CN108279214A - 一种元素形成挥发物时效率增强的方法 - Google Patents
一种元素形成挥发物时效率增强的方法 Download PDFInfo
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- CN108279214A CN108279214A CN201711398935.XA CN201711398935A CN108279214A CN 108279214 A CN108279214 A CN 108279214A CN 201711398935 A CN201711398935 A CN 201711398935A CN 108279214 A CN108279214 A CN 108279214A
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- 238000000034 method Methods 0.000 title claims abstract description 20
- 230000002708 enhancing effect Effects 0.000 title claims description 8
- 230000015572 biosynthetic process Effects 0.000 title claims description 5
- 239000003039 volatile agent Substances 0.000 claims abstract description 32
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 239000012488 sample solution Substances 0.000 claims abstract description 18
- 230000035945 sensitivity Effects 0.000 claims abstract description 16
- -1 small molecule organic compounds Chemical class 0.000 claims abstract description 16
- 238000001514 detection method Methods 0.000 claims abstract description 7
- 238000000921 elemental analysis Methods 0.000 claims abstract description 5
- 125000000623 heterocyclic group Chemical group 0.000 claims abstract description 4
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 27
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 14
- 150000002894 organic compounds Chemical class 0.000 claims description 13
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 12
- LMBWSYZSUOEYSN-UHFFFAOYSA-N diethyldithiocarbamic acid Chemical compound CCN(CC)C(S)=S LMBWSYZSUOEYSN-UHFFFAOYSA-N 0.000 claims description 12
- 229940116901 diethyldithiocarbamate Drugs 0.000 claims description 9
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 8
- 229910052737 gold Inorganic materials 0.000 claims description 8
- 239000010931 gold Substances 0.000 claims description 8
- 229910017052 cobalt Inorganic materials 0.000 claims description 7
- 239000010941 cobalt Substances 0.000 claims description 7
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 7
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 5
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 5
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- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 4
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- 229910052797 bismuth Inorganic materials 0.000 claims description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 3
- 229910052793 cadmium Inorganic materials 0.000 claims description 3
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 3
- 125000004432 carbon atom Chemical group C* 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 239000011651 chromium Substances 0.000 claims description 3
- 229910052741 iridium Inorganic materials 0.000 claims description 3
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 150000002576 ketones Chemical class 0.000 claims description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 3
- 150000002825 nitriles Chemical class 0.000 claims description 3
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- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- CZGGKXNYNPJFAX-UHFFFAOYSA-N Dimethyldithiophosphate Chemical compound COP(S)(=S)OC CZGGKXNYNPJFAX-UHFFFAOYSA-N 0.000 claims description 2
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 2
