CN105486651A - 一种铅基合金中镧的化学分析方法 - Google Patents
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- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 claims description 7
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- LMBWSYZSUOEYSN-UHFFFAOYSA-N diethyldithiocarbamic acid Chemical compound CCN(CC)C(S)=S LMBWSYZSUOEYSN-UHFFFAOYSA-N 0.000 abstract 2
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- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
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Abstract
本发明提供一种铅基合金中镧元素的化学分析方法,将含镧铅基合金、不含镧的铅基合金、镧标样分别经混酸溶解处理后,沉淀过滤;然后加入高氯酸,调PH,分别制备待测原液、参比溶液、镧标准液,然后配置标准溶液,绘制标准曲线,计算溶液浓度,计算镧元素含量。本发明用紫外-可见分光光度法测铅基合金中的元素含量;用不含镧相同条件下的铅基合金处理后做参比溶液;沉淀铅所选用试剂为铜试剂;加入高氯酸加热滤液至高氯酸冒烟,是为了破坏铜试剂及驱赶硝酸,比色样品中加入冰乙酸作用缓冲试剂,用来调节PH,避免引入其他酸而干扰。与现有技术相比:本发明具有操作简单方便,测试成本最低,测试精度高,测试结果可靠、准确等优点。
Description
技术领域
本发明涉及一种化学分析方法,具体为一种可用于紫外-可见分光光度计铅基合金中镧的化学测试方法。
背景技术
常规铅基合金中镧元素都是采用ICP光谱仪进行测试,测试结果准确可靠,但光谱测试样品制备时间较长,对样品制备过程要求较高,价值设备昂贵,较准难度大;而一般的化学分析测试方法主要为紫外-可见分光光度法,目前主要用于钢铁中稀土元素的检测,包括钢铁中镧元素的检测;还有采用荧光光谱中测铝合金中镧元素的含量,由于含镧铅基合金于2015年首次开发应用,目前无紫外-可见分光光度法及荧光光谱来检测铅基合金中镧元素的方法。
发明内容
本发明的目的是为了提供一种可降低试验成本,且测试结果准确的铅基合金中镧元素的化学分析方法。
本发明的技术方案是:将含镧的铅基合金经混酸溶解处理后,加入乙酸溶液;用铜试剂作为铅沉淀试剂将铅沉淀后,过滤收集滤液;然后用高氯酸破坏铜试剂后调节pH为1.5~2.5,全部移入容量瓶内定容摇匀,作为待测原液;用不含镧相同条件下的铅基合金用上述制备待测原液方法处理后做参比溶液;取分析纯氧化镧,用王水低温溶解,定容摇匀配制2.5mg/L镧标准溶液;用镧标准溶液和待测原液分别以冰乙酸为缓冲剂,以偶氮氯膦-mA溶液为显色剂,配置一系列相同体积的标准溶液和待测液作为比色样品;于分光光度计对比色样品的管内溶液进行比色测定,在检测波长为550-660nm时测试吸光值,以标准溶液浓度与吸光值绘制标准曲线,通过曲线以待测液的吸光值计算待测液浓度,再根据待测液浓度计算铅基合金镧元素含量。
本发明所述混酸为王水与高氯酸的体积比为2:1~3:1的混合酸。
本发明所述比色样品浓度小于1mg/L。比色样品中冰乙酸加入量为1-10ml/每50ml待测液。
