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铜试金预富集-辉光放电质谱法测定贵金属矿样中痕量铂钯铱金陈丁文;李斌;董守安;普朝光【摘要】对利用铜试金预富集后辉光放电质谱法(GDMS)测定贵金属矿样中痕量Pt、Pd、Ir、Au的方法进行了探索性研究.着重考察了铜试金条件的选择和辉光放电电极的匹配、质谱的测定条件和测定方法等.分析结果表明,痕量(μg级)贵金属元素Pt的含量在1.99～15.0μg,回收率为92.0%～111.9%;Pd的含量在3.15～29.78μg,回收率为88.4%～113.3%;Ir的含量在0.12～0.60 μg,回收率为68.3%～100.0%;Au的含量在10.43～24.08μg,回收率为98.9%～127.0%.方法可应用于矿石、矿物及其他物料中痕量贵金属的分析.【期刊名称】《岩矿测试》【年(卷),期】2008(027)005【总页数】4页(P329-332)【关键词】铜试金;辉光放电质谱法;贵金属;矿样【作者】陈丁文;李斌;董守安;普朝光【作者单位】云南警官学院,云南,昆明,650223;云南警官学院,云南,昆明,650223;昆明贵金属研究所,云南,昆明,650221;昆明物理研究所,云南,昆明,650223【正文语种】中文【中图分类】O652.6;O657.63;O614.82;O614.123铜的原子半径、晶体结构和价态等方面与贵金属相近或相似，能满足形成固熔体的要求而成为较好的试金捕集剂[1-4]。
以往铜试金所得的试金扣较大，湿法溶解后与贵金属分离再进行测定的工序是相当繁琐的，结果也欠可靠性。
因此，铜试金法的发展受到限制。
辉光放电质谱法(GDMS)具有检测灵敏度高、准确度好、重复性好、质量分辨率高而干扰少、线性动态范围宽等优点，是近年来迅速发展并广泛用于高纯物质中痕量和超痕量杂质元素分析的无机质谱新技术[5-7]。
GDMS法能直接使用固体材料，具备全面分析的能力，目前在高纯铂粉的分析中已有研究和应用[8]；但对于矿石、地质试样中痕量或超痕量铂族金属(PGEs)的分析，由于粉末试样的非导体性质，直接测定是困难的。
引用格式：汤云腾. 辉光放电质谱法测定合金钢中各元素的相对灵敏度因子[J]. 中国测试，2024, 50(3): 84-89. TANG Yunteng.Determination of relative sensitivity factors of elements in alloy steel by glow discharge mass spectrometry[J]. China Measurement &Test, 2024, 50(3): 84-89. DOI: 10.11857/j.issn.1674-5124.2021110130辉光放电质谱法测定合金钢中各元素的相对灵敏度因子汤云腾(中国科学院海西研究院厦门稀土材料研究中心，福建 厦门 361021)摘 要: 采用辉光放电质谱法（GDMS ）分析合金钢中元素相对灵敏度因子（RSF ），优化放电电流、气体流量和预溅射时间等条件，排除质谱干扰并选定合适同位素。
研究不同放电条件对元素RSF 的影响，并比较不同基体下RSF 的差异。
通过合金钢标准样品建立回归曲线，获得校正后的相对灵敏度因子(RSF steel )，用于定量分析。
结果表明，放电气体流量是元素RSF 的主要影响因素，轻元素RSF 随放电气体流量增加而减小，重元素RSF 随放电气体流量增加而增大。
合金钢基体下的大部分元素RSF 小于其标准RSF ，经RSF steel 校正的测量值与参考值间的相对偏差低于10%，相对标准偏差（RSD ）小于5%，准确度和精密度良好。
关键词: 辉光放电质谱法; 合金钢; 相对灵敏度因子中图分类号: O657.63; TB9文献标志码: A文章编号: 1674–5124(2024)03–0084–06Determination of relative sensitivity factors of elements in alloy steel by glowdischarge mass spectrometryTANG Yunteng(Xiamen Institute of Rare Earth Materials, Haixi Institutes, Chinese Academy of Sciences, Xiamen 361021, China)Abstract : This paper describes an analytical method to determine the relative sensitivity factors (RSF) of elements in alloy steel by GDMS. The parameters, such as discharge current, gas flow rate and pre-sputtering time were optimized. Also, The mass interferences were investigated and suitable isotopes were selected for analysis. The effects of different discharge conditions on RSF were studied and the differences of RSF between different substrates were compared. The relative sensitivity factors (RSF steel ) obtained by the regression curves established by alloy steel standard samples were used for quantitative analysis. The results showed that the main influence factor of RSF was gas flow rate. With the increase of gas flow rate, RSFs of light elements decreased, but RSFs of heavy elements increased. RSFs of most elements in alloy steel matrix were less than their standard RSFs. Relative deviations between the corrected values and the reference values were less than 10% and the relative standard deviations (RSDs) of most elements were less than 5%. The accuracy and precision were in good agreement.Keywords : glow discharge mass spectrometry (GDMS); alloy steel; relative sensitivity factors收稿日期: 2021-11-27；收到修改稿日期: 2022-02-07作者简介: 汤云腾（1989-），男，福建漳州市人，工程师，硕士，从事材料成分分析研究。
