1、Designation: D 4266 96 (Reapproved 2009)1Standard Test Methods forPrecoat Capacity of Powdered Ion-Exchange Resins1This standard is issued under the fixed designation D 4266; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year
2、 of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTEUpdated 5.2 editorially in June 2009.1. Scope1.1 These test methods cover the determination of theoperating ion-exchange
3、capacity of both powdered cation-exchange resins (hydrogen form) and powdered anion-exchange resins (hydroxide form). These test methods areintended for use in testing new powdered ion-exchange resinswhen used for the treatment of water. The following two testmethods are included:SectionsTest Method
4、 AOperating Capacity, Anion-ExchangeResin, Hydroxide Form7 to 15Test Method BOperating Capacity, Cation-ExchangeResin, Hydrogen Form16 to 241.2 The values stated in SI units are to be regarded as thestandard. The inch-pound units given in parentheses are forinformation only.1.3 This standard does no
5、t purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standard
6、s:2D 1125 Test Methods for Electrical Conductivity and Re-sistivity of WaterD 1129 Terminology Relating to WaterD 1193 Specification for Reagent WaterD 2687 Practices for Sampling Particulate Ion-ExchangeMaterialsD 4456 Test Methods for Physical and Chemical Propertiesof Powdered Ion Exchange Resins
7、E 200 Practice for Preparation, Standardization, and Stor-age of Standard and Reagent Solutions for ChemicalAnalysis3. Terminology3.1 Definitions of Terms Specific to This Standard:DefinitionsFor definitions of other terms used in these testmethods, refer to Terminology D 1129.3.1.1 powdered ion-exc
8、hange material, nan ion-exchangeresin that has undergone post-manufacturing size reduction toless than 300 m.3.1.2 resin dosage, nthe weight of mixed resin applied perunit area of precoatable filter surface. This is expressed as drypounds per square foot.3.1.3 resin floc, nthat voluminous aggregate
9、formed whenpowdered anion-exchange resin and powdered cation-exchange resin are slurried together in an aqueous suspension.3.1.4 resin ratio, nthe ratio of the weights of powderedcation-exchange resin to powdered anion-exchange resin usedto prepare a resin slurry. If not otherwise indicated, it isun
10、derstood to be the ratio of the dry resin weights.4. Significance and Use4.1 The salt removal capacity of a powdered resin precoat islimited by the capacity of either the anion-exchange resin orthe cation-exchange resin contained in it. Applications includecondensate polishing in fossil-fueled elect
11、ric generating plants,as well as condensate polishing, spent fuel pool water treat-ment, reactor water treatment, and low-level radioactive liquidwaste treatment in nuclear-powered electric generating plants.4.2 By determining the ion-exchange capacity profile ofeither a cation exchange resin or an
12、anion-exchange resin(capacity expended per unit of time under specific conditions),it is possible to estimate runlength and remaining capacitywhen treating a liquid of the same makeup. Although theycannot accurately predict performance during condenser leaks,these test methods are useful for determi
13、ning operating capaci-ties as measured under the test conditions used.4.3 These test methods may be used to monitor the perfor-mance of either powdered anion-exchange resin or powderedcation-exchange resin. The total capacity of either resin de-pends primarily upon the number density of ion-exchange
14、 siteswithin the resin. The operating capacity is a function of the1These test methods are under the jurisdiction of ASTM Committee D19 onWater and are the direct responsibility of Subcommittee D19.08 on Membranes andIon Exchange Materials.Current edition approved May 1, 2009. Published June 2009. O
15、riginallyapproved in 1983. Last previous edition approved in 2007 as D 4266 96 (2007).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary
16、 page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.total capacity, degree of conversion to the desired ionic formwhen received, and properties of the resin and the system thataffect ion exchange kinetics.5. Puri
