Research Progress on Pretreatment Methods for Analysis of Precious Metal Elements in Geological Samples
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摘要: 本文评述了近年来地质样品中贵金属元素分析预处理技术的研究现状和应用进展，对样品分解过程中常用的火试金法、碱熔融法、酸分解法以及样品分离富集过程中的吸附法、碲共沉淀法、离子交换法、溶剂萃取法、蒸馏法、生物吸附法等手段进行了归纳总结，分析了各方法的特点与不足，展望了技术方法未来发展方向。分解方法中的火试金法经分析工作者不断探索及改进，已成为分解贵金属的最佳手段，但其仍存在试剂消耗量大、成本高、流程长等缺点；碱熔融法虽可分解几乎所有地质样品，但其处理后的溶液存在大量钠盐，需经进一步的纯化；酸分解法主要以高压密闭和卡洛斯管的消解方式为主，但受到样品性质的制约。而不同分离富集的手段都具有较强的针对性，如：吸附法多用于Au、Pt、Pd的富集，蒸馏法仅适用于Os、Ru的分析。由于贵金属元素具有颗粒效应强、赋存形式复杂多样以及超痕量等特殊性，需要针对样品的类型特点选择相适应的预处理方法。本文提出，应当在现有的贵金属分解方法基础上，结合当前新的实验设备及实验条件，寻求更加高效、快捷的分解技术，严格控制流程的本底及各个环节的污染问题，实现多技术、多方法联用，满足贵金属分析的要求。要点
(1) 评述了地质样品中贵金属元素分析预处理技术的研究现状。
(2) 揭示了不同分解及富集方法的特点。
(3) 对未来贵金属分析方法的研究方向提出了展望。
HIGHLIGHTS(1) The research situation of pretreatment technology for the determination of precious metal elements in geological samples was summarized.
(2) The characteristics of different decomposition and enrichment methods were revealed.
(3) The future research direction of the precious metal analysis method was prospected.
Abstract:BACKGROUNDThis article reviewed the research progress of pretreatment techniques for the analysis of precious metal elements in geological samples in recent years. The fire assay, alkali fusion, acid decomposition and adsorption methods used in the separation and enrichment of samples and absorption, tellurium co-precipitation, ion exchange, solvent extraction, distillation, and biosorption methods commonly used for sample decomposition were reviewed. The characteristics and deficiencies of each method were investigated, and the future development direction of the method is prospected.OBJECTIVESIn order to make the analysis results accurate and reliable, it is necessary to select the appropriate means of sample decomposition and separation and enrichment to ensure complete sample decomposition, effectively eliminate the interference of co-existing ions and matrix effect, enhance the precious metal element test signal, and improve the signal-to-noise ratio.METHODSThe fire assay method used for sample decomposition has been continuously explored and improved by analysts, and has become the best method to