Discussion on the Analysis Method of Iodide in Natural Water Samples
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摘要:
水作为人体摄入碘元素的主要来源，准确测定其中的碘化物含量具有现实意义。目前常用于水样中碘化物分析的方法主要有离子色谱法、气相色谱法、比色法、分光光度法等，不同方法的测定结果会受到实际样品基质以及实验条件等因素的影响。本项目组织了38家实验室采用离子色谱法、淀粉分光光度法、催化还原分光光度法、电感耦合等离子体质谱法4种方法对天然水样中的碘化物含量进行测定，不同方法的测定值之间存在明显差异，数据间离散度较大，浓度在51.40~124.00mg/L范围内变化。基于此，本文采用HPLC-ICP-MS法对样品中的碘化物进行了定量分析，并通过考察该方法的精密度和正确度，在保证结果准确性的前提下，将碘化物测定结果与各家实验室结果进行比对。对比结果表明，对于碘离子，离子色谱法的测定值（83.38μg/L）与HPLC-ICP-MS的测定值基本一致（78.32μg/L），高浓度碘化物比色法的测定值（92.95μg/L）、硫酸铈催化分光光度法的测定值（101.84μg/L）和ICP-MS法的测定值（103.13μg/L）均高于HPLC-ICP-MS法的测定值。针对该结果，本文从各方法的原理和实验条件出发，探讨数据间存在差异的原因，阐述了水样中碘酸根离子、重金属离子等其他组分的存在，以及实验条件的选择均会对碘化物测定结果产生影响，并给出了不同情况下碘化物分析方法选择的建议。
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关键词:
- 碘化物 /
- 碘形态 /
- 高效液相色谱-电感耦合等离子体质谱法 /
- HPLC-ICP-MS /
- 天然水
Abstract:BACKGROUNDAs the main source of iodine intake, water is of practical significance to detect the content of iodide accurately. At present, the common methods for the analysis of iodide in water samples include ion chromatography, gas chromatography, colorimetry, spectrophotometry. The analysis results of different methods can be affected by the actual sample matrix and experimental conditions. Our project team organized 38 laboratories to determine the content of iodide in natural water samples by ion chromatography, starch spectrophotometry, catalytic reduction spectrophotometry, and inductively coupled plasma-mass spectrometry (ICP-MS), the results showed that there were significant differences among the measured values by different methods, and the data were obviously dispersed.
OBJECTIVESTo discuss the reasons for the differences between the results of different methods and give suggestions on the selection of iodide analysis methods under different conditions, based on the principles and conditions of each method.
METHODSFour analysis methods, including ion chromatography, starch spectrophotometry, catalytic reduction spectrophotometry, and ICP-MS, were used to determine the content of iodide of the groundwater sample by 38 laboratories. High performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) was used to determine the content of iodide by our own laboratory.
RESULTS(1) HPLC-ICP-MS can be used to effectively separate iodide and iodate ions in water samples. Through the quality control of the experimental process by blank samples, standard reference materials and replicate samples, the analytical results of this method were accurate and reliable. The determination results of iodide in JSH-2 samples were 78.32μg/L. (2) The determination values of iodide by ion chromatography (83.38μg/L) were consistent with those by HPLC-ICP-MS (78.32μg/L). However, the data of ion chromatography between different laboratories were obviously dispersed. The determination values of iodide by the starch spectrophotometry (92.95μg/L), catalytic reduction spectrophotometry (101.84μg/L) and ICP-MS (103.13μg/L) were higher than those by HPLC-ICP-MS. (3) The reasons for the differences between the results of different methods were discussed, based on the principles and conditions of each method: ① The determination results of ion chromatography may be affected by the selection of experimental conditions, such as sample pretreatment, chromatographic column and detector, and other interfering components. ② It is not considered whether there is iodate ion in the sample itself in the starch spectrophotometry. Therefore, when there are iodate ions in the water sample, the determination result is actually the total content of inorganic iodine. ③ The standard working curve of the catalytic reduction spectrophotometry is bent downward as a whole and does not show a good linear relationship. Therefore, when the response value of iodide is high, the concentration value will be high. ④ ICP-MS is only used to determine the total content of elements, and cannot be used for elemental speciation analysis. There are iodate ions in the samples of this experiment, so the determination results of ICP-MS should be the total content of iodine, rather than the content of iodide.