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- MZGNSEAPZQGJRB-UHFFFAOYSA-N dimethyldithiocarbamic acid Chemical compound CN(C)C(S)=S MZGNSEAPZQGJRB-UHFFFAOYSA-N 0.000 claims description 2
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims description 2
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- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 2
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- OYEHPCDNVJXUIW-UHFFFAOYSA-N plutonium atom Chemical compound [Pu] OYEHPCDNVJXUIW-UHFFFAOYSA-N 0.000 claims description 2
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims description 2
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- 229910052761 rare earth metal Inorganic materials 0.000 claims description 2
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims description 2
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 claims description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 2
- 229910052716 thallium Inorganic materials 0.000 claims description 2
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 claims description 2
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 claims description 2
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- 238000004458 analytical method Methods 0.000 abstract description 4
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- 238000002360 preparation method Methods 0.000 abstract description 3
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- 230000002572 peristaltic effect Effects 0.000 description 14
- 239000002699 waste material Substances 0.000 description 11
- 239000012159 carrier gas Substances 0.000 description 10
- 150000003839 salts Chemical class 0.000 description 10
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 9
- 229910052700 potassium Inorganic materials 0.000 description 9
- 239000011591 potassium Substances 0.000 description 9
- 238000000889 atomisation Methods 0.000 description 8
- 150000004678 hydrides Chemical class 0.000 description 7
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 6
- 238000004949 mass spectrometry Methods 0.000 description 6
- 229910052708 sodium Inorganic materials 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- WREDNSAXDZCLCP-UHFFFAOYSA-N methanedithioic acid Chemical compound SC=S WREDNSAXDZCLCP-UHFFFAOYSA-N 0.000 description 5
- ZKDDJTYSFCWVGS-UHFFFAOYSA-M sodium;diethoxy-sulfanylidene-sulfido-$l^{5}-phosphane Chemical class [Na+].CCOP([S-])(=S)OCC ZKDDJTYSFCWVGS-UHFFFAOYSA-M 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
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- IRDLUHRVLVEUHA-UHFFFAOYSA-N diethyl dithiophosphate Chemical compound CCOP(S)(=S)OCC IRDLUHRVLVEUHA-UHFFFAOYSA-N 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
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- 238000005070 sampling Methods 0.000 description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 description 4
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- 229910052783 alkali metal Inorganic materials 0.000 description 3
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- 229950004394 ditiocarb Drugs 0.000 description 3
