CN201141856Y - Coupling system for detecting organo-tin compound - Google Patents
Coupling system for detecting organo-tin compound Download PDFInfo
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- CN201141856Y CN201141856Y CNU2007201736107U CN200720173610U CN201141856Y CN 201141856 Y CN201141856 Y CN 201141856Y CN U2007201736107 U CNU2007201736107 U CN U2007201736107U CN 200720173610 U CN200720173610 U CN 200720173610U CN 201141856 Y CN201141856 Y CN 201141856Y
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Abstract
The utility model provides a combined system for detecting organic tin compound, which includes a liquid chromatography (1) and a liquid chromatographic column (2). The utility model is characterized in that the combined system also includes a four-way valve (3), a peristaltic pump (6), a membrane type gas-liquid separator(8), a drying tube (10), a gas chromatography flame photometric detector(11) and a chromatography workstation(18). The liquid chromatographic column (2) and the peristaltic pump (6) are communicated with the four-way valve (3) which is communicated with the membrane type gas-liquid separator(8) through a mixing tube(7); the membrane type gas-liquid separator(8) is communicated with the gas chromatography flame photometric detector(11) through the drying tube (10); the signal detected by the gas chromatography flame photometric detector(11) is recorded and processed by the chromatography workstation(18). The utility model organically combines the direct organic tin compound separation function of the liquid chromatography with the high sensitivity of the gas chromatography flame photometric detector, thereby the utility model can effectively separate and mensurate the organic tin compound such as methyltin, and meanwhile has the advantage of low cost.
Description
Technical field
The utility model relates to a kind of combined system, particularly a kind of combined system that is used to detect organo-tin compound.
Background technology
Gas chromatography is the determining instrument of the methyl tin compound used always, because it has higher sensitivity and lower detectability, but, organo-tin compound exists because being form with salt in environment, be difficult to directly measure with gas chromatography, so extraction and cleaning could detect must carry out the derivatization reaction of off-line to organo-tin compound before gas chromatographic detection after, this be one consuming time and cause the process of error.Liquid chromatography can directly be carried out the separation of methyl tin compound, but is difficult to analyze with conventional liquid chromatography ultraviolet and fluorescence detector, because organo-tin compound does not have uv absorption, can not produce fluorescence.Though liquid chromatography and Atomic Absorption Spectrometer (AAS), Atomic Emission Spectrometer AES (AES) and inductance coupled plasma mass spectrum Instrument crosslinkings such as (ICP-MS) are measured the methyl tin compound, can obtain higher sensitivity, these detecting devices involve great expense.
Summary of the invention
The purpose of this utility model provides a kind ofly to be had higher selectivity and is connected than the combined system that is easier to, with low cost being used to detects organo-tin compound with sensitivity, instrument.
The utility model is realized by following technical proposals:
A kind of combined system that is used to detect organo-tin compound, comprise liquid chromatograph 1 and liquid-phase chromatographic column 2, it is characterized in that, also comprise four-way valve 3, peristaltic pump 6, film gas-liquid separation vessel 8, drying tube 10, gas chromatographic flame photometric detector 11 and chromatographic work station 18;
Described liquid-phase chromatographic column 2 and peristaltic pump 6 are communicated with described four-way valve 3 fluids, described four-way valve 3 is communicated with described film gas-liquid separation vessel 8 fluids by a mixing tube 7, and described film gas-liquid separation vessel 8 is communicated with described gas chromatographic flame photometric detector 11 fluids by drying tube 10; Described gas chromatographic flame photometric detector 11 detects the signal that obtains and is write down and handled by chromatographic work station 18.
The utility model is a kind of brand-new combined system, with liquid chromatography to the direct separating power of organo-tin compound and the organically combination of high sensitivity of gas chromatography flame photometric detector (FPD), effectively organo-tin compound such as separation determination methyl tin also has advantage with low cost simultaneously.Adopt the combined system of gas chromatographic flame photometric detector, widened the range of application of liquid chromatography and gas chromatography, have brand-new design and break through as liquid chromatogram detector.In addition, it has higher selectivity and sensitivity, disturbs lessly, and it is relatively easy that instrument connects, and cost is lower, is with a wide range of applications in environmental chemistry study and environment measuring.