decompose precious metals. However, it still has the disadvantages of large reagent consumption, high cost, and long procedure. Although the alkali fusion method can decompose almost all geological samples, the resulted solution contained a large amount of sodium salt, which needed to be further purified. The acid decomposition method was mainly based on the high-pressure sealed Carius tube digestion, but it was limited by the nature of the sample. Different separation and enrichment methods were highly targeted. For example, the adsorption method was mostly used for the enrichment of Au, Pt, and Pd. The distillation method was only suitable for the analysis of Os and Ru.RESULTSPrecious metal elements had features such as strong particle effects, complex and diverse forms, and ultra-trace amounts, so it was necessary to choose a suitable pretreatment method according to the type of samples.CONCLUSIONSBased on the existing precious metal decomposition methods, in combination with the current new experimental equipment and conditions, more efficient and rapid decomposition technologies should be sought and the background of the procedure and pollution problems in each step strictly controlled, realizing multi-technology and multi-method integration and meeting the requirements of precious metal analysis. -
硫是地壳中含量最丰富的元素之一，也是一切生物必需的营养元素。硫通过在水、土壤、生物及大气圈内永不停息地循环，对生态环境和植物生长产生一系列的影响。土壤是水、生物和大气圈的交汇中心，并且硫与土壤环境和肥力、植物生长和地球变化有着密切联系，对土壤中硫的快速、准确分析具有非常重要的指导意义。土壤中的硫含量变化较大，一般在30~10000 μg/g之间，其平均值约700 μg/g[1]。土壤是一个复杂而多相的物质系统，它主要由硅酸盐颗粒和有机物组成，硫在土壤中的形态多样。据报道，在干旱土壤中，硫以水溶性硫酸盐和不溶性的硫化物(CaSO4·2H2O、MgSO4·7H2O、ZnSO4、CaFeS2和FeS2等)为主；在排水良好的温带农用土壤中，硫以有机束缚态为主；在温润、半温润的牧场和草原土壤中，绝大多数的硫为有机态[2]。
测定样品中的全硫主要采用管式炉燃烧法[3-4]、X射线荧光光谱法(XRF)[5-10]、硫酸钡重量法[11-12]、离子色谱法[13-15]等。其中重量法和离子色谱法因流程长、流程繁琐，难以满足行业大批量样品的快速分析需求；应用燃烧法测定低含量的硫，精密度、准确度较差；XRF法虽然可以同时测定二氧化硅、氧化钾、氧化钠及硫等主次量元素，但对于土壤样品中硫的分析结果不令人满意[16]，并且分析速度较慢[17]。电感耦合等离子体发射光谱法(ICP-OES)具有灵敏度高、检出限低、精密度好、线性范围广的特点，适合大批量样品的分析。目前已经建立了多种应用酸溶或碱熔分解样品，ICP-OES测定不同样品中硫含量的方法[18-28]。例如，马生凤等[26]用四酸溶样测定铁铜锌铅矿石中的硫等22个元素；苏凌云[18]在低温下用逆王水和溴水溶解测定铁矿石中的硫磷；李清彩等[22]以高氯酸、硝酸和氢氟酸溶解试样测定多金属矿中的砷铬铟硫锑；高小山等[23]用过氧化钠熔融测定黑钨矿中的硫；胡璇等[25]用过氧化钠熔融测定高硫铝土矿中的硫。上述方法中，分析对象均以矿石和矿物为主，其中一些方法采用了不完全分解法。由此可见，样品前处理是准确测定硫的前提条件。
