CN108181479A - Retaining molecular weight automatic analyzer - Google Patents

Retaining molecular weight automatic analyzer Download PDF

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Publication number
CN108181479A
CN108181479A CN201711452276.3A CN201711452276A CN108181479A CN 108181479 A CN108181479 A CN 108181479A CN 201711452276 A CN201711452276 A CN 201711452276A CN 108181479 A CN108181479 A CN 108181479A
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molecular weight
liquid
unit
bottle
filtrate
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CN108181479B (en
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黄彦
卜亚亮
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GAOQ FUNCTIONAL MATERIALS Co Ltd
Nanjing Tech University
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GAOQ FUNCTIONAL MATERIALS Co Ltd
Nanjing Tech University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor

Abstract

A kind of retaining molecular weight automatic analyzer, include feed liquid unit (1), film separation unit (2), filtrate sampling unit (3), five parts such as concentration analysis unit (4) and control, data acquisition and computing unit (5).Wherein, feed liquid unit (1) can choose primary standard substance solution as feed liquid automatically;Film separation unit (2) realizes the cross-flow filtration of feed liquid and obtains filtrate;Filtrate sampling unit (3) can choose filtrate sample automatically;Concentration analysis unit (4) can measure filter liquor concentration;Control, data acquisition control the automatic operating of each unit with computing unit (5) and realize the calculating of result.

Description

Retaining molecular weight automatic analyzer
Technical field
This patent is related to the detecting instrument of ultrafiltration and nanofiltration retaining molecular weight and relevant operation technique, for it is quick, Accurately detect membrane filtration and the molecular cut off of separation material.
Technical background
Ultrafiltration membrane generally refers to multi-hole filtering film of the aperture in 10-100nm, organic main polyvinylidene fluoride of ultrafiltration membrane material The high molecular materials such as alkene, polysulfones, polyacrylonitrile, poly-vinegar acid cellulose, Inorganic Ultrafiltration Membrane are mainly then aluminium oxide, titanium oxide, oxygen Change the ceramic materials such as zirconium, silica, composite oxides.The aperture of NF membrane is generally 0.1-10nm.Ultrafiltration and NF membrane are in water It is widely used, such as sea water desalination, drink water purifying, wastewater treatment in processing industry, is also largely used to chemical industry, medicine, food Separation process in product.With ultrafiltration and the rapid growth of the extensive use of NF membrane and related industry, countries in the world are all very Pay attention to the exploitation of the new production process and new material of film, high-performance, inexpensive ultrafiltration and the exploitation of NF membrane have become with production The hot spot of industry competition.Either the exploitation of film new material or the control of the film quality of production all be unable to do without the inspection of membrane separating property It surveys.At present, the evaluation index of ultrafiltration and nanofiltration membrane performance mainly have pure water flux, molecular cut off (MWCO, Molecular weight cut-off, also known as molecular weight cut off), pore-size distribution, backwash performance, filling area, Zeta electricity Position etc..Wherein, molecular cut off is the important indicator that most can directly reflect ultrafiltration and NF membrane rejection effect, and section of ultrafiltration membrane Stay performance that can also usually be detected by pore-size distribution.
The test method of ultrafiltration membrane pore-size distribution is mainly liquid-liquid displacement method, other hole measuring methods such as Vesicular protein (also known as hair Thin flow method, bubble platen press, gas-liquid system), BET method, mercury injection method, electron microscope method is all inapplicable or has very big limitation.Liquid liquid is put It is similar to the basic principle of Vesicular protein to change method, is all first fully to soak ultrafiltration membrane with wetting agent, then with compressed gas or separately It is a kind of that wetting agent is ejected and gets through fenestra road with wetting agent immiscible liquid.Wherein, the aperture the big, the trepanning needed Pressure is smaller, that is, aperture is inversely proportional with hole-forming pressure, and hole can be calculated according to the interfacial tension of hole-forming pressure and wetting agent Diameter.Since the interfacial tension between two kinds of liquid is much smaller than gas-liquid interface tension, Vesicular protein is generally not suitable for measuring 100nm Following aperture, that is, Vesicular protein is generally unsuitable for ultrafiltration membrane.Although for from calculation formula, as long as test pressure is carried High 10 times of apertures that can measure below 10nm, but it is in practical operation and infeasible, and reason is:Hi-pot test is not only Lead to that sealing is difficult, vapour lock is high, gas consumption is big, measurement error is big, and sample strength is proposed very high in duct It is required that such as test pressure needed for measuring 10nm apertures at least need 5MPa, such high pressure is enough to cause sample deformations even Damage;Most of ultrafiltration membrane is all flexible polymer material on the market, and when Hi-pot test is easy to due to sample compressive deformation Test result is caused to be distorted.For liquid-liquid displacement method, due to the poor reproducibility of manual operation, it is necessary to be carried out certainly by special instrument Dynamicization operates, and Nanjing Gao Qian functional materials company develops First full-automatic ultrafiltration membrane Porosimetry.Although liquid liquid is put The method of changing can measure smaller aperture, but be still extremely restricted when measuring nanofiltration membrane aperture.
