CN106680226A - Gas-liquid separation method and device for gas-state sample introduction of atomic spectrograph - Google Patents
Gas-liquid separation method and device for gas-state sample introduction of atomic spectrograph Download PDFInfo
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- CN106680226A CN106680226A CN201710029901.7A CN201710029901A CN106680226A CN 106680226 A CN106680226 A CN 106680226A CN 201710029901 A CN201710029901 A CN 201710029901A CN 106680226 A CN106680226 A CN 106680226A
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- 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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- G—PHYSICS
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- 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
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Abstract
The invention discloses a gas-liquid separation method and device for gas-state sample introduction of an atomic spectrograph. The method comprises the steps of mixing a sample solution and a reaction agent solution online, dropwise adding the mixed solution into a filter plate with micropores from a mixed solution entering pipe, bubble separating volatile matters in the solution by virtue of argon introduced from the lower part of the filter plate, and simultaneously and immediately blowing the separated volatile matters and the solution by carried air flow into a second gas-liquid separator in which the solution is settled to the bottom and discharged, but carrier gas and the volatile matters are introduced into the atomic spectrograph for determination. Compared with existing gas-liquid separation techniques, the device can be used for efficiently separating dissolved gas in the solution and is particularly applicable to gas-state sample introduction techniques in atomic spectrums.
Description
Technical field
The invention belongs to technical field of analytical chemistry, more particularly, to a kind of gas-liquid for atomic spectrograph gaseous state sample introduction
Separation method and device.
Background technology
Gas-liquid separation is widely used in the fields such as chemistry, biological and water process.Small-sized gas-liquid separator is in analysisization
Also tool is widely used on, particularly in atomic spectrum（ICP-AES、ICP-MS,AA,AFS）During gaseous state sample introduction, with very big
Application.Reacted by making element and some reagents in testing sample close very much online, generate the volatile matter of element to be measured,
The volatile matter has in the solution must dissolubility, it is therefore necessary to volatile matter is isolated from solution by gas-liquid separation device
To be measured.By such ON-LINE SEPARATION, the sensitivity decrease detection limit of atomic spectroscopic analysis is not only increased, and
Also element to be measured is separated well with the matrix in solution, reduce matrix interference.
At present, atomic spectrograph gaseous state sample introduction mainly includes following several technical methods：（1）Hydride generation method, or
It is chemical evapn genetic method.The method be make the acid solution of element to be measured online with the reducing agent reaction such as sodium borohydride, generate
The hydride of element, makes the hydride of generation separate from reacted solution by gas-liquid separator, in carrier gas effect
Lower volatile hydride is loaded in atomic spectrum and is measured；（2）Carbon dioxide genetic method, the method is by solution
Carbonate to be measured（Or bicarbonate）Mix online or offline with mineral acid, make carbonate or bicarbonate generate carbon dioxide,
Then the carbon dioxide that generation is made by gas-liquid separator is separated from reacted solution, the titanium dioxide under carrier gas effect
Carbon gas is loaded in atomic spectrum and is measured；（3）Chelate vapor generation, this is just to be sent out by the present inventor recently
There is sampling technique in a kind of existing chemical evapn.The method be make the acid solution of element to be measured online with ethylenediamine dithio ammonia
Base sodium formate etc. chelates reagent reacting, generates volatile element chelate, and by gas-liquid separator the volatile element of generation is made
Chelate is separated from reacted solution, and volatile element chelate is loaded in atomic spectrum under carrier gas effect
It is measured；（4）Other steam generation techniques：Including iodine vapor generation（Iodide ion and nitrite anions reaction are made online
Generate iodine）；Nickel tetracarbonyl. vapor generation（Nickel ion and sub- reaction of carbon monoxide is set to generate gaseous state Nickel tetracarbonyl. online）.
The presently used gas-liquid separator of above-mentioned these gaseous state sample injection methods has following several：
（1）Common gas-liquid separator, the separator is very simple, mainly enters into one including a reacted mixed solution
The separator of test tube shape, the separator bottom is passed through carrier gas, and after mixed solution enters into the separator, carrier gas is first by volatility
Plain compound is separated by the direct bubbling of intubation in solution or non-bubbling mode from solution, is then downloaded to atomic spectrograph
It is determined.
（2）Using existing inductively coupled plasma spectrometry（Mass spectrum）Nebulizer as gas-liquid separator, by
Mixed solution is sprayed in fog chamber, volatile element compound vapor is separated from solution, then instrument is downloaded to by carrier gas
It is measured in device.
