CN104655773A - Method for determining acetic acid content in biomass preprocessing fluid - Google Patents
Method for determining acetic acid content in biomass preprocessing fluid Download PDFInfo
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Abstract
The invention discloses a method for determining acetic acid content in a biomass preprocessing fluid, and relates to the detection of acetic acid content. The method comprises the following steps: adding a non-volatile acid solution to a biomass preprocessing fluid so as to obtain a to-be-detected solution, wherein hydrogen ion concentration of the to-be-detected solution is 10-4mol/L-5.0mol/L; respectively adding the to-be-detected solution and multiple acetic acid standard solutions differing in concentration to different upper-space bottles and sealing to obtain to-be-detected upper-space bottles, wherein the volume of solutions in the to-be-detected upper-space bottles is no more than 0.55mL/mL of the capacity of each upper-space bottle; transferring the acetic acid to a gas chromatograph by virtue of an all-volatile upper-space gas chromatography technology so as to detect a gas chromatography signal value of the acetic acid; and finally, calculating the acetic acid content in the biomass preprocessing fluid. The method for determining the acetic acid content in the biomass preprocessing fluid, disclosed by the invention, has the advantages of being simple and rapid in sample making, high in determination accuracy, good in repeatability and the like, and is widely applied to the detection of the acetic acid content in the biomass preprocessing fluid.
Description
Technical field
The present invention relates to the detection of acetic acid content, more specifically, relate to the detection method of acetic acid content in pretreatment fluid in a kind of biorefinery and association area.
Background technology
Acetic acid is a kind of simple carboxylic acid, and being made up of methyl carboxyl, is a kind of important chemical reagent.In chemical industry, it is used to manufacture polyethylene terephthalate, the major part of the latter and beverage bottle.Acetic acid is also used to manufacture the cellulose acetate required for cinefilm and the polyvinyl acetate in Wood Adhesive, and a lot of synthon and fabric.In family, dilute solution of acetic acid is often used as scale remover.Food industry aspect, in food additives list E260, acetic acid is a kind of acidity regulator of regulation.Annual worldwide acetic acid demand is at about 6,500,000 tons.Wherein about 1,500,000 tons is cycling and reutilization, and remaining 5,000,000 tons is directly produced by petrochemical material or pass through biofermentation.In recent years, along with the shortage increasingly of worldwide petrochemical raw material, with renewable starting material the abundantest in the world---Wooden Biomass is for raw material, and the technology adopting the medicaments such as diluted acid, hot water, green liquor, ethanol to obtain acetic acid in the process extracting hemicellulose is paid close attention to widely.Obviously, the rapid assay methods of acetic acid content in living beings pretreatment fluid, has important effect for the efficiency and benefit improving related science research and industry.
At present, in liquid phase sample, the detection method of acetic acid content mainly contains acid base titration, potentiometric titration, ultraviolet visible spectrometry, high performance liquid chromatography and gas chromatographic technique and detects.The complicacy (interference such as formic acid, laevulic acid, Multiple Weak Acid) of living beings pretreatment fluid composition makes acid base titration and potentiometric titration usually greatly over-evaluate acetic acid content in living beings pretreatment fluid, and the uv-vis spectra pretreatment fluid higher to colour cannot measure usually.Although acetic acid is separated with other interfering material by chromatographic technique with gas chromatographic technique by high performance liquid chromatography; But living beings pretreatment fluid contains a large amount of solid particulate matters and non-acetic acid class dissolved matter (high boiling substance and inorganic salts etc.), the injection port to gas chromatography, chromatographic column and chromatographic resolution are produced very large harm by these.No doubt, larger solid particulate matter is removed by method that is centrifugal and that filter, but the solid small particles particle being difficult to remove usually can block liquid-phase chromatographic column; In addition, the solution material in liquid phase or be attached in gas phase and liquid phase chromatographic column or affect the chromatographic resolution effect of acetic acid, also can generate carbonizing matter at the injection port of gas chromatography or chromatographic column front end; Greatly reduce the speed of detection and add cost of determination.
