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| 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 |
| Received:July 07, 2020 |
| 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) |
| Author Name | Affiliation | E-mail | | HU Dan-jing | Zhejiang Fangyuan Test Group Co. Ltd, Zhejiang Gold and GEM Testing Center, Hangzhou 310018, China | hu_danjing@126.com | | YAN Xue-jun | Zhejiang Fangyuan Test Group Co. Ltd, Zhejiang Gold and GEM Testing Center, Hangzhou 310018, China | 4849523@qq.com | | PENG Qiu-jin | Zhejiang Fangyuan Test Group Co. Ltd, Zhejiang Gold and GEM Testing Center, Hangzhou 310018, China | | | ZHANG Xu | Zhejiang Fangyuan Test Group Co. Ltd, Zhejiang Gold and GEM Testing Center, Hangzhou 310018, China | | | ZHU Yi-jie | Zhejiang Fangyuan Test Group Co. Ltd, Zhejiang Gold and GEM Testing Center, Hangzhou 310018, China | |
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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(RSD，n=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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