[用非抑制离子色谱法测定矿泉水中的硼酸和硅酸]。

IF 1.2 4区 化学 Q4 CHEMISTRY, ANALYTICAL 色谱 Pub Date : 2023-12-01 DOI:10.3724/SP.J.1123.2023.09025
Zhanqiang Yang, Fangfang Zhang, Chunxia Han, Hongguo Zheng
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引用次数: 0

摘要

硼和硅在自然界中分布广泛;在水中,这两种化合物通常分别以硼酸和硅酸的形式存在。相关国家和行业标准(如 GB 8538-2022)规定了水中硅酸和硼酸的最大允许含量。水质变化对水质评价具有重要意义,可以通过硅酸和硼酸的含量来了解。硼酸含量通常通过离子排阻色谱法测定,而硅酸含量通常通过柱后衍生法测定。因此,传统方法无法同时测定水中的硅酸和硼酸含量。现代离子色谱法已广泛应用于阴离子、阳离子、有机酸、有机胺、氨基酸和糖类等离子化合物的检测。硼酸(pKa=9.24)和硅酸(pKa=9.77)是弱酸,在碱性条件下会离解成离子状态。虽然这些化合物不能用抑制离子色谱法进行检测,但可以保留在离子色谱柱上。本研究建立了一种基于非抑制电导检测的方法,用于同时测定水中的硼酸和硅酸。使用 Dionex IonPacTM AS20 分析柱,采用非抑制离子色谱法检测硼酸和硅酸的含量。色谱条件为:流速 1.0 mL/min;柱温 30 ℃;洗脱液 6 mmol/L 氢氧化钠溶液和 60 mmol/L 甘露醇;进样量 50 μL。在 8 分钟内实现了硅酸和硼酸的有效分离。硅酸和硼酸在0.25-100 mg/L和0.5-100 mg/L浓度范围内分别呈现良好的线性关系(相关系数为0.9999)。SiO32- 的方法检出限(MDL)和定量限(MQL)分别为 0.078 mg/L 和 0.26 mg/L,硼酸的方法检出限(MDL)和定量限(MQL)分别为 0.18 mg/L 和 0.60 mg/L。硼酸和 SiO32- 的平均回收率(n=6)为 97.3%-105.3%。此外,硼酸在4个添加水平下的相对标准偏差小于0.9%,SiO32-在3个添加水平下的相对标准偏差小于0.30%。因此,该方法符合检测要求。前处理方法非常简单,样品可直接通过 0.22 μm 水过滤膜注入色谱柱。在优化的分析条件下,测定了九种矿泉饮用水样品中的硼酸和硅酸含量。在这九个样品中没有检测到硼酸,但在六个样品中检测到了硅酸。检测到的硅酸含量在 18.70 至 62.08 毫克/升之间,与生产商包装上标注的浓度范围一致。该方法可用于矿泉饮用水和实验室用水中硼酸和硅酸的检测,并为半导体行业超纯水中硼酸和硅酸的同时检测提供了参考。
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[Determination of boric acid and silicic acid in mineral water by nonsuppressed ion chromatography].

Boron and silicon are widely distributed in nature; in water, these compounds typically present in the forms of boric acid and silicic acid, respectively. The maximum allowable levels of silicic acid and boric acid in water are stipulated in relevant national and industry standards, such as GB 8538-2022. Quality changes in water, which are of great significance in water-quality evaluations, can be understood in terms of its silicic acid and boric acid contents. Boric acid content is usually determined by ion exclusion chromatography, whereas silicic acid content is usually determined by postcolumn derivatization. Therefore, traditional methods cannot achieve the simultaneous determination of silicic acid and boric acid contents in water. Modern ion chromatography has been widely used in the detection of ionic compounds, such as anions, cations, organic acids, organic amines, amino acids, and sugars. Boric (pKa=9.24) and silicic (pKa=9.77) acids are weak acids that dissociate into ionic states under alkaline conditions. Although these compounds cannot be tested using suppressed ion chromatography, they can be retained on ion chromatography columns. In this study, a method based on nonsuppressed conductance detection was established for the simultaneous determination of boric acid and silicic acid in water. The contents of boric acid and silicic acid were detected by nonsuppressed ion chromatography using a Dionex IonPacTM AS20 analytical column. The chromatographic conditions were as follows: flow rate, 1.0 mL/min; column temperature, 30 ℃; eluent, 6 mmol/L sodium hydroxide solution and 60 mmol/L mannitol; and sample injection volume, 50 μL. The effective separation of silicic acid and boric acid was achieved within 8 min. SiO32- and boric acid demonstrated good linear relationships in the concentration ranges of 0.25-100 and 0.5-100 mg/L (correlation coefficients, 0.9999), respectively. The method detection (MDL) and quantification (MQL) limits were 0.078 and 0.26 mg/L for SiO32-, and the MDL and MQL limits were 0.18 and 0.60 mg/L for boric acid. The average recoveries of boric acid and SiO32- (n=6) were 97.3%-105.3%. Moreover, the relative standard deviations were less than 0.9% for boric acid at four spiked levels and less than 0.30% for SiO32- at three spiked levels. Thus, the method meets detection requirements. The pretreatment method is very simple, and the sample can be directly injected through a 0.22 μm water filtration membrane and into the column. The boric acid and silicic acid contents in nine mineral drinking water samples were determined under the optimized analytical conditions. Boric acid was not detected in these nine samples, but silicic acid was detected in six samples. The silicic acid contents detected were between 18.70 and 62.08 mg/L, which was consistent with the concentration ranges marked on the manufacturers' packaging. The proposed method can be used for the determination of boric acid and silicic acid in mineral drinking water and laboratory water, and provides a reference for the simultaneous detection of boric acid and silicic acid in ultrapure water used in the semiconductor industry.

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来源期刊
色谱
色谱 CHEMISTRY, ANALYTICAL-
CiteScore
1.30
自引率
42.90%
发文量
7198
期刊介绍: "Chinese Journal of Chromatography" mainly reports the basic research results of chromatography, important application results of chromatography and its interdisciplinary subjects and their progress, including the application of new methods, new technologies, and new instruments in various fields, the research and development of chromatography instruments and components, instrument analysis teaching research, etc. It is suitable for researchers engaged in chromatography basic and application technology research in scientific research institutes, master and doctoral students in chromatography and related disciplines, grassroots researchers in the field of analysis and testing, and relevant personnel in chromatography instrument development and operation units. The journal has columns such as special planning, focus, perspective, research express, research paper, monograph and review, micro review, technology and application, and teaching research.
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