电感耦合等离子体原子发射光谱基体匹配校准法测定镍基合金中铬含量  

Determination of Chromium Content in Nickel Base Alloy by Matrix Matching Calibration Method of Inductively Coupled Plasma Atomic Emission Spectrometry

作　　者：刘洁 谭胜楠 戚振南 任玲玲 葛晶晶 孙中华 LIU Jie;TAN Sheng-nan;QI Zhen-nan;REN Ling-ling;GE Jing-jing;SUN Zhong-hua(Hebei HBIS Material Technology Research Institute Co.,Ltd.,Shijiazhuang 050000,China)

机构地区：[1]河北河钢材料技术研究院有限公司,河北石家庄050000

出　　处：《光谱学与光谱分析》2024年第8期2250-2255,共6页Spectroscopy and Spectral Analysis

基　　金：国家自然科学基金项目(51671076);重大科技成果转化专项(22281007Z)资助。

摘　　要：铬元素在镍基合金中具有多重作用,对增加合金涂层耐磨性具有突出贡献,同时,铬能在高温燃气作用下生成致密的氧化保护膜,显著提高合金抗高温氧化和热疲劳性能。在高铬含量的情况下,铬容易与合金中的钛、铝、钼等元素形成有害相而降低合金的强度。对镍基合金中铬元素的准确定值非常关键。镍基合金样品使用氢氟酸、盐酸、硝酸经过微波消解后,采用基体匹配,配制校准溶液测定镍基合金中铬元素在分析谱线的净强度从而计算得出含量。针对镍基合金中镍、钼、铁等高含量元素对铬含量测定有干扰,选择干扰元素少、灵敏度适中的266.602 nm为分析谱线,系统考察了基体效应和共存元素的干扰效应,采用配制校准溶液时,将含量大于5%的元素均进行等同含量的匹配,配制铬元素低标校准溶液Kl Cr,配制铬元素高标校准溶液Kh Cr,制备样品溶液KS Cr,利用电感耦合等离子体原子发射光谱仪,依次测定低标校准溶液Kl Cr、样品溶液KS Cr、高标校准溶液Kh Cr在分析谱线的净强度,按照公式计算得出铬含量。利用标准参考物质评价了方法的准确性,采用YS/T 539.4—2009进行对比分析验证了方法的可靠性。结果表明,方法的检出限(LOD)和定量限(LOQ)分别为0.05和0.10μg·mL^(-1),测定结果的相对标准偏差(RSD)不大于2.5%,标准参考物质的测定值与认定值对比分析结果的相对误差(RE)小于2.5%。该方法操作方便、检测准确,拓宽了ICP-OES光谱法测定镍基合金中铬元素含量的检测范围,检测下限由2%降为0.1%,检测范围上限由30%升为33.5%,大大提高了镍基合金中铬元素含量检测的效率和准确度,适用于各种牌号的镍基合金中铬元素含量的测定。Chromium has multiple roles in nickel-based alloy and has outstanding contributions to increasing the wear resistance of alloy coating.At the same time,chromium can form a dense oxidation protective film under the action of high-temperature gas,which significantly improves the alloy's resistance to high-temperature oxidation and thermal fatigue performance.However,in the case of high chromium content,chromium easily forms harmful phases with titanium,aluminum,molybdenum,and other elements in the alloy and reduces its strength.So,the quasi-determined value of chromium in nickel-base alloy is very important.Nickel base alloy samples are digested by microwave digestion using hydrofluoric acid,hydrochloric acid,and nitric acid.The matrix is matched by inductively coupled plasma atomic emission spectrometry,and the calibration solution is prepared to determine-chromium's net strength in the nickel-base alloy's analysis spectrum line to calculate the content.Given the interference of high-content elements such as Ni,Mo,and Fe in nickel-base alloys on the determination of Cr content,266.602 nm with fewer interference elements and moderate sensitivity was selected as the analytical spectral line;the matrix effect and the interference effect of coexisting elements were systematically investigated.When preparing the calibration solution,the elements with content greater than 5%were matched with the same content.Prepare the low standard calibration solution Kl Crfor the chromium element,prepare the high standard calibration solution Kh Crfor the chromium element,prepare the sample solution KS Cr,and use the ICP-OES spectrometer to determine the net strength of the low standard calibration solution Kl Cr,the sample solution KS Cr,and the high standard calibration solution Kh Cron the analytical spectrum line in turn,and calculate the chromium content according to the formula.The method's accuracy was evaluated using standard reference materials,and the reliability of the method was verified by comparative analysis using the

关 键 词：电感耦合等离子体原子发射光谱 基体匹配 校准法 镍基合金 铬 

分 类 号：O657.33[理学—分析化学]