电工钢 ›› 2026, Vol. 8 ›› Issue (5): 43-49.

• • 上一篇    下一篇

无取向硅钢中超低碳硫检出下限及准确性影响因素研究

易赛,向前,崔隽,黄双,夏军旗   

  1. 武汉钢铁有限公司质检中心,湖北武汉430080
  • 出版日期:2026-10-28 发布日期:2026-10-15

Study on the detection limit and accuracy of ultra-low C and S in non-oriented silicon steel

YI Sai, XIANG Qian, CUI Jun, HUANG Shuang, XIA Junqi   

  1. Quality Inspection Center of Wuhan Iron and Steel Co., Ltd., Wuhan 430080, China
  • Online:2026-10-28 Published:2026-10-15

摘要: 针对现行红外吸收法检测无取向硅钢中碳硫元素时超低含量段检测准确性不满足生产的问题,系统研究了超低碳硫检出下限的确定方法及对检测准确性有显著影响的因素,并提出一组最优配置参数。研究通过空白试验标准偏差法(3σ准则)测定了方法检出下限:碳为0.6×10??,硫为0.5×10??,可将超低碳硫检测下限由常规的10×10??延伸至5×10??以下。对坩埚预处理、载气、助熔剂、试样加工及分析功率等关键影响因素进行了优化,各项优化试验均以碳和硫双元素数据作为评价依据:坩埚预处理设定电炉温度为恒定1100 ℃灼烧30 min;选用加装氧气净化器的厂内管道氧(纯度99.99%);选用国产钨锡助熔剂,先加助熔剂再加试样;试样制备完成后无需预处理;分析功率设定为80%。优化后采用碳含量3.4×10??、硫含量4.4×10??的标准物质进行验证,测定结果准确、精密度良好,满足高端无取向硅钢生产检测需求。

关键词: 红外碳硫分析仪;超低碳硫;检出下限;准确性;影响因素

Abstract: To address the insufficient detection accuracy in the ultra-low content range for carbon and sulfur elements in non-oriented silicon steel using the conventional infrared absorption method, this study systematically investigated the determination of ultra-low carbon and sulfur detection limits and the factors significantly affecting detection accuracy, and proposed a set of optimal configuration parameters. The method detection limits of carbon 0.6×10?? and sulfur 0.5×10?? were determined by the blank test standard deviation method (3σ criterion), extending the detection limit from the conventional 10×10?? to below 5×10??. Key influencing factors including crucible pretreatment, carrier gas, fluxing agent, sample preparation, and analysis power were optimized, with both carbon and sulfur dual-element data used as evaluation criteria throughout all optimization experiments. The optimal parameters were obtained: crucible pretreatment at 1100 ℃ for 30 min; in-plant pipeline oxygen (99.99% purity) with oxygen purifier; domestic W-Sn flux added before sample; no sample pretreatment needed; analysis power at 80%. Verification using reference materials with carbon 3.4×10?? and sulfur 4.4×10?? demonstrated accurate results and good precision, meeting the quality control requirements for high-grade non-oriented silicon steel production.

Key words: infrared carbon-sulfur analyzer; ultra-low carbon and sulfur; detection limit; accuracy; influencing factors