CN114887491A - Method for judging membrane performance - Google Patents
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- CN114887491A CN114887491A CN202210460456.0A CN202210460456A CN114887491A CN 114887491 A CN114887491 A CN 114887491A CN 202210460456 A CN202210460456 A CN 202210460456A CN 114887491 A CN114887491 A CN 114887491A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D65/10—Testing of membranes or membrane apparatus; Detecting or repairing leaks
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G—PHYSICS
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- 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
- G01N30/8624—Detection of slopes or peaks; baseline correction
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Abstract
The invention discloses a method for judging membrane performance, which comprises the following steps: s1, collecting samples which pass through the filter membrane at different time periods; s2, filtering the obtained sample to obtain filtrate as a test solution for later use; s3, carrying out chromatographic analysis on the test solution to obtain a chromatogram of each test solution; s4, processing and calculating the chromatographic data of the test solution obtained in the S3 to obtain the retention time and the chromatographic peak area of each compound, and calculating the chromatographic peak area ratio of the compounds in different samples under the same retention time; and S5, judging whether the membrane performance is influenced or not based on the chromatographic peak area ratio of the compounds in different samples under the same retention time. The method has the characteristics of simple and easy operation and accurate judgment result, and is suitable for quickly and accurately judging whether the filter membranes of different types are polluted in the production process.
Description
Technical Field
The application relates to the technical field of product identification, in particular to a method for judging membrane performance.
Background
The membrane separation technology is a new separation technology which appears in the beginning of 20 th century and rapidly rises after 60 years of 20 th century. The membrane separation technology is characterized by taking a separation membrane as a core, taking pressure difference on two sides of the membrane as power, separating, concentrating, purifying and refining solute and solvent at normal temperature, and having the characteristics of high efficiency, energy conservation, environmental protection, simple molecular filtration and filtration process, easy control and the like, so the membrane separation technology is widely applied to the fields of food, medicine, biology, environmental protection, chemical industry, metallurgy, energy, petroleum, water treatment, electronics, bionics and the like, generates great economic benefit and social benefit, and becomes one of the most important means in the current separation science. The mixture of different particle size molecules on the molecular level realizes selective separation when passing through the semipermeable membrane, which is also called separation membrane or filter membrane, and the membrane wall is full of small holes, which can be divided into: microfiltration Membranes (MF), ultrafiltration membranes (UF), nanofiltration membranes (NF), reverse osmosis membranes (RO), and the like.
The microfiltration membrane can retain particles larger than 0.1 micron. Microfiltration membranes allow the passage of large molecules and dissolved solids (inorganic salts) and the like, but retain suspended matter, bacteria, high molecular weight colloids and the like. The concrete related field mainly includes: pharmaceutical industry, food industry (gelatin, wine, liquor, fruit juice, milk, etc.), high purity water, municipal sewage, industrial wastewater, drinking water, biotechnology, biological fermentation, etc.
The ultrafiltration membrane can intercept macromolecular substances and impurities between 0.002 and 0.1 micron. Ultrafiltration membranes allow the passage of small molecular substances and soluble solids (inorganic salts) etc. while retaining colloids, proteins, microorganisms and macromolecular organics, the cut molecular weight range for the size of the pore size of ultrafiltration membranes is typically between 1000-. Early industrial ultrafiltration was applied to wastewater and sewage treatment. With the development of ultrafiltration technology for over thirty years, ultrafiltration technology has now been involved in many fields such as food processing, beverage industry, pharmaceutical industry, biological agents, Chinese medicinal preparations, clinical medicine, printing and dyeing wastewater, wastewater treatment in food industry, resource recovery, environmental engineering, and the like.
Nanofiltration membranes can trap nano-sized (0.001 micron) substances. The operating interval of the nanofiltration membrane is between ultrafiltration and reverse osmosis, the molecular weight of the intercepted organic molecules is about 200-800, the capability of intercepting dissolved salts is 20-98%, the removal rate of soluble monovalent ions is lower than that of high-valence ions, such as 20-80% of sodium chloride and calcium chloride, and 90-98% of magnesium sulfate and sodium sulfate. The main application areas of nanofiltration relate to: food industry, plant deep processing, beverage industry, agricultural product deep processing, biological medicine, biological fermentation, fine chemical industry, environmental protection industry and the like.