17、ty of Reagents5.1 Reagent grade chemicals shall be used in all tests.Unless otherwise indicated, it is intended that all reagents shallconform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society, where suchspecifications are available.35.2 Purity of WaterUnl
18、ess otherwise indicated, referencesto water shall be understood to mean Type II reagent water,Specification D 1193.6. Sampling6.1 Obtain a representative sample of the powdered ion-exchange resin in accordance with Practices D 2687 butsubstituting a 12.5-mm (12-in.) inside diameter tube.TEST METHOD
19、AOPERATING CAPACITY,ANION-EXCHANGE RESIN, HYDROXIDE FORM7. Scope7.1 This test method covers the determination of ion-exchange capacity, on a dry weight basis, of new powderedanion-exchange resins in the hydroxide form.7.2 The ion-exchange capacity obtainable in commercialinstallations depends not on
20、ly upon the initial state of thepowdered resin, but also on how the resin floc is prepared andapplied, on the condition of the equipment on which it is to beused, and the pH and general chemistry of the water systembeing treated. Thus, this test method has comparative ratherthan predictive value and
21、 provides an upper limit on exchangecapacity that may be expected.8. Summary of Test Method8.1 The powdered anion-exchange resin to be tested isslurried with an appropriate amount of powdered cation-exchange resin in the hydrogen form, and the resulting floc isprecoated onto a filter disk. Then a di
22、lute standardized solutionof a strong acid is fed to the precoat while monitoring theeffluent stream conductometrically.9. Apparatus9.1 Test apparatus, as shown in Fig. 1, with the followingcomponents:9.1.1 Water Pumpadjustable between 0 to 7.57 L/min (0to 2 gal/min) at 2.76 3 105Pa (40 psig) pressu
23、re.49.1.2 Pressure Gauges (two), 0 to 4.137 3 105Pa (0 to 60psig) with appropriate snubbers.9.1.3 Disk Filter Holder, 142-mm diameter with sufficientclearance above the filter disk to allow for uniform applicationof resin precoat.59.1.4 Filter-Disk, 142-mm diameter, with nominal retentionrating of 2
24、5 to 30 m and absolute retention rating of 40 to60m.69.1.5 Flow Meter, 0 to 1.89 L/min (0 to 30 gal/h) withregulating valve.9.1.6 Beaker, stainless steel, 4 L to volume with bulkheadfittings installed at tubing penetrations.9.1.7 Chemical Pump, with pumping rate between8.33 3 106and 8.33 3 105L/s (3
25、0 to 300 mL/h) at3.45 3 106Pa (500 psig) pressure. Suction tubing should be3.2-mm (18-in.) outside diameter stainless steel and dischargetubing should be 1.6-mm (116-in.) outside diameter stainlesssteel.79.2 Electrical Conductivity Measurement Apparatus, con-forming to the requirements given in Test
26、 Methods D 1125,Method B.10. Reagents10.1 Hydrochloric Acid Solution, Standard (0.10 N)Prepare and standardize as described in Practice E 200.10.2 Polyacrylic Acid Solution, Standard (1+99)Pipet 1mL of polyacrylic acid8(25 weight % solids, MW 50 000)into a 100 mL volumetric flask and dilute to 100 m
27、L withwater. Mix well. Prepare this solution fresh daily.11. Sample Preparation11.1 Selection of Proper Sample WeightUse a resin dos-age of 1 kg/m2(0.2 lb/ft2) and a resin ratio of 2+1.11.1.1 If the purpose of the capacity test is to eliminate theresin as a consideration in a situation involving a p
28、erformanceproblem in a commercial plant, then the capacity test may beperformed using the same wet resin ratio and the same resindosage as is used in the commercial equipment.11.1.2 Using a resin dosage of 1 kg/m2(0.2 lb/ft2), thecorrect dry weight of resin to be used on a 142-mm diameter3Reagent Ch
29、emicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand Natio
30、nal Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.4The sole source of supply of the Millipore pump (ZPN100400) apparatusknown to the committee at this time is the Millipore Corporation, 290 Concord Rd.,Billerica, MA 01821. If you are aware of alternative suppliers, please provi
31、de thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou may attend.5The sole source of supply of the Millipore filter holder (YY2214230) withacrylic cylinder (XX4214201) and accessories appar
