CN101871921A - Needle type extraction device suitable for gas chromatography and using method - Google Patents
Needle type extraction device suitable for gas chromatography and using method Download PDFInfo
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- CN101871921A CN101871921A CN 201010215901 CN201010215901A CN101871921A CN 101871921 A CN101871921 A CN 101871921A CN 201010215901 CN201010215901 CN 201010215901 CN 201010215901 A CN201010215901 A CN 201010215901A CN 101871921 A CN101871921 A CN 101871921A
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Abstract
The invention relates to a needle type extraction device suitable for gas chromatography and a using method. The extraction device consists of a heat resistant stainless steel needle head and a section of adsorbents filled inside a needle cylinder, wherein the adsorbents serving as extraction media are used for absorbing a trace amount of volatile or semi-volatile organic compounds; and adsorbent microspheres are fixed inside the needle cylinder by using heat resistant glass cotton. A needle bed of the device can be connected with a simple gas pump or an exchangeable needle head type hermetically sealed injector to extract and concentrate a target material; after the extraction, the device is combined with the gas chromatography to realize thermal desorption under the condition of inert gas serving as a carrier gas and a high temperature of a vaporizing chamber so as to perform the separation and detection in the gas chromatography. The device can also store a sample by sealing the two ends of the device with a Teflon seal head for subsequent analysis when a field test is unavailable. The extraction device can be applied to the analysis of the fast extraction of a trace amount of gas samples in the chemical field.
Description
Technical field
The present invention relates to a kind of needle type extraction device and using method that is used for gas chromatographic analysis, be exactly to develop a kind of centralized procurement sample, extraction, enrichment method or rather, be used to volatilize and the analysis of half volatile organic compound in the novel sample pre-treatments technology of one.The invention belongs to technical field of analytical chemistry, described device can be applicable to environmental analysis.
Background technology
Solid-Phase Extraction (solid phase extraction, SPE) and solid-phase microextraction (solid phasemicroextraction SPME) is at present comparatively advanced sample pre-treatments technology, and these two kinds of technology are based on the adsorbent extraction and grow up.Solid-Phase Extraction is to utilize adsorbent with the absorption of the target compound in the fluid sample, separates with interfering material with the matrix of sample, uses the eluent wash-out again, finally reaches the purpose of separation and enrichment target compound.(liquidliquid extraction LLE) compares, and the SPE technology has many good qualities: the quantity of solvent that needs is little, easy and simple to handle, and environmental pollution is little, and is cheap with liquid-liquid extraction.At present, this technology has been widely used in every field such as medicine, environment, food, agricultural.But it also has some shortcomings, such as: the recovery and the precision of target compound are lower, are not suitable for the micro constitutent analysis.SPME is based on a kind of novel extraction technology that the SPE technology grows up in the early 1990s, and it is a kind of solvent-free abstraction technique.This technology centralized procurement sample, extraction, enrichment method are in one, and in the robotization of implement device, there has been very big improvement aspects such as microminiaturization.Yet SPME also has some limitation, and for example the target compound enriching quantity is little, and extracting head fractures easily, and price is high.
For the microminiaturization that adapts to analytical instrument, the development trend of robotization, the accuracy height simply saves time, and solvent-free novel extraction Study on Technology is becoming one of the advanced subject in analytical chemistry field, also is the mission requirements of advocating the Green Chemistry theory.In recent years, some novel extraction Study on Technology and development constantly are being applied to analytical chemistry and other field.Research based on the adsorbent abstraction technique has a lot of reports, calendar year 2001, Lipinski[Lipinski J, " Automated solid phase dynamic extraction-Extraction of organics usinga wall coated syringe needle " Fresenius J.Anal.Chem.2000,367:445-449.] developed solid phase dynamic extraction technology (solid phase dynamic extraction, SPDE), and the needle type extraction device that will have the sorbing material coating is applied to the extraction of pesticide, investigated the parameter condition of various influences extractions.
