CN111044666B - Analysis method for trace carbon powder and salt residue in dibasic acid - Google Patents
Analysis method for trace carbon powder and salt residue in dibasic acid Download PDFInfo
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- G—PHYSICS
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- 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
- G01N30/96—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 using ion-exchange
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- G—PHYSICS
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- 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
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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
- G01N30/14—Preparation by elimination of some components
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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
- G01N30/50—Conditioning of the sorbent material or stationary liquid
- G01N30/52—Physical parameters
- G01N30/54—Temperature
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
Abstract
The invention belongs to the technical field of chemical product detection, and particularly relates to a method for analyzing trace carbon powder and salt residue in dibasic acid. The method for analyzing the trace carbon powder and the salt residue in the dibasic acid utilizes the principle of similarity and intermiscibility to carry out pretreatment on a dibasic acid sample and separation and enrichment of the trace carbon powder and the residual salt, then detects the carbon powder by an optical method, and detects the salt by an ion chromatography. The sample treatment method provided by the invention has the advantages that the components to be detected are not lost, the components can be enriched, the accuracy of the detection result is guaranteed, the operation is simple, the result is accurate and reliable, the defects of measurement by a direct carbon powder observation method and a salt ash method are overcome, and the method is high in sensitivity, short in analysis time, accurate, reliable, simple and applicable.
Description
Technical Field
The invention belongs to the technical field of chemical product detection, and particularly relates to a method for analyzing trace carbon powder and salt residue in dibasic acid.
Background
Dibasic acids (such as sebacic acid, undecanedioic acid, dodecanedioic acid and other series products) are widely used, the production methods are different, for example, sebacic acid is produced by a castor oil cracking method, undecanedioic acid, dodecanedioic acid, tridecanedioic acid and the like are produced by a fermentation method, the product refining involves the preparation of the dibasic acids into monosodium salt or disodium salt, and the procedures of decolorization and neutralization by activated carbon, and the like, so that trace carbon powder and salt residues are caused by the method.
In addition, the salt residue is usually removed by adding a large amount of water and boiling, but some salt on the surface can be removed (because the long-chain dibasic acid is insoluble in water under normal pressure), so that the part wrapped in the interior of the granule cannot be removed, and therefore, the residue needs to be detected. The salinity is usually determined by an ash method, which has the following disadvantages: firstly, the salinity can decompose and lose partly when the high temperature, secondly this method is the salinity that detects the trace component, and when actually sampling according to ash method sample equivalent, the salinity content is too little, and weighing error is to the result influence very big.
The conventional method for detecting the carbon powder residue is direct observation (such as a magnifying glass or a microscope), which can only see the carbon powder particles on the particle surface, but cannot see the interior of the particle, which is a defect of the visual inspection method.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for analyzing trace carbon powder and salt residue in dibasic acid. The sample treatment method provided by the invention has the advantages that the components to be detected are not lost, the components can be enriched, the accuracy of the detection result is guaranteed, the operation is simple, the result is accurate and reliable, the defects of measurement by a direct carbon powder observation method and a salt ash method are overcome, and the method is high in sensitivity, short in analysis time, accurate, reliable, simple and applicable.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for analyzing trace carbon powder and salt residue in dibasic acid comprises sample pretreatment, carbon powder determination and salt determination, and specifically comprises the following steps:
(1) sample pretreatment: dissolving 80-120g of dibasic acid sample in 70-80 deg.C organic solvent, maintaining the temperature at 70-80 deg.C for 20-30min, vacuum filtering with 70-80 deg.C filter, washing, and vacuum drying; replacing the collection bottle, pressing 50-60 deg.C distilled water into the suction bottle of the suction filter, maintaining the temperature in the suction bottle for 10-15min to fully dissolve residual salt, suction filtering, washing the filter membrane with 50-60 deg.C distilled water for 3-5 times, collecting filtrate, and drying the filter membrane at 80-90 deg.C;
(2) carbon powder determination: observing the number of carbon powder on the filter membrane by using a microscope;
(3) and (3) salinity determination: the salt content of the filtrate was determined by ion chromatography.
The organic solvent is ethanol, and the water content in the ethanol is less than 0.05%.
The volume ratio of the mass of the dibasic acid to the absolute ethyl alcohol is 1: 3-5.
