工业硫磺产品检测新技术

New technology for detecting industrial sulfur products

关键词:  硫磺  砷含量  铁含量  硫化氢和多硫化氢含量  微波消解  原子吸收光谱法  原子荧光光谱法  红外光谱法  标准化

Key words:  sulfur  arsenic content  iron content  hydrogen sulfide and hydrogen polysulfide content  microwave digestion  atomic absorption spectrometry  atomic fluorescence spectroscopy  infrared spectroscopy  standardization

摘要:

硫磺是一种用途广泛的重要化工原料,其产品质量依据GB/T 2449.1-2014《工业硫磺 第1部分:固体产品》和GB/T 2449.2-2015《工业硫磺 第2部分:液体产品》指标和检测方法进行判别。针对工业硫磺标准中检测方法的局限性,建立了光谱法测定砷含量、铁含量、硫化氢和多硫化氢含量等新方法。结果 表明:原子荧光光谱法测定硫磺中砷含量,方法检出限0.005 μg/g、加标回收率94%~103%、与GB/T 2449.1-2014的比对偏差<0.16 μg/g；原子吸收光谱法测定硫磺中铁含量,方法检出限0.1 μg/g、加标回收率91%~109%、与GB/T 2449.1-2014的比对偏差<1 μg/g；红外光谱法测定硫化氢和多硫化氢含量,方法检出限5 μg/g、测量范围5~500 μg/g、重复性<8%；建立的方法满足检测要求。同时也探讨了光谱法测定砷含量、铁含量、硫化氢和多硫化氢含量制定成国家、行业或企业标准的可行性和适用性。

Abstract:

Sulfur is a widely used important chemical raw material, the quality of sulfur is determined according to the indicators and test methods stipulated in GB/T 2449.1-2014 Sulfur For Industrial Use-Part 1 :Solid Product and GB/T 2449.2-2015 Sulfur For Industrial Use-Part 2 :Liquid Product. In view of the limitations of the existing methods such as the content of iron and arsenic in industrial sulphur standards, new methods for the determination of arsenic content, iron content, hydrogen sulfide and hydrogen polysulfide content by spectrometry has been established. The results showed that:method for the determination of arsenic content in sulfur by atomic fluorescence spectroscopy has a detection limit of 0.005 μg/g, standard recovery rate of 94% to 103%, and comparison deviation with GB/T 2449.1-2014 less than 0.16 μg/g; method for the determination of iron content in sulfur by atomic absorption spectroscopy has a detection limit of 0.1 μg/g, standard recovery rate of 91% to 109%, and comparison deviation with GB/T 2449.1-2014 less than 1 μg/g; method for the determination of sulfur hydrogen and hydrogen polysulfide content in sulfur by infrared spectroscopy has a detection limit of 5 μg/g, measurement range of 5 μg/g to 500 μg/g and repeatability less than 8%. All the established methods meet the testing requirements. At the same time, the feasibility and applicability of methods for the determination of arsenic content, iron content, hydrogen sulfide and hydrogen polysulfide content by spectroscopy developed as national, industrial or enterprise standards are also discussed.