Description of drawings
Fig. 1 is for detecting the combined system synoptic diagram of methyl tin compound;
Fig. 2 is a kind of structural representation of film gas-liquid separation vessel;
Fig. 3 is 20ng ml
-1Monomethyl tin 2, stannous methide 3 and 10ng ml
-1The separate colors spectrogram of tin trimethyl 1 mixed solution.
Reference numeral:
1-liquid chromatograph 2-liquid-phase chromatographic column 3-four-way valve
The 4-first input port 5-second input port 6-peristaltic pump
7-mixing tube 8-film gas-liquid separation vessel 9-gas chromatography injection port
10-drying tube 11-gas chromatographic flame photometric detector
12-gas-liquid mixture outlet 13-goes up the aluminium disk
Disk body under the disk body 15-teflon on the 14-teflon
Aluminium disk under the spiral linear grooves 17-on the 16-teflon disk
The 18-chromatographic work station
Embodiment
Now technical characterictic of the present utility model is described in detail in conjunction with Fig. 1.The utility model comprises that mainly conventional liquid chromatograph 1, peristaltic pump 6, film gas-liquid separation vessel 8, drying tube 10 and gas chromatography quartz surfaces induce detecting device 11 and chromatographic work station 18 to form; Wherein, the output terminal of liquid chromatograph 1 is communicated with the first input end of four-way valve 3, and first, second delivery outlet of peristaltic pump 6 is connected respectively to second, third input end of four-way valve 3; The output terminal of described four-way valve 3 is connected to film gas-liquid separation vessel 8 by a mixing tube 7; Film gas-liquid separation vessel 8 isolated gases are connected to gas chromatographic flame photometric detector 11 by drying tube 10; The gas chromatographic flame photometric detector detects the signal that obtains and is write down and handled by chromatographic work station 18.
In the said apparatus, liquid-phase chromatographic column 2 has used commercial C18 liquid-phase chromatographic column, and its separating effect and sensitivity can obtain satisfied result; Chromatographic work station uses commercially available BF-2002 type chromatographic work station; Film gas-liquid separation vessel 8 can use common planar or hollow-fibre membrane gas-liquid separator, also can use structure as shown in Figure 2: this film gas-liquid separation vessel comprises discoid disk body 14 and the following disk body 15 gone up that polytetrafluoroethylmaterial material is made, and be clipped in described on, following disk body 14, microporous poly tetrafluoroethylene between 15, on described, the surface of contact of following disk body and described microporous poly tetrafluoroethylene is the plane of being carved with the spiral yarn shaped groove 16 that corresponds to each other, on described, spiral yarn shaped groove 16 initiating terminals of following disk body are respectively equipped with carrier gas inlet and gas-liquid mixture inlet (not shown), on, the spiral yarn shaped groove of following disk body finishes end and is respectively equipped with carrier gas outlet and gas-liquid mixture outlet (not shown), go up disk body 14 and following disk body 15 in order better to fix, can also use aluminium disk 13 and following aluminium disk 17 that above-mentioned film gas-liquid separation vessel is clipped in the middle, be fixed.Gas chromatographic flame photometric detector 11 can be bought from market, also can use the gas chromatography quartz surfaces to induce detecting device, and described gas chromatography quartz surfaces induces the concrete structure of detecting device to disclose in Chinese patent ZL 93108636.1.