The dibasic acid is one of sebacic acid, undecanedioic acid, dodecanedioic acid, tridecanedioic acid and dibasic acids prepared by the same or similar method.
The medium of the suction filter is a microporous filter membrane which is a polytetrafluoroethylene membrane.
After a sample dissolved in the organic solvent is filtered, the sample is washed for 3 to 5 times by using absolute ethyl alcohol at the temperature of between 70 and 78 ℃, and the using amount of the absolute ethyl alcohol is 8 to 12mL each time.
The total magnification of the microscope is 200-600 times.
And during the carbon powder measurement, dividing the obtained filter membrane into 40-60 visual fields, observing 2-3 visual fields for counting, and then calculating the quantity of residual carbon powder.
The chromatographic conditions of the ion chromatography are as follows:
a chromatographic column: the cation chromatographic column is 4.6 multiplied by 125mm and 5 mu m, the stationary phase is polyvinyl alcohol filler, and the bonding phase is carboxyl;
the flow rate is 0.6-1.0mL/min, the column temperature is 25-35 ℃, the detection temperature is 35-45 ℃, and the sample injection amount is 10-30 muL;
a detector: a conductance detector;
mobile phase: 3-5mmol/L methane sulfonic acid solution;
the quantitative method comprises the following steps: and (4) an external standard method.
The device adopted in the step (1) for pretreating the sample comprises a sample dissolving device, a dissolved solution suction filtration device and a pure water heating device which are connected together, wherein the sample dissolving device comprises a dissolved material bottle, and a dibasic acid feeding hole, an absolute ethyl alcohol feeding hole, a nitrogen inlet and a material liquid outlet are formed in the dissolved material bottle;
the dissolved solution suction filtration device comprises a suction filtration bottle and a liquid receiving bottle which are connected together through a connector, and an emptying pipe is arranged on the suction filtration bottle;
the pure water heating device comprises a pure water heating bottle, and a pure water inlet, a pure water outlet and a nitrogen inlet are formed in the pure water heating bottle;
the outer layers of the material dissolving bottle, the filtering bottle and the pure water heating bottle are all provided with heat preservation devices, temperature measuring points are arranged on the material dissolving bottle and the pure water heating bottle, and a material liquid outlet of the material dissolving bottle and a pure water outlet of the pure water heating bottle are converged together and connected to the filtering bottle.
Compared with the prior art, the invention has the following advantages:
the sample processing method of the invention utilizes the principle of similarity and intermiscibility to carry out pretreatment on a binary acid sample and separation and enrichment of trace carbon powder and residual salt, then detects the carbon powder by an optical method, detects the salt by an ion chromatography, has no loss of components to be detected, can enrich, provides guarantee for the accuracy of detection results, has simple operation and accurate and reliable results, solves the defects of direct observation of the carbon powder and determination by a salt ash separation method, and has the advantages of high sensitivity, shorter analysis time, accurate and reliable analysis results, simplicity, quickness and applicability.
Drawings
FIG. 1 is a schematic view of the structure of an apparatus used for pretreatment of a sample.
FIG. 2 is a diagram showing the carbon powder obtained by observing the filter in a 400-fold microscopic field.
Description of reference numerals: 1-a solvent bottle; 2-1-filter flask; 2-2-liquid receiving bottle; 2-3-a connector; 2-4-a blow-down pipe; 3-pure water heating bottle.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The procedures, conditions, reagents, methods and the like for carrying out the present invention are, except as specifically mentioned below, common general knowledge and common general knowledge in the art.
The following examples 1 to 5 and comparative examples 1 to 2 all adopt the device shown in fig. 1 for sample pretreatment, and the device adopted for sample pretreatment comprises a sample dissolving device, a dissolved solution suction filtration device and a pure water heating device which are connected together, wherein the sample dissolving device comprises a dissolved material bottle 1, and the dissolved material bottle 1 is provided with a dibasic acid feeding hole, an absolute ethyl alcohol feeding hole, a nitrogen inlet and a material liquid outlet;
the dissolved solution suction filtration device comprises a suction filtration bottle 2-1 and a liquid receiving bottle 2-2 which are connected together through a connector 2-3, and an emptying pipe 2-4 is arranged on the suction filtration bottle 2-1;
the pure water heating device comprises a pure water heating bottle 3, and a pure water inlet, a pure water outlet and a nitrogen inlet are formed in the pure water heating bottle 3;
the outer layers of the material dissolving bottle 1, the filter flask 2-1 and the pure water heating bottle 3 are all provided with heat preservation devices, the heat preservation devices are used for preserving heat through hot water, temperature measurement points are arranged on the material dissolving bottle 1 and the pure water heating bottle 3, and a material liquid outlet of the material dissolving bottle 1 and a pure water outlet of the pure water heating bottle 3 are converged together and connected to the filter flask 2-1.
