CN105445402B - A kind of ml headspace bottle for being used to remove sample moisture - Google Patents
A kind of ml headspace bottle for being used to remove sample moisture Download PDFInfo
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- CN105445402B CN105445402B CN201610006087.2A CN201610006087A CN105445402B CN 105445402 B CN105445402 B CN 105445402B CN 201610006087 A CN201610006087 A CN 201610006087A CN 105445402 B CN105445402 B CN 105445402B
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- bottle
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- head space
- headspace
- water removal
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- 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
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- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The present invention relates to a kind of ml headspace bottle for being used to remove sample moisture, it includes bottle (3), the head space outer blank (1) for placing sample to be analysed (8) and the head space bottle cap that can cover head space outer blank bottleneck (6) in water removal；Bottle outer (2) can be fastened on the head space outer blank bottleneck (6) of the head space outer blank (1) in the water removal of bottle (3) the top in wherein described water removal；Bottle (3) bottom has the sieve for being used for placing sorbing material layer (4) in the water removal, and Sample equilibration space (7) are formed above the sorbing material layer (4).The ml headspace bottle of the present invention is simple in structure, easy to operate, and sample is handled by the ml headspace bottle, quickly can carry out analysis test to the sample containing moisture.
Description
Technical field
The invention belongs to technical field of analytical chemistry, and in particular to a kind of ml headspace bottle for being used to remove sample moisture.
Background technology
Gas chromatography-mass spectrography (GC-MS) technology is by appropriate by gas-chromatography instrument (GC) with mass spectrograph (MS)
Interface (interface) is combined, and the technology of combination analysis is carried out by computer technology.GC-MS is two most ripe spectrum connection
Use technology.GC-MS is widely used in the separation and identification of complex component, its high-resolution and MS with GC it is highly sensitive
Degree, is the effective tool of the common qualitative, quantitative of analytical chemistry.The high sensitivity of GC-MS combination analysis, is suitable for degraded
Compound (molecular weight ＜ 1000) is analyzed, and is particularly suitable for the analysis of volatile ingredient.In each neck such as medicine, food and tobacco
Domain, GC-MS are essential instruments.
Headspace sampling technology is a kind of conveniently sample-pretreating method in gas chromatography, its principle is will be to be measured
Sample is inserted in a closed container, volatile component is evaporated from sample matrices by heat temperature raising, gas-liquid (or
Gas-solid) reach balance in two-phase, directly extract top gas and carry out chromatography, thus in sample survey volatile component into
Point and content.The sample pretreatment process of redundant and complicated can be exempted using headspace sampling technology, avoid organic solvent to analysis
Caused by interference, reduce pollution to chromatographic column and injection port.
Headspace sampling device can be connected with domestic and international various gas chromatographs, gas chromatograph-mass spectrometer, it is by liquid or solid
Volatile component in body sample is introduced directly into the preferable sampling device that gas chromatograph is separated and detected.But current
Headspace sampling device in, due to often some moisture in sample, with heating, pressurization, the moisture in sample also enters gas
In phase chromatography.Since damage of the water to gas chromatographic column is larger, and chromatographic peak is influenced, the present invention develops a kind of for going for this
Except the ml headspace bottle of sample moisture.
The content of the invention
It is an object of the invention to provide a kind of new ml headspace bottle for being used to remove sample moisture.
First aspect present invention is related to a kind of ml headspace bottle for being used to remove sample moisture, it includes bottle 3 in water removal, for putting
Put the head space outer blank 1 of sample to be analysed 8 and the head space bottle cap of head space outer blank bottleneck 6 can be covered；Bottle 3 is most upper in wherein described water removal
Bottle outer 2 can be fastened on the head space outer blank bottleneck 6 of the head space outer blank 1 in the water removal of side；3 bottom of bottle has in the water removal
For placing the sieve of sorbing material 4, the top of sorbing material 4 forms Sample equilibration space 7.
