CN113702277A - 一种新型快速测定金属腐蚀速率的方法 - Google Patents
一种新型快速测定金属腐蚀速率的方法 Download PDFInfo
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Abstract
本发明属于金属腐蚀的腐蚀速率测定领域,具体为一种新型快速测定金属材料腐蚀速率的方法,主要应用于各种金属材料腐蚀速率的测定。主要技术方案为按照各类不同被测金属内所含铁、铬、镍、铜、锌、锰、铝等离子配置不同组合的标准溶液,进行金属离子浓度测定,得到标准曲线,之后取腐蚀环境的腐蚀溶液进行金属离子浓度测定,由标准曲线得到被测离子的浓度,从而得到实际金属的被腐蚀量,由此计算出腐蚀速率。该方法不仅比挂片法的误差小,耗时短,还比电化学方法简单稳定,同时还可以进行腐蚀程度的实时测定。
Description
技术领域
本发明属于金属腐蚀的腐蚀速率测定领域,具体为一种快速测定金属材料腐蚀速率的方法,主要应用于各种金属材料腐蚀速率的测定。
技术背景
各类金属材料在某些情况下均会发生腐蚀。传统的腐蚀速率检测方法有失重法与电化学测定法。
挂片法通过比较腐蚀前后质量差来计算腐蚀速率,但是一方面对于耐腐蚀性能较好的不锈钢,铝合金类金属而言,若腐蚀时间短,会导致腐蚀前后重量改变值的测量误差较大,而若想误差较小,则需要耗费较长的时间:其次,由于腐蚀产物的特殊性,金属在腐蚀过程中可能出现增重、失重甚至重量不变的情况;最后,试样的表面预处理和腐蚀产物的清除也会极大地影响腐蚀速率的准确性。
电化学通过测定极化电阻、阴极塔菲尔斜率、阳极塔菲尔斜率等一系列参数来计算腐蚀速率。但是,一方面电化学测试容易受到外界的干扰,这导致电化学参数的计算结果经常会产生较大的偏差,而且腐蚀时间越长,测得腐蚀速率的偏差也会越大;另一方面,由于实际腐蚀体系十分复杂,锈层自身的氧化还原反应、锈层内不同相间的传质、锈层内相界面电荷迁移等均可影响电化学测量腐蚀速率的准确性。
发明内容
发明的目的:本发明的目的在于基于紫外分光光度法快速测定腐蚀掉的金属重量,从而计算出不锈钢的实际腐蚀速率。
本发明的技术方案:为实现上述发明内容,本发明采用如下技术方案:
第一步:配制标准溶液
配置被测金属所含金属离子的溶液如铁、铬、镍、铜、锌、锰、铝等,然后再配置PH缓冲溶液,以及被测金属所需要的显色剂如EDTA、磺基水杨酸、二苯卡巴肼、二甲酚橙、丁二酮肟、硫氰酸盐、亚铁氰化钾、邻二氮菲、双硫腙等。
第二步:绘制标准曲线
首先,在被测的金属离子的可显色范围内按一定浓度梯度划分成多组。若被测金属含多种金属离子,则将各金属离子各自进行浓度梯度划分,然后将得到的不同浓度的金属离子组分排列组合,随机抽取一定数量的样本。
然后,按照样本浓度配比配置各种离子的混合溶液。之后按照显色原理及其他原因先后加入PH缓冲溶液,显色剂等,等待显色稳定后进行紫外分光光度计检测,随后进行数据处理分析。
直接线性拟合法:根据不同离子的不同峰位的吸光度进行线性拟合,确定拟合曲线的线性回归系数是否合理,同时得到各种离子对应的标准曲线。
化学计量学分析法:存在多种离子峰位接近,难以确定的情况时,进行化学计量学分析,确定线性回归曲线以及回归系数,判断线性规律是否合理。
第三步:取实际腐蚀液
1.挂片法模拟得腐蚀溶液:模拟酸性、碱性或其他腐蚀环境。将用砂纸把表面氧化膜打磨干净的已知面积的被测金属完全浸入模拟腐蚀环境中,适当时间后取一定量腐蚀溶液。
