CN114894912A - Method for measuring acetic anhydride and acetic acid in reaction liquid based on gas chromatography - Google Patents
Method for measuring acetic anhydride and acetic acid in reaction liquid based on gas chromatography Download PDFInfo
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- CN114894912A CN114894912A CN202210273858.XA CN202210273858A CN114894912A CN 114894912 A CN114894912 A CN 114894912A CN 202210273858 A CN202210273858 A CN 202210273858A CN 114894912 A CN114894912 A CN 114894912A
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- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 title claims abstract description 267
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 title claims abstract description 231
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000004817 gas chromatography Methods 0.000 title claims abstract description 17
- 239000012295 chemical reaction liquid Substances 0.000 title claims abstract description 14
- 238000004364 calculation method Methods 0.000 claims abstract description 10
- 238000001514 detection method Methods 0.000 claims abstract description 10
- 238000012937 correction Methods 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 238000010926 purge Methods 0.000 claims description 3
- 239000000052 vinegar Substances 0.000 claims description 3
- 235000021419 vinegar Nutrition 0.000 claims description 3
- 238000012545 processing Methods 0.000 abstract description 5
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 4
- 230000009467 reduction Effects 0.000 abstract description 4
- 238000012795 verification Methods 0.000 abstract description 3
- 230000006872 improvement Effects 0.000 abstract description 2
- 238000010813 internal standard method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 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 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000012450 pharmaceutical intermediate Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
-
- 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
- G01N30/06—Preparation
-
- 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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
-
- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N30/68—Flame ionisation detectors
-
- 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
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8641—Baseline
-
- 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
- G01N30/86—Signal analysis
- G01N30/8665—Signal analysis for calibrating the measuring apparatus
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- 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)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to the technical field of chemical reagent content determination, in particular to a method for determining acetic anhydride and acetic acid in reaction liquid based on gas chromatography. The technical scheme is provided mainly aiming at the problems that the chromatograph is directly read without a verification step, the accuracy of data acquisition needs to be confirmed, the processing of a sample to be detected is insufficient, secondary reworking is needed, and the like: the method comprises the following steps: preparing a standard sample; step two: obtaining a standard sample curve; step three: detecting the reaction solution to be detected; step four: obtaining a numerical value required by calculation; step five: and calculating the concentration of acetic anhydride of the reaction solution to be detected. The method has the advantages of simple determination mode, two concentration acquisition modes, improvement of the concentration calculation accuracy of acetic anhydride and acetic acid in the reaction liquid, reduction of deviation, reduction of secondary processing, convenience and rapidness in detection, suitability for the requirement of high-efficiency work, high accuracy of detection data by checking the read data, and main application of the method in determination of the content of acetic anhydride and acetic anhydride in the reaction liquid.
Description
Technical Field
The invention relates to the technical field of chemical reagent content determination, in particular to a method for determining acetic anhydride and acetic acid in reaction liquid based on gas chromatography.
Background
Acetic anhydride and acetic acid are two important organic chemical raw materials, are mainly used for manufacturing cellulose acetate, pesticides, medicines, dyes, spices and the like, and are two common reaction reagents in the processes of chemical production and pharmaceutical intermediate production. When the two components are reacted, excessive acetic anhydride and acetic acid in the reaction liquid need to be removed by a distillation method or water washing in the post-treatment process of the reaction. Therefore, the contents of the two reagents in the reaction solution need to be accurately and rapidly measured; the existing section has no uniform and accurate detection method for the measurement requirements of acetic anhydride and acetic acid, so that the contents of the acetic anhydride and the acetic acid to be measured cannot be quickly obtained; in the patent CN102288699B, a method for measuring acetic anhydride and pyridine in reaction liquid by a gas chromatography internal standard method is provided, wherein a certain weight of pure substances are added into a certain amount of sample mixture to be analyzed by the internal standard method as internal standard substances, and then the sample containing the internal standard substances is subjected to chromatographic analysis. However, the accuracy of data accuracy cannot be determined by directly reading data through a chromatograph, so that the processing of a sample to be detected is insufficient, secondary rework is needed, the cost is high, more time is wasted, and the sample to be detected cannot be accurately and rapidly processed.
Disclosure of Invention
The invention aims to provide a method for measuring acetic anhydride and acetic acid in reaction liquid based on gas chromatography, aiming at the problems that in the background technology, the chromatograph is directly read without a verification step, and the accuracy of data acquisition needs to be confirmed, so that the sample to be measured is insufficiently processed, secondary rework is needed, and the like.