In a preferred embodiment of the present invention, it is equipped with the head space outer blank bottleneck 6 and the water removal between bottle outer 2
Sealing ring 5.The setting of sealing ring 5 ensures that it disclosure satisfy that the sealing of the ml headspace bottle.For example, the sealing ring 5 can be sleeved in water removal
Bottle epimere simultaneously can swimmingly slide up and down, so as to when bottle 3 is downwardly into head space outer blank 1 in water removal with bottle outer 2 in water removal
Move downward and be finally stuck in water removal between bottle outer 2 and head space outer blank bottleneck 6 and form reliable sealing.
In a preferred embodiment of the present invention, the lower section of head space outer blank bottleneck 6 has external screw thread, the head space bottle cap
With the internal thread that can be screwed with above-mentioned external screw thread.
In a preferred embodiment of the present invention, the sorbing material 4 is in anhydrous sodium sulfate, molecular sieve or calcium chloride
It is one or several kinds of.The sorbing material 4 is replaceable, and can be selected suitably according to the heterogeneity of sample to be analysed
Drier.
The application method of the ml headspace bottle of the present invention is as follows：It is analysed to sample 8 and is put into 1 bottom of head space outer blank, to water removal
Sorbing material 4 is placed on the sieve of interior 3 bottom of bottle, covers sealing ring 5 outside bottle 3 in water removal, it is then overall to be put into outside head space
In bottle 1, head space bottle cap is covered, whole ml headspace bottle is placed on to be analyzed on instrument.After being heated to sample to be analysed 8, wherein
Volatile ingredient by sorbing material 4, sample moisture during by sorbing material 4 is adsorbed, and is put down subsequently into sample
Weighing apparatus space 7, volatilizees in the sample to be analysed 8 in Sample equilibration space 7 is taken after wherein reaching Sample equilibration away by sample pin
Property component carry out chromatographic isolation analysis.So ensure to sample and moisture is not contained in sample, protection chromatographic column can simultaneously improve analysis
Sensitivity.
Second aspect of the present invention is related to the ml headspace bottle described according to a first aspect of the present invention in the solid sample containing moisture
Purposes in headspace sampling.Since solid sample is not easy fully to remove moisture removal by drier, the ml headspace bottle of the present invention is special
The headspace sampling analysis of volatile component suitable for the solid sample for having very much moisture.
Third aspect present invention is related to the ml headspace bottle described according to a first aspect of the present invention in the fluid sample containing moisture
Or the purposes in solid sample headspace sampling, the component that can be reacted with drier is contained in the fluid sample or solid sample.
For example, containing volatile component, nonvolatile element and moisture in such sample, some of which nonvolatile element may be with doing
Drying prescription reacts and influences the Accurate Determining to volatile component content, therefore such sample can not be by directly contacting with drier
And moisture removal is removed, and the ml headspace bottle of the present invention avoids such sample and is contacted with the direct of drier, is therefore particularly suitable for this
The headspace sampling of class sample.
Compared with prior art, the invention has the advantages that：
1st, the ml headspace bottle for being used to remove sample moisture of the invention is suitable for the headspace sampling of the sample containing moisture, it is tied
Structure is simple and convenient to operate, and sample is handled by the ml headspace bottle, quickly can carry out analysis survey to the sample containing moisture
Examination.
2nd, the use of the ml headspace bottle, not only improves the sensitivity for analysis of sample, but also makes the sample for eventually entering into chromatographic column
Moisture is not contained in product, chromatographic column is avoided and reduces service life because being influenced by moisture.
3rd, the ml headspace bottle can be effectively used for the analysis of the fragrant sample of the cause containing moisture such as fruit, flowers, essence and flavoring agent,
Method is feasible, easy to operate, accurate sensitive, has application value；Especially suitable for the solid sample containing moisture and
Wherein containing the fluid sample of component or the headspace sampling of solid sample that can be reacted with drier.
Brief description of the drawings
Fig. 1 is the ml headspace bottle structure diagram of the present invention；
Fig. 2 is the analysis chromatogram using the ml headspace bottle sample introduction sample of the present invention.
