CN107525776B - Sample feeding method and device for atomic spectrometers - Google Patents
Sample feeding method and device for atomic spectrometers Download PDFInfo
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- CN107525776B CN107525776B CN201710545032.3A CN201710545032A CN107525776B CN 107525776 B CN107525776 B CN 107525776B CN 201710545032 A CN201710545032 A CN 201710545032A CN 107525776 B CN107525776 B CN 107525776B
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- 238000000034 method Methods 0.000 title claims abstract description 10
- 239000000243 solution Substances 0.000 claims abstract description 47
- 239000007788 liquid Substances 0.000 claims abstract description 45
- 238000005259 measurement Methods 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 238000001514 detection method Methods 0.000 claims abstract description 4
- 239000011259 mixed solution Substances 0.000 claims abstract description 3
- 239000012159 carrier gas Substances 0.000 claims description 22
- 230000002572 peristaltic effect Effects 0.000 claims description 19
- 239000002699 waste material Substances 0.000 claims description 15
- LMBWSYZSUOEYSN-UHFFFAOYSA-N diethyldithiocarbamic acid Chemical compound CCN(CC)C(S)=S LMBWSYZSUOEYSN-UHFFFAOYSA-N 0.000 claims description 9
- 229950004394 ditiocarb Drugs 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 239000005373 porous glass Substances 0.000 claims description 6
- 239000000284 extract Substances 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 abstract description 13
- WREDNSAXDZCLCP-UHFFFAOYSA-N methanedithioic acid Chemical compound SC=S WREDNSAXDZCLCP-UHFFFAOYSA-N 0.000 abstract description 9
- 238000002347 injection Methods 0.000 abstract description 6
- 239000007924 injection Substances 0.000 abstract description 6
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 abstract description 4
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 13
- 239000012488 sample solution Substances 0.000 description 9
- 150000004678 hydrides Chemical class 0.000 description 8
- IOEJYZSZYUROLN-UHFFFAOYSA-M Sodium diethyldithiocarbamate Chemical compound [Na+].CCN(CC)C([S-])=S IOEJYZSZYUROLN-UHFFFAOYSA-M 0.000 description 7
- 125000003277 amino group Chemical group 0.000 description 6
- 238000005070 sampling Methods 0.000 description 6
- 230000035945 sensitivity Effects 0.000 description 6
- 238000000889 atomisation Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- 229910052783 alkali metal Inorganic materials 0.000 description 4
- 150000001340 alkali metals Chemical class 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 4
- 229910052753 mercury Inorganic materials 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 3
- 150000001342 alkaline earth metals Chemical class 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 239000003595 mist Substances 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 229910052718 tin Inorganic materials 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- 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 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- DKVNPHBNOWQYFE-UHFFFAOYSA-N carbamodithioic acid Chemical compound NC(S)=S DKVNPHBNOWQYFE-UHFFFAOYSA-N 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229940116901 diethyldithiocarbamate Drugs 0.000 description 2
- 239000012990 dithiocarbamate Substances 0.000 description 2
- 238000004993 emission spectroscopy Methods 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 229910052741 iridium Inorganic materials 0.000 description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 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 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052703 rhodium Inorganic materials 0.000 description 2
- 239000010948 rhodium Substances 0.000 description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 description 2
- 239000012279 sodium borohydride Substances 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 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 1
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910052765 Lutetium Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052778 Plutonium Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910052773 Promethium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 125000003368 amide group Chemical group 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
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 238000001675 atomic spectrum Methods 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 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
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- OYEHPCDNVJXUIW-UHFFFAOYSA-N plutonium atom Chemical compound [Pu] OYEHPCDNVJXUIW-UHFFFAOYSA-N 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- VQMWBBYLQSCNPO-UHFFFAOYSA-N promethium atom Chemical compound [Pm] VQMWBBYLQSCNPO-UHFFFAOYSA-N 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- NVIFVTYDZMXWGX-UHFFFAOYSA-N sodium metaborate Chemical compound [Na+].[O-]B=O NVIFVTYDZMXWGX-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 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
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 1
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
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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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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method and a device for sample injection of atomic spectrometers, which are characterized in that a solution of dithio formic acid (salt) containing amino is mixed with an element solution to be detected on line, the mixed solution is immediately subjected to gas-liquid separation and measurement, so that a volatile element complex enters an element analyzer for detection or is used for preparing a chemical vapor deposition film of the element.