Example 1
A method for analyzing trace carbon powder and salt residue in dibasic acid comprises the following steps:
(1) sample pretreatment: weighing 90g of sebacic acid sample, adding 400mL of absolute ethyl alcohol, heating to 75 ℃, completely dissolving the sebacic acid sample, and keeping the temperature for 30 min; filtering the solution to dryness in a heat-preservation filter flask (adopting a polytetrafluoroethylene membrane with the specification of phi 50 and the pore diameter of 0.22 mu m) at 75 ℃, washing with 30mL of 75-DEG C absolute ethyl alcohol for three times, each time washing with 10mL, and draining the solvent; changing a filter flask, adding 25mL of 55 ℃ distilled water into a filter cup, preserving the heat for 15min, carrying out suction filtration until the solution is dry, washing a filter membrane with 30mL of 55 ℃ distilled water for three times, washing the filter membrane with 10mL each time, carrying out suction filtration until the solution is dry, transferring the filtrate into a 100mL volumetric flask, cooling the volumetric flask to room temperature, and carrying out constant volume to obtain a sample treatment solution, which is shown in figure 1;
(2) carbon powder determination: drying the organic microporous filter membrane at 85 ℃, dividing the organic microporous filter membrane into 50 visual fields, observing the organic microporous filter membrane under a microscope with the magnification of 400 times, counting the 3 visual fields, then calculating the quantity of residual carbon powder, and recording the observation result;
(3) and (3) salinity determination:
1. the instrument comprises the following steps: in an ICS 1000 ion chromatograph, a conductivity detector;
2. experimental samples: sodium ion standard solution purchased from great industry measurement technical research institute in north of Beijing, in an amount of: 1 mg/mL. Anhydrous sodium sulfate, reference reagent, purchased from the institute of optochemical fine chemistry, tianjin, content: 99.9 to 100.1 percent.
3. Chromatographic conditions are as follows:
a. a chromatographic column: cation chromatographic column IC YS-504.6X 125mm, 5 μm, stationary phase is polyvinyl alcohol filler, bonding phase is carboxyl;
b. mobile phase: the mobile phase is 4mmol/L methane sulfonic acid solution;
c. flow rate: 0.8 mL/min;
d. detector temperature: 40 ℃;
e. column temperature: 30 ℃;
f. sample introduction amount: 20 μ L.
4. A detection step:
1. accurately sucking sodium ion standard solutions with different volumes into different volumetric flasks respectively, adding water for dilution, diluting to a constant volume to a scale, shaking up, and preparing into solutions with concentrations of 1 mug/mL, 5 mug/mL, 10 mug/mL, 25 mug/mL and 50 mug/mL respectively as a series of standard solutions for later use.
2. And (3) sucking 10.00mL of sample treatment solution into a 100mL volumetric flask, adding water for dilution, fixing the volume and shaking up to obtain the solution to be detected.
3. And respectively injecting the standard solution and the solution to be detected into an ion chromatograph, carrying out ion chromatographic analysis according to the chromatographic conditions, and recording a chromatogram.
4. According to the chromatogram, the content of sodium ions is in ω and the number is expressed in mg/g, calculated according to the external standard method, formula (1):
in the formula:
c: the concentration of sodium ions in the solution to be detected is mu g/mL;
m: diacid sample mass, g.
The concentration of sodium ions in the sample solution is obtained or calculated on a standard curve according to the peak area, the content of the sodium ions is calculated, and the result is shown in Table 3.
Experiment of accuracy
Samples with known sodium ion content were taken, 5 parts of the samples were taken, and a certain amount of anhydrous sodium sulfate was added, respectively, and then, quantitative analysis was performed according to the above method, and the results are shown in table 1. As can be seen from the table, the average recovery of sodium sulfate was 99.08%. The experimental result shows that the method has good accuracy and strong feasibility.
