Determination of Trace Phosphorus in Copper-Containing Stainless Steel by High Resolution Inductively Coupled Plasma Magnetic Massspectrometry
摘 要
作者通过试验,用电感耦合等离子体磁质谱(HR-ICP-MS)测定含铜不锈钢中磷含量时,采用高分辨率模式,选择分辨率为4 000,在此条件下磷峰可与干扰双原子分子或离子的峰分开。又通过以含铁基的磷标准溶液优化了气体流量和离子透镜的参数,使磷的信号值提高至3×105cps。而加入45Sc作为内标元素又可显著提高测定的稳定性。分别用不锈钢样品和纯铁粉作基体,加入标准溶液制作标准曲线。结果表明:两种方法的线性均较好,分别测得实际样品的结果及其相对标准偏差也基本一致。但两种方法的检出限(3s)不同,前者为1.0 μg·g-1,后者为0.18 μg·g-1。所提出方法的样品处理过程如下:称取样品0.10 g置于消解罐中,加入盐酸溶液2 mL及硝酸溶液1 mL,待剧烈反应缓解时,将消解罐加盖并置于微波消解仪中,于100℃消解10 min,升温至200℃继续消解20 min。冷却后将溶液转移至100 mL石英容量瓶中,加入0.2 mg·L-1钪内标溶液1 mL,加水至刻度,摇匀。此溶液在仪器工作条件下进行HR-ICP-MS测定。对含磷51 μg·g-1的含铜不锈钢,按本方法测定所得结果的相对标准偏差(n=10)小于4%。应用本方法分析了7种标准物质或已知样品(包括低合金钢、含铜不锈钢、高温合金),并同时用ICP-AES进行校对分析。结果表明,本方法与ICP-AES的测定结果基本一致。但本方法的结果与标准物质的认定值更接近,而且对低含量磷(9 μg·g-1)也可很好测定。
Abstract
Through testing, modifications were made and a method for determination of trace amount of phosphorus in copper containing stainless steel by high resolution inductively coupled plasma magneto-mass spectrometry (HR-ICP-MS) was proposed in this paper. By using resolution of 4 000, response peak of phosphorus was well-separated from the interfering peaks of several bi-atomic molecules or ion, thus to have the interferences eliminated. A mixed solution containing 1 μg·L-1 of phosphorus and Fe(Ⅲ) as matrix was used in tuning of the instrument to optimize the parameters of gas flow and ionic lens, the signal of phosphorus was raised to 3×105cps. And 45Sc was added as internal standard to overcome the matrix effect and to improve stability of analytical results. Two different ways for preparation of standard curves, i.e. 1 adding standard solutions of phosphorus to a matrix of stainless steel sample, and 2 adding standard solutions of phosphorus to pure iron as matrix, were tested comparatively, and as shown by the results, good linearity was obtained for the standard curves prepared by both of the 2 ways, and the results of phosphorus together with the values of RSD found by either of the 2 curves in analyzing a sample were in satisfactory conformity. However, detection limits (3s) found rom the 2 curves were quite different, giving values of 1.0 μg·g-1 for the former way, and of 0.18 μg·g-1 for the latter. Procedure for pretreatment of sample was given as follows:0.10 g of the sample was reacted with 2 mL of hydrochloric acid and 1 mL of nitric acid in the digestion vessel and when the vigorous reaction subsides, the vessel was capped and placed into the microwave digestor, and the digestion of the sample was carried on for 10 min at 100℃ and for 20 min further at 200℃. After cooling, the solution was transferred to a 100 mL quartz volumetric flask, and after adding 1 mL of 0.2 μg·L-1 scandium internal standard solution, water was added to the mark, and mix thoroughly. This was the sample solution used for HR-ICP-MS analysis under the working condition of the instrument. A Cu-containing stainless steel sample having its P-content of 15 μg·g-1was analyzed by the propose method, giving value of RSDs (n=10) less than 4%. To test for its accuracy, 7 CRMs and known samples (including low alloy steel, copper-containing stainless steel, high temperature alloy and etc) were analyzed by the present method and by ICP-AES simultaneously. It was shown that the results of phosphorus found by the 2 methods were in consistency, but the results given by HR-ICP-MS method were more closer to the certified values of the CRMs; and that the HR-ICP-MS method was more effective in determination of phosphorus in trace amount (9 μg·g-1).
