CN106124387A - A kind of method of testing of ultrafilter membrane rejection - Google Patents
A kind of method of testing of ultrafilter membrane rejection Download PDFInfo
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- CN106124387A CN106124387A CN201610843125.XA CN201610843125A CN106124387A CN 106124387 A CN106124387 A CN 106124387A CN 201610843125 A CN201610843125 A CN 201610843125A CN 106124387 A CN106124387 A CN 106124387A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/082—Investigating permeability by forcing a fluid through a sample
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N2015/086—Investigating permeability, pore-volume, or surface area of porous materials of films, membranes or pellicules
Abstract
The present invention relates to the method for testing of a kind of ultrafilter membrane rejection.Thing on the basis of star Polyethylene Glycol (star PEG), under room temperature, ultrafiltration retention experiments is carried out under the conditions of determining intake pressure, take material liquid and filtrate after colour reagent color development treatment, ultraviolet-uisible spectrophotometer is used to measure the absorbance at 510 nm, the concentration of star PEG is calculated, then according to formula calculating rejection R (%): R=(1 C according to known standard curve p /C f ) × 100%, in formula, C p It is the concentration of star PEG in filtrate；C f It is the concentration of star PEG in material solution.The rejection using star PEG to measure is affected little by concentration and pressure.Therefore, star PEG can overcome water soluble linear macromolecule and the deficiency of protein-based spherical macromolecule primary standard substance, the problems such as current primary standard substance quantity few, narrow application range, fouling membrane can be solved as the preferable primary standard substance of ultrafilter membrane rejection test, improve the accuracy of test result.
Description
Technical field
The present invention relates to the method for testing of a kind of ultrafilter membrane rejection.
Background technology
Molecular cut off is that different industries is distinguished for difference separation demand and selects ultrafilter membrane, makes ultrafilter membrane apply
Important evidence (Kanagaraj P, Nagendran A, Rana D, the Matsuura T, Neelakandan shot the arrow at the target
S, Karthikkumar T, Muthumeenal A. Influence of N-phthaloyl chitosan on poly
(ether imide) ultrafiltrationmembranes and its application in biomolecules
and toxic heavy metalion separation and their antifouling properties. Applied Surface Science, 2015,329:165-173.).Therefore, the molecular cut off the most accurately measuring ultrafilter membrane becomes
For the most important research topic.By measuring a series of primary standard substance with known molecular amount rejection on ultrafilter membrane
Determine the method for molecular cut off be used widely because it is easy and directly perceived (Rohani R, Hyland M,
Patterson D. A refined one-filtration method for aqueous based nanofiltration
and ultrafiltration membrane molecular weight cut-off determination using
polyethylene glycols. Journal of Membrane Science, 2011,382 (1-2): 278-290.),
But currently used primary standard substance disunity, lack of standardization, therefore the rejection measurement result accuracy of ultrafilter membrane and repeatability are not
Good, there is the biggest error.
According to China's ultrafilter membrane testing standard " hollow fiber ultrafiltration membrane method of testing " (HY/T 050-1999), commonly use at present
Ultrafilter membrane rejection rate test primary standard substance mainly have Polyethylene Glycol (PEG), polyvinylpyrrolidone, poly(ethylene oxide), Portugal
The protides such as the water-soluble linear macromolecule such as polysaccharide and bovine serum albumin, ovalbumin, cytochrome C, gamma globulin are spherical
The big class of macromolecule two.
Although the compounds such as Polyethylene Glycol, poly(ethylene oxide) and glucosan possess purity height, stable in properties, molecular weight distribution
The advantage such as narrow.But, these water-soluble linear high molecular random coil structures are more easily damaged in fluid field, and extended chain leads to
Crossing " snakelike effect " and pass less hole, susceptiveness and the repeatability of test result are poor, it is impossible to definitely symbolize ultrafilter membrane
Cutoff performance, the rejection measured is unreliable.