It is as follows to use said system that the sample that contains the methyl tin compound is carried out method for measuring:
Contain the sampling valve injection liquid-phase chromatographic column 2 of the testing sample of methyl tin compound by liquid chromatograph 1, become the chromatogram effluent through the testing sample that separates, described chromatogram effluent enters four-way valve 3 from liquid-phase chromatographic column 2 output terminals, simultaneously, derivative reagent potassium borohydride and acetate 4,5 enter four-way valve 3 by peristaltic pump 6 from first, second input port respectively with flow velocity 0.4ml/min, and and above-mentioned chromatogram effluent in four-way valve 3, mix and be incorporated in mixing tube 7 and fully carry out hydrogenation; Hydrogenated products separates through film gas-liquid separation vessel 8, waste liquid 12 directly flows out from gas-liquid mixture outlet 12, gas enters in the groove of opposite side by microporous poly tetrafluoroethylene, take away by carrier gas (being generally nitrogen) from gas chromatography injection port 9, enter gas chromatographic flame photometric detector 11 through behind the drying tube 10, write down and handle the experimental data that described gas chromatographic flame photometric detector 11 obtains by BF-2002 chromatographic work station 18.
In above-mentioned mensuration process, selection, moving phase composition and flow velocity, derivative reagent composition and the parameters such as ratio, gas chromatography gas circuit of chromatographic column are all optimized:
1. used commercial C18 liquid-phase chromatographic column in the utility model, separating effect and sensitivity all obtain satisfied result.
2. the moving phase composition of the utility model use is defined as through testing repeatedly: 70% methyl alcohol, 3% (v/v) acetate, 0.1% (m/v) tropolone (tropolone) and water.Flow rate pump is 0.3ml/min.Derivative reagent is defined as: potassium borohydride (0.5% (m/v) contains 0.2% (m/v) potassium hydroxide) and 2% (v/v) acetate.
3. the gas chromatography carrier gas is defined as nitrogen, and is inserted by the gas chromatography injection port.
Under operating conditions, every index of native system has been carried out test repeatedly, to 10ng ml
-1Monomethyl tin 2,10ng ml
-1Stannous methide 3 and 5ng ml
-1Tin trimethyl 1 mixed solution is measured for parallel 3 times, and its relative standard deviation is respectively 2.0%, 3.7 and 3.8%.To their standard series (1-100ng ml
-1) measure, its peak height and solution concentration have good linear relationship, and related coefficient (r) is respectively 0.9980,0.9911 and 0.9975.The system of present embodiment is respectively 1.69,0.51 and 0.36ng ml to the detection limit of monomethyl tin, stannous methide and tin trimethyl
-1
Fig. 2 is 20ngml
-1Monomethyl tin 2, stannous methide 3 and 10ngml
-1The separate colors spectrogram of tin trimethyl 1 mixed solution, visible monomethyl tin, stannous methide can separate fully with tin trimethyl.This system has been used to the morphological analysis of methyl tin in the water sample at present, can predict, this liquid chromatography and gas chromatography quartz surfaces are induced the mode of thinking of flame photometric detector (FPD) combined system novelty, will aspect liquid chromatography and other gas chromatography detector coupling, produce material impact, and in analytical chemistry and environmental chemistry study, will be with a wide range of applications.
