CN107525776A - 一种原子光谱仪样品进样的方法和装置 - Google Patents
一种原子光谱仪样品进样的方法和装置 Download PDFInfo
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- 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
- G01N21/3103—Atomic absorption analysis
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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Abstract
本发明公开了一种原子光谱仪样品进样的方法和装置,它是将含胺基的二硫代甲酸(盐)的溶液与待测元素溶液在线混合,混合后的溶液立即进行气液分离测定,使挥发性元素络合物进入到元素分析仪进行检测或用于元素的化学气相沉积膜的制备。本发明可用于仪器分析中的元素样品引入,以提高元素分析的灵敏度、改善检出限;也可用于化学气相沉积及无机镀膜的气态先驱物的制备。
Description
技术领域
本发明属于仪器分析技术领域,涉及一种原子光谱仪样品进样的方法和装置。
背景技术
目前,原子光谱仪中所使用的氢化物发生进样***,大部分是使用硼氢化钠(钾)作氢化物发生的还原试剂,通过硼氢化钠(钾)中的氢将样品溶液中的元素还原成气态氢化物后,元素在原子光谱仪中进行测定。由于氢化物进样效率比较原子光谱中的常规气动雾化进样,有更高的进样效率(常规气动雾化进样只有3-5%,测定灵敏度较低,而氢化物进样效率接近100%),因而在测定上具有更高的灵敏度和更低的检出限的特点。已经应用的是用硼氢化钠(钾)和传统上易形成氢化物的九个元素( 砷,锑,铋,锗,锡,铅,硒,碲,汞)形成这些元素的氢化物而被原子光谱仪进行测定。
近年来,随着科技人员研究的不断深入,一些从事分析的工作人员,相继发现,有关其它元素也可和硼氢化钠(钾)发生氢化反应,并先后发表了多篇研究论文。例如郭小伟等于1995年发现了在常温下酸性水溶液中的锌和镉可以被硼氢化钠溶液还原成可挥发性氢化物,并且运用该氢化发生样品进入***,在原子荧光上测定了实际样品中的锌和镉的含量测定。Aderval.SLuna和P.Pohl分别在下2000年和2001年报到了一些元素如金,银,铜,锰,钛等在常温下也可以和硼氢化钠(钾)反应形成氢化物。但上述文献报道的方法,存在形成氢化物效率比较低、残留现象比较严重的缺陷,从而使该方法在实际使用中受到阻碍。
使用硼氢化钠化学蒸气发生另外一个不足是硼氢化钠价格比较贵,而且不稳定。其固体试剂放置时间长了会分解成块状偏硼酸钠,溶液放置时间久了会分解。一般需要现用现配。另外,硼氢化钠做还原剂从测定元素个数上来说,还是有限。比如,用于测锌钴的时候其灵敏度就很低,也不能测稀土。
发明内容
本发明的目的在于克服现有技术的缺点与不足,提供一种全新的原子光谱仪样品进样的方法和装置。
本发明的技术方案如下:
一种原子光谱仪样品进样的方法,其特征在于将含胺基的二硫代甲酸(盐)的溶液与待测元素溶液在线混合,混合后的溶液立即进行气液分离测定,使挥发性元素络合物进入到元素分析仪进行检测或用于元素的化学气相沉积膜的制备。
本发明中的含胺基的二硫代甲酸(盐)为可溶于水的可溶性盐。
本发明中的含胺基的二硫代甲酸(盐)优选为二乙基二硫代氨基甲酸与碱金属、碱土金属及氨形成的盐。其中碱金属为锂、钠、钾;碱土金属为镁和钙,优选二乙基二硫代氨基甲酸与碱金属锂、钠和钾形成的盐,特别优选的是二甲基二硫代氨基甲酸钠(Na-DDTC)
本发明中的待测元素是指部分主族元素、部分过渡元素、贵金属元素和稀土元素。
本发明的特征在于将0.005-35%(w/w)含胺基的二硫代氨基甲酸(盐)的溶液与酸度0.005-10.0 M的待测元素溶液在线混合。
本发明的特征在于含胺基的二硫代甲酸(盐)在与元素溶液混合后的质量浓度是0.005-5%;优选0.01-1%;更加优选0.015-0.5%。
