CN102636595A - Continuous gas in-tube solid phase microextraction device combined with gas chromatography for use - Google Patents

Continuous gas in-tube solid phase microextraction device combined with gas chromatography for use Download PDF

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CN102636595A
CN102636595A CN2012101067796A CN201210106779A CN102636595A CN 102636595 A CN102636595 A CN 102636595A CN 2012101067796 A CN2012101067796 A CN 2012101067796A CN 201210106779 A CN201210106779 A CN 201210106779A CN 102636595 A CN102636595 A CN 102636595A
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gas
solid phase
phase microextraction
tube
sample
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CN2012101067796A
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朴相范
李东浩
赵娜娜
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延边大学
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Abstract

The invention discloses a continuous gas in-tube solid phase microextraction device combined with gas chromatography (GC) for use. The continuous gas in-tube solid phase microextraction device comprises a continuous gas in-tube solid phase microextraction device and a sampling device, wherein the continuous gas in-tube solid phase microextraction device is composed of an in-tube solid phase microextraction needle, a semiconductor condenser, a microheater and an inert gas connecting pipe, and the sampling device is composed of the in-tube solid phase microextraction needle, and a stop valve, a carrier gas flow controller and a gas source which are connected in sequence through a connector connected with a port of an extraction needle on one end of the in-tube solid phase microextraction needle and are used with the gas chromatography. According to the invention, the extraction needle performs thermal desorption at a GC sample inlet without changing the GC sample inlet and thus the continuous gas in-tube solid phase microextraction device is applied to the GC with any brand. The invention has the advantages of simple operating method, high extraction rate, accurate quantification, hydrophilic environment, convenient automatic operation and the like and also provides a sample pretreatment method integrated with extraction, separation and concentration. The continuous gas in-tube solid phase microextraction device can greatly promote the combination use of the SPME (solid phase microextraction) technology and the GC/MS (mass spectra) technology and applications of micro constituents in complex samples in aspects of on-site analysis, on-line analysis and in-situ analysis.

Description

与气相色谱联用的连续气体管内固相微萃取装置 Gas chromatography and gas in a continuous solid phase microextraction tube apparatus associated with the

技术领域 FIELD

[0001] 本发明涉及一种固相微萃取样品前处理方法并与气相色谱联用装置,具体是指一种与气相色谱联用的连续气体管内固相微萃取装置。 [0001] The present invention relates to gas chromatography combined with means, in particular to a gas chromatograph coupled with a continuous pipe gas solid phase microextraction device for sample processing before the phase microextraction method solid.

背景技术 Background technique

[0002] 对挥发性或半挥发性的微量/痕量有机成分分析而言,固相微萃取(SPME)技术和气相色谱/质谱(GC/MS)分析技术是当前最富有魅力的样品前处理技术和分析工具。 [0002] volatile or semi-volatile micro / organic trace component analysis, the solid phase microextraction (the SPME) technique and gas chromatography / mass spectrometry (GC / MS) analysis before the sample is the most attractive process technical and analytical tools. 固相微萃取是1989年由Pawliszyn等提出并发展起来的快速、灵敏、方便地适用于气体和液体样品的新颖样品前处理技术。 Solid phase microextraction 1989 and the like proposed by Pawliszyn develop rapid, sensitive, easy to apply before the new sample gas and the liquid sample handling techniques. 该技术是在固相萃取(SPE)的基础上发展起来的一种新的萃取分离技术。 This technique was developed based on solid phase extraction (SPE) on a new extraction technology. 它几乎克服了传统样品处理方法的所有缺点。 It overcomes almost all of the disadvantages of the conventional sample processing methods. 无需有机溶剂、简单方便、测试快、费用低,集采样萃取、浓缩、进样于一体,能够与气相或液相色谱仪联用,可手动和自动操作,使得样品处理技术及分析操作简单省时。 No organic solvent, simple, rapid test, low cost, sample set extraction, concentration, in one sample, can be used in combination with gas or liquid chromatography, can be manual and automatic operation, so that sample processing and analysis operations simple Province Time. 基于上述优点,固相微萃取一经问世便得到了快速发展,进入分析化学的各个领域。 Based on the above advantages, the solid phase micro extraction will be available to the rapid development into various fields of analytical chemistry. SPME经过近二十年的发展,已经出现了多种形式,包括纤维针式固相微萃取(Fiber-SPME),管内固相微萃取(In-tube-SPME)等。 SPME After nearly two decades of development, there have been a variety of forms, including solid-phase microextraction fiber needle (Fiber-SPME), the inner tube solid-phase microextraction (In-tube-SPME) and the like. 但固相微萃取也仍然存在某些不足,有待于进一步发展和完善,如可靠性差、定量不准确,萃取的富集倍数和选择性仍有待进一步提高等。 Solid phase microextraction but there are some deficiencies still needs further development and improvement, such as poor reliability, inaccurate quantitative, selective extraction and enrichment factors yet to be further improved and the like. 目前所使用的顶空-固相微萃取方法具有萃取、纯化、浓缩为一体的优点,但是始终没有满足完全富集的要求,并且此方法对半挥发性物质而言总是给出非常低的萃取率。 Currently used headspace - solid phase microextraction method extraction, purification, and concentration of one of the advantages, but has not fully satisfy the requirements of enrichment, and this method for semi-volatile material always gives a very low extraction rate.