Description
Technical Field
The invention belongs to the technical field of instrument analysis, and relates to a sample feeding method and device for atomic spectrometers.
Background
At present, most hydride generation sample injection systems used in atomic spectrometers use sodium (potassium) borohydride as a hydride generation reduction reagent, and after elements in a sample solution are reduced to gaseous hydrides by hydrogen in the sodium (potassium) borohydride, the elements are measured in the atomic spectrometers. Compared with the conventional pneumatic atomization sampling in atomic spectrum, the hydride sampling efficiency has higher sampling efficiency (the conventional pneumatic atomization sampling is only 3-5%, the determination sensitivity is lower, and the hydride sampling efficiency is close to 100%), so the hydride sampling efficiency has the characteristics of higher sensitivity and lower detection limit in determination. It has been used that hydrides of sodium (potassium) borohydride and nine elements (arsenic, antimony, bismuth, germanium, tin, lead, selenium, tellurium, mercury) which are traditionally easy to form hydrides are formed and measured by an atomic spectrometer.
In recent years, with the intensive research of scientific and technical personnel, workers engaged in analysis have successively found that other elements can also react with sodium (potassium) borohydride to generate hydrogenation reaction, and have published a plurality of research papers one after another.
Another defects caused by using sodium borohydride chemical vapor is that sodium borohydride is expensive and unstable, a solid reagent is decomposed into blocky sodium metaborate after long-term standing, and a solution is decomposed after long-term standing. needs to be prepared at present.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides brand-new methods and devices for sample injection of atomic spectrometers.
The technical scheme of the invention is as follows:
sample introduction method for atomic spectrometer, which is characterized in that the solution of dithioformic acid (salt) containing amido is mixed with the solution of element to be detected on line, the mixed solution is immediately subjected to gas-liquid separation and measurement, and the volatile element complex enters an element analyzer for detection or is used for preparing chemical vapor deposition film of the element.
The dithioformic acid (salt) containing amino group in the invention is soluble salt which is soluble in water.
The dithiocarbamate (salt) containing an amino group in the present invention is preferably a salt of diethyldithiocarbamate with an alkali metal, an alkaline earth metal and ammonia. Wherein the alkali metal is lithium, sodium and potassium; the alkaline earth metal is magnesium and calcium, preferably the salt of diethyldithiocarbamate with the alkali metals lithium, sodium and potassium, particularly preferably sodium dimethyldithiocarbamate (Na-DDTC)
The elements to be measured in the invention refer to part of main group elements, part of transition elements, noble metal elements and rare earth elements.
The present invention is characterized in that 0.005-35% (w/w) of a solution of dithiocarbamate containing an amine group is mixed in-line with a solution of an element to be measured having an acidity of 0.005-10.0M.
The invention is characterized in that the mass concentration of the dithio formic acid (salt) containing amino after being mixed with the element solution is 0.005-5%, preferably 0.01-1%; more preferably 0.015 to 0.5%.
The invention is characterised in that the acidity of the solution after the in-line mixing is between 0.01 and 3.0 mol/l, preferably between 0.02 and 1M,
more preferably, the acidity is 0.05 to 0.6M.
The element to be detected in the invention refers to a main group metal element excluding alkali metal and alkaline earth metal; a partial transition element; noble metal elements and rare earth elements. These elements include (but are not limited to): main group metal elements of indium, thallium, tin, lead and bismuth; transition elements of titanium, chromium, manganese, iron, cobalt, nickel, copper, zinc, cadmium and mercury; noble metal elements such as ruthenium, rhodium, palladium, silver, iridium, platinum and gold; the rare earth elements cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, uranium, thorium, and plutonium.
Preferred elements among the above elements refer to tin, lead, ruthenium, rhodium, palladium, silver, iridium, platinum, gold, titanium, chromium, manganese, iron, cobalt, nickel, copper, zinc, cadmium and mercury.
typical embodiments of the present invention include the steps of (1) continuously pumping a sodium diethyldithiocarbamate solution having a mass concentration of 0.01 to 0.5% and an element-containing sample solution having an acidity of 0.02 to 0.3M at an equal flow rate of 1 to 5 ml, respectively, by using a peristaltic pump, (2) causing the two solutions to join together in a micro three-way tube and then immediately performing gas-liquid separation in a gas-liquid separator, and (3) introducing the separated gas into an atomic spectrometer for measurement.