2.实际腐蚀环境得腐蚀溶液:取一定量实际被测金属所在腐蚀环境腐蚀溶液。
第四步:调节显色并进行紫外分光光度法检测
将腐蚀溶液进行pH调节,之后按顺序加入各种显色剂,最终用去离子水定容,放入比色皿内进行紫外分光光度计检测。
第五步:数据处理分析
选取不同峰位的吸光度,依照标准曲线得到相应离子浓度C1、C2、C3等。峰位重合时,采用化学计量学分析数据,得到相应离子浓度C1、C2、C3等。
具体实施方法
实例1:测不锈钢金属腐蚀速率
第一步:配制标准溶液
配置10mg/L二价镍离子溶液,0.9g/mL氨水,500g/L柠檬酸铵溶液,0.05mol/L碘溶液,5g/L丁二酮肟溶液,50g/LNa2-EDTA溶液。配置70mg/L三价铁离子酸性溶液,100g/L磺基水杨酸溶液,0.15mol/L硫酸溶液。配置20mg/L六价铬离子溶液,0.5g/L二苯卡巴肼溶液,40g/L高锰酸钾溶液,20g/L亚硝酸钠溶液,200g/L尿素溶液。
第二步:绘制标准曲线
6个25ml容量瓶内分别加入0,1.0,2.0,3.,4.0,及5.0ml二价镍离子溶液,加水至10mL,加入500g/L柠檬酸铵溶液2mL,碘溶液1mL,加水至20mL,摇匀,加丁二酮肟溶液2mL,摇匀,加入Na2-EDTA溶液2mL,于530nm处测量吸光度,根据镍离子吸光度进行线性拟合,得到镍离子标准曲线。
体系中铁离子可显色浓度范围为0.5mg/L-22.5mg/L,取离子间隔浓度为0.5mg/L,铬离子可显色浓度范围为0.05mg/L-9mg/L,取离子间隔浓度为0.05mg/L。用MATLAB软件编程将两种离子随机排列组合得到8100种不同浓度组合,之后从中随机抽取50组数据。按照50组浓度配比配置两种离子的混合溶液于10mL试管中,随后滴加0.2mL磺基水杨酸溶液,2mL二苯卡巴肼溶液,加水定容至10ml。显色5min后于300nm-800nm测得50条吸光度曲线。此时两峰基本重合,所以利用MATLAB进行化学计量学分析,确定线性回归系数并得到回归曲线。
第三步:取实际腐蚀液
挂片法模拟得腐蚀溶液:模拟酸性腐蚀环境,腐蚀液容量为50mL。将用砂纸把表面的氧化膜打磨干净的已知面积为0.001m2的被测不锈钢片完全浸入酸性腐蚀环境中,10min后取1mL腐蚀溶液。
第四步:调节显色并进行紫外分光光度计检测
取1mL腐蚀溶液三份导入两个试管I、II中,pH调节至中性。
于I号试管内加入500g/L柠檬酸铵溶液2mL,碘溶液1mL,加水至6mL,摇匀,加丁二酮肟溶液2mL,摇匀,加入Na2-EDTA溶液2mL,于530nm处测量吸光度。读取镍离子峰位的吸光度,依照标准曲线得到相应离子浓度CNi。
推算得铁离子与铬离子大概浓度,此时两者浓度均在显色范围内故不需要稀释。
于II号试管内加入1ml硫酸溶液,加水定容至20mL,后滴加高锰酸钾溶液直至紫红色不再退去,放入玻璃珠,煮沸至剩余5mL,冷却后加入0.1mL尿素溶液,随后滴加亚硝酸钠直至高锰酸钾紫红色退去。后滴加0.2mL磺基水杨酸溶液,2mL二苯卡巴肼溶液,加水定容至10ml,显色5min后于300nm-800nm测得吸光度曲线。
第五步:数据处理分析
读取镍离子峰位的吸光度,依照标准曲线得到相应离子浓度CNi。
将测得铁离子与铬离子的吸光度曲线输入编写好的程序后,得到相应离子浓度CFe、CCr。
