CN102967590B - 一种直接进样同时测定汞和镉的方法和仪器 - Google Patents
一种直接进样同时测定汞和镉的方法和仪器 Download PDFInfo
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- 229910052753 mercury Inorganic materials 0.000 title claims abstract description 104
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 229910052793 cadmium Inorganic materials 0.000 title claims abstract description 83
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000012360 testing method Methods 0.000 title claims abstract description 34
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000001514 detection method Methods 0.000 claims abstract description 21
- 238000000197 pyrolysis Methods 0.000 claims abstract description 21
- 229910052786 argon Inorganic materials 0.000 claims abstract description 20
- 238000001704 evaporation Methods 0.000 claims abstract description 15
- 230000008020 evaporation Effects 0.000 claims abstract description 15
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- 239000001257 hydrogen Substances 0.000 claims abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 13
- 238000004458 analytical method Methods 0.000 claims abstract description 11
- 239000007789 gas Substances 0.000 claims abstract description 11
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 11
- 239000010937 tungsten Substances 0.000 claims abstract description 11
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 10
- 239000011733 molybdenum Substances 0.000 claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 8
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000010521 absorption reaction Methods 0.000 claims abstract description 6
- 239000012298 atmosphere Substances 0.000 claims abstract description 6
- PWKWDCOTNGQLID-UHFFFAOYSA-N [N].[Ar] Chemical compound [N].[Ar] PWKWDCOTNGQLID-UHFFFAOYSA-N 0.000 claims abstract description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052737 gold Inorganic materials 0.000 claims abstract description 4
- 239000010931 gold Substances 0.000 claims abstract description 4
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Abstract
本发明涉及一种直接进样同时测定汞和镉的方法和仪器,样品无需消解,步骤如下:在有氧气氛下,加热样品,温度控制在120-500℃,样品中大部分Hg和分解物析出;由空气气流将Hg和析出物载入催化炉中进一步分解,Hg被金齐化吸收,Cd仍存在于样品中;将前述处理过的样品置裂解炉中进一步热分解,样品中Cd和残余Hg被高温汽化;由氩气载带进入镉原子捕集阱,镉被钨丝选择性捕获,残余汞被汞捕集阱吸收;在氩氢气氛中,先后将钨丝或钼丝、金汞加热释放Cd、Hg,由氩氢气载带进入一个原子荧光光谱仪联机。在实现样品中Hg和Cd同时测量功能的基础上,简化整个检测仪器结构,实现小型化,方便常规分析和应急需求,可车载野外使用,具备现场检测的应用前景。
Description
技术领域
本发明涉及重金属测定技术,特别涉及一种样品免消解直接进样且同时测定汞和镉的方法和仪器。
背景技术
伴随着工、农、矿业的发展,越来越多的重金属污染到生活环境、生活用品、食品、药品中,严重污染了环境,严重危害着人类的健康。汞(Hg)、镉(Cd)尤其如此,因其在人体和动物体内累积,具有致癌、致畸和突变的作用,因此其引起的污染一直备受重视,相应的检测技术也是研究者竞相发展的重要领域。
目前,检测技术有紫外-可见分光光度法、原子吸收光谱法、原子荧光光谱法、等离子体发射光谱法,电感耦合等离子体发射光谱法、等离子体质谱法和高效液相色谱法等分析技术。上述方法中,紫外-可见分光光度法不适合多元素同时测定;原子吸收光谱法线性范围窄且每次只能测定一种元素;原子荧光光谱法光谱简单,谱线重叠少,所以可以使用无色散的检测方式,是发展较快的一种原子光谱技术;电感耦合等离子体原子发射光谱法光谱干扰严重,适于测定含量差别较大的不同元素;高效液相色谱法测定重金属则是通过柱前衍生,让重金属元素和有机试剂生成稳定的有色络合物,通过色谱柱分离后,再用紫外可见光度检测器测定,步骤较为繁琐,只能检验单一项目,检测耗时长。除上述适用因素不同之外,诸多方法由于灵敏度低,选择性差,回收率低、操作过程烦琐或所用仪器较为昂贵,对操作者的素质要求颇高等因素,在食品药品等检验领域难以大规模推广普及,短时间内难以广泛应用于检验。
另外,多数检测方法局限于将样品消解成液体后上机测量,且Hg、Cd两元素通常不易用同一种方法提取,分析两个元素的时间很长,过程很繁琐,且基体干扰一直是困扰着直接进样原子光谱检测分析技术的一大难题,虽然经过基体校正后,影响程度能够得以减轻,但并不能从根本上解决这一问题。近年来,对于Hg的检测分析,市场上出现了关于液体、固体粉末或气体直接进样分析的方法和商品仪器,免去复杂的前处理过程,大大节约了分析时间;同样也有关于Cd的直接进样测量相关文献报道和商品仪器出现。可见,Hg、Cd两元素的快速测量在分析检测领域的重要性和必要性。上述Hg、Cd的直接进样分析,是不同的分析手段,通过两种完全不一样的原理、方法和仪器来实现Hg、Cd各自的独立测量。单独分析Hg、Cd两元素商品仪器是分别建立在原子吸收光谱法(AAS)和原子荧光光谱法(AFS)作为终极检测手段的仪器装置,两者虽具有灵敏度高的特点,但是,皆无法实现Hg和Cd两元素同时分析。关键是在现有技术中,将Hg和Cd两元素同时进样,且在同一台仪器中同步检测分析的方法和仪器尚未见报道。
因此,开发出一种快速准确、易于操作的有效检测分析方法,满足更广泛的分析检测单位的使用,也是该检测领域的发展的目标,也将是对现有技术的一种突出贡献。
发明内容
