CN108535185A - A kind of sample injection method occurred for atomic spectrograph gaseous state chelate - Google Patents
A kind of sample injection method occurred for atomic spectrograph gaseous state chelate Download PDFInfo
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- CN108535185A CN108535185A CN201810375925.2A CN201810375925A CN108535185A CN 108535185 A CN108535185 A CN 108535185A CN 201810375925 A CN201810375925 A CN 201810375925A CN 108535185 A CN108535185 A CN 108535185A
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- 238000000034 method Methods 0.000 title claims abstract description 38
- 239000013522 chelant Substances 0.000 title claims abstract description 24
- 238000002347 injection Methods 0.000 title claims abstract description 11
- 239000007924 injection Substances 0.000 title claims abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 41
- 239000007788 liquid Substances 0.000 claims abstract description 37
- 239000012159 carrier gas Substances 0.000 claims abstract description 21
- 239000000523 sample Substances 0.000 claims abstract description 21
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 13
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 238000000926 separation method Methods 0.000 claims abstract description 13
- 239000012488 sample solution Substances 0.000 claims abstract description 8
- 239000007789 gas Substances 0.000 claims abstract description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 6
- 239000011591 potassium Substances 0.000 claims abstract description 6
- 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 claims abstract description 5
- 239000002253 acid Substances 0.000 claims abstract description 5
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 5
- 239000011734 sodium Substances 0.000 claims abstract description 5
- 230000002378 acidificating effect Effects 0.000 claims abstract description 4
- LMBWSYZSUOEYSN-UHFFFAOYSA-N diethyldithiocarbamic acid Chemical group CCN(CC)C(S)=S LMBWSYZSUOEYSN-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229950004394 ditiocarb Drugs 0.000 claims abstract description 3
- 238000001704 evaporation Methods 0.000 claims abstract description 3
- 230000008020 evaporation Effects 0.000 claims abstract description 3
- 230000007935 neutral effect Effects 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000004611 spectroscopical analysis Methods 0.000 abstract description 3
- 239000012670 alkaline solution Substances 0.000 abstract 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 8
- 229910052793 cadmium Inorganic materials 0.000 description 8
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 8
- 230000005587 bubbling Effects 0.000 description 7
- 239000011521 glass Substances 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 235000013495 cobalt Nutrition 0.000 description 5
- 238000005194 fractionation Methods 0.000 description 5
- 150000004678 hydrides Chemical class 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- 239000001569 carbon dioxide Substances 0.000 description 4
- 229910017052 cobalt Inorganic materials 0.000 description 4
- 239000010941 cobalt Substances 0.000 description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 230000035945 sensitivity Effects 0.000 description 4
- NTZRDKVFLPLTPU-UHFFFAOYSA-N CC[Na] Chemical compound CC[Na] NTZRDKVFLPLTPU-UHFFFAOYSA-N 0.000 description 3
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 239000013535 sea water Substances 0.000 description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 239000004280 Sodium formate Substances 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 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
- 150000001875 compounds Chemical class 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- NAGJZTKCGNOGPW-UHFFFAOYSA-N dithiophosphoric acid Chemical compound OP(O)(S)=S NAGJZTKCGNOGPW-UHFFFAOYSA-N 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 230000002068 genetic effect Effects 0.000 description 2
- 229910052732 germanium Inorganic materials 0.000 description 2
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 2
- 239000011630 iodine Substances 0.000 description 2
- 229910052740 iodine Inorganic materials 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 description 2
- 235000019254 sodium formate Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- -1 thio ammonia Chemical compound 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- IOEJYZSZYUROLN-UHFFFAOYSA-M Sodium diethyldithiocarbamate Chemical compound [Na+].CCN(CC)C([S-])=S IOEJYZSZYUROLN-UHFFFAOYSA-M 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 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
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910052733 gallium Inorganic materials 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