Compare with traditional SPME technology, needle type extraction device has following clear superiority: (1) is strong to the accumulation ability of target compound; (2) sample processing throughput height; (3) recovery, accuracy and precision height; (4) realize the robotization of sample preparation and instrumental analysis easily; (5) physical strength height is not easy to damage long service life.
Summary of the invention
The purpose of this invention is to provide a kind of trace volatile organic compounds (volatileorganic compound that is applicable to, VOC) and half volatile organic compound (semi-volatile organiccompound, SVOC) sampling, extraction, the needle type extraction device and the using method thereof that concentrate.This device has overcome shortcomings such as the poor selectivity, the accumulation ability that occur in the existing abstraction technique are low, bad mechanical strength, and can with the gas chromatography coupling, easy to use, for the accurate analysis of trace gas provides a novel abstraction technique with detecting.
A kind of needle type extraction device provided by the invention is characterized in that described extraction equipment comprises a resistant to elevated temperatures stainless steel syringe needle, and the end of syringe needle is to put down mouth, and its other end needle stand can be connected with exchangeable needle formula airproof syringe; One section adsorbent is filled as extraction media in the inside of syringe.Wherein adsorbent can use commercial adsorbent or adopt molecular imprinting synthetic voluntarily, is used for target substance is carried out the high selectivity extraction.It is 10-50mm that adsorbent is typically filled length, and the adsorbent two ends are fixed by resistant to elevated temperatures glass wool, should guarantee after the filling that the adsorbent in the needle tubing has aeration, so that gaseous sample can be by the adsorbent microballoon by its selective adsorption; After extracting operation is finished, can be directly by means of the mouth that carries out of gas chromatography, inert gas is done under the situation of carrier gas, carries out sufficient thermal desorption at vaporizer, and then realizes that gas chromatography is separated and detection; In the time can't realizing on-the-spot the detection, available special teflon end socket seals the device two ends, seals adsorbed gas, can carry out subsequent analysis after the preservation and detect.
Particularly, before carrying out sample extraction, at first needle type extraction device is inserted thermal desorption device or gas chromatography injection port, at vaporizer to the device 1-10min that wears out; Needle stand end with extraction equipment after the cooling is connected with gas pump or impermeability syringe, tip portion is inserted into gas sampling bag or other sample collecting apparatus, open gas pump or pulling impermeability syringe to sample enforcement extraction, the extraction volume is decided according to the actual requirements; After extraction is finished, needle type extraction device is taken off, be connected with exchangeable needle formula small size airproof syringe immediately, this syringe is drawn a spot of inert gas in advance, needle type extraction device is inserted into the gas chromatography injection port, the pushing syringe push rod makes the target extract realize thermal desorption under inert gas and vaporizer hot conditions simultaneously; The material that is extracted is detected after separating through gas chromatography.
The present invention compares with existing solid-phase micro-extracting device, has the sample processing throughput height, and accumulation ability is strong, realizes the advantages such as robotization of instrumental analysis easily.In addition, this device can overcome the fragile easily broken shortcoming of solid-phase micro-extraction fibre extracting head, and increase serviceable life greatly.
Description of drawings
Fig. 1 is a needle type extraction device structural representation of the present invention.
Fig. 2 is that needle type extraction device is connected extraction sample synoptic diagram with the large volume syringe.
Fig. 3 is with extraction equipment and small size syringe connection diagram after extraction is finished.
Fig. 4 is that needle type extraction device and gas chromatography coupling are carried out thermal desorption and analyzed synoptic diagram.
Fig. 5 is for using the gas chromatogram that the present invention extracts trace benzene series thing post analysis.
Among the figure: 1-high temperature resistant stainless steel syringe needle; 2-extracts adsorbent; 3-pyroceram cotton; The 4-needle stand; 5-large volume impermeability syringe; 6-gas sampling bag or gathering-device; 7-small size impermeability syringe; The 8-inert gas; The 9-vaporizer; The 10-gas chromatography.