本发明旨在克服现有技术缺陷,弥补现有技术中有关同时检测重金属Hg和Cd方法及仪器的空白,发展一种快速准确、易于操作的有效检测分析方法和仪器,满足更广泛的分析检测单位的使用。另一方面,在实现一个样品中Hg和Cd两元素同时测量的完善功能的基础上,简化仪器结构,实现仪器小型化,可实现车载野外使用,方便实验室常规分析和应急需求,具备现场检测的应用前景。
本发明提供的一种直接进样同时测定汞和镉的方法,包括如下步骤:
样品灰化过程:在有氧气氛下,加热样品,温度控制在120-500℃,样品中大部分汞和分解物析出;由空气气流将汞和析出物载入管式催化炉中进一步分解,汞被汞捕集阱吸收,镉仍存在于样品中;
热裂解、汽化:将前述处理后样品置于裂解炉中,裂解炉炉温度是1600-2000℃,进一步热分解,样品中镉和残余的汞被高温汽化;
捕获与吸收:上述汽化出来的物质,由氩气载带先后进入镉原子捕集阱和汞捕集阱,镉被镉原子捕集阱中的钨丝或钼丝选择性捕获之后,残余的汞被汞捕集阱吸收;
被释放与检测分析:在氩氢气氛中,先后将钨丝或钼丝、金汞加热,镉、汞先后释放出来,由氩氢气载带进入原子荧光光谱仪中检测分析。
本发明所述一种直接进样同时测定汞和镉的方法,其中所述裂解炉置于氩气气氛保护下。
本发明所述一种直接进样同时测定汞和镉的方法,其中所述汞捕集阱含有负载金的吸附剂,与汞形成金汞。
本发明所述一种直接进样同时测定汞和镉的方法,其中所述裂解炉是碳素裂解炉。
本发明所述一种直接进样同时测定汞和镉的方法,其中所述氢气和氩气气氛,氢气的体积百分比为10-90%,所述的空气是由空气压缩机或钢瓶提供,且经净化处理。
本发明所提供的一种直接进样同时测定汞和镉的仪器,是一种原子荧光光谱仪,包括进样***、光源、原子化器、气路***、光路***、检测***、显示装置,其中,所述进样***包括进样联动部件、管式灰化炉、管式催化炉、电热蒸发装置、汞捕集阱和镉原子捕集阱;气路***由带阻尼的转子流量计和稳压阀组成。
本发明所提供的一种直接进样同时测定汞和镉的仪器,所述管式灰化炉和所述管式催化炉为一体化设计,由加热炉丝、保温件、电源和控温***组成,固定于仪器底板的一侧;所述电热蒸发装置由屏蔽罩、蒸发舟、电极、电极托架与电源组成,其中,电极位于蒸发舟的下部,设置在电极托架上,与蒸发舟连接,电源与电极电连接,屏蔽罩与电极托架形成密封空间,所述蒸发舟位于所述密封空间中,屏蔽罩与电极托架活动式连接,屏蔽罩上设有进口和出口,屏蔽罩的出口通过三通管与所述镉原子捕集阱的外罩的进口相连;所述汞捕集阱置于镉原子捕集阱后,通过夹管阀和电路控制实现先后释放,由电源供电加热,从而被捕获的Hg和Cd先后释放,由氩氢气载带进入原子荧光光谱仪器中检测。
本发明所提供的一种直接进样同时测定汞和镉的仪器,所述汞捕集阱由贵金属材料(金、铂、铑等)、支架、装填石英管和电源组成,镉原子捕集阱由钨丝或钼丝、支架、外罩和电源组成,外罩和支架形成密封空间,钨丝或钼丝设置在支架上,所述钨丝或钼丝位于外罩和支架形成的密封空间中,外罩上设有进口和出口。
本发明所提供的一种直接进样同时测定汞和镉的仪器,还包括一个原子荧光光谱仪器,由管式灰化炉、管式催化燃烧炉、电源***、气路***、裂解炉、汞捕集阱、镉原子捕获器和夹管阀组成;
本发明所提供的一种直接进样同时测定汞和镉的仪器,还与另一个原子荧光光谱仪联合使用,是独立于上述所述仪器之外的另一联机检测仪,由原子化器、检测***、光路***组成。
本发明所提供的一种直接进样同时测定汞和镉的方法和仪器的有益效果是:该检测方法在实现一个样品中Hg和Cd两元素同时测量的完善功能的基础上,快速准确,灵敏度高,易于操作,是一种能够满足更广泛的分析检测使用要求的有效检测分析方法;所提供仪器结构大大简化,容易实现小型化,能够实现车载野外使用,方便实验室常规分析和应急需求,具备现场检测的应用前景。
附图说明
图1为本发明一种直接进样同时测定汞和镉的仪器的连接示意图;
图2为本发明一种直接进样同时测定汞和镉的仪器的结构示意图;
图1中,2管式灰化炉,3管式催化炉,4汞捕集阱,5镉原子捕集阱,6裂解炉,7夹管阀(71,72,73,74和75不同位置的夹管阀),8空气,9氩气,10氩氢气,11除水装置,12原子荧光光谱仪器;
图2中,1,进样联动部件,2管式灰化炉,3管式催化炉,4汞捕集阱,5镉原子捕集阱,6裂解炉,9氩气,10氩氢气,11除水装置,12原子荧光光谱仪器。