本发明所述配制待测原液所用含镧的铅基合金的量为0.01~0.5g。
本发明所述配制待测原液具体方法为:称取0.5g含镧铅基合金试样于250ml烧杯中,加入王水30ml低温溶解后,加入高氯酸15ml蒸发至高氯酸冒白烟,反复滴加盐酸至溶液颜色基本褪去,继续冒烟蒸发至近干,然后加入30ml乙酸溶液(乙酸溶液的体积分数为10%),再加入20ml200g/L铜试剂溶液,沉淀以后用快速滤纸干过滤;滤液收集至500ml锥形瓶内,加入5ml高氯酸,加热滤液至高氯酸冒烟,破坏铜试剂,加入少量水溶解盐类,全部转入100ml容量瓶内定容摇匀,制得待测原液;另取一支50ml比色管,移入10ml待测原液,2ml冰乙酸,5ml偶氮氯膦-mA溶液,定容摇匀。
本发明比色测定的最佳显色时间为5-30min。
本发明所述配制参比溶液的方法为:称取0.5g不含镧相同铅基合金,按照上述制备待测原液方法配制参比溶液。
本发明所述配制标准溶液的方法为:称取0.1173克分析纯氧化镧,加入30ml王水溶液,低温溶解,冷却后移入1L容量瓶内,定容摇匀,形成镧浓度为100mg/L的标准贮备液。取2.5ml标准储备液至100ml容量瓶中,定容摇匀,稀释至2.5mg/L。
本发明所述绘制标准曲线的方法为:各移取10ml参比溶液于5支50ml比色管中,分别加入0、1ml、2ml,3ml,4ml镧标准溶液,加入2ml冰乙酸,5ml偶氮氯膦-mA溶液,定容摇匀;于分光光度计上测试吸光度,以吸光度为纵坐标,标准溶液的溶度为横坐标,绘制标准曲线。
本发明测试吸光值的方法为:在721型分管光度计上对6支比色管内溶液进行比色测定:在721分光光度计上设定检测波长660nm测试,记录各支比色管对应的吸光值。
本发明用紫外-可见分光光度法测铅基合金中的元素含量;用不含镧相同条件下的铅基合金处理后做参比溶液;沉淀铅所选用试剂为铜试剂;加入高氯酸加热滤液至高氯酸冒烟,是为了破坏铜试剂及驱赶硝酸,比色样品中加入冰乙酸作用缓冲试剂,用来调节PH,避免引入其他酸而干扰。
与现有技术相比:本发明具有操作简单方便,测试成本最低,测试精度高,测试结果可靠、准确等优点。
附图说明
图1为本发明的流程图。
具体实施方式
图1中,用含镧铅基合金、不含镧的铅基合金、镧标样分别用混酸溶解、沉淀过滤;然后加入高氯酸,调PH,分别制备待测原液、参比溶液、镧标准液,然后配置标准溶液,绘制标准曲线,计算溶液浓度,计算镧元素含量。
称取0.5g含镧铅基合金试样于250ml烧杯中,加入王水30ml低温溶解后,加入高氯酸15ml蒸发至高氯酸冒白烟,反复滴加盐酸至溶液颜色基本褪去,继续冒烟蒸发至近干,取下加入30ml乙酸溶液(乙酸含量为10%),再加入20ml200g/L铜试剂溶液,沉淀以后用快速滤纸干过滤。滤液收集至500ml锥形瓶内,加入5ml高氯酸,加热滤液至高氯酸冒烟,破坏铜试剂,加入少量水溶解盐类,转入100ml容量瓶内定容摇匀。称取0.5g不含镧铅基合金,按照含镧铅基合金方法配制参比溶液。称取0.1173克分析纯氧化镧,加入30ml王水溶液,低温溶解,冷却后移入1L容量瓶内,定容摇匀,形成镧浓度为100mg/L的标准贮备液。取2.5ml标准储备液至100ml容量瓶中,定容摇匀,稀释至2.5mg/L。各移取10ml参比溶液于5支50ml比色管中,分别加入0、1ml、2ml,3ml,4ml镧标准溶液(浓度为2.5mg/L),加入2ml冰乙酸,5ml偶氮氯膦-mA溶液,定容摇匀。另取一支50ml比色管,移入10ml待测液,2ml冰乙酸,5ml偶氮氯膦-mA溶液,定容摇匀。于723型分管光度计上对6支比色管内溶液进行比色测定,显色时间为10min。在720分光光度计上设定检测波长660nm进行测试,记录各支比色管对应的吸光度数值,以标准溶液浓度与吸光值绘制标准曲线,根据曲线推算待测液浓度,进而计算铅基合金含镧量。
