrate, 2g/L thiourea, and 5g/L sodium thiosulfate. The extraction time was 24h, and the active carbon was used to preconcentrate gold in the acidic thiourea medium. The gold adsorption rates were 89.6%-109.2%, and the ashing temperature of the concentration materials were 650-700℃. The detection limit of the method was 0.05ng/g, the relative standard deviations (RSDs) ranged from 9.4% to 10.2%, and the recoveries were from 91.2% to 93.4%.CONCLUSIONSCompared with the published method, extraction with ferric sulfate-thiourea-sodium thiosulfate solution and determination by GFAAS, this method has the advantages of low detection limit, wide linear range and fast analysis. This method has been successfully applied in the geochemical exploration of gold deposits in the forest swamp landscape area of Dongan, Heilongjiang Province. Gold anomaly delineated is consistent with the location of the concealed gold deposit. -
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表 1 不同提取剂提取金测定结果的对比
Table 1 Comparison of analytical results of gold by using different leaching methods
活动态提取剂 GBW07806(n=3) GBW07246(n=3) GBW07247(n=3) 金测定平均值
(ng/g)RSD
(%)金测定平均值
(ng/g)RSD
(%)金测定平均值
(ng/g)RSD
(%)提取剂1(5g/L柠檬酸铵) 2.17 21.0 3.36 20.5 2.34 25.9 提取剂2(2g/L硫脲) 1.43 4.3 5.78 14.1 2.40 13.6 提取剂3(5g/L硫代硫酸钠) 0.23 19.0 3.43 18.1 1.96 12.9 提取剂4(2g/L硫脲-5g/L硫代硫酸钠) 1.31 23.3 5.09 13.2 2.64 23.5 提取剂5(5g/L柠檬酸铵-2g/L硫脲-5g/L硫代硫酸钠) 1.70 7.7 7.33 6.8 1.87 9.9 
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表 2 提取时间变化对金活动态提取量的影响
Table 2 Effect of extraction time on the mobile fraction of gold
提取时间
(h)活动态金提取量(ng/g) GBW07246 GBW07247 GBW07248 0.5 2.26 1.42 8.16 1 3.25 1.87 10.2 3 4.63 1.70 14.2 5 5.42 1.81 15.6 24 7.26 1.77 30.4 36 7.00 1.83 32.0 48 7.12 1.58 37.4
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表 3 提取液酸介质及酸度对金回收率的影响
Table 3 Effect of acid medium and acidity of extraction solution on adsorption recovery of gold
提取液介质 金回收率
(%)提取液介质 金回收率
(%)2g/L硫脲 94.2 2g/L硫脲-2%盐酸 92.7 2g/L硫脲-1%硝酸 98.3 2g/L硫脲-5%盐酸 97.9 2g/L硫脲-5%硝酸 100.6 2g/L硫脲-2%王水 87.2 2g/L硫脲-5%王水 88.4
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表 4 方法精密度
Table 4 Precision tests of the method
标准物质
编号金全量
认定值
(ng/g)柠檬酸铵-2g/L硫脲-5g/L硫代
硫酸钠提取法(本文方法)硫酸铁-硫脲
-硫代硫酸钠
提取法金活动态含量测定
平均值(ng/g)相对标准偏差
RSD(%)金活动态含量
测定平均值
(ng/g)GBW07246 20.8 7.56 9.4 6.92 GBW07248 100 30.6 10.2 26.5
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