将CFe、CCR、CNi、0.05L、0.001L、0.001m2、10min输入MATLAB计算程序得到不锈钢材料在酸性环境下的腐蚀速率。
实例2:检测铜铝合金工件腐蚀速率
第一步:配制标准溶液
铜离子溶液10mg/L,铝离子溶液10mg/L,乙酸溶液0.2mol/L,乙酸钠溶液0.2mol/L,0.03%二甲酚橙溶液。
第二步:绘制标准曲线
将铝离子浓度设置在0.05mg/L-2.5mg/L的范围内,离子间隔浓度为0.05mg/L,将铜离子浓度设置在0.005mg/L-0.25mg/L的范围内,离子间隔浓度为0.05mg/L,用MATLAB软件编程将两种离子随机排列组合得到2500种不同浓度组合,之后从中随机抽取50组数据。按照50组浓度配比配置两种离子的混合溶液于10mL试管中,随后滴加1mL乙酸缓冲溶液,1mL0.03%-甲酚橙溶液,加水定容至10ml。显色50min后于300nm-800nm测得50条吸光度曲线。此时两峰基本重合,所以利用MATLAB进行化学计量学分析,确定线性回归系数并得到回归曲线。
第三步:取实际腐蚀液
取工件所在环境的1mL腐蚀溶液。
第四步:调节显色并进行紫外分光光度计检测
取1mL腐蚀溶液三份导入试管中,pH调节至中性。
于试管内加入滴加1mL乙酸缓冲溶液,1mL0.03%二甲酚橙溶液,加水定容至10ml。显色50min后于300nm-800nm测得吸光度曲线。
第五步:数据处理分析
将测得铜离子与铝离子的吸光度曲线输入编写好的程序后,得到相应离子浓度CCu、CAL。
将CCu、CAL、0.05L、0.001L、0.001m2、10min输入MATLAB计算程序得到该工件的腐蚀速率。
Claims (5)
1.一种测金属腐蚀速率的方法,其特征包括如下步骤:
(1)按被测金属内所含金属离子配置相应的溶液,缓冲溶液,以及被测金属所需要的显色剂;
(2)在被测的金属离子的可显色范围内按一定浓度梯度划分成多组。若被测金属含多种金属离子,则将各金属离子各自进行浓度梯度划分,然后将得到的不同浓度的金属离子组分排列组合,随机抽取一定数量的样本;之后按照显色原理及其他原因先后加入缓冲溶液,显色剂等,等待显色稳定后进行紫外分光光度法检测,并进行数据处理分析,确定标准曲线;
(3)取一定量的腐蚀溶液:
(4)将腐蚀溶液进行pH调节,之后按顺序加入各种显色剂,最终用去离子水定容,放入比色皿内进行紫外分光光度计检测;
(5)进行数据处理分析得到相应离子浓度C1、C2、C3等。
2.根据权利要求1所述的一种方法,其特征是被测金属可以是铸铁、碳钢、硅铁、不锈钢、铝合金、镁合金、锰钢、铜合金、锌合金、铅锡合金、钛合金,耐热合金、磁性合金、钾钠合金、以及各种新型合金。
3.根据权利要求1所述的一种方法,其特征是所述显色剂为EDTA、磺基水杨酸、二苯卡巴肼、二甲酚橙、丁二酮肟、硫氰酸盐、亚铁氰化钾、邻二氮菲、双硫腙、氨水、钼酸铵、罗丹明B、铬天青S中的一种或多种显色剂按先后不同比例混合达到测腐蚀速率的方法。
4.根据权利要求1所述的一种方法,其特征是所述一定量的腐蚀溶液包括模拟酸性、碱性以及其他腐蚀环境所得腐蚀溶液或被测金属实际所在腐蚀环境所得腐蚀溶液。
5.根据权利要求1所述的一种方法,其特征是所述数据处理分析包括直接线性拟合或者化学计量学分析。
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