Reverse osmosis membranes are the most delicate product of membrane separation that effectively retains all dissolved salts and organic matter with molecular weight greater than 100 while allowing water to pass through. Due to the characteristics of advanced, high-efficiency and energy-saving reverse osmosis separation technology, the method is widely applied to various departments of national economy, is mainly applied to water treatment and concentration of heat sensitive substances, and mainly applied to the following fields: food industry, milk industry, beverage industry, deep processing of plants (agricultural products), biomedicine, biological fermentation, preparation of drinking water, pure water, ultrapure water, seawater, brackish water desalination, electric power, electronics, semiconductor industry water, pharmaceutical industry process water, preparation water, injection water, sterile pyrogen-free pure water, process water for food and beverage industry, chemical industry and other industries, boiler water, washing water and cooling water.
In the process of using the membrane, the membrane flux is reduced due to the reduction or blockage of the membrane pore diameter caused by the adsorption and deposition of solids or solutes on the membrane surface or in the membrane pores, so that the separation performance is deteriorated, and the phenomenon of temporary irreversible change is called membrane pollution. Contamination must occur with the membrane. The traditional method for judging membrane pollution mainly comprises two methods, firstly, the method depends on the naked eyes of workers to observe, the method depends on the workers to develop, the defects of strong subjectivity and inaccurate result exist, once a membrane without pollution is replaced or cleaned by a judgment error, economic burden can be brought to an enterprise, and the operation cost of the enterprise is increased; and secondly, judgment is carried out by depending on experience, so that the defects of dependence on past experience and easiness in judgment error exist, and the invisible burden is brought to enterprises.
Disclosure of Invention
The invention aims to provide a method for judging membrane performance, which solves the defects of dependence on workers and experience and easy judgment error existing in the existing membrane pollution judgment, has the characteristics of simple and easy operation and accurate result, overcomes the defect of inaccurate judgment result in the prior art, and saves production cost.
A method of determining the performance of a membrane, comprising the steps of:
s1, collecting samples which pass through the filter membrane in different time periods;
s2, filtering the obtained sample to obtain filtrate as a test solution for later use;
s3, carrying out chromatographic analysis on the test solution to obtain a chromatogram of each test solution;
s4, processing and calculating the chromatographic data of the test solution obtained in the step S3 to obtain the retention time and chromatographic peak area of each compound, and calculating the chromatographic peak area ratio of the compounds in different samples under the same retention time;
and S5, judging whether the membrane performance is influenced or not based on the chromatographic peak area ratio of the compounds in different samples under the same retention time.
Preferably, the sample passed through the filter membrane is collected at the beginning of production in S1, followed by a fixed time interval or random collection of samples passed through the filter membrane.
Preferably, the sample obtained in S2 is filtered using a needle filter, and the filtrate is obtained as a test solution for use.
Preferably, if the ratio of S5 is greater than or equal to 2, the filter membrane needs to be replaced with a new one.
The method has the characteristics of simple and easy operation and accurate judgment result, and is suitable for quickly and accurately judging whether the filter membranes of different types are polluted in the production process.
Drawings
FIG. 1 is a chromatogram of a radix Puerariae nanofiltration membrane permeate collected 1 hour after starting up in example 1;
FIG. 2 is a chromatogram of a radix Puerariae nanofiltration membrane permeate collected 12 hours after the start of the device in example 1;
FIG. 3 is a chromatogram of an ultrafiltration membrane retentate of Gorgon fruit collected after 1 hour of starting up in example 2;
FIG. 4 is a chromatogram of an ultrafiltration membrane retentate of Gorgon fruit collected 26 hours after the start of the apparatus in example 2;
FIG. 5 is a chromatogram of the yam ceramic membrane retentate collected 1 hour after the start-up of example 3;
FIG. 6 is a chromatogram of the yam ceramic membrane retentate collected 18 hours after the start of the machine in example 3.
Detailed Description
Preferred embodiments of the present application will be described in further detail below with reference to the accompanying drawings.