TABLE 1 accuracy test results
Precision test
A batch of sebacic acid was taken, 5 groups of samples were accurately weighed from this batch, quantitative analysis was performed according to the above-described detection method, the content of sodium ions was determined, and the average value, standard deviation and relative standard deviation of the content were calculated, and the results are shown in table 2.
TABLE 2 results of the precision test
As can be seen from Table 2, the average value of the content of sodium ions is 0.103mg/g, the standard deviation is 0.0019, and the relative standard deviation is 1.87%, and the experimental result shows that the invention has good precision and strong feasibility.
As can be seen from the accuracy test and the precision test, the salt detection method has higher accuracy and precision.
Example 2
The same pretreatment method, the same sampling amount (same batch of product), the same test conditions and the results are shown in Table 3, which are exactly the same as those in example 1, and this example is used to examine the reproducibility and stability of the test method.
Example 3
The same pretreatment method, the same sampling amount (same batch of product), the same test conditions and the results are shown in Table 3, which are exactly the same as those in example 1, and this example is used to examine the reproducibility and stability of the test method.
Example 4 (varying sample dissolution incubation times within the scope of the claimed invention)
A method for analyzing trace carbon powder and salt residue in dibasic acid comprises the following steps:
(1) sample pretreatment: weighing 90g of sebacic acid sample, adding 400mL of absolute ethyl alcohol, heating to 75 ℃, completely dissolving the sebacic acid sample, and keeping the temperature for 20 min; filtering the solution to dryness in a heat-preservation filter flask (adopting a polytetrafluoroethylene membrane with the specification of phi 50 and the pore diameter of 0.22 mu m) at 75 ℃, washing the filter membrane with 10mL of 75-DEG C absolute ethyl alcohol for three times at each time, and draining the solvent; changing a filter flask, adding 25mL of 55 ℃ distilled water into a filter cup, preserving the heat for 15min, carrying out suction filtration until the solution is dry, washing a filter membrane with 30mL of 55 ℃ distilled water for three times, washing the filter membrane with 10mL of water each time, carrying out suction filtration until the solution is dry, transferring the filtrate into a 100mL volumetric flask, cooling to room temperature, and fixing the volume to obtain the sample treatment solution.
(2) Carbon powder determination: drying the organic microporous filter membrane at 85 ℃, dividing the organic microporous filter membrane into 50 visual fields, observing the organic microporous filter membrane under a microscope with the magnification of 400 times, counting the 3 visual fields, then calculating the quantity of residual carbon powder, and recording the observation result;
(3) salinity determination
Quantitative analysis was carried out according to the detection method of example 1, and the content of sodium ions was measured, and the results are shown in Table 3.
Example 5 (varying sample quality within the scope of the invention as claimed)
A method for analyzing trace carbon powder and salt residue in dibasic acid comprises the following steps:
(1) sample pretreatment: weighing 120g of sebacic acid sample, adding 400mL of absolute ethyl alcohol, heating to 75 ℃, completely dissolving the sebacic acid sample, and keeping the temperature for 30 min; filtering the solution to dryness in a heat-preservation filter flask (adopting a polytetrafluoroethylene membrane with the specification of phi 50 and the pore diameter of 0.22 mu m) at 75 ℃, washing with 30mL of 75-DEG C absolute ethyl alcohol for three times, each time washing with 10mL, and draining the solvent; and (3) changing a filter flask, adding 25mL of 55 ℃ distilled water into a filter cup, preserving the temperature for 15min, performing suction filtration until the solution is dry, washing the filter membrane by using 30mL of 55 ℃ distilled water for three times, performing suction filtration until the solution is dry, transferring the filtrate into a 100mL volumetric flask, cooling to room temperature, and fixing the volume to obtain the sample treatment solution.
(2) Carbon powder determination: drying the filter membrane at 85 ℃, dividing the filter membrane into 50 visual fields, observing 3 visual fields under a microscope with the magnification of 400 times for counting, then calculating the quantity of residual carbon powder, and recording the observation result;
(3) salinity determination
Quantitative analysis was carried out according to the detection method of example 1, and the content of sodium ions was measured, and the results are shown in Table 3.
