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惰气熔融-红外吸收法测定锆铌合金中氢

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锆铌合金中氢的含量会影响材料的机械性能,因此需要对其准确测定和严格控制.将锆铌合金样品用线切割的方法制备成3 mm×3 mm×20 mm的条状样品,样品经打磨至表面光滑,剪切至0.1 g左右的小粒,使用丙酮进行清洗.称取0.10 g样品,投入脱气后的石墨套坩埚中,控制分析功率为4.0 kW,积分时间为50 s,实现了惰气熔融-红外吸收法对锆铌合金中低含量(小于5 μg/g)氢的测定.方法检出限为0.03 μg/g,定量限为0.1 μg/g.按照实验方法测定2个锆铌合金样品中氢含量,测定值分别为4.3、2.2 μg/g,相对标准偏差(n=11)分别为8.6%、20%.用氢含量为4.3 μg/g的锆铌合金样品采用热导法测定其氢含量进行方法比对,测定结果与红外法测定结果吻合.
Determination of hydrogen in zirconium-niobium alloy by inert gas fusion-infrared absorption method
The hydrogen content in zirconium-niobium alloy will influence on the mechanical property of ma-terial.Therefore,it should be accurately determined and strictly controlled.The zirconium-niobium alloy sample was cut into strip specimens(3 mm×3 mm×20 mm)by wire cutting method.Then the specimens were polished until the surface was smooth.After cutting into small particles with mass of about 0.1 g,the specimens were cleaned with acetone.0.10 g of specimen was weighed and transferred into duplex graphite crucible after degassing.The analysis power was controlled at 4.0 kW,and the integral time was 50 s.The determination of low content hydrogen(less than 5 μg/g)in zirconium-niobium alloy by inert gas fusion-infrared absorption method was realized.The limit of detection was 0.03 μg/g,and the limit of quantification was 0.1 μg/g.The hydrogen content in two zirconium-niobium alloy samples was deter-mined according to the experimental method,and the found result was 4.3 and 2.2 μg/g,respectively.The relative standard deviation(RSD,n=11)was 8.6%and 20%,respectively.The hydrogen content in zirconium-niobium alloy samples(with hydrogen content of 4.3 µg/g)was measured by thermal conductiv-ity method for comparison,and the determination results were consistent with those by the infrared meth-od.

inert gas fusioninfrared absorption methodzirconium-niobium alloylow hydrogen

王宽、高东旭、石新层、王芳、张哲、郑伟

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西安汉唐分析检测有限公司,陕西西安 710201

西北有色金属研究院,陕西西安 710016

惰气熔融 红外吸收法 锆铌合金 低氢

陕西省创新能力支撑计划

2021PT-024

2024

冶金分析
中国钢研科技集团有限公司(钢铁研究总院) 中国金属学会

冶金分析

CSTPCD北大核心
影响因子:1.124
ISSN:1000-7571
年,卷(期):2024.44(5)