CN1081942C - Treatment method of headspace feeding sample for acid/neutral or alkaline/neutral substance - Google Patents
Treatment method of headspace feeding sample for acid/neutral or alkaline/neutral substance Download PDFInfo
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- CN1081942C CN1081942C CN98125049A CN98125049A CN1081942C CN 1081942 C CN1081942 C CN 1081942C CN 98125049 A CN98125049 A CN 98125049A CN 98125049 A CN98125049 A CN 98125049A CN 1081942 C CN1081942 C CN 1081942C
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- Prior art keywords
- chromatographic peak
- neutrality
- solution
- headspace sampling
- substances
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- 239000000126 substance Substances 0.000 title claims abstract description 22
- 239000002253 acid Substances 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 12
- 230000007935 neutral effect Effects 0.000 title abstract description 13
- 230000002378 acidificating effect Effects 0.000 claims abstract description 8
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 30
- 238000005070 sampling Methods 0.000 claims description 25
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 20
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 150000001555 benzenes Chemical class 0.000 claims description 10
- 238000003672 processing method Methods 0.000 claims description 10
- 239000012808 vapor phase Substances 0.000 claims description 9
- XVMSFILGAMDHEY-UHFFFAOYSA-N 6-(4-aminophenyl)sulfonylpyridin-3-amine Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=N1 XVMSFILGAMDHEY-UHFFFAOYSA-N 0.000 claims description 3
- 239000010842 industrial wastewater Substances 0.000 claims description 3
- 239000002351 wastewater Substances 0.000 claims description 3
- 238000005259 measurement Methods 0.000 abstract description 5
- 150000003839 salts Chemical class 0.000 abstract description 2
- 239000003513 alkali Substances 0.000 abstract 3
- 230000001105 regulatory effect Effects 0.000 abstract 2
- 238000002347 injection Methods 0.000 abstract 1
- 239000007924 injection Substances 0.000 abstract 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 239000000523 sample Substances 0.000 description 7
- 239000012535 impurity Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 239000012488 sample solution Substances 0.000 description 3
- 238000004587 chromatography analysis Methods 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- 238000007445 Chromatographic isolation Methods 0.000 description 1
- 238000003988 headspace gas chromatography Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention discloses a treatment method of headspace sample injection for acidic/neutral or alkaline/neutral substances, which belongs to the measurement field of trace substances, and solves the problems that substances with similar structure are not easy to separate and are not accurate in measurement. In the method, firstly, the acidity of aikalinity of samples is regulated so that weak acid substances or weak alkali substances become salts, and thereby, a chromatographic peak of neutral substances is obtained; then the acidity of aikalinity is again regulated to obtain a mixed chromatographic peak of weak acid substances and neutral substances or of weak alkali substances and neutral substances; finally, a chromatographic peak of weak acid substances or weak alkali substances is obtained by a subtracting method, and thereby, the content of the substances is obtained. The method can be used for measuring substances with similar structure.
Description
The present invention relates to a kind of headspace gas chromatography, particularly relate to a kind of neutrality and acidic materials, the neutrality of structural similarity and headspace sampling processing method of alkaline matter of structural similarity.
A kind of ancillary technique of the gas chromatographic analysis that the headspace sampling technology is got up as new development, owing to avoided the pollution of sample matrices to chromatographic system, particularly chromatographic column, both separation that the sample component is obtained, the life-span of chromatographic column be can prolong again, trace or trace volatile matter now have been widely used in various liquid and the solid material analytically.Present gas-liquid headspace sampling technology just adds the forceful electric power that reduces the solution vapor pressure and separates material in sample solution, sample is placed closed container with certain headspace, after gas-liquid two-phase reaches dynamic equilibrium under uniform temperature, the pressure, get vapor phase and carry out chromatography.Such operation, the organic matter that molecular structure, vapour pressure and solubility property are close in all samples all can enter vapor phase, runs into sample component complexity, just may produce interference, and chromatographic isolation is influenced, even can not separate.To the neutrality of structural similarity and the neutrality and the alkaline matter of acidic materials or structural similarity, as contain the akin acidulous material of character and neutral substance or alkalescent material and neutral substance, they may form common chromatographic peak, and chromatogram can not be separated, thereby can not survey the content of each material.A kind of method is arranged in the prior art, is to the sample solution removal of impurity, promptly remove neutral substance, but this method is removed easily to such an extent that too or do not eliminate, and makes measurement result inaccurate.