具体实施方式
结合附图1和附图2具体解释本发明的实施例。
本发明的直接进样同时测定汞和镉的仪器,由进样***、气路***、光源、原子化器、光路***、检测***、显示装置组成,其中,光源、原子化器、光路***、检测***、显示装置均与现有的原子荧光光谱仪相同;光源、光路***、检测***、显示装置、原子化器之间相互连接与位置关系与现有的原子荧光光谱仪12相同;而气路***、进样***的结构则本质不同,气路***由带阻尼的转子流量计和稳压阀构成,进样***由管式灰化炉2、管式催化炉3、除水装置11、裂解炉6、汞捕集阱4、镉原子捕集阱5以及一系列的夹管阀7构成。
具体检测的操作方法及过程如下:
将样品置于本发明所述进样***中进样联动部件1的碳素样品舟中,载有样品的样品舟随进样联动部件1进入管式灰化炉2,进行灰化处理,此时夹管阀71打开,灰化温度由控温***精确控制,在50-500℃实现程序控温,来满足不同样品的灰化条件。灰化过程中释放出来的有机分解物质夹带着样品中大部分Hg,由空气8作为载气,被载带进入管式催化炉3中作进一步燃烧分解,样品被高温汽化,途径管式催化炉3与汞捕集阱4的中间连接装置即除水装置11,除去多余的水份,当分解物经过常温或120℃的汞捕集阱4时,汞被选择性的吸附下来,形成金汞。随后,待管式灰化炉2的炉温降至100-120℃时,进样联动部件1退出管式灰化炉2,进入裂解炉6中,此时,夹管阀71关,夹管阀74开,裂解炉6开始加热到1600-2000℃,样品镉和残余的汞被汽化蒸出,由氩气9载带进入镉原子捕集阱5和汞捕集阱4。当夹管阀74关,夹管阀71和72开时,镉原子捕集阱5被加热至1600-2000℃,镉原子被氩氢气10载带进入原子化器中,此时,原子荧光光谱仪12联机采集数据,得到Cd的信号峰值。将夹管阀72关,夹管阀71开,此时,对金汞齐化吸收阱加热到500-600℃,然后,同时打开73、74、75号夹管阀,由氩氢气10作为载气,将汞载带进入原子荧光光谱仪12的原子化器中,此时,原子荧光联机12采集数据,得到Hg的信号峰值。
实施例1
以10mg白菜(国标物GBW10014)为例,用本发明提供的直接进样同时测定Hg和Cd的原子荧光光谱仪测定样品中Cd为41微克/公斤,在该标准物质的Cd标准值35±6微克/公斤之内;Hg的标准值为11.5微克/公斤,在该标准物质的Hg标准值10.9±1.6微克/公斤之内,Hg、Cd高、中、低水平的加标回收率均在90-110%之间。
实施例2
以10mg米粉(国标物GBW10010)为例,用本发明提供的直接进样测定Hg和Cd的原子荧光光谱仪测定样品中Cd为85微克/公斤,在该标准物质的Cd标准值87±5微克/公斤之内;Hg的测定值为4.8微克/公斤,在该标准物质的Hg标准值5.3±0.5微克/公斤之内,Hg、Cd高、中、低水平的加标回收率均在90-105%之间。
上述两个具体实施例充分说明,采用本发明所述的方法和仪器来直接进样同时测定Hg和Cd,简便可行,且能够准确测得固体样品中的Hg、Cd。
以上的实施例仅仅是对本发明的优选实施方式进行描述,并非对本发明的范围进行限定,在不脱离本发明构思和实质技术方案的前提下,本领域普通工程技术人员对本发明的技术方案作出的各种替换或者相似的技术方案,均应落入本发明公开的权利要求书所确定的保护范围内。
本发明不仅限于上述实施例,除上述实施例外,本发明还可以有其他的实施方式,凡采用本发明所公开的构思、等同替换或等效变换的技术方案,均落在本发明要求的保护范围。
Claims (12)
1.一种直接进样同时测定汞和镉的方法,其特征在于,包括以下步骤:
样品灰化过程:在有氧气氛下,加热样品,温度控制在120-500℃,样品中大部分汞和分解物析出蒸发;由空气气流(8)将汞和析出物载入管式催化炉(3)中进一步分解,汞被汞捕集阱(4)吸收,镉仍存在于样品中;
热裂解、汽化:将前述处理后样品置于裂解炉(6)中,裂解炉(6)炉温度是1600-2000℃,进一步热分解,样品中镉和残余的汞被高温汽化;
捕获与吸收:上述汽化出来的物质,由氩气(9)载带先后进入镉原子捕集阱(5)和汞捕集阱(4),镉被镉原子捕集阱(5)中的钨丝或钼丝选择性捕获之后,残余的汞被汞捕集阱(4)吸收;