The technical scheme of the invention is as follows: the method for measuring acetic anhydride and acetic acid in reaction liquid based on gas chromatography comprises the following steps:
the method comprises the following steps: selecting acetic anhydride and acetic acid with the purity of more than or equal to 99.6 percent as standard substances, and preparing 30 to 70 percent of acetic anhydride with different concentrations and 70 to 30 percent of acetic acid with different concentrations as standard samples;
step two: analyzing the plurality of standard samples with different concentrations obtained in the first step on the same gas chromatograph by the same mass under the same chromatographic condition, calibrating the peak area of each standard sample, wherein the peak area of acetic anhydride is B1, the peak area of acetic acid is B2, the peak area of acetic anhydride in each standard sample B1 is respectively used as a vertical coordinate, the concentration of acetic anhydride in the corresponding standard sample is used as a horizontal coordinate, the peak area of acetic acid in each standard sample B2 is used as a vertical coordinate, and the concentration of acetic acid in the corresponding standard sample is used as a horizontal coordinate, and respectively drawing curves for obtaining the standard samples for drawing the acetic anhydride and the acetic acid;
step three: analyzing the acetic anhydride peak area C1 and the acetic acid peak area C2 in the reaction solution to be detected in the same detection standard as the detection standard in the step two, drawing curves of C1 and C2 on the standard sample curve in the step two, and comparing and reading the concentrations of acetic anhydride and acetic acid on the standard sample curve in the reaction solution to be detected;
step four: reading an acetic anhydride standard curve, an acetic anhydride linear equation and an acetic anhydride linear correlation coefficient from the standard sample curve in the second step, and calculating an absolute correction factor y1 of each standard sample, reading an acetic acid standard curve, an acetic acid linear equation and an acetic acid linear correlation coefficient from the standard sample curve in the second step, and calculating an absolute correction factor y2 of each standard sample;
step five: checking the read data: according to the acetic anhydride peak area C1 and the acetic acid peak area C2 in the step III, the concentration of the acetic anhydride and the concentration of the acetic acid in the reaction liquid to be measured are respectively calculated by combining absolute correction factors y1 and y 2.
Preferably, the concentration of acetic anhydride in the standard sample in the step one is 30%, and the concentration of acetic acid in the standard sample in the step one is 70%.
Preferably, the concentration of acetic anhydride in the standard sample in the step one is 40%, and the concentration of acetic acid in the standard sample is 60%.
Preferably, the concentration of acetic anhydride in the standard sample in the step one is 50%, and the concentration of acetic acid in the standard sample in the step one is 50%.
Preferably, the concentration of acetic anhydride in the standard sample in the step one is 60%, and the concentration of acetic acid in the standard sample is 40%.
Preferably, in the first step, the concentration of acetic anhydride in the standard sample is 70%, and the concentration of acetic acid in the standard sample is 30%.
Preferably, the concentration of acetic anhydride in the step five is N1, and the calculation formula is N1 (%) ═ y1 × C1;
the concentration calculated by vinegar was N2, and the calculation formula was N2 (%) ═ y2 × C2.
Preferably, the gas chromatograph has gas phase conditions of:
a detector: a hydrogen flame ionization detector;
sample injector temperature: 130 ℃, detector temperature: 200 ℃, column box temperature: keeping the temperature at 70-110 ℃;
carrier gas: helium with the pressure of 98-109.3 KPa;
total flow rate: 50.1-68.2 mL/min, capillary chromatographic column flow: 0.69-1.90 mL/min, purge flow: 2.8.0 mL/min;
sample introduction amount: 1 μ L, split ratio: 48-57: 1.
Compared with the prior art, the invention has the following beneficial technical effects:
1. according to the method, a standard sample is prepared and is conveyed to a gas chromatograph for analysis, so that the peak area and the corresponding concentration curve of the standard sample are obtained, and meanwhile, the linear equation, the linear correlation coefficient and the absolute correction factor of acetic anhydride and acetic acid in the standard sample are obtained through calculation; secondly, analyzing data of the reaction solution to be measured by combining a gas chromatograph, and drawing the peak area of the sample to be measured through the peak area of the standard sample and the corresponding concentration curve, so that the corresponding concentration curve can be read; the read concentration data of the reaction solution to be detected is measured and calculated by simultaneously calculating a linear equation and a linear correlation coefficient of acetic anhydride and acetic acid in the standard sample and an absolute correction factor, and the measurement and calculation are used for detecting the accuracy of the read data, so that the accuracy of post-processing is ensured, and secondary processing is avoided;
2. the method has the advantages of simple determination mode, two concentration acquisition modes, improvement of the concentration calculation accuracy of acetic anhydride and acetic acid in the reaction liquid, reduction of deviation, reduction of secondary processing, convenience and rapidness in detection, suitability for the requirement of high-efficiency work, verification of read data and high accuracy of detected data.
Detailed Description
The technical solution of the present invention is further described with reference to the following specific examples.