The spherical macromolecule of protide has the advantages such as range of molecular weight distributions is the least, molecular shape is the most rounded,
As reflecting the true aperture of ultrafilter membrane during primary standard substance, the therefore good stability of test result, experimental repeatability is good (to be wished and shakes
Prosperous, Wu Liming, Hu Xiao. the molecular weight cut off of conventional ultrafilter membrane is measured with the ovalbumin in Ovum Gallus domesticus album.Membrane science with Technology, 1995,19 (5): 44-50.).But they there is also some defects: the spherical of (1) protein is nonrigid,
It is easily subject to the impact of test condition (such as pressure, temperature variation)；(2) the molecular weight scope of application of protein is the least, therefore
When the ultrafilter membrane that mensuration molecular cut off is different, needing to select the protein-based primary standard substance of different molecular weight, this is in certain journey
Error is easily caused on degree；(3) absorption property of protein substance membrane material is bigger, easily causes fouling membrane, impact test
Accuracy；(4) price of protein is the most costly.The most water-soluble linear macromolecule or protein-based spherical
All there is certain defect in macromolecule.
Summary of the invention
It is an object of the invention to provide the method for testing of a kind of new ultrafilter membrane rejection, the method selects the poly-second of star
Thing on the basis of glycol (star PEG), can overcome water soluble linear macromolecule and protein-based spherical macromolecule primary standard substance not
Foot, solves the problem such as primary standard substance quantity few, narrow application range, fouling membrane in the test of current Retention Ratio of The Ultrafiltration Membrane, improves test
The repeatability of result and accuracy.
The step that the method for testing of a kind of ultrafilter membrane rejection that the present invention provides includes: thing on the basis of star PEG, joins
The star PEG aqueous solution of the given concentration of system, under room temperature, carries out ultrafiltration retention experiments, material liquid under the conditions of determining intake pressure
After colour reagent (Dragendoff reagent and acetic acid-sodium acetate buffer solution) processes, UV-vis spectroscopy is used with filtrate
Photometer (Lambda45, PerkinElmer company of the U.S.) measures the absorbance at 510 nm, according to known standard curve
Calculate the concentration of star PEG, then according to formula calculating rejection R (%):
R = (1-C p /C f ) × 100%
In formula, C p It is the concentration of star PEG in filtrate；C f It is the concentration of star PEG in material solution.
Described star PEG refers to that the PEG side chain of at least more than 3 and each bar chain dereliction take second place point, pass through chemical bond
The special branched PEG of class and the derivant thereof being connected on same centronucleus, in water soluble, and has Series Molecules amount.
The step that the method for testing of a kind of ultrafilter membrane rejection that the present invention provides specifically includes:
1) compound concentration is the star PEG aqueous solution of 500 mg/L ~ 5000 mg/L, under room temperature, is 0.1 MPa at intake pressure
Carrying out ultrafiltration retention experiments under the conditions of ~ 0.3 MPa, ultrafiltration runs time 30 min ~ 60 min.
2) material liquid and filtrate are taken at colour reagent (Dragendoff reagent and acetic acid-sodium acetate buffer solution) colour developing
Ultraviolet-visible spectrophotometer is used to measure the absorbance at 510 nm after managing 15 min.
3) concentration of star PEG is calculated according to known standard curve, then according to formula calculating rejection R (%):
R = (1-C p /C f ) × 100%
In formula, C p It is the concentration of star PEG in filtrate；C f It is the concentration of star PEG in material solution.
