CN108627483B - 区分稀土La3+、Gd3+和Tb3+的方法 - Google Patents
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Abstract
一种区分稀土La3+、Gd3+和Tb3+的方法,其技术要点是,包括以下步骤:步骤1,配制标准溶液;步骤2,配制稀土溶液;步骤3,荧光光谱仪扫描;步骤4,比对扫描结果。其具有灵敏度高、样品用量少、检测成本低、操作简单快捷等优点。
Description
技术领域
本发明涉及化学分析领域,具体说是一种区分稀土La3+、Gd3+和Tb3+的方法。
背景技术
现有技术中,在对稀土成分检测时,通常需要借助多种试剂及仪器对各元素进行有效区分,如申请公布号为CN105784683A的发明专利申请公开的“二氧化钍中稀土元素含量的测定方法”,该技术方案涉及建立新的化学检测方法,具体涉及到采用等离子体发射光谱法测定二氧化钍粉末及芯块15种稀土元素含量的方法。样品溶解:二氧化钍溶解时加入0.2%~0.5%的氢氟酸溶液并且控制在0.1mL以内;钍与稀土元素的分离:采用在3mol/L的硝酸介质下用,四氯化碳:磷酸三丁脂=1:1萃取剂萃取三次进行钍与稀土元素的分离;进行样品的测定。目前,尚缺乏一种检测过程简单、操作简便、检测精度高的区分方法。
发明内容
本发明的目的是提供一种区分稀土La3+、Gd3+和Tb3+的方法,从根本上解决了上述问题,其具有灵敏度高、样品用量少、检测成本低、操作简单快捷等优点。
为实现上述目的,本发明提供了如下技术方案:该区分稀土La3+、Gd3+和Tb3+的方法,其技术要点是,包括以下步骤:
步骤1,配制标准溶液:
步骤101,配制TCPP溶液:准确称取TCPP固体粉末,加入DMSO溶解,用去离子水稀释,定容至50mL,得到0.02mol/L的DMSO溶液;取0.02mol/L的DMSO溶液1mL,用去离子水稀释,定容至100mL,得到2×10-4mol/L的TCPP溶液;
步骤102,配制OVA溶液:准确称取OVA固体,加去离子水溶解,定容至100mL,得到2.93g/L的OVA溶液;
步骤103,配制HEPES缓冲溶液:称取HEPES固体粉末,用去离子水溶解,用盐酸和氢氧化钠调节溶液的pH值为7.0,定容至100mL,得到0.01mol/L的HEPES溶液;
步骤104,取步骤101配制的2×10-4mol/L TCPP溶液,取步骤102配制的2.93g/LOVA溶液,取步骤103配制的0.01mol/L HEPES缓冲溶液,按照体积比1:1:6加入到荧光杯中;
步骤2,配制稀土溶液:
步骤201,配制La3+溶液:准确称取六水合硝酸镧,用去离子水溶解,定容至50mL,得到5×10-3mol/L的La3+溶液;
步骤202,配制Gd3+溶液:准确称取六水合硝酸钆,用去离子水溶解,定容至50mL,得到5×10-3mol/L的Gd3+溶液;
步骤203,配制Tb3+溶液:准确称取氧化铽,加入适量稀盐酸溶解后,用去离子水定容至50mL,得到5×10-3mol/L的Tb3+溶液;
步骤3,荧光光谱仪扫描:
步骤301,设定扫描条件:激发310nm,范围400nm~700nm,激发和发射狭缝分别10,20;电压150V,记录扫描结果;
步骤302,设定与步骤301相同的扫描条件:在步骤1的荧光杯中加入步骤201配制的5×10-3mol/L La3+溶液100uL,记录扫描结果;
步骤303,设定与步骤301相同的扫描条件:在步骤1的荧光杯中加入步骤202配制的5×10-3mol/L Gd3+溶液100uL,记录扫描结果;
步骤304,设定与步骤301相同的扫描条件:在步骤1的荧光杯中加入步骤203配制的5×10-3mol/L Tb3+溶液100uL,记录扫描结果;