The object of the present invention is to provide a kind of neutrality and alkaline matter or neutral headspace sampling processing method of being separated that can make structural similarity with acidic materials.
The object of the present invention is achieved like this:
The headspace sampling processing method of the neutrality of the neutrality of structural similarity of the present invention and acidic materials, structural similarity and alkaline matter is
(1) pH value that makes the neutrality of structural similarity and acidic materials with highly basic is more than 11, make the pH value of the neutrality of structural similarity and alkaline matter below 2 with strong acid, thereby make faintly acid or alkalescent material salify in the solution, adopt the headspace sampling technology to make neutrality, alkalescence or neutrality, acid volatile materials enter vapor phase then, obtain corresponding chromatographic peak;
(2) solution that carries out in (1) after headspace sampling is handled is cooled to room temperature;
(3) (2) gained solution is added strong acid or highly basic makes pH value below 2 or more than 11, thereby make faintly acid or the release of alkalescent material in the solution, adopt the headspace sampling technology to make neutrality, acidity or neutrality, alkaline volatile materials enter vapor phase then, obtain corresponding chromatographic peak;
(4) compare (1) and (3) resulting chromatographic peak, deduct (1) resulting chromatographic peak with (3) resulting chromatographic peak, thereby obtain the chromatographic peak of required mensuration material, thereby obtain the concentration of tested each material.
Described strong acid is hydrochloric acid, and highly basic is NaOH solution.
The neutrality of described structural similarity and alkaline substance solution are the industrial wastewater that contains benzene series things such as dimethylbenzene and pyridine, and its processing method is
(1) add hydrochloric acid earlier to PH-≤2 in wastewater sample, the pyridine salify adopts the headspace sampling technology to make tested benzene series thing enter vapor phase then, obtains the chromatographic peak of dimethylbenzene and other benzene series thing;
(2) solution that carried out the headspace sampling processing in (1) is cooled to room temperature;
(3) (2) gained solution is added NaOH and make pH value 〉=11, thereby the pyridine in the solution is discharged, adopt the headspace sampling technology to obtain dimethylbenzene and a common chromatographic peak of pyridine generation and the chromatographic peak of other benzene series thing then;
(4) with (3) resulting chromatographic peak deduction (1) resulting chromatographic peak, can obtain the chromatographic peak of pyridine, thereby obtain the concentration of pyridine.
Below the present invention is further specified: to containing the sample of close neutrality of structure and alkalescent material or neutral and acidulous material, the method that those skilled in the art at first expect the removal of impurity, go to disturb or impurity is sheltered, think the most every possible means removal of impurity, but be difficult for eliminating, do not know when eliminate yet, removed too, may remove the material of required measurement, influenced measurement result.The present invention overcomes above-mentioned technology prejudice, utilize the physicochemical property of measured object, regulate the Acidity of Aikalinity of sample solution, make acidulous material or alkalescent material salify earlier, and salt does not produce volatilization in alkalescence or acid solution, thereby obtain the chromatographic peak of neutral substance, and then adjusting Acidity of Aikalinity, obtain the mixed chromatogram peak, the method for taking then to deduct obtains the chromatographic peak of acidulous material or alkalescent material, thereby draws its content.
The present invention has the following advantages than prior art: method is simple, effective, and it is very accurate to record the result.
Introduce one embodiment of the present of invention below: a kind of neutrality of structural similarity and alkaline substance solution, for containing the industrial wastewater of benzene series things such as benzene,toluene,xylene and pyridine, its headspace sampling processing method is, in wastewater sample, add hydrochloric acid earlier to PH≤2, the pyridine salify, adopt the headspace sampling technology to make tested benzene series thing enter vapor phase then, obtain three chromatographic peaks of benzene,toluene,xylene; The solution that will carry out the headspace sampling processing is cooled to room temperature; Add NaOH to cooled solution and make pH value 〉=11, thereby the pyridine in the solution is discharged, adopt the headspace sampling technology to obtain the chromatographic peak of benzene, toluene and a common chromatographic peak of dimethylbenzene and pyridine generation then; The chromatographic peak of the common chromatographic peak deduction dimethylbenzene that dimethylbenzene and pyridine produce can obtain the chromatographic peak of pyridine, thereby obtain the concentration of pyridine.