The invention further discloses a sample introduction device applicable to an atomic spectrometer, which is characterized by comprising an element-containing sample solution introduction pipe 1, an amino-containing dithioformic acid (salt) solution introduction pipe 2, a peristaltic pump 3, a three-way pipe 4, a gas-liquid separator 5, a gas-liquid separator, a gas-liquid permeable and water-tight semipermeable membrane made of a porous glass sintered plate, a carrier gas inlet 6, a carrier gas outlet 7 and a waste liquid discharge pipe 8, wherein the peristaltic pump 3 extracts two solutions, then the two solutions are mixed through a tee joint and then are connected with the gas-liquid separator 5, the gas-liquid separator is provided with the carrier gas inlet 6 and the carrier gas inlet 7, and waste liquid for separating gas volatile matters is discharged through the waste liquid discharge pipe 8 by the peristaltic pump.
The invention further discloses an application of the sample injection method of atomic spectrometer in chemical vapor deposition and preparation of inorganic coating gaseous precursor.
The typical sample introduction device for atomic spectrometer (see attached figure 1 in description) comprises an element-containing sample solution introduction pipe, an amino-containing dithioformic acid (salt) solution introduction pipe, a peristaltic pump, a three-way pipe, a gas-liquid separator (containing porous glass sintered plate and other gas-permeable and water-impermeable semipermeable membranes), a carrier gas inlet, a carrier gas outlet and a waste liquid discharge pipe 8, wherein the peristaltic pump extracts two solutions, the two solutions are converged in the three-way pipe to react and then connected with the gas-liquid separator, the gas-liquid separator is provided with the carrier gas inlet and the carrier gas inlet, and waste liquid for separating gas volatile matters is discharged by the peristaltic pump through a waste liquid discharge pipe.
A second exemplary sample introduction device for an atomic spectrometer (see the attached drawing 2 in the specification) suitable for the present invention comprises an element-containing sample solution introduction tube 1, an amine group-containing dithioformic acid (salt) solution introduction tube 2, a peristaltic pump 3, a three-way tube 4, an atomizer 9 for atomization sample introduction of atomic absorption or inductively coupled plasma emission spectroscopy (or mass spectrometry), a mist chamber (a cyclone mist chamber or a Scott mist chamber) 5 for atomic absorption or inductively coupled plasma emission spectroscopy (or mass spectrometry), a carrier gas inlet 6, a carrier gas outlet 7 and a waste liquid discharge tube 8; the peristaltic pump extracts the two solutions, the two solutions are mixed through the tee joint and then enter the atomizer, the atomizer sprays the two solutions and then enters the fog chamber, the gas-liquid separator is provided with a carrier gas inlet and a carrier gas outlet, and waste liquid of separated gas volatile matters is discharged by the peristaltic pump through a waste liquid discharge pipe.
Description of the drawings:
FIG. 1 is a diagram of an apparatus suitable for sample injection in an atomic spectrometer;
FIG. 2 is a diagram of a sample injection device of a suitable atomic spectrometer with an atomizer;
1. sample solution introducing tube for element, 2 dithioformic acid (salt) solution introducing tube containing amino group
3. A peristaltic pump 4, a three-way pipe 5, a gas-liquid separator 6, a carrier gas inlet,
7 carrier gas outlet 8 and waste liquid discharge pipe 9 atomizer.
Detailed Description
In order to more fully explain the practice of the invention, the following preparative examples of the invention are provided. These examples are merely illustrative and do not limit the scope of the invention.
Example 1
(1) Respectively preparing sample solutions containing gold and silver elements (the element content is 500ppb, the nitric acid acidity is 0.3M) and 0.4% sodium diethyldithiocarbamate (copper reagent, DDTC) solutions, and then respectively pumping the two solutions at the flow rate of 2 ml/min by adopting a peristaltic pump so that the two solutions are converged in three-way pipes and then react.
(2) Separating the generated element volatile matters and the solution after reaction in an gas-liquid separator;
(3) the reaction solution from the three-way outlet pipe immediately flows into gas-liquid separator, where the volatile element (DDTC and element complex) is separated by bubbling through a porous glass sintered plate, and the volatile element is introduced into an atomic spectrometer atomization or ionization device for spectral or mass spectrometric measurement, the measured element sensitivity is 25-40 times that of the solution without DDTC under conditions, the measurement sensitivity is greatly improved, and the detailed illustration is shown in figure 1 of the specification.