发明内容 SUMMARY

[0003] 本发明的目的是克服现有技术的不足而提供一种操作方便可靠、定量准确,萃取及富集率高的与气相色谱联用的连续气体管内固相微萃取装置。 [0003] The object of the present invention is to overcome the disadvantages of the prior art and provide a convenient method of operating a reliable, accurate, and extraction with high enrichment of gas chromatography with the gas continuous tube SPME device.

[0004] 为实现本发明的目的,提供以下技术方案: [0004] To achieve the object of the present invention, there is provided the following technical solutions:

一种与气相色谱联用的连续气体管内固相微萃取装置,由连续气体管内固相微萃取装置和将其与气相色谱联用的进样装置组成,其中所述的连续气体管内固相微萃取装置是由管内固相微萃取针、半导体冷凝器、微型加热器、惰性气体连接管组成,管内固相微萃取针一端设置为萃取针连接口,管内固相微萃取针另一端经半导体冷凝器的传热体置于微型加热器内设置的样品管内,惰性气体连接管经微型加热器底部连接于样品管内; One kind with Gas Chromatography microextraction solid gas continuous tube apparatus, solid phase microextraction unit, and which with the gas chromatography with the sampling device consists of a continuous gas pipe, a continuous gas pipe wherein the solid phase microextraction the extraction means is an inner tube solid phase microextraction needles, semiconductor condenser, a micro-heater, an inert gas connecting pipe, the inner pipe solid phase Microextraction needle end is provided as the extraction pin connector, the other end of the inner tube solid phase microextraction needle through the semiconductor condensed the heat transfer device disposed within the micro-heater is placed in the sample tube, an inert gas through the bottom connection pipe connected to the micro-heater within the sample tube;

所述的进样装置是由上述的管内固相微萃取针、通过与管内固相微萃取针一端萃取针连接口连接的连接头依次连接有的截止阀、载气流量控制器、气体源组成。 Said injection means is formed by said inner tube solid phase microextraction pin, there are sequentially connected via shut-off valve connection port connected to the first inner tube solid phase microextraction extraction pin end of the needle, the carrier gas flow controller, the composition of the gas source .