（3）Solution bubbling is separated by sintered glass core filter plate, the technology is to make carrier gas from a sintered glass
Bubbling is carried out under core filter plate towards the solution on sintered glass core filter plate to be separated, there is the method good gas-liquid separation to imitate
Rate, but up to the present, without any document or patent impact of the aperture on sintered glass to separation efficiency is disclosed.Some
The method that document is introduced simply proposes to be used for Bubble fractionation using the sintered glass, does not carry out any in-depth study and examines
Examine.Which limits the optimization of gas-liquid separator.
As described above, several gas-liquid separating methods recited above and device, the deficiency for existing is：Separation efficiency is not high,
In addition to the volatile matter that sodium borohydride and arsenic, hydrargyrum, lead, selenium, germanium, tellurium, bismuth, antimony, stannum and cadmium reaction are generated is easily separated, other
Online reaction-gaseous state separating effect be not very good.Therefore, have impact on sensitivity and the detection limit of gaseous state sample introduction.
The present inventor invents recently the sample introduction skill that a kind of new element gaseous state sampling technique, i.e. volatility chelate are generated
Art.The know-why is to make the acid solution of element to be measured anti-with the chelating reagent such as ethylenediamine nabam online
Should, volatile element chelate is generated, by gas-liquid separator the volatile element chelate of generation is made from reacted solution
In separate, carrier gas effect under volatile element chelate be loaded into atomic spectrum in be measured.Under study for action originally
Inventor has found：The technology only can be only achieved very good when being separated to solution bubbling using sintered glass core filter plate
Effect.The present inventor has found again in further research：Only using aperture（Diameter）The sintered glass core of 10-80 microns
Filter plate could realize the present invention.Last the present inventor have studied in more detail the detailed of whole separator when reaching maximum separation efficiency
Optimal separation method and device is carefully configured and has drawn, by other steam generation techniques（Hydride occurs, carbon dioxide
Occur）Popularization, the inventors discovered that the device has identical optimum efficiency in these gas-liquid separations, this completes this
Invention.
The content of the invention
A kind of gas-liquid separating method of atomic spectrograph gaseous state sample introduction, it is characterised in that：On-line mixing element to be measured and anti-
Reagent solution is answered, mixed solution is entered on porous filter plate from mixed solution into pipe, volatile material in solution
The bubbling argon being passed through below by filter plate is separated, while the volatile matter isolated and solution are again immediately by one or two strands of carrier gas streams
Purging enters into the second gas-liquid separator, and here solution is deposited to bottom and is discharged, and carrier gas and volatile material are then entered
Enter to atomic spectrograph and be measured.Described carrier gas is generally consistent with the carrier gas that concrete instrument is used, and does not specify.
Pore diameter of the pore diameter on screen plate described in the present invention on 2-40 microns, particularly preferred screen plate exists
5-15 microns.
Screen plate upper space maximum height 0.2-3 centimetre of the present invention, preferred screen plate upper space is maximum high
0.5-1 centimetre of degree.
It is of the present invention that the volatile matter separated in first gas-liquid separator and solution are purged to into the second gas-liquid point
From device, it is possible to use one or two strands of air-flows are realizing：（1）When volatile matter and solution purging are entered into the using one carrier gas stream
During two gas-liquid separators, now this strand of carrier gas stream is passed through from filter plate bottom, and it plays Bubble fractionation and purging volatile matter and molten simultaneously
Liquid is acted on into the second gas-liquid separator.Now solution upper space arranges best（But it is not limited to）It is the shape of Figure of description 2
Shape；（2）When volatile matter and solution purging are entered into the second gas-liquid separator using two strands of stock carrier gas streams, now except under filter plate
Outside the bubbling carrier gas stream that face is passed through, there is one laterally purging carrier gas stream in the side on filter plate top, now solution upper space
It is best（But it is not limited to）It is arranged to the shape of Figure of description 1.
Device in the present invention is communicated by left and right（A）, (B) two gas-liquid separators constitute, it is main to include that mixing is molten
Liquid enters pipe（1）, micropore bubbling screen plate（2）, carrier gas inlet pipe（3）, carrier gas outlet（5）, discharging of waste liquid pipe after separation
（6）, wherein mixed solution is entered from mixed solution managing（1）Enter into micropore bubbling screen plate（2）On, volatility in solution
Material is by the first gas-liquid separator（A）The bubbling argon being passed through from below filter plate is separated, while the volatile matter isolated and solution
Again the second gas-liquid separator is entered into by carrier gas purge（B）, here solution be deposited to bottom from discharging of waste liquid pipe（6）Discharge,
And carrier gas and element evaporation thing then pass through the second gas-liquid separator（B）The carrier gas outlet of upper end（5）Enter into atomic spectrograph to enter
Row is determined.
