CN207575847U - A kind of head space micro-extraction device - Google Patents

A kind of head space micro-extraction device Download PDF

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Publication number
CN207575847U
CN207575847U CN201721247045.4U CN201721247045U CN207575847U CN 207575847 U CN207575847 U CN 207575847U CN 201721247045 U CN201721247045 U CN 201721247045U CN 207575847 U CN207575847 U CN 207575847U
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CN
China
Prior art keywords
head space
needle
bottle
extraction device
goblet
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Expired - Fee Related
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CN201721247045.4U
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Chinese (zh)
Inventor
郭秋爽
莫镜池
速敏
高云涛
熊华斌
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Yunnan Minzu University
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Yunnan Minzu University
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Abstract

The utility model discloses a kind of head space micro-extraction device, including ml headspace bottle, microextraction needle and electric heating cover, it is characterised in that:The ml headspace bottle is screw socket ml headspace bottle, and head cover is equipped with hassock piece, and hassock piece center is equipped with the ferrule fitting with aperture;The microextraction needle cylindrical unit is fixed on ferrule fitting, and needle head body is set in sample injection bottle body;The electric heating cover is goblet, and ml headspace bottle bottle is set in goblet;The electric heating cover is equipped with insulated thermal insulating layer equipped with measurement and control of temperature module, goblet outer wall.The utility model uses the design of the traditional head space bottle cap shim liner of hassock piece replacement equipped with cutting ferrule interface, extraction droplet is remained on the vertical line of ml headspace bottle center, and the utility model, using flexible silicone rubber electric heating cover, compact structure, assembling is easy, use scope is wide.