Summary of the invention
The object of the invention is to the deficiency overcoming existing acetic acid content assay method, a kind of method measuring acetic acid content in living beings pretreatment fluid is provided.Described method adopts full volatilization Headspace-Gas Chromatography to measure the method for acetic acid content in living beings pretreatment fluid.Described method effectively can overcome the obstacle and interference that in sample, fine solid particles thing, inorganic salts and high boiling substance cause, have simply, feature fast, the mass being applicable to acetic acid in living beings (needlebush, leaf wood, grass and other biomass castoff etc.) pretreatment fluid detects.
For realizing object of the present invention, the technical scheme adopted is:
A kind of method measuring acetic acid content in living beings pretreatment fluid of the present invention, is characterized in that, comprise the steps:
(1) sample acidifying: add non-acetic acid class acid solution or non-Acetates aqueous slkali adjust ph in living beings pretreatment fluid, obtain solution to be measured after mixing, the pH of described solution to be measured is 10
-4mol/L ~ 5.0mol/L;
(2) sample preparation: the acetic acid standard solution of the solution to be measured and some variable concentrations of getting step (1) gained is respectively in different ml headspace bottle, and obtaining ml headspace bottle to be measured after ml headspace bottle being sealed, in described ml headspace bottle to be measured, the volume of solution to be measured and acetic acid standard solution is no more than 0.55mL/mL ml headspace bottle volume;
(3) Sample equilibration and detection: the ml headspace bottle to be measured of step (2) gained is placed in automatic headspace sample injector and carries out Balance Treatment, then adopt the gas chromatograph being furnished with flame ionization detector to measure, record the acetic acid gas chromatography signal value A of different ml headspace bottle to be measured respectively;
The condition of automatic headspace sample injector is: stove case temperature is 40 ~ 200
oc, equilibration time are 2 ~ 60min;
(4) content of acetic acid in solution to be measured is calculated according to the acetic acid gas chromatography signal value A obtained in step (3);
Described in step (1), the pH of solution to be measured is 2.5 × 10
-4mol/L ~ 1.0mol/L.
Step (1) also comprises ultrasonic for solution to be measured process 0 ~ 10min.
Described in step (3), the condition of automatic headspace sample injector is: stove case temperature is 40 ~ 170
oc, equilibration time are 3 ~ 15min.
Described in step (3), the condition of automatic headspace sample injector also comprises: assisted gas pressure is higher than 0.5bar, nebulizer gas pressure is higher than 0.25bar, quantitative loop volume 0.5 ~ 3mL, pressing time, quantitative loop gas filling time and/or gas transport are not less than 5s to the time in gas chromatograph.
The condition of gas chromatograph is in step (3): injection port adopt do not shunt or split ratio at 0.1:1 to 250:1, inlet pressure is 5 ~ 150psi, and post case temperature is 20 ~ 260 DEG C, and retention time is 1 ~ 25min, detector temperature is 150 ~ 300 DEG C, and flow rate of carrier gas is 5 ~ 30mL/min.
In step (3), gas chromatograph adopts polarity chromatographic column.
According to the acetic acid gas chromatography signal value A drawing standard working curve of the acetic acid standard solution of some variable concentrations in step (4), and calculate the concentration of acetic acid in solution to be measured according to standard working curve.
Adopt in step (2) and do not react with acetic acid and do not adsorb the dottle pin of acetic acid and lid seals ml headspace bottle.
Step (1) also comprises to be removed the solid particulate matter in solution to be measured.
