作者：董礼男, 周莉莉, 朱春要, 张继明

作者单位：江苏省（沙钢）钢铁研究院，江苏 张家港 215625

关键词：高频感应燃烧;红外吸收法;轧钢;含油污泥;硫

摘要：

钢铁厂在热轧、酸洗、冷轧等工序产生的固体混合物被称为轧钢含油污泥，其主要成分为氧化铁皮和油脂，这类固体废弃物经一系列处理后可作为烧结原料被重新利用。轧钢含油污泥中含一定量的硫，硫元素在钢铁冶炼过程中作为有害杂质需严格控制其含量，因此准确测定轧钢含油污泥中硫含量对其后续回收利用具有重要意义。该文建立高频感应燃烧红外吸收法测定轧钢含油污泥中硫含量的方法，重点讨论样品除油前处理的温度、称样量、助熔剂等参数，确定最佳工作条件：样品除油温度为500 ℃，称样量为0.10 g，助熔剂用量为1.2 g W+0.2 g Sn+0.2 g Fe，采用铁矿石、炉渣标准样品校准曲线，结果表明：方法的检出限为0.00067%，定量限为0.0022%。按照本实验方法测定轧钢含油污泥中硫含量，测定结果的相对标准偏差（RSD, n=8）小于3.0%，加标回收率在97.4%~102%之间。

Determination of sulfur contents in rolling oily sludge by high frequency induction combustion infrared absorption method
DONG Linan, ZHOU Lili, ZHU Chunyao, ZHANG Jiming
Institute of Research of Iron and Steel, Jiangsu Province/Sha-Steel, Zhangjiagang 215625, China
Abstract: The mixture of scale and grease producted in hot rolling, pickling, cold rolling and other rolling processes of mills is called rolling oily sludge. This kind of solid waste can be reused as sintering material after a series of treatment. Amounts of sulfur must be existed in rolling oily sludge. It must be strictly controlled as a detrimental element in iron and steel smelting process. Therefore, accurate determination of sulfur in rolling oily sludge is useful to guide its subsequent treatment. The determination of sulfur content in rolling oily sludge by high frequency induction combustion infrared absorption method was established. The key parameters such as pre-treatment temperature of sample degreasing, sample mass and flux were focused. The optimum experimental conditions were obtained as follow: oil removal temperature was 500 ℃, 0.10 g of sample were weighed, then multiple fluxes were added (1.2 g of tungsten+0.2 g of tin+0.2 g of iron), the instrument was calibration using certified reference materials of iron ore and slag. The results showed that the limit of detection was 0.00067%, and the limit of quantitation was 0.0022%. The contents of sulfur in rolling oily sludge sample were determined according to the experimental method. The relative standard deviations (RSD, n=8) of determination results were less than 3.0%. The recoveries were 97.4% to 102%.
Keywords: high frequency induction combustion;infrared absorption method;rolling;oil sludge;sulfur
2022, 48(10):68-72  收稿日期: 2021-08-28;收到修改稿日期: 2021-11-16
基金项目:
作者简介: 董礼男（1988-），女，辽宁丹东市人，工程师，研究方向为钢铁冶金分析、金属表面处理等
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