本文试验了王水、王水水浴和盐酸-硝酸-氢氟酸-高氯酸(四酸)三种酸溶方法，认为盐酸-硝酸-氢氟酸-高氯酸体系比其他两种方法更具优势，建立了四酸敞口溶解ICP-OES测定硫的方法。
1. 实验部分
1.1 仪器及工作条件
VISTA-MPX全谱直读电感耦合等离子体发射光谱仪(美国Varian公司)。仪器工作条件为：射频功率1200 W，辅助气(Ar)流量1.5 L/min, 冷却气流量15.0 L/min，雾化器压力200 kPa, 观察高度10 mm，蠕动泵转速15 r/min，清洗时间30 s，进样稳定延时20 s，读数稳定延时10 s，读数时间10 s，读数次数3次。
CT1461-35智能电热板(天津拓至明实验仪器有限公司)。
1.2 标准溶液和主要试剂
硫标准溶液(1000 mg/L)：准确称取2.2139 g于105℃干燥2 h的基准无水硫酸钠于100 mL烧杯中，加适量水溶解完全，加5 mL盐酸，转移至500 mL容量瓶中，定容。
硫标准溶液：由硫标准溶液用10%盐酸逐级稀释至所需浓度。
所需的盐酸、硝酸、氢氟酸、高氯酸均为优级纯(国药集团化学试剂有限公司)。
实验用水为二次去离子水(电阻率≥18 MΩ·cm)。
1.3 实验方法
将土壤样品中各种形态的硫定量转入溶液是样品前处理的关键，本研究首先借鉴了苏凌云[18]采用王水溶矿的方案(方法1)，实验发现样品在最后蒸干阶段易跳溅；进而对上述方法进行了改进，试验了王水水浴溶矿方法(方法2)，部分土壤标准物质的测定结果偏低比较严重，并且样品溶液需放置、澄清较长时间才能上机测定。可见，上述两种前处理方法对有些土壤样品不太适用。
本研究拟定了四酸全溶方法(方法3)，土壤中的二氧化硅是主量元素，在二氧化硅晶格中经常包裹着一些元素，可以通过加入氢氟酸打开晶格并挥发除去硅来解决。土壤中大部分硫为有机硫，加入高氯酸可以分解破坏有机物且将低价硫氧化为硫酸根。
1.3.1 方法1——王水溶解
准确称取0.2500 g样品置于100 mL玻璃烧杯中，用少量去离子水润湿样品，加入5 mL硝酸和15 mL盐酸，将烧杯放置于电热板上，盖上表面皿，于150℃加热分解，蒸至湿盐状，取下加入15 mL盐酸，微热溶解盐类，用少量水冲洗杯壁和表面皿，取下烧杯，冷却，并将溶液转移至25 mL聚乙烯比色管中，去离子水定容至25 mL，静置8 h后测定。
1.3.2 方法2——王水水浴溶解
准确称取0.2500 g样品置于25 mL比色管中，加入新配制的王水25 mL，沸水浴2 h, 取出比色管，冷却，去离子水定容至25 mL，静置8 h后测定。
1.3.3 方法3——四酸敞口溶解
准确称取0.2500 g样品置于50 mL聚四氟乙烯烧杯中，用少量去离子水润湿样品，加入2.5 mL硝酸、2.5 mL盐酸、5 mL氢氟酸和1 mL高氯酸，盖好盖子，轻轻摇动，置于排风橱中放置过夜。将聚四氟乙烯烧杯放置于电热板上, 取下盖子，用少量水冲洗，于190~210℃加热分解，蒸干至白烟冒尽(若样品分解不完全，可在未蒸干之前补加硝酸、氢氟酸继续蒸干)；关闭电源，然后加入5 mL 50%的盐酸，在电热板上利用余温继续加热至固体盐类完全溶解，用大约5 mL的去离子水冲洗杯壁，继续加热5~10 min至溶液清亮；取下烧杯冷却，并将溶液转移至25 mL聚乙烯比色管中，去离子水定容至25 mL，静置4 h后测定。
2. 结果与讨论
2.1 三种样品前处理方法的准确度比较
王水溶解、王水水浴溶解和四酸敞口溶解三种前处理方法的测定结果见表 1。王水溶样和王水水浴溶样的测定结果系统偏低，对于个别标准样品的相对误差甚至达到27%, 可能与王水不能完全破坏硅酸盐晶格造成样品分解不完全及硫元素不能全部进入溶液有关。刘峰等[29]研究了不同混合酸消解土壤样品对土壤中重金属含量测定的影响，认为完全消解体系(盐酸、硝酸、氢氟酸和高氯酸)的测定结果高于不完全消解体系。四酸溶样测定结果优于王水溶解、王水水浴溶解，所以本文采用四酸溶解。
表 1 四酸、王水、王水水浴溶解结果Table 1. Analytical results of samples disoluted with four acids, aqua regia and aqua waterbath methods标准物质编号 硫含量(μg/g) 三种溶解方法测定值与标准值的相对误差(%) 标准值 四酸溶解测定值 王水溶解测定值 王水水浴溶解测定值 四酸溶解 王水溶解 王水水浴溶解 GBW07446 108±14 112 99 103 3.70 -8.33 -4.63 GBW07451 440±42 436 390 410 -0.91 -11.36 -6.82 GBW07456 254±12 257 238 246 1.18 -6.30 -3.15 GBW07457 281±26 279 203 214 -0.71 -27.76 -23.84 2.2 样品溶解条件的选择
2.2.1 电热板温度