铝合金中微量元素辉光放电质谱定量分析研究李继东;王长华;郑永章【摘要】以辉光放电质谱法对牌号为6063铝合金标样(E421a)中9个元素进行测定,获得每个元素的灵敏度因子(RSF),并考察了辉光放电电流、放电氩气流速以及离子源冷却温度对RSF值的影响.实验结果表明,辉光放电电流和氩气流速对RSF值有明显的影响,离子源冷却温度对其没有影响.以获得的RSF值对6063铝合金标样另一个点(E422a)进行测定验证,测定值与标示值的相对误差在0.5％～5.6％之间,精密度( RSD)小于5％；以同样方法测定了一个7系铝合金样品中的相应元素,并与ICP-AES测定结果对比,结果的准确度和精密度良好.%The nine elements content in 6063 (trademark) alumina alloy standard sample (E421a) were determined, and the relative sensitivity factor (RSF) of each element was obtained. The effects of discharge current, gas rate and the ion source temperature for the RSF were investigated. The results show that the discharge current and gas rate have the obvious effects for the RSF, while the ion source temperature has no effects. In order to verify the RSF accuracy, the nine elements content of another standard sample (E422a) were analyzed by GD-MS through the obtained RSF calibration and the relative deviation, which the actual and marked-value are among 0. 5%-5. 6% with precision of less than 5%. Using the same method for the analysis of 7 series alumina alloy, the good accuracy and precision are achieved, and prove by the comparison of ICP-AES analytical results.【期刊名称】《质谱学报》【年(卷),期】2012(033)001【总页数】5页(P18-22)【关键词】辉光放电质谱;铝合金;相对灵敏度因子;定量分析【作者】李继东;王长华;郑永章【作者单位】北京有色金属研究总院,北京100088;北京有色金属研究总院,北京100088;北京有色金属研究总院,北京100088【正文语种】中文【中图分类】O657.63辉光放电质谱（glow discharge mass spectrometry，GD－MS）是利用辉光放电源作为离子源与质谱仪结合进行元素含量测定的一种分析方法。
辉光放电光谱法分析镀锌钢板张毅,陈英颖,张志颖(宝山钢铁股份有限公司技术中心,上海201900)摘要:介绍了利用辉光放电光谱法分析不同种类的热镀锌板和电镀锌板的镀层定量分析;在锌铁合金化热镀锌板上界面定量计算方法的设计;锌铁合金化热镀锌板表面问题的发现。
试验结果表明,辉光放电光谱法是配合镀锌板产品质量控制、研究开发的一种有效的分析手段。
关键词:辉光放电;光谱法;镀锌板中图分类号:O657.31文献标识码:A文章编号:1001-4020(2004)04-0191-04ANALYSIS OF GALVANIZED ST EEL SHEET S BY GLOW DISCHARGE AESZHANG Yi,CHEN Ying-ying,ZHANG Zh-i ying(T echnical Center,Baoshan I ron and S teel Co.Ltd.,Shanghai201900,China)Abstract:G low discharge A ES(GD-A ES)w as applied effectively to the analysis of galvanized steel sheets.I n application of this analytical technique to the analysi s of galvanized steel sheets,a method was established to meet w ith the analysis of galvanized steel sheets of different pro duction-technolog ies(i.e.the hot-dipping galvanization o f pure zinc or of Zn-Fe alloy,the electroplating of zinc or of Zn-N i alloy and etc.)and to g ive chemical composition of elements in majo r, minor and micro amounts in the coating layer and t heir changes with the change of dept h of the coating layer simultaneously.T he results of the thickness and mass of the coating layer w er e also given,tog ether w ith the results of chemical composition of the substr ate metal.T he proposed method w as also applied to the analysis o f surface-defects.I n t he analysis of samples produced by hot-dipping process w ith Zn-Fe alloy,a correctio n factor was proposed in the calculation of Fe co ntent in the coating lay er to elimite the error due to the coarseness appeared on t he surface of the coating layer.Keywords:G low discharge atomic emission spectrometr y;Surface analysis;Galvanized steel sheet钢板表面镀锌处理是提高抗大气腐蚀的有效方法。