Comparative example 1 (changing the sample dissolution incubation time outside the scope of the invention as claimed)
(1) Sample pretreatment: weighing 90g of sebacic acid sample, adding 400mL of absolute ethyl alcohol, heating to 75 ℃, completely dissolving the sebacic acid sample, and keeping the temperature for 15 min; filtering in a heat-preserving filter flask (device shown in figure 1) equipped with 0.22 μm organic microporous filter membrane at 75 deg.C, washing with 75 deg.C anhydrous ethanol 30mL for three times, each time 10mL, and draining off solvent; changing a filter flask, adding 25mL of 55 ℃ distilled water into a filter cup, preserving the temperature for 15min, performing suction filtration until the solution is dry, washing the filter membrane by using 30mL of 55 ℃ distilled water for three times, performing suction filtration until the solution is dry, transferring the filtrate into a 100mL volumetric flask, cooling to room temperature, and fixing the volume to obtain the sample treatment solution.
(2) Carbon powder determination: drying the filter membrane at 85 ℃, dividing the filter membrane into 50 visual fields, observing 3 visual fields under a microscope with the magnification of 400 times for counting, then calculating the quantity of residual carbon powder, and recording the observation result;
(3) salinity determination
Quantitative analysis was carried out according to the detection method of example 1, and the content of sodium ions was measured, and the results are shown in Table 3.
Comparative example 2 (removal of the Filter from the Hot Water washing operation)
(1) Sample pretreatment: weighing 90g of sebacic acid sample, adding 400mL of absolute ethyl alcohol, heating to 75 ℃, completely dissolving the sebacic acid sample, and keeping the temperature for 30 min; filtering the solution to dryness in a heat-preservation filter flask (adopting a polytetrafluoroethylene membrane with the specification of phi 50 and the pore diameter of 0.22 mu m) at 75 ℃, washing with 50mL of 75-DEG C absolute ethyl alcohol for three times, each time washing with 10mL, and draining the solvent; and (3) changing a filter flask, adding 25mL of distilled water with the temperature of 55 ℃ into a filter, preserving the temperature for 15min, carrying out suction filtration until the solution is dry, transferring the filtrate into a 100mL volumetric flask, cooling to the room temperature, and fixing the volume to obtain the sample treatment solution.
(2) Carbon powder determination: drying the filter membrane at 85 ℃, dividing the filter membrane into 50 visual fields, observing 3 visual fields under a microscope with the magnification of 400 times for counting, then calculating the quantity of residual carbon powder, and recording the observation result;
(3) and (3) salinity determination: quantitative analysis was carried out according to the detection method of example 1, and the content of sodium ions was measured, and the results are shown in Table 3.
The results of the detection of the carbon powder and the salt in examples 1 to 5 and comparative examples 1 to 2 were compared, and the results are shown in the following Table 3:
TABLE 3 determination of charcoal powder and salt content in dibasic acid
In summary, as can be seen from the comparison between the examples and the comparative examples in table 3, the detection conditions are the same and the detection results are substantially the same in examples 1 to 3; from examples 1-5, it can be seen that the operation conditions are changed within the allowable condition variation range of the invention, the detection result is not affected, the trace carbon powder and salt residue in the dibasic acid are detected according to the method of the invention, the result is accurate, the method is reliable, and the method can be practically used for detecting and monitoring the trace carbon powder and salt in the dibasic acid product;
as can be seen from comparative examples 1-2, the operation conditions (e.g., the dissolution holding time and the number of hot water washing) which are not changed within the range of the allowable conditions in the present invention have no influence on the results of carbon powder detection, and have a large influence on the results of salt detection, which requires strict control.
In the sample pretreatment process, the temperature of a sample dissolving solution is kept for 25-30min at 70-80 ℃, so that on one hand, the dibasic acid can be fully dissolved, and carbon powder and salt in particles are completely released; on the other hand, the salts are combined into larger particles to facilitate separation.
The organic microporous filter membrane is made of polytetrafluoroethylene, because an organic solvent is used, the filter membrane is prevented from being damaged by the solvent, and the pore diameter is 0.22 mu m to prevent small-particle carbon powder and salt from leaking (the carbon powder with smaller particle size is meaningless in product detection).
The present invention is not limited to the following embodiments, and variations and advantages that can be realized by one skilled in the art are intended to be included within the scope of the present invention and the appended claims.
