CN106645007B - 一种钢中硫化物含量的检测方法 - Google Patents
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Abstract
一种钢中硫化物含量的检测方法,属于钢板化学分析技术领域。包括用两种电解液对试样进行电解,用有机滤膜过滤收集电解析出物渣样;连同滤膜空气干燥后,锡箔包裹放入预先覆盖0.5g~1g氧化铝粉末的专用瓷舟待测;采用管式炉-红外线吸收法测定钢中硫化物含量,设定管炉温度1250~1300℃,氧气流速3.0L/min,分析时间为100~300秒;进行样品测定,保证在设定分析时间内燃烧完全。优点在于,操作简单、快速准确,成本低廉,适合于工业广泛应用。
Description
技术领域
本发明属于钢板化学分析技术领域,特别涉及一种钢中硫化物含量的检测方法。
背景技术
硫化物是钢中最常见的夹杂物之一,它对钢的性能有显著的影响,因此,为改善钢的性能,尽可能排除钢中夹杂物影响到最低限度,是冶金工作者多年的愿望。然而,近年来人们对夹杂物及其存在又有了新的认识和评价。对不少的钢种,如易切削钢、滚珠钢、高速工具钢等,钢中存在适量的硫并使其以适当形态的硫化物存在,不但无害反而有利,因此控制钢中硫化物形态和硫含量是至关重要的。
钢中硫化物的提取一般是采用电解法,针对不同的钢种,选择不同的电解液,得到电解析出物渣样,对其进行测定,得到钢中硫化物的含量。
钢中硫化物测定没有国家标准,有文献介绍,针对某一种硫化物的测定,如硫化钙和硫化锰,可以采用测定钙和锰的含量来换算硫的含量;也有资料介绍,采用高频红外吸收法测定硫化物的硫含量。但是经过试验,因为钢样的电解析出物渣样是用有机滤膜过滤收集,由于有机滤膜的存在,在使用高频红外碳硫仪进行测定时,试样不易分解,且会影响红外碳硫仪对碳的测定,而去除滤膜刮取试样测定,会损失试样导致测定不准确。
本发明采用管式炉红外吸收法,对钢中硫化物的测定进行试验研究,对钢样的电解提取试样,采用锡箔包裹,用氧化铝和氧化镁助熔和缓燃的样品制备方法,在1250-1300℃条件下进行测定,解决了钢的硫化物析出物渣样反应时间长,不易分解的难题,同时解决了有机滤膜对测定的干扰问题,获得准确的测定结果。同时实现专用坩埚的重复使用,实现成本节约。本发明方法完全能满足钢中硫化物含量的测定要求,测定结果有良好的稳定性、重现性和准确性,并且具有检测范围宽,操作简单,数据准确,速度快的特点,目前已应用于本企业的生产实践,值得推广。
发明内容
本发明的目的在于提供了一种钢中硫化物含量的检测方法,解决了钢中硫化物电解析出物渣样不易分解,包裹有机滤膜干扰测定的问题,实现了专用坩埚的重复使用,提供了全新的样品制备方法,从而获得准确的测定结果。
一种钢中硫化物含量的检测方法,具体步骤及参数如下:
1、选用非水电解液或水电解液两种电解液对试样进行电解,用有机滤膜过滤收集电解析出物渣样。非水电解液,即:1wt%四甲基氯化铵+10wt%乙酰丙酮的甲醇溶液,在-24℃,总电流0.6A,电流密度0.03~0.05A/㎝2,进行电解,用有机滤膜过滤收集电解析出物渣样;水电解液,即:5wt%氯化钾+1wt%柠檬酸+水,在+2~+5℃,总电流0.6A,电流密度0.03~0.05A/㎝2,进行电解,取4-10份电解渣样合并,用有机滤膜过滤收集电解析出物渣样。
2、测定样品制备:将用有机滤膜过滤收集的钢的电解析出物渣样,连同滤膜空气干燥后,用锡箔包裹,放入预先覆盖0.5g~1g氧化铝粉末的专用瓷舟,在样膜上先覆盖约0.1~0.15g光谱纯氧化铜粉末,再覆盖1g~2g氧化铝粉末,做为待测样品。
3、采用管式炉-红外线吸收法测定钢中硫化物含量,设定管炉温度1250~1300℃,氧气流速3.0L/min,分析时间为100~300秒;进行样品测定,保证所有样品试料,在设定分析时间内燃烧完全,获得准确的试验数据。
