CN100590066C - Method and device for extracting combined hydrogen phosphide - Google Patents
Method and device for extracting combined hydrogen phosphide Download PDFInfo
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- CN100590066C CN100590066C CN200810023259A CN200810023259A CN100590066C CN 100590066 C CN100590066 C CN 100590066C CN 200810023259 A CN200810023259 A CN 200810023259A CN 200810023259 A CN200810023259 A CN 200810023259A CN 100590066 C CN100590066 C CN 100590066C
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- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000007789 gas Substances 0.000 claims abstract description 50
- 238000012360 testing method Methods 0.000 claims abstract description 34
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- 239000007787 solid Substances 0.000 claims abstract description 14
- 238000000605 extraction Methods 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 7
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000003513 alkali Substances 0.000 claims abstract description 5
- 230000008569 process Effects 0.000 claims abstract description 4
- 239000001257 hydrogen Substances 0.000 claims description 35
- 229910052739 hydrogen Inorganic materials 0.000 claims description 34
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 7
- 230000029087 digestion Effects 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 239000000284 extract Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000006073 displacement reaction Methods 0.000 claims description 3
- 150000002431 hydrogen Chemical class 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 230000005855 radiation Effects 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 229910000073 phosphorus hydride Inorganic materials 0.000 abstract description 10
- 238000001514 detection method Methods 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 4
- 229910000037 hydrogen sulfide Inorganic materials 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 150000007513 acids Chemical class 0.000 abstract 2
- 238000012544 monitoring process Methods 0.000 abstract 1
- 239000012808 vapor phase Substances 0.000 abstract 1
- 238000005259 measurement Methods 0.000 description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 229910052698 phosphorus Inorganic materials 0.000 description 5
- 239000011574 phosphorus Substances 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000004737 colorimetric analysis Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000005374 membrane filtration Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000003822 preparative gas chromatography Methods 0.000 description 2
- 238000012207 quantitative assay Methods 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000000207 volumetry Methods 0.000 description 2
- 206010012735 Diarrhoea Diseases 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 206010037423 Pulmonary oedema Diseases 0.000 description 1
- 208000010513 Stupor Diseases 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- RCTYPNKXASFOBE-UHFFFAOYSA-M chloromercury Chemical compound [Hg]Cl RCTYPNKXASFOBE-UHFFFAOYSA-M 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 210000003608 fece Anatomy 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- JGJLWPGRMCADHB-UHFFFAOYSA-N hypobromite Inorganic materials Br[O-] JGJLWPGRMCADHB-UHFFFAOYSA-N 0.000 description 1
- 229910052816 inorganic phosphate Inorganic materials 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 206010025482 malaise Diseases 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 208000005333 pulmonary edema Diseases 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- -1 settling Substances 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000008673 vomiting Effects 0.000 description 1
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Abstract
The invention discloses a method and a device for extracting binding state phosphine, belonging to the environmental monitoring technical field. The device of the invention comprises a gas sample collector, wherein the gas sample collector is connected with a preabsorption tube the other end of which is connected with a lightproof closed test tube, one end of which is communicated with another lightproof closed test tube and the other end of which is connected with an injector; steps of the extraction method are as follows: samples are collected; samples to be tested are counteracted in an anaerobic lightproof closed system by acids or alkali liquors; gases counteracted are preabsorbed by solid sodium hydroxide powders so as to remove acid gases and vapors generated in the process of counteraction; the phosphine content of gas samples counteracted is measured by the secondary online cold trap quick enrichment fitting vapor-phase chromatography-NPD method. The detection sensitivity of phosphine is high and the detection limit is as low as 0.01pg, thereby the method is applied to the detection of binding state phosphine gases in different environmental samples. While counteraction isperformed by acids, the method is also applied to the detection of reducing gases such as sulfureted hydrogen and methane, etc.
Description
Technical field
The present invention relates to the extracting method and the device of trace combined hydrogen phosphide gas in a kind of physical environment.