[0005] 上述的管内固相微萃取针为长50 mm、内径O. 26、. 41 mm的色谱进样注射针,其内壁上涂敷一层厚度为30〜100 μ m的萃取吸附剂,所述的萃取吸附剂为无机材料吸附齐U、有机大分子或有机聚合物。 [0005] The inner pipe of solid-phase microextraction needle length 50 mm, an inner diameter of the needle chromatographic sample O. 26 ,. 41 mm, which layer is coated on an inner wall thickness of 30~100 μ m of the adsorbent extraction, the extraction homogeneous adsorbent adsorbing inorganic material U, organic molecules or organic polymers. 所述的萃取吸附剂为CuCl2、CuS涂层、烷基键合硅胶固定相C8、C18、聚硅氧烷富勒烯涂层或聚苯甲基硅氧烷。 The extracted adsorbent is CuCl2, CuS coating, an alkyl group bonded silica stationary phase C8, C18, fullerene silicone coating or a polyphenylene siloxane.

[0006] 上述的微型加热器是由加热体、加热体内部开有空腔的样品池、放入样品池内的样品管、加热体上部封闭样品池和样品管的进样垫、加热体上设有的加热片和温度传感器、、惰性气体连接管组成,惰性气体连接管经加热体下部开有气体连接接口连接于样品管下部。 [0006] The micro-heater by the heating body, heating the interior cavity of the opening and the sample cell, the sample tube into the sample cell, the upper heating body is closed sample cell sample pad and the sample tube, the heating body is provided some heating plate and a temperature sensor ,, inert gas connecting pipe, an inert gas connecting pipe through the lower opening and the heating gas is connected to the lower connection interface sample tube.

[0007] 上述的冷凝器由内部加工有通孔的传热体、传热体上设置的温度传感器、与传热体外壁接触连接的制冷片、与制冷片连接的散热片及风扇组成。 [0007] The internal processing by the condenser heat transfer body with a through-hole, a temperature sensor is provided on the heat transfer body, the heat transfer member in contact with an outer wall connected to the cooling plate, the cooling fan and the heat sink plate and connected components.

[0008] 上述的进样装置是管内固相微萃取针与接头连接,接头经过截止阀连接载气流量控制器,载气流量控制器另一端经过气体气连接管连接以惰性气体钢瓶为主的气体源。 [0008] The injector tube means is a solid-phase microextraction and pin header, shut-off valve is connected via the joint carrier gas flow controller, a carrier gas through a gas flow controller and the other end connected to an inert gas connecting pipe of the gas cylinder based gas source.

[0009] 所述的管内固相微萃取针热解吸在气相色谱进样口进行。 [0009] The inner tube Solid Phase Microextraction needles in thermal desorption GC injection port.

[0010] 本发明包括两个部分:第一部分为连续气体管内固相微萃取装置;第二部分为管内固相微萃取针与GC联用进样装置。 [0010] The present invention comprises two parts: the first part is a solid phase microextraction gas continuous tube means; second portion into the sample tube apparatus Solid Phase Microextraction by GC-needles. 其工作原理:石英玻璃样品管(长20 mm、直径5 mm、 壁厚O. 5 mm)底部装入一定量玻璃棉,玻璃棉上方放入微量固体或液体样品,把样品管放入微型加热器里面的样品池内,然后盖上耐温硅胶进样垫,萃取针通过冷凝器和进样垫插入加热器里。 Its working principle: a quartz glass sample tube (length 20 mm, diameter 5 mm, thickness O. 5 mm) was charged a certain amount of glass wool at the bottom, the top of the glass wool into a solid or liquid micro sample, the sample tube into the micro heating inside the sample cell is then covered with the sample pad of silica gel temperature and extracted through a needle inserted into the condenser and the heater mat in the sample. 加热器100°C /分速率进行加热升温(加热温度20(T350°C),同时从加热器底部吹扫惰性气体(流量O. 5〜2ml/min),惰性气体把样品中蒸发的挥发性、半挥发性目标物吹过固相萃取针管内时,被固相吸附剂冷凝富集,冷凝富集温度为_20°C左右。几分钟的富集结束后拔出萃取针与接头连接,同时移到气相色谱进样口后萃取针迅速插入到进样口里,萃取针在GC衬管进行热解吸,充分解析后,惰性气体吹萃取针,使气化的目标物送到色谱柱进行分析。 The heater 100 ° C / min rate of heating temperature (heating temperature 20 (T350 ° C), while an inert gas purge (flow rate O. 5~2ml / min) from the bottom of the heater, the sample gas evaporated in the inert volatile when the object is blown through semi-volatile solid-phase extraction tube inner needle is solid phase adsorbent enriched condensate, condensing temperature of about enriched _20 ° C. after a few minutes pulled enriched extraction pin connector is connected, GC injector is moved while the rear mouth rapid extraction needle is inserted into the injection mouth, needle extraction thermal desorption GC liner was thoroughly resolved, an inert gas blow needle is extracted, the object to vaporized column for analysis.