Embodiment
Below in conjunction with accompanying drawing and example operating position of the present invention and characteristics are further specified.
Fig. 1 is a needle type extraction device structural representation of the present invention.This device is made of the glass wool of stainless steel syringe needle, filling adsorbent and the fixed adsorbent of a 21G standard specification.
Fig. 2 is that needle type extraction device is connected extraction sample synoptic diagram with the large volume syringe.Four kinds of benzene series thing calibrating gas with the extraction low concentration are that example is elaborated to extraction process below.Use inert gas to prepare the calibrating gas of the benzene of trace, toluene, ethylbenzene, o-xylene in the gas sampling bag, the needle stand 4 of needle type extraction device is connected with simple gas pump or large volume impermeability syringe 5, needle point is inserted in the gas sampling bag 6, open gas pump or pulling injector push-rod, make calibrating gas in the sampler bag by adsorbent, it is adsorbed that four kinds of target components are adsorbed agent.
As shown in Figure 3, after extraction is finished, take off large volume syringe 5, be replaced by the small size impermeability syringe 7 of drawing small amounts of inert gas 8 in advance, prepare to carry out thermal desorption and analysis with gas chromatography 10 couplings.
As shown in Figure 4, the composite set among Fig. 3 is inserted into the injection port of gas chromatography 10, the push rod of pushing syringe 7 makes inert gas pass through adsorbent, realizes thermal desorption to four kinds of target substances by means of the high temperature of vaporizer 9 simultaneously.Four kinds of materials after the desorb are detected after separating by gas chromatographic column.
Among the embodiment shown in Figure 5, use the nitrogen compound concentration only to be the potpourri of the foregoing four kinds of benzene series things of 5ng/mL, after using needle type extraction device extraction 50mL of the present invention, assay determination is carried out in direct and gas chromatography coupling, and its gas chromatogram as shown in Figure 5.1-benzene among Fig. 5; 2-toluene; 3-ethylbenzene; The 4-o-xylene.
Claims (4)
1. needle type extraction device that is used for gas chromatographic analysis is characterized in that:
1. described needle type extraction device is enclosed glass wool (3) formation of syringe with solid-phase adsorbent (2), with adsorbent by a high temperature resistant all steel syringe needle (1), filling.
The end portion of 2. described syringe needle (1) is flat mouth, and its other end needle stand (4) can be connected with exchangeable needle formula airproof syringe (5 or 7), conveniently to sample and the desorb operation.
3. described syringe needle two ends can seal by enough special teflon end sockets, so that stored sample.
2. needle type extraction device as claimed in claim 1, the internal diameter that it is characterized in that stainless steel syringe needle (1) is 0.51mm, external diameter is 0.82mm, enters vaporizer and carries out desorb to be suitable for piercing through gas chromatography injection port liner.
3. needle type extraction device as claimed in claim 1, the needle tubing length that it is characterized in that stainless steel syringe needle (1) is 80mm, to make things convenient for sample collecting.
4. needle type extraction device as claimed in claim 1 is characterized in that the Solid-Phase Extraction media that adopts is commercial adsorbent or synthetic voluntarily molecularly imprinted polymer.
