CN113624878A - Method for analyzing purity and organic impurity content of electronic grade homogeneous anhydride - Google Patents
Method for analyzing purity and organic impurity content of electronic grade homogeneous anhydride Download PDFInfo
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- 239000012535 impurity Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims description 15
- 150000008064 anhydrides Chemical class 0.000 title claims description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 69
- 239000000243 solution Substances 0.000 claims abstract description 51
- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 claims abstract description 19
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000012488 sample solution Substances 0.000 claims abstract description 11
- 239000012086 standard solution Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 238000004811 liquid chromatography Methods 0.000 claims abstract description 9
- 238000001514 detection method Methods 0.000 claims abstract description 8
- 238000012545 processing Methods 0.000 claims abstract description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 68
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 34
- 239000000126 substance Substances 0.000 claims description 26
- 239000000523 sample Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000012452 mother liquor Substances 0.000 claims description 11
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 7
- WSGYTJNNHPZFKR-UHFFFAOYSA-N 3-hydroxypropanenitrile Chemical compound OCCC#N WSGYTJNNHPZFKR-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 2
- 238000003672 processing method Methods 0.000 claims description 2
- 238000012360 testing method Methods 0.000 abstract description 7
- 238000004458 analytical method Methods 0.000 abstract description 5
- 239000012071 phase Substances 0.000 description 10
- 239000007791 liquid phase Substances 0.000 description 6
- 229920001721 polyimide Polymers 0.000 description 5
- 239000004642 Polyimide Substances 0.000 description 4
- 238000010587 phase diagram Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 239000008037 PVC plasticizer Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001045 blue dye Substances 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
Images
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
-
- 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
- G01N2030/042—Standards
Abstract
The invention relates to the technical field of detection, and provides an analysis method for purity and organic impurity content of electronic grade pyromellitic dianhydride, which comprises the following steps: s1, preparing a mobile phase, a sample solution to be detected and a standard solution, wherein the mobile phase is a triethylamine solution, methanol and acetonitrile in a volume ratio of 80:5: 15; s2, sequentially feeding the sample solution to be detected and the standard solution by using a liquid chromatograph for liquid chromatography detection, wherein the feeding amount is 60 mu L; and S3, carrying out data processing to obtain the purity of the pyromellitic dianhydride and the content of the organic impurities. Through the technical scheme, the problem that the analysis and test of trace impurities in the pyromellitic dianhydride cannot be carried out in the prior art is solved.
Description
Technical Field
The invention relates to the technical field of detection, in particular to an analysis method for purity and organic impurity content of electronic grade pyromellitic dianhydride.
Background
Pyromellitic anhydride, also known as 1,2,4, 5-pyromellitic dianhydride, with the molecular formula C10H2O6The molecular weight is 218.1193, the material is mainly used for preparing polyimide resin, high temperature resistant electric insulating paint, PVC plasticizer, synthetic resin cross-linking agent and epoxy resin curing agent, and is also used for preparing phthalocyanine blue dye and the like. Among them, polyimide has excellent mechanical, electrical, physical and chemical properties, and is widely used in many fields such as electromechanical, aerospace, nuclear and electronic industries. In recent years, polyimide manufacturers have made higher requirements on the purity of pyromellitic dianhydride, and not only the main content of the polyimide is required, but also the content of trace impurities (TMA) is provided for the polyimide, but the prior art does not relate to the test of the TMA content.
A high performance liquid chromatography analysis method (CN103969392A) of pyromellitic dianhydride uses the solvent tetrahydrofuran: belongs to B carcinogen and brings harm to the health of people and the environment. A method (CN111707738A) for determining purity of pyromellitic dianhydride by liquid chromatography only tests the purity of pyromellitic dianhydride, and does not relate to a method for determining organic impurities in products. A test method of a method (CN 108061692A) for accurately measuring the content of fine foreign matters in pyromellitic dianhydride needs to consume a large amount of samples and organic solvents.