第21卷，第3期光谱学与光谱分析V ol.21，No.3，pp 400-4032001年6月S p ectrosco py and S p ectral A nal y sis June ，!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!2001X -射线荧光光谱法测定溶样后熔融制样金属硅中铁、铝、钙、钛、磷、铜谷松海宋义李旭辉天津出入境检验检疫局，300201天津摘要本文提出了溶解、蒸干然后用熔剂熔融残渣的样品制备方法，解决了金属硅不易直接熔融制样的难题，可以同时测定金属硅中多种杂质元素，消除了基体效应的影响，克服了标准样品对测定的限制，测定范围广，准确度高，通过安排正交试验确定了样品制备条件。
主题词X -射线荧光光谱仪，金属硅，熔融残渣制样方法2000-09-26收，2001-02-11接受；谷松海，1964年3月生，天津检验检疫局技术中心高级工程师金属硅是我国重要的出口产品之一，传统上只对其中铁、铝、钙进行检测。
但近年来越来越多的国家对其中钛、磷、铜等元素提出了检测要求。
现行检测标准［1!3］仅有铁、铝、钙的检测方法。
文献［4］提出了采用正丁醇-三氯甲烷萃取富集，S nC l 2还原显色后反萃取吸光光度测磷的方法。
X -射线荧光光谱具有分析结果准确、快速、简便、成本低的特点。
但金属硅及铁合金类样品因单质元素的存在不易直接采用熔融法制样，大多采用粉末压片法制备样品［5!7］，使得分析结果准确度受样品粒度影响较大［8］，又因采用固体制样，所测元素受标准样品限制，不易检测标准样品标示值以外的其它元素。
本文提出了一种新的熔融制样方法，解决了金属硅熔融制样问题。
既使用各待测元素标准溶液配制所需的标准熔融样片，又可根据要求同时测定多种元素，且不受固体标准样品测试范围限制，各元素测定准确度满足标准方法［1!3］要求。
1实验部分1.1仪器和测试条件1.1.1仪器德国西门子公司SRS 3000型顺序式X -射线荧光光谱仪，端窗铑靶X -射线管，满功率为3k W ，8位自动进样器。
辉光放电光谱法测定因瓦合金中14种元素刘洁;葛晶晶;孙中华【摘要】After the calibration curve was prepared using 11 certified reference materials of nickel-based alloy with similar content to invar alloy, a method for simultaneous determination of fourteen elements (C, Si, Mn, P, S, Ni, Cr, Mo, Cu, Al, Nb, Ti, Co and Fe) in invar alloy was established by glow discharge optical emission spec-trometry without sample treatment. The optimal conditions of glow discharge spectrometer for the determination of invar alloy were obtained as follows:the module voltage and phase voltage was 8. 22 V and 3. 82 V, respectively;the power was 70 W;the flushing time was 80 s; the integral time was 60 s. The calibration curves were plotted with mass fraction of each element as horizontal ordinate and its corresponding spectral intensity as vertical coordi-nate. The correlation coefficients of calibration curves were all higher than 0. 99. The actual sample of invar alloy was analyzed by the experimental method. The results showed that the mass fraction of Cr,Ni, Mo, Ti, and Fe were all higher than 0. 3% with relative standard deviations (RSD, n=11) all not higher than 1%, the mass frac-tion of C, Si, Mn, P, S, Cu, Al,Nb and Co were all less than 0. 3% with relative standard deviations (RSD, n=11 ) all less than 5%. The proposed method was applied to the determination of fourteen elements in invar alloy samples. The results were basically consistent with those obtained by titration method (Ni and Fe), high frequency combustion-infrared absorption method ( C and S) orinductively coupled plasma atomic emission spectrometry ( Si, Mn, P, Cr, Mo, Cu, Al,Nb,Ti and Co).%采用11种与因瓦合金成分含量相接近的镍基合金标准样品绘制校准曲线,建立了基本不需要样品处理即可对因瓦合金中14种元素( C、Si、Mn、P、S、Ni、Cr、Mo、Cu、Al、Nb、Ti、Co、Fe)同时测定的辉光放电光谱法。
