CN107702949A - Head-space sampling pin and sampling method - Google Patents
Head-space sampling pin and sampling method Download PDFInfo
- Publication number
- CN107702949A CN107702949A CN201710695998.5A CN201710695998A CN107702949A CN 107702949 A CN107702949 A CN 107702949A CN 201710695998 A CN201710695998 A CN 201710695998A CN 107702949 A CN107702949 A CN 107702949A
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- China
- Prior art keywords
- pin
- interior
- stomata
- head
- sampling
- Prior art date
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- Pending
Links
- 238000005070 sampling Methods 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims description 12
- 239000000523 sample Substances 0.000 claims description 31
- 239000007789 gas Substances 0.000 claims description 23
- 238000010926 purge Methods 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 7
- 238000003466 welding Methods 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 4
- 230000010354 integration Effects 0.000 claims description 4
- 238000003780 insertion Methods 0.000 claims description 3
- 230000037431 insertion Effects 0.000 claims description 3
- 238000010079 rubber tapping Methods 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 238000010586 diagram Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 230000003321 amplification Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2226—Sampling from a closed space, e.g. food package, head space
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2226—Sampling from a closed space, e.g. food package, head space
- G01N2001/2229—Headspace sampling, i.e. vapour over liquid
Abstract
A kind of head-space sampling pin, including needle body, the needle body includes the interior pin for carrying pin end and outer pin, outer needle guard are located on interior pin, and outer pin is stretched out at interior pin both ends, and interior pin is consistent with the pin end direction of outer pin；Interior pin and outer pin are respectively equipped with hollow inner-cavity structure, and the pin end of interior pin is nearby provided with the stomata one connected with the inner chamber of interior pin, and through-flow gap is provided between interior pin and the intracavity sidewall of outer pin, and the pin end of outer pin is nearby provided with the stomata two connected with through-flow gap；The bottom wall of inner cavity of stomata one and interior pin is tangent, and the bottom wall of inner cavity of stomata two and outer pin is tangent.The invention provides a kind of head-space sampling pin, can not only realize continuous Dynamic sampling, and effectively prevent residual and the cross pollution of sample without dead volume between aperture and pin end.
Description
Technical field
The invention belongs to head-space sampling apparatus technical field, refers in particular to a kind of head-space sampling pin.
Background technology
Headspace analysis techniques, it is a kind of gas-chromatography pretreatment technology quantitatively accurate, sensitivity and automaticity are high.
The sampling method of head space can be divided into static sampling and Dynamic sampling, as people analyze trace samplings desired raising, dynamic
Sampling mode receives much concern because its enrichment times is high.The sampling probe of head space instrument is usually single current line structure, and it is close to point
Generally have at end one to two can the aperture that passes through of supplied gas, the carrier gas of pressure process and fill the sample gas of sample process in sequential control
Same needle tubing stream is flowed through by aperture respectively under system.The sampling probe of such a structure is although simple in construction and completes static top enough
Sky sampling, but continuous dynamic purging sampling can not be completed.And published head-space sampling pin, aperture and pin near its needle point
Pipe end often has a certain distance, and the pipeline of this section of aperture and needle tubing end is the dead band of gas flowing, and sample gas easily exists
The section forms residual, and causes the cross pollution of different sample rooms, impact analysis result.
The content of the invention
It is an object of the invention to provide a kind of head-space sampling pin, can not only realize continuous Dynamic sampling, and aperture and pin
Without dead volume between end, residual and the cross pollution of sample effectively prevent.
The object of the present invention is achieved like this：A kind of head-space sampling pin, including needle body, the needle body include carrying pin end
Interior pin and outer pin, outer needle guard be located on interior pin, outer pin is stretched out at interior pin both ends, and interior pin is consistent with the pin end direction of outer pin；Interior pin
Hollow inner-cavity structure is respectively equipped with outer pin, the pin end of interior pin is nearby provided with the stomata one connected with the inner chamber of interior pin, interior pin
Through-flow gap is provided between the intracavity sidewall of outer pin, the pin end of outer pin is nearby provided with the stomata two connected with through-flow gap；Gas
The bottom wall of inner cavity of pin is tangent in Kong Yiyu, and the bottom wall of inner cavity of stomata two and outer pin is tangent.
Preferably, the inner chamber of the interior pin forms interior stream with stomata one, and the through-flow gap is formed with stomata two to outflow
Road；Three-way connection is combined with the needle body, interior pin and outer pin are plugged on one of port of three-way connection, three-way connection
Two other port respectively as interior stream and the external tapping of outer stream.
Preferably, the first port of the three-way connection is connected and sealed with the tail end of outer pin by welding；Interior pin is from outer
Backshank end passes and stretches to the second port of three-way connection, and is connected and seals with second port by welding；Three-way connection
3rd port is welded to connect metal tubes, and metal tubes connect with the through-flow gap.
