Simultaneous Determination of Silicon, Aluminum, Titanium and Manganese in Ferroniobium by Inductively Coupled Plasma-Atomic Emission Spectrometry

Jing-nan QI; Li YANG; Jian-dong LI

doi:10.13718/j.cnki.xdzk.2017.01.018

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Ferroniobium samples dissolved by HNO₃ and HF at room temperature were examined, and the matrix matching method was used to eliminate interference of coexisting elements. The stability was enhanced by adding yttrium as the internal standard. In addition, such parameters as RF power, atomized air flow and auxiliary air flow for the inductively coupled plasma spectrometer were investigated, and the optimum analysis parameters for the instruments were determined. An editing analysis program of the ICP analysis software was used to realize automatic drawing of the working curves and the calculation of the data. The results of an experiment showed that this method is simple, fast and accurate and, therefore, is recommended for application in determining silicon, aluminum, titanium or manganese in ferroniobium.

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近年来，铌铁的应用领域不断拓展，冶金行业主要用来冶炼含铌钢.在高温钢和工具钢中，铌的加入可以提高钢的热强度性、抗蠕变性和韧性.在铁素体不锈钢中，加入铌可以改善钢的焊接性能和抗蚀性能等.铌铁中硅、铝、钛、锰元素的含量对铌铁的性质也很重要.然而，硅的检测方法不多，国家标准采用重量法^[1]，但对质量分数小于1.0%的硅不能测定.文献报导的方法大多用分光光度法，铝和钛也多用光度法与滴定法测定^[2-4]，这些方法都存在操作步骤繁琐和周期长的缺点；也有应用ICP-AES光谱法测定硅、铝等多元素的分析方法^[5-21]，但用硫酸高温冒烟处理样品技术，易造成硅损失，使测定结果偏低.本研究通过大量的试验，采用硝酸、氢氟酸和过氧化氢在常温下溶解样品，找出酸的最佳比例；建立了电感耦合等离子体光谱法同时测定铌铁中硅、铝、钛、锰的质量分数的分析方法，试验结果表明方法准确可靠.

1. 试验部分

1.1. 试剂及标准储备溶液

硝酸(ρ约1.42 g/mL)；氢氟酸(ρ约1.15 g/mL).硝酸(唐山市迁乔科技有限公司)、氢氟酸(宜春金浩科技有限公司)均为优级纯.

标准储备溶液包括：硅标准溶液(500 μg/mL)；铝标准溶液(1 000 μg/mL)；锰标准溶液(1 000 μg/mL)；钛标准溶液(1 000 μg/mL).这些标准溶液均购自北京钢研纳克公司.

1.2. 仪器及工作条件

OPERTIMA-4300DV型电感耦合等离子体发射光谱仪(美国PE公司)，雾化器为耐氢氟酸的雾化器，工作参数为辅助气流量0.2 L/min；雾化气流量0.8 L/min；等离子气流量15 L/min；RF功率1 300 W.

1.3. 分析方法

称0.100 0 g试样于200 mL塑料烧杯中，加10 mL HNO₃(1+1)，分次滴加5 mL HF，边滴边摇，加5滴过氧化氢助溶；待样品溶解完全时，移入100 mL塑料容量瓶中，加入10 μg钇，用水稀释至刻度，混匀.

1.4. 校准曲线的绘制

在5个塑料容量瓶加入相同的铌质量分数为60.0%(高纯铌)和铁质量分数为40.0%(基准纯铁)的溶液，按表 1加入待测元素标准溶液及10 μg钇(北京钢研纳克公司)，用水稀释至刻度，混匀.

将校准溶液与试样溶液在ICP光谱仪上测定，绘制工作曲线，通过软件程序计算样品结果.

3. 样品分析

3.1. 精密度试验

选取某一铌铁试样，按试验方法进行10次测定，精密度结果见表 3.

3.2. 准确度试验

对铌铁GSB03-2202-2008(钢铁研究总院)和铌铁EURO-CRM579-1(英国BAS)两个参考样品进行准确度试验，测定结果见表 4.

3.3. 回收率试验

对铌铁样品进行了铝、钛、锰、硅元素回收率的试验，测定结果见表 5.

4. 结语

通过精密度试验可看到，硅、铝、锰、钛元素的相对标准偏差均小于2.5%，方法的回收率在98%~102%之间；选择2个标准样品进行了准确度试验，其测得值与标准值之间的偏差能满足分析方法的要求.综上所述，通过使用适当比例的硝酸、氢氟酸和过氧化氢实现了室温下溶解样品；采用内标法和基体匹配法提高了方法的精密度和准确度，实现了电感耦合等离子体发射光谱法同时测定铌铁中硅、铝、锰、钛元素的目的，试验表明，方法准确、可靠，结果令人满意.

Figure (4) Table (5) Reference (21)

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Simultaneous Determination of Silicon, Aluminum, Titanium and Manganese in Ferroniobium by Inductively Coupled Plasma-Atomic Emission Spectrometry

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Simultaneous Determination of Silicon, Aluminum, Titanium and Manganese in Ferroniobium by Inductively Coupled Plasma-Atomic Emission Spectrometry