Molecular cut off method can detect the cutoff performance of various films (including NF membrane), test result and Vesicular protein and It can also be carried out mutually estimating [Calvo J I, Peinador R I, Pr á danos according to practical experience between liquid-liquid displacement method P, et al.Liquid-liquid displacement porometry to estimate the molecular weight Cut-off of ultrafiltration membranes.Desalination, 2011,268268 (13):174-181.]. The common detection methods of molecular cut off are:First measure a series of rejection (i.e. envelope of the film to known molecular amount primary standard substances The solute of retention accounts for the percentage of the solute total amount in solution), rejection-molecular weight relation curve is then drawn, works as rejection The molecular weight of corresponding primary standard substance is the molecular cut off of the film when being 90%.The accuracy of molecular cut off test result It is heavily dependent on the accuracy of the selection of primary standard substance, the selection of detection method and rejection value.
Primary standard substance for molecular cut off detection should have following condition:Purity is high, and molecular structure is clear and definite;Molecular weight Narrowly distributing, molecular weight wide coverage;Physicochemical properties are stable, are not easy coating material absorption;Molecular shape is preferably spherical in shape (linear molecule rejection will be well below the global molecular of same molecular weight);It is cheap and easy to get etc..At present, domestic and international molecular cut off Primary standard substance as defined in examination criteria is mainly polyethylene glycol, protein and glucan [HY/T 050-1999, Hollow Fiber Ultrafiltration Film test method;ASTM E1343-90 (2001), Standard test method for molecular weight cut off evaluation of flat sheet ultrafiltration membranes;GB/T 32360-2015, ultrafiltration membrane Test method].According to professional standard HY/T050-1999, for measuring the primary standard substance of Retention Ratio of The Ultrafiltration Membrane as polyethylene glycol (molecular weight 6000,10000,20000Da), cromoci (molecular weight 13000Da), ovalbumin (molecular weight 45000Da), Bovine serum albumin (molecular weight 67000Da).The testable molecular cut off range of these primary standard substances is only limitted to 6000-67000Da, And without poor [Wu Jinke, Wang Bin Retention Ratio of The Ultrafiltration Membrane the measure side of comparativity between the molecular cut off measured in different primary standard substances Method Tianjin chemical industry, 2000 (2):24-26;Dong Shenghua, Zheng lead the comparison water of English various criterions object characterization Retention Ratio of The Ultrafiltration Membrane Treatment technology, 1993 (6):319-323;Yan Zhongsen, Qu Fangshu, the identical of beam carry out ultrafiltration membrane using glucan and protein and cut Cut molecular weight test comparative study membrane science and technologies, 2015,35 (3):44-50;Liu Ting favour ultrafiltration is developing mainly to ask Inscribe water technologies, 1988,14 (4):193-197.], application receives very big limitation.In addition, protein is also easy to be surpassed Filter membrane absorption, testing cost are high.In contrast, glucan is that more preferably primary standard substance, range of molecular weight distributions are wide (10000-2500000Da), film adsorb less, chemical property is stablized, and have won favor [Pan Xianhui, the Wang Xiao of most of researcher The such as nanmu, Zhang Yanping Retention Ratio of The Ultrafiltration Membrane detection primary standard substance advances and application membrane science and technologies, 2013,33 (2):103-108;Tian Yan, Dong Shenghua, one polished hollow fiber ultrafiltration membranes rejection of woods are measured at the discussion water of normalization method Reason technology, 1994,20 (4):192-196.].