Preferably, the pin end of the interior pin is made into integration with interior pin body or split coordinates；The pin end of the outer pin with
Outer pin body is made into integration or split coordinates.
Preferably, when the pin end split of the interior pin and interior pin coordinates, the pin end head of interior pin is cone point, and afterbody is set
There are a cylindrical end tangs, the lumen openings of pin in cylindrical end tangs insertion, with welded seal at interior pin seamed；In cylindrical end tangs top surface is formed
The bottom wall of inner cavity of pin, the lower edge of stomata one and the top surface of cylindrical end tangs are tangent.
Preferably, when the pin end split of the outer pin and outer pin coordinates, it is provided with what is passed through for interior pin in the middle part of the pin end of outer pin
Through hole, the pin end of outer pin is set in the setting position on interior pin, and is welded and fixed sealing；The pin end head of outer pin is for convenience of piercing
The conical ring structure of ml headspace bottle, the pin end afterbody of outer pin are provided with the annular boss with through hole uniform internal diameter, and annular boss inserts outer pin
Welded seal at lumen openings, with interior pin seamed；Annular boss top surface forms the bottom wall of inner cavity of outer pin, the lower edge of stomata two and
The top surface of annular boss is tangent.
It is a further object of the present invention to provide a kind of sampling method using above-mentioned head-space sampling pin, realization continuously dynamically takes
Sample, and avoid residual and the cross pollution of sample.
A kind of sampling method, sampling probe is penetrated into ml headspace bottle, depth at least makes the stomata two of outer pin enter in ml headspace bottle；Blow
Scavenging enters interior pin, from the outlet of stomata two of interior pin and enters ml headspace bottle, this is interior stream；With being passed through for carrier gas, ml headspace bottle
Interior pressure rise, under differential pressure action, the sample gas that ml headspace bottle internal upper part contains sample enters outer pin by the stomata two of outer pin
With the through-flow gap between interior pin, and by three-way connection, sample gas is exported from the 3rd port of three-way connection, this is outflow
Road；Purge gass can also be introduced into through-flow gap, the exchange of sample gas stream and outer stream out of interior pin pass-out, realization, change stream
Logical direction.
Preferably, when carrying out head-space sampling, purge gass and sample gas are simultaneously respectively from interior stream or outer stream by entering
The continuous dynamic purging sampling of row.
Preferably, the closed end of stomata one and interior pin is tangent, and the closed end of stomata two and outer pin is tangent；Purge gass band
When sample component and passing through stomata one or stomata two, without flow dead at the closed end of interior pin or outer pin.
The present invention is prominent and beneficial compared with prior art to be had the technical effect that：
1st, present invention employs the structure of trocar, dual flow path can be formed in interior pin and interior pin and with the gap of outer pin,
It can be applied to continuous dynamic purging head-space sampling.
2nd, the aperture and pin end that the supplied gas on interior pin of the invention and outer pin passes through are tangent, i.e., aperture and pin end it
Between will not be formed about in end when passing through aperture without dead volume, purge gass or sample gas flow dead (refer to Fig. 4, Fig. 5,
Fig. 6 is contrasted), therefore do not have sample component and be detained or remain in pin end, it can effectively avoid head-space sampling caused by being detained
Peak stretching and residual caused by cross pollution.
Brief description of the drawings
Fig. 1 is the overall structure figure of the present invention；
Fig. 2 is the pin end part drawing of the outer pin of the present invention；
Fig. 3 is the pin end part drawing of pin in the present invention；
Fig. 4 be gas of the present invention from stomata two pass in and out when flow schematic diagram；
Fig. 5 be gas of the present invention from stomata one pass in and out when flow schematic diagram；
Fig. 6 is gas flow schematic diagram when stomata one and stomata two have certain distance with closed end.
Reference：1st, interior pin；2nd, outer pin；3rd, three-way connection；3a, first port；3b, second port；3c, the 3rd end
Mouthful；4th, the pin end of interior pin；4a, cone point；4b, cylindrical end tangs；5th, the pin end of outer pin；5a, conical ring；5b, annular boss；5c、
Through hole；6th, stomata two；7th, stomata one；8th, metal tubes；9th, through-flow gap.