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-M iodide Chemical compound [I-] XMBWDFGMSWQBCA-UHFFFAOYSA-M 0.000 description 1
- 229940006461 iodide ion Drugs 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- UQJQVUOTMVCFHX-UHFFFAOYSA-L nabam Chemical compound [Na+].[Na+].[S-]C(=S)NCCNC([S-])=S UQJQVUOTMVCFHX-UHFFFAOYSA-L 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000012279 sodium borohydride 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
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- AALQBIFJJJPDHJ-UHFFFAOYSA-K trisodium;thiophosphate;dodecahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].[Na+].[O-]P([O-])([O-])=S AALQBIFJJJPDHJ-UHFFFAOYSA-K 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
Abstract
The invention discloses a kind of sample injection method occurred for atomic spectrograph gaseous state chelate, this method includes：The mixed solution, is then carried out the gas-liquid separation of element evaporation object by weakly acidic pH that is online or mixing element to be measured offline or basic sample solution solution and chelating reagent solution on a gas-liquid separator using carrier gas.The neutrality or basic sample solution solution of element wherein to be measured refer to solution ph between 6.0 10.5；Chelating reagent is preferably sodium diethyldithiocarbamate（Potassium or ammonium）, diethyldithioposphoric acid sodium（Potassium or ammonium）；The volume of mixed solution in the separator is 0.5 milliliter 3 milliliters.Compared with previous gas-liquid separation technology, the element chelate gas in the efficient Separation of Neutral of method energy or alkaline solution of the invention is particularly suitable for sample entering method when atomic spectroscopic analysis element.
Description
Technical field
The invention belongs to technical field of analytical chemistry, be especially for the generation of atomic spectrograph gaseous state chelate into
Quadrat method.
Background technology
Gas-liquid separation is widely used in the fields such as chemistry, biology and water process.Small-sized gas-liquid separator is in analysisization
Also there is extensive use, especially in atom spectrum on（ICP-AES、ICP-MS,AA,AFS）When gaseous state sample introduction, have very big
Application.In the application field, makes the element in sample to be tested and the reaction of some reagents by reacting online, generate element to be measured
Volatile matter, which has in the solution must solubility, it is therefore necessary to make volatile matter from molten by gas-liquid separation device
It separates and is measured in liquid.Online separation in this way, not only increases the sensitivity decrease of atomic spectroscopic analysis
Detection limit, and element to be measured is made to be detached well with the matrix in solution, reduce Matrix effects.
Currently, atomic spectrograph gaseous state sample introduction includes mainly following several technical methods：（1）Hydride generation method, or
It is chemical evapn genetic method.This method is that the acid solution of element to be measured is made to be reacted online with reducing agents such as sodium borohydrides, is generated
The hydride of element makes the hydride of generation be separated from the solution after reaction by gas-liquid separator, is acted in carrier gas
Lower volatile hydride, which is loaded into atom spectrum, to be measured；（2）Carbon dioxide genetic method, this method is will be in solution
Carbonate to be measured（Or bicarbonate）It mixes online or with inorganic acid offline, carbonate or bicarbonate is made to generate carbon dioxide,
Then the carbon dioxide of generation is made to separate from the solution after reaction by gas-liquid separator, the titanium dioxide under carrier gas effect
Carbon gas, which is loaded into atom spectrum, to be measured；（3）Chelate vapor generation, this is just to have been sent out by the present inventor recently
Sampling technique occurs for a kind of existing chemical evapn.This method be make the acid solution of element to be measured online with two thio ammonia of ethylenediamine
The chelating reagents such as base sodium formate react, and generate volatile element chelate, the volatile element of generation is made by gas-liquid separator
Chelate is separated from the solution after reaction, and volatile element chelate is loaded into atom spectrum under carrier gas effect
It is measured；（4）Other steam generation techniques：Including iodine vapor generation（It is online that iodide ion and nitrite anions is made to react
Generate iodine）；Carbonyl nickel vapor generation（It is online that nickel ion and sub- reaction of carbon monoxide is made to generate gaseous state carbonyl nickel）.
