CN108760435A - A kind of electrochemical appliance and purposes being used for preparing element hydride - Google Patents
A kind of electrochemical appliance and purposes being used for preparing element hydride Download PDFInfo
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- CN108760435A CN108760435A CN201810787646.7A CN201810787646A CN108760435A CN 108760435 A CN108760435 A CN 108760435A CN 201810787646 A CN201810787646 A CN 201810787646A CN 108760435 A CN108760435 A CN 108760435A
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- 150000004678 hydrides Chemical class 0.000 title claims abstract description 31
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 29
- 239000010439 graphite Substances 0.000 claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 230000002572 peristaltic effect Effects 0.000 claims abstract description 13
- 239000002699 waste material Substances 0.000 claims abstract description 11
- 238000009413 insulation Methods 0.000 claims abstract description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 24
- 239000000523 sample Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 9
- 239000012488 sample solution Substances 0.000 claims description 7
- 238000004458 analytical method Methods 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 5
- PWKSKIMOESPYIA-UHFFFAOYSA-N 2-acetamido-3-sulfanylpropanoic acid Chemical compound CC(=O)NC(CS)C(O)=O PWKSKIMOESPYIA-UHFFFAOYSA-N 0.000 claims description 3
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims 6
- 235000013878 L-cysteine Nutrition 0.000 claims 3
- 239000004201 L-cysteine Substances 0.000 claims 3
- 239000000470 constituent Substances 0.000 claims 2
- 238000007599 discharging Methods 0.000 claims 1
- 230000005518 electrochemistry Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 26
- 229910052785 arsenic Inorganic materials 0.000 description 9
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 9
- 238000005868 electrolysis reaction Methods 0.000 description 6
- 238000005070 sampling Methods 0.000 description 6
- 230000009102 absorption Effects 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000012279 sodium borohydride Substances 0.000 description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 230000007812 deficiency Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 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 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000012491 analyte Substances 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
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- 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
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
- G01N21/6404—Atomic fluorescence
Landscapes
- Physics & Mathematics (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)
- Optics & Photonics (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
A kind of electrochemical appliance and purposes being used for preparing element hydride.The invention discloses the electrochemistry preparation facilities and purposes of a kind of hydride.The device includes：Two are connected graphite tube cathode together and graphite tube anode with insulation tube, DC power supply, peristaltic pump, gas-liquid separator, sample to be analysed solution deposit bottle, waste liquid bottle.Wherein graphite tube cathode and graphite tube anode are separately connected gas-liquid separator and the deposit bottle of solution containing sample to be analysed；The positive and negative anodes of DC power supply are connected with the anode and cathode of graphite-pipe respectively.Waste liquid bottle is connected with the sewer pipe above gas-liquid separator.The device is simply easy to implement, and can be applied to the related field of analytical chemistry.
Description
Technical field
The invention belongs to element hydride preparing technical fields, more particularly to one kind is for certain elements inspections in analytical chemistry
The sampling device occurred by hydride when survey and purposes.
Background technology
The analysis worker that sample injection method has been vast occurs for hydrogenation, is especially engaged in the scientific research people of atomic spectroscopic analysis
Known to member.This method have very high sample introduction efficiency, not only have excellent analysis detection limit, can also carry out analyte with
The matrix of sample solution detaches, and reduces interference.However, since the technology generally uses sodium borohydride（Potassium）Reducing agent is made, therefore
Or there is some shortcomings：First, sodium borohydride reagent price is relatively high, keeps analysis cost also relatively high；Secondly, boron hydrogen
It is unstable in aqueous solution to change sodium, is easy to be water dispersible releasing hydrogen, keeps the stability of analytic process poor, which increase usage amounts
Increased analysis cost.In order to overcome disadvantage possessed by sodium borohydride, the hydrogen of nascent state is generated by electrolytic method to replace
The electrochemical hydride generation technique that sodium borohydride generates hydrogen in statu nascendi has been suggested.However existing scheme is shown at present,
This method still remains deficiency：Device is more complicated first, wherein the anode chamber and cathode chamber when electrolysis need to hand over using ion
It changes film to separate, and individual anolyte is needed to carry out anode electrolysis cycle；Secondly, it is needed in constant current when electrolysis
It is carried out under pattern, needs to use proprietary power supply.This just increases the cost of equipment.
Invention content
Against the above deficiency, the present inventor breaks through the forbidden zone of prior art in an experiment, is attempted using simple mechanism,
Therefore the present invention is completed.