Disclosure of Invention
The invention provides an analysis method for purity and organic impurity content of electronic grade pyromellitic dianhydride, which solves the problem that trace impurities in pyromellitic dianhydride cannot be analyzed and tested in the prior art.
The technical scheme of the invention is as follows:
the method for analyzing the purity and the content of organic impurities of the electronic grade pyromellitic anhydride comprises the following steps of:
s1, preparing a mobile phase, a sample solution to be detected and a standard solution, wherein the mobile phase is a triethylamine solution, methanol and acetonitrile in a volume ratio of 80:5: 15;
s2, sequentially feeding the sample solution to be detected and the standard solution by using a liquid chromatograph for liquid chromatography detection, wherein the feeding amount is 60 mu L;
and S3, carrying out data processing to obtain the purity of the pyromellitic dianhydride and the content of the organic impurities.
As a further technical scheme, the preparation method of the triethylamine solution comprises the following steps: sucking 1.3-1.4mL of triethylamine and 3.2-3.3mL of phosphoric acid into a 1000mL volumetric flask by a pipette, adding distilled water to the scale, and shaking up to obtain a triethylamine solution.
As a further technical scheme, the preparation method of the phosphoric acid solution comprises the steps of sucking 6.50-6.60mL of phosphoric acid into a volumetric flask of 1000mL by a pipette, and fixing the volume to the scale by using distilled water to obtain the phosphoric acid solution.
As a further technical scheme, the preparation method of the standard solution comprises the following steps:
s1, preparing TMA and EMA standard substances into standard substance mother liquor TMA and EMA, wherein the concentrations are 0.09-0.1mg/mL and 0.09-0.1mg/mL respectively;
s2, sucking 1mL of TMA mother liquor serving as the standard substance and 10.0mL to 100mL of EMA mother liquor serving as the standard substance in the S1 by a pipette, fixing the volume to a scale by using a phosphoric acid solution, shaking up, and passing through a syringe type water film with the diameter of 0.45 mu m to prepare TMA and EMA with the concentrations of 0.0009-0.001mg/mL and 0.009-0.01mg/mL respectively.
As a further technical scheme, the preparation method of the sample solution to be tested comprises the following steps: weighing a sample 0.5g to 100mL in a volumetric flask, adding 79-80mL of phosphoric acid solution, heating to completely dissolve the sample, cooling to room temperature, fixing the volume to the scale with the phosphoric acid solution, shaking up, and filtering with a 0.45-micrometer syringe type water film for later use.
As a further technical solution, the data processing method comprises:
firstly, making a standard curve according to the concentration of a standard substance to peak area, and then calculating according to the standard curve, wherein the calculation formula is as follows:
TMA content (%) - (TMA peak area)(sample)X concentration of(TMA Standard)Area of TMA peak(Standard substance))×100÷500×100％；
EMA content (%) ═ EMA peak area(sample)X concentration of(EMA standard)EMA peak area(Standard substance))×100÷500×100％；
PMDA content (%) -100% to TMA content-EMA content.
As a further technical scheme, the liquid chromatography conditions are as follows:
mobile phase: 0.01mol/L triethylamine solution methanol acetonitrile 80:5:15
A chromatographic column: sinochrom ODS-BP (5 μm, 4.6X 250mm)
Flow rate: 0.8-0.9mL/min
Wavelength: 210nm
Sample introduction amount: 60 μ L
Column temperature: 28-30 ℃.
