CN101551366B - Method for quickly separating and detecting volatile gaseous arsenic compound - Google Patents
Method for quickly separating and detecting volatile gaseous arsenic compound Download PDFInfo
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- CN101551366B CN101551366B CN2009100744078A CN200910074407A CN101551366B CN 101551366 B CN101551366 B CN 101551366B CN 2009100744078 A CN2009100744078 A CN 2009100744078A CN 200910074407 A CN200910074407 A CN 200910074407A CN 101551366 B CN101551366 B CN 101551366B
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Abstract
A method for quickly separating and detecting volatile gaseous arsenic compound belongs to the field of chemical detecting technology. The method of the invention is used for settling the problem of segregation analysis of gaseous arsenic compound. The technical solution comprises two steps of arsenic compound collecting and arsenic compound separating. The method of the invention adopts a separating column and a detecting device. In the step of arsenic compound collecting, the PTFE column which is filled with absorbent cotton is adopted as the separating column. In the step of arsenic compound separating, the separating column after collecting is quickly transferred into a vacuum thermal insulating bucket for slowing increasing the temperature. The volatile gaseous arsenic compound captured on the filler of separating column is released sequentially for realizing the quick baseline separation. The method of the invention does not use the conventional color spectrum filler and has the advantages of quick separation, low cost, simple operation, excellent suitability, excellent repeatability, low analysis cost, and convenience for realizing on-line cooperation with specific arsenic detecting devices of ICPMS, AFS, etc.
Description
Technical field
The present invention relates to a kind of compound separation method, especially for volatile gaseous arsenic compound AsH
3, CH
3AsH
2, (CH
3)
2AsH, (CH
3)
3The separation method of materials such as As belongs to the chemical detection analysis technical field.
Background technology
Important environmental contaminants arsenic can be produced the different shape gaseous arsenic compound by biological methylation in environment, comprise AsH
3, CH
3AsH
2, (CH
3)
2AsH, (CH
3)
3As etc.The toxicity of these gaseous arsenic compounds is huge, and the gaseous state arsenic toxicity of different shape is difference to some extent again.The gaseous arsenic compound of utmost point low content can cause strong toxicity, so require the gaseous arsenic compound analytical approach not only to have good separating effect, simultaneously very high sensitivity will be arranged.It is a difficult point of Environmental Health and the research of arsenic biomass geochemistry that different gaseous state arsenic in the environment are accurately monitored, this mainly be because: the disengaging time that (1) gaseous arsenic compound volatility is separated on the common chromatographic column is longer, and separating effect is undesirable; (2) owing to do not have the special efficacy selectivity, if adopt conventional gas chromatographic detection instrument, poor sensitivity is difficult to satisfy the content analysis requirement of surrounding medium; (3) the gaseous arsenic compound separation temperature is low, makes common gas phase chromatographic device cause very big difficulty to the application of gaseous arsenic compound compartment analysis.In sum; Comparatively effective method is to adopt separation means and arsenic special efficacy sensitive analysis means such as icp ms (ICPMS), AFS coupling modes such as (AFS) to measure; And this just requires separation means to have good separating effect, fast and be convenient to the advantage with the detecting instrument coupling; Weigh with this standard, the effective ways of gaseous state arsenic compartment analysis also lack very much at present.Comparatively commonly adopt expensive gas chromatography stationary phase to process the gas chromatography packed column, to realize the separation of gaseous arsenic compound as separating medium.But the gas chromatography packed column needs carrier gas to keep higher pressure, thereby has increased gas circuit disclosure risk and the online difficulty that is connected test of instrument; Simultaneously, gas chromatographic column stationary phase fill method is comparatively complicated, and operation easier is big, and reappearance is difficult for holding, and analysis cost is high.
Summary of the invention
Technical matters to be solved by this invention provide a kind ofly reduce analysis cost, operation is simple, can satisfy the different shape method for quickly separating and detecting volatile gaseous arsenic compound.