本发明的特征在于在线待混合后的溶液的酸度是0.01-3.0摩尔/升,优选0.02-1M,
更加优选的酸度是0.05-0.6M。
本发明中待测元素指的是不包括碱金属和碱土金属的主族金属元素;部分过渡元素;贵金属元素和稀土元素。这些元素包括(但不限于):主族金属元素铟、铊、锡、铅、铋;过渡元素钛、铬、锰、铁、钴、镍、铜、锌、镉、汞;贵金属元素钌、铑、钯、银、铱、铂、金;稀土元素铈、镨、钕、钷、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥、铀、钍和钚。
上述元素中优选的元素指的是锡、铅、钌、铑、钯、银、铱、铂、金、钛、铬、锰、铁、钴、镍、铜、锌、镉和汞。
本发明的一个典型实施例包括如下步骤:其包括如下步骤:(1)使用蠕动泵分别以1-5毫升的相等流速连续抽取质量浓度为0.01-0.5%的二乙基二硫代氨基甲酸钠溶液和酸度为0.02-0.3 M的含元素样品溶液;(2)使两股溶液在一微型三通管内汇合反应,然后立即在气液分离器中进行气液分离;(3)分离出的气体被导入原子光谱仪中进行测定。
本发明进一步公开了适用原子光谱仪样品进样的装置;其特征在于该装置包括含元素的样品溶液导入管1、含胺基的二硫代甲酸(盐)溶液的导入管2、蠕动泵3、三通管4、气液分离器5、气液分离器中含多孔玻璃烧结板制成的透气不透水的半透膜,载气入口6、载气出口7和废液排放管8;蠕动泵3抽取两个溶液后通过三通后两股溶液混合,然后与气液分离器5相连,气液分离器设有载气入口6,和载气入口7,分离气体挥发物的废液被蠕动泵经废液排放管8排出。
本发明更进一步公开了原子光谱仪样品进样的方法在用于化学气相沉积及无机镀膜气态先驱物的制备方面的应用。
本发明的第一个典型的原子光谱仪样品进样装置(见说明书附图1),包括含元素的样品溶液导入管、含胺基的二硫代甲酸(盐)溶液的导入管、蠕动泵、三通管、气液分离器(含多孔玻璃烧结板等透气不透水的半透膜)、载气入口、载气出口和废液排放管8;蠕动泵抽取两个溶液后在三通管中汇合发生反应,然后与气液分离器相连,气液分离器设有载气入口,和载气入口,分离气体挥发物的废液被蠕动泵经废液排放管排出。
适用于本发明的第二个典型的原子光谱仪样品进样装置(见说明书附图2),包括含元素的样品溶液导入管1、含胺基的二硫代甲酸(盐)溶液的导入管2、蠕动泵3、三通管4、原子吸收或电感耦合等离子体发射光谱(或质谱)的雾化进样用的雾化器9、原子吸收或电感耦合等离子体发射光谱(或质谱)的用的雾室(旋流雾室或Scott雾室)5、载气入口6、载气出口7和废液排放管8;蠕动泵抽取两个溶液后通过三通后两股溶液混合,然后进入雾化器,雾化器喷雾后进入雾室,气液分离器设有载气入口和载气出口,分离气体挥发物的废液被蠕动泵经废液排放管排出。
附图说明:
图1为适用于原子光谱仪样品进样的装置图;
图2为带有雾化器的适用原子光谱仪样品进样的装置图;
1、元素的样品溶液导入管、2含胺基的二硫代甲酸(盐)溶液导入管
3、蠕动泵 4三通管 5气液分离器、6载气入口、
7载气出口 8、废液排放管 9雾化器。
具体实施方式
为了更充分的解释本发明的实施,提供下述本发明的制备实施实例。这些实施实例仅仅是解释、而不是限制本发明的范围。
实施例1
(1)分别配制含元素金、银的样品溶液(元素含量均为500ppb,硝酸酸度0.3 M)和0.4 %的二乙基二硫代氨基甲酸钠(铜试剂,DDTC)溶液, 然后采用蠕动泵分别以2毫升/分钟的流速抽取上述二个溶液,使两个溶液在一个三通管中汇合后发生反应。
(2)将产生的元素挥发物和反应后的溶液在一气液分离器中分离;
(3)从三通出口管流出的反应液立即流入到一气液分离器中,在这里通过多孔玻璃烧结板鼓泡的方式,分离出的元素挥发物(DDTC和元素的络合物)。该挥发物被导入原子光谱仪原子化或离子化器中进行光谱或质谱测定。所测得的元素灵敏度是同一条件下溶液不含DDTC时的25-40倍。可见测定的灵敏度具有很大的提高。详细图解见说明书附图1.
