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研究了电感耦合等离子体发射光谱法测定船舶和海洋工程用结构钢中微量酸溶硼的分析方法，考察了样品消解器皿和无机酸对硼元素测定的影响，优选了分析谱线，讨论了铁离子、共存离子对测定结果的背景干扰。仪器最佳工作条件为：射频功率1.15 kW、雾化压力0.18 MPa、辅助气流量0.5 L/min、泵速100 r/min。称取0.500 g试样于石英器皿中，采用1 mL高纯水、9 mL盐酸和3 mL硝酸加热消解制备待测试液。将试液导入电感耦合等离子体发射光谱仪，优选B 182.64 nm分析谱线，候选182.58及208.96 nm，采用铁基体匹配配制工作曲线消除背景干扰，线性相关系数达0.999。经多家实验室协同验证，方法定量限为0.0002%～0.0005%，钢铁标准样品测定结果与认定值相符；在95%的显著性水平下，0.001%、0.004%、0.012%、0.150%四个水平实验结果的重复性限（r）分别为0.0003%、0.0008%、0.002%、0.015%，再现性限（R）分别为0.0005%、0.001%、0.002%、0.023%，精密度水平与经典方法甲醇蒸馏-姜黄素光度法基本相符。
Abstract：An analytical method was developed for the determination of trace acid-soluble boron in structural steels for ship and ocean engineering by inductively coupled plasma optical emission spectrometry(ICP-OES). The effects of sample digestion vessels,inorganic acids,and instrumental parameters, including radio frequency power,nebulizer pressure,auxiliary gas flow rate,and pump speed on the determination of boron were investigated. The optimal analytical spectral line was selected,and the background interferences from the iron matrix and coexisting ions were discussed. The optimal working conditions were determined as follows:radio frequency power of 1. 15 kW, nebulizer pressure of 0. 18 MPa,auxiliary gas flow rate of 0. 5 L/min,and pump speed of 100 r/min. A 0. 500 g sample was weighed into a quartz vessel and digested with 1 mL of water,9 mL of hydrochloric acid,and 3 mL of nitric acid by heating to prepare the test solution. The B 182. 64 nm spectral line was selected for analysis,with 182. 58 nm and 208. 96 nm as alternatives. A matrix-matching method was employed to eliminate background interference,and a series of calibration curves were established using an iron matrix solution,achieving a linear correlation coefficient of 0. 999. Through an inter-laboratory collaborative study,the limit of quantification(LOQ) of the method was found to be 0. 0002%-0. 0005%. The results for steel standard reference materials were in good agreement with their certified values. At a 95% confidence level,the repeatability limits(r) for the four concentration levels of 0. 001%,0. 004%,0. 012%,and 0. 150% were 0. 0003%,0. 0008%,0. 002%,and 0. 015% respectively,while the reproducibility limits(R) were 0. 0005%,0. 001%,0. 002%,and 0. 023% respectively. The precision of the method was generally comparable to that of the classical methanol distillationcurcumin photometric method.
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基本信息:
DOI：10.20236/j.CJIAC.2026.05.014
中图分类号:O657.31;TG142
引用信息:
[1]胡剑,刘攀,李亚,等.电感耦合等离子体发射光谱（ICP-OES）法测定船舶和海洋工程用结构钢中微量酸溶硼[J].中国无机分析化学,2026,16(05):841-851.DOI:10.20236/j.CJIAC.2026.05.014.
基金信息:
国防科工委基础科研项目（T082005A001）; 国防科工局技术基础科研项目（JSBZ2014207A008）; 国家新材料生产应用示范平台项目（TC180A6MR/2）; ASTM标准制修订计划项目（WK49476,WK60405）~~
2026-02-24
2026-02-24
2026-02-24