Description

A kind of head space micro-extraction device
Technical field
The utility model is related to a kind of head space micro-extraction device, more particularly to a kind of stability is good, needle point is away from object sample height Adjustable, the convenient head space micro-extraction device of heating, belongs to section's grinding device class field.
Background technology
Head space micro-extraction as a kind of novel Sample Pretreatment Technique, have extraction equipment it is simple, it is easy to operate it is quick, The advantage that consumption of organic solvent is few, bioaccumulation efficiency is high, environmental-friendly, develop in recent years it is very fast, be widely used to food, In the analysis detection of the samples such as drug, environment and biology.Head space list drop micro-extraction is that organic solvent drop is hung on sample is molten The top extraction volatility of liquid and the compound of half volatile.For the more complicated sample of some matrix, sample can be eliminated The interference of matrix effect reduces the requirement to further purifying.
In the head space micro-extraction device reported at present, it is micro- that patent CN200410101811.7 provides a kind of hanging drop type liquid-liquid Extracting process, sample requirements are few, bioaccumulation efficiency is high, but sample introduction needle needle head body can only be passed through the thin of ml headspace bottle head cover by the device Gasket is inserted into ml headspace bottle, and muff folder is cased with outside the extraction flask of the invention, is passed through in set folder by thermostatic water-circulator bath The gas or liquid of the constant temperature of offer keeps the constant of extraction flask temperature;Patent CN200810072068.5 devise from The device of sub- liquid multiple-dropping liquid-phase microextraction, the needle point of microextraction needle pass through the shim liner of seal bottle cap, and needle point connection carries The porous extracting head of machine filter film, temperature regulating device use temperature control magnetic stirring apparatus, can only heat ml headspace bottle bottom device.
Above-mentioned micro-extraction device takes sample introduction needle point to be fixed on the method for the closed shim liner of head cover, and sample introduction needle center of gravity is not Surely, needle point is easily swung, and is not only extracted droplet and is easily fallen, also affects the air-tightness of ml headspace bottle, and be difficult to accurately adjust The distance of droplet and liquid level is extracted, extraction results precision is caused to be deteriorated;In addition, the mode of heating of traditional head space micro-extraction device is equal Water-bath, magnetic agitation heating etc. are taken, device volume is big, sample uneven heating is even, the thermal efficiency is low, and is difficult to reach certain higher Volatilization temperature needed for boiling organics.
Utility model content
The extraction droplet stability that is directed to existing head space micro-extraction device is poor, easy drippage, heating unit volume it is big plus The deficiencies of required temperature that heat is uneven, the higher organic matter that is difficult to meet boiling point volatilizees, the utility model, which uses, is equipped with card The hassock piece of socket replaces the shim liner of traditional head space bottle cap and silicon special rubber-heating set substitution traditional heating side Formula, its object is to:It is good, accurately adjustable away from liquid level to provide a kind of extraction droplet stability, and compact, heating rate Soon, the head space list of the volatile organic matter higher available for processing boiling point drips micro-extraction device.
To achieve the above object, the technical solution adopted in the utility model is:A kind of head space micro-extraction device, including head space Bottle, microextraction needle and electric heating cover, it is characterised in that:The ml headspace bottle is screw socket ml headspace bottle, and head cover is equipped with hassock piece, thick Gasket center is equipped with the ferrule fitting with aperture;The microextraction needle cylindrical unit is fixed on ferrule fitting, and needle head body is set on sample introduction In bottle;The electric heating cover is goblet, and ml headspace bottle bottle is set in goblet;The electric heating cover is surveyed equipped with temperature Module is controlled, goblet outer wall is equipped with insulated thermal insulating layer.
As preferred technical solution, a kind of head space micro-extraction device, it is characterised in that:The screw socket head space Bottle volume is 10-50 mL, and circular hole is equipped among ml headspace bottle head cover, and Circularhole diameter is less than 2 mm of head cover internal diameter, and circular hole position is equipped with Hassock piece.
As preferred technical solution, a kind of head space micro-extraction device, it is characterised in that:The hassock piece is Tetrafluoroethene material, diameter is consistent with head cover Circularhole diameter, and thickness is 4-6 mm, and hassock piece center is equipped with inner bolt hole.
As preferred technical solution, a kind of head space micro-extraction device, it is characterised in that:It is described with aperture Ferrule fitting is set to hassock piece center, and ferrule fitting internal orifice dimension is consistent with microextraction needle cylindrical unit outer diameter.
As preferred technical solution, a kind of head space micro-extraction device, it is characterised in that:The ferrule fitting Include cutting ferrule, fittings body and nut three parts;The cutting ferrule is the hollow short tube body of polytetrafluoroethylene material, inside sets sealing ring, Wall thickness 1 mm, height 4-6 mm;The fittings body height is consistent with hassock piece, and is equipped with what is be coupled with hassock piece center inner bolt hole External screw thread;The nut can realize the fixation and lifting of microextraction needle by adjusting elasticity compresses seal.
As preferred technical solution, a kind of head space micro-extraction device, it is characterised in that:The microextraction Needle is chromatogram sampling needle, volume 10-50 μ L, during installation, microextraction needle, ferrule fitting, ml headspace bottle center line with always On line, and microextraction needle needle point is away from liquid level 0.5-1 cm.
