CN105445402A - Headspace bottle for removing water in sample - Google Patents
Headspace bottle for removing water in sample Download PDFInfo
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- CN105445402A CN105445402A CN201610006087.2A CN201610006087A CN105445402A CN 105445402 A CN105445402 A CN 105445402A CN 201610006087 A CN201610006087 A CN 201610006087A CN 105445402 A CN105445402 A CN 105445402A
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- bottle
- sample
- headspace
- head space
- outer blank
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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
-
- 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
-
- 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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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to a headspace bottle for removing water in a sample. The headspace bottle comprises a water removing inner bottle (3), a headspace outer bottle (1) and a headspace bottle cover, wherein the headspace outer bottle (1) is used for placing a to-be-analyzed sample (8); the headspace bottle cover can cover a headspace outer bottle opening (6); a water removing inner bottle outer edge (2) which is positioned at the uppermost position of the water removing inner bottle (3) can be clamped on the headspace outer bottle opening (6) of the headspace outer bottle (1); a screen which is used for placing an adsorption material layer (4) is arranged at the bottom part of the water removing inner bottle (3); a sample balance space (7) is formed above the adsorption material layer (4). The headspace bottle disclosed by the invention has the advantages that the structure is simple, the operation is convenient, a sample can be processed through the headspace bottle, and the sample containing water can be quickly analyzed and tested.
Description
Technical field
The invention belongs to technical field of analytical chemistry, being specifically related to a kind of ml headspace bottle for removing sample moisture.
Background technology
Gas chromatography-mass spectrography (GC-MS) technology is combined by suitable interface (interface) with mass spectrometer (MS) by gas chromatography instrument (GC), and computer technology carries out the technology of combination analysis.GC-MS is two the most ripe spectrum coupling techniques.GC-MS is widely used in the Isolation and ldentification of complex component, and it has the high resolving power of GC and the high sensitivity of MS, is the effective tool of the qualitative, quantitative that analytical chemistry is commonly used.GC-MS combination analysis highly sensitive, is suitable for low molecular compound (molecular weight < 1000) analysis, is particularly suitable for the analysis of volatile ingredient.In every field such as medicine, food and tobaccos, GC-MS is absolutely necessary instrument.
Headspace sampling technology is one conveniently sample-pretreating method in vapor-phase chromatography, its principle is inserted by testing sample in an airtight container, by heat temperature raising, volatile constituent is evaporated from sample matrices, balance is reached in gas-liquid (or gas-solid) two-phase, direct extraction top gas carries out stratographic analysis, thus the composition of volatile constituent and content in check sample.Use headspace sampling technology can exempt the sample pretreatment process of redundant and complicated, avoid organic solvent to analyze cause interference, reduce pollution to chromatographic column and injection port.
Headspace sampling device can be connected with domestic and international various gas chromatograph, gas chromatograph-mass spectrometer, and it the volatile constituent in liquid or solid sample is directly imported the desirable sampling device that gas chromatograph carries out separation and detection.But in current headspace sampling device, owing to often some moisture in sample, along with heating, pressurization, the moisture in sample also enters in gas chromatography.Because water is comparatively large to the damage of gas chromatographic column, and affecting chromatographic peak, this invention exploits a kind of ml headspace bottle for removing sample moisture for this reason.
Summary of the invention
The object of the present invention is to provide a kind of ml headspace bottle for removing sample moisture newly.
First aspect present invention relates to a kind of ml headspace bottle for removing sample moisture, and it comprises the interior bottle 3 that dewaters, for placing the head space outer blank 1 of sample 8 to be analyzed and can covering the head space bottle cap of head space outer blank bottleneck 6; The interior bottle outer 2 that dewaters of wherein said interior bottle 3 the top that dewaters can be fastened on the head space outer blank bottleneck 6 of described head space outer blank 1; There is bottom the described interior bottle 3 that dewaters the screen cloth for placing sorbing material 4, above described sorbing material 4, forming Sample equilibration space 7.
In a preferred embodiment of the present invention, described head space outer blank bottleneck 6 and described dewatering between interior bottle outer 2 are provided with O-ring seal 5.The setting of O-ring seal 5 guarantees that it can meet the sealing of this ml headspace bottle.Such as, sealing circle 5 can be enclosed within the interior bottle epimere that dewaters and also can slide up and down swimmingly, forms positiver sealing to be finally stuck in dewater between interior bottle outer 2 and head space outer blank bottleneck 6 along with the interior bottle outer 2 that dewaters moves downward when the interior bottle 3 that dewaters inserts head space outer blank 1 downwards.
In a preferred embodiment of the present invention, have external thread below described head space outer blank bottleneck 6, described head space bottle cap has the internal thread that can screw with above-mentioned external thread.
In a preferred embodiment of the present invention, described sorbing material 4 is one or several in anhydrous sodium sulfate, molecular sieve or lime chloride.Described sorbing material 4 is replaceable, and can select suitable drying agent according to the heterogeneity of sample to be analyzed.