Claims (1)
1. combined system that is used to detect organo-tin compound, comprise liquid chromatograph (1) and liquid-phase chromatographic column (2), it is characterized in that, also comprise four-way valve (3), peristaltic pump (6), film gas-liquid separation vessel (8), drying tube (10), gas chromatographic flame photometric detector (11) and chromatographic work station (18);
Described liquid-phase chromatographic column (2) and peristaltic pump (6) are communicated with described four-way valve (3) fluid, described four-way valve (3) is communicated with described film gas-liquid separation vessel (8) fluid by a mixing tube (7), and described film gas-liquid separation vessel (8) is communicated with described gas chromatographic flame photometric detector (11) fluid by drying tube (10); Described gas chromatographic flame photometric detector (11) detects the signal that obtains and is write down and handled by chromatographic work station (18).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNU2007201736107U CN201141856Y (en) | 2007-10-12 | 2007-10-12 | Coupling system for detecting organo-tin compound |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNU2007201736107U CN201141856Y (en) | 2007-10-12 | 2007-10-12 | Coupling system for detecting organo-tin compound |
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| Publication Number | Publication Date |
|---|---|
| CN201141856Y true CN201141856Y (en) | 2008-10-29 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNU2007201736107U Expired - Lifetime CN201141856Y (en) | 2007-10-12 | 2007-10-12 | Coupling system for detecting organo-tin compound |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101936963A (en) * | 2010-07-28 | 2011-01-05 | 河北科技大学 | Automatic test instrument for organic tin |
| CN104569272A (en) * | 2015-01-20 | 2015-04-29 | 山东出入境检验检疫局检验检疫技术中心 | Tandem mass spectrometry method capable of simultaneously detecting five organic tin pesticide residues in livestock and poultry meat products |
| CN105548381A (en) * | 2015-12-09 | 2016-05-04 | 浙江万里学院 | Method for detecting tributyltin in marine fishes and shellfishes |
| CN106442762A (en) * | 2016-08-31 | 2017-02-22 | 湖北犇星化工有限责任公司 | Detection method for methyltin chloride for methyltin mercaptide synthetic process |
| CN106872636A (en) * | 2017-03-31 | 2017-06-20 | 四川大学 | The method that the combination of low pressure ion chromatography inductivity coupled plasma mass spectrometry determines inorganic tin and organo-tin compound simultaneously |
| CN110018259A (en) * | 2019-05-05 | 2019-07-16 | 中国热带农业科学院分析测试中心 | A kind of measuring method of organic tin compound |
| CN111948322A (en) * | 2020-07-30 | 2020-11-17 | 河海大学 | Method for detecting organic tin in water body |
-
2007
- 2007-10-12 CN CNU2007201736107U patent/CN201141856Y/en not_active Expired - Lifetime
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101936963A (en) * | 2010-07-28 | 2011-01-05 | 河北科技大学 | Automatic test instrument for organic tin |
| CN101936963B (en) * | 2010-07-28 | 2012-10-03 | 河北科技大学 | Automatic test instrument for organic tin |
| CN104569272A (en) * | 2015-01-20 | 2015-04-29 | 山东出入境检验检疫局检验检疫技术中心 | Tandem mass spectrometry method capable of simultaneously detecting five organic tin pesticide residues in livestock and poultry meat products |
| CN104569272B (en) * | 2015-01-20 | 2016-03-30 | 山东出入境检验检疫局检验检疫技术中心 | Detect the second order ms method that in poultry meat goods, five kinds of organic tin pesticides are residual simultaneously |
| CN105548381A (en) * | 2015-12-09 | 2016-05-04 | 浙江万里学院 | Method for detecting tributyltin in marine fishes and shellfishes |
| CN106442762A (en) * | 2016-08-31 | 2017-02-22 | 湖北犇星化工有限责任公司 | Detection method for methyltin chloride for methyltin mercaptide synthetic process |
| CN106442762B (en) * | 2016-08-31 | 2019-02-05 | 湖北犇星化工有限责任公司 | The detection method of methyl chloride tin for thiol methyl tin synthesis technology |
| CN106872636A (en) * | 2017-03-31 | 2017-06-20 | 四川大学 | The method that the combination of low pressure ion chromatography inductivity coupled plasma mass spectrometry determines inorganic tin and organo-tin compound simultaneously |
| CN106872636B (en) * | 2017-03-31 | 2018-05-25 | 四川大学 | The method that low pressure ion chromatography-inductivity coupled plasma mass spectrometry combination measures inorganic tin and organo-tin compound simultaneously |
| CN110018259A (en) * | 2019-05-05 | 2019-07-16 | 中国热带农业科学院分析测试中心 | A kind of measuring method of organic tin compound |
| CN110018259B (en) * | 2019-05-05 | 2022-05-10 | 中国热带农业科学院分析测试中心 | Method for determining organic tin compounds |
| CN111948322A (en) * | 2020-07-30 | 2020-11-17 | 河海大学 | Method for detecting organic tin in water body |
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| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term |
Granted publication date: 20081029 |
|
| CX01 | Expiry of patent term |