[0011] 本发明是固相微萃取的延伸,比现有的石英纤维SPME显著地增加了萃取表面积。 [0011] The present invention extends the solid phase micro extraction, significantly increasing the extracted surface area than a conventional quartz fiber SPME. 在高温下,被气化的目标物随着惰性气体的气流达到萃取针内壁表面,然后被涂敷的吸附剂而富集,从而实现目标物的完全萃取。 At high temperature, with the object to be vaporized stream of an inert gas to reach the inner wall surface of the needle is extracted, and then the coated adsorbent enriched in order to achieve complete extraction of the object. 萃取针热解吸可以用独立的热解吸装置,也可以用气相色谱仪(GC)进样口作为热解吸装置。 Needle extraction thermal desorption may be used independently of the thermal desorption apparatus, gas chromatography may be used (GC) as a thermal desorption inlet means. 本发明是在GC进样口进行热解吸,把萃取后的注射针插到GC进样口,热解吸一段后,利用惰性气体吹扫进样,所以不改动GC进样口,可使用于任何品牌的GC。 The present invention is in the GC injection port for feeding thermal desorption, the extract after the injection needle into the GC inlet, after a period of thermal desorption, purging with an inert gas injection, so do not change the GC inlet, may be used to any brand of GC. 本发明克服了富集率低、易碎、柱头昂贵、需要装用设备等问题,具有操作方法简单、萃取率高、定量准确、亲环境、易自动化等优点,是一种集提取、分离、浓缩为一体的样品前处理方法。 The present invention overcomes the low enrichment, fragile, expensive stigma, and other issues need to install equipment, with simple operation, high extraction efficiency, accurate, environment-friendly, easy to automate, etc., is a set of extraction, separation, concentration as one of the sample before treatment. 本发明将极大地推进SPME技术与GC/MS的联用以及复杂样品中微量成分的现场、在线、原位分析方面的应用。 The present invention will greatly promote the application associated with the field trace components in complex samples, online and in-situ analysis of SPME technology and the GC / MS.

附图说明 BRIEF DESCRIPTION

[0012] 图I是本发明连续气体管内固相微萃取装置结构示意图。 [0012] FIG. I is a schematic of the present solid phase microextraction gas continuous tube apparatus inventive structure.

[0013] 图2是本发明与气相色谱GC联用的进样装置结构示意图。 [0013] FIG. 2 is a schematic view of the structure of the injection apparatus of the present invention in combination with gas chromatography GC.

[0014] 图I中,I.萃取针,2.制冷片,3.传热体,4.进样垫,5.加热片,6.加热体,7.惰性气体连接管,8.温度传感器,9.玻璃棉,10.样品,11.样品管,12.散热片,13.风扇,19.萃取针接口,21.温度传感器。 [0014] In Figure I, I. And extracted needle, 2 coolers, 3 heat transfer body 4. Sample pad 5 heated sheet, 6. heating body 7. Inert gas connecting pipe 8. The temperature sensor , 9. wool, 10. The sample 11 sample tube, 12 fin, 13 fan, 19, extracted needle hub, 21 temperature sensor.

[0015] 图2中,14.气体连接管,15.载气流量控制器,16.截止阀,17.接头,18. GC进样口,20. GC/MS。 In [0015] FIG. 2, 14 gas connection pipe 15. The carrier gas flow controller, 16 valve, 17. Joint, 18. GC injection port, 20. GC / MS.

