CN117368339A - Detection method for flocculant residue in machine-made sand - Google Patents
Detection method for flocculant residue in machine-made sand Download PDFInfo
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- CN117368339A CN117368339A CN202311148772.5A CN202311148772A CN117368339A CN 117368339 A CN117368339 A CN 117368339A CN 202311148772 A CN202311148772 A CN 202311148772A CN 117368339 A CN117368339 A CN 117368339A
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- 239000004576 sand Substances 0.000 title claims abstract description 68
- 238000001514 detection method Methods 0.000 title claims abstract description 43
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 47
- 238000004458 analytical method Methods 0.000 claims abstract description 31
- 238000004811 liquid chromatography Methods 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 26
- 238000012360 testing method Methods 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 claims abstract description 12
- 238000005303 weighing Methods 0.000 claims abstract description 10
- 229920000642 polymer Polymers 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 113
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 48
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 42
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 41
- 239000007853 buffer solution Substances 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 23
- 238000002347 injection Methods 0.000 claims description 17
- 239000007924 injection Substances 0.000 claims description 17
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000010413 mother solution Substances 0.000 claims description 12
- 241001411320 Eriogonum inflatum Species 0.000 claims description 9
- 125000000129 anionic group Chemical group 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 9
- 238000000605 extraction Methods 0.000 claims description 9
- 238000005259 measurement Methods 0.000 claims description 9
- 239000000872 buffer Substances 0.000 claims description 8
- 239000012071 phase Substances 0.000 claims description 8
- 239000003153 chemical reaction reagent Substances 0.000 claims description 6
- 238000004587 chromatography analysis Methods 0.000 claims description 6
- 239000003085 diluting agent Substances 0.000 claims description 6
- 238000010790 dilution Methods 0.000 claims description 6
- 239000012895 dilution Substances 0.000 claims description 6
- 230000014759 maintenance of location Effects 0.000 claims description 6
- 230000010355 oscillation Effects 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 238000010586 diagram Methods 0.000 claims description 4
- 239000012452 mother liquor Substances 0.000 claims description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 238000010276 construction Methods 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 10
- 235000019799 monosodium phosphate Nutrition 0.000 description 10
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 10
- 229910000162 sodium phosphate Inorganic materials 0.000 description 10
- 239000011521 glass Substances 0.000 description 9
- 239000008394 flocculating agent Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000005406 washing Methods 0.000 description 5
- 238000007865 diluting Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000011435 rock Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
-
- 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
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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
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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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
- G01N30/88—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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
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- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a detection method for flocculant residues in machine-made sand, which comprises the following steps: s1, preparing detection conditions, S2, preparing a sample, S3, preparing a standard curve, S4, confirming analysis conditions, and S5, calculating flocculant content. The specific process of S5 is as follows: and weighing a certain amount of machine-made sand containing the flocculant, extracting in different modes, testing the peak area of the polymer by utilizing a liquid chromatography, calculating the concentration of the polyacrylamide according to the standard working curve equation, and finally calculating the flocculant content in the machine-made sand according to the concentration value of the polyacrylamide. Compared with the prior art, the method is simple to operate and low in cost, the flocculant content in the machine-made sand can be detected more accurately, the error of the detection result is smaller, the quality condition of the machine-made sand is judged more accurately, the difficulty of controlling the concrete mixing building is reduced, the cost of deflocculating agent work is also reduced, and the method is more beneficial to guiding the on-site concrete production and construction.
Description
Technical Field
The invention relates to the field of buildings, in particular to a detection method for flocculant residues in machine-made sand.
Background
With the increasing development of the Chinese building industry, the usage amount of the building sand is increased, natural river sand is exploited for a long time, domestic high-quality river sand resources are scarce, the ecological balance and hydrologic stability of a river channel are seriously affected by the excessive exploitation and use of the natural river sand, the natural river sand is highly valued by the China, and the exploitation of the natural sand is forbidden by the corresponding policy, so that the replacement of the river sand by the machine-made sand is particularly important, and the replacement of the natural sand by the machine-made sand as the fine aggregate of cement concrete is promoted. Because the machine-made sand generates a large amount of rock powder in the production process, the rock powder contained in the machine-made sand is usually cleaned in a water washing mode at home. In recent years, because polyacrylamide has good thermal stability, is easy to dissolve in cold water and has long molecular chains, the polyacrylamide can bridge between two particles, accelerates the sedimentation of the particles, is a good flocculant, and is widely applied to a machine-made sand washing process by a machine-made sand factory.