用国家标准物质GBW07446和GBW07453加入四酸溶样，考察了11种电热板温度(表面温度)对测定结果的影响。表 2测定结果表明，电热板的温度低于140℃，硫的溶出率最低为68.52%；电热板的温度高于220℃，硫的溶出率最低为70.37%；电热板的最佳温度在150~210℃。考虑到温度过低，溶解时间较长并且不利于赶除氟离子，所以温度选择190~210℃。
表 2 电热板温度的影响Table 2. Effect of electric heating plate temperature电热板表面温度(℃) GBW07446 GBW07453 硫标准值(μg/g) 硫测定值(μg/g) 硫溶出率(%) 硫标准值(μg/g) 硫测定值(μg/g) 硫溶出率(%) 130 108±14 74 68.52 2000±300 1632 81.60 140 108±14 98 90.74 2000±300 1730 86.50 150 108±14 113 104.63 2000±300 1977 98.85 160 108±14 107 99.07 2000±300 1993 99.65 170 108±14 110 101.85 2000±300 1998 99.90 180 108±14 116 107.41 2000±300 2013 100.65 190 108±14 112 103.70 2000±300 2007 100.35 200 108±14 110 101.85 2000±300 1987 99.35 210 108±14 104 96.30 2000±300 1965 98.25 220 108±14 87 80.56 2000±300 1891 94.55 230 108±14 76 70.37 2000±300 1874 93.70 2.2.2 酸溶浸泡时间和酸介质的选择
为减少试剂用量，降低空白值，减少对环境的污染，本文根据二氧化硅含量选取了4个有代表性的土壤标准样品，用少量去离子水润湿样品，加入2.5 mL硝酸、2.5 mL盐酸、5 mL氢氟酸和1 mL高氯酸，盖好盖子，轻轻摇动，置于排风橱中，分别进行了0、4、8、12 h酸溶浸泡试验。表 3测定结果表明，浸泡12 h，一般样品基本溶解清亮，本文选择浸泡过夜。
表 3 浸泡时间的选择Table 3. Choice of soaking time标准物质编号 粗粒级主要矿物 不同浸泡时间下溶解情况 0 h 4 h 8 h 12 h GBW07401 石英、长石 反应，冒泡 有少量固体 有极少量固体 基本清亮 GBW07403 石英、长石 无明显反应 有少量固体 基本清亮 基本清亮 GBW07407 褐铁矿、石英、高岭土 无明显反应 有少量固体 基本清亮 基本清亮 GBW07408 碳酸盐物质、长石、石英、黑云母、白云母、褐铁矿、贝壳 反应剧烈，大量冒泡 有少量白色、黑色固体 有极少量固体 基本清亮 实验配制了与样品浓度相近的硫、钾、钠、钙、镁、铁、锰、铍、锂、镧、铈、钪、钒、钴、镍、钛标准溶液，酸介质分别为10%的盐酸和硝酸，实验发现硝酸介质中大部分元素的谱线强度略高于盐酸介质，但锰、钛谱线除外。为了能在一份溶液中同时测定硫、钾、钠、钙、镁、铁、锰、铍、锂、镧、铈、钪、钒、钴、镍、钛等多个元素，本文采用10%的盐酸介质。
2.3 ICP-OES测量条件的选择
2.3.1 分析波长
硫元素主要分析谱线有两条，分别是180.669 nm和181.972 nm。在180.669 nm处，基体元素钙(180.672 nm)会对硫产生正干扰，181.972 nm的谱线没有干扰，并且其信背比高出180.669 nm谱线将近一倍，所以选择181.972 nm作为分析线。
2.3.2 氩气吹扫时间
波长在10~200 nm远紫外光能被光路中的空气(氧、氮、二氧化碳和水气)所吸收，波长越短的远紫外光越容易被空气吸蚀[30]，本文选定的硫的分析谱线181.972 nm处于远紫外区，需要用氩气对光路和接口进行吹扫。在VISTA-MPX光谱仪仪器说明书中推荐氩气吹扫时间不小于30 min，本文通过试验发现氩气吹扫50 min后，同一浓度硫标准的谱线强度在1 h内变化小于1%，所以氩气吹扫时间定在50 min。
2.3.3 功率
几乎所有的谱线强度随功率的增大而增大，但背景值也会增大，造成信背比变差，本文综合考虑采用功率1200 W。
2.4 分析方法技术指标和评价
2.4.1 方法线性范围和检出限
在仪器最佳实验条件下测定标准曲线溶液，硫的质量浓度在0~500 μg/mL范围内，硫标准曲线呈线性关系，相关系数为0.9993。
在仪器最佳实验条件下连续测定12次试验空白溶液，检出限为0.1 μg/mL(3倍测量值的标准偏差)，乘以稀释因子100，方法检出限为10 μg/g，方法测定下限(k=10)为33.3 μg/g，方法的最佳测量范围33.3~50000 μg/g。本方法的检出限0.1 μg/mL略高于马生凤等[26]获得的检出限0.04 μg/mL。其原因可能与曝光时间有关，马生凤等[26]采用的曝光时间为20 s，本文曝光时间为10 s。
2.4.2 标准物质分析