In order to increase gas-liquid separation efficiency, in the side on filter plate top one laterally purging carrier gas can also be in addition applied with
（Argon）Stream（4）.
First gas-liquid separator in the present invention（A）In mixed solution enter pipe（1）Cling to micropore bubbling screen plate（2）
On, Deca solution is primarily used to, in the first gas-liquid separator（A）Middle micropore bubbling screen plate（2）Upper space is highly
0.5-1 centimetre.
What left and right of the present invention communicated（A）, (B) two gas-liquid separators material be preferably transparent glass or high score
Sub- polymer, the material of micropore bubbling screen plate is the sintered glass with fine pore likely or polymeric film.
The rotary spray chamber used in the preferred plasma emission spectroscopy of the second gas-liquid separator or Scott mists in the present invention
Room.
The present invention is had for the gas-liquid separating method and device of atomic spectrograph gaseous state sample introduction compared with now with technology
Some good effects are：
（1）Gas liquid interfacial area can be made using diameter in 5-15 micrometer Millipore bubbling screen plates in 2-40 microns, particularly diameter
Than larger, element evaporation thing is by detached efficiency high.
（2）Connecting second gas-liquid separator by the first gas-liquid separator, solution and volatile matter is all purged
To in second gas-liquid separator, this ensures that there solution and do not led to the thin pneumatic floating of coming below filter plate on microwell plate
Stop, it is ensured that not dissolving or the decomposition again of element evaporation thing, separation efficiency can be higher.
Description of the drawings：
Fig. 1 is for the gas-liquid separation device of atomic spectrograph gaseous state sample introduction；
Fig. 2 is the gas-liquid separation device another kind device for atomic spectrograph gaseous state sample introduction；
Wherein gas-liquid separators of A. first：
1. mixed solution enters pipe；2. micropore bubbling screen plate；
3. carrier gas inlet pipe；4. side carrier gas purge inlet tube；
B. the second gas-liquid separator：
5. carrier gas outlet；6. the discharging of waste liquid pipe after separating.
Specific embodiment
Below by the specific embodiment narration present invention.Unless stated otherwise, technological means used in the present invention
It is method known in those skilled in the art.In addition, embodiment be interpreted as it is illustrative, and it is unrestricted the present invention
Scope, 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
On the premise of invention spirit and scope, various changes that the material component and consumption in these embodiments is carried out or change
Belong to protection scope of the present invention.
Embodiment 1
Referring to Figure of description 1.A kind of gas-liquid separating method for atomic spectrograph gaseous state sample introduction：Mixed online using peristaltic pump
After closing sample solution and reaction reagent solution, mixed solution is entered into into porous polymer membrane filtration from mixed solution into pipe
On plate, the pore diameter on filter plate is in 5-10 microns, 1.5 centimetres of screen plate upper space height, volatile material in solution
The bubbling argon being passed through below is separated, while the volatile matter isolated and solution are again by the load gas flow purging of porous filter plate side
The second gas-liquid separator is entered into, here solution is deposited to bottom and is discharged, and carrier gas and volatile material are then entered
Atomic spectrograph is measured.
Embodiment 2
Referring to Figure of description 2.For the gas-liquid separation device of atomic spectrograph gaseous state sample introduction, it is characterised in that the device be by
What left and right communicated（A）, (B) two gas-liquid separators constitute, mainly include mixed solution enter pipe 1, micropore bubbling screen plate 2,
Discharging of waste liquid pipe 6 after carrier gas inlet pipe 3, carrier gas outlet 5, separation, wherein mixed solution enters from mixed solution into pipe
Enter on micropore bubbling screen plate, volatile material is by the first gas-liquid separator in solution（A）The bubbling argon being passed through is separated, together
When the volatile matter isolated and solution and be purged into into the second gas-liquid separator by the carrier gas purge entrance pipe flow（B）, at this
In solution be deposited to bottom and discharge from discharging of waste liquid pipe 6, and carrier gas and element evaporation thing then pass through the second gas-liquid separator（B）On
The carrier gas outlet at end enters into atomic spectrograph and is measured.