At present, most domestic machine-made sand production processes use anionic polyacrylamide as a flocculant to flocculate and precipitate floating substances and fine particles in the sand, but due to the recycling of cleaning water, some flocculant components remain in the water-washing machine-made sand, and the residual flocculant in the machine-made sand causes the problems of poor workability, high viscosity, low flow rate, high loss and the like of the mixed concrete. At present, an effective method for flocculating agents in machine-made sand is to add deflocculant into an additive or add substances for degrading flocculating agents in the production process of finished machine-made sand, but the amount of flocculating agents contained in the produced machine-made sand cannot be controlled due to the fact that the adding amount of the flocculating agents is random in the production process of the machine-made sand and the circulation times of water washing machine-made sand are different. For specific content of flocculant in machine-made sand, rapid quantitative detection cannot be performed, most of the flocculant is estimated through the working performance of concrete mixture after concrete mixing, but the detection result is inaccurate by adopting the method, interference factors are more, the content of flocculant in the machine-made sand cannot be detected accurately, the difficulty of controlling building of a concrete mixing building is increased, the cost of deflocculating agent working is increased, and the quality of concrete is difficult to guarantee.
Therefore, the detection method which can accurately detect the flocculant content in the finished sand and provide data support for guiding concrete production is particularly important and has obvious significance in promoting the wider application of machine-made sand.
Disclosure of Invention
Aiming at the technical problems in the related art, the invention provides a detection method for flocculant residues in machine-made sand, which can overcome the defects in the prior art.
In order to achieve the technical purpose, the technical scheme of the invention is realized as follows:
a detection method for flocculant residues in machine-made sand comprises the following steps:
s1, preparing detection conditions: before detection, determining a liquid chromatograph, a chromatographic column, column temperature, mobile phase, reagent, buffer solution, detection wavelength, flow and sample injection amount to be adopted, wherein:
the mobile phase adopts 0.5mol/L NaH2PO4 aqueous solution and methanol, the pH value of the mobile phase is 3, and the volume ratio of the NaH2PO4 aqueous solution to the methanol in the mobile phase is 90:10 or 80:20, said diluent for said mobile phase being said buffer;
the reagent adopts an anionic polyacrylamide solution, wherein the anionic polyacrylamide solution is prepared into a mother solution by dissolving 0.5g of polyacrylamide into 1L of the buffer solution, namely, 0.5mg of polyacrylamide is contained in each milliliter of the mother solution;
the buffer solution is prepared from 0.5mol/L NaH2PO4 solution and distilled water, wherein the volume ratio of NaH2PO4 solution to distilled water in each 1L buffer solution=the volume ratio of methanol to NaH2PO4 aqueous solution in the mobile phase;
the detection wavelength is 200-220nm;
the flow rate is controlled between 1.0ml/min and 1.5ml/min;
the sample injection amount is 10-50 mu L;
s2, preparing a sample: sucking 1ml, 20ml, 40ml, 80ml, 120ml, 180ml and 200ml of the mother liquor, and then respectively adding the buffer solution for dilution, so as to respectively prepare 7 concentrations of standard samples of 5mg/L, 10mg/L, 20mg/L, 40mg/L, 60mg/L, 80mg/L and 100 mg/L;
s3, manufacturing a standard curve: measuring the peak area of each standard sample by using the liquid chromatograph in combination with the detection conditions, and drawing a standard curve of the relation between the peak area and the concentration of the standard sample to obtain a corresponding standard working curve equation;
s4, confirming analysis conditions: selecting different chromatographic conditions, measuring the retention time or the retention distance of each component on a chromatogram, namely measuring the peak area of each component, and measuring the content of each corresponding component by adopting a working curve method as a quantitative measurement parameter;
s5, calculating flocculant content: and weighing a certain amount of machine-made sand containing the flocculant, extracting in different modes, testing the peak area of the polymer by utilizing a liquid chromatography, and calculating the concentration of the polyacrylamide according to the standard working curve equation, namely the flocculant content in the machine-made sand.
Further, the step S3 specifically includes the following steps:
s301: taking each standard sample with the sample injection amount, carrying out chromatographic analysis on chromatographic conditions of each standard sample, and after a liquid chromatograph baseline is stabilized, carrying out sample injection analysis on the standard samples in sequence from low to high according to concentration, and timely recording and storing a spectrogram;
s302: and (3) repeating the operation steps of the step (S301) to carry out parallel measurement to obtain two groups of test data, wherein the relative deviation of the two groups of parallel test results is less than 5%, taking the average value of the two groups of test results, and drawing a standard curve according to the corresponding relation of each concentration.
Further, the step S5 specifically includes the following steps:
s501, preparation of an extractant: preparing a solution A, B, C, wherein each 1L of the solution A is prepared from 540mL of isopropanol, 450mL of deionized water and 10mL of ethanol; each 1L of the solution B is prepared from 740mL of isopropanol, 250mL of deionized water and 10mL of ethanol; each 1L of the solution C comprises 5mL of ethanol and isopropanol;
s502 sample treatment: weighing machine-made sand with a certain mass m as a sample to be measured, sequentially mixing the sample with a solution A, B, C, performing liquid chromatography analysis, calculating a peak response area according to a peak diagram obtained by the liquid chromatography analysis, and then bringing the peak response area into the standard working curve equation to obtain the concentration of polyacrylamide contained in the sample;
step 503 calculates the flocculant content in the machine-made sand: the content W of the polyacrylamide is calculated according to the following formula, wherein the W is calculated according to mass fraction, and the numerical value is expressed as percent;
in the formula:
x-is a concentration value of polyacrylamide calculated by the standard working curve equation, and the unit is mg/L;
v—the value of the volume of the solution, v=20, in mL;
m-the mass of the sample in g.