步骤4,比对扫描结果:
将步骤301至步骤304的扫描结果进行比较,分别在660nm、665nm、669nm、667nm得到最大发射峰,且Tb3+离子在667nm出现的发射峰相对于La3+离子、Gd +离子更宽。
本发明的有益效果:基于荧光发射光谱建立了区分稀土La3+、Gd3+和Tb3+离子的方法,敏化了稀土离子的荧光。
目前,常用的区分稀土离子的方法是化学合成的方法合成配体,再与稀土离子作用形成配合物。步骤繁琐,费时费力,实验条件不好控制,操作起来很不方便。还可以通过电感耦合等离子体原子发射光谱对稀土离子进行定性分析,但此方法仪器昂贵,对样品的要求高。
本发明选择的卵清蛋白(VOA),价格低廉,稳定性好,对稀土离子荧光的敏化程度强,可直接与TCPP作用对三种稀土离子La3+、Gd3+和Tb3+进行区分。减少了实验步骤,节省实验时间,使实验更易与操作。
本发明可直接使用普通的荧光光谱仪进行检测,仪器价格低廉,测量步骤简单,对样品的要求低,直接配制成溶液就可以对三种稀土离子进行定性分析。
附图说明
图1为本发明的主视结构示意图。
具体实施方式
以下通过具体实施例详细说明本发明的内容。该区分稀土La3+、Gd3+和Tb3+的方法包括以下步骤:
步骤1,配制标准溶液:
步骤101,配制TCPP溶液:准确称取0.7908gTCPP固体粉末,加入少量DMSO溶解,用去离子水稀释,定容至50mL,即得0.02mol/L的DMSO溶液;
取0.02mol/L溶液1mL,用去离子水稀释,定容至100mL,即得2×10-4mol/L的TCPP溶液;
步骤102,配制OVA溶液:准确称取0.2929g OVA固体,加去离子水溶解,定容至100mL,即得2.93g/L的OVA溶液;
步骤103,配制HEPES缓冲溶液:称取0.2383gHEPES固体粉末,用去离子水溶解,用盐酸和氢氧化钠调节溶液的pH值为7.0,定容至100mL,即得0.01mol/L的HEPES溶液;
步骤104,取步骤103配制的0.01mol/L HEPES缓冲溶液1200uL,取步骤101配制的2×10-4mol/L TCPP溶液200uL,取步骤102配制的2.93g/L OVA溶液200uL加入到荧光杯中;
步骤2,配制稀土溶液:
步骤201,配制La3+溶液:准确称取六水合硝酸镧0.1082g,用去离子水溶解,定容至50mL,即得5×10-3mol/L的La3+溶液;
步骤202,配制Gd3+溶液:准确称取六水合硝酸钆0.1128g,用去离子水溶解,定容至50mL,即得5×10-3mol/L的Gd3+溶液;
步骤203,配制Tb3+溶液:准确称取0.0915g氧化铽,加入适量的稀盐酸溶解后用去离子水定容至50mL,即得5×10-3mol/L的Tb3+溶液;
步骤3,荧光光谱仪扫描:
步骤301,设定扫描条件:激发310nm,范围400nm~700nm,激发和发射狭缝分别10,20;电压150V,记录扫描结果,如图1实线所示,在660nm出现最大发射峰;
步骤302,设定与步骤301相同的扫描条件:在步骤1的荧光杯中加入步骤201配制的5×10-3mol/L La3+溶液100uL,记录扫描结果,如图1长虚线所示,在665nm出现最大发射峰;
步骤303,设定与步骤301相同的扫描条件:在步骤1的荧光杯中加入步骤202配制的5×10-3mol/L Gd3+溶液100uL,记录扫描结果,如图1点划线所示,在669nm出现最大发射峰;
步骤304,设定与步骤301相同的扫描条件:在步骤1的荧光杯中加入步骤203配制的5×10-3mol/L Tb3+溶液100uL,记录扫描结果,如图1断虚线所示,在667nm出现最大发射峰;
步骤4,比对扫描结果:
