CN109991352A - The method for measuring adipic acid in soil - Google Patents
The method for measuring adipic acid in soil Download PDFInfo
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- CN109991352A CN109991352A CN201910279716.2A CN201910279716A CN109991352A CN 109991352 A CN109991352 A CN 109991352A CN 201910279716 A CN201910279716 A CN 201910279716A CN 109991352 A CN109991352 A CN 109991352A
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- adipic acid
- testing sample
- sample solution
- soil
- measurement soil
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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
- G01N30/06—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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
-
- 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
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/047—Standards external
-
- 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
- G01N30/14—Preparation by elimination of some components
- G01N2030/146—Preparation by elimination of some components using membranes
-
- 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
- G01N2030/884—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 organic compounds
Abstract
The present invention relates to the methods of adipic acid in measurement soil comprising step: takes pedotheque to be added in ultrapure water, extracts testing sample solution；Prepare a series of adipic acid standard solution of various concentrations；Testing sample solution and adipic acid standard solution are tested and analyzed respectively using gas chromatograph；The concentration of adipic acid in testing sample solution is calculated according to the result of detection and analysis.In measurement soil provided by the invention in the method for adipic acid, sample treatment is simple and convenient to operate, and detection process is quick, and this method have the advantages that error it is small, detection limit it is low, it can be achieved that in practical pedotheque adipic acid direct quick detection.
Description
Technical field
The present invention relates to the methods of adipic acid in measurement soil.
Background technique
Adipic acid (Adipic Acid) is a kind of dicarboxylic acids being industrially of great significance, can be together with hexamethylene diamine
Synthesize important industrial products nylon, it may also be used for production senior lubricant, food additives, medicine intermediate, flavors and fragrances
Controlling agent, novel monocrystal material, plastics blowing agent, coating, adhesive, insecticide, dyestuff etc., the application in modern industry
It is very extensive.But adipic acid is for eyes, skin, mucous membrane and the irritating effect of the upper respiratory tract, it is also harmful to environment, if
It is discharged into workplace, will cause certain pollution, such as soil pollution.
At present there are many ways to measurement adipic acid content, such as volumetric method, high performance liquid chromatography, capillary electrophoresis
Deng, these methods respectively have its advantage, but also have deficiency, while the country also temporarily without suitable standard.And since adipic acid has
Polarity is big, boiling point is high, is not easy the problems such as gasifying, and gas-chromatography or gas chromatography-mass spectrography need to be generally carried out again after derivative
Detection, reported derivatization method includes esterification, methylation, silanization etc., but its pre-treating method is very complicated, not only consumes
When, and derivatization reagent toxicity is big, there is presently no a kind of not only fast and stable, but also it is sensitive, with specificity, and economy, energy
Direct method for measuring.
Summary of the invention
An object of the present invention is for overcome the deficiencies in the prior art, to provide a kind of side for measuring adipic acid in soil
Method.
In order to achieve the above object, the invention is realized by the following technical scheme:
The method for measuring adipic acid in soil, which is characterized in that comprising steps of
A, it takes pedotheque to be added in ultrapure water, extracts testing sample solution；
B, a series of adipic acid standard solution of various concentrations is prepared；
C, using gas chromatograph respectively to the adipic acid standard solution in the testing sample solution and step B in step A
It is tested and analyzed；
D, the concentration of adipic acid in testing sample solution is calculated according to the detection and analysis result in step C.
According to one embodiment of present invention, in the step A, soil weight and ultrapure water volume ratio are 1:(2-10),
Wherein unit of weight is g, volume unit mL.
According to one embodiment of present invention, in the step A, soil weight and ultrapure water volume ratio are 1:2.5, wherein
Unit of weight is g, volume unit mL.
According to one embodiment of present invention, in the step A, ultrasound 20min or more after soil is added in ultrapure water,
30min is stood again.
According to one embodiment of present invention, the supernatant after standing is taken to pass through 0.22 μm of water phase filtering with microporous membrane,
Collection obtains testing sample solution.