Example 1
A method for judging the performance of a nanofiltration membrane comprises the following steps:
collecting radix Puerariae samples passing through membrane at different time periods
The method comprises the steps of collecting samples passing through the membrane in different time periods in a workshop production field, collecting the radix puerariae sample (nanofiltration membrane permeate) passing through the membrane once 1h after the startup, and collecting the radix puerariae nanofiltration membrane permeate once again after 12 hours.
② preparation of test solution
And (4) filtering the sample obtained in the step (i) by using a needle filter to obtain filtrate as a test solution for later use.
③ chromatographic data acquisition
Carrying out chromatographic analysis on the test solution obtained in the step II to obtain a chromatogram of each test solution, wherein the specific chromatographic analysis conditions are as follows:
chromatograph: the Agilent 1260 series (G1311C quaternary gradient pump, G1329B autosampler, G1316A column oven, G4212B diode array detector or G1314C variable wavelength ultraviolet detector);
a chromatographic column: waters T3 column, 5 μm, 4.6X 250 mm;
mobile phase: methanol-0.1% phosphoric acid in water as mobile phase gradient (elution gradient see table below):
TABLE 1
Flow rate: 1.0 mL/min; detection wavelength: 250 nm; column temperature: at 30 ℃.
Chromatographic data analysis and processing
Processing and calculating the chromatographic data of the test solution obtained in the step three to obtain the retention time and chromatographic peak area of each compound, and calculating the chromatographic peak area ratio of the compounds in different samples under the same retention time. The chromatogram is shown in the figures 1-2, and the calculation results are shown in the table 2.
TABLE 2
Membrane performance judgment
And (d) judging whether the membrane performance is influenced or not by combining the chromatographic peak area ratios of the compounds in different samples under the same retention time obtained in the step (iv) and the control requirements of the production process. The ratio of the chromatographic peak areas of the two samples in the same retention time is more than 2, which indicates that the membrane performance is affected, and the nanofiltration membrane needs to be replaced in order to ensure the production effect.
Example 2
A method for judging the performance of an ultrafiltration membrane comprises the following steps:
collecting gordon euryale seed samples passing through an ultrafiltration membrane in different time periods
Samples which pass through the membrane in different time periods are collected on a workshop production field, samples which pass through the membrane once (gordon euryale seed ultrafiltration membrane trapped fluid) are collected 1h after the machine is started, and ultrafiltration membrane trapped fluid is collected once again after 26 h intervals.
② preparation of test solution
And (4) filtering the sample obtained in the step (i) by using a needle filter to obtain filtrate as a test solution for later use.
③ chromatographic data acquisition
Carrying out chromatographic analysis on the test solution obtained in the step II to obtain a chromatogram of each test solution, wherein the specific chromatographic analysis conditions are as follows:
chromatograph: the Agilent 1260 series (G1311C quaternary gradient pump, G1329B autosampler, G1316A column oven, G4212B diode array detector or G1314C variable wavelength ultraviolet detector);
a chromatographic column: agilent ZORBAX SB-Aq column, 5 μm, 4.6 × 250 mm;
mobile phase: the gradient elution is carried out by taking acetonitrile-0.1 percent phosphoric acid aqueous solution as a mobile phase, and the elution gradient is shown in a table 3.
TABLE 3
| Time (min) | Acetonitrile (%) | 0.1% phosphoric acid aqueous solution (%) |
| 0 | 2 | 98 |
| 20 | 40 | 60 |
| 35 | 100 | 0 |
| 45 | 100 | 0 |
Flow rate: flow rate 1.0 mL/min; detection wavelength: 210 nm; column temperature: at 30 ℃.
Chromatographic data analysis and processing
Processing and calculating the chromatographic data of the test solution obtained in the step three to obtain the retention time and chromatographic peak area of each compound, and calculating the chromatographic peak area ratio of the compounds in different samples under the same retention time. The chromatogram is shown in FIGS. 3-4, and the calculation results are shown in Table 4.
TABLE 4
Membrane performance judgment
And (d) judging whether the membrane performance is influenced or not by combining the chromatographic peak area ratios of the compounds in different samples under the same retention time obtained in the step (iv) and the control requirements of the production process. The chromatographic peak area ratios of the two samples under the same retention time are close, which indicates that the membrane has good performance and is not influenced and can be continuously used.