There are two types of in a manner of analyte detection molecular cut off on the basis of glucan.When exclusion chromatography, i.e., with different points The mixed solution of son amount glucan carries out single ultrafiltration, and mixed liquor Zhong Ge molecular weight Portugal gathers before and after measuring ultrafiltration by gel chromatography [such as Dong Shenghua, Tian Yan, Yang Lanna exclusion chromatographies are measured at Characterization of Ultrafiltration Membranes Cut-off Molecular-weight water for the concentration variation of sugar Reason technology, 1990,16 (4):323-327;Bottino A, Capannelli G, Imperato A, et al.Ultrafiltration of hydrosoluble polymers:Effect of operating conditions on The performance of the membrane.Journal of Membrane Science, 1984,21 (3):247- 267;Dong Shenghua, Zheng's neck English exclusion chromatographies characterize rejection-Molecular weight plots water of several representative ultrafiltration membranes in China Treatment technology, 1991,17 (4):268-271.].Exclusion chromatography is although convenient, but analytical instrument is expensive, is difficult to promote.It is another Kind method is more easy to be acceptable to the market, i.e., carries out Ultrafiltration experiment successively with the solution of different molecular weight glucan, measure ultrafiltration respectively The concentration of front and rear each dextran solution changes and calculates and to obtain rejection.The measure object of the method be unimolecule amount glucan, measure side Method is simple, including nephelometry, spectrophotometry and COD methods etc..[such as Dai Haiping, Zhang Huixin, beam Fu Hai are gathered Dai Haiping etc. with Portugal The simple and easy method membrane science and technologies of sugar determination ultrafiltration membrane molecular weight cut off, 2005,25 (4):63-65.] propose nephelometry It is by the principle of " water extract-alcohol precipitation ", adding in ethyl alcohol precipitates polysaccharide, so as to cause the increase of turbidity.Work as dextran solution When being mixed in equal volume with ethyl alcohol and keeping 30min at room temperature, solution turbidity and glucan concentration are in a linear relationship.Spectrophotometric Method (i.e. sulfuric acid-phynol method) is classical polysaccharide quantitative detecting method, and the furfural that glucan hydrolyzed-be dehydrated generation through the concentrated sulfuric acid spreads out With phenol chromogenic reaction occurs for biology, and when wavelength is 490nm, the absorbance and glucan concentration of solution are in a linear relationship.It should Method is easy to operate, result is accurate, measurement is quick and without precision instrument, thus as whole world method the most general.COD methods Glucan concentration is measured by measuring the COD value of dextran solution and being compared with standard curve, it is anti-compared with spectrophotometry Answer condition more harsh.
Membrane material and membrane technology become increasingly popular the research and development and production for greatly exciting membrane material, also excite film detection The exploitation of technology and pertinent instruments, especially efficiently, reliably, automation retaining molecular weight test technology and equipment development gesture It must go.Opening meeting equality, [hollow fiber ultrafiltration membrane rejection detection devices of Zhang Huiping, Jiang Yinping, Li Cong the coral based on PLC is set Count and apply [J] instrumental techniques and sensor, 2016 (1):37-40.] it devises a set of doughnut controlled based on PLC and surpasses Membrane filtration device, but the device only realizes membrane filtration operation, is not directed to the automatic sampling of filtrate and the automation of concentration Detection can not still solve the problems, such as that rejection analyzes faced time and effort consuming, there is no full-automatic molecular cut off detection work so far The report of skill and relevant device.
Invention content
The purpose of this patent is to develop retaining molecular weight automatic analyzer and relevant operation technique to analyze various films The molecular cut off of material, realization include feed liquid selection, UF membrane, filtrate sampling, concentration analysis, data acquisition and retention molecule The entire analytic processes such as amount calculating, for given various membrane materials, can automatically, quickly realize the test of molecular cut off Work.
The technical solution of this patent:Retaining molecular weight automatic analyzer includes 5 parts, respectively:Feed liquid unit, film point From unit, filtrate sampling unit, concentration analysis unit and control, data acquisition and computing unit.