According to one embodiment of present invention, in the step B, using ultrapure water as solvent, a series of various concentrations are prepared
Adipic acid standard solution, concentration range be 0~200 μ g/ml.
According to one embodiment of present invention, in the step C, the chromatographic column used is DB-FFAP, having a size of 30m ×
0.32mm × 0.5 μm, using flame ionization ditector.
According to one embodiment of present invention, take adipic acid standard solution and the testing sample solution of various concentration straight respectively
Sample is tapped into, sampling volume is 0.5 μ l, and injector temperature is 310 DEG C, and input mode is Splitless injecting samples, and carrier gas is nitrogen, column stream
Mode is constant current mode, flow 2.0ml/min.
According to one embodiment of present invention, the gas chromatograph is detected according to following condition:
Using temperature programming, 180 DEG C of initial temperature, 1min is kept, 240 DEG C is warming up to the rate of 35 DEG C/min, keeps
20min；The heter temperature of flame ionization ditector is 300 DEG C, nitrogen flow 40ml/min, and air mass flow is
300ml/min, hydrogen flowing quantity 40ml/min, tail flow 25ml/min, detector frequency are 5Hz.
According to one embodiment of present invention, in the step D, adipic acid standard solution is detected with gas chromatograph
Chromatographic peak peak area and corresponding concentration draw standard curve, then by the standard curve and testing sample solution oneself two
The calculated by peak area of acid goes out concentration of adipic acid.
Compared with the prior art, the invention has the advantages that:
1, the present invention provides the method for adipic acid content in measurement pedotheque, sample treatment is simple, operation side
Just, detection process is quick, and this method have the advantages that error it is small, detection limit it is low, it can be achieved that in practical pedotheque oneself two
The direct quick detection of acid；
2, optimize temperature programming condition in method provided by the invention, make target components generate stronger stick effect and with
Matrix is kept completely separate out；
3, the present invention develop the pre-treating method of soil, and carried out sample mark-on comparison, it was demonstrated that this method it is feasible
Property.
Detailed description of the invention
Fig. 1 is the standard solution chromatogram of adipic acid in embodiment 1 (by taking 200 μ g/ml as an example).
Fig. 2 is the standard curve of adipic acid in embodiment 1.
Specific embodiment
The present invention is described in detail below with reference to embodiment:
Embodiment 1
In order to achieve the above object, the method for being achieved through the following technical solutions adipic acid in measurement soil, which is characterized in that
Comprising steps of
It A, is 1:2.5 according to soil weight and water volume ratio, wherein unit of weight is g, and volume unit mL is weighed
10.0g pedotheque is placed in 100mL vial and adds 25ml ultrapure water, and vial is placed in supersonic wave cleaning machine and is surpassed
Sound 20min stands 30min；Pedotheque after standing is obtained testing sample solution, taken with 0.22 μm of water phase membrane filtration
1ml is in sample injection bottle to sample introduction.
B, using ultrapure water as solvent, the standard solution of various concentration adipic acid is prepared, wherein the concentration of adipic acid is followed successively by
20μg/ml、50μg/ml、100μg/ml、200μg/ml。
C, using gas chromatograph-flame ionization ditector respectively to above-mentioned testing sample solution and various concentration oneself
The standard solution of diacid is tested and analyzed, testing conditions are as follows:
Chromatographic column is DB-FFAP, and specification is 30m × 0.32mm × 0.5 μm, takes above-mentioned testing sample solution and difference respectively
The standard solution direct injected of concentration adipic acid, sampling volume be 0.5 μ l, injector temperature be 310 DEG C, input mode be regardless of
Sample is flowed into, carrier gas is nitrogen, using constant current mode, flow 2.0ml/min；
Temperature program:, keeping 1min by 180 DEG C of initial temperature, is warming up to 240 DEG C with the rate of 35 DEG C/min, keeps
20min；
The heter temperature of hydrogen flame ionization detector is 300 DEG C, nitrogen flow 40ml/min, and air mass flow is
300ml/min, hydrogen flowing quantity 40ml/min, tail flow 25ml/min, detector frequency are 5Hz.