本方法测定钢中硫化物含量加标回收率在98%以上,精密度试验RSD小于3%。
说明采用管式炉-红外线吸收法测定钢中硫化物含量,完全能够满足科研生产的要求,数据准确可靠。
本发明的优点在于:
1、提供了一种钢中硫化物含量的检测方法,即管式炉-红外线吸收法,该方法操作简单、快速准确,适合于工业广泛应用。
2、提供了一种全新的样品制备方法,即在1250~1300℃条件下,样品用锡箔包裹,采用氧化铝和氧化铜进行缓燃和助熔,解决了析出物渣样不易分解的难题,同时解决了有机滤膜对测定的干扰问题,保证样品分解完全,获得准确的数据。同时本法的燃烧反应无喷溅,残渣少,对仪器气路和管炉的污损小,反应后坩埚中无熔块附着,能够实现专用坩埚的重复使用,实现成本节约。
具体实施方式
实施例1
易切削钢中硫化物的测定:
1、选用非水电解液,即:1wt%四甲基氯化铵+10wt%乙酰丙酮的甲醇溶液,在-24℃,总电流0.6A,电流密度0.03~0.05A/㎝2,电解1小时,用有机滤膜过滤收集电解析出物渣样。
2、测定样品制备:将用有机滤膜过滤收集的钢的电解析出物渣样,连同滤膜空气干燥后,用锡箔包裹,放入预先覆盖0.5g氧化铝粉末的专用瓷舟,在样膜上先覆盖约0.1~0.15g光谱纯氧化铜粉末,再覆盖1g氧化铝粉末,做为待测样品。
3、选定试验参数为管炉温度1300℃,氧气流速3.0L/min,最短分析时间为80秒,最长分析时间为180秒;比较水平选择1,进行样品测定。
4、钢中硫化物样品的测定:按上述方法进行样品测定,两次测定值为S(w/%):0.229,0.227,平均值S(w/%):0.228%。
实施例2
IF钢中硫化物的测定:
1、选用水电解液,即:5wt%氯化钾+1wt%柠檬酸+水,在+2~+5℃,总电流0.6A,电流密度0.03~0.05A/㎝2,电解2小时,取4份电解渣样合并,用有机滤膜过滤收集电解析出物渣样。
2、测定样品制备:将用有机滤膜过滤收集的钢的电解析出物渣样,连同滤膜空气干燥后,用锡箔包裹,放入预先覆盖0.5g氧化铝粉末的专用瓷舟,在样膜上先覆盖约0.1~0.15g光谱纯氧化铜粉末,再覆盖1g氧化铝粉末,做为待测样品。
3、选定试验参数为管炉温度1300℃,氧气流速3.0L/min,最短分析时间为100秒,最长分析时间为300秒;比较水平选择1,进行样品测定。
4、钢中硫化物样品的测定:两次测定值为S(w/%):0.0040,0.0038,平均值为S(w/%)0.0039%。
Claims (2)
1.一种钢中硫化物含量的检测方法,其特征在于,具体步骤及参数如下:
1)选用非水电解液或水电解液两种电解液对试样进行电解,用有机滤膜过滤收集电解析出物渣样;
2)测定样品制备:将用有机滤膜过滤收集的钢的电解析出物渣样,连同滤膜空气干燥后,用锡箔包裹,放入预先覆盖0.5g~1g氧化铝粉末的专用瓷舟,在上先覆盖约0.1~0.15g光谱纯氧化铜粉末,再覆盖1g~2g氧化铝粉末,作为待测样品;
3)采用管式炉-红外线吸收法测定钢中硫化物含量,设定管炉温度1250~1300℃,氧气流速3.0L/min,分析时间为100~300秒;进行样品测定,保证所有样品试料在设定分析时间内燃烧完全,获得准确的试验数据。
2.根据权利要求1所述的方法,其特征在于,所述的步骤1)中的两种电解液为非水电解液,即:1wt%四甲基氯化铵+10wt%乙酰丙酮的甲醇溶液,在-24℃,总电流0.6A,电流密度0.03~0.05A/㎝2,进行电解,用有机滤膜过滤收集电解析出物渣样;以及水电解液,即:5wt%氯化钾+1wt%柠檬酸+水,在+2~+5℃,总电流0.6A,电流密度0.03~0.05A/㎝2,进行电解,取4~10份电解渣样合并,用有机滤膜过滤收集电解析出物渣样。
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