The using method of ml headspace bottle of the present invention is as follows: put into bottom head space outer blank 1 by sample 8 to be analyzed, sorbing material 4 is placed on the screen cloth bottom the interior bottle 3 that dewaters, O-ring seal 5 on the outer cover of the interior bottle 3 that dewaters, then entirety is put in head space outer blank 1, cover head space bottle cap, whole ml headspace bottle is placed on instrument to be analyzed.After sample 8 to be analyzed is heated, volatile ingredient is wherein by sorbing material 4, sample moisture in by sorbing material 4 process is adsorbed, then enter Sample equilibration space 7, taken away volatile ingredient in the sample to be analyzed 8 in Sample equilibration space 7 after reaching Sample equilibration wherein by sample pin and carry out chromatographic resolution analysis.Guarantee that, not containing moisture in sampling sample, protection chromatographic column also can improve sensitivity for analysis like this.
Second aspect present invention relates to the purposes of ml headspace bottle in the solid sample headspace sampling containing moisture described according to a first aspect of the present invention.Due to solid sample not easily fully dried dose remove moisture, therefore ml headspace bottle of the present invention is specially adapted to have very much the headspace sampling analysis of volatile component in the solid sample of moisture.
Third aspect present invention relates to the purposes of ml headspace bottle in the fluid sample containing moisture or solid sample headspace sampling described according to a first aspect of the present invention, contains the component can reacted with drying agent in described fluid sample or solid sample.Such as, containing volatile constituent, nonvolatile element and moisture in this type of sample, wherein some nonvolatile element may react with drying agent and the Accurate Determining had influence on volatile component content, so class sample cannot by directly contacting with drying agent and remove moisture, and ml headspace bottle of the present invention avoids this type of sample with the direct of drying agent contacts, be therefore specially adapted to the headspace sampling of such sample.
Compared with prior art, the present invention has following beneficial effect:
1, the ml headspace bottle for removing sample moisture of the present invention is applicable to the headspace sampling of the sample containing moisture, and its structure is simple, easy to operate, is processed sample by this ml headspace bottle, can carry out analytical test fast to the sample containing moisture.
2, the use of this ml headspace bottle, not only makes the sensitivity for analysis of sample improve, and not containing moisture in the sample making finally to enter chromatographic column, avoids chromatographic column and reduce serviceable life because the impact by moisture.
3, this ml headspace bottle can effectively for the analysis causing fragrant sample containing moisture such as fruit, flowers, essence and flavoring agent, and method is feasible, easily operates, accurately sensitive, has application value; Be specially adapted to the solid sample containing moisture and wherein contain the fluid sample of component or the headspace sampling of solid sample that can react with drying agent.
Accompanying drawing explanation
Fig. 1 is ml headspace bottle structural representation of the present invention;
Fig. 2 is the analysis chromatogram utilizing ml headspace bottle sample introduction sample of the present invention.
In figure: 1-head space outer blank, 2-dewaters interior bottle outer, and 3-dewaters interior bottle, 4-sorbing material, 5-O-ring seal, 6-head space outer blank bottleneck, 7-Sample equilibration space, 8-sample to be analyzed.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail, but limited the present invention never in any form, and any conversion done based on training centre of the present invention or improvement, all fall into protection scope of the present invention.
Embodiment 1
Ml headspace bottle is as described in Figure 1 adopted to analyze to sample introduction in GC-MS aroma component in essence and flavoring agent.
The ml headspace bottle for removing sample moisture as shown in Figure 1, it comprises the interior bottle 3 that dewaters, for placing the head space outer blank 1 of sample 8 to be analyzed and can covering the head space bottle cap of head space outer blank bottleneck 6; The interior bottle outer 2 that dewaters of wherein said interior bottle 3 the top that dewaters can be fastened on the head space outer blank bottleneck 6 of described head space outer blank 1; There is bottom the described interior bottle 3 that dewaters the screen cloth for placing sorbing material 4, above described sorbing material 4, forming Sample equilibration space 7.
Described head space outer blank bottleneck 6 and described dewatering between interior bottle outer 2 are provided with O-ring seal 5.The setting of O-ring seal 5 guarantees that it can meet the sealing of this ml headspace bottle.
Have external thread below described head space outer blank bottleneck 6, described head space bottle cap has the internal thread that can screw.
Described sorbing material 4 is the composition in anhydrous sodium sulfate, molecular sieve and lime chloride.Described sorbing material 4 is replaceable.