It is used for preparing the electrochemical appliance of element hydride the invention discloses a kind of, it is characterised in that the device includes：
Two are connected graphite tube cathode 1 together and graphite tube anode 2 with insulation tube, DC power supply 4, peristaltic pump 5, gas-liquid separator 6,
Sample to be analysed solution lays in bottle 8, waste liquid bottle 9；Wherein graphite tube cathode 1 and graphite tube anode 2 is separately connected gas-liquid separator 6
Bottle 8 is laid in solution containing sample to be analysed；
The positive and negative anodes of DC power supply 4 are separately connected the cathode and anode for the electrolytic cell made with two graphite-pipes, two graphite-pipes
Between spacing be 0.5-2 centimetres, peristaltic pump 5 be used for extract sample to be analysed solution and discharge separation gas after waste liquid, give up
Liquid bottle 9 is connected with the sewer pipe above gas-liquid separator 6.
To be disposed vertically or slant setting after the series connection of two graphite-pipes in the present invention.The direct current to work under constant voltage mode
The operating voltage in source 3 lies prostrate for 6-30, and preferably 9-24 volts, more preferred operating voltage lies prostrate for 12-18.
The preferred high purity graphite of graphite-pipe of the present invention（99.9%）Manufactured graphite-pipe.The reality for facilitating acquisition as one
Example can directly use the coating in sampling Graphite Furnace Atomic Absorption without platform-graphite tube, including use the graphite furnace of used discarding former
The graphite-pipe that son absorbs.
The DC power supply to work under constant voltage mode can be the proprietary power supply that can carry out voltage adjusting, can also be to hand
Machine or the DC power source adapter that can be plugged on wall of laptop computer charging.It is emphasized that respectively as electricity in the present invention
The cathode of Xie Chi and the two of anode graphite-pipes, ordinal position do not specially require.Can cathode can also anode before
Preceding.But it is general to require to be preferably cathode preceding.Ie in solution from anode graphite pipe enter from cathode graphite-pipe out then into
Enter gas-liquid separator.
Sample to be analysed solution in the present invention is the acid solution containing thiocarbamide or L-cysteine, and the quality of thiocarbamide is dense
Degree is 0.5-2%.In addition, the sample solution to be analyzed in the present invention also contains acid, used acid preferably hydrochloric acid and sulfuric acid.
The molar concentration of acid is 0.5M -6M, preferably 1M -2M.The flow velocity of sample to be analysed solution is 0.5-5 ml/mins, excellent
Select 2.5-4 ml/mins.
The present invention further discloses the methods for preparing element hydride using the device, it is characterised in that：Use one
Input voltage 220-240 lies prostrate alternating current, and the DC voltage and electric current of output are respectively the DC power supply of 12-18 volt 0.5-2 peaces,
It is electrolysed to two graphite pipe electrodes, the solution 5-20ngml containing arsenic to be analyzed of peristaltic pump conveying-1, thiocarbamide 1-1.5%
（m/v）, hydrochloric acid or sulfuric acid concentration 1.2-2.5M, 3-4 milliliters of solution flow rate is per minute, in an atomic fluorescence of zero dispersion photometer
Upper measurement arsenic content.
The present invention further discloses prepare element hydride method to improve measurement element hydride content accuracy side
The application in face.Typical experimental result is shown：The measurement of arsenic content is due to easy to operate, easy implementation and signal stabilization, therefore
Than existing method accuracy higher.
The device of the invention mainly solves：
（1）Traditional electrochemical hydride generating means is complicated, needs in advance the use of processing ability finishing device meticulously.It uses
The present apparatus, any laboratory, anyone Fast Installation and can at once come into operation；
（2）The power supply that traditional electrochemical hydride uses is the proprietary DC power supply of constant current mode work, price ratio
It is higher；And the present invention need to only use the socket type charger of mobile phone or laptop computer, not only reduce cost, also make power supply more
It is easy to get.
（3）Two electrodes that traditional electrochemical hydride occurs, are substantially anode, Qi Tayou using noble metal platinum
Malicious poisonous metal lead cadmium etc. does cathode, not only makes electrolytic cell cost of manufacture very high in this way, but also cause environmental pollution.
（4）Traditional electrochemical hydride generating means, need using amberplex come separate anolyte and
Catholyte, two electrolyte need to prepare and carry out using more peristaltic pumps the extraction of solution respectively.And this hair
It is bright not need amberplex.Individual anolyte is not needed, therefore either electrolytic cell cost of manufacture is still wriggled yet
Pumping unit acquisition cost all substantially reduces.
（5）There are the interference of prodigious coexisting ion when Conventional electrochemical hydride measures, and the present invention does not interfere with.
（6）The efficiency and sensitivity that traditional electrochemical hydride occurs are unadjustable, and index is bad.
It is possessed positive compared with now with technology that volatile element chelate of the present invention generates sampling device
Effect is：
（1）Device is simply very easy to implement, and autonomous Fast Installation and actually detected answer can be put into any one laboratory
With.