The alleged problem of the present invention is solved by following technical scheme:
A kind of method for quickly separating and detecting volatile gaseous arsenic compound, its special feature are that it carries out according to following steps:
A. arsenic compound captures: get the separating column that filling material is housed; Separating column being inserted in the middle of the cold-trap liquid nitrogen, make filling material part 3-5cm under the submergence liquid nitrogen liquid level fully, is carrier gas with the helium; Gaseous arsenic compound to be analyzed is written into through the separating column carrier gas inlet; The logical detecting instrument of separating column carrier gas outlet captures time 3-4min, and said filling material is a medical absorbent cotton;
B. gaseous arsenic compound separates: after capturing completion; Rapidly separating column is transferred in the vacuum thermal insulation bucket; It is slowly heated up in the vacuum thermal insulation bucket, and the volatile gaseous arsenic compound that is captured on the separating column filling material is discharged at low temperatures successively, realizes quick baseline separation.
Above-mentioned method for quickly separating and detecting volatile gaseous arsenic compound, said separating column cylinder length 50-60cm, it is 20-30cm that absorbent cotton is filled length; The absorbent cotton quality is 0.5-1.0g; The cylinder two ends are respectively left 10～15cm and are put the sky part, cylinder external diameter 6.0mm, internal diameter 4.0mm.
Above-mentioned method for quickly separating and detecting volatile gaseous arsenic compound, said helium are high-purity helium, and purity is 99.999%, and flow velocity is 50-80mL/min, pressure 0.1-0.15Mpa.
Above-mentioned method for quickly separating and detecting volatile gaseous arsenic compound, said separating column adopts the PTFE cylinder; Said detecting instrument adopts icp ms or AFS.
The present invention is directed to present gaseous arsenic compound and separate the simple and effective method for separating and analyzing of shortage; And need to rely on the problem that the gas chromatography packed column separates, proposed a kind ofly to use simple and easy separation to realize the quick method of separating of gaseous arsenic compound with attemperating unit, under the situation that need not carry out complex operations.This method is not used the conventional chromatogram filler, but separate quick, with low cost, simple to operate, suitability is good, and have simple to operate, be easy to characteristics such as realization, favorable reproducibility, analysis cost be low.Experiment shows; Adopt the inventive method, can in 3 minutes, reach baseline separation for the volatile gaseous arsenic compound of different shape, desirable to the separating effect of gaseous arsenic compound; Reappearance (n=7; Relative standard deviation (RSD)≤10%), good stability, to variable concentrations gaseous arsenic compound linear dependence good (more than the r=0.99), the range of linearity is wide.Simultaneously, what greatly reduce analytic system because do not adopt chromatographic column plants gas and gas circuit pressure, makes that tripping device is convenient realizes on-line couplings with arsenic special efficacy detecting instrument such as ICPMS, AFS etc.
Description of drawings
Fig. 1 is an arsenic compound capturing device synoptic diagram of the present invention;
Fig. 2 is a gaseous arsenic compound tripping device synoptic diagram of the present invention;
Fig. 3 is that the atomic fluorescence spectrophotometry that gaseous arsenic compound separates detects collection of illustrative plates.
Each label is following in the accompanying drawing: 1. adiabatic heat-insulation shell, 2. liquid nitrogen, 3. heat insulation foam lid, 4. carrier gas inlet, 5. carrier gas outlet, 6. separating column, 7. absorbent cotton, 8. vacuum thermal insulation bucket.
Embodiment
The gas chromatography packed column of the present invention's abandoning tradition in the gaseous arsenic compound detachment process, used separating column select to have flexible PTFE material cylinder, and the filling material in the cylinder is selected common medical absorbent cotton.PTFE is a kind of (per) fluoropolymer that is made by tetrafluoroethene free radical polymerization, is crystalline polymer, and PTFE has excellent chemical-resistant; Loss factor is low; Stable performance, good mechanical property, friction factor is low; Nonflammable, it is stable to have certain thermal adaptability scope, material physicochemical property.Another fundamental purpose of selecting this material for use be the PTFE tube Louis in bending, be convenient to be connected with detecting instrument.The separating column inner stuffing is selected medical absorbent cotton for use; The agent structure of absorbent cotton is a cotton fiber; Has strong polarity adsorptive power; Have fluffy reticulate texture simultaneously, in the compound separation process, can play the effect that gaseous state arsenide and the intensification of stabilization column internal temperature are resolved in absorption simultaneously, guaranteed that gaseous arsenic compound reaches quick baseline separation.The absorbent cotton filling quality is between 0.5-1.0g, and filling absorbent cotton should not be too much or very few, fills length and should guarantee between 20-30cm, otherwise can have a strong impact on separating effect.