CONCLUSIONSWhen iodate ions are present in water samples, starch spectrophotometry and ICP-MS may lead to a high result of iodide determination. Among them, starch spectrophotometry is usually suitable for samples with an iodide concentration of 25-500μg/L, and ICP-MS can be combined with other separation techniques to improve method selectivity. When iodate ions are present in water samples, catalytic reduction spectrophotometry and ion chromatography can be used to analyze the concentration of iodide, but the influence of sample concentration level, matrix interference components, experimental conditions and other factors should be considered. HPLC-ICP-MS can be applied to the quantitative analysis of iodine species in water samples, which can avoid the influence of iodate ions on the accuracy of iodide determination results.
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碲和硒是稀散元素，在高新科技领域具有重要应用，已被中国和欧美国家列为战略性关键矿产资源［1-2］。一直以来全球碲、硒矿产资源主要采自斑岩-矽卡岩铜金矿床，如中国广东大宝山铜矿和江西城门山铜矿［3-4］，研究斑岩矿床中碲、硒的产出情况对国家资源战略保障具有重要意义。云南普朗斑岩型铜金矿床位于三江特提斯成矿域义敦岛弧南部，属于超大型斑岩矿床，已探明铜资源储量4.31Mt，金资源量113t［5］。矿区内出露的地层为中三叠统尼汝组和上三叠统图姆沟组，侵入岩为普朗复式岩体，由石英闪长玢岩（～216Ma）、石英二长斑岩（～215Ma）和花岗闪长斑岩（～206Ma）组成，岩体出露总面积约为11km2（图1）。前人对普朗矿床的地质特征、成岩成矿时代、成矿物质来源、成矿流体性质等作了大量工作，但对矿床中碲硒的含量和赋存状态等研究还较为薄弱。本文报道了普朗矿床中产出的碲化物和硒化物，以期为斑岩矿床中碲硒的勘查和综合利用提供资料。
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本次研究对象主要为普朗矿床中的铜精矿和钼精矿样品，测试分析均在东华理工大学核资源与环境国家重点实验室完成。样品的矿相学观察利用ZEISS Axio Scope A1光学显微镜及ZEISS Sigma 300场发射扫描电镜完成，扫描电镜的加速电压为20kV，发射电流为10μA［6］。矿物成分利用JXA-8530F Plus型电子探针分析完成，实验设定加速电压为15kV，电流为20nA，探针直径为1μm，使用ZAF方法对X射线强度进行校正。分析标样选择砷化镓（As），黄铜矿（Cu），黄铁矿（Fe、S），自然银（Ag），碲铋矿（Te、Bi），辉钼矿（Mo），自然铅（Pb），自然锑（Sb），硒化镉（Se），自然金（Au），自然铂（Pt），自然钯（Pd）。测试主量元素的精确度和准确度均小于2%。
普朗铜金矿床中的碲和硒含量高，并形成大量碲化物、硒化物和富硒矿物。矿床精矿中的碲和硒含量分别达74.3×10−6和270×10−6。碲在钾化带中的含量为0.3×10−6～0.43×10−6，较绢英岩化带中的高（0.02×10−6～0.12×10−6），由矿体中心向外，碲品位逐渐降低［7］。硒在钾化带和绢英岩化带的含量无明显差别，分别为1.49×10−6～2.44×10−6和1.04×10−6～3.00×10−6。矿石中的碲与金呈正相关关系，硒与银呈正相关关系。普朗铜矿床中，碲和硒主要以碲化物、硒化物和富硒矿物形式存在，形成辉碲铋矿、碲钯矿、硒银矿和富硒方铅矿等（图2）。辉碲铋矿是普朗含量最多的碲化物，反射光下为白色略带淡蓝色，矿物成分较均一，Bi含量为58.36%～61.24%，Te含量为31.03%～34.50%，S含量为3.76%～4.54%（图2e）。普朗辉碲铋矿中含有较高的Se（0.77%～3.63%）。辉碲铋矿的化学式为Bi2.02～2.08（Te1.74～1.93S0.85～1.01Se0.08～0.33）2.90～2.98。碲钯矿属于独立铂族元素矿物，在自然界很少见，中国斑岩矿床中仅江西德兴有报道［8］，在全球其他斑岩矿床中非常少见。普朗碲钯矿粒径为1～5μm，反射光下呈亮白色（图2a）。碲钯矿中Pd和Pt可以类质同象取代，因此含量变化较大，Pd含量为16.26%～25.69%，Pt含量为4.82%～17.66%，Te含量为61.25%～66.76%（图2f）。