Claims (9)
1.一种铅基合金中镧的化学分析方法,其特征在于:将含镧的铅基合金经混酸溶解处理后,加入乙酸溶液;用铜试剂作为铅沉淀试剂将铅沉淀后,过滤收集滤液;然后用高氯酸破坏铜试剂后调节pH为1.5~2.5,全部移入容量瓶内定容摇匀,作为待测原液;用不含镧相同条件下的铅基合金用上述制备待测原液方法处理后做参比溶液;取分析纯氧化镧,用王水低温溶解,定容摇匀配制2.5mg/L镧标准溶液;用镧标准溶液和待测原液分别以冰乙酸为缓冲剂,以偶氮氯膦-mA溶液为显色剂,配置一系列相同体积的标准溶液和待测液作为比色样品;于分光光度计对比色样品的管内溶液进行比色测定,在检测波长设定为550-660nm时测试吸光值,以标准溶液浓度与吸光值绘制标准曲线,通过曲线以待测液的吸光值计算待测液浓度,再根据待测液浓度计算铅基合金镧元素含量。
2.根据权利要求1所述铅基合金中镧的化学分析方法,其特征在于:所述混酸为王水与高氯酸的体积比为2:1~3:1的混合酸。
3.根据权利要求1所述铅基合金中镧的化学分析方法,其特征在于:所述比色样品浓度小于1mg/L;比色样品中冰乙酸加入量为1-10ml/每50ml待测液。
4.根据权利要求1所述铅基合金中镧的化学分析方法,其特征在于:所述配制待测原液所用含镧的铅基合金的量为0.01~0.5g。
5.根据权利要求1所述铅基合金中镧的化学分析方法,其特征在于:所述配制待测原液具体方法为:称取0.5g含镧铅基合金试样于250ml烧杯中,加入王水30ml低温溶解后,加入高氯酸15ml蒸发至高氯酸冒白烟,反复滴加盐酸至溶液颜色基本褪去,继续冒烟蒸发至近干,然后加入30ml乙酸溶液,再加入20ml200g/L铜试剂溶液,沉淀以后用快速滤纸干过滤;滤液收集至500ml锥形瓶内,加入5ml高氯酸,加热滤液至高氯酸冒烟,破坏铜试剂,加入少量水溶解盐类,全部转入100ml容量瓶内定容摇匀,制得待测原液;另取一支50ml比色管,移入10ml待测原液,2ml冰乙酸,5ml偶氮氯膦-mA溶液,定容摇匀。
6.根据权利要求1所述铅基合金中镧的化学分析方法,其特征在于:比色测定的最佳显色时间为5-30min。
7.根据权利要求1所述铅基合金中镧的化学分析方法,其特征在于:所述配制参比溶液的方法为:称取0.5g不含镧相同铅基合金,按照上述制备待测原液方法配制参比溶液。
8.根据权利要求1所述铅基合金中镧的化学分析方法,其特征在于:所述绘制标准曲线的方法为:各移取10ml参比溶液于5支50ml比色管中,分别加入0、1ml、2ml,3ml,4ml镧标准溶液,加入2ml冰乙酸,5ml偶氮氯膦-mA溶液,定容摇匀;于分光光度计上测试吸光度,以吸光度为纵坐标,标准溶液的溶度为横坐标,绘制标准曲线。
9.根据权利要求1所述铅基合金中镧的化学分析方法,其特征在于:测试吸光值的方法为:在721型分管光度计上对6支比色管内溶液进行比色测定:在721分光光度计上设定检测波长660nm测试,记录各支比色管对应的吸光值。
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CN109529778A (zh) * | 2018-08-17 | 2019-03-29 | 南昌航空大学 | 一种可对Ce4+同时快速吸附和定量检测的纳米材料的制备方法 |
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