In figure：1- head space outer blanks, 2- water removal in bottle outer, 3- water removal in bottle, 4- sorbing materials, 5- sealing rings, 6- head spaces
Outer blank bottleneck, 7- Sample equilibrations space, 8- sample to be analysed.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples, but not in any way to the present invention
It is any limitation as, based on present invention teach that any conversion or improvement made, each fall within protection scope of the present invention.
Embodiment 1
Using ml headspace bottle as described in Figure 1, into GC-MS, sample introduction analyzes aroma component in essence and flavoring agent.
The ml headspace bottle for being used to remove sample moisture as shown in Figure 1, it includes bottle 3 in water removal, for placing sample to be analyzed
The head space outer blank 1 of product 8 and the head space bottle cap that head space outer blank bottleneck 6 can be covered；In wherein described water removal in the water removal of 3 the top of bottle
Bottle outer 2 can be fastened on the head space outer blank bottleneck 6 of the head space outer blank 1；3 bottom of bottle has to be used to place and inhales in the water removal
The sieve of enclosure material 4, the top of sorbing material 4 form Sample equilibration space 7.
Sealing ring 5 is equipped with the head space outer blank bottleneck 6 and the water removal between bottle outer 2.The setting of sealing ring 5 ensures
It disclosure satisfy that the sealing of the ml headspace bottle.
The lower section of head space outer blank bottleneck 6 has external screw thread, and the head space bottle cap has the internal thread that can be screwed.
The sorbing material 4 is the composition in anhydrous sodium sulfate, molecular sieve and calcium chloride.The sorbing material 4 can be more
Change.
The application method of the ml headspace bottle is as follows：It is analysed to sample 8 and is put into 1 bottom of head space outer blank, 3 bottom of bottle into water removal
Sorbing material 4 is placed on the sieve in portion, covers sealing ring 5 outside bottle 3 in water removal, it is then overall to be put into head space outer blank 1, cover
Upper head space bottle cap, whole ml headspace bottle is placed on to be analyzed on instrument.After being heated to sample to be analysed 8, volatility therein
By sorbing material 4, sample moisture during by sorbing material 4 is adsorbed component, subsequently into Sample equilibration space 7,
In the sample to be analysed 8 in Sample equilibration space 7 is taken after wherein reaching Sample equilibration away by sample pin volatile ingredient into
Row chromatographic isolation is analyzed.So ensure to sample and moisture is not contained in sample, protection chromatographic column can simultaneously improve sensitivity for analysis.
Headspace sampling condition：100 DEG C of head space outer blank temperature, is kept for 40 minutes；120 DEG C of sampling probe, 160 DEG C of transmission line, stove
100 DEG C of temperature, pressurize 0.2min, sample introduction 0.1min, pulls out pin 0.5min, keeps the temperature 45min, GC analysis circulation 58min, chromatographic column
30psi, sample introduction 35psi.
GC conditions：Injector temperature：250℃；Temperature programming：50 DEG C of initial temperature, keep 1min, with 5 DEG C/
Min rises to 220 DEG C, keeps 20min；Input mode：Split sampling, split ratio 20：1；Sampling volume：1μL.
Mass Spectrometry Conditions：Ion gun：EI sources；Ionization energy：70eV；Ion source temperature：180℃；Transmission line temperature：220℃；Inspection
Survey pattern：Full ion scan monitoring, mass scan range：50~550amu；Solvent delay：2min.The result is shown in figure for sample analysis
2。
Claims (5)
- A kind of 1. ml headspace bottle for being used to remove sample moisture, it is characterised in that：It includes bottle (3) in water removal, is treated point for placing The head space outer blank (1) of analysis sample (8) and the head space bottle cap that head space outer blank bottleneck (6) can be covered；Bottle (3) is most in wherein described water removal Bottle outer (2) can be fastened on the head space outer blank bottleneck (6) of the head space outer blank (1) in the water removal of top；Bottle in the water removal (3) bottom has the sieve for being used for placing sorbing material layer (4), and Sample equilibration space is formed above the sorbing material layer (4) (7)；Sealing ring (5) is equipped with the head space outer blank bottleneck (6) and the water removal between bottle outer (2).