- 239000006199 nebulizer Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- GSFSVEDCYBDIGW-UHFFFAOYSA-N 2-(1,3-benzothiazol-2-yl)-6-chlorophenol Chemical compound OC1=C(Cl)C=CC=C1C1=NC2=CC=CC=C2S1 GSFSVEDCYBDIGW-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 150000001342 alkaline earth metals Chemical class 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 238000000559 atomic spectroscopy Methods 0.000 description 2
- KXDHJXZQYSOELW-UHFFFAOYSA-N carbamic acid group Chemical class C(N)(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
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- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- AJNBOIIIBVQARG-UHFFFAOYSA-N [K].CCCOP(S)(=S)OCCC Chemical compound [K].CCCOP(S)(=S)OCCC AJNBOIIIBVQARG-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- ZUNFAOLVHKUWCL-UHFFFAOYSA-N dipropoxy-sulfanyl-sulfanylidene-$l^{5}-phosphane Chemical compound CCCOP(S)(=S)OCCC ZUNFAOLVHKUWCL-UHFFFAOYSA-N 0.000 description 1
- 239000012990 dithiocarbamate Substances 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- NDBRRRXCHZEEMS-UHFFFAOYSA-M sodium;dimethoxy-sulfanylidene-sulfido-$l^{5}-phosphane Chemical compound [Na+].COP([S-])(=S)OC NDBRRRXCHZEEMS-UHFFFAOYSA-M 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- DNYWZCXLKNTFFI-UHFFFAOYSA-N uranium Chemical compound [U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U] DNYWZCXLKNTFFI-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
-
- 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Pathology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Immunology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
本发明公开一种元素形成挥发物时效率增强的方法，它是向形成元素挥发物的反应体系中添加水溶性的小分子有机化合物，其中添加水溶性的小分子有机化合物的体积浓度是反应体系体积的0.25‑4%；所述的反应体系指的是：螯合试剂和含元素样品溶液的混合溶液；所述的水溶性的小分子有机化合物是水溶性的醇、杂环。所述的螯合试剂：含元素样品溶液体积比为0.1:1‑1:0.25。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，涉及原子光谱仪样品进样的方法，更广泛的，本发明也用于化学气相沉积及无机镀膜的气态先驱物的制备，特别是一种元素形成挥发物时效率增强的方法。
背景技术
目前，原子光谱仪中所使用的氢化物发生进样系统，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。已经具有成熟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20年来，研究发现硼氢化钠也能和其它元素（如金银等贵金属元素，钴镍等过渡元素）生成元素挥发物。
近来，随着科技人员研究的不断深入，一些从事分析的工作人员发现：一些螯合试剂，如乙二胺二硫代氨基甲酸（钠或钾）和二乙基二硫代磷酸钠（钾）能与众多金属元素的水溶液在室温下形成元素挥发物，并用于原子光谱的样品进入方法。如上所述，该方法也提高了元素的分析灵敏度，降低了检出限。并也可用于元素的化学气相沉积技术用于半导体和薄膜的制作。
现有的技术不足：
如上所述的螯合试剂和元素形成挥发物的方法，尽管有许多优点，但还是有如下不足：（1）目前能用于形成挥发物的螯合试剂还有限，主要是乙二胺二硫代氨基甲酸（钠或钾等）和二乙基二硫代磷酸钠（或钾等），而其它螯合试剂形成的效率确很低，没有实际应用价值；（2）即使是乙二胺二硫代氨基甲酸（钠或钾等）和二乙基二硫代磷酸钠（或钾等）两种试剂，尽管发现其能和许多元素形成挥发物，但不同的元素，形成挥发物的效率并不同。有的比较高，有的比较低。因此使有些元素分析的检测灵敏度还是受到影响。
发明内容
本发明的目的在于克服现有技术的缺点与不足，提供一种能够增强螯合物与元素反应时元素挥发物生成效率的方法。
本发明的技术方案如下：
一种元素形成挥发物时效率增强的方法，其特征在于向形成元素挥发物的反应体系中添加水溶性有机化合物，所述的反应体系指的是：螯合试剂和含元素样品溶液的混合溶液；其中螯合试剂是指烷基二硫代胺基甲酸盐、烷基二硫代磷酸盐。
本发明中水溶性有机物是指含碳原子数小于等于4的水溶性的醇、腈、酮和杂环
其中优选的水溶性的有机化合物是（但不限于）甲醇、乙醇、正丙醇、异丙醇、乙腈、四氢呋喃、丙酮。更加优选的水溶性有机化合物是甲醇、乙醇。
上述的水溶性的有机化合物添加体积浓度是反应体系体积的0.25-4%，优选水溶性的有机化合物添加体积浓度是反应体系体积的0.25-1.5%。
本发明中的螯合试剂优选（但不限于）的是二乙基二硫代氨基甲酸盐、二甲基二硫代胺基甲酸盐、二乙基二硫代磷酸盐、二甲基二硫代磷酸盐、二丙基二硫代磷酸盐。其中的盐是指上述螯合试剂与碱金属碱土金属形成的螯合试剂的盐。
本发明中的螯合试剂(以钠盐为计)用量的质量体积浓度（m/V）是0.1-0.6%，该浓度是在元素溶液与螯合试剂溶液混合时体积比为1:1时为基础计算的。当二个溶液混合体积比发生变化时，螯合试剂浓度应该做相应调整，使混合后的溶液含螯合试剂浓度在0.05%-0.3%之间，优选0.1%-0.25%。
所述的向形成元素挥发物的反应体系中的一个事先加入水溶性小分子有机化合物优选向螯合试剂溶液中事先加入极性小于水的水溶性小分子有机化合物。
本发明进一步公开了元素形成挥发物时效率增强的方法在提高提高元素分析灵敏度、改善检出限方面的应用。实验结果显示：本发明的方法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；使其增强元素形成挥发物的效率。也可用于化学气相沉积及无机镀膜的气态先驱物的制备。
本发明更加详细的描述如下：
本发明中所述的水溶性的小分子有机化合物是极性小于水的水溶性的含碳原子数小于等于4的水溶性的醇、腈、酮和杂环；优选水溶性的小分子有机化合物是水溶性的醇；更加优选的水溶性的小分子有机化合物是甲醇、乙醇。
其中水溶性的小分子有机化合物添加浓度（体积浓度）是反应体系体积（螯合试剂与元素溶液体积之和）的0.25-4%.优选的水溶性的小分子有机化合物添加浓度（体积浓度）是反应体系体积的0.5-1.5%.