碲钯矿化学式为（Pd0.64～0.98Pt0.09～0.37）0.98～1.03Te1.97～1.02。硒银矿是普朗含量最多的硒化物，反射光下为白色带微蓝绿色（图2c）。硒银矿中普遍含S，含量为0.55%～2.65%，Ag含量普遍偏低，为70.22%～72.77%，Se含量为24.09%～27.31%（图2g）。硒银矿化学式为Ag1.89～1.98（Se0.87～1.01S0.05～0.24）1.02～1.11。富硒方铅矿属于PbS1-xSex矿物，其中x值可在0～1之间连续变化。普朗富硒方铅矿S和Se的含量变化大，分别为4.01%～12.52%和1.85%～19.13%，Pb含量为73.91%～82.52%，大多数样品中含有Ag，最高含量达1.61%。普朗富硒方铅矿形成了较完整的PbS-PbSe固溶体系列（图2h），化学式为Pb0.98～1.01（S0.35～0.97Se0.07～0.67）0.99～1.02。
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图 2 碲硒矿物显微照片及矿物元素含量三元图a—碲钯矿反射光镜下照片； b—碲钯矿BSE照片； c—硒银矿反射光镜下照片； d—硒银矿BSE照片； e— Bi-Te-S体系三元图； f— Te-Pd-Pt体系三元图； g—Ag-Se-S体系三元图； h—Pb-Se-S体系三元图。Mol—辉钼矿； Mrk—碲钯矿； Nau—硒银矿； Py—黄铁矿。Figure 2. Photomicrographs of tellurium and selenium minerals and ternary plots of element contents. a—Reflected light photomicrograph of merenskyite; b—BSE image of merenskyite; c—Reflected light photomicrograph of naumannite; d—BSE image of naumannite; e—Ternary plot of Bi-Te-S system; f—Ternary plot of Te-Pd-Pt system; g—Ternary plot of Ag-Se-S system; h—Ternary plot of Pb-Se-S system. Mol=Molybdenite, Mrk=Merenskyite, Nau=Naumannite, Py=Pyrite.矿床中的碲和硒可以指示物质来源和成矿过程。碲和硒具有亲硫特点，碲会部分进入硫化物晶格，但更易形成碲的独立矿物;硒属于强亲硫元素，在较高温的条件下易于进入硫化物晶格，在中低温条件下，硫含量较低时，可形成硒的独立矿物。洋壳中的铁锰结壳、页岩及浮游沉积物等是自然界中碲和硒的重要储库［9］，因此在洋陆俯冲过程中，大陆岩石圈地幔和洋壳的部分熔融会形成富碲、硒的岩浆［10-11］。碲和硒在硫化物熔体中的相容性很高（D硫化物/硅酸盐＞600），碲倾向于存在液相硫化物（SL）中，而硒则更易进入单硫化物固熔体（MSS）（DTe SL/硅酸盐/DSe SL/硅酸盐为5～9，DTe MSS/硅酸盐/DSe MSS/硅酸盐为0.5～0.8）［12］。当富碲、硒的岩浆到达下地壳，会结晶分异形成富Co、Ni的硅酸盐矿物，碲、硒存在硫化物熔体中继续向上运移；当岩浆到达中地壳，温度低于900℃时，硫化物熔体与Te-Se熔体发生相分离；当岩浆到达上地壳，侵位形成班岩体及Cu矿床，Ag-Pt-Pd则高度集中在富Te-Se熔体中，并最终形成贵金属矿物［13］。普朗铜金矿床中的碲和硒可能与区内晚三叠世的俯冲造山密切相关，富碲和硒的岩浆也促进了铂族元素的富集成矿。
普朗斑岩铜金矿床中碲化物和硒化物的发现，对资源的综合利用及矿床成因研究具有重要意义。矿床中碲和硒的资源量规模大，大部分以独立矿物形式存在，且常与Au-Ag-PGE共生，具有较好的经济回收利用价值。碲化物和硒化物的产出也为成矿物质来源及岩浆演化过程提供了新的研究方向。
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图 1 实验室间数据处理与结果评价
a—频率分布直方图； b—实验结果分布图； c—标准化偏倚条形图； d—Z值结果分布图。
Figure 1. Statistic treatment and performance evaluation by interlaboratory comparison.
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图 2 混合标准溶液中两种碘形态的色谱分离图
Figure 2. Chromatogram of two iodine species in mixed standard solution by HPLC-ICP-MS.
The concentration of two iodine species in mixed standard solution: c(IO3 −)=59.30μg/L, c(I−)=76.45μg/L; anion-exchange column: Dionex IonPac AS14; mobile phase: pH=9.8, 50mmol/L (NH4)2CO3.