被释放与检测分析:在氩氢气氛中,先后将钨丝或钼丝、金汞加热,镉、汞先后释放出来,由氩氢气(10)载带进入原子荧光光谱仪(12)中检测分析。
2.根据权利要求1所述的一种直接进样同时测定汞和镉的方法,其特征在于,所述金汞是指,在样品灰化过程中,汞被汞捕集阱(4)吸收后,与所述汞捕集阱(4)中的负金吸附剂所形成。
3.根据权利要求1所述的一种直接进样同时测定汞和镉的方法,其特征在于,所述裂解炉(6)处于氩气气氛保护下。
4.根据权利要求1所述的一种直接进样同时测定汞和镉的方法,其特征在于,所述裂解炉(6)是碳素裂解炉。
5.根据权利要求1所述的一种直接进样同时测定汞和镉的方法,其特征在于,所述氩氢气氛,氢气含量的体积百分比为10-90%;所述空气气流(8)是由空气压缩机或钢瓶提供,且经净化处理。
6.一种直接进样同时测定汞和镉的仪器,是一种原子荧光光谱仪,包括进样***、光源、原子化器、气路***、光路***、检测***、显示装置,其中所述进样***包括进样联动部件(1)、管式灰化炉(2)、管式催化炉(3)、汞捕集阱(4)、镉原子捕集阱(5)和裂解炉(6);
所述气路***由带阻尼的转子流量计和稳压阀组成,具体检测过程为:
将样品置于进样联动部件(1)的碳素样品舟中,碳素样品舟随进样联动部件(1)进入管式灰化炉(2),进行灰化处理,此时第一夹管阀(71)打开,灰化温度由控温***精确控制;灰化过程中释放出来的有机分解物质夹带着样品中大部分Hg,由空气(8)作为载气,被载带进入管式催化炉(3)中作进一步燃烧分解,并途径管式催化炉(3)与汞捕集阱(4)中间的除水装置(11);接着分解物经过汞捕集阱(4)时,汞被选择性的吸附下来,形成金汞;随后,进样联动部件(1)退出管式灰化炉(2),进入裂解炉(6)中,此时,第一夹管阀(71)关,第四夹管阀(74)开,裂解炉(6)开始加热,样品镉和残余的汞被汽化蒸出,由氩气(9)载带进入镉原子捕集阱(5)和汞捕集阱(4);当第四夹管阀(74)关,第一夹管阀(71)和第二夹管阀(72)开时,镉原子捕集阱(5)被加热,镉原子被氩氢气(10)载带进入原子化器中,此时原子荧光光谱仪(12)联机采集数据,得到Cd的信号峰值;将第二夹管阀(72)关,第一夹管阀(71)开,此时,对汞捕集阱(4)加热,然后,同时打开第三夹管阀(73)、第四夹管阀(74)、第五夹管阀(75),汞原子被氩氢气(10)载带进入原子化器中,此时原子荧光光谱仪(12)联机采集数据,得到Hg的信号峰值。
7.根据权利要求6所述的一种直接进样同时测定汞和镉的仪器,其特征在于,所述管式灰化炉(2)和所述管式催化炉(3)为一体化设计,由加热炉丝、保温件、电源和控温***组成,固定于仪器底板的一侧。
8.根据权利要求6所述的一种直接进样同时测定汞和镉的仪器,其特征在于,所述-裂解炉(6)由屏蔽罩、蒸发舟、电极、电极托架与电源组成,以及
电极位于蒸发舟的下部,设置在电极托架上,与蒸发舟连接,电源与电极电连接,屏蔽罩与电极托架形成密封空间,所述蒸发舟位于所述密封空间中,屏蔽罩与电极托架活动式连接,屏蔽罩上设有进口和出口,屏蔽罩的出口通过三通管与所述镉原子捕集阱(5)的外罩的进口相连。
9.根据权利要求6所述的一种直接进样同时测定汞和镉的仪器,其特征在于,所述汞捕集阱(4)由贵金属材料、支架、装填石英管和电源组成。
10.根据权利要求9所述的一种直接进样同时测定汞和镉的仪器,其特征在于,所述贵金属材料包括金、铂和铑。
11.根据权利要求6所述的一种直接进样同时测定汞和镉的仪器,其特征在于,所述镉原子捕集阱(5)由钨丝或钼丝、支架、外罩和电源组成,以及
外罩和支架形成密封空间;
钨丝或钼丝设置在支架上,且位于外罩和支架形成的密封空间中;
外罩上设有进口和出口。
12.根据权利要求6所述的一种直接进样同时测定汞和镉的仪器,其特征在于,所述直接进样同时测定汞和镉的仪器,还需要与独立于上述仪器之外的另一个原子荧光光谱仪(12)联机检测,所述另一个原子荧光光谱仪(12)由原子化器、检测***、光路***组成。
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