Background technology
In the biomass geochemistry circulation of phosphorus, think always that for a long time gaseous state phosphuret-(t)ed hydrogen is non-existent at nature.Up to 1988, the investigator found that first the phosphorus of sewage work's loss is to enter atmospheric with gaseous state phosphuret-(t)ed hydrogen form.Subsequently, in refuse landfill, plant, river and organism, detected the phosphuret-(t)ed hydrogen that exists with the free state form successively, along with phosphuret-(t)ed hydrogen is detected in varying environment one after another, phosphuret-(t)ed hydrogen finally is confirmed to be a kind of trace gas that extensively is present in the atmosphere.The discovery of phosphuret-(t)ed hydrogen is the important supplement to the phosphorus Cyclical Theory in the physical environment, has changed the phosphorus of thinking in the past in the atmosphere and is by attached to the incorrect view that inorganic phosphate constituted on air participates or the depositing dust particle.Therefore, in the biomass geochemistry circulation of phosphorus, must consider existence and the status and the effect of phosphuret-(t)ed hydrogen.Because phosphuret-(t)ed hydrogen content is very little in the physical environment, be subjected to condition effect such as sample collecting, preservation, enrichment and detection technique, early stage analytical procedure and technique means are difficult to realize the quantitative assay to trace phosphuret-(t)ed hydrogen in the environment, and the research of phosphuret-(t)ed hydrogen behavior is not also extensively carried out in the relevant environment.
Phosphuret-(t)ed hydrogen is a kind of poisonous and active reducing gas that can be carcinogenic, human body suck just can cause on a small quantity feeling sick, symptoms such as vomiting, uncomfortable in chest, diarrhoea, can cause pulmonary edema even stupor dead when serious.So the discovery of this compound in environment causes people's common concern at once, setting up sensitive reliable analytical method is the prerequisite of carrying out phosphuret-(t)ed hydrogen research in the environment.The analytical procedure that phosphuret-(t)ed hydrogen is commonly used has colorimetry, volumetry and vapor-phase chromatography.Colorimetry is that phosphuret-(t)ed hydrogen is oxidized to behind the phosphoric acid salt by spectrphotometric method for measuring, oxygenant commonly used has the vitriol oil, concentrated nitric acid, potassium permanganate and dense bromine water, volumetry is to utilize the irreversible reaction of phosphuret-(t)ed hydrogen and Silver Nitrate or mercury chloride to carry out, the major defect of these two kinds of methods is can not be qualitative, detect limit for height (mg level), thereby can not be used for the detection of physical environment trace phosphuret-(t)ed hydrogen (ng～pg level).Conventional vapor-phase chromatography does not also reach carries out quantitative requirement to trace phosphuret-(t)ed hydrogen in the environment, the online cold-trap fast enriching of improved secondary cooperates gas-chromatography-NPD method, realized the accurately measurement fast of trace phosphine gas in the environment, make the detectability of phosphuret-(t)ed hydrogen reduce to 0.01pg, applicable to the mensuration of phosphuret-(t)ed hydrogen in the physical environment.
Phosphuret-(t)ed hydrogen in the environment removes small portion and is present in the gaseous environment with free gaseous state (free-gaseous phosphine) form, and this part phosphine gas can directly be used improved gas chromatography determination; Most of phosphuret-(t)ed hydrogen exists (ocean and harbour settling in the fine and close environmental sample with matrix combined (matrix-bound phosphine) form, sewage plant sludge, human and animal excreta, Suspended Particles in Water etc.), this part combined hydrogen phosphide be in the environment free phosphuret-(t)ed hydrogen accumulate the storehouse, it is the important place of the generation mechanism and the migration transformation rule thereof of research phosphuret-(t)ed hydrogen, but combined hydrogen phosphide is owing to combine closely with sample, must adopt suitable extracting method to transfer in the gas phase, just can be with gas-chromatography to its qualitative, quantitative, and the solution that existing literature proposes this.
Summary of the invention
1. invent the technical problem that will solve:
Be difficult to extract combined hydrogen phosphide at prior art, the invention provides a kind of extracting method and device of combined hydrogen phosphide, can extract the combined hydrogen phosphide gas in the environmental sample, take the online cold-trap enrichment of secondary to cooperate gas-chromatography-NPD method again, realize quantitative assay combined hydrogen phosphide in the environment.