Further, the step S502 specifically includes the following steps:
s5021 mixing solution a: the mass m of the sample is 5g plus or minus 0.1mg, the sample is placed in a 50mL measuring cylinder with a plug, 15mL of the solution A is added for extraction, the bottle stopper of the measuring cylinder is covered, and stirring or forced oscillation is carried out for 40min;
s5022 mixing solution B: adding 15mL of the solution B, extracting, covering the bottle stopper of the measuring cylinder, stirring or shaking forcefully for 40min, and if the solution is not sticky, using the solution for liquid chromatography analysis; if the solution B is added and becomes sticky, re-weighing the sample to be measured, adding 15mL of the solution A, covering a measuring cylinder plug, and stirring or forcefully oscillating for 40min;
s5023 mixing solution C: adding 15mL of the solution C, stirring or shaking forcefully for 40min, and performing liquid chromatography analysis;
s5024 performs liquid chromatography analysis: the supernatant of the extracted solution was filtered with a 0.45 μm filter, and 20mL of the filtered solution was analyzed by a liquid chromatograph.
Further, the liquid chromatograph may be selected according to the actual needs, and a dishonest LC4000 type may be used.
Further, the column is preferably Eclipse XDB-C18 depending on the actual need.
Further, the column temperature setting of the chromatographic column is preferably 30-40 ℃ depending on the actual need.
The invention has the beneficial effects that: compared with the prior art, the method is simple to operate and low in cost, the flocculant content in the machine-made sand can be detected more accurately, the error of the detection result is smaller, and the quality condition of the machine-made sand can be judged more accurately; the flocculant content detected by the method is more accurate, so that the difficulty in controlling the concrete mixing building is reduced, the cost for deflocculating the flocculant is also reduced, and the concrete quality can be effectively ensured, thereby being more beneficial to guiding the on-site concrete production and construction.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but embodiments of the present invention are not limited thereto. The examples of the present invention are given solely for the purpose of illustration and are not intended to be limiting, so any modification of the present invention that is made by the method of the present invention falls within the scope of the present invention.
In order to facilitate understanding of the above technical solutions of the present invention, the following describes the above technical solutions of the present invention in detail by a specific usage manner.
A detection method for flocculant residues in machine-made sand comprises the following steps:
s1, preparing detection conditions: before detection, determining a liquid chromatograph, a chromatographic column, column temperature, mobile phase, reagent, buffer solution, detection wavelength, flow and sample injection amount to be adopted, wherein:
the mobile phase adopts 0.5mol/L NaH2PO4 aqueous solution and methanol, the pH value of the mobile phase is 3, and the volume ratio of the NaH2PO4 aqueous solution to the methanol in the mobile phase is 90:10 or 80:20, said diluent for said mobile phase being said buffer;
the reagent adopts an anionic polyacrylamide solution, wherein the anionic polyacrylamide solution is prepared into a mother solution by dissolving 0.5g of polyacrylamide into 1L of the buffer solution, namely, 0.5mg of polyacrylamide is contained in each milliliter of the mother solution;
the buffer solution is prepared from 0.5mol/L NaH2PO4 solution and distilled water, wherein the volume ratio of NaH2PO4 solution to distilled water in each 1L buffer solution=the volume ratio of methanol to NaH2PO4 aqueous solution in the mobile phase;
the detection wavelength is 200-220nm;
the flow rate is controlled between 1.0ml/min and 1.5ml/min;
the sample injection amount is 10-50 mu L;
s2, preparing a sample: sucking 1ml, 20ml, 40ml, 80ml, 120ml, 180ml and 200ml of the mother liquor, and then respectively adding the buffer solution for dilution, so as to respectively prepare 7 concentrations of standard samples of 5mg/L, 10mg/L, 20mg/L, 40mg/L, 60mg/L, 80mg/L and 100 mg/L;
s3, manufacturing a standard curve: measuring the peak area of each standard sample by using the liquid chromatograph in combination with the detection conditions, and drawing a standard curve of the relation between the peak area and the concentration of the standard sample to obtain a corresponding standard working curve equation;
s4, confirming analysis conditions: selecting different chromatographic conditions, measuring the retention time or the retention distance of each component on a chromatogram, namely measuring the peak area of each component, and measuring the content of each corresponding component by adopting a working curve method as a quantitative measurement parameter;
s5, calculating flocculant content: and weighing a certain amount of machine-made sand containing the flocculant, extracting in different modes, testing the peak area of the polymer by utilizing a liquid chromatography, and calculating the concentration of the polyacrylamide according to the standard working curve equation, namely the flocculant content in the machine-made sand.