Term: star PEG typically refers to the PEG side chain of at least more than 3 and each bar chain dereliction takes second place point, by chemistry
The bonded special branched PEG of class and a derivant thereof on same centronucleus.Such as, four side chains it is bonded by chemistry
It is connected on same centronucleus the branched PEG, the star PEG(of referred to as four arms formed and is expressed as 4-arm PEG-OH), its structure
Formula is:The derivant of star PEG or star PEG has star polymerization
The general characteristic of thing, such as its molecule spherical structure symmetrically, it is to avoid intramolecular is tangled, and intermolecular reciprocal action is less, therefore
Its bulk viscosity is less than the linear polymer of same molecular amount.Comprising several in the derivant of described star PEG is radiation
The PEG construction unit of shape, wherein the terminal substituent of every PEG strand can be amido, sulfydryl, carboxyl, aldehyde radical, hydroxyl,
Methylol etc..
It is an advantage of the current invention that star PEG is connected on same centronucleus be formed with chemical bond by multiple side chains
Branched polymer, molecules in solution structure spherical in shape, stably it is unlikely to deform, avoids the entanglement between strand simultaneously, use it
The rejection measured then is affected little by concentration and pressure.Therefore, star PEG can overcome water soluble linear macromolecule and protein
The deficiency of class spherical macromolecule primary standard substance, becomes the preferable primary standard substance of ultrafilter membrane rejection test, solves current primary standard substance number
Amount less, the problem such as narrow application range, fouling membrane, improve the accuracy of test result.These features meet ultrafilter membrane and retain molecule
Measure the requirement of primary standard substance on probation.Range of application of the present invention is suitable for the wafer type ultrafilter membrane that molecular cut off is 1000-100000
Or the test of the rejection of fiber film component.The present invention is that Accurate Determining ultrafilter membrane rejection provides a kind of simple side
Method.
Accompanying drawing explanation
Fig. 1 molecular weight be 10000 4-arm PEG-OH on the basis of the standard curve of thing.
The rejection of the ultrafilter membrane that Fig. 2 difference primary standard substance concentration measures.
The rejection of the ultrafilter membrane measured under the conditions of Fig. 3 different pressures.
Detailed description of the invention
Below in conjunction with specific embodiment, it is further elaborated on the present invention.The experiment of unreceipted actual conditions in embodiment
Method, generally according to the condition described in normal condition and handbook, or according to the condition proposed by manufacturer；Used is logical
With equipment, material, reagent etc., if no special instructions, the most commercially obtain.
Embodiment 1
By wafer type ultrafilter membrane (PES10K, Pu Nasi), it is installed in ultrafiltration cup (8000 types, millipore), with 4-arm
PEG-OH(this star PEG has four PEG arms, and the end group of every PEG arm is hydroxyl, and molecular weight is 10000 g/mol, and product is compiled
Number: PJK-401, purchased from Wuxi spirit stannum medical apparatus and instruments science and technology company limited, network address: http://www.lxbiotech.com/
product1.asp?Pcid1=1&pcid2=23) thing on the basis of, compound concentration is the 4-arm PEG-OH solution of 5000 mg/L,
At room temperature, intake pressure is to carry out ultrafiltration retention experiments under conditions of 0.1 MPa, and ultrafiltration runs time 30 min, takes raw material
Liquid and filtrate are adopted after conventional colour reagent (Dragendoff reagent and acetic acid-sodium acetate buffer solution) color development treatment 15 min
The absorbance at 510 nm, root is measured with ultraviolet-visible spectrophotometer (Lambda45, PerkinElmer company of the U.S.)
The concentration of 4-arm PEG-OH is calculated, then according to formula calculating rejection R (%) according to known standard curve:
R = (1-C p /C f ) × 100%
In formula, C p It is the concentration of 4-arm PEG-OH in filtrate；C f It is the concentration of 4-arm PEG-OH in material solution.