Claims (9)
1. A method for analyzing trace carbon powder and salt residue in dibasic acid comprises sample pretreatment, carbon powder determination and salt determination, and is characterized by comprising the following steps:
(1) sample pretreatment: dissolving 80-120g of dibasic acid sample in 70-80 deg.C organic solvent, maintaining the temperature at 70-80 deg.C for 20-30min, vacuum filtering with 70-80 deg.C filter, washing, and vacuum drying; replacing a collection bottle, pressing distilled water with the temperature of 50-60 ℃ into a suction filter bottle of a suction filter, preserving the heat in the suction filter bottle for 10-15min to fully dissolve residual salt, carrying out suction filtration, washing the filter membrane for 3-5 times by using distilled water with the temperature of 50-60 ℃, collecting filtrate, and drying the filter membrane at the temperature of 80-90 ℃, wherein the organic solvent is absolute ethyl alcohol;
(2) carbon powder determination: observing the number of carbon powder on the filter membrane by using a microscope;
(3) and (3) salinity determination: the sodium ions in the filtrate were detected by ion chromatography.
2. The method for analyzing trace carbon powder and salt residue in dibasic acid as claimed in claim 1, wherein the volume ratio of the mass of the dibasic acid to the absolute ethanol is 1: 3-5.
3. The method as claimed in claim 1, wherein the dibasic acid is one of sebacic acid, undecanedioic acid, dodecanedioic acid and tridecanedioic acid.
4. The method for analyzing trace carbon powder and salt residue in dibasic acid as claimed in claim 1, wherein the medium of the filter is a microporous filter membrane, and the microporous filter membrane is a polytetrafluoroethylene membrane.
5. The method for analyzing trace carbon powder and salt residue in dibasic acid as claimed in claim 1, wherein the sample dissolved with organic solvent is filtered, and washed with 70-78 deg.C absolute ethanol for 3-5 times, wherein the amount of absolute ethanol used is 8-12mL each time.
6. The method as claimed in claim 1, wherein the total magnification of the microscope is 200-600 times.
7. The method for analyzing trace carbon powder and salt residue in dibasic acid as claimed in claim 1, wherein the filter membrane is divided into 40-60 fields for carbon powder measurement, 2-3 fields are observed for counting, and the amount of residual carbon powder is calculated.
8. The method for analyzing trace carbon powder and salt residue in dibasic acid as claimed in claim 1, wherein the chromatographic conditions of the ion chromatography are as follows:
a chromatographic column: the cation chromatographic column is 4.6 multiplied by 125mm and 5 mu m, the stationary phase is polyvinyl alcohol filler, and the bonding phase is carboxyl;
the flow rate is 0.6-1.0mL/min, the column temperature is 25-35 ℃, the detection temperature is 35-45 ℃, and the sample injection amount is 10-30 muL;
a detector: a conductance detector;
mobile phase: 3-5mmol/L methane sulfonic acid solution;
the quantitative method comprises the following steps: and (4) an external standard method.
9. The method for analyzing trace carbon powder and salt residue in dibasic acid according to claim 1, wherein the device used in the step (1) of pre-treating the sample comprises a sample dissolving device, a dissolving solution suction filtration device and a pure water heating device which are connected together, wherein the sample dissolving device comprises a dissolving bottle (1), and the dissolving bottle (1) is provided with a dibasic acid feeding port, an absolute ethyl alcohol feeding port, a nitrogen inlet and a feed liquid outlet;
the dissolved solution suction filtration device comprises a suction filtration bottle (2-1) and a liquid receiving bottle (2-2) which are connected together through a connector (2-3), and a vent pipe (2-4) is arranged on the suction filtration bottle (2-1);
the pure water heating device comprises a pure water heating bottle (3), and a pure water inlet, a pure water outlet and a nitrogen inlet are formed in the pure water heating bottle (3);
the outer layers of the material dissolving bottle (1), the filter flask (2-1) and the pure water heating bottle (3) are all provided with heat preservation devices, wherein the material dissolving bottle (1) and the pure water heating bottle (3) are all provided with temperature measuring points, and a material liquid outlet of the material dissolving bottle (1) and a pure water outlet of the pure water heating bottle (3) are gathered together and connected to the filter flask (2-1).
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