CN1892213A - Solid-phase micro-extracting device and method in gas-sampling tube - Google Patents
Solid-phase micro-extracting device and method in gas-sampling tube Download PDFInfo
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- CN1892213A CN1892213A CN 200610057576 CN200610057576A CN1892213A CN 1892213 A CN1892213 A CN 1892213A CN 200610057576 CN200610057576 CN 200610057576 CN 200610057576 A CN200610057576 A CN 200610057576A CN 1892213 A CN1892213 A CN 1892213A
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Abstract
Method and device for making solid phase micro-extraction gas sampling tube includes putting sampling tube lay in special designed heating arrangement, local heating only in adsorbent zone, to make adsorbed organic matter removing adsorption entering gas phase. Solid phase micro-extracting fiber is inserted into sampling tube extracting above adsorbent, completing analysing substance transferring from adsorbent extracting fiber, then fiber sample injection analysing on gas chromatograph. Heating cavity of heating arrangement adopts special materials and design, to make temperature distribution uniform and temperature fluctuation less than positive-negative 1 degree centigrade.
Description
Technical field
The present invention is a kind of with the substance transfer of adsorbing in the gas sample tube new technology to the gas chromatography injection port, belongs to the analysis and testing technology field.
Background technology
The method of organic compound component is in the at present general mensuration gas, earlier gather gaseous sample with sampling pipe, then sampling pipe is put into the thermal desorptioner that is connected with gas chromatograph, making organism take off absorption by heating enters gas phase, by inert gas organic gas is sent into gas chromatograph analysis again.The thermal desorptioner complex structure, volume is big, also need dispose inert gas and blow, and is unfavorable for carrying and works in the open air.Another kind of disposal route is to use the eluent solvent sampling pipe, and organism is eluted from adsorbent, collects leacheate, concentrates the back inject gas chromatograph and measures.This method need be employed more glassware and concentrator, and with an organic solvent, step is many, and the time is long, only is suitable for being used by the personnel that are skilled in technique in the laboratory.
Solid phase micro-extraction technique is a kind of new sample preparation technology that grows up nineteen nineties, comes adsorb organic compound with the fiber of band coating, then fiber is inserted the injection port of gas chromatograph, makes organism enter gas chromatograph, analyzes.Be mainly used in the immersion extraction or the headspace extraction of solution example.Solid phase micro-extraction technique is used widely in the organic analysis field, and solid-phase micro-extraction fibre has the supply of commodities of multiple model.
Solid-phase micro-extracting device and corresponding method yet there are no report in the gas sample tube.
Summary of the invention
The objective of the invention is to overcome the equipment heaviness that exists when carrying out the analysis of gas sample tube with thermal desorptioner or eluent solvent method, unhandy shortcoming, with a kind of solid-phase micro-extracting device the organism on the adsorbent in the sampling pipe is transferred on the extracting fiber, then fiber is inserted gas chromatograph analysis.Device of the present invention is easy to carry, and is swift to operate, is suitable for open-air the use.
The present invention is a kind of device that carries out solid-phase microextraction in the gas sample tube, it is characterized in that this device is made up of solid-phase microextraction handle (1) and fiber (3), gas sample tube (6), heating arrangement (10) and attemperating unit (9); Solid-phase micro-extraction fibre (3) inserts in the sampling pipe (6), and sampling pipe (6) is placed in the heating chamber (5) of heating arrangement (10), and attemperating unit (9) connects the temperature sensor (7) and the heating element (8) of heating arrangement (10) respectively.
The extracting process of solid-phase micro-extracting device is in this gas sample tube: go up at attemperating unit (9) and set 70 ℃～250 ℃ of required temperature.Chamber to be heated (5) temperature arrive desired level and constant after, sampling pipe (6) is placed in the heating chamber (5), make adsorbent zone (4) in heating chamber (5) and the top of adsorption tube (6) must place outside the heating chamber when placing sampling pipe (6), only, make the organism desorption that is adsorbed enter gas phase in the regional spot heating of adsorbent (4).Solid-phase micro-extraction fibre (3) is inserted sampling pipe (6), place adsorbent (4) superjacent air space, constantly adsorb the organism that desorbs from adsorbent (4).After desorb-absorption proceeds to required time 5min～40min, extract fiber (3) out, insert gas chromatograph, the sample introduction analysis.The key of this method is to adsorbent zone (4) spot heating, and the adsorbent upper space does not heat.Organism Yin Gaowen on the adsorbent and desorbing enters upper space, and this space temperature is low to help solid-phase micro-extraction fibre (3) to organic absorption, so just can finish the transfer of organism from the adsorbent to the fiber.
Heating arrangement is made of heating chamber (5), heating element (8), temperature sensor (7) and attemperating unit (9), and the diameter that it is characterized in that heating chamber (5) is 3mm～10mm, highly is 20mm～120mm, up/down perforation.The heating chamber thermal capacitance is little, and heat conduction is fast, uniformity of temperature profile.Go up the temperature that setting needs at attemperating unit (9), heat by heating element (8), temperature sensor (7) is sent to attemperating unit (9) to the heating chamber that records (5) temperature signal, compare with the temperature value of setting, then power when being lower than setting value to heating element (8), being higher than setting value and then stopping power supply, make heating chamber (5) keep required steady temperature, the fluctuation range of temperature is not more than ± and 1 ℃.The temperature of setting is control accurately, and it is excessive to fluctuate, in order to avoid organism is crossed thermal decomposition.Attemperating unit (9) is gone up display setting temperature and observed temperature simultaneously.