（2）Operating cost is low, does not need expensive device materials not only（Film）Separation layer is done, your special gold is not needed yet
Belong to（Platinum）Electrode is done, does not need proprietary constant current mode power supply more.
（3）Strong antijamming capability：When authentic sample is analyzed, coexisting ion, especially transition element ion do not interfere with.
Description of the drawings：
Fig. 1 is the structural diagram of the present invention, wherein：
1- graphite tube cathodes；2- graphite tube anodes；The plastic union pipe of two graphite-pipes of 3-；
4. DC power supply；5- peristaltic pumps；6- gas-liquid separators；The connecting tube of 7- graphite-pipes and solution pipeline；8- sample to be analysed
Solution lays in bottle；9- waste liquids.
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 structure in these embodiments also belong to the present invention
Protection domain.
Embodiment 1
It is a kind of to be used for preparing the electrochemical appliance of element hydride, it is characterised in that the device includes：Two are connected with insulation tube
Graphite tube cathode 1 together and graphite tube anode 2, DC power supply 4, peristaltic pump 5, gas-liquid separator 6, the storage of sample to be analysed solution
Standby bottle 8, waste liquid bottle 9；Wherein graphite tube cathode and graphite tube anode is separately connected gas-liquid separator and solution containing sample to be analysed
Lay in bottle；The positive and negative anodes of DC power supply are separately connected the cathode and anode for the electrolytic cell made with two graphite-pipes, two graphite
Spacing between pipe is 1 centimetre, and peristaltic pump is used to extract the waste liquid after sample to be analysed solution and discharge separation gas, waste liquid bottle
It is connected with the sewer pipe above gas-liquid separator.
To be disposed vertically or slant setting after the series connection of two graphite-pipes.The work of the DC power supply to work under constant voltage mode
Voltage is 15 volts.Sample to be analysed solution is the acid solution containing thiocarbamide or L-cysteine, and the mass concentration of thiocarbamide is 1%.
In addition.Acid（Hydrochloric acid or sulfuric acid）Molar concentration be 2M.The flow velocity of sample to be analysed solution is 2.5 ml/mins.
Embodiment 2
A method of element hydride is prepared using the device：Alternating current is lied prostrate using an input voltage 220-240, output
DC voltage and electric current are respectively 2 peace of 12-18 volts, are electrolysed to two graphite pipe electrodes, peristaltic pump conveying
Solution 5ngml containing arsenic to be analyzed-1, thiocarbamide 1%（m/v）, concentration of hydrochloric acid 1.2M, 3 milliliters of per minute, gas-liquid separators of solution flow rate
In flow rate of carrier gas 400mlmin-1
Embodiment 3
Referring to Figure of description 1.Alternating current, the DC voltage and electric current point of output are lied prostrate using an input voltage 220-240
It Wei not pacify for 12 volt 2, the power supply adaptor for mobile phone charging.As shown in Figure 1, two graphite-pipe (sampling Graphite Furnace Atomic Absorptions are given
The graphite-pipe used blocks the aperture on former graphite-pipe.Catholyte pipe is on top, and anode electrolysis pipe is in lower part) electrode confession
Electricity is electrolysed.The solution 10ngml containing arsenic to be analyzed of peristaltic pump conveying-1, thiocarbamide 1%（m/v）, concentration of hydrochloric acid 1.2M, solution stream
3 milliliters of speed is per minute.The result that arsenic is measured on an atomic fluorescence of zero dispersion photometer is 9.810ngml-1.It can be seen that this method
Device has good accuracy.
Embodiment 4
Referring to Figure of description 1.Alternating current, the DC voltage and electric current point of output are lied prostrate using an input voltage 220-240
It Wei not pacify for 18 volt 2, the power supply adaptor for mobile phone charging.As shown in Figure 1, giving two graphite-pipes, (sampling Graphite Furnace Atomic Absorption makes
Graphite-pipe blocks the aperture on former graphite-pipe.Catholyte pipe is on top, and anode electrolysis pipe is in lower part) electrode power supply
It is electrolysed.The solution 20ngml containing antimony to be analyzed of peristaltic pump conveying-1, thiocarbamide 1%（m/v）, concentration of hydrochloric acid 2M, 4 milli of solution flow rate
Liter Per Minute.The result that arsenic is measured on an atomic fluorescence of zero dispersion photometer is 20.05ngml-1.It can be seen that party's subtraction unit
There is good accuracy.