将步骤301至步骤304的扫描结果进行比较,分别在660nm、665nm、669nm、667nm得到最大发射峰,且Tb3+离子在667nm出现的发射峰相对于La3+离子、Gd +离子更宽。
Claims (1)
1.一种区分稀土La3+、Gd3+和Tb3+的方法,其特征在于,包括以下步骤:
步骤1,配制标准溶液:
步骤101,配制TCPP溶液:准确称取TCPP固体粉末,加入DMSO溶解,用去离子水稀释,定容至50mL,得到0.02mol/L的DMSO溶液;取0.02mol/L的DMSO溶液1mL,用去离子水稀释,定容至100mL,得到2×10-4mol/L的TCPP溶液;
步骤102,配制OVA溶液:准确称取OVA固体,加去离子水溶解,定容至100mL,得到2.93g/L的OVA溶液;
步骤103,配制HEPES缓冲溶液:称取HEPES固体粉末,用去离子水溶解,用盐酸和氢氧化钠调节溶液的pH值为7.0,定容至100mL,得到0.01mol/L的HEPES溶液;
步骤104,取步骤101配制的2×10-4mol/L TCPP溶液,取步骤102配制的2.93g/L OVA溶液,取步骤103配制的0.01mol/L HEPES缓冲溶液,按照体积比1:1:6加入到荧光杯中;
步骤2,配制稀土溶液:
步骤201,配制La3+溶液:准确称取六水合硝酸镧,用去离子水溶解,定容至50mL,得到5×10-3mol/L的La3+溶液;
步骤202,配制Gd3+溶液:准确称取六水合硝酸钆,用去离子水溶解,定容至50mL,得到5×10-3mol/L的Gd3+溶液;
步骤203,配制Tb3+溶液:准确称取氧化铽,加入适量稀盐酸溶解后,用去离子水定容至50mL,得到5×10-3mol/L的Tb3+溶液;
步骤3,荧光光谱仪扫描:
步骤301,设定扫描条件:激发310nm,范围400nm~700nm,激发和发射狭缝分别10,20;电压150V,记录扫描结果;
步骤302,设定与步骤301相同的扫描条件:在步骤1的荧光杯中加入步骤201配制的5×10-3mol/L La3+溶液100uL,记录扫描结果;
步骤303,设定与步骤301相同的扫描条件:在步骤1的荧光杯中加入步骤202配制的5×10-3mol/L Gd3+溶液100uL,记录扫描结果;
步骤304,设定与步骤301相同的扫描条件:在步骤1的荧光杯中加入步骤203配制的5×10-3mol/L Tb3+溶液100uL,记录扫描结果;
步骤4,比对扫描结果:
将步骤301至步骤304的扫描结果进行比较,分别在660nm、665nm、669nm、667nm得到最大发射峰,且Tb3+离子在667nm出现的发射峰相对于La3+离子、Gd +离子更宽;
TCPP为5,10,15,20-四(4-羧基苯基)卟啉;DMSO为二甲基亚砜;OVA为鸡卵清白蛋白;HEPES为羟乙基哌嗪乙磺酸;Tb2O3为氧化铽。
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CN103575900A (zh) * | 2012-07-23 | 2014-02-12 | 苏州长光华医生物试剂有限公司 | 一种检测erbb2蛋白的试剂盒及其制备方法 |
CN105784683A (zh) * | 2014-12-26 | 2016-07-20 | 中核北方核燃料元件有限公司 | 二氧化钍中稀土元素含量的测定方法 |
CN107421930A (zh) * | 2017-07-14 | 2017-12-01 | 信阳师范学院 | 一种采用荧光光谱法研究稀土金属La3+与BSA的相互作用的方法 |
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