For realizing object of the present invention, the concrete technical scheme adopted is:
A kind of described method measuring acetic acid content in living beings pretreatment fluid, comprises the steps:
(1) sample acidifying: add non-acetic acid class acid solution or non-Acetates aqueous slkali adjust ph in living beings pretreatment fluid, obtain solution to be measured after mixing, the pH of described solution to be measured is 10
-4mol/L ~ 5.0mol/L;
(2) sample preparation: the acetic acid standard solution of the solution to be measured and some variable concentrations of getting step (1) gained is respectively in different ml headspace bottle, and obtaining ml headspace bottle to be measured after ml headspace bottle being sealed, in described ml headspace bottle to be measured, the volume of solution to be measured and acetic acid standard solution is no more than 0.55mL/mL ml headspace bottle volume;
(3) Sample equilibration and detection: the ml headspace bottle to be measured of step (2) gained is placed in automatic headspace sample injector and carries out Balance Treatment, then adopt the gas chromatograph being furnished with flame ionization detector to measure, record the acetic acid gas chromatography signal value A of different ml headspace bottle to be measured respectively;
The condition of automatic headspace sample injector is: stove case temperature is 90 ~ 200
oc, equilibration time are 2 ~ 60min;
(4) content of acetic acid in solution to be measured is calculated according to the acetic acid gas chromatography signal value A obtained in step (3);
First the present invention adopts non-acetic acid class acid solution to be 10 by the pH of living beings pretreatment fluid
-4mol/L ~ 5.0mol/L, is all converted into acetic acid by acetate and ensures unlikelyly because acidity is excessive, disturbance reponse to occur; Then in ml headspace bottle, add the solution to be measured of specified quantitative, control liquid-gas ratio (the ml headspace bottle volume addition of every milliliter is no more than the solution to be measured of 0.55mL) ultralow in ml headspace bottle, Balance Treatment is carried out at automatic headspace sample injector, at high temperature the acetic acid in ml headspace bottle liquid phase is all evaporated into gas phase, thus eliminate the matrix effect of sample; Acetic acid employing in gas phase is furnished with flame ionization detector gas chromatograph and measures; Finally, standard working curve is utilized to be calculated by the Acetometer in living beings pretreatment fluid.
Preferably, described non-acetic acid class acid solution is sulfuric acid, phosphoric acid, oxalic acid and formic acid etc., described non-Acetates alkaline solution is NaOH, potassium hydroxide, sodium carbonate and sodium formate etc., adopts non-acetic acid class acid solution or non-Acetates solution can avoid causing interference to the mensuration of acetic acid content in living beings pretreatment fluid.
Preferably, described in step (1), the pH of solution to be measured is 2.5 × 10
-4mol/L ~ 1.0mol/L.Thus, acetate all can be converted into the form of acetic acid, but also can not cause because pH is too high acetic acid in testing process with other organism generation chemical reaction.
Preferably, step (1) also comprises ultrasonic for solution to be measured process 0 (being greater than 0) ~ 10min.Utilize ultrasonic oscillation by the bubble removal in solution to be measured, the problem that the sampling degree of accuracy caused to avoid a large amount of bubble is poor.
Preferably, described in step (3), the condition of automatic headspace sample injector is: stove case temperature is 90 ~ 170
oc, equilibration time are 3 ~ 15min.Based on this condition, the acetic acid in sample will avoided all evaporating into gas phase under the prerequisite producing interference chemical reaction as far as possible.
Preferably, described in step (3), the condition of automatic headspace sample injector also comprises: assisted gas pressure is higher than 0.5bar, nebulizer gas pressure is higher than 0.25bar, quantitative loop volume 0.5 ~ 3mL, pressing time, quantitative loop gas filling time and/or gas transport are not less than 5s to the time in gas chromatograph.
Preferably, the condition of gas chromatograph is in step (3): injection port adopt do not shunt or split ratio at 0.1:1 to 250:1, inlet pressure is 5 ~ 150psi, post case temperature is 20 ~ 260 DEG C, retention time is 1 ~ 25min, detector temperature is 150 ~ 300 DEG C, and flow rate of carrier gas is 5 ~ 30mL/min.
Further preferably, the condition of gas chromatograph is in step (3): injection port adopt do not shunt or split ratio at 10:1 to 150:1, inlet pressure is 10 ~ 50psi, post case temperature is 80 ~ 250 DEG C, retention time is 1 ~ 15min, detector temperature is 250 ~ 300 DEG C, and flow rate of carrier gas is 10 ~ 25mL/min.
Preferably, the carrier gas that gas chromatograph adopts is nitrogen or helium, and combustion gas is hydrogen, combustion-supporting gas is air.