In a preferred embodiment, step S3 specifically includes the steps of:
s301: taking each standard sample with the sample injection amount, carrying out chromatographic analysis on chromatographic conditions of each standard sample, and after a liquid chromatograph baseline is stabilized, carrying out sample injection analysis on the standard samples in sequence from low to high according to concentration, and timely recording and storing a spectrogram;
s302: and (3) repeating the operation steps of the step (S301) to carry out parallel measurement to obtain two groups of test data, wherein the relative deviation of the two groups of parallel test results is less than 5%, taking the average value of the two groups of test results, and drawing a standard curve according to the corresponding relation of each concentration.
In a preferred embodiment, step S5 specifically comprises the steps of:
s501, preparation of an extractant: preparing a solution A, B, C, wherein each 1L of the solution A is prepared from 540mL of isopropanol, 450mL of deionized water and 10mL of ethanol; each 1L of the solution B is prepared from 740mL of isopropanol, 250mL of deionized water and 10mL of ethanol; each 1L of the solution C comprises 5mL of ethanol and isopropanol;
s502 sample treatment: weighing machine-made sand with a certain mass m as a sample to be measured, sequentially mixing the sample with a solution A, B, C, performing liquid chromatography analysis, calculating a peak response area according to a peak diagram obtained by the liquid chromatography analysis, and then bringing the peak response area into the standard working curve equation to obtain the concentration of polyacrylamide contained in the sample;
step 503 calculates the flocculant content in the machine-made sand: the content W of the polyacrylamide is calculated according to the following formula, wherein the W is calculated according to mass fraction, and the numerical value is expressed as percent;
in the formula:
x-is a concentration value of polyacrylamide calculated by the standard working curve equation, and the unit is mg/L;
v—the value of the volume of the solution, v=20, in mL;
m-the mass of the sample in g.
In a preferred embodiment, step S502 specifically includes the steps of:
s5021 mixing solution a: the mass m of the sample is 5g plus or minus 0.1mg, the sample is placed in a 50mL measuring cylinder with a plug, 15mL of the solution A is added for extraction, the bottle stopper of the measuring cylinder is covered, and stirring or forced oscillation is carried out for 40min;
s5022 mixing solution B: adding 15mL of the solution B, extracting, covering the bottle stopper of the measuring cylinder, stirring or shaking forcefully for 40min, and if the solution is not sticky, using the solution for liquid chromatography analysis; if the solution B is added and becomes sticky, re-weighing the sample to be measured, adding 15mL of the solution A, covering a measuring cylinder plug, and stirring or forcefully oscillating for 40min;
s5023 mixing solution C: adding 15mL of the solution C, stirring or shaking forcefully for 40min, and performing liquid chromatography analysis;
s5024 performs liquid chromatography analysis: the supernatant of the extracted solution was filtered with a 0.45 μm filter, and 20mL of the filtered solution was analyzed by a liquid chromatograph.
In a preferred embodiment, the liquid chromatograph is selected as desired, preferably of the dishonest LC4000 type.
In a preferred embodiment, the chromatographic column is selected as desired, preferably eclipse XDB-C18.
In a preferred embodiment, the column temperature setting of the chromatographic column is, depending on the actual need, preferably 30-40 ℃.
Example 1
1. Sequentially preparing detection conditions, preparing samples and preparing standard curves
Instrument and conditions
High performance liquid chromatograph: dishonest LC4000 type;
chromatographic column: ecl ipse XDB-C18 (5 μm,4.6 mm. Times.150 mm);
mobile phase volume ratio: naH (NaH) 2 PO 4 Aqueous solution: methanol=90: 10, ph=3, naH 2 PO 4 The concentration of the aqueous solution is 0.5mol/L;
detection wavelength: 200nm;
flow rate: 1.0mL/min;
column temperature: 30 ℃;
sample injection amount: 50. Mu.L;
the specific implementation process comprises the following steps:
1. the mobile phase adopts NaH of 0.5mol/L 2 PO 4 Aqueous and methanol=90:10 (V: V), diluent NaH was used 2 PO 4 And (3) a buffer solution.
2. NaH of 0.5mol/L 2 PO 4 The volume ratio of the solution to distilled water is 10:90, configured as 1L buffer.
3. 0.5g of polyacrylamide is taken and dissolved in 1L of buffer, and the solution is mother solution, and each milliliter of the solution contains 0.5mg of polyacrylamide.
4. The mother solution is sucked into 1ml, 20ml, 40ml, 80ml, 120ml, 180ml and 200ml, and respectively put into a 1000ml volumetric flask, and buffer solution is added for dilution to the scale, so that 7 kinds of standard samples with the concentration of 5mg/L, 10mg/L, 20mg/L, 40mg/L, 60mg/L, 80mg/L and 100mg/L are prepared.
5. And (3) adopting a 50 mu L metering tube, carrying out chromatographic analysis according to the chromatographic condition described in 1, and after the baseline of the liquid chromatograph is stabilized, sequentially feeding samples for analysis from low to high according to the concentration of the standard sample, and timely recording and storing a spectrogram.
6. Repeating the operation steps of 5 to carry out parallel measurement to obtain two groups of test data, wherein the relative deviation of the two groups of parallel test results is below 5%, taking the average value of the two groups of test results, drawing a standard curve according to the corresponding concentration relation, and obtaining a standard working curve equation: y=6135X, and the linear correlation coefficient (R2) is 0.9689.