Embodiment 3
Referring to Figure of description 2.Using peristaltic pump online with the ethylenediamine aminodithioformic acid of equal flow velocity mixing 0.4%
Sodium（Na-DDTC）With the sample solution (sample acidity 0.075M of zinc) containing 2ppb zinc, mixed solution is set to enter into from pipe 1
One aperture is the porous sintered fritillarine of 5-15 microns（30 millimeters of diameter, 2 centimetres of filter plate upper space height）On, solution
In the carrier gas that is passed through below at once of volatile zinc-DDTC（Argon）Bubble fractionation, while the volatile matter isolated and molten
Liquid enters into the second gas-liquid separator by the carrier gas stream purging again, and here solution is deposited to bottom and is discharged, and carrier gas and zinc
Volatile matter be then entered atomic spectrograph and be measured.Using this device, the volatilization efficiency that can make zinc reaches 95%, colourless
Scattered atomic fluorescence detection is limited to 0.2ppb.Contrast only has the single Bubble fractionation device of 80 micron pore sizes, and this device makes the volatilization of zinc
Efficiency improves 5 times, and detection limit reduces by 2 times.
Embodiment 4
Referring to Figure of description 2.Using peristaltic pump online with the sodium borohydride of equal flow velocity mixing 1.2% and containing 2ppb cadmiums
Sample solution（Cadmium sample acidity 0.05M）, make mixed solution that the porous high score that aperture is 10 microns is entered into from pipe 1
Sub- membrane filtration plate（35 millimeters of diameter, 3 centimetres of filter plate upper space height）On, the hydride of the volatile cadmium in solution at once by
The carrier gas being passed through below（Argon）Bubble fractionation, while the volatile matter and solution of the cadmium isolated are purged into by this strand of carrier gas stream again
Enter to the second gas-liquid separator, here solution is deposited to bottom and is discharged, and the volatile hydride of carrier gas and cadmium is then entered
Enter to atomic spectrograph and be measured.Using this device, the volatilization efficiency that can make cadmium reaches 80%, and the detection of Atomic Absorption is limited to
0.1ppb.The single Bubble fractionation device of 80 traditional micron pore sizes of contrast, this device makes the volatilization efficiency of zinc improve 3 times, detection
Limit reduces by 1 times.
Embodiment 5
Referring to Figure of description 1.Using peristaltic pump online with the hydrochloric acid of equal flow velocity mixing 2% and the carbonate containing 5ppm
Sample solution, makes mixed solution that the porous sintered fritillarine that aperture is 15 microns is entered into from pipe 1（The milli of diameter 30
Rice, 1 centimetre of filter plate upper space height）On, the carrier gas that the volatile carbon dioxide in solution is passed through below at once（Argon
Gas）Bubble fractionation, while the volatile matter isolated and solution enter into the second gas by the carrier gas stream purging of porous filter plate side again
Liquid/gas separator, here solution is deposited to bottom and is discharged, and carrier gas and carbon dioxide are then entered atomic spectrograph and carry out
Determine.Using this device, DIC volatilization efficiency can be made to reach 98%, ICP-AES detections and to be limited to 15ppb.The traditional ICP- of contrast
AES is atomized separator, and this device makes the volatilization efficiency of DIC improve 1.5 times, and detection limit reduces by 2 times.
Claims (10)
1. a kind of gas-liquid separating method for atomic spectrograph gaseous state sample introduction, it is characterised in that：On-line mixing element to be measured and
Reaction reagent solution, mixed solution is entered on porous filter plate from mixed solution into pipe, volatile thing in solution
The bubbling argon that matter is passed through below by filter plate is separated, while the volatile matter isolated and solution are again immediately by one or two bursts of carrier gas
Stream purging enter into the second gas-liquid separator, here solution is deposited to bottom and is discharged, and carrier gas and volatile material then by
Enter into atomic spectrograph to be measured.
2. the gas-liquid separating method described in claim 1, it is characterised in that the pore diameter on screen plate is in 2-40 microns.
3. the gas-liquid separating method described in claim 1, it is characterised in that the pore diameter on screen plate is in 5-15 microns.
4. the gas-liquid separating method described in claim 1, it is characterised in that screen plate upper space maximum height 0.2-3 centimetre.
5. the gas-liquid separating method described in claim 1, it is characterised in that screen plate upper space maximum height 0.5-1 centimetre.
