四硼酸锂-偏硼酸锂熔融电感耦合等离子体发射光谱法(ICP-AES)测定氮化硅中铁的含量
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沈阳有色金属研究院有限公司, 辽宁 沈阳 110141

作者简介:

迟生威(1998—),男,辽宁丹东人,硕士研究生,助理工程师,主要从事有色金属、合金、贵金属、钢铁等分析检测工作。

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O657.3

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Determination of iron content in silicon nitride by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) with lithium tetraborate-lithium metaborate fusion
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CNMC Shenyang Research Institute of Nonferrous Metals Co.,Ltd., Shenyang 110141 , China

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    摘要:

    本文建立了四硼酸锂- 偏硼酸锂熔融电感耦合等离子体发射光谱法(ICP-AES)测定氮化硅中铁的含量的方法。采用四硼酸锂- 偏硼酸锂混合熔剂对样品进行溶解,考察了称样量、四硼酸锂- 偏硼酸锂混合熔剂用量对铁测定结果的影响。结果表明,铁标准溶液的质量浓度与光谱强度线性良好,相关系数大于0.999;采用基体匹配法绘制校准曲线可消除基体效应的影响,铁的检出限为0.0085mg/L;以标准氮化硅样品JCRM R005为例,测定结果的相对标准偏差为3.12%(n=6),测定值与标准值基本一致;3个氮化硅实际样品中的Fe元素测定的标准偏差在2.80%~3.70%;用该法对氮化硅标准样品进行测定,测定结果在标准值允许范围内。该方法具有快速、准确、灵敏度高等优点,适用于氮化硅中铁元素含量的检测。

    Abstract:

    The paper establishes a method for the determination of iron content in silicon nitride by inductively coupled plasma atomic emission spectrometry (ICP-AES) after fusion with lithium tetraborate-lithium metaborate. Lithium tetraborate-lithium metaborate is used to dissolve the sample, and the effects of the sample weighing amount and the dosage of the lithium tetraborate-lithium metaborate mixed solvent on the determination results of iron are investigated. The results show that there is a good linear relationship between the mass concentration of the iron standard solution and the spectral intensity, and the correlation coefficient is greater than 0.999. Drawing the calibration curve by the matrix matching method can eliminate the influence of the matrix effect, and the detection limit of iron is 0.0085mg/L. Taking the standard silicon nitride sample JCRM R005 as an example, the relative standard deviation (RSD) of the determination results is 3.12% (n=6), and the measured value is basically consistent with the standard value. The standard deviation of the Fe element determination in the three actual silicon nitride samples was between 2.80% and 3.70%. When this method is used to determine the standard silicon nitride samples, the determination results are within the allowable range of the standard values. The method has the advantages of rapidity, accuracy, high sensitivity, etc., and is suitable for the detection of iron element content in silicon nitride.

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迟生威,佡云,马晓卉,等.四硼酸锂- 偏硼酸锂熔融电感耦合等离子体发射光谱法(ICP-AES)测定氮化硅中铁的含量[J].有色设备,2025,39(6):41-46.

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  • 收稿日期:2025-06-25
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  • 在线发布日期: 2026-02-13
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