2. Confirming analysis conditions and calculating flocculant content
1. Preparation of extractant
(1) Solution a: a 1000mL graduated cylinder was taken, 540mL of isopropyl alcohol was mixed with 450mL of deionized water, 10mL of ethanol was added with a pipette, added dropwise to a 1000mL scale, and mixed well in a glass bottle.
(2) Solution B: taking a 1000mL measuring cylinder, mixing 740mL of isopropanol with 250mL of deionized water, adding 10mL of ethanol by a pipette, dripping to a 1000mL scale, and uniformly mixing in a glass bottle.
(3) Solution C: taking a 1000mL measuring cylinder, taking 5mL of ethanol by a pipette, adding the ethanol into the 1000mL measuring cylinder, diluting the mixture to a scale by isopropanol, uniformly mixing the mixture and storing the mixture in a glass bottle.
2. Sample processing
(1) The sample mass m=5 g (accurate to 0.1 mg) is weighed, the sample to be measured is placed in a 50mL measuring cylinder with a plug, 15mL of extraction solution a is added, the bottle stopper of the measuring cylinder is covered tightly, and stirring or forced oscillation is carried out for 40min.
(2) Then adding 15mL of the extraction solution B, covering the cylinder stopper, stirring or shaking forcefully for 40min, and if the solution is not sticky, performing liquid chromatography analysis.
(3) If the solution B is added and becomes sticky, the sample to be measured is re-weighed, 15mL of the solution A is added, the measuring cylinder stopper is tightly covered,
stirring or shaking with force for 40min. Then 15mL of solution C was added and stirred or vigorously shaken for 40min for liquid chromatography.
(4) Filtering the supernatant with 0.45 μm filter membrane, collecting 20mL of the filtered solution, analyzing with liquid chromatograph, and using NaH as buffer solution 2 PO 4 And (3) a buffer solution.
(5) And calculating the peak response area according to a peak diagram obtained by liquid chromatography, and substituting a standard working curve equation Y=6135X to obtain the concentration X, wherein the concentration is the concentration of polyacrylamide contained in 5g of sample.
3. Finally, the polyacrylamide is calculated according to mass fraction, and the numerical value is expressed in percent according to the following formula:
in the formula:
x-is the value of the concentration of polyacrylamide calculated by a standard working curve equation, and the unit is milligrams per liter (mg/L);
v—the value of the volume of the solution in milliliters (mL) (v=20);
m-the mass of the sample in grams (g).
Example 2
1. Sequentially preparing detection conditions, preparing samples and preparing standard curves
Instrument and conditions
High performance liquid chromatograph: dishonest LC4000 type
Chromatographic column: eclipse XDB-C18 (5 μm,4.6 mm. Times.150 mm)
Mobile phase volume ratio: naH (NaH) 2 PO 4 Aqueous solution: methanol=90: 10, ph=3, naH 2 PO 4 The concentration of the aqueous solution is 0.5mol/L;
detection wavelength: 210nm;
flow rate: 1.5mL/min;
column temperature: 40 ℃;
sample injection amount: 20. Mu.L;
the implementation steps are as follows:
1. the mobile phase adopts NaH of 0.5mol/L 2 PO 4 Aqueous and methanol=90:10 (V: V), diluent NaH was used 2 PO 4 And (3) a buffer solution.
2. NaH of 0.5mol/L 2 PO 4 The solution and distilled water were prepared in a volume ratio of 10:90 to 1L buffer.
3. 0.5g of polyacrylamide is taken and dissolved in 1L of buffer, and the solution is mother solution, and each milliliter of the solution contains 0.5mg of polyacrylamide.
4. The mother solution is sucked into 1ml, 20ml, 40ml, 80ml, 120ml, 180ml and 200ml, and respectively put into a 1000ml volumetric flask, and buffer solution is added for dilution to the scale, so that 7 kinds of standard samples with the concentration of 5mg/L, 10mg/L, 20mg/L, 40mg/L, 60mg/L, 80mg/L and 100mg/L are prepared.
5. And (3) adopting a 20 mu L metering tube, carrying out chromatographic analysis according to the chromatographic condition described in 1, and after the baseline of the liquid chromatograph is stabilized, sequentially feeding samples for analysis from low to high according to the concentration of the standard sample, and timely recording and storing a spectrogram.
6. Repeating the operation steps of 5 to carry out parallel measurement to obtain two groups of test data, wherein the relative deviation of the two groups of parallel test results is below 5%, taking the average value of the two groups of test results, drawing a standard curve according to the corresponding concentration relation, and obtaining a standard working curve equation: y=6725x, and the linear correlation coefficient (R2) is 0.9812.
2. Confirming analysis conditions and calculating flocculant content
1. Preparation of extractant
(1) Solution a: a 1000mL graduated cylinder was taken, 540mL of isopropyl alcohol was mixed with 450mL of deionized water, 10mL of ethanol was added with a pipette, added dropwise to a 1000mL scale, and mixed well in a glass bottle.