Preferably, in step (3), gas chromatograph adopts polarity chromatographic column.Described polarity chromatographic column is HP-5, HP-INNOWAX, DB-5 and HP-FFAP isopolarity chromatographic column.
Preferably, according to the acetic acid gas chromatography signal value A drawing standard working curve of the acetic acid standard solution of some variable concentrations in step (4), and the concentration of acetic acid in solution to be measured is calculated according to standard working curve.
Preferably, adopt in step (2) and do not react with acetic acid and do not adsorb the dottle pin of acetic acid and lid seals ml headspace bottle.
Preferably, step (1) also comprises the solid particulate matter removal in solution to be measured.The present invention uses the solid particulate matter in the method removal sample of centrifugation separation or filtration, prevents from blocking micro syringe syringe needle or liquid-transfering gun rifle head, and problem solid particulate matter can avoided to continue generation acid hydrolysis and cause detection limit higher.
Preferably, in step (2), the concentration range of the acetic acid standard solution of variable concentrations comprises the acetic acid concentration of solution to be measured, to improve precision and the accuracy of detection.The number of the acetic acid standard solution of variable concentrations described in the present invention is 3 ~ 8, the gradient uniformity of its concentration change.
Relative to prior art, the present invention has following advantage:
(1) method of the present invention adopts the Headspace-Gas Chromatography that entirely volatilizees, and has the advantage that sample preparation is simple, sample requirement is few, detect fast and be suitable for batch detection.
(2) method of the present invention effectively overcomes the impact of inorganic salts in living beings pretreatment fluid, fine solid particles and non-volatile high boiling product confrontation gas chromatography.
(3) method of the present invention effectively eliminates the matrix effect of non-second acid in living beings pretreatment fluid, avoids the problem adopting the workload that causes of standard addition method excessive.
(4) method of the present invention has detection degree of accuracy and accuracy advantages of higher.
Accompanying drawing explanation
The standard working curve of Fig. 1 for using in the embodiment of the present invention one.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly, below technical scheme of the present invention is clearly and completely described.Obviously, described embodiment is the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making other embodiments all obtained under creative work prerequisite, belong to the scope of protection of the invention.
The identical instrument used in each embodiment below and medicine as follows:
Automatic headspace sample injector: DANI 86.50 Plus
Gas chromatograph-flame ionization detector: Agilent 7890B
Embodiment one
(1) be placed in dry ml headspace bottle with the Bamboo ethanol pretreatment fluid that liquid-transfering gun accurately measures 1mL, add 50mL sulfuric acid solution (0.2mol/L), jiggle greatly to mix and obtain solution to be measured, the pH of solution to be measured is 10
-2mol/L, and be placed in the ultrasonic bubble removing solution to be measured for 5 minutes of ultrasonic oscillator.
(2) 0.45mm aqueous phase filter is adopted to be filtered by the solution to be measured in (1), solution to be measured after using micro syringe accurately to measure 5mL filtration joins in dry ml headspace bottle (20mL), and with the aluminium lid being furnished with teflon/butyl rubber pad, ml headspace bottle is sealed, obtain ml headspace bottle to be measured.
(3) ml headspace bottle to be measured in (2) is placed in automatic headspace sample injector and carries out Balance Treatment, the balance acetic acid terminated in rear ml headspace bottle gas phase adopts HS GC-flame ionization detector to measure, and records acetic acid gas chromatography signal value A
0=151.7.Wherein the condition of automatic headspace sample injector is: stove case temperature is set as 70
oc, equilibration time is 55min, sampling interval 3min, and assisted gas pressure is 1.5bar, and nebulizer gas pressure is 0.5bar, quantitative loop volume 0.5mL, and pressing time, quantitative loop gas filling time and the gas time transferred in gas chromatograph is 5s;
The condition of gas chromatograph is: injection port is not shunted, and inlet pressure is 20psi, and injector temperature is 250
oc, post case temperature is 180
oc, retention time is 2.9min, and detector temperature is 300 DEG C, and flow rate of carrier gas is 12mL/min, and carrier gas is nitrogen, and combustion gas is hydrogen, combustion-supporting gas is air, adopts HP-5 chromatographic column.
