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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:BACKGROUND As 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.
OBJECTIVES To 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.
METHODS Four 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.
CONCLUSIONS When 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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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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