ICP-AES法测定铸铝合金全元素的溶样优化与准确度验证OA
Optimization of Sample Dissolution and Accuracy Verification for Multi-Element Determination in Cast Aluminum Alloy by ICP-AES
针对铸铝合金(低硅 Si<0.50%、高硅 Si:4.0%~10.0%)全元素精准分析的需求,聚焦高硅体系溶样难题与多元素检测干扰控制,通过系统优化前处理条件、仪器参数及干扰消除方法,建立了高效可靠的 ICP-AES 分析技术.实验明确两类合金最优方案:低硅铸铝合金以 0.10 g 为称样量,采用 15 mL(6 mol/L)盐酸在 70℃溶解;高硅铸铝合金以 0.05 g为称样量,通过 5 mL 体积分数 50%硝酸与 1 mL 氢氟酸混合体系实现完全溶解,有效规避硅元素损失与胶体膜生成问题.通过基体匹配校准抵消铝基体效应,优化分析线选择与酸度控制消除光谱及化学干扰,构建的校准曲线对 Si、Fe、Cu、Mn、Ti、Zr、Ni、Sb、Co、Mg、Pb、Sn、Zn、Be 等14种目标元素的线性相关系数 R2≥0.995,检出限低至 0.001~0.012 mg/L.准确度验证显示,低硅与高硅铸铝合金标准样品的测定值与标准值高度吻合,相对标准偏差(RSD)分别介于 0.197%~3.26%和 0.19%~4.87%之间.方法简化了前处理流程,突破了高硅铸铝合金全元素同步检测的技术瓶颈,兼顾准确性与实用性,为铸铝合金质量控制及成分溯源提供了全面的技术支撑.
To address the need for accurate full-element analysis of cast aluminum alloys,including low-silicon(Si<0.50%)and high-silicon(4.0%~10.0%Si)systems,this study focused on overcoming sample dissolution challenges in high-silicon alloys and minimizing multi-element interference during detection.An efficient and reliable ICP-AES method was developed through systematic optimization of sample pretreatment procedures,instrumental parameters,and interference control strategies.Experimental optimization established the following protocols:for low-silicon cast aluminum alloys,0.10 g of sample was dissolved in 15 mL of 6 mol/L hydrochloric acid at 70℃;for high-silicon cast aluminum alloys,0.05 g of sample was completely dissolved using a mixed acid system consisting of 5 mL of volume fraction 50%nitric acid and 1 mL of hydrofluoric acid.This approach effectively prevented silicon loss and avoided colloidal film formation.Matrix effects from the aluminum base were compensated using matrix-matched calibration,while spectral and chemical interferences were minimized through optimized analytical line selection and acidity control.The calibration curves for 14 target elements(Si,Fe,Cu,Mn,Ti,Zr,Ni,Sb,Co,Mg,Pb,Sn,Zn,and Be)demonstrated excellent linearity(R2≥0.995),with limits of detection ranging from 0.001 to 0.012 mg/L.Accuracy validation showed strong agreement between measured and certified values for both low-and high-silicon reference materials;the relative standard deviations ranged from 0.197%to 3.26%and 0.19%to 4.87%,respectively.The proposed method simplifies sample pretreatment,overcomes key technical challenges in simultaneous full-element determination of high-silicon cast aluminum alloys,and achieves s balance between analytical accuracy and practical applicability.It provides robust technical support for quality control and compositional traceability of cast aluminum alloys.
张亮亮;袁琪;李娅娟;谢培均
中航金属材料理化检测科技有限公司,陕西 西安 710000中航金属材料理化检测科技有限公司,陕西 西安 710000西部超导材料科技股份有限公司,陕西 西安 710000中航金属材料理化检测科技有限公司,贵州 安顺 561000
化学化工
铸铝合金ICP-AES全元素检测溶样优化基体匹配准确度验证
cast aluminum alloyICP-AESfull-element detectionsample dissolution optimizationmatrix-matched calibrationaccuracy validation
《化学试剂》 2026 (4)
63-69,7
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