The presently used gas-liquid separator of these above-mentioned gaseous state sample injection methods has following several：
（1）Common gas-liquid separator, the separator is very simple, and the main mixed solution including after a reaction enters one
The separator of test tube shape, the separator bottom are passed through carrier gas, and after mixed solution enters the separator, carrier gas is first by volatility
Plain compound is separated by being intubated directly bubbling or non-bubbling mode in solution from solution, and atomic spectrograph is then downloaded to
It is measured.
（2）Use existing inductively coupled plasma spectrometry（Mass spectrum）Atomizer as gas-liquid separator, by
Mixed solution is sprayed in fog chamber, so that volatile element compound vapor is separated from solution, instrument is then downloaded to by carrier gas
It is measured in device.
（3）Solution bubbling is detached by sintered glass core filter plate, which is to make carrier gas from a sintered glass
Towards the solution on sintered glass core filter plate be bubbled under core filter plate and be detached, this method is imitated with good gas-liquid separation
Rate, but up to the present, influence of the aperture on sintered glass to separative efficiency is disclosed without any document or patent.Some
The method that document is introduced only proposes to be used for Bubble fractionation using the sintered glass, does not carry out any in-depth study and examine
It examines.Which limits the optimizations of gas-liquid separator.
As described above, several gas-liquid separating methods recited above and device, existing deficiency are：Separative efficiency is not high,
It is other other than the volatile matter that sodium borohydride and arsenic, mercury, lead, selenium, germanium, tellurium, bismuth, antimony, tin and cadmium reaction generate is easily separated
Online reaction-gaseous state separating effect be not very ideal.Therefore, sensitivity and the detection limit of gaseous state sample introduction are affected.
The present inventor invents a kind of new element gaseous state sampling technique, i.e., the sample introduction skill that volatility chelate generates recently
Art.The technical principle is to keep the acid solution of element to be measured anti-with the chelating reagents such as ethylenediamine nabam online
It answers, generates volatile element chelate, make the volatile element chelate of generation from the solution after reaction by gas-liquid separator
In separate, volatile element chelate is loaded into atom spectrum and is measured under carrier gas effect.Under study for action originally
Inventor has found：It is very good that the technology only can be only achieved when being detached to solution bubbling using sintered glass core filter plate
Effect.The present inventor has found again in further research：Only using aperture（Diameter）10-80 microns of sintered glass core
Filter plate could realize the present invention.Last the present inventor has studied the detailed of entire separator when reaching maximum separation efficiency in more detail
Carefully best separation method and device are configured and have obtained, by other steam generation techniques（Hydride occurs, carbon dioxide
Occur）Popularization, the inventors discovered that this method optimum efficiency having the same, has thus completed the present invention.
Invention content
A kind of sample injection method occurred for atomic spectrograph gaseous state chelate, this method include：Online or offline mixing
The weakly acidic pH or basic sample solution solution and chelating reagent solution of element to be measured, then by the mixed solution in a gas-liquid separator
On using carrier gas carry out element evaporation object gas-liquid separation.
The neutrality or basic sample solution solution of element wherein to be measured refer to solution ph between 6.0-10.5, preferable ph
Between 6.5-9, most preferred pH value between 6.5-8.0
Chelating reagent solution in the present invention refers to（But it is not limited to）Sodium diethyldithiocarbamate（Potassium or ammonium）, diethyl
Base phosphordithiic acid sodium（Potassium or ammonium）.
The volume of mixed solution in the separator in the present invention is 0.1 milliliter -10 milliliters, preferably 0.2 milliliter -5 milliliters,
Most preferably 0.5 milliliter -3 milliliters.
Element of the present invention refers to that can generate volatile element chelate with chelating reagent under weakly acidic pH or alkalinity
Element, these elements include（But it is not limited to）Lead, nickel, cobalt, cadmium, zinc, germanium, tin, bismuth, chromium, vanadium, gallium, indium, titanium, platinum, palladium etc..