Effect of the present invention is to finish the transfer of organism from adsorbent (4) to extracting fiber (3) of need measuring with portable device, then solid-phase micro-extraction fibre (3) sample introduction on gas chromatograph easily.This technology has thoroughly been broken away from the use of thermal desorptioner, has overcome many limitation of thermal desorptioner and eluent solvent method, and equipment is simply light and handy, is easy to carry, and is suitable for carrying out on-the site analysis.
Description of drawings
The synoptic diagram of solid-phase micro-extracting device and the longitudinal diagram of heating arrangement in Fig. 1 gas sample tube.1. the solid-phase microextraction handle 2. adsorbs pipe cap, 3. extracting fiber, 4. adsorbent, 5. heating chamber, 6. sampling pipe, 7. temperature sensor, 8. heating element, 9. temperature control equipment, 10. heating arrangement.
Fig. 2 records the gas chromatogram of yperite (HD).
Fig. 3 records the gas chromatogram of dimethyl methyl phosphonate (DMMP).
Embodiment
Example 1
Sampling pipe to be processed is the sampling pipe that the Tenax-TA adsorbent is housed of having gathered 17.3ng yperite (HD).Going up the setting extraction temperature at attemperating unit (9) earlier is 170 ℃, and this temperature is to determine according to sorbent used characteristic with the compound of surveying.Chamber to be heated (5) temperature arrive desired level and constant after, sampling pipe (6) is put into heating chamber (5), note only adsorbent zone (4) being put into the chamber, the above part sampling pipe of adsorbent is stayed outside the chamber, does not heat.Extracting fiber (3) is passed sampling pipe cap (2) insert in the sampling pipe (6), place the adsorbent superjacent air space to extract.Take out fiber behind the extraction 10min, analyze at the gas chromatograph sample introduction.The gas chromatogram that records yperite is seen Fig. 2.
Example 2
Sampling pipe to be processed is the sampling pipe that the XAD-4 adsorbent is housed of having gathered 11.5ng dimethyl methyl phosphonate (DMMP).Going up the setting extraction temperature at attemperating unit (9) earlier is 80 ℃, and this temperature is according to the characteristic decision of sorbent used and the compound of surveying.Chamber to be heated (5) temperature arrive desired level and constant after, sampling pipe (6) is put into heating chamber (5), note only adsorbent zone (4) being put into the chamber, the above part sampling pipe of adsorbent is stayed outside the chamber, does not heat.Extracting fiber (3) is passed sampling pipe cap (2) insert in the sampling pipe (6), place the adsorbent superjacent air space to extract.Take out fiber behind the extraction 5min, analyze at the gas chromatograph sample introduction.The gas chromatogram that records dimethyl methyl phosphonate (DMMP) is seen Fig. 3.
Claims (4)
1. device that carries out solid-phase microextraction in the gas sample tube is characterized in that this device is made up of solid-phase microextraction handle (1) and fiber (3), gas sample tube (6), heating arrangement (10) and attemperating unit (9); Solid-phase micro-extraction fibre (3) inserts in the sampling pipe (6), and sampling pipe (6) is placed in the heating chamber (5) of heating arrangement (10), and attemperating unit (9) connects the temperature sensor (7) and the heating element (8) of heating arrangement (10) respectively.
2. device that carries out solid-phase microextraction in the gas sample tube, the extracting process that it is characterized in that this device is: be warmed up to heating chamber (5) temperature required, adsorbent (4) district of gas sample tube (6) places heating chamber (5), solid-phase micro-extraction fibre (3) is inserted sampling pipe (6) place adsorbent (4) superjacent air space, after being extracted into required time, extract fiber (3), analyze at the gas chromatograph sample introduction.
3. heating arrangement according to claim 1 (10), the diameter that it is characterized in that heating chamber (5) is 3mm～10mm, highly is 20mm～120mm, up/down perforation.
4. extracting process according to claim 2 is characterized in that the extraction time is 3min～40min, and extraction temperature is 70 ℃～250 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610057576 CN1892213A (en) | 2006-03-16 | 2006-03-16 | Solid-phase micro-extracting device and method in gas-sampling tube |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610057576 CN1892213A (en) | 2006-03-16 | 2006-03-16 | Solid-phase micro-extracting device and method in gas-sampling tube |
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| CN1892213A true CN1892213A (en) | 2007-01-10 |
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| CN 200610057576 Pending CN1892213A (en) | 2006-03-16 | 2006-03-16 | Solid-phase micro-extracting device and method in gas-sampling tube |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104007461A (en) * | 2014-05-29 | 2014-08-27 | 中国原子能科学研究院 | Method for analyzing solution sample in hot cell |
| CN105606745A (en) * | 2015-11-27 | 2016-05-25 | 中山大学惠州研究院 | Detection method for odor substances in exhaust gas of perfume and essence industry |
| CN107290189A (en) * | 2016-03-31 | 2017-10-24 | 庞英明 | A kind of portable multi-mode sampler |
-
2006
- 2006-03-16 CN CN 200610057576 patent/CN1892213A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104007461A (en) * | 2014-05-29 | 2014-08-27 | 中国原子能科学研究院 | Method for analyzing solution sample in hot cell |
| CN105606745A (en) * | 2015-11-27 | 2016-05-25 | 中山大学惠州研究院 | Detection method for odor substances in exhaust gas of perfume and essence industry |
| CN107290189A (en) * | 2016-03-31 | 2017-10-24 | 庞英明 | A kind of portable multi-mode sampler |
| CN107290189B (en) * | 2016-03-31 | 2021-03-30 | 庞英明 | Portable multi-mode sampler |
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