2. technical scheme
Principle of the present invention:
In homemade anaerobism lucifuge system, clear up fine and close sample (soil, settling, mud, water sample, organism or its movement etc.), clear up the back extracting gases sample that finishes, be stored in to gas do not absorb and the lucifuge airbag that adsorbs in, adopt the online cold-trap enrichment of secondary to cooperate gas-chromatography-NPD method to measure the gaseous sample of clearing up subsequently, the response signal that reads nitrogen phosphorous detector is integration in addition, according to integral area, typical curve equation by phosphuret-(t)ed hydrogen content in the integral area set up and the sample introduction gas, calculate the total amount of phosphuret-(t)ed hydrogen in the sample introduction gas, according to the amount of clearing up sample, calculate the combined hydrogen phosphide concentration in the testing sample.
Technical scheme of the present invention:
A kind of extraction element of combined hydrogen phosphide, comprise gas sampler, gas sampler and preabsorption pipe coupling, the other end of preabsorption pipe connect the airtight test tube of second lucifuge, the airtight test tube of second lucifuge is communicated with the airtight test tube of first lucifuge, and the other end of the airtight test tube of first lucifuge connects syringe.
This extraction element also comprises the constant temperature whipping appts, can constant temperature water bath the airtight test tube of lucifuge after the heating.
The solid sodium hydroxide powder is housed in the preabsorption pipe, clears up the gas that and fall steam and clear up the sour gas that through solid sodium hydroxide powder preadsorption.This extraction element uses polyfluortetraethylene pipe that each several part is connected firmly.
A kind of extracting method of combined hydrogen phosphide, its step comprises:
(1) sample collecting:
Gathered a certain amount of fine and close sample before solar radiation, solid sample is preserved in airtight light tight sampler bag, and the water sample sample is preserved in the tetrafluoroethylene bottle, notes not introducing bubble, and all samples is all stored 0～4 ℃ of following lucifuge;
(2) release of combined hydrogen phosphide:
(a) take by weighing fine and close solid sample, or measure water sample and place the airtight test tube of lucifuge together with the tetrafluoroethylene magnetic stir bar;
(b), add diluted acid or alkali lye and place the airtight test tube of lucifuge according to the character of testing sample;
(c) draw the high pure nitrogen cleaning system with syringe, displacements such as oxygen are gone out, make whole pipeline remain on anaerobic state, and in syringe, maintain nitrogen;
(d) digestion solution with the airtight test tube of first lucifuge is transferred in the airtight test tube of second lucifuge;
(e) the airtight test tube of heating second lucifuge seethes with excitement solution rapidly; Be placed on then in the warm water bath,, clear up the gas that through being filled in ducted solid sodium hydroxide powder preadsorption and falling steam and clearing up the sour gas that with temperature control magnetic stirrer 5～60min;
(f) get high pure nitrogen with syringe and inject to take the gas that digestion process produces out of, extract the mixed gas of being discharged by system with gas sampler simultaneously, this mixed gas is for extracting the combined hydrogen phosphide gas that obtains.
The mixed gas that obtains in the step (f) cooperates gas-chromatography-NPD method to measure with the online cold-trap fast enriching of secondary, and recording instrumnet is to the integral result of phosphuret-(t)ed hydrogen characteristic peak area.
3. beneficial effect:
The invention provides a kind of extracting method and device of combined hydrogen phosphide, reduction characteristic according to phosphuret-(t)ed hydrogen, total system is the airtight lucifuge of an anaerobism system, adopt acid or alkali to clear up and discharge combined hydrogen phosphide gas in the fine and close sample, the back adopts the online cold-trap fast enriching of secondary to cooperate gas-chromatography-NPD method to measure, phosphuret-(t)ed hydrogen detection sensitivity height, and detectability is low, reach 0.01pg, be applicable to the mensuration of phosphine gas in the varying environment sample.The present invention not only is suitable for the mensuration of combined hydrogen phosphide, when clearing up with acid, also applicable to the mensuration of reducing gas such as hydrogen sulfide, methane.
Description of drawings
Fig. 1 is the extraction element of combined hydrogen phosphide gas.
Embodiment
The present invention will be further described below in conjunction with drawings and Examples.
Embodiment 1:
The extraction of combined hydrogen phosphide and the basic step of mensuration:
A, sample collecting
Gathered a certain amount of fine and close sample with suitable sampling thief before solar radiation, solid sample is preserved in airtight light tight sampler bag, and the water sample sample is preserved in the tetrafluoroethylene bottle, notes not introducing bubble, and all samples is all stored 0～4 ℃ of following lucifuge.