Description of the drawings
Fig. 1 is the gas-liquid separation device for the present invention；Wherein：
1 gas-liquid separator shell；2 be sample and chelating reagent entry to mixed solution
3 be waste liquid outlet；4 are used for the bubbling porous plate of gas-liquid separation；
5 be carrier gas inlet；6 export for carrier gas.
Specific implementation mode
The present invention is described below by specific embodiment.Unless stated otherwise, technological means used in the present invention
It is method known in those skilled in the art.In addition, embodiment is interpreted as illustrative, it is not intended to limit the present invention
Range, the spirit and scope of the invention are limited only by the claims that follow.To those skilled in the art, without departing substantially from this
Under the premise of invention spirit and scope, the various changes or changes that carried out to the method and structure in these embodiments also belong to
Protection scope of the present invention.
Embodiment 1
By 1 milliliter of neutral seawater aqueous sample to be analyzed（pH=7.2）With 1 milliliter 0.4%（m/V）Diethyl-dithio ammonia
Base sodium formate（Chelating reagent, DDTC）After neutral aqueous solution mixing, mixed solution is injected into from sample feeding pipe in gas-liquid separator,
Start carrier gas（250 ml/min of inlet flow rate）, then carrier gas is sent to from gas-liquid separator outlet in atomic spectrograph and is surveyed
It is fixed.This method Accurate Determining Ni in Seawater, the element chelate of generation can divide with seawater matrix aqueous solution in neutral conditions
From.Sensitivity is not only increased, the interference of other elements is also eliminated.
Embodiment 2
Referring to Figure of description 1.Using peristaltic pump online with equal flow velocity（3 ml/mins）Mixing 0.4%（m/V）Diethyl
Base phosphordithiic acid sodium（Ethyl Sodium Aerofloat）Aqueous solution and the cadmium containing 2ppb neutral species solution (pH7.5), make mixed
Solution is entered from pipe 1 containing there are one the porous sintered fritillarines that aperture is 5-15 microns（30 millimeters of diameter, filter plate top are empty
Between height 3 centimetres）Gas-liquid separator in, sample injection time be 20 seconds, at this time without discharging of waste liquid.It is volatile in solution
The carrier gas that the chelate of cadmium and ethyl black powder is passed through below（Argon gas）The volatile matter of Bubble fractionation, carrier gas and cadmium is then entered
Atomic spectrograph is measured.Using the present apparatus, the volatilization efficiency of cadmium can be made close to 100%, atomic fluorescence of zero dispersion detection is limited to
0.1ppb.The single Bubble fractionation device of 80 traditional micron pore sizes is compared, the present apparatus makes the volatilization efficiency of cadmium improve 2 times, detection
Limit reduces by 3 times.Using this method, the solution after bubbling can carry out waste liquid row without being immediately disconnected after gas-liquid is kept completely separate
It puts.
Embodiment 3
By 1 milliliter of neutral aqueous solution sample to be analyzed（pH=7）With 1 milliliter 0.4%（m/V）Ethyl Sodium Aerofloat（Chelating reagent）
Mixed solution be injected into gas-liquid separator from sample feeding pipe, start carrier gas（250 ml/min of inlet flow rate）, then will carry
Gas is sent in atomic spectrograph from gas-liquid separator outlet and measures.This method can Accurate Determining lead in neutral conditions, generation
Element chelate can be detached with matrix aqueous solution.Sensitivity is not only increased, the interference of other elements is also eliminated.Carrier gas and lead
Volatile matter be then entered atomic spectrograph and be measured.Using the present apparatus, the volatilization efficiency of lead can be made to reach 20%, ICP-
The detection of AES is limited to 0.6ppb.
