火花放电原子发射光谱法分析钢铁屑状样品的探讨  

Discussion on the analysis of chip steel sample by spark discharge atomic emission spectrometry

作　　者：黄太忠 周西林 王娇娜 王亚森 叶反修 HUANG Tai-zhong;ZHOU Xi-lin;WANG Jiao-na;WANG Ya-sen;YE Fan-xiu(Chong Qing Academy of Metrology and Quality Inspection, Chongqing 401123, China;National Quality Supervision and Inspection Center for Aluminum Magnesium Alloys and Products,Chongqing 408403,China;Wuxi Jin Yi Bo Instrument Technology Co., Ltd., Wuxi 214151,China)

机构地区：[1]重庆市计量质量检测研究院,重庆401123 [2]国家铝镁合金及制品质量监督检验中心,重庆408403 [3]无锡市金义博仪器科技有限公司,江苏无锡 214151

出　　处：《冶金分析》2019年第8期38-44,共7页Metallurgical Analysis

基　　金：国家质量监督检验检疫总局科技攻关项目(2017QK031)

摘　　要：屑状样品其外观呈无规则状态,并具有一定的流动性。在一般情况下,它不能完全覆盖仪器的激发孔,无法形成一个密闭的氩气气氛,因此不能采用火花放电原子发射光谱法直接检测。为了能采用该法测定屑状样品,试验将钢铁屑状样品进行分类,根据各类金属屑状样品的强度和硬度选择合适的制样方法,将样品制备成规则的块状样品。其中塑性和韧性较好的样品采用冷压法制样,而超高强度、脆性大以及不适合冷压法制样的样品采用熔融法制样。制备好的样品选择合适的校准曲线,采用控样法,对样品进行定量分析。对样品10个不同部位测定的数据进行统计,测定结果的相对标准偏差(RSD,n=10)均小于2%,符合标准JJG768-2005中的A级要求。用一级或二级标准物质/样品进行验证,测定值与认定值的差值都在标准物质规定的不确定度范围内。The chip samples have irregular appearance and certain flowability. Under normal circumstances, the chip samples cannot fully cover the excitation hole of instrument to form a closed argon atmosphere. As a result, they cannot be directly detected by spark discharge atomic emission spectrometry. In order to determine the chip samples by this method, the chip steel samples in experiments were classified. The appropriate sample preparation method was selected based on the strength and hardness of various chip metal samples.The samples with good plasticity and toughness were cold pressure samples, while those with high strength and brittleness and unsuitable for cold pressure samples were melt samples.The prepared samples were quantitatively analyzed using sample control method by selecting the suitable calibration curve. The determined data of ten different positions of sample were used for statistic analysis. The relative standard deviations (RSD, n =10) were all less than 2%, which could meet the level-A requirements in standard JJG 768-2005. The primary and secondary reference materials/samples were used for verification. The differences between the experimental values and the certified values were all within the range of uncertainty specified by the certified reference materials.

关 键 词：火花放电原子发射光谱法 钢铁 屑状样品 成分分析 

分 类 号：O657.31[理学—分析化学]