The invention has the beneficial effects that:
the method makes up the blank of the prior art, realizes the test of the purity of the pyromellitic dianhydride, measures TMA and EMA in the pyromellitic dianhydride as another index for judging the quality of the pyromellitic dianhydride, and creatively realizes the measurement of trace impurities of the pyromellitic dianhydride. The inventor researches through numerous experiments, selects a proper mobile phase and test conditions according to the physicochemical properties of the pyromellitic dianhydride, and fills the blank of the prior art.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a TMA EMA standard liquid phase spectrum,
figure 2 is a graph of a standard TMA,
figure 3 is a graph of an EMA standard curve,
figure 4 is a liquid phase diagram of example 1,
figure 5 is a liquid phase diagram of example 2,
figure 6 is a liquid phase diagram of example 3,
FIG. 7 is a liquid phase diagram of example 4.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any inventive step, are intended to be within the scope of the present invention. The test methods described in the following examples are all conventional methods unless otherwise specified; the reagents, unless otherwise specified, are commercially available.
The invention adopts the following instruments:
high performance liquid chromatograph
P3100 high-pressure constant flow pump
UV3100 UV-Vis Detector
O3100 chromatographic column thermostat
Four groups of the homoanhydride samples were tested, respectively in examples 1-4.
Example 1
Solution preparation:
sucking 6.60mL of phosphoric acid into a 1000mL volumetric flask by a pipette, and fixing the volume to the scale by deionized water to obtain a phosphoric acid solution for later use.
Sucking 1.4mL of triethylamine and 3.26mL of phosphoric acid into a 1000mL volumetric flask by a pipette, adding distilled water to the scale mark, and shaking up to obtain a triethylamine solution for later use.
And preparing a mobile phase according to the volume ratio of triethylamine solution to methanol to acetonitrile of 80:5: 15.
Respectively weighing 10mg TMA and 10mg EMA standard substance (accurate to 0.0001g), respectively adding into a 100mL volumetric flask, adding phosphoric acid solution to constant volume to scale, wherein the concentration of TMA and EMA of the standard substance mother liquor is 0.1 mg/mL.
Sucking 1mL (accurate to 0.01mL) of TMA mother liquor serving as a standard substance and 10.0mL (accurate to 0.01mL) of EMA mother liquor serving as a standard substance into a 100mL volumetric flask by using a pipette, fixing the volume to a scale by using a phosphoric acid solution, shaking up, and passing through a syringe type water film of 0.45 mu m for later use (the TMA and EMA concentrations are 0.001mg/mL and 0.01mg/mL respectively).
Weighing 0.5g (accurate to 0.0001g) of sample into a 100mL volumetric flask, adding 80mL of phosphoric acid solution, heating to completely dissolve the sample, cooling to room temperature, fixing the volume to the scale with the phosphoric acid solution, shaking up, and passing through a 0.45-micrometer syringe type water film for later use.
And sequentially injecting the sample solution to be detected and the standard solution by using a liquid chromatograph to perform liquid chromatography detection, wherein the chromatographic conditions are as follows:
mobile phase: 0.01mol/L triethylamine solution methanol acetonitrile 80:5:15
A chromatographic column: sinochrom ODS-BP (5 μm, 4.6X 250mm)
Flow rate: 0.9mL/min
Wavelength: 210nm
Sample introduction amount: 60 μ L
Column temperature: at 30 ℃.
Example 2
Solution preparation:
sucking 6.50mL of phosphoric acid into a 1000mL volumetric flask by a pipette, and fixing the volume to the scale by deionized water to obtain a phosphoric acid solution for later use.
Sucking 1.3mL of triethylamine and 3.3mL of phosphoric acid into a 1000mL volumetric flask by a liquid transfer machine, adding distilled water to the scale, and shaking up to obtain a triethylamine solution for later use.
And preparing a mobile phase according to the volume ratio of triethylamine solution to methanol to acetonitrile of 80:5: 15.
Respectively weighing 9mg TMA and 9mg EMA standard substance (accurate to 0.0001g), respectively adding into a 100mL volumetric flask, adding phosphoric acid solution to constant volume to scale, wherein the concentration of TMA and EMA of the standard substance mother liquor is 0.09 mg/mL.
Pipette 1mL (to 0.01mL) of TMA master solution and 10.0mL (to 0.01mL) of EMA master solution into 100mL volumetric flasks, add volume to the scale with phosphoric acid solution, shake, and pass through a 0.45 μm syringe water membrane for use (TMA and EMA concentrations 0.0009mg/mL and 0.009mg/mL, respectively).