Retaining molecular weight automatic analyzer described in this patent, construction are as shown in Figure 1.Wherein, feed liquid unit (1) is main To include sampler (101), pure water bottle (102), feed liquid bottle (103), feed pipe (104) and discharge nozzle (105).Film separation unit (2) mainly include constant flow pump (201), pressure sensor (204) after pressure sensor (202), membrane separator (203), film before film, Electric control valve (205) and flowmeter (206).Filtrate sampling unit (3) mainly includes sampler (301), electrical turntable (302), specimen cup (303), sampling pipe (304), pure water bottle (305) and waste liquid bottle (306).Concentration analysis unit (4) mainly wraps Include pure water bottle (401), syringe pump (402), multi direction changeover valve (403), electric switching valve (404), darkroom (405), reaction tank (406), photometric analysis light source (407), light intensity inductor (408), nephelometric analysis light source (409), turbidity light intensity inductor (410), chemical reagent bottle (411), waste liquid bottle (412) and liquid storage coil pipe (413).Control, data acquisition and computing unit (5) are main To include computer (501) and communication accessory (502).Wherein, communication accessory mainly includes data collecting card, driver, controller Wait components.
Material pipeline connection between different units is as shown in Figure 1.Membrane separator (203) feeding line is equipped with constant flow pump (201) and before film pressure sensor (202), phegma pipeline are equipped with pressure sensor (204), electric control valve after film (205) and flowmeter (206).The feed pipe (104) of feeding line end and the discharge nozzle (105) of phegma outlet line end All be fixed on the sliding block of sampler (101), the sliding block can up and down, move left and right, so as to from each feed liquid bottle (103) liquid is taken to test in.The filtrate of membrane separator (203) is discharged into the specimen cup (303) on electrical turntable (302), electric rotating Platform (302) goes to the specimen cup (303) equipped with filtrate to be analyzed below sampling pipe (304), and sampling pipe (304), which is fixed on, to be taken On the sliding block of sample device (301), which can move up and down.Therefore, sampling pipe (304) can be stretched into sample by sampler (301) In cup (303), pass through syringe pump (402) and multi direction changeover valve (403) suction sampling.
Syringe pump (402) pumping hole pipeline connects a threeway, and one end stretches into pure water bottle through electric switching valve (404) (401) in, the other end is connected to the central passage of multi direction changeover valve (403) through liquid storage coil pipe (413).Multi direction changeover valve (403) Central passage can two-by-two be communicated with any one branched bottom, but between branched bottom can not intercommunication, and branched bottom number is many In 5.A logical air is stayed in the channel of multi direction changeover valve (403), remaining difference coupled reaction pond (406), chemical reagent bottle (411), waste liquid bottle (412) and sampling pipe (304).Photometric analysis light source (407) and nephelometric analysis light source are equipped in darkroom (405) (409), after light passes through reaction liquid, transmitted light is with scattering the intensity of light respectively by light intensity inductor (408) and turbidity light intensity sense Device (410) is answered to detect, the light intensity signal of acquisition is then converted by concentration value by the standard curve built in computer (501), and Rejection of the film to the feed liquid is calculated according to the original concentration of each feed liquid and filter liquor concentration, by drawing rejection and standard mistake The relation curve of filter medium molecular weight, you can calculate the molecular cut off of filter membrane.Above-mentioned electronic device and electric element pass through Communication accessory (502) is connect with computer (501).
Liquid line described in this patent used in retaining molecular weight automatic analyzer should select plastic material as possible, The region that the middle concentrated sulfuric acid is reached must then select corrosion-resistant material such as polytetrafluoroethylene (PTFE).So when reaction is related to the concentrated sulfuric acid, All channel attached pipelines of multi direction changeover valve (403) are polytetrafluoroethylene (PTFE) material.The pipeline internal diameter of liquid storage coil pipe (413) is 0.5-4mm, but to reduce influence caused by solution is spread in in-pipe, the preferred 1-2mm of pipeline internal diameter.Liquid storage coil pipe (413) volume is determined by pipeline internal diameter and total length, but not less than syringe pump (402) volume.Due to meeting in liquid storage coil pipe (413) It is flowed through there are many liquid, to improve the cleaning performance of liquid storage coil pipe (413), inner surface of tube wall should be smooth, is preferably provided with certain Hydrophobicity.Liquid to reduce instrument liquid pipeline system remains and improves cleaning performance, and inner wall of the pipe absolute roughness is less than 10μm。
Major function of the retaining molecular weight automatic analyzer described in this patent per unit.Feed liquid unit (1):For UF membrane Unit chooses feed liquid automatically;Film separation unit (2):It realizes the cross-flow filtration of feed liquid and obtains filtrate;Filtrate sampling unit (3): It is automatic to choose filtrate sample;Concentration analysis unit (4):Measure filter liquor concentration;Control, data acquisition and computing unit (5):According to The program of setting and the signal of acquisition, control the automatic operating of each unit, and realize the calculating of result.