(2) Solution B: taking a 1000mL measuring cylinder, mixing 740mL of isopropanol with 250mL of deionized water, adding 10mL of ethanol by a pipette, dripping to a 1000mL scale, and uniformly mixing in a glass bottle.
(3) Solution C: taking a 1000mL measuring cylinder, taking 5mL of ethanol by a pipette, adding the ethanol into the 1000mL measuring cylinder, diluting the mixture to a scale by isopropanol, uniformly mixing the mixture and storing the mixture in a glass bottle.
2. Sample processing
(1) The sample mass m=5 g (accurate to 0.1 mg) is weighed, the sample to be measured is placed in a 50mL measuring cylinder with a plug, 15mL of extraction solution a is added, the bottle stopper of the measuring cylinder is covered tightly, and stirring or forced oscillation is carried out for 40min.
(2) Then adding 15mL of the extraction solution B, covering the cylinder stopper, stirring or shaking forcefully for 40min, and if the solution is not sticky, performing liquid chromatography analysis.
(3) If the solution B is added and becomes sticky, the sample to be measured is re-weighed, 15mL of the solution A is added, the measuring cylinder stopper is tightly covered,
stirring or shaking with force for 40min. Then 15mL of solution C was added and stirred or vigorously shaken for 40min for liquid chromatography.
(4) Filtering the supernatant with 0.45 μm filter membrane, collecting 20mL of the filtered solution, analyzing with liquid chromatograph, and using NaH as buffer solution 2 PO 4 And (3) a buffer solution.
(5) The peak response area was calculated from the peak pattern obtained by liquid chromatography, and the concentration X, which is the concentration of polyacrylamide contained in 5g of the sample, was obtained by substituting the standard operation curve equation y=6725x.
3. Finally, the polyacrylamide is calculated according to mass fraction, and the numerical value is expressed in percent according to the following formula:
in the formula:
x-is the value of the concentration of polyacrylamide calculated by a standard working curve equation, and the unit is milligrams per liter (mg/L);
v—the value of the volume of the solution in milliliters (mL) (v=20);
m-the mass of the sample in grams (g).
Example 3
1. Sequentially preparing detection conditions, preparing samples and preparing standard curves
Instrument and conditions
High performance liquid chromatograph: dishonest LC4000 type
Chromatographic column: eclipse XDB-C18 (5 μm,4.6 mm. Times.150 mm)
Mobile phase volume ratio: naH (NaH) 2 PO 4 Aqueous solution: methanol=90: 10, ph=3, naH 2 PO 4 The concentration of the aqueous solution is 0.5mol/L;
detection wavelength: 210nm;
flow rate: 1.5mL/min;
column temperature: 40 ℃;
sample injection amount: 20. Mu.L;
the implementation steps are as follows:
1. the mobile phase adopts NaH of 0.5mol/L 2 PO 4 Aqueous and methanol=80:20 (V: V), diluent NaH was used 2 PO 4 And (3) a buffer solution.
2. NaH of 0.5mol/L 2 PO 4 The solution and distilled water were prepared as 1L buffer solution at a volume ratio of 20:80.
3. 0.5g of polyacrylamide is taken and dissolved in 1L of buffer, and the solution is mother solution, and each milliliter of the solution contains 0.5mg of polyacrylamide.
4. The mother solution is sucked into 1ml, 20ml, 40ml, 80ml, 120ml, 180ml and 200ml, and respectively put into a 1000ml volumetric flask, and buffer solution is added for dilution to the scale, so that 7 kinds of standard samples with the concentration of 5mg/L, 10mg/L, 20mg/L, 40mg/L, 60mg/L, 80mg/L and 100mg/L are prepared.
5. And (3) adopting a 20 mu L metering tube, carrying out chromatographic analysis according to the chromatographic condition described in 1, and after the baseline of the liquid chromatograph is stabilized, sequentially feeding samples for analysis from low to high according to the concentration of the standard sample, and timely recording and storing a spectrogram.
6. Repeating the operation steps of 5 to carry out parallel measurement to obtain two groups of test data, wherein the relative deviation of the two groups of parallel test results is below 5%, taking the average value of the two groups of test results, drawing a standard curve according to the corresponding concentration relation, and obtaining a standard working curve equation: y=6362x, the linear correlation coefficient (R2) is 0.9554.
2. Confirming analysis conditions and calculating flocculant content
1. Preparation of extractant
(1) Solution a: a 1000mL graduated cylinder was taken, 540mL of isopropyl alcohol was mixed with 450mL of deionized water, 10mL of ethanol was added with a pipette, added dropwise to a 1000mL scale, and mixed well in a glass bottle.
(2) Solution B: taking a 1000mL measuring cylinder, mixing 740mL of isopropanol with 250mL of deionized water, adding 10mL of ethanol by a pipette, dripping to a 1000mL scale, and uniformly mixing in a glass bottle.