具体实施方式 detailed description

[0016] 与气相色谱联用的连续气体管内固相微萃取装置,由连续气体管内固相微萃取装置和将其与气相色谱联用的进样装置两部分组成,连续气体管内固相微萃取装置如图I,是由管内固相微萃取针I、半导体冷凝器、微型加热器、惰性气体连接管7组成,管内固相微萃取针I采用HAMILTONRN带金属手持部的更换针,型号为N726、N724、N723、N722等,针长为50mm,内径为O. 26〜O. 41 mm,注射针管内壁通过电化学的方法、溶胶凝胶法或直接氧化法涂覆萃取吸附剂(涂层),吸附剂可用无机材料吸附剂、有机大分子或有机聚合物,即CuCI2XuS涂层、烷基键合硅胶固定相C8、C18、聚硅氧烷富勒烯涂层或聚苯甲基硅氧烷等吸附材料。 [0016] and gas chromatography with microextraction solid phase within a continuous gas pipe means, a continuous gas tube solid phase microextraction device and which with GC sampling device in combination with the two parts, solid phase micro extraction in a continuous gas pipe FIG apparatus I, the inner tube by solid phase microextraction needles I, semiconductor condenser, a micro-heater, consisting of an inert gas connecting pipe 7, the inner tube needle I of the solid-phase microextraction using HAMILTONRN belt replacing metal needle holding portion, model N726 , N724, N723, N722, etc., the needle length of 50mm, an inner diameter of O. 26~O. 41 mm, an inner wall of the needle tube by electrochemical method, a sol-gel method, or direct oxidation and extracted adsorbent coated (coating) , with inorganic adsorbent adsorbent material, an organic macromolecule, or organic polymers, i.e. CuCI2XuS coating, an alkyl group bonded silica stationary phase C8, C18, polystyrene or polysiloxane coating dimethylsiloxane fullerene and other absorbent material. [0017] 冷凝器由内部加工有通孔的传热体3、传热体上设置的数字温度传感器21、与传热体外壁接触连接的制冷片2、与制冷片2连接的散热片12及风扇13组成,具体为:制冷片2为二级半导体制冷片由FPH1-7103NC (电压8. 8V,电流3A)和FPH1-12703AC (电压15. 7V,电流3A)半导体制冷片模块叠加而成,制冷片的冷端贴传热体3,制冷片的热端与散热片12及风扇13相连,传热体3内部加工了一个直径为O. 8_的通孔,用以放置固相微萃取针1,固相微萃取针I和萃取针接口19连成一体。 [0017] The digital processing by an internal condenser temperature sensor is provided on the 3, heat transfer heat transfer through hole 21, the refrigerant heat transfer sheet in contact with the outer wall 2 is connected with the cooling fins 12 and the second connecting plate composition fan 13, specifically: a semiconductor for the two cooling plate 2 sheet by the cooling FPH1-7103NC (voltage 8. 8V, current 3A) and FPH1-12703AC (voltage 15. 7V, current 3A) peltier module superposition sheet, refrigeration attached to the cold end heat transfer sheet 3, sheet cooling the hot end of the heat sink 12 and fan 13 are connected, the heat transfer body 3 inside a machined through hole diameter O. 8_ allowed to stand for solid-phase microextraction a needle, needle I of the solid phase microextraction extraction needle hub 19 and integrally connected. 管内固相微萃取针另一端经传热体6的通孔置于微型加热器内设置的样品管11内。 Solid phase microextraction inner tube the other end of the needle through the through hole 6 of heat placed in a sample tube 11 provided in the micro heater body.