实施例2
(1)分别配制含元素汞的样品溶液(元素含量为500ppb,硝酸酸度0.10 M)和0.4%的二乙基二硫代氨基甲酸钠(铜试剂,DDTC)溶液, 然后采用蠕动泵分别以1.8毫升/分钟的流速抽取上述二个溶液,使两个溶液在一个三通管中汇合后发生反应。
(2)将产生的元素挥发物和反应后的溶液在一气液分离器中分离;
(3)从三通出口管流出的反应液立即流入到一气液分离器中,在这里通过多孔玻璃烧结板鼓泡的方式,分离出的元素挥发物(DDTC和元素的络合物)。该挥发物被导入原子光谱仪原子化或离子化器中进行光谱或质谱测定。所测得的元素灵敏度是同一条件下溶液不含DDTC时的25-40倍。可见测定的灵敏度具有很大的提高。详细图解见说明书附图1。
实施例 3
一种原子光谱仪样品进样的装置,包括含元素的样品溶液导入管1、含胺基的二硫代甲酸(盐)溶液的导入管2、蠕动泵3、三通管4、气液分离器,其中的气液分离器中含多孔玻璃烧结板制成的透气不透水的半透膜、载气入口、载气出口和废液排放管;蠕动泵抽取两个溶液后在三通管中汇合发生反应,然后与气液分离器相连,气液分离器设有载气入口,和载气入口,分离气体挥发物的废液被蠕动泵经废液排放管排出。
在详细说明的较佳实施例之后,熟悉该项技术人士可清楚地了解,在不脱离上述申请专利范围与精神下可进行各种变化与修改,凡依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰,均属于本发明技术方案的范围。
Claims (10)
1.一种原子光谱仪样品进样的方法,其特征在于它是将含胺基的二硫代甲酸(盐)的溶液与待测元素溶液在线混合,混合后的溶液立即进行气液分离测定,使挥发性元素络合物进入到元素分析仪进行检测或用于元素的化学气相沉积膜的制备。
2.根据权利要求1所述原子光谱仪样品进样的方法,其中含胺基的二硫代甲酸(盐)为可溶性金属盐。
3.根据权利要求1所述原子光谱仪样品进样的方法,其中含胺基的二硫代甲酸(盐)为二乙基二硫代氨基甲酸与碱金属、碱土金属及氨形成的盐;其中碱金属为锂、钠、钾;碱土金属为镁和钙。
4.根据权利要求1所述原子光谱仪样品进样的方法,其中待测元素为部分主族金属元素、部分过渡元素、贵金属元素和稀土元素。
5.根据权利要求1所述的形成方法,其特征在于将0.005-35%(w/w)含胺基的二硫代氨基甲酸(盐)的溶液与酸度0.005-10.0 M的待测元素溶液在线混合。
6.根据权利要求1所述原子光谱仪样品进样的方法,其中含胺基的二硫代甲酸(盐)在与元素溶液混合后的质量浓度是0.005-5%。
7.根据权利要求1所述的形成方法,其中在线待混合后的溶液的酸度是0.01-3.0摩尔/升。
8.一种原子光谱仪样品进样的方法,其包括如下步骤:(1)使用蠕动泵分别以1-5毫升的相等速度连续抽取质量浓度为0.01-0.5%的二乙基二硫代氨基甲酸钠溶液和酸度为0.02-1.0 M的含元素样品溶液;(2)使两股溶液在一微型三通管内汇合反应,然后立即在气液分离器中进行气液分离;(3)分离出的气体被导入原子光谱仪中进行测定。
9.一种用于原子光谱仪样品进样的装置,其特征在于该装置包括含元素的样品溶液导入管(1)、含胺基的二硫代甲酸(盐)溶液的导入管(2)、蠕动泵(3)、三通管(4)、气液分离器(5)载气入口(6)、载气出口(7)和废液排放管(8);蠕动泵(3)抽取两个溶液后通过三通后两股溶液混合,然后与气液分离器(5)相连,气液分离器中含多孔玻璃烧结板制成的透气不透水的半透膜,气液分离器设有载气入口(6),和载气入口(7),分离气体挥发物的废液被蠕动泵带动经废液排放管(8)排出。
10.权利要求1所述的原子光谱仪样品进样方法在用于化学气相沉积及无机镀膜气态先驱物的制备方面的应用。
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