D, the adipic acid standard solution of testing sample solution and various concentration is detected respectively using gas chromatograph
Analysis obtain chromatographic peak area, using the chromatographic peak area of adipic acid standard solution as ordinate Y-axis, adipic acid standard solution it is dense
Degree is that abscissa X-axis draws standard curve, as shown in Fig. 2, obtaining slope and intercept and corresponding equation of linear regression: Y=
1.2584X-32.5290 R2=0.9927, it can thus be seen that having between the chromatographic peak area of adipic acid standard solution and its concentration
There is good linear relationship.The calculated by peak area of the testing sample solution obtained according to above-mentioned equation of linear regression and detection obtains
The concentration of adipic acid into testing sample solution.
For the accuracy for judging this method, the adipic acid of known quantity is added in the pedotheque of blank, with embodiment 1 into
The operation of row sample treatment and detection and analysis operation, measure the peak area of adipic acid, substitute into above-mentioned standard curve, acquire above-mentioned soil
The content of adipic acid in sample according to known magnitude and acquires content value comparison discovery, and the detection error of the method for the present invention is 5%
Within.
Embodiment 2
In order to achieve the above object, the method for being achieved through the following technical solutions adipic acid in measurement soil, which is characterized in that
The following steps are included:
It A, is 1:2 according to soil weight and water volume ratio, wherein unit of weight is g, and volume unit mL weighs 10.0g
Pedotheque is placed in 100mL vial and adds 20ml ultrapure water, vial is placed in supersonic wave cleaning machine ultrasonic
30min stands 30min；Pedotheque after standing is obtained testing sample solution, taken with 0.22 μm of water phase membrane filtration
1ml is in sample injection bottle to sample introduction.
The operation of step B- step D obtains in the present embodiment concentration of adipic acid in testing sample solution with embodiment 1.
Embodiment 3
In order to achieve the above object, the method for being achieved through the following technical solutions adipic acid in measurement soil, which is characterized in that
The following steps are included:
It A, is 1:5 according to soil weight and water volume ratio, wherein unit of weight is g, volume unit mL；Weigh 10.0g
Pedotheque is placed in 100mL vial and adds 50ml ultrapure water, vial is placed in supersonic wave cleaning machine ultrasonic
30min stands 30min；Pedotheque after standing is obtained testing sample solution, taken with 0.22 μm of water phase membrane filtration
1ml is in sample injection bottle to sample introduction.
The operation of step B- step D obtains in the present embodiment concentration of adipic acid in testing sample solution with embodiment 1.
Embodiment 4
In order to achieve the above object, the method for being achieved through the following technical solutions adipic acid in measurement soil, which is characterized in that
The following steps are included:
It A, is 1:10 according to soil weight and water volume ratio, wherein unit of weight is g, and volume unit mL weighs 10.0g
Pedotheque is placed in 100mL vial and adds 100ml ultrapure water, vial is placed in supersonic wave cleaning machine ultrasonic
30min stands 30min；Pedotheque after standing is obtained testing sample solution, taken with 0.22 μm of water phase membrane filtration
1ml is in sample injection bottle to sample introduction.
The operation of step B- step D obtains in the present embodiment concentration of adipic acid in testing sample solution with embodiment 1.
Embodiment 5
In order to achieve the above object, the method for being achieved through the following technical solutions adipic acid in measurement soil, which is characterized in that
The following steps are included:
Only reprogramming Elevated Temperature Conditions, other conditions and operating procedure and embodiment 1 are all the same.
Scheme one:, keeping 1min by 200 DEG C of initial temperature, is warming up to 240 DEG C with the rate of 35 DEG C/min, keeps 15min；
Scheme two:, keeping 1min by 180 DEG C of initial temperature, is warming up to 240 DEG C with the rate of 35 DEG C/min, keeps 20min.