中图分类号 O657.63 DOI 10.11973/lhjy-hx202003014
所属栏目 工作简报
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收稿日期 2019/11/5
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备注朱莉,高级工程师,研究方向为痕量分析方法及相关数理统计技术的应用及研究,zhuli@baosteel.com
引用该论文: ZHU Li,ZHANG Yi,JI Hongling,LIU Xiaoping. Determination of Trace Phosphorus in Copper-Containing Stainless Steel by High Resolution Inductively Coupled Plasma Magnetic Massspectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(3): 332~335
朱莉,张毅,纪红玲,刘小平. 高分辨电感耦合等离子体磁质谱法测定含铜不锈钢中痕量磷[J]. 理化检验-化学分册, 2020, 56(3): 332~335
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参考文献
【1】马涛,杨桂宇,邓美乐,等.含铜钢的研究现状及展望[J].热加工工艺, 2017,46(2):36-39.
【2】陈维青,陈泽明.多重谱线拟合(MSF)扣除光谱干扰法在电感耦合等离子体发射光谱法测定钢铁中磷的应用研究[J].光谱实验室, 2000,17(2):185-189.
【3】朱莉,纪红玲,赵君威.背景扣除光谱干扰-单道扫描电感耦合等离子体原子发射光谱法测定高合金钢中磷[J].冶金分析, 2015,35(10):42-48.
【4】李安,乔军,张国翠.微波消解-ICP-AES测定锰铁中的磷[J].光谱实验室, 2012,29(6):3743-3745.
【5】顾继红,于媛君,王铁,等.合金元素对ICP-AES分析磷的准确度的影响[J].鞍钢技术, 2010(5):32-35.
【6】胡净宇,王海舟电感耦合等离子体质谱法测定高温合金中痕量镉和碲[J].冶金分析, 2010,30(2):8-12.
【7】刘正,张翠敏,氨水络合分离-电感耦合等离子体质谱法测定高温合金中痕量银[J].冶金分析, 2004,24(1):1-4.
【8】刘虎生,邵宏翔.电感耦合等离子体质谱技术与应用[M].北京:化学工业出版社, 2005.
【9】王小如.电感耦合等离子体质谱应用实例[M].北京:化学工业出版社, 2005.
【10】陈玉红,刘正,王海舟.电感耦合等离子体质谱法测定钢铁及合金中痕量磷[J].冶金分析, 2007,27(12):17-20.
【11】李鑫德.铈和钇在钢铁工业中的应用[J].稀土信息, 2000,29(5):14-16.
【2】陈维青,陈泽明.多重谱线拟合(MSF)扣除光谱干扰法在电感耦合等离子体发射光谱法测定钢铁中磷的应用研究[J].光谱实验室, 2000,17(2):185-189.
【3】朱莉,纪红玲,赵君威.背景扣除光谱干扰-单道扫描电感耦合等离子体原子发射光谱法测定高合金钢中磷[J].冶金分析, 2015,35(10):42-48.
【4】李安,乔军,张国翠.微波消解-ICP-AES测定锰铁中的磷[J].光谱实验室, 2012,29(6):3743-3745.
【5】顾继红,于媛君,王铁,等.合金元素对ICP-AES分析磷的准确度的影响[J].鞍钢技术, 2010(5):32-35.
【6】胡净宇,王海舟电感耦合等离子体质谱法测定高温合金中痕量镉和碲[J].冶金分析, 2010,30(2):8-12.
【7】刘正,张翠敏,氨水络合分离-电感耦合等离子体质谱法测定高温合金中痕量银[J].冶金分析, 2004,24(1):1-4.
【8】刘虎生,邵宏翔.电感耦合等离子体质谱技术与应用[M].北京:化学工业出版社, 2005.
【9】王小如.电感耦合等离子体质谱应用实例[M].北京:化学工业出版社, 2005.
【10】陈玉红,刘正,王海舟.电感耦合等离子体质谱法测定钢铁及合金中痕量磷[J].冶金分析, 2007,27(12):17-20.
【11】李鑫德.铈和钇在钢铁工业中的应用[J].稀土信息, 2000,29(5):14-16.
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