(4) the acetic acid standard solution of seven variable concentrations is prepared, that is: 1.0g/L, 2.0g/L, 3.0g/L, 4.0g/L, 5.0g/L, 7.5g/L, 10.0g/L, detects the acetic acid gas chromatography signal value of acetic acid standard solution according to the method for step (1) ~ (3).With the acetic acid solution concentration be equipped with in the ml headspace bottle of acetic acid standard solution be independent variable, the gas chromatography signal value of its correspondence for dependent variable, adopt linear fit will obtain following standard working curve.By the acetic acid gas chromatography signal value of solution to be measured in step (3), substitute into and obtain in acetic acid standard working curve, obtain the concentration c of acetic acid in this bamboo hot-water pretreatment liquid
0for 5.36g/L.
In order to the reliability of this result is described, the acetic acid solution (1.0g/L, 2.0g/L, 3.0g/L, 4.0g/L, 5.0g/L) of five concentration is added respectively in solution to be measured, and measure according to above-mentioned steps (1) ~ (4), the result recorded shows that the recovery of this method is between 95.6% ~ 103.9%; Further, the testing result of this testing result and liquid chromatography compared, result shows that the relative standard deviation of method described in this patent is 3.9%.This illustrates that this method has very high accuracy to acetic acid concentration in mensuration wood-based composites pretreatment fluid.
Embodiment two
(1) be placed in dry ml headspace bottle with the Eucalyptus dilute acid pretreatment liquid that liquid-transfering gun accurately measures 1mL, add 100mL oxalic acid solution (0.1mol/L), jiggle greatly to mix and obtain solution to be measured, the pH of solution to be measured is 10
-3mol/L, and be placed in the ultrasonic bubble removing solution to be measured for 1 minute of ultrasonic oscillator.
(2) 0.45mm aqueous phase filter is adopted to be filtered by the solution to be measured in (1), solution to be measured after using micro syringe accurately to measure 11mL filtration joins in dry ml headspace bottle (20mL), and with the aluminium lid being furnished with teflon/butyl rubber pad, ml headspace bottle is sealed, obtain ml headspace bottle to be measured.
(3) ml headspace bottle to be measured in (2) is placed in automatic headspace sample injector and carries out Balance Treatment, the balance acetic acid terminated in rear ml headspace bottle gas phase adopts HS GC-flame ionization detector to measure, and records acetic acid gas chromatography signal value A
0=231.2.Wherein the condition of automatic headspace sample injector is: stove case temperature is set as 120
oc, equilibration time are 10min, sampling interval 3min, and assisted gas pressure is 2bar, and nebulizer gas pressure is 1bar, quantitative loop volume 1mL, and pressing time, quantitative loop gas filling time and the gas time transferred in gas chromatograph is 6s;
The condition of gas chromatograph is: injection port is not shunted, inlet pressure is 10psi, injector temperature is 250
oc, post case temperature is 80
oc, retention time is 9min, and detector temperature is 300 DEG C, and flow rate of carrier gas is 20mL/min, and carrier gas is nitrogen, and combustion gas is hydrogen, combustion-supporting gas is air, adopts HP-FFAP chromatographic column.
(4) prepare the acetic acid standard solution of 4 variable concentrations, that is: 3.0g/L, 5.0g/L, 7.5g/L, 10.0g/L, detect the acetic acid gas chromatography signal value of acetic acid standard solution according to the method for step (1) ~ (3).With the acetic acid solution concentration be equipped with in the ml headspace bottle of acetic acid standard solution be independent variable, the gas chromatography signal value of its correspondence for dependent variable, adopt linear fit will obtain following standard working curve.By the acetic acid gas chromatography signal value of solution to be measured in step (3), substitute in the standard working curve obtaining acetic acid, obtain the concentration c of acetic acid in this Eucalyptus dilute acid pretreatment liquid
0for 8.25g/L.