Weighing 0.5g (accurate to 0.0001g) of sample into a 100mL volumetric flask, adding 79mL of phosphoric acid solution, heating to completely dissolve the sample, cooling to room temperature, fixing the volume to the scale with the phosphoric acid solution, shaking up, and passing through a 0.45-micrometer syringe type water film for later use.
And sequentially injecting the sample solution to be detected and the standard solution by using a liquid chromatograph to perform liquid chromatography detection, wherein the chromatographic conditions are as follows:
mobile phase: 0.01mol/L triethylamine solution methanol acetonitrile 80:5:15
A chromatographic column: sinochrom ODS-BP (5 μm, 4.6X 250mm)
Flow rate: 0.8mL/min
Wavelength: 210nm
Sample introduction amount: 60 μ L
Column temperature: 28 deg.C
Example 3
Solution preparation:
sucking 6.50mL of phosphoric acid into a 1000mL volumetric flask by a pipette, and fixing the volume to the scale by deionized water to obtain a phosphoric acid solution for later use.
Sucking 1.3mL of triethylamine and 3.3mL of phosphoric acid into a 1000mL volumetric flask by a liquid transfer machine, adding distilled water to the scale, and shaking up to obtain a triethylamine solution for later use.
And preparing a mobile phase according to the volume ratio of triethylamine solution to methanol to acetonitrile of 80:5: 15.
Respectively weighing 9mg TMA and 9mg EMA standard substance (accurate to 0.0001g), respectively adding into a 100mL volumetric flask, adding phosphoric acid solution to constant volume to scale, wherein the concentration of TMA and EMA of the standard substance mother liquor is 0.09 mg/mL.
Pipette 1mL (to 0.01mL) of TMA master solution and 10.0mL (to 0.01mL) of EMA master solution into 100mL volumetric flasks, add volume to the scale with phosphoric acid solution, shake, and pass through a 0.45 μm syringe water membrane for use (TMA and EMA concentrations 0.0009mg/mL and 0.009mg/mL, respectively).
Weighing 0.5g (accurate to 0.0001g) of sample into a 100mL volumetric flask, adding 80mL of phosphoric acid solution, heating to completely dissolve the sample, cooling to room temperature, fixing the volume to the scale with the phosphoric acid solution, shaking up, and passing through a 0.45-micrometer syringe type water film for later use.
And sequentially injecting the sample solution to be detected and the standard solution by using a liquid chromatograph to perform liquid chromatography detection, wherein the chromatographic conditions are as follows:
mobile phase: 0.01mol/L triethylamine solution methanol acetonitrile 80:5:15
A chromatographic column: sinochrom ODS-BP (5 μm, 4.6X 250mm)
Flow rate: 0.8mL/min
Wavelength: 210nm
Sample introduction amount: 60 μ L
Column temperature: 30 deg.C
Example 4
The test conditions were the same as in example 1.
Firstly, making a standard curve according to the concentration of a standard substance to the peak area, and then calculating according to the standard curve, wherein the calculation formula is as follows:
TMA content (%) - (TMA peak area)(sample)X concentration of(TMA Standard)Area of TMA peak(Standard substance))×100÷500×100％
EMA content (%) ═ EMA peak area(sample)X concentration of(EMA standard)EMA peak area(Standard substance))×100÷500×100％
PMDA content (%) -100% to TMA content-EMA content
Examples 1-4 were tested according to the procedure described above:
FIG. 1 is a TMA EMA standard sample chart, FIG. 2 is a TMA standard curve chart, FIG. 3 is an EMA standard curve chart, FIGS. 4 to 7 are liquid phase maps of examples 1 to 4, respectively, and Table 1 shows the test results.