适用于本发明的螯合试剂主要是（但不限于）指：（1）含胺基的二硫代甲酸（盐），如二乙基二硫代氨基甲酸盐、二甲基二硫代胺基甲酸盐等；（2）含烷基的二硫代磷（膦）酸盐，如二乙基二硫代磷酸钠、二甲基二硫代磷酸钠、二丙基二硫代磷酸钾等。上面所述的螯合试剂的盐主要是（但不限于）指螯合试剂与碱金属、碱土金属及氨形成的盐；其中碱金属主要是指锂、钠、钾；碱土金属为镁和钙。
上述的含胺基的二硫代甲酸（盐）优选为二乙基二硫代氨基甲酸钠、二乙基二硫代磷酸钠。
本发明中待测元素主要包括（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。
本发明中的两个溶液优选的浓度分别是0.1-0.5%（w/w）螯合试剂的溶液与0.1-0.4 M酸度的待测元素溶液在线混合，其体积混合比为1:1。在此基础上，向两个溶液中的一个事先加入水溶性小分子有机化合物。优选添加在螯合试剂溶液中。
本发明的一个典型实施例包括如下步骤：（1）使用蠕动泵分别连续抽取质量浓度为0.4%的二乙基二硫代氨基甲酸钠（DDTC），并添加了3%体积的乙醇的溶液和酸度为0.15M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。
本发明的另外一个典型实施例包括如下步骤：（1）使用蠕动泵分别连续抽取质量浓度为0.4%的二乙基二硫代磷酸钠（DDTP）溶液和酸度为0.15M并添加了2%体积的甲醇的含元素样品溶液；（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。
本发明的再一个典型实施例包括如下步骤：（1）使用蠕动泵分别连续抽取添加了3%体积的甲醇的质量浓度为0.4%的二甲基基二硫代氨基甲酸钠（福百钠）溶液和酸度为0.1M并含元素样品的样品溶液；（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。
本发明的第一个典型的装置（见说明书附图1），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为适用于元素挥发物形成的装置图（已知）；
图2为带有雾化器的适用于元素挥发物形成的装置图（已知）；
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
下面通过具体的实施方案叙述本发明。除非特别说明，本发明中所用的技术手段均为本领域技术人员所公知的方法。另外，实施方案应理解为说明性的，而非限制本发明的范围，本发明的实质和范围仅由权利要求书所限定。对于本领域技术人员而言，在不背离本发明实质和范围的前提下，对这些实施方案中的物料成分和用量进行的各种改变或改动也属于本发明的保护范围。本发明所用原料及试剂均有市售。
实施例1
（1）配制含元素金的样品溶液（金含量为50ppb，硝酸酸度0.1 M）和0.4%的二乙基二硫代氨基甲酸钠（铜试剂，DDTC）溶液（该溶液含有2%的体积浓度的乙醇）, 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）从三通出口管流出的反应液立即流入到一气液分离器中，在这里通过鼓泡或喷雾的方式，分离出的元素挥发物（DDTC和元素的络合物），同时产生的反应完的废液被及时排除。生成的金的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乙醇时的2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）使含元素镍的样品溶液（镍含量为40ppb，硝酸酸度0.15M，甲醇添加量为2%体积浓度）和0.5%的二乙基二硫代磷酸钠（DDTP）溶液在线混合反应, 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）从三通出口管流出的反应液立即流入到一气液分离器中，在这里通过鼓泡或喷雾的方式，分离出的元素挥发物（DDTC和元素的络合物），同时产生的反应完的废液被及时排除。生成的金的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。所测得的镍元素灵敏度是同一条件下溶液不含甲醇时的2.5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
（1）配制含元素钴的样品溶液（钴含量为50ppb，硝酸酸度0.1 M）和0.5%的二甲基二硫代氨基甲酸钠（福百钠）溶液（该溶液含有2%的体积浓度的乙腈）, 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）从三通出口管流出的反应液立即流入到一气液分离器中，在这里通过鼓泡或喷雾的方式，分离出的元素挥发物（DDTC和元素的络合物），同时产生的反应完的废液被及时排除。生成的钴的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乙腈时的3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4