In order to the reliability of this result is described, the acetic acid solution (1.0g/L, 2.0g/L, 3.0g/L, 4.0g/L, 5.0g/L) of five concentration is added respectively at solution to be measured, and measure according to above-mentioned steps (1) ~ (4), the result recorded shows that the recovery of this method is between 94.3% ~ 105.2%; Further, the testing result of this testing result and liquid chromatography compared, result shows that described in this patent, the relative standard deviation of method is-4.5%.This illustrates that this method has very high accuracy to acetic acid concentration in mensuration living beings dilute acid pretreatment liquid.
Embodiment three
(1) be placed in dry ml headspace bottle with the Southern Pine green liquor pretreatment liquid that liquid-transfering gun accurately measures 1mL, add 300mL phosphoric acid solution (2mol/L), jiggle greatly to mix and obtain solution to be measured, the pH of solution to be measured is 0.1 mol/L, and is placed in the ultrasonic bubble removing solution to be measured for 3 minutes of ultrasonic oscillator.
(2) 0.45mm aqueous phase filter is adopted to be filtered by the solution to be measured in (1), solution to be measured after using micro syringe accurately to measure 8mL filtration joins in dry ml headspace bottle (20mL), and with the aluminium lid being furnished with teflon/butyl rubber pad, ml headspace bottle is sealed, obtain ml headspace bottle to be measured.
(3) ml headspace bottle to be measured in (2) is placed in automatic headspace sample injector and carries out Balance Treatment, the balance acetic acid terminated in rear ml headspace bottle gas phase adopts HS GC-flame ionization detector to measure, and records acetic acid gas chromatography signal value A
0=73.8.Wherein the condition of automatic headspace sample injector is: stove case temperature is set as 190
oc, equilibration time are 3min, sampling interval 3min, and assisted gas pressure is 1.5bar, and nebulizer gas pressure is 1.5bar, quantitative loop volume 3mL, and pressing time, quantitative loop gas filling time and/or gas transport to the time in gas chromatograph is 7s;
The condition of gas chromatograph is: injection port is not shunted, and inlet pressure is 30psi, and injector temperature is 150
oc, post case temperature is 220
oc, retention time is 25min, and detector temperature is 300 DEG C, and flow rate of carrier gas is 30mL/min, and carrier gas is nitrogen, and combustion gas is hydrogen, combustion-supporting gas is air, adopts HP-5 chromatographic column.
(4) the acetic acid standard solution of seven variable concentrations is prepared, that is: 1.0g/L, 2.0g/L, 3.0g/L, 4.0g/L, 5.0g/L, 7.5g/L, 10.0g/L, detects the acetic acid gas chromatography signal value of acetic acid standard solution according to the method for step (1) ~ (3).With the acetic acid solution concentration be equipped with in the ml headspace bottle of acetic acid standard solution be independent variable, the gas chromatography signal value of its correspondence for dependent variable, adopt linear fit will obtain following standard working curve.By the acetic acid gas chromatography signal value of solution to be measured in step (3), substitute in the standard working curve obtaining acetic acid, obtain the concentration c of acetic acid in this Southern Pine green liquor pretreatment liquid
0for 2.53g/L.
In order to the reliability of this result is described, the acetic acid solution (0.5g/L, 1.0g/L, 1.5g/L, 2.0g/L, 2.5g/L) of five concentration is added respectively at solution to be measured, and measure according to above-mentioned steps (1) ~ (4), the result recorded shows that the recovery of this method is between 98.8% ~ 104.7%; Further, the testing result of this testing result and liquid chromatography compared, result shows that the relative standard deviation of method described in this patent is 6.1%.This illustrates that this this method has very high accuracy to acetic acid concentration in mensuration Eucalyptus green liquor pretreatment liquid.