[0018] 微型加热器是由加热体6、加热体6内部开有圆柱形空腔的样品池、摆放于样品池内的样品管11、加热体6上部封闭样品池和样品管的进样垫4、加热体6上设有的加热片5和温度传感器8、惰性气体连接管7组成,由不锈钢制成的惰性气体连接管7经加热体下部开有气体连接接口连接于样品管下部,通过惰性气体连接管7可向微型加热器中通入惰性气体。 [0018] The micro-heater is a heater 6, the heating body 6 inside a cylindrical cavity open sample cell, placing the sample tube in the sample cell 11, an upper heating body 6 enclosed sample cell and the sample injection tube pad 4, the heating member 6 provided on the heating plate 5 and a temperature sensor 8, the composition of the inert gas connecting pipe 7, the inert gas is made of stainless steel tube connected to the heating body 7 is opened through the lower gas connecting interface to the lower sample tube, through inert gas connecting pipe 7 can pass into the inert gas in the micro-heater. 进行萃取实验时,样品10置入样品管中玻璃棉9层的上方,进行加热。 When the extraction experiment, 10 samples were placed above the sample tube 9 of glass wool layer, it is heated. 加热器由高温硅胶进样垫4密封,不锈钢惰性气体连接管7由加热器底部接入样品管11内部。 The injection temperature silicone heater mat 4 sealed stainless steel tube connected to inert gas from the bottom of the heater inside 7 access the sample tube 11.

[0019] 上述的传热体3可为紫铜传热体,进样垫4可为高温硅胶进样垫,加热片5可为氧化铝陶瓷加热片,加热体6可为铜加热体,温度传感器8可为钼电阻温度传感器,样品管11可为石英玻璃样品管,温度传感器21可为数字温度传感器。 [0019] The heat transfer member may be a copper heat transfer body 3, the injection temperature silicone pad 4 may be a sample pad, a heating plate 5 may be an alumina ceramic sheet is heated, the heating member 6 may be a copper heater, a temperature sensor 8 may be a molybdenum resistance temperature sensor, sample tube 11 may be a quartz glass sample tube, a temperature sensor 21 may be a digital temperature sensor.

[0020] 进样装置的管内固相微萃取针I与接头17连接,接头17经过截止阀16连接载气流量控制器15,载气流量控制器15另一端经过气体气连接管14连接以惰性气体钢瓶为主的气体源。 [0020] Solid phase microextraction inner tube and the connector 17 is connected to pin I sampling device, shut-off valve fitting 17 through gas flow controller 16 connected to the carrier 15, the carrier gas flow controller 15 connected to the other end of the gas through the gas pipe 14 is connected to an inert gas cylinder based gas source. 如图2中,载气流量控制器15经过气体气连接管14连接惰性气体钢瓶,载气流量控制器15另一端经过截止阀16和接头17及微萃取针接口19连接微萃取针I,微萃取针I插入气相色谱仪进样口18,再与GC/MS20相连接。 2, the carrier gas through a gas flow controller 15 connected to the gas pipe 14 is connected to an inert gas cylinder, the other end of the carrier 15 via gas flow controller 16 and shut-off valve fitting 17 and needle hub 19 is connected microextraction microextraction needles I, micro I extraction needle is inserted into a gas chromatograph injection port 18, and then connected to the GC / MS20. 微萃取针热解吸在气相色谱进样口进行。 Microextraction needles in thermal desorption GC injection port. 载气流量控制器15可由微流量传感器、分流器通道、电磁调节阀构成。 Carrier gas flow rate controller 15 may be comprised of a micro flow sensor, a channel splitter, magnetic valves.

[0021] 连续气体管内固相微萃取与气相色谱联用方法:本方法以干燥植物样品前处理及挥发油分析作为实施实例。 [0021] The continuous pipe gas and solid phase microextraction gas chromatography method: This method prior to drying and handling plant volatile oil sample analysis as an example.

[0022] 样品采集与保存:根据中国药典或相关中药类书籍和实验要求,将采集来的植物样品进行晾晒或阴干(当采用间接处理法时可以直接冷冻保存),将样品剪成小片或粉碎过筛(200目),放到棕色瓶中,冷冻保存(-4° C)。 [0022] Sample collection and preservation: according to China Pharmacopeia or related medicine books and test requirements to a plant sample collected for drying or dried (when using the indirect approach may be directly frozen), the samples were cut into small pieces or pulverized sieved (200 mesh), placed in a brown bottle and stored frozen (-4 ° C).