As preferred technical solution, a kind of head space micro-extraction device, it is characterised in that:The heating mantle is The goblet that the silicon rubber heating plate of low profile flexible is rolled into, goblet internal diameter are slightly larger than ml headspace bottle diameter, are highly body height 3/4.
As preferred technical solution, a kind of head space micro-extraction device, it is characterised in that:The measurement and control of temperature Module includes temperature sensor and temperature control circuit and intelligent digital temperature control, and temperature adjusting control work(is assisted by temperature controller Can, 20-150 DEG C of temperature control range, temperature measurement accuracy ± 1 DEG C.
As preferred technical solution, a kind of head space micro-extraction device, it is characterised in that:The insulated heat Layer is gel heat-insulation pad, is covered in heating mantle outer wall.
The beneficial effects of the utility model:
The utility model uses the hassock piece equipped with cutting ferrule interface to replace the design of traditional head space bottle cap shim liner, extracts Needle stability is good, is not easy to swing, and extraction droplet is made to remain on the vertical line of ml headspace bottle center, and droplet can away from liquid level Accurate to adjust, the accuracy of data is good.
The utility model uses flexible silicone rubber electric heating cover, can more preferably be attached at heating object, homogeneous heating, heat transfer It is efficient, heating rate is fast, and compact structure, assembling easily, use scope it is wide.
Description of the drawings
It is required in being described below to embodiment in order to illustrate more clearly of the technical scheme in the embodiment of the utility model Attached drawing to be used is described further, wherein:
Fig. 1 is a kind of structure diagram of head space micro-extraction device;
Fig. 2 is a kind of half sectional view of ferrule fitting in head space micro-extraction device;
1 ml headspace bottle in figure, 2 bottle caps, 3 hassock pieces, 4 ferrule fittings, 4-1 ferrule fittings nut, 4-2 ferrule fittings card Set, the fittings body of 4-3 ferrule fittings, 4-4 ferrule fittings internal orifice dimension, 5 microextraction needles, 6 goblet electric heating covers, 7 gels are exhausted Edge heat-barrier material, 8 measurement and control of temperature modules.
Specific embodiment
The utility model is explained further and illustrated with reference to embodiment, but does not form any limit to the utility model System.
Fig. 1 is a kind of schematic diagram of head space micro-extraction device provided by the utility model, including ml headspace bottle, microextraction needle With electric heating cover three parts.The utility model replaces the shim liner of traditional head space bottle cap with the hassock piece equipped with cutting ferrule interface, uses Silicon special rubber-heating set replaces traditional heating water bath mode.
The specific implementation step of the utility model is as follows:
Silicon rubber heating plate is rolled into the goblet heating mantle slightly larger than experiment ml headspace bottle, it is exhausted that goblet outer wall is wrapped with gel Edge thermal insulation layer adjusts the measurement and control of temperature module of electric heating cover, sets suitable extraction temperature;
Sample is added in ml headspace bottle 1, tightens the bottle cap for being equipped with hassock piece, and the inner bolt hole and ferrule fitting of hassock piece External screw thread tighten;
Suitable extractant is drawn with the microextraction needle of appropriate volume, sample introduction needle needle cylindrical unit is worn from ferrule fitting internal orifice dimension Go out, adjustment needle head body screws the nut of ferrule fitting upper end, fix microextraction needle away from liquid level proper height;
Ml headspace bottle is set in the goblet for having reached set temperature, microextraction needle push rod is slowly depressed, works as extraction It takes and mutually starts timing when microextraction needle needle point hangs suitable volumes, after a certain period of time, gently pull-up extraction needle pushes away for extraction Bar makes the extractant for being suspended on needle point be sucked back into completely in microextraction needle, is analyzed detect with gas-chromatography instrument later.
Embodiment 1:
The utility model specifically includes following steps to measure in waste water for benzene homologues:As shown in Figure 1, by silicon rubber Heating plate is rolled into the goblet heating mantle 6 slightly larger than 20 mL ml headspace bottles, and goblet outer wall is wrapped with the gel insulated heat of 8 mm of thickness Layer 7, adjusts the measurement and control of temperature module 8 of electric heating cover, and set temperature is 30 DEG C;5 mL are added in 20 mL ml headspace bottles 1 containing benzene It is the waste water and 1 g solid sodium chlorides of object, tightens bottle cap 2 and shake up, bottle cap is equipped with the gasket 3 of 5 mm thickness, and hassock piece The external screw thread 4-3 of inner bolt hole and ferrule fitting 4 is tightened;The ionic liquid of 10 μ L, sample introduction needle are drawn with 50 μ L microextractions needles 5 Needle cylindrical unit is pierced by from ferrule fitting internal orifice dimension 4-4, is adjusted to needle head body away from 1 cm of liquid level, is screwed the nut 4- of ferrule fitting upper end 1, fix microextraction needle;Ml headspace bottle is set in the goblet for having reached set temperature, slowly depresses microextraction Needle push rod starts timing when extraction phase ionic liquid is in microextraction needle needle point 2 μ L volumes of suspension, after extracting 15 min, delays Slow ground pull-up extraction needle push rod, makes the ionic liquid for being suspended on needle point be sucked back into completely in microextraction needle, later with 20 μ L just Hexane is stripped, its content is measured through gas chromatographicanalyzer device.
The above, only one of specific embodiment of the present utility model, but the scope of protection of the utility model is not Limitation is here, any variations and alternatives expected without creative work, should all cover in the scope of protection of the utility model It is interior.Therefore the scope of protection of the utility model should be determined by the scope of protection defined in the claims.