Example 2
(1) Sample solutions containing element mercury (element content is 500ppb, nitric acid acidity is 0.10M) and 0.4% sodium diethyldithiocarbamate (copper reagent, DDTC) solutions are prepared respectively, and then the two solutions are extracted by a peristaltic pump at the flow rate of 1.8 ml/min respectively, so that the two solutions are converged in tee pipes and then react.
(2) Separating the generated element volatile matters and the solution after reaction in an gas-liquid separator;
(3) the reaction solution from the three-way outlet pipe immediately flows into gas-liquid separator, where the volatile element (DDTC and element complex) is separated by bubbling through a porous glass sintered plate, and the volatile element is introduced into an atomic spectrometer atomization or ionization device for spectral or mass spectrometric measurement, the measured element sensitivity is 25-40 times that of the solution without DDTC under conditions, the measurement sensitivity is greatly improved, and the detailed illustration is shown in figure 1 of the specification.
Example 3
sample introduction device for atomic spectrometer, comprising an element-containing sample solution introduction tube 1, an amino group-containing dithioformic acid (salt) solution introduction tube 2, a peristaltic pump 3, a three-way tube 4, and a gas-liquid separator, wherein the gas-liquid separator comprises a gas-permeable and water-impermeable semipermeable membrane made of a porous glass sintered plate, a carrier gas inlet, a carrier gas outlet and a waste liquid discharge tube, the peristaltic pump draws the two solutions, then the two solutions are converged in the three-way tube for reaction, and then the gas-liquid separator is connected with the gas-liquid separator, the gas-liquid separator is provided with the carrier gas inlet and the carrier gas inlet, and the waste liquid for separating gas volatile matters is discharged by the.
It will be apparent to those skilled in the art that various changes and modifications can be made in the above embodiments without departing from the scope and spirit of the invention, and it is intended that all simple changes, equivalents and modifications made to the above embodiments in accordance with the technical spirit of the invention shall fall within the scope of the invention.
Claims (1)
- The sample introduction method of atomic spectrometers is characterized in that sodium diethyldithiocarbamate solution and element solution to be detected are mixed on line, the mixed solution is immediately subjected to gas-liquid separation and determination, and volatile element complex enters the atomic spectrometer for detection;the method comprises the following steps:(1) continuously pumping a sodium diethyldithiocarbamate solution with the mass concentration of 0.01-0.5% and a to-be-detected element solution with the acidity of 0.02-1.0M at the same speed of 1-5 ml/min by using a peristaltic pump;(2) the two solutions are converged and reacted in a three-way pipe, and then gas-liquid separation is immediately carried out in a gas-liquid separator;(3) the separated gas is introduced into an atomic spectrometer for measurement;the device adopted by the method comprises an element solution inlet pipe (1) to be detected, a sodium diethyldithiocarbamate solution inlet pipe (2), a peristaltic pump (3), a three-way pipe (4), a gas-liquid separator (5), a carrier gas inlet (6), a carrier gas outlet (7) and a waste liquid discharge pipe (8); the peristaltic pump (3) extracts the element solution to be detected and the sodium diethyldithiocarbamate solution, the two solutions are mixed after passing through the three-way pipe (4) and then are connected with the gas-liquid separator (5), the gas-liquid separator contains a permeable and impermeable semipermeable membrane made of a porous glass sintered plate, the gas-liquid separator is provided with a carrier gas inlet (6) and a carrier gas outlet (7), and the waste liquid for separating gas volatile matters is driven by the peristaltic pump (3) to be discharged through a waste liquid discharge pipe (8).
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| CN201610557720.7A CN106248593A (en) | 2016-07-15 | 2016-07-15 | A kind of method and apparatus of atom spectrometer sample feeding |
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| CN108535185A (en) * | 2018-04-25 | 2018-09-14 | 天津师范大学 | A kind of sample injection method occurred for atomic spectrograph gaseous state chelate |
| CN108732162B (en) * | 2018-05-29 | 2024-07-26 | 四川轻化工大学 | Rapid detection device and detection method for arsenic concentration in water |
| CN109709054A (en) * | 2019-01-21 | 2019-05-03 | 广西科技大学鹿山学院 | Flame atomic absorption spectrophotometer aeration sample introduction regulating device |
| CN109900683A (en) * | 2019-03-26 | 2019-06-18 | 攀钢集团攀枝花钢铁研究院有限公司 | The online internal standard hybrid system of Element detection |
| CN115561228B (en) * | 2022-09-28 | 2024-10-29 | 攀钢集团攀枝花钢铁研究院有限公司 | Element content detection device and detection method |
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