[0023] 样品称量:使用电子分析天平(差减法)进行称量5 mg。 [0023] The sample is measured: using an electronic analytical balance (subtraction) was weighed 5 mg.

[0024] 装样:用镊子在两通的样品管的下端装入一定量玻璃棉,将称量好的样品慢慢倒入样品管内,随后用镊子取一定量玻璃棉装入到样品管的上端。 [0024] Sample loading: tweezers amount of glass wool was charged through the lower end of the two sample tube, the sample was slowly poured into the weighed sample tubes, and then a certain amount of glass wool was charged with forceps to sample tube the upper end.

[0025] 固相微萃取:样品管放入加热器的样品池中,塞上进样垫,萃取针通过冷凝器穿刺进样垫,针尖刚好穿过进样垫底端即可。 [0025] Solid phase microextraction: heater sample tube into the sample cell, the plug-like progress pad, condenser extraction puncturing needle injection through a pad of injection needle just passing through the bottom end of the can. 设置加热温度280°C,惰性气体流速lm/min,冷凝温度_20°C,萃取时间6分钟。 The heating temperature of 280 ° C, an inert gas flow rate of lm / min, the condensation temperature of _20 ° C, the extraction time of six minutes. 先启动冷凝器使冷凝温度达到设定值之后进行加热萃取。 First start after the extraction is heated condenser condensing temperature reaches the set value. [0026] 气相色谱进样: 萃取结束后萃取针迅速插入到GC进样口里,萃取针在GC衬管进行I〜3分钟热解吸。 [0026] Gas chromatographic sample: after extraction rapid extraction needle is inserted into the mouth GC injector, the needle is extracted in I~3 minutes for GC liner thermal desorption. 充分解析后,打开钢瓶阀和减压阀,压力调整为比气相色谱仪原柱前压高出O. IMpa左右,打开截止阀,被解吸出的样品蒸汽瞬间被吹洗到仪器的汽化室中,从而实现了色谱进样分析。 After sufficient resolution, open the cylinder and pressure reducing valve, pressure was adjusted to the previous gas chromatograph column pressure above about the original O. IMpa, shut-off valve is opened, the sample is desorbed vapor is purged into the instant apparatus the vaporization chamber sample analysis, thereby achieving chromatography. 流量控制器控制流量为I〜2mL,进样时间为10〜20秒。 The flow controller controls the flow I~2mL, injection time of 10-20 seconds.

Claims (7)