（1）配制含元素铅的样品溶液（铅含量为50ppb，硝酸酸度0.1 M）和0.4%的二甲基二硫代磷酸钠溶液（该溶液含有3%的体积浓度的乙醇）, 然后采用蠕动泵分别以2.2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）从三通出口管流出的反应液立即流入到一气液分离器中，在这里通过鼓泡或喷雾的方式，分离出的元素挥发物（DDTC和元素的络合物），同时产生的反应完的废液被及时排除。生成的铅的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丙醇时的2.3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。
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 (7)
1.一种元素形成挥发物时效率增强的方法，其特征在于向形成元素挥发物的反应体系中添加水溶性的小分子有机化合物，其中添加水溶性的小分子有机化合物的体积浓度是反应体系体积的0.25-4%；所述的反应体系指的是：螯合试剂溶液和含元素样品溶液的混合溶液；其中螯合试剂溶液与含元素样品溶液体积比为0.1:1-1:0.25所述的水溶性的小分子有机化合物是含碳原子数小于等于4的水溶性的醇、腈、酮和杂环。
2.权利要求1所述元素形成挥发物时效率增强的方法，其中水溶性的有机化合物是甲醇、乙醇、正丙醇、异丙醇、乙腈、四氢呋喃、丙酮。
3.权利要求1所述元素形成挥发物时效率增强的方法，其中水溶性的有机化合物是甲醇和乙醇。
4.权利要求1所述元素形成挥发物时效率增强的方法，其中含元素样品溶液指的是待测元素为主族元素铟、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、镥和锕系元素铀、钍和钚的样品溶液。
5.权利要求1所述元素形成挥发物时效率增强的方法，其中水溶性的有机化合物添加体积浓度是反应体系体积的0.25-1.5%。
6.权利要求1所述元素形成挥发物时效率增强的方法，其中螯合试剂指的是二乙基二硫代氨基甲酸盐、二甲基二硫代胺基甲酸盐、二乙基二硫代磷酸盐、二甲基二硫代磷酸盐。
7.权利要求1所述元素形成挥发物时效率增强的方法在提高提高元素分析灵敏度、改善检出限方面的应用。
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| US20060256330A1 (en) * | 2001-05-18 | 2006-11-16 | Esytec Energie-Und Systemtechnik Gmbh | Method and device for comprehensive characterization and monitoring of exhaust gas and control of engines, and components for aftertreatment of exhaust gases |
| CN102230897A (zh) * | 2011-06-27 | 2011-11-02 | 天津师范大学 | 一种用于增强原子光谱气态进样效率的方法 |
| CN106198391A (zh) * | 2016-08-30 | 2016-12-07 | 天津师范大学 | 一种通过元素生成挥发物来测定元素的方法及装置 |
| CN106226252A (zh) * | 2016-07-15 | 2016-12-14 | 天津师范大学 | 一种元素挥发物的形成方法及装置 |
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| US20060256330A1 (en) * | 2001-05-18 | 2006-11-16 | Esytec Energie-Und Systemtechnik Gmbh | Method and device for comprehensive characterization and monitoring of exhaust gas and control of engines, and components for aftertreatment of exhaust gases |
| CN102230897A (zh) * | 2011-06-27 | 2011-11-02 | 天津师范大学 | 一种用于增强原子光谱气态进样效率的方法 |
| CN106226252A (zh) * | 2016-07-15 | 2016-12-14 | 天津师范大学 | 一种元素挥发物的形成方法及装置 |
| CN106198391A (zh) * | 2016-08-30 | 2016-12-07 | 天津师范大学 | 一种通过元素生成挥发物来测定元素的方法及装置 |
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