Embodiment 5
Referring to Figure of description 1.Alternating current, the DC voltage and electric current point of output are lied prostrate using an input voltage 220-240
It Wei not pacify for 18 volt 2, the power supply adaptor for mobile phone charging.As shown in Figure 1, giving two graphite-pipes, (sampling Graphite Furnace Atomic Absorption makes
Graphite-pipe blocks the aperture on former graphite-pipe.Catholyte pipe is on top, and anode electrolysis pipe is in lower part) electrode power supply
It is electrolysed.The solution 5ngml containing arsenic to be analyzed of peristaltic pump conveying-1, thiocarbamide 1,5%（m/v）, sulfuric acid acid concentration 2.4M, solution stream
4 milliliters of speed is per minute.The result that arsenic is measured on an atomic fluorescence of zero dispersion photometer is 5.2ngml-1.It can be seen that this method fills
It is equipped with good accuracy.
Embodiment 6
Comparative test
Conclusion：The present invention is easy to carry out rapid processing in any one time and be measured.It is not only at low cost, but also runs
Simply.Strong antijamming capability simultaneously, accuracy are high.
Claims (9)
1. a kind of be used for preparing the electrochemical appliance of element hydride, it is characterised in that the device includes：Two with insulation tube string
The graphite tube cathode of connection together（1）With graphite tube anode（2）, DC power supply（4）, peristaltic pump（5）, gas-liquid separator（6）, wait for point
It analyses sample solution and lays in bottle（8）, waste liquid bottle（9）；
Wherein graphite tube cathode（1）With graphite tube anode（2）It is separately connected gas-liquid separator（6）It is stored up with solution containing sample to be analysed
Standby bottle（8）；DC power supply（4）Positive and negative anodes be separately connected the cathode and anode of the electrolytic cell made with two graphite-pipes, wriggle
Pump（5）For extracting sample to be analysed solution and discharging the waste liquid after detaching gas, waste liquid bottle（9）With gas-liquid separator（6）On
The sewer pipe in face is connected；Two graphite-pipes are disposed vertically after connecting or slant setting.
2. the electrochemical appliance according to claim 1 for being used for preparing element hydride, it is characterised in that in constant voltage mode
The operating voltage of the DC power supply of lower work lies prostrate for 6-30.
3. the electrochemical appliance according to claim 1 for being used for preparing element hydride, it is characterised in that in constant voltage mode
The operating voltage of the DC power supply of lower work lies prostrate for 12-18.
4. according to claim 1 be used for preparing the electrochemical appliance of element hydride, it is characterised in that described to wait for point
The sample to be analysed solution analysed in sample solution deposit bottle is the acid solution containing thiocarbamide or L-cysteine, wherein containing thiocarbamide
Or the mass concentration of L-cysteine is 0.5-4%.
5. according to claim 1 be used for preparing the electrochemical appliance of element hydride, it is characterised in that described to wait for point
Sample to be analysed solution in analysis sample solution deposit bottle is that the acidity of the molar concentration of the acid solution of L-cysteine is
0.2M—6M。
6. according to claim 1 be used for preparing the electrochemical appliance of element hydride, it is characterised in that described to wait for point
The flow velocity for analysing sample solution is 0.5-6 ml/mins.
7. according to claim 1 be used for preparing the electrochemical appliance of element hydride, it is characterised in that described to wait for point
The flow velocity for analysing sample solution is 2.5-4 ml/mins.
8. the method for preparing element hydride using device described in claim 1, it is characterised in that：Use an input voltage
220-240 lies prostrate alternating current, and the DC voltage and electric current of output are respectively the DC power supply of 6-30 volt 0.5-3 peaces, give two stones
Black pipe electrode is electrolysed, solution to be analyzed in addition to containing it is to be determined form the element of hydride other than, also add thiocarbamide
（Or L-cysteine）1-1.5%（m/v）, the hydrochloric acid or sulfuric acid of a concentration of 1.2-2.5M, 3-4 milliliters of solution flow rate is per minute,
The constituent content of hydride can be formed by being measured on one atomic fluorescence of zero dispersion photometer.
9. preparing element hydride method answering in terms of the constituent content for quickly measuring hydride using according to any one of claims 8
With.
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| CN201810787646.7A CN108760435A (en) | 2018-07-18 | 2018-07-18 | A kind of electrochemical appliance and purposes being used for preparing element hydride |
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| US20110272290A1 (en) * | 2010-04-02 | 2011-11-10 | Dasgupta Purnendu K | Systems and methods for electrochemical analysis of arsenic |
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| US20140076740A1 (en) * | 2012-09-17 | 2014-03-20 | Blue Planet Strategies, L.L.C. | Apparatus and method for electrochemical modification of liquids |
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| CN105092763A (en) * | 2015-08-26 | 2015-11-25 | 北京市理化分析测试中心 | Electrochemical pre-reduction method and device for mercury speciation analysis by HPLC-AFS (high performance liquid chromatography and atomic fluorescence spectroscopy) |
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2018
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