6. the gas-liquid separating method described in claim 1, it is characterised in that when being blown volatile matter and solution using one carrier gas stream
When sweeping into into the second gas-liquid separator, now this strand of carrier gas stream is passed through from filter plate bottom, while playing Bubble fractionation and purging volatilization
Thing and solution are acted on into the second gas-liquid separator.
7. the gas-liquid separating method described in claim 1, it is characterised in that when being blown volatile matter and solution using two strands of carrier gas streams
When sweeping into into the second gas-liquid separator, now except in addition to the bubbling carrier gas stream being passed through below filter plate, filter plate top side also
There is one laterally purging carrier gas stream.
8. a kind of gas-liquid separation device for atomic spectrograph gaseous state sample introduction, it is characterised in that the device is communicated by left and right
（A）, (B) two gas-liquid separators constitute, mainly include that mixed solution enters pipe（1）, micropore bubbling screen plate（2）, carrier gas enters
Mouth pipe（3）, carrier gas outlet（5）, discharging of waste liquid pipe after separation（6）, wherein mixed solution is entered from mixed solution managing（1）
Enter into micropore bubbling screen plate（2）On, volatile material is by the first gas-liquid separator in solution（A）It is passed through from below filter plate
Bubbling argon is separated, while the volatile matter isolated and solution enter into the second gas-liquid separator by carrier gas purge again（B）, at this
In solution be deposited to bottom from discharging of waste liquid pipe（6）Discharge, and carrier gas and element evaporation thing then pass through the second gas-liquid separator（B）
The carrier gas outlet of upper end（5）Enter into atomic spectrograph to be measured.
9. the gas-liquid separation device for atomic spectrograph gaseous state sample introduction according to claim 8, it is characterised in that in order to
Increase gas-liquid separation efficiency, also have one laterally purging carrier gas stream in the side on filter plate top（4）.
10. the gas-liquid separation device for atomic spectrograph gaseous state sample introduction according to claim 8, it is characterised in that first
Gas-liquid separator（A）In mixed solution enter pipe（1）Cling to micropore bubbling screen plate（2）On, it is primarily used to Deca molten
Liquid, in the first gas-liquid separator（A）Middle micropore bubbling screen plate（2）Upper space is highly 0.5-1 centimetre.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710029901.7A CN106680226B (en) | 2017-01-17 | 2017-01-17 | A kind of gas-liquid separating method and device for atomic spectrograph gaseous state sample introduction |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710029901.7A CN106680226B (en) | 2017-01-17 | 2017-01-17 | A kind of gas-liquid separating method and device for atomic spectrograph gaseous state sample introduction |
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| CN106680226A true CN106680226A (en) | 2017-05-17 |
| CN106680226B CN106680226B (en) | 2019-07-09 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109425720A (en) * | 2017-08-24 | 2019-03-05 | 上海利元环保检测技术有限公司 | A kind of Mercury in Soil residue detection equipment |
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| JPH02240538A (en) * | 1989-03-14 | 1990-09-25 | Fuji Electric Co Ltd | Analysis apparatus for ozone in solution |
| CN1979129A (en) * | 2005-12-03 | 2007-06-13 | 厦门搏傲科技有限公司 | Integrated chemical gas-phase generating apparatus |
| CN201732060U (en) * | 2010-05-25 | 2011-02-02 | 王伟 | Gas-liquid separator for atomic fluorescence spectroscopy |
| 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 |
| CN206114528U (en) * | 2016-10-27 | 2017-04-19 | 北京宝德仪器有限公司 | Atomic fluorescence spectrograph |
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2017
- 2017-01-17 CN CN201710029901.7A patent/CN106680226B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02240538A (en) * | 1989-03-14 | 1990-09-25 | Fuji Electric Co Ltd | Analysis apparatus for ozone in solution |
| CN1979129A (en) * | 2005-12-03 | 2007-06-13 | 厦门搏傲科技有限公司 | Integrated chemical gas-phase generating apparatus |
| CN201732060U (en) * | 2010-05-25 | 2011-02-02 | 王伟 | Gas-liquid separator for atomic fluorescence spectroscopy |
| 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 |
| CN206114528U (en) * | 2016-10-27 | 2017-04-19 | 北京宝德仪器有限公司 | Atomic fluorescence spectrograph |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109425720A (en) * | 2017-08-24 | 2019-03-05 | 上海利元环保检测技术有限公司 | A kind of Mercury in Soil residue detection equipment |
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