Claims (3)
1, the headspace sampling processing method of the neutrality of the neutrality of structural similarity and acidic materials, structural similarity and alkaline matter, it is characterized in that: this method is
(1) pH value that makes the neutrality of structural similarity and acidic materials with highly basic is more than 11, make the pH value of the neutrality of structural similarity and alkaline matter below 2 with strong acid, thereby make faintly acid or alkalescent material salify in the solution, adopt the headspace sampling technology to make neutrality, alkalescence or neutrality, acid volatile materials enter vapor phase then, obtain corresponding chromatographic peak;
(2) solution that carries out in (1) after headspace sampling is handled is cooled to room temperature;
(3) (2) gained solution is added strong acid or highly basic makes pH value below 2 or more than 11, thereby faintly acid or alkalescent material in the solution are discharged, adopt the headspace sampling technology to make neutrality, acidity or neutrality, alkaline volatile materials enter vapor phase then, obtain corresponding chromatographic peak;
(4) compare (1) and (3) resulting chromatographic peak, deduct (1) resulting chromatographic peak with (3) resulting chromatographic peak, thereby obtain the chromatographic peak of required mensuration material, thereby obtain the concentration of tested each material.
2, headspace sampling processing method according to claim 1 is characterized in that described strong acid is hydrochloric acid, and highly basic is NaOH solution.
3, headspace sampling processing method according to claim 1 is characterized in that the neutrality of described structural similarity and alkaline substance solution are the industrial wastewater that contains benzene series things such as dimethylbenzene and pyridine, and its processing method is
(1) add hydrochloric acid earlier to PH≤2 in wastewater sample, the pyridine salify adopts the headspace sampling technology to make tested benzene series thing enter vapor phase then, obtains the chromatographic peak of dimethylbenzene and other benzene series thing;
(2) solution that carried out the headspace sampling processing in (1) is cooled to room temperature;
(3) (2) gained solution is added NaOH and make pH value 〉=11, thereby the pyridine in the solution is discharged, adopt the headspace sampling technology to obtain dimethylbenzene and a common chromatographic peak of pyridine generation and the chromatographic peak of other benzene series thing then;
(4) with (3) resulting chromatographic peak deduction (1) resulting chromatographic peak, can obtain the chromatographic peak of pyridine, thereby obtain the concentration of pyridine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98125049A CN1081942C (en) | 1998-11-30 | 1998-11-30 | Treatment method of headspace feeding sample for acid/neutral or alkaline/neutral substance |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98125049A CN1081942C (en) | 1998-11-30 | 1998-11-30 | Treatment method of headspace feeding sample for acid/neutral or alkaline/neutral substance |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1219442A CN1219442A (en) | 1999-06-16 |
| CN1081942C true CN1081942C (en) | 2002-04-03 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98125049A Expired - Lifetime CN1081942C (en) | 1998-11-30 | 1998-11-30 | Treatment method of headspace feeding sample for acid/neutral or alkaline/neutral substance |
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| Country | Link |
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| CN (1) | CN1081942C (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85101205A (en) * | 1985-04-01 | 1987-01-24 | 株式会社岛津制作所 | Multi-channel detection data processing device for liquid chromatography |
| JP3085448B2 (en) * | 1995-03-17 | 2000-09-11 | 矢崎総業株式会社 | Communications system |
-
1998
- 1998-11-30 CN CN98125049A patent/CN1081942C/en not_active Expired - Lifetime
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85101205A (en) * | 1985-04-01 | 1987-01-24 | 株式会社岛津制作所 | Multi-channel detection data processing device for liquid chromatography |
| JP3085448B2 (en) * | 1995-03-17 | 2000-09-11 | 矢崎総業株式会社 | Communications system |
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| Publication number | Publication date |
|---|---|
| CN1219442A (en) | 1999-06-16 |
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