Embodiment
With specific embodiment, the invention will be further described below in conjunction with the accompanying drawings, referring to Fig. 1-6：
A kind of head-space sampling pin, specifically sees Fig. 1, including the pin end 4 of interior pin 1, interior pin, outer pin 2, outer pin pin end 5 and
3 five critical pieces of three-way connection, interior pin 1 and outer pin 2 are respectively hollow and both ends open member structure, and outer pin 2 is interior
Footpath is more than the external diameter of interior pin 1, and length is more slightly shorter than interior pin 1；With reference to Fig. 3, the pin end 4 of interior pin is by cone point 4a as head and post
Shape boss 4b is formed as afterbody, generally solid construction；With reference to Fig. 2, the welding of the pin end 5 of outer pin as outer pin 2 and interior pin 1
Transition piece, its generally loop configuration, is made up of, the pin end 5 of outer pin conical ring 5a as head and annular boss 5b as afterbody
The outer wall of pin 1 in centrally disposed through hole 5c cooperations.Threeway has the first port 3a and second port 3b positioned at upper and lower side, and
The usual welding metal pipeline 8 of the 3rd port 3c positioned at side, the 3rd port 3c, in order to be connected with subsequent parts.
During installation, the pin end 5 of outer pin is welded in the interior specified location of pin 1, then outer pin 2 is placed on the outside of annular boss 5b,
Seam crossing is with welded seal so that the interior both ends of pin 1 are exposed to outer pin 2 respectively, due to interior pin 1 and the size difference of outer pin 2 so that
Certain through-flow gap 9 is formed between interior pin 1 and outer pin 2；Similarly, the pin end 4 of interior pin passes through under pin 1 in cylindrical end tangs 4b insertions
End opening, with the interior seam crossing of pin 1 with welded seal.
After interior pin 1 and outer pin 2 are worked good, the other end of interior pin 1 and outer pin 2 is inserted to the first end of three-way connection 3 respectively
Mouth 3a, interior pin 1 are directly stretched out due to longer from the second port 3b of three-way connection 3, and the head of outer pin 2 is then embedded in due to shorter
Inside three-way connection 3, and by the inner passage of three-way connection 3 by the metal on through-flow gap 9 and the port 3c of three-way connection 3 the 3rd
Pipeline 8 connects；Pass through welded seal respectively between interior pin 1 and second port 3b, outer pin 2 and first port 3a.
Fig. 1 amplification units specifically are seen, stomata 1 are provided with pin end 4 of the interior pin 1 close to interior pin, in outer pin 2 close to outer pin
Pin end 5 at be provided with stomata 26, stomata 1 and the tangent settings of cylindrical end tangs 4b, stomata 26 and the tangent settings of annular boss 5b,
So that gas flow dead is not present in closed end corresponding to stomata 1 and stomata 26；Comparison diagram 6 is understood, is arranged such,
Cross pollution caused by the peak stretching of head-space sampling caused by avoiding delay and residual.
Understood with reference to Fig. 4 and Fig. 5, as technological level meets the requirements, then the pin end 5 of outer pin can be wholely set with outer pin 2, interior
The pin end 4 of pin can be wholely set with interior pin 1.
The specific sampling method of this programme is as follows：Sampling probe is penetrated into ml headspace bottle, depth at least makes the stomata 26 of outer pin 2
Into in ml headspace bottle；Purge gass enter interior pin 1, from the outlet of stomata 26 of interior pin 1 and enter ml headspace bottle, this is interior stream；With
Carrier gas is passed through, and the rise of the head space pressure in the bottle, under differential pressure action, the sample gas that ml headspace bottle internal upper part contains sample passes through outer pin
The through-flow gap 9 that 2 stomata 26 enters between outer pin 2 and interior pin 1, and by three-way connection 3, by sample gas from three-way connection 3
The 3rd port 3c output, this is outer stream；Purge gass can also be introduced into through-flow gap 9, and sample gas is realized from the interior pass-out of pin 1
The exchange of interior stream and outer stream, change circulating direction.When carrying out head-space sampling, purge gass and sample gas are simultaneously respectively from interior stream
Road or outer stream are by carrying out continuous dynamic purging sampling.
Above-described embodiment is only presently preferred embodiments of the present invention, is not limited the scope of the invention according to this, therefore：It is all according to
The equivalence changes that structure, shape, the principle of the present invention is done, all should be covered by within protection scope of the present invention.
Claims (9)
1. a kind of head-space sampling pin, including needle body, it is characterised in that：The needle body includes interior pin (1) and outer pin with pin end
(2), outer pin (2) is set on interior pin (1), and pin end (5) direction of outer pin (2), interior pin (1) and outer pin is stretched out at interior pin (1) both ends
Unanimously；Interior pin (1) and outer pin (2) are respectively equipped with hollow inner-cavity structure, and the pin end (4) of interior pin is nearby provided with and interior pin (1)
The stomata one (7) of inner chamber connection, is provided with through-flow gap (9), the pin end of outer pin between interior pin (1) and the intracavity sidewall of outer pin (2)
(5) nearby it is provided with the stomata two (6) connected with through-flow gap (9)；Stomata one (7) and the bottom wall of inner cavity of interior pin (1) are tangent, stomata
The bottom wall of inner cavity of two (6) and outer pin (2) is tangent.