Compare with other common organic compounds; The separation condition of volatile gaseous arsenic compound is unique; The ingenious cryogenic trapping that utilizes of the present invention also separates at low temperatures; Adopt liquid nitrogen cold trap that volatile gaseous arsenic is captured, the gaseous arsenic compound after the capture is temporarily stored on cylinder leading portion absorbent cotton.After capture accomplishing, rapidly separating column being transferred in the vacuum thermal insulation bucket, slowly heats up in space limited in bucket, and the heat-preserving container temperature reaches balance with the separating column temperature at first rapidly, slowly rising naturally, and maintenance lower temperature then.The inventive method is utilized the low temperature of separating column itself, is transferred to heat-preserving container rapidly, and programming rate has slowly guaranteed gaseous arsenic compound separating on absorbent cotton with low-temperature condition.The vacuum thermal insulation bucket can guarantee each synchronous and reappearance of analyzing that heats up.The present invention is not owing to adopt any chromatographic column or chromatograph packing material in the process of compartment analysis gaseous arsenic compound; Only having adopted absorbent cotton is separating medium; So entire separation system gas circuit pressure is very little; The carrier gas disclosure risk is low, is convenient to simultaneously and other Sensitive Detection instrument such as ICPMS or AFS coupling.
Absorbent cotton has the netted and fascircular texture of a large amount of cotton fibers; At low temperatures gaseous arsenic compound strong absorption and good separating effect have been shown; But experiment shows that absorbent cotton can not separate gaseous arsenic compound at normal temperatures, and adsorption effect is also not obvious simultaneously.Equally, if the PTFE column jecket is not filled absorbent cotton, only can not reach the purpose that gaseous arsenic compound separates with temperature-rising method through the mentioned cold trapping of this method yet.Adopt the inventive method, must just can reach the desired separated effect in strict accordance with operation steps operation mentioned in the method.
Practical implementation process of the present invention is following: referring to Fig. 1, get PTFE material separating column 6, and separating column cylinder length 60cm, cylinder external diameter 6.0mm, internal diameter 4.0mm fills 1.0g absorbent cotton 7 in the separating column, fill length 30cm, and the separating column middle part is curved ring-type or U-shaped; Get the cold-trap of forming by liquid nitrogen 2, adiabatic heat-insulation shell 1 and heat insulation foam lid 3; Liquid nitrogen degree of depth 20cm in the adiabatic heat-insulation shell, adiabatic heat-insulation bucket housing diameter 20cm, foam insulation lid thickness is 4cm; Get the hole of two diameters and separating column external diameter coupling on it, separating column is by passing in the hole.Separating column carrier gas inlet 4 is from sample collection device or gaseous arsenic compound standard deriving device, and detecting instruments are led in carrier gas outlet 5, and carrier gas is high-purity helium, and purity is 99.999%, and flow velocity is 50-80mL/min, and pressure is 0.1-0.15Mpa.When arsenic compound captures, cylinder is put in the middle of the liquid nitrogen cold trap, made and fill absorbent cotton part 4cm under the submergence liquid nitrogen liquid level fully.Volatile gaseous arsenic compound is by on the leading portion absorbent cotton of cold trapping in separating column.After capturing 3-5min, from liquid nitrogen cold trap, take out separating column, be transferred to rapidly in the vacuum thermal insulation bucket 8, it is slowly heated up in the vacuum thermal insulation bucket naturally, as shown in Figure 2.Gaseous arsenic compound AsH
3, CH
3AsH
2, (CH
3)
2AsH, (CH
3)
3A can reach baseline separation in 3min, separate spectrogram and see accompanying drawing 3.
Separating column of the present invention is once loaded and can repeatedly be used, if separating effect reduces, can remove waste and old filling absorbent cotton easily, fills new absorbent cotton, and the PTFE cylinder can be filled use repeatedly, and is convenient and swift, and cost is very cheap.