表 1 碘形态标准溶液系列浓度
Table 1 Standard solution serial concentration of iodine species.
碘形态 标准系列1 标准系列2 标准系列3 标准系列4 标准系列5 KI（μg/L，以I计） 7.65 19.11 38.23 76.45 152.90 KIO3（μg/L，以I计） 0.59 2.97 5.93 14.83 59.30 
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表 2 各家实验室的碘化物分析方法采用情况
Table 2 Adoption of iodide analysis methods of 38 laboratories.
检测方法 参考方法 实验室编号 实验室个数 离子色谱法
（IC）《水质 碘化物的测定 离子色谱法》
（HJ 778—2015）1、6、12、13、14、15、18、20、21、23、29、30、31、32、36、38 16 催化还原分光光度法
[SP（催化）]《地下水质分析方法 第55部分：碘化物的测定 催化还原分光光度法》
（DZ/T 0064.55—2021）；
《生活饮用水标准检验方法 无机非金属指标》（GB/T 5750.5—2006）4、5、7、9、10、26、33、35、37、40 10 淀粉分光光度法
[SP（淀粉）]《地下水质分析方法 第56部分：碘化物的测定 淀粉分光光度法》
（DZ/T 0064.56—2021）；
《食品安全国家标准 饮用天然矿泉水检验方法》（GB 8538—2016）；
《生活饮用水标准检验方法 无机非金属指标》（GB/T 5750.5—2006）2、8、11、16、
19、24、287 电感耦合等离子体质谱法（ICP-MS） 电感耦合等离子体质谱法同时测定地下水中
硼溴碘（NJTC/DM07-CH18-1）
3、17、22、25、39 5
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表 3 实验室间碘化物含量测定值的格拉布斯检验结果
Table 3 Results of Grubbs test for determination of iodide content between laboratories.
统计参数 结果值 大小比较 评价 结果平均值 $\bar{x}$（µg/L） 92.31 - - 标准差s（µg/L） 13.98 - - 格拉布斯统计量Gp 2.27 <3.0250 正确值 检验统计量G1 2.93 <3.0250 正确值 注：上5%临界值：3.0250；上1%临界值：3.3690（p=39）。对于一个离群观测值的格拉布斯检验，大于1%临界值的为离群值，大于5%临界值的为歧离值。
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表 4 实验室间碘化物含量测定值的稳健统计法计算结果
Table 4 Results of the robust statistics method for determination of iodide content between laboratories.
统计参数 计算结果 统计参数 计算结果 个案数 38 上四分位数Q1 81.35 中位值 95.00μg/L 下四分位数Q3 102.25 众数 80.00μg/L 四分位距IQR（Q3-Q1） 20.90 标准偏差 13.98 标准化四分位距
NIQR（0.7413×IQR）15.49 最小值 51.40μg/L 稳健CV（%）
（NIQR/中位值×100%）16.31 最大值 124.00μg/L 峰度 0.887 偏度 −0.355
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表 5 各实验室对样品JSH-2碘化物含量的分析结果
Table 5 Analytical results of sample JSH-2 by different laboratories.
样品
JSH-2
分析方法各实验室采用不同方法测定结果平均值（μg/L） 各实验室测定结果平均值（μg/L） 各实验室采用不同方法测定结果中位值（μg/L） 各实验室测定结果中位值（μg/L） IC 83.38 92.31 80.00 95.00 SP（催化） 101.84 102.00 SP（淀粉） 92.95 92.00 ICP-MS 103.13 101.05
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表 6 HPLC-ICP-MS法的样品碘形态含量分析结果
Table 6 Analytical results of the iodine species of samples by HPLC-ICP-MS.
样品编号 碘形态测定值（μg/L） 总无机
碘含量（μg/L）总无机碘
平均值
（μg/L）RSD（%）
（n=3）I− IO3 − JSH-2 79.42 12.06 91.48 90.40 1.99 79.03 12.36 91.39 76.49 11.83 88.32 GBW08621 - 20.60 20.60 - - GBW（E）082815 97.10 - 97.10 - - 注：GBW08621：IO3 −证书值为21.17±0.21μg/L；GBW（E）082815：I−证书值为100±10μg/L。
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表 7 样品JSH-2的分析结果对比
Table 7 Comparison of analytical results in sample JSH-2.
样品JSH-2
分析方法I-测定平均值
（μg/L）IO3-测定平均值
（μg/L）总无机碘含量
（μg/L）HPLC-ICP-MS 78.32 12.08 90.04 IC 83.38 - - SP（催化） 101.84 - - SP（淀粉） 92.95 - -
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