按照1.3.3节分析方法和1.1节仪器条件测定了GBW07446~GBW07457中的硫含量，测定结果见表 4，12次测定平均值与标准值的相对误差的绝对值在0.00%~2.93%，12次测定平均值与标准值的对数偏差小于0.01，相对标准偏差(RSD)在0.47%~4.05%，方法的精密度和准确度完全满足DZ/T 0258—2014《多目标区域地球化学调查规范》要求(规范要求土壤中硫的检出限为50 μg/g；硫含量在三倍检出限以上的对数值≤0.05，硫含量大于1%的对数值≤0.04；硫含量在三倍检出限以上的RSD≤10%，硫含量大于1%的RSD≤8)。
表 4 国家标准物质中硫含量的分析结果Table 4. Analytical results of sulfur in national standard references标准物质编号 硫含量(μg/g) 相对误差(%) RSD (%) 标准值 本法测定平均值(n=12) GBW07446 108±14 108.4 0.37 4.05 GBW07447 (7000) 7041.94 0.60 0.50 GBW07448 (816) 820.06 0.50 2.00 GBW07449 27000±2900 26995.59 -0.02 0.47 GBW07450 (167) 171.17 2.50 3.66 GBW07451 440±42 442.96 0.67 1.12 GBW07452 (420) 422.02 0.48 1.46 GBW07453 2000±300 2000.51 0.03 1.63 GBW07454 170±22 170 0.00 3.02 GBW07455 162±10 157.25 -2.93 3.59 GBW07456 254±12 254.93 0.37 2.58 GBW07457 281±21 281.36 0.13 2.04 注：括号内数据为参考值。 2.4.3 实际样品分析
本文从实际样品中抽取了20件不同土壤类型、硫含量从低到高的土壤样品，分别用XRF法、管式炉燃烧碘量法和本法进行测试比较，每件样品用不同方法独立测定三次，结果见表 5。从分析结果来看，XRF法具有较高的精密度，但低含量和高含量样品与碘量法相比易超差(表 5中标注“*”的数据为超差值)；管式炉碘量法的数值波动性较大；本法与碘量法相比有较好的准确度和精密度，并且分析速度和分析效率优于碘量法。
表 5 三种分析方法的结果比较Table 5. A comparison of the three analytical methods样品编号 XRF法 管式炉碘量法 本法(四酸溶样ICP-OES法) 硫含量三次测定平均值(μg/g) RSD(%) 硫含量三次测定平均值(μg/g) RSD(%) 硫含量三次测定平均值(μg/g) RSD(%) 1 112* 5.63 83.1 11.46 78.3 6.42 2 143 2.42 124 8.97 136.7 3.82 3 266 2.41 270 5.43 274.2 2.33 4 355 1.62 349 4.32 343.1 2.67 5 527 1.74 534 3.66 536.3 1.82 6 832 0.86 827 4.22 816.4 0.69 7 966 2.42 933 5.21 946.6 1.11 8 1386 1.57 1276 4.14 1233 0.68 9 5233 2.44 4320 3.12 4362 2.43 10 5604* 1.87 7465 4.17 7654 3.26 11 28335* 1.52 21364 3.13 21362 2.03 12 55027* 1.62 42187 1.86 43227 2.74 13 176 2.87 188 7.33 182.4 3.11 14 256 2.11 263 4.87 261.2 2.46 15 687 1.14 693 3.22 684.2 2.03 16 778 1.06 786 4.16 781.4 1.06 17 1125 1.68 1139 3.55 1132 0.97 18 7864* 1.93 8546 3.68 8574 1.33 19 29365* 1.44 24652 4.15 24468 2.36 20 43225* 1.67 40271 2.87 40298 1.93 3. 结论
本文用盐酸-硝酸-氢氟酸-高氯酸溶解样品，ICP-OES法测定硫含量，解决了采用现有分析方法测定多目标区域地球化学调查样品时，分析效率低和高、低含量段分析质量问题。应用本方法，样品溶解完全，硫没有损失，并且可以在不增加分析成本和分析时间的情况下，在一份溶液中同时测定钾、钠、钙、镁、铁、锰、铍、锂、镧、铈、钪、钒、钴、镍、钛等元素，提高了分析效率，适合于大批量土壤样品中硫及主次量元素的测定。该方法已进行了实际样品测试，硫元素的成图及接图效果良好，外部控制样(256件)合格率为99%。方法上报给中国地质调查局区化样品质量检查组并获得批准，在地质行业进行了推广。
本方法的不足之处在于某几个岩石标准样品测定结果不尽如人意，其原因需要进一步实验研究。
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