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| CN 201010215901 CN101871921A (en) | 2010-07-02 | 2010-07-02 | Needle type extraction device suitable for gas chromatography and using method |
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| CN 201010215901 CN101871921A (en) | 2010-07-02 | 2010-07-02 | Needle type extraction device suitable for gas chromatography and using method |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102062763A (en) * | 2010-12-07 | 2011-05-18 | 中国科学院南京土壤研究所 | Sampling device |
| CN102419355A (en) * | 2011-09-02 | 2012-04-18 | 娄大伟 | Molecular engram integral-pin type extraction device suitable for gas chromatography analysis |
| CN102565236A (en) * | 2011-12-31 | 2012-07-11 | 聚光科技(杭州)股份有限公司 | Substance testing method |
| CN103558322A (en) * | 2013-11-01 | 2014-02-05 | 上海化工研究院 | Low-temperature pressurization head space sample injection device for measuring volatile substances in atmosphere through GC-MS (gas chromatography-mass spectrometer) technology |
| CN103675157A (en) * | 2013-09-18 | 2014-03-26 | 中国地质大学（武汉） | Rapid pre-treatment method and device for crude oil sample |
| CN104391063A (en) * | 2014-12-01 | 2015-03-04 | 吉林大学 | New purpose of miniature-needle trapping device |
| CN103995069B (en) * | 2014-05-23 | 2016-03-09 | 吉林大学 | The microneedle capturing device of volatilization Semi-volatile organism emergency monitoring and using method |
| 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 |
| CN106422413A (en) * | 2016-09-14 | 2017-02-22 | 济南海能仪器股份有限公司 | Injection needle used on mechanical arm type solid-phase extraction instrument |
| CN110361462A (en) * | 2019-06-21 | 2019-10-22 | 深圳市检验检疫科学研究院 | Molecular engram tip micro-extracting head and preparation method thereof |
| CN115453018A (en) * | 2022-04-06 | 2022-12-09 | 吉林化工学院 | Preparation and application of cyclodextrin modified biochar coating fiber filling needle trap micro-extraction device |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101672734A (en) * | 2008-10-04 | 2010-03-17 | 华东理工大学 | A dynamic membrane sampler for trace components in air and method for detecting the trace components in the air |
-
2010
- 2010-07-02 CN CN 201010215901 patent/CN101871921A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101672734A (en) * | 2008-10-04 | 2010-03-17 | 华东理工大学 | A dynamic membrane sampler for trace components in air and method for detecting the trace components in the air |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102062763A (en) * | 2010-12-07 | 2011-05-18 | 中国科学院南京土壤研究所 | Sampling device |
| CN102419355A (en) * | 2011-09-02 | 2012-04-18 | 娄大伟 | Molecular engram integral-pin type extraction device suitable for gas chromatography analysis |
| CN102565236A (en) * | 2011-12-31 | 2012-07-11 | 聚光科技(杭州)股份有限公司 | Substance testing method |
| CN103675157B (en) * | 2013-09-18 | 2015-10-14 | 中国地质大学（武汉） | A kind of quick pretreatment method of crude oil sample |
| CN103675157A (en) * | 2013-09-18 | 2014-03-26 | 中国地质大学（武汉） | Rapid pre-treatment method and device for crude oil sample |
| CN103558322A (en) * | 2013-11-01 | 2014-02-05 | 上海化工研究院 | Low-temperature pressurization head space sample injection device for measuring volatile substances in atmosphere through GC-MS (gas chromatography-mass spectrometer) technology |
| CN103995069B (en) * | 2014-05-23 | 2016-03-09 | 吉林大学 | The microneedle capturing device of volatilization Semi-volatile organism emergency monitoring and using method |
| CN104391063A (en) * | 2014-12-01 | 2015-03-04 | 吉林大学 | New purpose of miniature-needle trapping device |
| 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 |
| CN106422413A (en) * | 2016-09-14 | 2017-02-22 | 济南海能仪器股份有限公司 | Injection needle used on mechanical arm type solid-phase extraction instrument |
| CN110361462A (en) * | 2019-06-21 | 2019-10-22 | 深圳市检验检疫科学研究院 | Molecular engram tip micro-extracting head and preparation method thereof |
| CN115453018A (en) * | 2022-04-06 | 2022-12-09 | 吉林化工学院 | Preparation and application of cyclodextrin modified biochar coating fiber filling needle trap micro-extraction device |
| CN115453018B (en) * | 2022-04-06 | 2023-06-09 | 吉林化工学院 | Preparation and application of cyclodextrin modified biochar coating fiber filling needle trap microextraction device |
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Application publication date: 20101027 |