It is found by the Experimental comparison of the temperature programming condition of above two gas Chromatographic Determination, adipic acid in scheme two
Chromatographic peak retention time is more advantageous to chromatographic isolation, therefore selection scheme two carries out gas Chromatographic Determination than long in scheme one.
The method of adipic acid in measurement soil in the present invention, sample treatment is easy to operate, and the chromatographic condition of optimization is advantageous
In chromatographic isolation, detection process is quick, resultant error is small, detection limit it is low, it can be achieved that in practical pedotheque adipic acid it is direct
Quickly detection.
Embodiment in the present invention is only used for that the present invention will be described, and is not construed as limiting the scope of claims limitation,
It may occur to persons skilled in the art that other substantially equivalent substitutions, all fall in the scope of protection of the present invention.
Claims (10)
1. the method for measuring adipic acid in soil, which is characterized in that comprising steps of
A, it takes pedotheque to be added in ultrapure water, extracts testing sample solution；
B, a series of adipic acid standard solution of various concentrations is prepared；
C, the adipic acid standard solution in the testing sample solution and step B in step A is carried out respectively using gas chromatograph
It tests and analyzes；
D, the concentration of adipic acid in testing sample solution is calculated according to the detection and analysis result in step C.
2. the method for adipic acid in measurement soil according to claim 1, which is characterized in that in the step A, soil weight
Amount is 1:(2-10 with ultrapure water volume ratio), wherein unit of weight is g, volume unit mL.
3. the method for adipic acid in measurement soil according to claim 2, which is characterized in that in the step A, soil weight
Amount is 1:2.5 with ultrapure water volume ratio, and wherein unit of weight is g, volume unit mL.
4. the method for adipic acid in measurement soil according to claim 1, which is characterized in that in the step A, by soil
Ultrasound 20min or more after being added in ultrapure water, then stand 30min.
5. the method for adipic acid in measurement soil according to claim 4, which is characterized in that take the supernatant after standing logical
0.22 μm of water phase filtering with microporous membrane is crossed, collection obtains testing sample solution.
6. the method for adipic acid in measurement soil according to claim 1, which is characterized in that in the step B, with ultrapure
Water is solvent, prepares a series of adipic acid standard solution of various concentrations, and concentration range is 0~200 μ g/ml.
7. the method for adipic acid in measurement soil according to claim 1, which is characterized in that in the step C, use
Chromatographic column is DB-FFAP, having a size of 30m × 0.32mm × 0.5 μm, using flame ionization ditector.
8. the method for adipic acid in measurement soil according to claim 1, which is characterized in that take oneself of various concentration respectively
Diacid standard solution and testing sample solution direct injected, sampling volume are 0.5 μ l, and injector temperature is 310 DEG C, input mode
For Splitless injecting samples, carrier gas is nitrogen, and column stream mode is constant current mode, flow 2.0ml/min.
9. it is according to claim 1 measurement soil in adipic acid method, which is characterized in that the gas chromatograph according to
Following condition is detected:
Using temperature programming, 180 DEG C of initial temperature, 1min is kept, 240 DEG C is warming up to the rate of 35 DEG C/min, keeps
20min；The heter temperature of flame ionization ditector is 300 DEG C, nitrogen flow 40ml/min, and air mass flow is
300ml/min, hydrogen flowing quantity 40ml/min, tail flow 25ml/min, detector frequency are 5Hz.
10. the method for adipic acid in measurement soil according to claim 1, which is characterized in that in the step D, with gas
Chromatography detects the chromatographic peak peak area of adipic acid standard solution and corresponding concentration draws standard curve, then by described
The calculated by peak area of adipic acid goes out concentration of adipic acid in standard curve and testing sample solution.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113176372A (en) * | 2021-05-20 | 2021-07-27 | 北京化工大学 | Gas chromatography method for detecting content of adipic acid in fermentation liquor |
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Application publication date: 20190709 |