Claims (10)
1. measure a method for acetic acid content in living beings pretreatment fluid, it is characterized in that, comprise the steps:
(1) sample acidifying: add non-acetic acid class acid solution or non-Acetates aqueous slkali adjust ph in living beings pretreatment fluid, obtain solution to be measured after mixing, the pH of described solution to be measured is 10
-4mol/L ~ 5.0mol/L;
(2) sample preparation: the acetic acid standard solution of the solution to be measured and some variable concentrations of getting step (1) gained is respectively in different ml headspace bottle, and obtaining ml headspace bottle to be measured after ml headspace bottle being sealed, in described ml headspace bottle to be measured, the volume of solution to be measured and acetic acid standard solution is no more than 0.55mL/mL ml headspace bottle volume;
(3) Sample equilibration and detection: the ml headspace bottle to be measured of step (2) gained is placed in automatic headspace sample injector and carries out Balance Treatment, then adopt the gas chromatograph being furnished with flame ionization detector to measure, record the acetic acid gas chromatography signal value A of different ml headspace bottle to be measured respectively;
The condition of automatic headspace sample injector is: stove case temperature is 40 ~ 200
oc, equilibration time are 2 ~ 60min;
(4) content of acetic acid in solution to be measured is calculated according to the acetic acid gas chromatography signal value A obtained in step (3).
2. measure the method for acetic acid content in living beings pretreatment fluid according to claim 1, it is characterized in that, described in step (1), the pH of solution to be measured is 2.5 × 10
-4mol/L ~ 1.0mol/L.
3. measure the method for acetic acid content in living beings pretreatment fluid according to claim 1, it is characterized in that, step (1) also comprises ultrasonic for solution to be measured process 0 ~ 10min.
4. measure the method for acetic acid content in living beings pretreatment fluid according to claim 1, it is characterized in that, described in step (3), the condition of automatic headspace sample injector is: stove case temperature is 40 ~ 170
oc, equilibration time are 3 ~ 15min.
5. measure the method for acetic acid content in living beings pretreatment fluid according to claim 1, it is characterized in that, described in step (3), the condition of automatic headspace sample injector also comprises: assisted gas pressure is higher than 0.5bar, nebulizer gas pressure is higher than 0.25bar, quantitative loop volume 0.5 ~ 3mL, pressing time, quantitative loop gas filling time and/or gas transport are not less than 5s to the time in gas chromatograph.
6. measure the method for acetic acid content in living beings pretreatment fluid according to claim 1, it is characterized in that, the condition of gas chromatograph is in step (3): injection port adopt do not shunt or split ratio at 0.1:1 to 250:1, inlet pressure is 5 ~ 150psi, post case temperature is 20 ~ 260 DEG C, retention time is 1 ~ 25min, and detector temperature is 150 ~ 300 DEG C, and flow rate of carrier gas is 5 ~ 30mL/min.
7. according to claim 1 or 2 or 3 or 4 or 5 or 6, measure the method for acetic acid content in living beings pretreatment fluid, it is characterized in that, in step (3), gas chromatograph adopts polarity chromatographic column.
8. according to claim 1 or 2 or 3 or 4 or 5 or 6, measure the method for acetic acid content in living beings pretreatment fluid, it is characterized in that, according to the acetic acid gas chromatography signal value A drawing standard working curve of the acetic acid standard solution of some variable concentrations in step (4), and calculate the concentration of acetic acid in solution to be measured according to standard working curve.
9. according to claim 1 or 2 or 3 or 4 or 5 or 6, measure the method for acetic acid content in living beings pretreatment fluid, it is characterized in that, adopt in step (2) and do not react with acetic acid and do not adsorb the dottle pin of acetic acid and lid seals ml headspace bottle.
10. according to claim 1 or 2 or 3 or 4 or 5 or 6, measure the method for acetic acid content in living beings pretreatment fluid, it is characterized in that, step (1) also comprises to be removed the solid particulate matter in solution to be measured.
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Cited By (2)
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| CN107132309A (en) * | 2017-03-31 | 2017-09-05 | 美巢集团股份公司 | The detection method of acetic acid content in a kind of polyvinyl acetate emulsion and its copolymer |
| CN114624372A (en) * | 2022-03-10 | 2022-06-14 | 大连大特气体有限公司 | Method for detecting acetic acid in air and gas chromatograph |
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