Example 3
A method for judging the performance of a ceramic membrane comprises the following steps:
firstly, collecting yam samples passing through a ceramic membrane in different time periods
Collecting samples passing through the membrane in different time periods in a workshop production field, collecting samples (yam ceramic membrane trapped fluid) passing through the membrane once 1h after starting up, and collecting the ceramic membrane trapped fluid once after 18 h.
② preparation of test solution
And (4) filtering the sample obtained in the step (i) by using a needle filter to obtain filtrate as a test solution for later use.
③ chromatographic data acquisition
Carrying out chromatographic analysis on the test solution obtained in the step II to obtain a chromatogram of each test solution, wherein the specific chromatographic analysis conditions are as follows:
chromatograph: agilent 1260 series, USA (G1311C quaternary gradient pump, G1329B autosampler, G1316A column oven, G4212B diode array detector or G1314C variable wavelength ultraviolet detector); a chromatographic column: waters T3 column, 5 μm, 4.6X 250 mm; mobile phase: methanol/0.1% phosphoric acid/water as mobile phase gradient (elution gradient see table 5 below).
TABLE 5
Flow rate: 1.0 mL/min; detection wavelength: the detection wavelength is 230nm in 0-7 min and 258nm in 7-65 min; column temperature: at 30 ℃.
Chromatographic data analysis and processing
Processing and calculating the chromatographic data of the test solution obtained in the step three to obtain the retention time and chromatographic peak area of each compound, and calculating the chromatographic peak area ratio of the compounds in different samples under the same retention time. The chromatogram is shown in FIGS. 5-6, and the calculation results are shown in Table 6.
TABLE 6
Membrane performance judgment
And (d) judging whether the membrane performance is influenced or not by combining the chromatographic peak area ratios of the compounds in different samples under the same retention time obtained in the step (iv) and the control requirements of the production process. The ratio of the chromatographic peak areas of the two samples at the same retention time exceeds 2, which indicates that the membrane performance is affected, and the two samples need to be replaced in order to ensure the production effect.
Claims (4)
1. A method of determining the performance of a membrane, comprising the steps of:
s1, collecting samples which pass through the filter membrane at different time periods;
s2, filtering the obtained sample to obtain filtrate as a test solution for later use;
s3, carrying out chromatographic analysis on the test solution to obtain a chromatogram of each test solution;
s4, processing and calculating the chromatographic data of the test solution obtained in the step S3 to obtain the retention time and chromatographic peak area of each compound, and calculating the chromatographic peak area ratio of the compounds in different samples under the same retention time;
and S5, judging whether the membrane performance is influenced or not based on the chromatographic peak area ratio of the compounds in different samples under the same retention time.
2. The method of claim 1, wherein the sample passed through the filter membrane is collected at the beginning of production in S1, followed by a fixed time interval or random collection of the sample passed through the filter membrane.
3. The method of claim 1, wherein the sample obtained in S2 is filtered using a needle filter to obtain a filtrate as a test solution for use.
4. The method of claim 1, wherein if the ratio of S5 is greater than or equal to 2, the filter membrane needs to be replaced with a new one.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2017094259A (en) * | 2015-11-20 | 2017-06-01 | 株式会社クラレ | Membrane fouling inhibitor |
| WO2017164540A1 (en) * | 2016-03-21 | 2017-09-28 | 고려대학교 산학협력단 | Apparatus for predicting membrane fouling in forward osmosis and method for predicting membrane fouling in forward osmosis |
| CN114280106A (en) * | 2021-12-29 | 2022-04-05 | 杭州电子科技大学 | Online discrimination system and discrimination method for membrane pollution in industrial sewage treatment process |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2017094259A (en) * | 2015-11-20 | 2017-06-01 | 株式会社クラレ | Membrane fouling inhibitor |
| WO2017164540A1 (en) * | 2016-03-21 | 2017-09-28 | 고려대학교 산학협력단 | Apparatus for predicting membrane fouling in forward osmosis and method for predicting membrane fouling in forward osmosis |
| CN114280106A (en) * | 2021-12-29 | 2022-04-05 | 杭州电子科技大学 | Online discrimination system and discrimination method for membrane pollution in industrial sewage treatment process |
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