The remarkable advantage of this patent is embodied in:
1. feed liquid switching, UF membrane, filtrate sampling, sample introduction, pipeline cleaning, chemical reaction, signal acquisition, result operation etc. The automation of operating process not only saves manpower and avoids human error, but also improve testing efficiency.
2. by the ingenious cooperation of syringe pump, liquid storage coil pipe and multi direction changeover valve, reaction accurately can be quantitatively controlled Liquid inlet volume improves the reproducibility and accuracy of test result.When extracting chemical reagent and filtrate, the pump housing only using pure water as Current-carrying liquid, pump body is not contaminated and corrosion, and pure water and chemical reagent or filtrate can be also isolated in the air column in liquid storage coil pipe Contact, avoids cross contamination.
3. instrument described in this patent integrates spectrophotometry and nephelometry concentration analysis, test applicability is improved.
4. automation equipment degree described in this patent is high, easy to operate.The system of each operating procedure can be achieved in blocking design Operation is raised, saves run time.
Description of the drawings
Fig. 1 is the structure diagram of instrument described in this patent.Wherein:101- samplers;102- pure water bottles;103- feed liquids Bottle;104- feed pipes;105- discharge nozzles;201- constant flow pumps;Pressure sensor before 202- films;203- membrane separators;After 204- films Pressure sensor;205- electric control valves;206- flowmeters;301- samplers;302- electrical turntables;303- specimen cups;304- Sampling pipe;305- pure water bottles;306- waste liquid bottles;401- pure water bottles;402- syringe pumps;403- multi direction changeover valves;404- driven openings Close valve;405- darkrooms;406- reaction tanks;407- photometric analysis light sources;408- light intensity inductors;409- nephelometric analysis light sources; 410- turbidity light intensity inductors;411- chemical reagent bottles;412- waste liquid bottles;413- liquid storage coil pipes;501- computers;502- communications are attached Part.
Specific embodiment
The feed liquid bottle (103) of feed liquid unit (1) is placed in using the dextran standards solution of different molecular weight as feed liquid, it will Pure water injection pure water bottle (102), (401) and (305), concentration is respectively placed in by the concentrated sulfuric acid, 5% phenol solution and absolute ethyl alcohol In the chemical reagent bottle (411) of analytic unit (4).If not using turbidity rule absolute ethyl alcohol that can omit, without using light splitting Then the concentrated sulfuric acid can be omitted with phenol solution during photometry.Water in pure water bottle (102) is not less than 500ml.Feed liquid is with cross-flow The mode of filter is driven into membrane separator (203), flow and transmembrane pressure and is controlled by constant flow pump (201) and electric control valve (205), Phegma returns to original feed liquid bottle (103), and filtrate is collected by specimen cup (303).It waits after collecting, constant flow pump (201) will Feed liquid in pipeline is all aspirated in feed back liquid bottle (103).Therefore, constant flow pump (201) need to have bidirectional transfusion function.Such as Fig. 1 Shown, less than discharge nozzle (105), when work, makes feed pipe (104) stretch under liquid level, and discharges for the end of feed pipe (104) Pipe (105) is then maintained on liquid level, can avoid sampler (101) frequently lifting behaviour when exporting and recycling feed liquid in this way Make, and the short circuit phenomenon that can occur due to end is close to avoid feed pipe (104) and discharge nozzle (105).Filter operation is complete Cheng Hou can test different feed liquids by sampler (101), (301) and electrical turntable (302) and acquire its filtrate.It is anti- The only pollution between different feed liquid in the following way cleans system when switching feed liquid:Using constant flow pump (201) from It draws water in pure water bottle (102) and water is run as feed liquid, the ejected wash water flowed out from filtrate side then enters waste liquid bottle (306), Initial water in pure water bottle (102) is not less than 500ml.To improve cleaning performance, pure water bottle (102) may also set up 2-3, with Realize multipass cleaning.Alternatively, pure water bottle (102) is equal with the number of feed liquid bottle (103), all automatically selected during cleaning every time new Pure water bottle.