The release of B, combined hydrogen phosphide
(a) take by weighing an amount of fine and close solid sample, or the water sample (Suspended Particles in Water of former water, filtered water or 0.45 μ m membrane filtration) of measuring certain volume places the airtight test tube 4 of lucifuge together with the tetrafluoroethylene magnetic stir bar;
(b) according to the character of testing sample, add diluted acid or alkali lye and place the airtight test tube 3 of lucifuge, the each several part pipe connecting is connected firmly by synoptic diagram with the tetrafluoroethylene pipeline, syringe 1 and gas sampler 9 use T-valve 2,7 and 8 to communicate with other parts respectively;
(c) draw 500mL high pure nitrogen cleaning system with syringe 1, displacements such as oxygen are gone out, make whole pipeline remain on anaerobic state, about residue 100mL;
(d) move in the airtight test tube 4 of second lucifuge with the digestion solution of 50mL high pure nitrogen the airtight test tube 3 of first lucifuge;
(e) the airtight test tube 4 of heating second lucifuge seethes with excitement solution rapidly; Then the airtight test tube 4 of second lucifuge is placed constant temperature whipping appts 5,, clear up the solid sodium hydroxide powder preadsorption of gas in being filled in preabsorption pipe 6 that and fall steam and clear up the sour gas that with temperature control magnetic stirrer 5～60min;
(f) get the 50mL high pure nitrogen with syringe 1 and inject to take the gas that digestion process produces out of from system's left end, the right-hand member in system extracts the mixed gas of being discharged by system with gas sampler 9 simultaneously.
The mensuration of C, combined hydrogen phosphide gas
Clear up the mixed gas that discharges and cooperate gas-chromatography-NPD method to measure with the online cold-trap fast enriching of secondary, recording instrumnet is to the integral result of phosphuret-(t)ed hydrogen characteristic peak area.
D, data processing and numerical value convert
In the characteristic peak area substitution fitting formula with gas sample to be measured, calculate the quality of institute's phosphine containing in the gas sample to be measured, subsequently the following formula of calculation result substitution calculated:
C (ng/m
3, the ng/kg dry weight)--the phosphuret-(t)ed hydrogen mass concentration of-testing sample; m
1(ng)--the quality of institute's phosphine containing in the-testing sample; V (m
3)----clear up volume of water sample; m
2(kg)---clear up sample quality; W (%)---solid sample water ratio;
Calculation result is the phosphine concentration of testing sample.
From Yancheng, Jiangsu section Huanghai Sea seashore adopt pedotheque, take by weighing 1g left and right sides sample, adopt 0.5moL/L sulfuric acid to clear up 20min for 60 ℃ and measure wherein combined hydrogen phosphide content.Experimental result is as shown in table 1, and the measurement result relative standard deviation is 4.41%～6.44%.
Table 1 pedotheque combined hydrogen phosphide measurement result
Embodiment 2:
The different depths sediment sample of gathering from Taihu Lake takes by weighing 1g left and right sides sample, adopts 1moL/L hydrochloric acid to clear up 5min for 100 ℃ and measures wherein combined hydrogen phosphide content, and elementary operation is with embodiment 1.Experimental result is as shown in table 2, and this law relative standard deviation is 2.92%～7.73%.
Table 2 settling cylindrical sample combined hydrogen phosphide measurement result
Embodiment 3:
Mud sample from different workshop sections of sewage work gather takes by weighing 0.8g left and right sides sample, uses the 2moL/L sodium hydroxide solution to clear up 10min for 80 ℃ and measures wherein combined hydrogen phosphide content, and other elementary operation is with embodiment 1.
Experimental result is as shown in table 3, and this law relative standard deviation is 1.47%～8.84%.
Table 3 mud sample combined hydrogen phosphide measurement result
Embodiment 4:
Water sample from certain eutrophic lake collection, adopt the former water sample of 0.45 μ m membrane filtration, measure former water respectively and contain phosphuret-(t)ed hydrogen in the filtering material of particle residue, measure the 20mL water sample or, adopt 50 ℃ of 2moL/L potassium hydroxide solutions to clear up attitude phosphuret-(t)ed hydrogen content in the 30min mensuration water body the whole filter paper that contains particulate matter.Other elementary operation is with embodiment 1.
Experimental result is as shown in table 4, and measurement result shows that the phosphuret-(t)ed hydrogen overwhelming majority in the water body is adsorbed in the Suspended Particles in Water, and this law relative standard deviation is 6.15%～6.74%.