(3) Solution C: taking a 1000mL measuring cylinder, taking 5mL of ethanol by a pipette, adding the ethanol into the 1000mL measuring cylinder, diluting the mixture to a scale by isopropanol, uniformly mixing the mixture and storing the mixture in a glass bottle.
2. Sample processing
(1) The sample mass m=5 g (accurate to 0.1 mg) is weighed, the sample to be measured is placed in a 50mL measuring cylinder with a plug, 15mL of extraction solution a is added, the bottle stopper of the measuring cylinder is covered tightly, and stirring or forced oscillation is carried out for 40min.
(2) Then adding 15mL of the extraction solution B, covering the cylinder stopper, stirring or shaking forcefully for 40min, and if the solution is not sticky, performing liquid chromatography analysis.
(3) If the solution B is added and becomes sticky, the sample to be measured is re-weighed, 15mL of the solution A is added, the measuring cylinder stopper is tightly covered,
stirring or shaking with force for 40min. Then 15mL of solution C was added and stirred or vigorously shaken for 40min for liquid chromatography.
(4) Filtering the supernatant with 0.45 μm filter membrane, collecting 20mL of the filtered solution, analyzing with liquid chromatograph, and using NaH as buffer solution 2 PO 4 And (3) a buffer solution.
(5) The peak response area was calculated from the peak pattern obtained by liquid chromatography, and the peak response area was taken into the standard working curve equation y=6362x to obtain a concentration X, which is the concentration of polyacrylamide contained in 5g of the sample.
3. Finally, the polyacrylamide is calculated according to mass fraction, and the numerical value is expressed in percent according to the following formula:
in the formula:
x-is the value of the concentration of polyacrylamide calculated by a standard working curve equation, and the unit is milligrams per liter (mg/L);
v—the value of the volume of the solution in milliliters (mL) (v=20);
m-the mass of the sample in grams (g).
Comparative example 1
In comparison with example 2, comparative example 1 replaces the isopropanol of solution a in the extractant with an equal amount of methanol, the other being the same as in example 2.
Comparative example 2
In comparison with example 2, the sample of comparative example 2 was treated by stirring or shaking vigorously for 20 minutes, and the other steps were the same as in example 2.
Comparison of detection results
Finally, testing the flocculant content in the machine-made sand:
the method comprises the steps of selecting machine-made sand which is produced in a Jinshan stone crushing field and does not contain flocculating agent, preparing the flocculating agent into 4 kinds of machine-made sand containing different concentrations according to 0.02%, 0.04%, 0.06% and 0.08% for dissolution, then uniformly stirring, adding the machine-made sand into the selected machine-made sand, and drying the machine-made sand in a drying box. 4 kinds of sand containing flocculants at different concentrations were tested according to the above examples and comparative examples, and the results are shown in table 1 below.
TABLE 1 detection of sand by different flocculant concentration water washing machine
The final conclusion is that the detection shows that the flocculant content in the machine-made sand can be accurately detected in the examples compared with the comparative examples, the error between the flocculant content in the machine-made sand detected in the examples and the actual concentration is within 5%, and the machine-made sand has good fitting performance. As can be seen by comparing different embodiments, the volume ratio, the detection wavelength, the sample injection amount and the column temperature have influence on the detection result, but the influence is not great. The detection method is high in accuracy and has remarkable significance for machine-made sand production and on-site concrete construction.
The basic principle of the invention is as follows: the invention firstly uses anionic polyacrylamide to prepare flocculant samples without concentration, uses a high performance liquid chromatograph to measure the peak area of the anionic polyacrylamide solution, and draws a standard curve of the relation between the peak area and the concentration of the polyacrylamide solution. The test and actual errors are compared by changing the conditions of volume ratio, detection wavelength, sample injection amount, column temperature and the like in the embodiment, and the result shows that the error of the flocculant content in the machine-made sand and the actual concentration is within 5%. By varying the extractant type and agitation and vibration times in example 2, the results showed that the test and actual errors were 5% to 15%, and the lower the concentration, the greater the error.