2. head-space sampling pin according to claim 1, it is characterised in that：The inner chamber of the interior pin (1) and stomata one (7) shape
Into interior stream, the through-flow gap (9) forms outer stream with stomata two (6)；Three-way connection (3) is combined with the needle body, it is interior
Pin (1) and outer pin (2) are plugged on one of port of three-way connection (3), two other port difference of three-way connection (3)
As interior stream and the external tapping of outer stream.
3. head-space sampling pin according to claim 2, it is characterised in that：The first port (3a) of the three-way connection (3)
It is connected and seals with the tail end of outer pin (2) by welds；Interior pin (1) passes from outer pin (2) tail end and stretches to three-way connection (3)
Second port (3b), and be connected and seal with second port (3b) by welding；The 3rd port (3c) welding of three-way connection (3)
Metal tubes (8) are connected, metal tubes (8) connect with the through-flow gap (9).
4. head-space sampling pin according to claim 1, it is characterised in that：The pin end (4) of the interior pin and interior pin (1) body
It is made into integration or split coordinates；The pin end (5) of the outer pin is made into integration with outer pin (2) body or split coordinates.
5. head-space sampling pin according to claim 4, it is characterised in that：The interior pin (1) and pin end (4) split of interior pin
During cooperation, pin end (4) head of interior pin is cone point (4a), and afterbody is provided with cylindrical end tangs (4b), cylindrical end tangs (4b) insertion
The lumen openings of interior pin (1), with interior pin (1) seam crossing welded seal；The interior bottom of chamber of pin (1) in cylindrical end tangs (4b) top surface composition
Wall, the lower edge of stomata one (7) and the top surface of cylindrical end tangs (4b) are tangent.
6. head-space sampling pin according to claim 4, it is characterised in that：The outer pin (2) and pin end (5) split of outer pin
The through hole (5c) passed through for interior pin (1) is provided with during cooperation, in the middle part of the pin end (5) of outer pin, the pin end (5) of outer pin is set in interior pin
(1) setting position on, and it is welded and fixed sealing；Tied for convenience of the conical ring (5a) for being pierced into ml headspace bottle on pin end (5) head of outer pin
Structure, pin end (5) afterbody of outer pin are provided with the annular boss (5b) with through hole (5c) uniform internal diameter, and annular boss (5b) inserts outer pin
(2) lumen openings, with interior pin (1) seam crossing welded seal；Annular boss (5b) top surface forms the bottom wall of inner cavity of outer pin (2),
The lower edge of stomata two (6) and the top surface of annular boss (5b) are tangent.
7. a kind of sampling method, sampling probe is penetrated into ml headspace bottle, depth at least makes the stomata two (6) of outer pin (2) enter ml headspace bottle
It is interior；Purge gass enter interior pin (1), from stomata two (6) outlet of interior pin (1) and enter ml headspace bottle, this is interior stream；With carrier gas
Be passed through, the head space pressure in the bottle rise, under differential pressure action, the sample gas that ml headspace bottle internal upper part contains sample passes through outer pin (2)
The through-flow gap (9) that enters between outer pin (2) and interior pin (1) of stomata two (6), and by three-way connection (3), by sample gas from
The 3rd port (3c) output of three-way connection (3), this is outer stream；Purge gass can also be introduced into through-flow gap (9), sample gas from
Interior pin (1) pass-out, the exchange of stream and outer stream in realization, changes circulating direction.
8. sampling method according to claim 7, when carrying out head-space sampling, purge gass and sample gas are simultaneously respectively from interior stream
Road or outer stream are by carrying out continuous dynamic purging sampling.
9. sampling method according to claim 8, stomata one (7) and the closed end of interior pin (1) are tangent, stomata two (6)
It is tangent with the closed end of outer pin (2)；When purge gass pass through stomata one (7) or stomata two (6) with sample component, in interior pin
(1) without flow dead or at the closed end of outer pin (2).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710695998.5A CN107702949A (en) | 2017-08-15 | 2017-08-15 | Head-space sampling pin and sampling method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710695998.5A CN107702949A (en) | 2017-08-15 | 2017-08-15 | Head-space sampling pin and sampling method |
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| Publication Number | Publication Date |
|---|---|
| CN107702949A true CN107702949A (en) | 2018-02-16 |
Family
ID=61170885
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710695998.5A Pending CN107702949A (en) | 2017-08-15 | 2017-08-15 | Head-space sampling pin and sampling method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110031267A (en) * | 2019-04-01 | 2019-07-19 | 北京鹏宇昌亚环保科技有限公司 | Soil VOCs processing instrument head space mechanism and soil VOCs processing instrument |
| JP7386722B2 (en) | 2019-02-12 | 2023-11-27 | テカン・トレーディング・アクチェンゲゼルシャフト | Hollow needle for sample pipettor |
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