- 2. ml headspace bottle according to claim 1, it is characterised in that：There is external screw thread below the head space outer blank bottleneck (6), The head space bottle cap has the internal thread that can be screwed with above-mentioned external screw thread.
- 3. ml headspace bottle according to claim 1, it is characterised in that：The sorbing material layer (4) is anhydrous sodium sulfate, molecule One or several kinds in sieve or calcium chloride.
- 4. purposes of the ml headspace bottle according to claim 1 in the solid sample headspace sampling containing moisture.
- 5. use of the ml headspace bottle according to claim 1 in the fluid sample containing moisture or solid sample headspace sampling On the way, it is characterised in that contain the component that can be reacted with drier in the fluid sample or solid sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610006087.2A CN105445402B (en) | 2016-01-07 | 2016-01-07 | A kind of ml headspace bottle for being used to remove sample moisture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610006087.2A CN105445402B (en) | 2016-01-07 | 2016-01-07 | A kind of ml headspace bottle for being used to remove sample moisture |
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| Publication Number | Publication Date |
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| CN105445402A CN105445402A (en) | 2016-03-30 |
| CN105445402B true CN105445402B (en) | 2018-04-17 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610006087.2A Active CN105445402B (en) | 2016-01-07 | 2016-01-07 | A kind of ml headspace bottle for being used to remove sample moisture |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106093267B (en) * | 2016-08-24 | 2017-12-22 | 浙江中烟工业有限责任公司 | A kind of method of infrared auxiliary hydration reaction on-line headspaces chromatography mass spectrometric determination tobacco water extract |
| CN106474764B (en) * | 2016-11-24 | 2018-09-18 | 福州大学 | A kind of device and method of the headspace solid-phase microextraction removed water |
| CN107247104A (en) * | 2017-06-26 | 2017-10-13 | 上海化工研究院有限公司 | A kind of organic half volatile matter sampling apparatus and its application |
| CN109991343A (en) * | 2018-01-02 | 2019-07-09 | 青岛谱尼测试有限公司 | A kind of novel ml headspace bottle |
| CN109856297B (en) * | 2019-01-18 | 2021-01-29 | 梁永革 | Headspace sampling device for medicine inspection |
| CN116773303B (en) * | 2023-08-21 | 2023-10-24 | 成都市产品质量监督检验研究院 | Pretreatment device for fiber sample in headspace detection |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4351802A (en) * | 1978-02-28 | 1982-09-28 | British-American Tobacco Co., Ltd. | Headspace-sampling apparatus |
| EP0567782A1 (en) * | 1992-05-01 | 1993-11-03 | Hewlett-Packard Company | Headspace sampling system |
| US5753791A (en) * | 1995-09-12 | 1998-05-19 | Seagate Technology, Inc. | Multisample dynamic headspace sampler |
| CN203422237U (en) * | 2013-09-03 | 2014-02-05 | 上海化工研究院 | Sampling device for GC-MS (gas chromatography-mass spectrometer) headspace analysis |
| CN205280674U (en) * | 2016-01-07 | 2016-06-01 | 云南中烟工业有限责任公司 | A head space bottle for getting rid of sample moisture |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102101557A (en) * | 2009-12-21 | 2011-06-22 | 蔡丰德 | Drying container |
-
2016
- 2016-01-07 CN CN201610006087.2A patent/CN105445402B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4351802A (en) * | 1978-02-28 | 1982-09-28 | British-American Tobacco Co., Ltd. | Headspace-sampling apparatus |
| EP0567782A1 (en) * | 1992-05-01 | 1993-11-03 | Hewlett-Packard Company | Headspace sampling system |
| US5753791A (en) * | 1995-09-12 | 1998-05-19 | Seagate Technology, Inc. | Multisample dynamic headspace sampler |
| CN203422237U (en) * | 2013-09-03 | 2014-02-05 | 上海化工研究院 | Sampling device for GC-MS (gas chromatography-mass spectrometer) headspace analysis |
| CN205280674U (en) * | 2016-01-07 | 2016-06-01 | 云南中烟工业有限责任公司 | A head space bottle for getting rid of sample moisture |
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| CN105445402A (en) | 2016-03-30 |
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