Examples
The invention provides a method for measuring acetic anhydride and acetic acid in reaction liquid based on gas chromatography, which comprises the following steps:
the method comprises the following steps: selecting acetic anhydride and acetic acid with the purity of more than or equal to 99.6 percent as standard substances, and preparing five groups of samples with the concentration of the acetic anhydride of 30 percent, the concentration of the acetic acid of 70 percent, the concentration of the acetic anhydride of 40 percent, the concentration of the acetic acid of 60 percent, the concentration of the acetic anhydride of 50 percent, the concentration of the acetic anhydride of 60 percent, the concentration of the acetic acid of 40 percent, the concentration of the acetic anhydride of 70 percent and the concentration of the acetic acid of 30 percent as standard samples;
step two: analyzing five groups of standard samples with different concentrations obtained in the step one on the same gas chromatograph under the same chromatographic conditions and with the same mass, wherein the gas conditions of the gas chromatograph are as follows: a detector: a hydrogen flame ionization detector; sample injector temperature: 130 ℃, detector temperature: 200 ℃, column box temperature: keeping the temperature at 70-110 ℃; carrier gas: helium with the pressure of 98-109.3 KPa; total flow rate: 50.1-68.2 mL/min, capillary chromatographic column flow: 0.69-1.90 mL/min, purge flow: 2.8.0 mL/min; sample introduction amount: 1 μ L, split ratio: 48-57: 1; calibrating the peak area of each standard sample, wherein the peak area of acetic anhydride is B1, the peak area of acetic acid is B2, the peak area B1 of the acetic anhydride in each standard sample is used as the ordinate, the concentration of the acetic anhydride in the corresponding standard sample is used as the abscissa, the peak area B2 of the acetic acid in each standard sample is used as the ordinate, the concentration of the acetic acid in the corresponding standard sample is used as the abscissa, and curves for drawing the standard samples of the acetic anhydride and the acetic acid are respectively drawn;
step three: analyzing the acetic anhydride peak area C1 and the acetic acid peak area C2 in the reaction solution to be detected in the same detection standard as the detection standard in the step two, drawing curves of C1 and C2 on the standard sample curve in the step two, and comparing and reading the concentrations of acetic anhydride and acetic acid on the standard sample curve in the reaction solution to be detected;
step four: reading an acetic anhydride standard curve, an acetic anhydride linear equation and an acetic anhydride linear correlation coefficient from the standard sample curve in the second step, and calculating an absolute correction factor y1 of each standard sample, reading an acetic acid standard curve, an acetic acid linear equation and an acetic acid linear correlation coefficient from the standard sample curve in the second step, and calculating an absolute correction factor y2 of each standard sample;
step five: checking the read data: respectively calculating the concentration of acetic anhydride and the concentration of acetic acid in the reaction solution to be measured according to the acetic anhydride peak area C1 and the acetic acid peak area C2 in the step five and combining absolute correction factors y1 and y2, wherein the concentration of the acetic anhydride in the step five is N1, and the calculation formula is N1 (%) -y 1 ═ C1; the concentration calculated by vinegar is N2, and the calculation formula is N2 (%) ═ y2 × C2; the linear equation of acetic anhydride is calculated by the data of five groups of standard samples: y is 692577X-831067, the linear range is 50-70%, the linear correlation coefficient of the acetic anhydride is 0.9999, and the absolute correction factor y1 of the acetic anhydride is 1.59 multiplied by 10 -6 (ii) a Linear equation of acetic acid: y is 522577X-731067, the linear range is 50-70%, the linear correlation coefficient of the acetic anhydride is 0.9999, and the absolute correction factor y2 of the acetic anhydride is 1.81 multiplied by 10 -6 ；
Dividing the reaction solution to be measured into five groups, wherein the mass of each group is 50g, and repeating the measuring steps to obtain the following data:
from the above table, it can be known that the accuracy of the data obtained in the scheme is lower than the standard deviation, so that the scheme has small deviation of obtaining acetic anhydride and acetic acid in the reaction solution to be measured and has higher accuracy.
The above-described embodiments are merely preferred embodiments of the present invention, and those skilled in the art can make various alternative modifications and combinations of the above-described embodiments based on the technical solution of the present invention and the related teachings of the above-described embodiments.
