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Determination of Boron in Nickel-Based Brazing Material by ICP-AES
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摘要: 探讨了电感耦合等离子体发射光谱法(ICP-AES)测定镍基钎料中硼的分析条件.试样经王水低温溶解, 然后高温发硫酸烟, 选择182.641nm作为分析谱线, 同时采用基体匹配法配制标准样品, 不仅有效降低了基体效应, 同时解决了无标校正的问题, 校准曲线的线性范围为0~0.06mg/mL, 相关系数为0.99998.方法应用于实际样品分析, 方法检出限为3×10-5mg/mL(n=11), 方法相对标准偏差为0.32%~0.65%, 回收率为99.2%~100.6%.
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关键词:
- 电感耦合等离子体发射光谱法 /
- 镍基钎料 /
- 硼 /
- 溶样方法 /
- 基体匹配
Abstract: The analytical conditions of boron in nickel-based brazing material by ICP-AES were discussed in this paper. The samples were dissolved in aqua regia at low temperature, and fumed in sulfuric acid at high temperature with a large quantity of smoke. The standard samples were prepared according to the matrix matching method, which not only reduced the matrix effect, but also solved the problem of lack of standard reference material. The linearity range was 0~0.06 mg/mL with a correlation coefficient of 0.999 98. The contents of boron in the nickel-based brazing samples were determined by ICP-AES using the spectral line of 182.641 nm. The detection limit was 3×10-5mg/mL (n=11). The relative standard deviations (RSD) was 0.32%~0.65% and the recovery was 99.2%~100.6%.-
Key words:
- ICP-AES /
- nickel-based brazing materials /
- boron /
- dissolution method /
- matrix matching
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表 1 仪器工作条件
Table 1. Working conditions of instrument
高频功率/W 雾化器 泵速/(r/min) 积分时间/s 压力/Mpa 流量/(L/min) 长波 短波 1 150 1.79×10 -4 1.0 125 10 10 
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表 2 精密度及加标回收试验
Table 2. Analytical results of precision and recovery tests
% 样品 测得质量分数 已知质量分数 RSD 加标质量分数 测定质量分数 回收率 Cr17Ni25 1.86 1.85 1.87 1.85 1.87 1.86 1.86 0.65 1.50 3.38 100.6 B2标样2.00 3.85 99.7 B-Ni82Cr 2.54 2.54 2.53 2.53 2.54 2.52 2.51 0.32 2.50 5.01 99.6 SiB试样13.00 5.55 100.4 B-Ni82Cr 2.87 2.86 2.84 2.85 2.86 2.85 2.90 0.32 2.50 5.34 99.2 SiB试样2 4.00 6.85 99.8
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