Embodiment 4
Referring to Figure of description 1.Successively extract the 0.4% of 1.5 milliliters in chronological order using plunger pump（m/V）Diethyl two
Sodium thiophosphate（Ethyl Sodium Aerofloat）Aqueous solution and 1.5 milliliters of cobalts containing 10ppb neutral species solution (pH7.5), then make
The mixed solution is entered from pipe 1 containing there are one the porous sintered fritillarines that aperture is 5-15 microns（30 millimeters of diameter, filter plate
3 centimetres of upper space height）Gas-liquid separator in, at this time without discharging of waste liquid.Volatile cobalt in solution and ethyl
The carrier gas that the chelate of black powder is passed through below（Argon gas）The volatile matter of Bubble fractionation, carrier gas and cobalt is then entered atom spectrum
Instrument is measured.Using the present apparatus, the volatilization efficiency of cobalt can be made close to 40%, atomic fluorescence of zero dispersion detection is limited to 0.14ppb.
The single Bubble fractionation device of 80 traditional micron pore sizes is compared, the present apparatus makes the volatilization efficiency of cadmium improve 2 times.Using this method,
Solution after bubbling can carry out discharging of waste liquid without being immediately disconnected after gas-liquid is kept completely separate.
Claims (4)
1. a kind of sample injection method occurred for atomic spectrograph gaseous state chelate, this method include：Online or offline mixing waits for
The weakly acidic pH or basic sample solution solution and chelating reagent solution of element are surveyed, then by 0.1-10 milliliters of the mixed solution in a gas
The gas-liquid separation of element evaporation object is carried out on liquid/gas separator using carrier gas or negative pressure；The neutrality or basic sample solution of element wherein to be measured
Solution refers to solution ph between 6.0-10.5；The chelating reagent refers to sodium diethyldithiocarbamate
（Potassium or ammonium）, diethyldithioposphoric acid sodium（Potassium or ammonium）.
2. the sample injection method described in claim 1 occurred for atomic spectrograph gaseous state chelate, it is characterised in that member to be measured
The neutrality or basic sample solution solution of element refer to solution ph between 6.5-9.
3. the sample injection method described in claim 1 occurred for atomic spectrograph gaseous state chelate, it is characterised in that member to be measured
The neutrality or basic sample solution solution of element refer to solution ph between 6.5-8.0
The sample injection method described in claim 1 occurred for atomic spectrograph gaseous state chelate, it is characterised in that mixed
The volume of solution in the separator is 0.2-5 milliliters.
4. the sample injection method described in claim 1 occurred for atomic spectrograph gaseous state chelate, it is characterised in that after mixing
Solution volume in the separator be 0.5 milliliter -3 milliliters.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810375925.2A CN108535185A (en) | 2018-04-25 | 2018-04-25 | A kind of sample injection method occurred for atomic spectrograph gaseous state chelate |
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|---|---|---|---|---|
| CN205263037U (en) * | 2015-12-25 | 2016-05-25 | 北京吉天仪器有限公司 | Element form on -line measuring device |
| CN106198391A (en) * | 2016-08-30 | 2016-12-07 | 天津师范大学 | A kind of method and device being measured element by Element generation volatile matter |
| CN106248593A (en) * | 2016-07-15 | 2016-12-21 | 天津师范大学 | A kind of method and apparatus of atom spectrometer sample feeding |
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| CN205263037U (en) * | 2015-12-25 | 2016-05-25 | 北京吉天仪器有限公司 | Element form on -line measuring device |
| CN106248593A (en) * | 2016-07-15 | 2016-12-21 | 天津师范大学 | A kind of method and apparatus of atom spectrometer sample feeding |
| CN106198391A (en) * | 2016-08-30 | 2016-12-07 | 天津师范大学 | A kind of method and device being measured element by Element generation volatile matter |
| CN107462569A (en) * | 2016-08-30 | 2017-12-12 | 天津师范大学 | A kind of method and device that element is determined by Element generation volatile matter |
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