Claims (9)

1. a kind of head space micro-extraction device, including ml headspace bottle, microextraction needle and electric heating cover, it is characterised in that:The head space Bottle is screw socket ml headspace bottle, and head cover is equipped with hassock piece, and hassock piece center is equipped with the ferrule fitting with aperture;The microextraction needle Cylinder is fixed on ferrule fitting, and needle head body is set in sample injection bottle body;The electric heating cover is goblet, and ml headspace bottle bottle is set to In goblet;The electric heating cover is equipped with insulated thermal insulating layer equipped with measurement and control of temperature module, goblet outer wall.
2. a kind of head space micro-extraction device according to claim 1, it is characterised in that:The screw socket ml headspace bottle volume is 10-50 mL, ml headspace bottle head cover centre are equipped with circular hole, and Circularhole diameter is less than 2 mm of head cover internal diameter, and circular hole position is equipped with hassock piece.
3. a kind of head space micro-extraction device according to claim 1, it is characterised in that:The hassock piece is tetrafluoroethene Material, diameter is consistent with head cover Circularhole diameter, and thickness is 4-6 mm, and hassock piece center is equipped with inner bolt hole.
4. a kind of head space micro-extraction device according to claim 1, it is characterised in that:The ferrule fitting with aperture Hassock piece center is set to, ferrule fitting internal orifice dimension is consistent with microextraction needle cylindrical unit outer diameter.
5. a kind of head space micro-extraction device according to claim 1, it is characterised in that:The ferrule fitting includes card Set, fittings body and nut three parts;The cutting ferrule is the hollow short tube body of polytetrafluoroethylene material, inside sets sealing ring, 1 mm of wall thickness, Height 4-6 mm;The fittings body height is consistent with hassock piece, and equipped with the external screw thread being coupled with hassock piece center inner bolt hole;Institute The fixation and lifting of microextraction needle can be realized by adjusting elasticity compresses seal by stating nut.
6. a kind of head space micro-extraction device according to claim 1, it is characterised in that:The microextraction needle is chromatography Sample introduction needle, volume 10-50 μ L, during installation, microextraction needle, ferrule fitting, ml headspace bottle center line on the same line, and Microextraction needle needle point is away from liquid level 0.5-1 cm.
7. a kind of head space micro-extraction device according to claim 1, it is characterised in that:The electric heating cover is slim soft Property the goblet that is rolled into of silicon rubber heating plate, goblet internal diameter is slightly larger than ml headspace bottle diameter, highly 3/4 for body height.
8. a kind of head space micro-extraction device according to claim 1, it is characterised in that:The measurement and control of temperature module includes Temperature sensor and temperature control circuit and intelligent digital temperature control assist temperature adjusting control function, temperature control model by temperature controller 20-150 DEG C is enclosed, temperature measurement accuracy ± 1 DEG C.
9. a kind of head space micro-extraction device according to claim 1, it is characterised in that:The insulated thermal insulating layer is gel Heat insulating mattress is covered in heating mantle outer wall.
CN201721247045.4U 2017-09-27 2017-09-27 A kind of head space micro-extraction device Expired - Fee Related CN207575847U (en)

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Application Number Priority Date Filing Date Title
CN201721247045.4U CN207575847U (en) 2017-09-27 2017-09-27 A kind of head space micro-extraction device

Publications (1)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111257399A (en) * 2018-11-30 2020-06-09 中国科学院大连化学物理研究所 Direct mass spectrum detection device for high-throughput measurement of volatile organic compounds in blood
CN115856178A (en) * 2023-02-24 2023-03-28 成都科林分析技术有限公司 Headspace solid phase microextraction sample injection device and method

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111257399A (en) * 2018-11-30 2020-06-09 中国科学院大连化学物理研究所 Direct mass spectrum detection device for high-throughput measurement of volatile organic compounds in blood
CN115856178A (en) * 2023-02-24 2023-03-28 成都科林分析技术有限公司 Headspace solid phase microextraction sample injection device and method
CN115856178B (en) * 2023-02-24 2023-05-23 成都科林分析技术有限公司 Headspace solid-phase microextraction sampling device and method

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CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20180706

Termination date: 20190927

CF01 Termination of patent right due to non-payment of annual fee