文章摘要
火花直读光谱法测定合质金的含铂量
Determination of platinum content in alloy gold by spark emission spectrometry
投稿时间:2020-07-07  
DOI:
中文关键词: 分析化学  火花直读光谱法  合质金  铂含量
英文关键词: analytical chemistry  spark emission spectrometry  alloy gold  platinum content
基金项目:浙江省市场监督管理局科研计划项目(20190321);国家自然科学基金(21506187)
作者单位E-mail
胡丹静 浙江方圆检测集团股份有限公司浙江省黄金珠宝饰品质量检验中心杭州 310018 hu_danjing@126.com 
严雪俊 浙江方圆检测集团股份有限公司浙江省黄金珠宝饰品质量检验中心杭州 310018 4849523@qq.com 
彭秋瑾 浙江方圆检测集团股份有限公司浙江省黄金珠宝饰品质量检验中心杭州 310018  
张旭 浙江方圆检测集团股份有限公司浙江省黄金珠宝饰品质量检验中心杭州 310018  
朱毅杰 浙江方圆检测集团股份有限公司浙江省黄金珠宝饰品质量检验中心杭州 310018  
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中文摘要:
      为了解决合质金成分快速测定需求,建立了火花直读光谱法测定合质金中铂含量的方法。用铣削法处理试样表面,优化光源激发条件为:高压设定1000 V、冲洗时间3 s、预燃时间10 s、曝光时间5 s,氩气流量3.5 L/min,以319.80 nm谱线作为参比线,优选Pt 265.95 nm为分析谱线。该方法下铂元素在0.0002%~0.105%范围内与发射强度的线性关系良好,相关系数大于0.999。利用高、低铂含量的光谱金标样进行精密度试验,铂元素测定结果的相对标准偏差(RSDn=6)在1.3%~7.4%之间。对合质金未知样品进行正确度试验,铂含量测试结果与ICP-AES法基本一致。另外通过漂移校正验证了仪器的测试稳定性。
英文摘要:
      In order to meet the rapid determination requirements of chemical components in alloy gold, the determination method of platinum by spark emission spectrometry was developed. The sample was prepared by a milling method. The optimized spark excitation conditions were as follows: 1000 V of voltage setting, 3 sec of flush time, 10 sec of pre-burning time, 5 sec of integral time, and 3.5 L/min of argon flow. Line 319.80 nm was used as a reference line,and the spectral line of Pt 265.95 nm was selected as the analytical line. Platinum element has a good linear relationship with the emission intensity in the concentration range of 0.0002%~0.105%, and the correlation coefficient is greater than 0.999. The precision tests were performed using purchased certified reference gold materials with high and low contents, and the relative standard deviation (RSD, n=6) of platinum was between 1.3% and 7.4%. The unknown alloy gold samples were used for accuracy tests, and the measured platinum contents were consistent with those obtained by ICP-AES. Besides, the stability of the instrument was verified by drift calibration.
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