Electric switching valve (404) is opened, adjusting multi direction changeover valve (403) closes central passage, starts syringe pump (402) It draws water from pure water bottle (401);Electric switching valve (404) is closed, adjusting multi direction changeover valve (403) makes central passage and waste liquid bottle (412) it is connected, by the water injection liquid storage coil pipe (413) in syringe pump (402), extra water is discharged into waste liquid bottle (412);Control electricity Specimen cup (303) equipped with filtrate to be analyzed is threaded under sampler (301) by turn platform (302), and sampler (301) is by sampling pipe (304) it stretches into filtrate;Adjusting multi direction changeover valve (403) makes central passage be connected with air, is aspirated with syringe pump (402) a small amount of Air makes to generate one section of air column in liquid storage coil pipe (413);Adjusting multi direction changeover valve (403) makes syringe pump (402) and sampling pipe (304) it is connected and filtrate is extracted into liquid storage coil pipe (413), adjusting multi direction changeover valve (403) makes central passage and reaction tank (406) it is connected, filtrate is squeezed into reaction tank (406) by syringe pump (402), similarly, will be corresponding with detection method with syringe pump (402) Chemical reagent also squeeze into reaction tank (406), pass through spectrophotometry or nephelometry after reaction and analyze filter liquor concentration, i.e., survey in advance Determine the standard curve between concentration and absorbance and turbidity, be then converted into the absorbance of acquisition with turbid ity signal by computer Concentration value.The wavelength of photometric analysis light source (407) is 480-500nm, and the wavelength of nephelometric analysis light source (409) is 870-890nm. The rejection of film can be calculated, then draw rejection and standard filter media according to the original concentration of each feed liquid and filter liquor concentration The relation curve of molecular weight, you can calculate the molecular cut off of filter membrane.

Claims (14)

1. a kind of retaining molecular weight automatic analyzer includes feed liquid unit (1), film separation unit (2), filtrate sampling unit (3), five parts such as concentration analysis unit (4) and control, data acquisition and computing unit (5);Feed liquid unit (1) selects automatically Taking primary standard substance solution, film separation unit (2) realizes the cross-flow filtration of feed liquid and obtains filtrate, filtrate sampling unit as feed liquid (3) filtrate sample is chosen automatically, and concentration analysis unit (4) measures filter liquor concentration, and control, data acquisition are controlled with computing unit (5) The automatic operating of each unit processed and the calculating for realizing result;Feed liquid unit (1) mainly includes sampler (101), pure water bottle (102), feed liquid bottle (103), feed pipe (104) and discharge nozzle (105);Film separation unit (2) mainly include constant flow pump (201), Pressure sensor (204), electric control valve (205) and flowmeter after pressure sensor (202), membrane separator (203), film before film (206);Filtrate sampling unit (3) mainly includes sampler (301), electrical turntable (302), specimen cup (303), sampling pipe (304), pure water bottle (305) and waste liquid bottle (306);Concentration analysis unit (4) mainly includes pure water bottle (401), syringe pump (402), multi direction changeover valve (403), electric switching valve (404), darkroom (405), reaction tank (406), photometric analysis light source (407), light intensity inductor (408), nephelometric analysis light source (409), turbidity light intensity inductor (410), chemical reagent bottle (411), Waste liquid bottle (412) and liquid storage coil pipe (413);Control, data acquisition mainly include computer (501) and communication with computing unit (5) Attachment (502).
2. retaining molecular weight automatic analyzer according to claim 1, it is characterised in that:It is selected by sampler (101) The feed liquid taken is driven into membrane separator (203) in a manner of cross-flow filtration, is controlled with constant flow pump (201) and electric control valve (205) Flow and transmembrane pressure processed, phegma return to original feed liquid bottle (103), and filtrate is collected by specimen cup (303), then constant flow pump (201) feed liquid in pipeline is all aspirated into feed back liquid bottle (103).