Claims (8)
1. The method for measuring acetic anhydride and acetic acid in the reaction solution based on gas chromatography is characterized by comprising the following steps of:
the method comprises the following steps: selecting acetic anhydride and acetic acid with the purity of more than or equal to 99.6 percent as standard substances, and preparing 30 to 70 percent of acetic anhydride with different concentrations and 70 to 30 percent of acetic acid with different concentrations as standard samples;
step two: analyzing the plurality of standard samples with different concentrations obtained in the first step on the same gas chromatograph by the same mass under the same chromatographic condition, calibrating the peak area of each standard sample, wherein the peak area of acetic anhydride is B1, the peak area of acetic acid is B2, the peak area of acetic anhydride in each standard sample B1 is respectively used as a vertical coordinate, the concentration of acetic anhydride in the corresponding standard sample is used as a horizontal coordinate, the peak area of acetic acid in each standard sample B2 is used as a vertical coordinate, and the concentration of acetic acid in the corresponding standard sample is used as a horizontal coordinate, and respectively drawing curves for obtaining the standard samples for drawing the acetic anhydride and the acetic acid;
step three: analyzing the acetic anhydride peak area C1 and the acetic acid peak area C2 in the reaction solution to be detected in the same detection standard as the detection standard in the step two, drawing curves of C1 and C2 on the standard sample curve in the step two, and comparing and reading the concentrations of acetic anhydride and acetic acid on the standard sample curve in the reaction solution to be detected;
step four: reading an acetic anhydride standard curve, an acetic anhydride linear equation and an acetic anhydride linear correlation coefficient from the standard sample curve in the second step, and calculating an absolute correction factor y1 of each standard sample, reading an acetic acid standard curve, an acetic acid linear equation and an acetic acid linear correlation coefficient from the standard sample curve in the second step, and calculating an absolute correction factor y2 of each standard sample;
step five: checking the read data: according to the acetic anhydride peak area C1 and the acetic acid peak area C2 in the step III, the concentration of the acetic anhydride and the concentration of the acetic acid in the reaction liquid to be measured are respectively calculated by combining absolute correction factors y1 and y 2.
2. The method for measuring acetic anhydride and acetic acid in a reaction solution based on gas chromatography as claimed in claim 1, wherein the concentration of acetic anhydride in the standard sample in the first step is 30% and the concentration of acetic acid in the standard sample is 70%.
3. The method for measuring acetic anhydride and acetic acid in a reaction solution based on gas chromatography as claimed in claim 1, wherein the concentration of acetic anhydride in the standard sample in the first step is 40% and the concentration of acetic acid in the standard sample is 60%.
4. The method for measuring acetic anhydride and acetic acid in a reaction solution based on gas chromatography as claimed in claim 1, wherein the concentration of acetic anhydride in the standard sample in the first step is 50% and the concentration of acetic acid in the standard sample is 50%.
5. The method for measuring acetic anhydride and acetic acid in a reaction solution based on gas chromatography as claimed in claim 1, wherein the concentration of acetic anhydride in the standard sample in the first step is 60% and the concentration of acetic acid in the standard sample is 40%.
6. The method for measuring acetic anhydride and acetic acid in a reaction solution based on gas chromatography as claimed in claim 1, wherein the concentration of acetic anhydride in the standard sample in the first step is 70% and the concentration of acetic acid in the standard sample is 30%.
7. The method for measuring acetic anhydride and acetic acid in a reaction solution based on gas chromatography as claimed in claim 1, wherein the concentration of acetic anhydride in the fifth step is N1, and the formula is N1 (%) ═ y1 × C1;
the concentration calculated by vinegar was N2, and the calculation formula was N2 (%) ═ y2 × C2.
8. The method for measuring acetic anhydride and acetic acid in a reaction solution based on gas chromatography as claimed in claim 1, wherein the gas chromatography has gas conditions of:
a detector: a hydrogen flame ionization detector;
sample injector temperature: 130 ℃, detector temperature: 200 ℃, column box temperature: keeping the temperature at 70-110 ℃;
carrier gas: helium with the pressure of 98-109.3 KPa;
total flow rate: 50.1-68.2 mL/min, capillary chromatographic column flow: 0.69-1.90 mL/min, purge flow: 2.8.0 mL/min;
sample introduction amount: 1 μ L, split ratio: 48-57: 1.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102288699A (en) * | 2011-07-19 | 2011-12-21 | 济南圣泉集团股份有限公司 | Method for measuring acetic anhydride and pyridine in reaction liquid with gas phase chromatography internal standard method |
| CN109632983A (en) * | 2018-12-12 | 2019-04-16 | 宁波大安化学工业有限公司 | The method of aceticanhydride and acetic acid in gas Chromatographic Determination reaction solution |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102288699A (en) * | 2011-07-19 | 2011-12-21 | 济南圣泉集团股份有限公司 | Method for measuring acetic anhydride and pyridine in reaction liquid with gas phase chromatography internal standard method |
| CN109632983A (en) * | 2018-12-12 | 2019-04-16 | 宁波大安化学工业有限公司 | The method of aceticanhydride and acetic acid in gas Chromatographic Determination reaction solution |
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