In summary, by means of the technical scheme, compared with the prior art, the method is simple to operate and low in cost, the flocculant content in the machine-made sand can be detected more accurately, the detection result error is smaller, and the quality condition of the machine-made sand can be judged more accurately; the flocculant content detected by the method is more accurate, so that the difficulty in controlling the concrete mixing building is reduced, the cost for deflocculating the flocculant is also reduced, and the concrete quality can be effectively ensured, thereby being more beneficial to guiding the on-site concrete production and construction.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (7)
1. A detection method for flocculant residues in machine-made sand comprises the following steps:
s1, preparing detection conditions: before detection, determining a liquid chromatograph, a chromatographic column, column temperature, mobile phase, reagent, buffer solution, detection wavelength, flow and sample injection amount to be adopted, wherein:
the mobile phase adopts NaH of 0.5mol/L 2 PO 4 An aqueous solution and methanol, the pH value of the mobile phase is 3, and NaH in the mobile phase 2 PO 4 The volume ratio of the aqueous solution to the methanol is 90:10 or 80:20, said diluent for said mobile phase being said buffer;
the reagent adopts an anionic polyacrylamide solution, wherein the anionic polyacrylamide solution is prepared into a mother solution by dissolving 0.5g of polyacrylamide into 1L of the buffer solution, namely, 0.5mg of polyacrylamide is contained in each milliliter of the mother solution;
the buffer solution adopts NaH with the concentration of 0.5mol/L 2 PO 4 The solution and distilled water are prepared, and NaH in each 1L of the buffer solution 2 PO 4 Volume ratio of solution to distilled water = methanol to NaH in the mobile phase 2 PO 4 The volume ratio of the aqueous solution;
the detection wavelength is 200-220nm;
the flow rate is controlled between 1.0ml/min and 1.5ml/min;
the sample injection amount is 10-50 mu L;
s2, preparing a sample: sucking 1ml, 20ml, 40ml, 80ml, 120ml, 180ml and 200ml of the mother liquor, and then respectively adding the buffer solution for dilution, so as to respectively prepare 7 concentrations of standard samples of 5mg/L, 10mg/L, 20mg/L, 40mg/L, 60mg/L, 80mg/L and 100 mg/L;
s3, manufacturing a standard curve: measuring the peak area of each standard sample by using the liquid chromatograph in combination with the detection conditions, and drawing a standard curve of the relation between the peak area and the concentration of the standard sample to obtain a corresponding standard working curve equation;
s4, confirming analysis conditions: selecting different chromatographic conditions, measuring the retention time or the retention distance of each component on a chromatogram, namely measuring the peak area of each component, and measuring the content of each corresponding component by adopting a working curve method as a quantitative measurement parameter;
s5, calculating flocculant content: and weighing a certain amount of machine-made sand containing the flocculant, extracting in different modes, testing the peak area of the polymer by utilizing a liquid chromatography, and calculating the concentration of the polyacrylamide according to the standard working curve equation, namely the flocculant content in the machine-made sand.
2. The method according to claim 1, wherein step S3 specifically comprises the steps of:
s301: taking each standard sample with the sample injection amount, carrying out chromatographic analysis on chromatographic conditions of each standard sample, and after a liquid chromatograph baseline is stabilized, carrying out sample injection analysis on the standard samples in sequence from low to high according to concentration, and timely recording and storing a spectrogram;
s302: and (3) repeating the operation steps of the step (S301) to carry out parallel measurement to obtain two groups of test data, wherein the relative deviation of the two groups of parallel test results is less than 5%, taking the average value of the two groups of test results, and drawing a standard curve according to the corresponding relation of each concentration.
3. The method according to claim 1, wherein step S5 specifically comprises the steps of:
s501, preparation of an extractant: preparing a solution A, B, C, wherein each 1L of the solution A is prepared from 540mL of isopropanol, 450mL of deionized water and 10mL of ethanol; each 1L of the solution B is prepared from 740mL of isopropanol, 250mL of deionized water and 10mL of ethanol; each 1L of the solution C comprises 5mL of ethanol and isopropanol;
s502 sample treatment: weighing machine-made sand with a certain mass m as a sample to be measured, sequentially mixing the sample with a solution A, B, C, performing liquid chromatography analysis, calculating a peak response area according to a peak diagram obtained by the liquid chromatography analysis, and then bringing the peak response area into the standard working curve equation to obtain the concentration of polyacrylamide contained in the sample;
step 503 calculates the flocculant content in the machine-made sand: the content W of the polyacrylamide is calculated according to the following formula, wherein the W is calculated according to mass fraction, and the numerical value is expressed as percent;
in the formula:
x-is a concentration value of polyacrylamide calculated by the standard working curve equation, and the unit is mg/L;
v—the value of the volume of the solution, v=20, in mL;
m-the mass of the sample in g.
4. The method according to claim 3, wherein step S502 specifically comprises the steps of:
s5021 mixing solution a: the mass m of the sample is 5g plus or minus 0.1mg, the sample is placed in a 50mL measuring cylinder with a plug, 15mL of the solution A is added for extraction, the bottle stopper of the measuring cylinder is covered, and stirring or forced oscillation is carried out for 40min;
s5022 mixing solution B: adding 15mL of the solution B, extracting, covering the bottle stopper of the measuring cylinder, stirring or shaking forcefully for 40min, and if the solution is not sticky, using the solution for liquid chromatography analysis; if the solution B is added and becomes sticky, re-weighing the sample to be measured, adding 15mL of the solution A, covering a measuring cylinder plug, and stirring or forcefully oscillating for 40min;
s5023 mixing solution C: adding 15mL of the solution C, stirring or shaking forcefully for 40min, and performing liquid chromatography analysis;
s5024 performs liquid chromatography analysis: the supernatant of the extracted solution was filtered with a 0.45 μm filter, and 20mL of the filtered solution was analyzed by a liquid chromatograph.
5. The method according to claim 1, wherein the liquid chromatograph is of the dishonest LC4000 type.
6. The method of claim 1, wherein the chromatographic column is Eclipse XDB-C18.
7. The method according to claim 1, wherein the column temperature of the chromatographic column is set to 30-40 ℃.
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