Embodiment 2
Hyperfiltration membrane assembly (PVDF10K, self-control) is installed on ultrafilter membrane rejection test device, with 4-arm PEG-OH(this
Star PEG has four PEG arms, and the end group of every PEG arm is hydroxyl, and molecular weight is 10000 g/mol, production code member: PJK-
401, Wuxi spirit stannum medical apparatus and instruments science and technology company limited) on the basis of thing, compound concentration is that the 4-arm PEG-OH of 5000 mg/L is molten
Liquid, at room temperature, intake pressure is to carry out ultrafiltration retention experiments under conditions of 0.1 MPa, and ultrafiltration runs time 60 min, takes former
Feed liquid and filtrate are after conventional colour reagent (Dragendoff reagent and acetic acid-sodium acetate buffer solution) color development treatment 15 min
Ultraviolet-visible spectrophotometer (Lambda45, PerkinElmer company of the U.S.) is used to measure the absorbance at 510 nm,
The concentration of 4-arm PEG-OH is calculated, then according to formula calculating rejection R (%) according to known standard curve:
R = (1-C p /C f ) × 100%；
In formula, C p It is the concentration of 4-arm PEG-OH in filtrate；C f It is the concentration of 4-arm PEG-OH in material solution.
Embodiment 3
By wafer type ultrafilter membrane (PES10K, Pu Nasi), it is installed in ultrafiltration cup (8000 types, millipore), with 4-arm
PEG-OH(this star PEG has four PEG arms, and the end group of every PEG arm is hydroxyl, and molecular weight is 10000 g/mol, and product is compiled
Number: PJK-401, Wuxi spirit stannum medical apparatus and instruments science and technology company limited) on the basis of thing, compound concentration is the 4-arm of 500 mg/L
PEG-OH solution, at room temperature, intake pressure is to carry out ultrafiltration retention experiments under conditions of 0.1 MPa, and ultrafiltration runs the time 30
Min, takes material liquid and filtrate through conventional colour reagent (Dragendoff reagent and acetic acid-sodium acetate buffer solution) color development treatment
Ultraviolet-visible spectrophotometer (Lambda45, PerkinElmer company of the U.S.) is used to measure at 510 nm after 15 min
Absorbance, calculates the concentration of 4-arm PEG-OH, then according to formula calculating rejection R (%) according to known standard curve:
R = (1-C p /C f ) × 100%
In formula, C p It is the concentration of 4-arm PEG-OH in filtrate；C f It is the concentration of 4-arm PEG-OH in material solution.
Embodiment 4
By wafer type ultrafilter membrane (PES10K, Pu Nasi), it is installed in ultrafiltration cup (8000 types, millipore), with 4-arm
PEG-OH(this star PEG has four PEG arms, and the end group of every PEG arm is hydroxyl, and molecular weight is 10000 g/mol, and product is compiled
Number: PJK-401, Wuxi spirit stannum medical apparatus and instruments science and technology company limited) on the basis of thing, compound concentration is the 4-arm of 5000 mg/L
PEG-OH solution, under room temperature, intake pressure is to carry out ultrafiltration retention experiments under conditions of 0.3 MPa, and ultrafiltration runs the time 60
Min, takes material liquid and filtrate through conventional colour reagent (Dragendoff reagent and acetic acid-sodium acetate buffer solution) color development treatment
After, use ultraviolet-visible spectrophotometer (Lambda45, PerkinElmer company of the U.S.) to measure the extinction at 510 nm
Degree, calculates the concentration of 4-arm PEG-OH, then according to formula calculating rejection R (%) according to known standard curve:
R = (1-C p /C f ) × 100%
In formula, C p It is the concentration of 4-arm PEG-OH in filtrate；C f It is the concentration of 4-arm PEG-OH in material solution.
Molecular weight be 10000 4-arm PEG-OH on the basis of the standard curve of thing as it is shown in figure 1, use different 4-arm
The rejection of the ultrafilter membrane that PEG-OH concentration measures is as shown in Figure 2.4-arm PEG-OH concentration keeps 5000mg/L constant, different
The rejection of the ultrafilter membrane measured under pressure condition is as shown in Figure 3.Result shows, on the basis of selection 4-arm PEG-OH during thing,
Change test concentrations and intake pressure, the least on the impact of rejection test result.