The using method of this ml headspace bottle is as follows: put into bottom head space outer blank 1 by sample 8 to be analyzed, sorbing material 4 is placed on the screen cloth bottom the interior bottle 3 that dewaters, O-ring seal 5 on the outer cover of the interior bottle 3 that dewaters, then entirety is put in head space outer blank 1, cover head space bottle cap, whole ml headspace bottle is placed on instrument to be analyzed.After sample 8 to be analyzed is heated, volatile ingredient is wherein by sorbing material 4, sample moisture in by sorbing material 4 process is adsorbed, then enter Sample equilibration space 7, taken away volatile ingredient in the sample to be analyzed 8 in Sample equilibration space 7 after reaching Sample equilibration wherein by sample pin and carry out chromatographic resolution analysis.Guarantee that, not containing moisture in sampling sample, protection chromatographic column also can improve sensitivity for analysis like this.
Headspace sampling condition: head space outer blank temperature 100 DEG C, keeps 40 minutes; Sampling probe 120 DEG C, transmission line 160 DEG C, furnace temperature 100 DEG C, pressurization 0.2min, sample introduction 0.1min, pull out pin 0.5min, insulation 45min, GC analysis cycle 58min, chromatographic column 30psi, sample introduction 35psi.
GC conditions: injector temperature: 250 DEG C; Temperature programme: initial temperature 50 DEG C, keeps 1min, rises to 220 DEG C with 5 DEG C/min, keeps 20min; Input mode: split sampling, split ratio 20:1; Sampling volume: 1 μ L.
Mass Spectrometry Conditions: ion gun: EI source; Ionization energy: 70eV; Ion source temperature: 180 DEG C; Transmission line temperature: 220 DEG C; Detecting pattern: full ion scan monitoring, mass scan range: 50 ~ 550amu; Solvent delay: 2min.Sample analysis the results are shown in Figure 2.
Claims (6)
1. for removing a ml headspace bottle for sample moisture, it is characterized in that: it comprises the interior bottle (3) that dewaters, for placing the head space outer blank (1) of sample to be analyzed (8) and can covering the head space bottle cap of head space outer blank bottleneck (6); The interior bottle outer (2) that dewaters of wherein said interior bottle (3) the top that dewaters can be fastened on the head space outer blank bottleneck (6) of described head space outer blank (1); Described interior bottle (3) bottom that dewaters has the screen cloth for placing sorbing material layer (4), and described sorbing material layer (4) top forms Sample equilibration space (7).
2. ml headspace bottle according to claim 1, is characterized in that: described head space outer blank bottleneck (6) and described dewatering between interior bottle outer (2) are provided with O-ring seal (5).
3. ml headspace bottle according to claim 1, is characterized in that: described head space outer blank bottleneck (6) below has external thread, and described head space bottle cap has the internal thread that can screw with above-mentioned external thread.
4. ml headspace bottle according to claim 1, is characterized in that: described sorbing material layer (4) is anhydrous sodium sulfate, one or several in molecular sieve or lime chloride.
5. the purposes of ml headspace bottle according to claim 1 in the solid sample headspace sampling containing moisture.
6. the purposes of ml headspace bottle according to claim 1 in the fluid sample containing moisture or solid sample headspace sampling, is characterized in that, contains the component can reacted with drying agent in described 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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| CN105445402A true CN105445402A (en) | 2016-03-30 |
| CN105445402B CN105445402B (en) | 2018-04-17 |
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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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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106093267A (en) * | 2016-08-24 | 2016-11-09 | 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 tabacco water extract |
| CN106474764A (en) * | 2016-11-24 | 2017-03-08 | 福州大学 | A kind of can eliminating water headspace solid-phase microextraction device and method |
| 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 |
| CN109856297A (en) * | 2019-01-18 | 2019-06-07 | 梁永革 | A kind of drug inspection head-space sampling device |
| 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 |
| CN116773303A (en) * | 2023-08-21 | 2023-09-19 | 成都市产品质量监督检验研究院 | Pretreatment device for fiber sample in headspace detection |
Citations (6)
| 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 |
| CN102101557A (en) * | 2009-12-21 | 2011-06-22 | 蔡丰德 | Drying container |
| 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 |
-
2016
- 2016-01-07 CN CN201610006087.2A patent/CN105445402B/en active Active
Patent Citations (6)
| 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 |
| CN102101557A (en) * | 2009-12-21 | 2011-06-22 | 蔡丰德 | Drying container |
| 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 |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106093267A (en) * | 2016-08-24 | 2016-11-09 | 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 tabacco water extract |
| 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 |
| CN106474764A (en) * | 2016-11-24 | 2017-03-08 | 福州大学 | A kind of can eliminating water headspace solid-phase microextraction device and method |
| 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 |
| CN109856297A (en) * | 2019-01-18 | 2019-06-07 | 梁永革 | A kind of drug inspection head-space sampling device |
| CN109856297B (en) * | 2019-01-18 | 2021-01-29 | 梁永革 | Headspace sampling device for medicine inspection |
| CN116773303A (en) * | 2023-08-21 | 2023-09-19 | 成都市产品质量监督检验研究院 | Pretreatment device for fiber sample in headspace detection |
| 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 |
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| Publication number | Publication date |
|---|---|
| CN105445402B (en) | 2018-04-17 |
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