【作者】 王静；

【导师】 于永丽；

【作者基本信息】 东北大学 ， 分析化学， 2008， 硕士

【摘要】 我国是铜产品消费大国,由于铜合金独特的物理性质和加工性能,铜合金材料被广泛应用在国民经济的许多领域,如冶金、电子、交通运输等。因此,实现对铜合金的快速、准确分析具有十分重要意义。等离子体原子发射光谱(ICP-AES)检测技术具有精密度好、灵敏度高、线性范围宽及多元素同时测定等优点,在元素分析领域被广泛应用。本实验将离子交换分离法与ICP-AES检测方法结合,进行铜合金中微(痕)量磷的分析测定。由于铜对磷存在严重的光谱干扰,所以在基体铜存在的情况下,ICP-AES测定微(痕)量磷不能进行,必须首先进行铜磷的分离。实验采用强酸性阳离子交换树脂分离铜磷,确定了交换分离的最佳条件：选用25 mL交换柱,当上柱溶液中铜的质量为800.0mg,上柱溶液体积为20mL,上柱溶液酸度≤0.5%,溶液流速为1.0 mL/min,淋洗液体积为30mL。用ICP-AES法测定磷,根据谱线强度大、信背比高的原则确定了磷的最佳分析波长为213.617 nm。用干扰系数法校正铜对磷的光谱干扰,当铜的浓度为0.50-50.00mg/L,cCu/Cp≤20时,磷的测定误差≤5.0%。确定了背景校正方式为右校正,上机溶液适宜的酸度为5%。对铜合金中常见的12种元素对磷测定的干扰进行了研究,在考察的浓度范围内,共存元素不干扰磷的测定。应用阳离子交换分离-ICP-AES测定铜合金标准样品中微(痕)量磷,测定结果为0.0030～0.024%,实验的相对标准偏差为0.2～4.7%,相对误差为2.5～9.1%,表明该分析方法的精密度和准确度均较好。更多还原

【Abstract】 Because of the unique physical and processing property, copper products are demanded greatly in our country and the products are used wildly in many national economic fields, such as metallurgy, electronic industry, transportation and others. Therefore the determination of the elements in copper alloy accurately and fast is very important.The advantages of inductive coupled plasma-atomic emission spectrometry (ICP-AES) are good precision, high sensitivity, wide linear range and multi-element simultaneous determination, and then it is applied extensively in the analysis of elements. In our experiment combining ion-exchange separation with ICP-AES determination of minim (trace) amount phosphorus in copper alloy is carried out.Because of serious spectrum interference of copper to phosphorus, the minim (trace) amount phosphorus could not be measured directly by ICP-AES. It is necessary to separate copper and phosphorus before determination when there is a great amount of matrix in copper alloy. In the experiment the separation was completed by strong acidic cation exchange resin and the best separation conditions are as follows:when exchange column was 25mL and the mass of copper was 800.0mg, volume of sample solution was 20mL, acidity was below 0.5%, flowing rate was 1.0mL/min, and volume of washing solution was 30mL.In order to determine phosphorus by ICP-AES, the best analysis wavelength was chosen 213.617nm according to high spectrum intensity and high SBR value. When the concentration of copper was between 0.50～50.00mg/L and Ccu/cp was below 20, IEC method was used to calibrate the spectrum interference of copper to phosphorus and the determination error was below 5.0%. In this work, right correction was selected as the best background correction and the proper acidity of solution was 5%. The interference from 12 elements was studied which are common elements in copper alloy, and the results showed that no interference exist when the concentration of the elements are in the range as the experiment.Using the method of cation exchange-ICP-AES to analyze minim (trace) amount phosphorus in copper alloy standard samples mass percent of phosphorus are 0.0030～0.024%, RSD are 0.2%～4.7%, and RE are 2.5%～9.1%, which proves that the method is precise and accurate.更多还原