3. retaining molecular weight automatic analyzer according to claim 2, it is characterised in that:To prevent between different feed liquid Pollution, every time before feed liquid is chosen, drawn water from pure water bottle (102) using constant flow pump (201) and water transported as feed liquid Row, the ejected wash water flowed out from filtrate side then enter waste liquid bottle (306), and the initial water in pure water bottle (102) is not less than 500ml; To improve cleaning performance, pure water bottle (102) may also set up 2-3, to realize that multipass cleans;Alternatively, pure water bottle (102) and feed liquid The number of bottle (103) is equal, all automatically selects new pure water bottle during cleaning every time.
4. retaining molecular weight automatic analyzer according to claim 2, it is characterised in that:Constant flow pump (201) has double To infusion function.
5. retaining molecular weight automatic analyzer according to claim 2, it is characterised in that:Sampler (101) chooses material When liquid or pure water, feed pipe (104) mouth need to be stretched under liquid level, and discharge nozzle (105) mouth need to be on liquid level.
6. retaining molecular weight automatic analyzer according to claim 1, it is characterised in that:When carrying out concentration analysis, Electric switching valve (404) is first opened, adjusting multi direction changeover valve (403) closes central passage, starts syringe pump (402) from pure water It draws water in bottle (401);Electric switching valve (404) is closed, adjusting multi direction changeover valve (403) makes central passage and waste liquid bottle (412) Conducting, by the water injection liquid storage coil pipe (413) in syringe pump (402), extra water is discharged into waste liquid bottle (412);Control electric rotating Specimen cup (303) equipped with filtrate to be analyzed is threaded under sampler (301) by platform (302), and sampler (301) is by sampling pipe (304) it stretches into filtrate;Adjusting multi direction changeover valve (403) makes central passage be connected with air, is aspirated with syringe pump (402) a small amount of Air makes to generate one section of air column in liquid storage coil pipe (413);Adjusting multi direction changeover valve (403) makes syringe pump (402) and sampling pipe (304) it is connected and filtrate is extracted into liquid storage coil pipe (413), adjusting multi direction changeover valve (403) makes central passage and reaction tank (406) it is connected, filtrate is squeezed into reaction tank (406), chemical reagent is also squeezed into reaction with syringe pump (402) by syringe pump (402) Filter liquor concentration is analyzed in pond (406) after reaction by spectrophotometry or nephelometry.
7. the retaining molecular weight automatic analyzer according to claim 2 or 6, it is characterised in that:Fluid pipeline is mainly Plastic material, and the absolute roughness of inner wall is less than 10 μm.
8. retaining molecular weight automatic analyzer according to claim 6, it is characterised in that:It is set simultaneously in darkroom (405) After having photometric analysis light source (407) and nephelometric analysis light source (409), light to pass through reaction liquid, transmitted light and scattering light are by light intensity Inductor (408) is detected with turbidity light intensity inductor (410).
9. retaining molecular weight automatic analyzer according to claim 6, it is characterised in that:The pipe of liquid storage coil pipe (413) Line internal diameter is 0.5-4mm, preferably 1-2mm.
10. the retaining molecular weight automatic analyzer according to item claim 6, it is characterised in that:Multi direction changeover valve (403) Central passage can two-by-two be communicated with any one branched bottom, but between branched bottom can not intercommunication, and branched bottom number is not Less than 5.
11. the retaining molecular weight automatic analyzer according to claim 2 or 6, it is characterised in that:Feed liquid is molten for glucan Liquid.
12. retaining molecular weight automatic analyzer according to claim 11, it is characterised in that:Photometric analysis light source (407) wavelength is 480-500nm, and the wavelength of nephelometric analysis light source (409) is 870-890nm.
13. retaining molecular weight automatic analyzer according to claim 12, it is characterised in that:Divide when detection method uses During light photometry, corresponding chemical reagent is respectively the concentrated sulfuric acid and 5% phenol solution.When detection method uses nephelometry, Corresponding chemical reagent is absolute ethyl alcohol.
14. retaining molecular weight automatic analyzer according to claim 13, it is characterised in that:Multi direction changeover valve (403) All channel attached pipelines are polytetrafluoroethylene (PTFE) material.
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