The present invention propose a kind of on the basis of star PEG the ultrafilter membrane rejection method of testing of thing be different from water solublity line
Shape macromolecule and protein-based spherical macromolecule primary standard substance, it is possible to increase the repeatability of ultrafilter membrane rejection test is with accurate
Property.
Claims (5)
1. the method for testing of a ultrafilter membrane rejection, it is characterised in that step is as base with star Polyethylene Glycol (star PEG)
Quasi-thing, the star PEG aqueous solution of the given concentration of preparation, under room temperature, under the conditions of determining intake pressure, carry out ultrafiltration retention experiments,
Ultrafiltration runs a period of time, takes material liquid and filtrate through colour reagent Dragendoff reagent and acetic acid-sodium acetate buffer solution
After color development treatment 15 min, ultraviolet-visible spectrophotometer is used to measure the absorbance at 510 nm, according to known standard
Curve calculates the concentration of star PEG, then according to formula calculating rejection R (%):
R = (1-C p /C f ) × 100%
In formula, C p It is the concentration of star PEG in filtrate；C f It is the concentration of star PEG in material solution.
Method of testing the most according to claim 1, it is characterised in that described star PEG refers to the PEG of at least more than 3
Side chain and each bar chain dereliction take second place point, the special branched PEG of class that is connected on same centronucleus by chemical bond and spreading out
Biology, in water soluble, and has Series Molecules amount.
Method of testing the most according to claim 1, it is characterised in that the star of described star PEG specifically four arm
PEG, has four PEG arms, and the end group of every PEG arm is hydroxyl, and molecular weight is 10000 g/mol.
4. the method for testing of a ultrafilter membrane rejection, it is characterised in that the step included:
1) compound concentration is the star PEG aqueous solution of 500 mg/L ~ 5000 mg/L, under room temperature, intake pressure be 0.1 MPa ~
Carrying out ultrafiltration retention experiments under the conditions of 0.3 MPa, ultrafiltration runs time 30 min ~ 60 min；
2) material liquid and filtrate are taken through colour reagent, i.e. Dragendoff reagent and acetic acid-sodium acetate buffer solution color development treatment
After 15 min, ultraviolet-visible spectrophotometer is used to measure the absorbance at 510 nm；
3) concentration of star PEG is calculated according to known standard curve, then according to formula calculating rejection R (%):
R = (1-C p /C f ) × 100%
In formula, C p It is the concentration of star PEG in filtrate；C f It is the concentration of star PEG in material solution.
5., according to claim 4 method of testing, it is characterised in that the star PEG of described star PEG specifically four arm, have four
Individual PEG arm, the end group of every PEG arm is hydroxyl, and molecular weight is 10000 g/mol.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106823823A (en) * | 2017-02-27 | 2017-06-13 | 中国人民大学 | A kind of method for determining supermicro filtration membrane pore size and pore size distribution |
| CN107153037A (en) * | 2017-05-17 | 2017-09-12 | 国家海洋局天津海水淡化与综合利用研究所 | A kind of milipore filter rejection detection method based on narrow ditribution chitosan |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106823823A (en) * | 2017-02-27 | 2017-06-13 | 中国人民大学 | A kind of method for determining supermicro filtration membrane pore size and pore size distribution |
| CN106823823B (en) * | 2017-02-27 | 2019-08-09 | 中国人民大学 | A method of measurement supermicro filtration membrane pore size and pore size distribution |
| CN107153037A (en) * | 2017-05-17 | 2017-09-12 | 国家海洋局天津海水淡化与综合利用研究所 | A kind of milipore filter rejection detection method based on narrow ditribution chitosan |
| CN107153037B (en) * | 2017-05-17 | 2019-11-26 | 自然资源部天津海水淡化与综合利用研究所 | A kind of ultrafiltration membrane rejection detection method based on narrow ditribution chitosan |
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