离子色谱法测定土壤中3种水溶性阴离子的不确定度评定及方法改进

doi:10.13228/j.boyuan.issn1000-7571.012017

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摘要以JJF 1059.1—2012《测量不确定度评定与表示》和CNAS—GL06:2019《化学分析中不确定度的评估指南》为依据,对离子色谱法同时测定土壤中水溶性氯离子、硝酸根离子、硫酸根离子等3种无机阴离子过程进行不确定度评定,以期为方法的改进提供依据。对试样称量、试样浸提体积、试样浸提条件、标准溶液系列的配制、校准曲线拟合及试样重复性测量等6个不确定度分量逐一讨论,计算了各分量的相对标准不确定度及合成相对标准不确定度。比较了合成相对标准不确定度中各相对标准不确定度分量的权重,结果表明,试样的浸提条件、标准溶液系列的配制、校准曲线拟合为主要的测量不确定度来源,并提出了对测定方法的几点改进。水溶性无机阴离子的浸提条件需要严格控制,才能得到相对可靠的结果;配制标准溶液系列过程中,小量程吸量管移液的相对标准不确定度较大,使用逐级稀释法可有效降低移液误差;校准曲线中被测离子的标准点跨度不宜过大,低含量样品宜用低浓度标准点拟合计算,高含量样品宜用高浓度标准点拟合计算。

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	王文杰
	刘彤彤
	刘安安

关键词 ：土壤, 水溶性阴离子, 离子色谱法, 不确定度, 氯离子, 硝酸根, 硫酸根

Abstract：Based on JJF 1059.1-2012 Evaluation and Expression of Measurement Uncertainty and CNAS-GL06:2019 Guide for Evaluation of Uncertainty in Chemical Analysis, the uncertainty of the simultaneous determination of 3 inorganic anions in soil by ion chromatography, including water-soluble chloride ion, nitrate ion and sulfate ion, was evaluated to provide a basis for the method improvement. Six uncertainty components such as sample weighing, sample extraction volume, sample extraction conditions, preparation of standard solution series, calibration curve fitting and sample repeatability measurement were discussed one by one. The relative standard uncertainty of each component and synthetic relative standard uncertainty were calculated. By comparing the weights of each relative standard uncertainty component in the synthetic relative standard uncertainty, the results showed that the main sources of measurement uncertainty were the samples extraction conditions, the preparation of standard solutions series, and the fitting of calibration curves, and some improvements to the determination method were proposed. The extraction conditions of water-soluble inorganic anions need to be strictly controlled to obtain relatively reliable results. In the process of preparing standard solution series, the relative standard uncertainty of pipetting with small range pipette was relatively large, and the stepwise dilution method could effectively reduce the pipetting error. The span of the calibration curve point of the measured ion should not be too large. Low-concentration samples should be calculated by fitting low-concentration standard points, and high-concentration samples should be calculated by fitting high-concentration standard points.

Key words： soil water-soluble anion ion chromatography uncertainty chloride nitrate sulfate

收稿日期: 2022-10-24

ZTFLH:	O657.7
	O213.1

通讯作者: *刘彤彤(1985—),男,工程师,大学本科,主要从事地质、土壤、水质样品的光谱、色谱分析;E-mail:gstvliutt@163.com

作者简介: 王文杰(1988—),男,工程师,大学本科,主要从事地质、土壤样品的光谱分析;E-mail:493007179@qq.com

引用本文:

王文杰, 刘彤彤, 刘安安. 离子色谱法测定土壤中3种水溶性阴离子的不确定度评定及方法改进[J]. 冶金分析, 2023, 43(6): 90-97. WANG Wenjie, LIU Tongtong, LIU An’an. Uncertainty evaluation and method improvement for determination of 3 water-soluble anions in soil by ion chromatography. , 2023, 43(6): 90-97.

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http://yjfx.chinamet.cn/CN/10.13228/j.boyuan.issn1000-7571.012017 或 http://yjfx.chinamet.cn/CN/Y2023/V43/I6/90

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