Table 4 water sample phosphuret-(t)ed hydrogen measurement result
Claims (6)
1. the extraction element of a combined hydrogen phosphide, comprise gas sampler (9), it is characterized in that gas sampler (9) is connected with preabsorption pipe (6), the other end of preabsorption pipe (6) connects the airtight test tube of second lucifuge (4), the airtight test tube of second lucifuge (4) is communicated with the airtight test tube of first lucifuge (3), and the other end of the airtight test tube of first lucifuge (3) connects syringe (1).
2. the extraction element of a kind of combined hydrogen phosphide according to claim 1 is characterized in that also comprising constant temperature whipping appts (5).
3. the extraction element of a kind of combined hydrogen phosphide according to claim 2 is characterized in that in the preabsorption pipe (6) the solid sodium hydroxide powder being housed.
4. according to the extraction element of claim 2 or 3 described a kind of combined hydrogen phosphides, it is characterized in that using polyfluortetraethylene pipe that each several part is connected firmly.
5. the extracting method of a combined hydrogen phosphide, its step comprises:
(1) sample collecting:
Gathered a certain amount of fine and close sample before solar radiation, solid sample is preserved in airtight light tight sampler bag, and the water sample sample is preserved in the tetrafluoroethylene bottle, notes not introducing bubble, and all samples is all stored 0～4 ℃ of following lucifuge;
(2) release of combined hydrogen phosphide:
(a) take by weighing fine and close solid sample, or measure water sample and place the airtight test tube of lucifuge together with the tetrafluoroethylene magnetic stir bar;
(b), add diluted acid or alkali lye and place the airtight test tube of lucifuge according to the character of testing sample;
(c) draw the high pure nitrogen cleaning system with syringe, displacements such as oxygen are gone out, make whole pipeline remain on anaerobic state, and in syringe, maintain nitrogen;
(d) digestion solution with the airtight test tube of first lucifuge is transferred in the airtight test tube of second lucifuge;
(e) the airtight test tube of heating second lucifuge seethes with excitement solution rapidly; Be placed on then in the warm water bath,, clear up the gas that through being filled in ducted solid sodium hydroxide powder preadsorption and falling steam and clearing up the sour gas that with temperature control magnetic stirrer 5～60min;
(f) get high pure nitrogen with syringe and inject to take the gas that digestion process produces out of, extract the mixed gas of being discharged by system with gas sampler simultaneously, this mixed gas is for extracting the combined hydrogen phosphide gas that obtains.
6. the extracting method of a kind of combined hydrogen phosphide according to claim 5, it is characterized in that the mixed gas that obtains in the step (f) cooperates gas-chromatography-NPD method to measure with the online cold-trap fast enriching of secondary, recording instrumnet is to the integral result of phosphuret-(t)ed hydrogen characteristic peak area.
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| CN200810023259A CN100590066C (en) | 2008-04-03 | 2008-04-03 | Method and device for extracting combined hydrogen phosphide |
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| CN102493776A (en) * | 2011-12-02 | 2012-06-13 | 中煤科工集团重庆研究院 | Hole sealing bag with magnetic stirring function |
| CN105044090B (en) * | 2015-06-24 | 2018-05-08 | 陕西师范大学 | A kind of detection method and device of sulfide |
| CN106526015B (en) * | 2016-10-28 | 2020-05-05 | 中国南玻集团股份有限公司 | Detection device and detection method for trace phosphorus impurities in hydrogen |
| CN112782340A (en) * | 2020-12-24 | 2021-05-11 | 青海盐湖工业股份有限公司 | Method for measuring hydrogen content in chlorine |
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Non-Patent Citations (4)
| Title |
|---|
| Phosphine(PH3) in the biosphere. Gassmann G., Glindemann D.Angewandte Chemie:international edition in English,Vol.32 No.5. 1993 |
| Phosphine(PH3) in the biosphere. Gassmann G.,Glindemann D.Angewandte Chemie:international edition in English,Vol.32 No.5. 1993 * |
| 结合态磷化氢在厌氧微生物产酸过程中的释放行为. 朱益新等.环境科学，第26卷第4期. 2005 |
| 结合态磷化氢在厌氧微生物产酸过程中的释放行为. 朱益新等.环境科学，第26卷第4期. 2005 * |
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