Purity and organic impurities of examples 1 to 4
| Grouping | TMA content% | Content of EMA% | Content of PMDA% |
| Example 1 | 0.01 | 0.038 | 99.952 |
| Example 2 | 0.01 | 0.032 | 99.958 |
| Example 3 | 0.01 | 0.088 | 99.902 |
| Example 4 | 0.014 | 0.088 | 99.898 |
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. The method for analyzing the purity and the content of organic impurities of electronic grade pyromellitic dianhydride is characterized by comprising the following steps of:
s1, preparing a mobile phase, a sample solution to be detected and a standard solution, wherein the mobile phase is a triethylamine solution, methanol and acetonitrile in a volume ratio of 80:5: 15;
s2, sequentially feeding the sample solution to be detected and the standard solution by using a liquid chromatograph for liquid chromatography detection, wherein the feeding amount is 60 mu L;
and S3, carrying out data processing to obtain the purity of the pyromellitic dianhydride and the content of the organic impurities.
2. The method for analyzing the purity and the content of the organic impurities of the electronic-grade pyromellitic anhydride according to claim 1, wherein the triethylamine solution is prepared by the following steps: sucking 1.3-1.4mL of triethylamine and 3.2-3.3mL of phosphoric acid into a 1000mL volumetric flask by a pipette, adding distilled water to the scale, and shaking up to obtain a triethylamine solution.
3. The method for analyzing the purity and the content of the organic impurities of the electronic grade anhydride according to claim 2, wherein the phosphoric acid solution is prepared by sucking 6.50-6.60mL of phosphoric acid into a 1000mL volumetric flask by a pipette, and metering to a scale with distilled water.
4. The method for analyzing the purity and the content of the organic impurities of the electronic grade pyromellitic anhydride according to claim 1, wherein the preparation method of the standard solution comprises the following steps:
s1, preparing TMA and EMA standard substances into standard substance mother liquor TMA and EMA, wherein the concentrations are 0.09-0.1mg/mL and 0.09-0.1mg/mL respectively;
s2, sucking 1mL of TMA mother liquor serving as the standard substance and 10.0mL to 100mL of EMA mother liquor serving as the standard substance in the S1 by a pipette, fixing the volume to a scale by using a phosphoric acid solution, shaking up, and passing through a syringe type water film with the diameter of 0.45 mu m to prepare TMA and EMA with the concentrations of 0.0009-0.001mg/mL and 0.009-0.01mg/mL respectively.
5. The method for analyzing the purity and the content of the organic impurities of the electronic-grade pyromellitic anhydride according to claim 1, wherein the preparation method of the sample solution to be tested comprises the following steps: weighing a sample 0.5g to 100mL in a volumetric flask, adding 79-80mL of phosphoric acid solution, heating to completely dissolve the sample, cooling to room temperature, fixing the volume to the scale with the phosphoric acid solution, shaking up, and filtering with a 0.45-micrometer syringe type water film for later use.
6. The method for analyzing the purity and the content of the organic impurities in the electronic grade pyromellitic anhydride according to claim 1, wherein the data processing method comprises the following steps:
firstly, making a standard curve according to the concentration of a standard substance to peak area, and then calculating according to the standard curve, wherein the calculation formula is as follows:
TMA content (%) - (TMA peak area)(sample)X concentration of(TMA Standard)Area of TMA peak(Standard substance))×100÷500×100％；
EMA content (%) ═ EMA peak area(sample)X concentration of(EMA standard)÷EArea of MA Peak(Standard substance))×100÷500×100％；
PMDA content (%) -100% to TMA content-EMA content.
7. The method of claim 1, wherein the liquid chromatography conditions comprise:
mobile phase: 0.01mol/L triethylamine solution methanol acetonitrile 80:5:15
A chromatographic column: sinochrom ODS-BP (5 μm, 4.6X 250mm)
Flow rate: 0.8-0.9mL/min
Wavelength: 210nm
Sample introduction amount: 60 μ L
Column temperature: 28-30 ℃.
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