Claims (4)
1. a method for quickly separating and detecting volatile gaseous arsenic compound is characterized in that, it utilizes separating column and detecting instrument, and carries out according to following steps:
A. arsenic compound captures: get the separating column that filling material is housed; Separating column being inserted in the middle of the cold-trap liquid nitrogen, make filling material part 3-5cm under the submergence liquid nitrogen liquid level fully, is carrier gas with the helium; Gaseous arsenic compound to be analyzed is written into through the separating column carrier gas inlet; The logical detecting instrument of separating column carrier gas outlet captures time 3-4min, and said filling material is a medical absorbent cotton; It is 20-30cm that said absorbent cotton is filled length, and the absorbent cotton quality is 0.5-1.0g;
B. gaseous arsenic compound separates: after capturing completion; Rapidly separating column is transferred in the vacuum thermal insulation bucket; It is slowly heated up in the vacuum thermal insulation bucket, and the volatile gaseous arsenic compound that is captured on the separating column filling material is discharged at low temperatures successively, realizes quick baseline separation.
2. method for quickly separating and detecting volatile gaseous arsenic compound according to claim 1 is characterized in that, said separating column cylinder length 50-60cm, and the cylinder two ends are respectively left 10～15cm and are put the sky part, cylinder external diameter 6.0mm, internal diameter 4.0mm.
3. method for quickly separating and detecting volatile gaseous arsenic compound according to claim 2 is characterized in that, said helium is high-purity helium, and purity is 99.999%, and flow velocity is 50-80mL/min, nebulizer gas pressure 0.1-0.15Mpa.
4. method for quickly separating and detecting volatile gaseous arsenic compound according to claim 3 is characterized in that, said separating column adopts the PTFE cylinder; Said detecting instrument adopts icp ms or AFS.
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| CN2009100744078A CN101551366B (en) | 2009-05-20 | 2009-05-20 | Method for quickly separating and detecting volatile gaseous arsenic compound |
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|---|---|---|---|
| CN2009100744078A CN101551366B (en) | 2009-05-20 | 2009-05-20 | Method for quickly separating and detecting volatile gaseous arsenic compound |
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| CN101551366A CN101551366A (en) | 2009-10-07 |
| CN101551366B true CN101551366B (en) | 2012-04-25 |
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| CN103111155A (en) * | 2013-01-23 | 2013-05-22 | 中国农业科学院农业环境与可持续发展研究所 | Enrichment device for volatile arsenic and mounting method thereof |
Citations (3)
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|---|---|---|---|---|
| SU1481206A1 (en) * | 1987-06-16 | 1989-05-23 | Химико-металлургический институт АН КазССР | Method of extracting arsenic from copper-arsenic slurry as arsenic sulfide |
| CN101261258A (en) * | 2008-01-04 | 2008-09-10 | 中国水产科学研究院黄海水产研究所 | Aquatic product inorganic arsenic determination method |
| CN101329311A (en) * | 2008-08-04 | 2008-12-24 | 华北电力大学（保定） | Gas chromatograph pillar for volatile gaseous state arsenic compounds separation and preparation method thereof |
-
2009
- 2009-05-20 CN CN2009100744078A patent/CN101551366B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1481206A1 (en) * | 1987-06-16 | 1989-05-23 | Химико-металлургический институт АН КазССР | Method of extracting arsenic from copper-arsenic slurry as arsenic sulfide |
| CN101261258A (en) * | 2008-01-04 | 2008-09-10 | 中国水产科学研究院黄海水产研究所 | Aquatic product inorganic arsenic determination method |
| CN101329311A (en) * | 2008-08-04 | 2008-12-24 | 华北电力大学（保定） | Gas chromatograph pillar for volatile gaseous state arsenic compounds separation and preparation method thereof |
Non-Patent Citations (3)
| Title |
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| 罗丽云 等.中药中砷的形态分析.《中国中药杂志》.2005,第30卷(第22期),1790-1793. * |
| 苑春刚 等.砷形态分析.《化学进展》.2009,第21卷(第2/3期),467-473. * |
| 迟玉广 等.以脱脂棉作为固相萃取填料柱切换高效液相色谱法测定环境水样中的多环芳烃.《第十四次全国色谱学术报告会论文集(上册) 》.2003,277-278. * |
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