1. 一种与气相色谱联用的连续气体管内固相微萃取装置,由连续气体管内固相微萃取装置和将其与气相色谱联用的进样装置组成,其特征在于: 所述的连续气体管内固相微萃取装置是由管内固相微萃取针、半导体冷凝器、微型加热器、惰性气体连接管组成,管内固相微萃取针一端设置为萃取针连接口,管内固相微萃取针另一端经半导体冷凝器的传热体置于微型加热器内设置的样品管内,惰性气体连接管经微型加热器底部连接于样品管内; 所述的进样装置是由上述的管内固相微萃取针、通过与管内固相微萃取针一端萃取针连接口连接的连接头依次连接有的截止阀、载气流量控制器、气体源组成。 A gas chromatography with the use of a solid phase microextraction gas continuous tube apparatus, and a solid phase microextraction device with the gas chromatography with the sampling device consists of a continuous gas pipe, characterized in that: said continuous inner gas pipe solid phase microextraction device consists of an inner tube solid phase microextraction needles, semiconductor condenser, a micro-heater, an inert gas connecting pipe, the inner pipe solid phase Microextraction needle end is provided as the extraction pin connector port, the inner tube solid phase microextraction needle the other end of the heat transfer through the condenser is placed a semiconductor micro-heater disposed within the sample tube, an inert gas through the bottom connection pipe connected to the micro-heater sample tube; said apparatus is a micro sample extracted from the inner tube of the above-described solid phase pins, connected to the connector port is connected to the inner tube via a needle extraction solid phase microextraction sequentially connecting pin end and some cut-off valve, the carrier gas flow controller, the composition of the gas source.
2.根据权利要求I所述的与气相色谱联用的连续气体管内固相微萃取装置,其特征是所述的管内固相微萃取针为长50 mm、内径O. 26、. 41 mm的色谱进样注射针,其内壁上涂敷一层厚度为30〜100 μ m的萃取吸附剂,所述的萃取吸附剂为无机材料吸附剂、有机大分子或有机聚合物。 The I and the solid phase microextraction with inline continuous gas pipe gas chromatography apparatus, characterized in that the solid phase micro extraction needle within said tube length 50 mm, an inner diameter O. claimed in claim 26 ,. 41 mm chromatographic injection needle, on its inner wall is coated to a thickness of 30~100 μ m of the adsorbent extraction, the extracted adsorbent is an adsorbent inorganic material, an organic macromolecule or organic polymers.
3.根据权利要求I所述的与气相色谱联用的连续气体管内固相微萃取装置,其特征是所述的微型加热器是由加热体、加热体内部开有空腔的样品池、放入样品池内的样品管、加热体上部封闭样品池和样品管的进样垫、加热体上设有的加热片和温度传感器、惰性气体连接管组成,惰性气体连接管经加热体下部开有气体连接接口连接于样品管下部。 The gas chromatography with the use of a continuous pipe gas SPME device according to claim I, wherein the micro-heater is a heating body, heating the interior cavity of the opening and the sample cell, the discharge the sample tube into the sample cell, the upper heating body is closed sample cell and the sample injection tube pad, provided on the heated sheet and the heated temperature sensor, an inert gas connecting pipe, an inert gas connecting pipe through the lower opening and a gas heating a connection interface connected to a lower portion of the sample tube.
4.根据权利要求I所述的与气相色谱联用的连续气体管内固相微萃取装置,其特征是所述的冷凝器由内部加工有通孔的传热体、传热体上设置的温度传感器、与传热体外壁接触连接的制冷片、与制冷片连接的散热片及风扇组成。 The use of gas chromatography and gas continuous tube SPME device according to claim I, wherein said condenser temperature by the internal working of the heat transfer member disposed through hole, the heat transfer member sensor, a contact piece connected to the refrigerant heat transfer outer wall, connected to the heat sink and fan coolers composition.
5.根据权利要求I所述的与气相色谱联用的连续气体管内固相微萃取装置,其特征是所述的进样装置是管内固相微萃取针与接头连接,接头经过截止阀连接载气流量控制器,载气流量控制器另一端经过气体气连接管连接以惰性气体钢瓶为主的气体源。 The use of gas chromatography and gas continuous tube SPME device according to claim I, wherein said sample means is a tube and solid-phase microextraction pin header, header carrying through shut-off valve gas flow controller, a carrier gas through a gas flow controller and the other end connected to an inert gas connecting pipe gas cylinder based gas source.
6.根据权利要求I所述的与气相色谱联用的连续气体管内固相微萃取装置,其特征是所述的管内固相微萃取针热解吸在气相色谱进样口进行。 The gas chromatography with the use of a continuous pipe gas SPME device according to claim I, wherein said inner tube Solid Phase Microextraction needles in thermal desorption GC injection port.
7.根据权利要求2所述的与气相色谱联用的连续气体管内固相微萃取装置,其特征是所述的萃取吸附剂为CuCl2、CuS涂层、烷基键合硅胶固定相C8、C18、聚硅氧烷富勒烯涂层或聚苯甲基硅氧烷。 The gas chromatograph coupled with a solid phase microextraction gas continuous tube apparatus according to claim 2, wherein said adsorbent is extracted CuCl2, CuS coating, an alkyl group bonded silica stationary phase C8, C18 , polystyrene or polysiloxane coating fullerene siloxane.
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