32、atus known to the committee atthis time is the Millipore Corporation, 290 Concord Rd., Billerica, MA 01821. Ifyou are aware of alternative suppliers, please provide this information to ASTMInternational Headquarters. Your comments will receive careful consideration at ameeting of the responsible tec
33、hnical committee,1which you may attend.6The sole source of supply of the BG or DG filter apparatus known to thecommittee at this time is the Pall Corporation, 30 Sea Cliff Ave., Glen Cove, NY11542. If you are aware of alternative suppliers, please provide this information toASTM International Headqu
34、arters. Your comments will receive careful consider-ation at a meeting of the responsible technical committee,1which you may attend.7The sole source of supply of the Milton Roy pump (1960066002) apparatusknown to the committee at this time is Milton Roy USA, 201 Ivyland Rd., Ivyland,PA 18974. If you
35、 are aware of alternative suppliers, please provide this informationto ASTM International Headquarters. Your comments will receive careful consid-eration at a meeting of the responsible technical committee,1which you may attend.8The sole source of supply of the Accumer (1510) apparatus known to thec
36、ommittee at this time is the Rohm and Haas Company, 100 Independence MallWest, Philadelphia, PA 19106. If you are aware of alternative suppliers, pleaseprovide this information to ASTM International Headquarters. Your comments willreceive careful consideration at a meeting of the responsible technic
37、al committee,1which you may attend.D 4266 96 (2009)12filter is 15.5 g. At a resin ratio of 2+1, the dry weights to useare 10.3 g of cation and 5.2 g of anion exchange resins. Thesolids contents should be determined by Method B of TestMethods D 4456.11.1.3 From the known solids content of the resins,
38、 and thedry weight of resin desired for the test, calculate the weight ofwet resin to be taken for analysis as follows:W 5 B/S! 3 100where:W = weight of wet resin, g,B = weight of dry resin, g, andS = solids content of resin, %.11.2 Resin Slurry Preparation:(A) Pump, adjustable between 0 to 2 gal/mi
39、n at 40 psig (0.27 MPa) pressure. Millipore pump (ZPN100400) has been found satisfactory for this use.(B) Gauges, 0 to 60 psig (0.41 Pa) pressure with appropriate snubbers.(C) Disk filter holder, 142-mm diameter with sufficient clearance above the filter disk to allow for a12 in. (12.5 mm) powdered
40、resin precoat.Millipore filter holder (YY2214230) with acrylic cylinder (XX4214201) and accessories has been found satisfactory for this use.(D) Flow metre, 0 to 30 gal/h with regulating valve.(E) Stainless steel beaker, 4-L volume with bulkhead fittings installed at the tubing penetrations.(F) Magn
41、etic stirrer and hotplate.(G) Instrument Pump, with pumping rate between 30300 mL/h at 100-psig pressure. Provide external pressure relief protection set for 100 psig.Milton Roy pump (1960066002) has been found satisfactory for this use.(H) Tubing,38 in. (9.5 mm), precoat circuit.(I) Tubing,14 in. (
42、6.4 mm), including regulating valve.(J) Tubing,18 in. (3.2 mm).(K) Tubing,116 in (1.6 mm), including three-way ball valve and flushing line.(L) Graduated Cylinder, 250 mL.Disk Filters, 142 mm, either polypropylene or cellulose.Nominal rating 2530 m.Absolute rating 4060 m.BG or DG filters have been f
43、ound satisfactory for this use.(M) Electrical conductivity cell and measurement apparatus, including temperature measurement.FIG. 1 Equipment Layout for Precoat Capacity DeterminationD 4266 96 (2009)1311.2.1 Measure 300 mL of water into each of three 500-mLbeakers and place each beaker on a magnetic
44、 stirrer.Adjust thestirring speed to as high as possible without appreciable vortexformation.11.2.2 Accurately weigh three portions each of the cationresin and the anion resin, using the wet weights as determinedin 11.1. Place the proper amount of cation resin and anion resinin each of the three bea
45、kers and stir gently for 5 min.11.2.3 For each beaker, after mixing for five min, turn offthe magnetic stirrer and allow the floc to settle for 5 min. Thedesired floc density is obtained if the top surface of the settledfloc appears flat and uniform.11.2.4 If the desired settled floc density is not
46、obtained afterthe initial 5 min settling time, turn the magnetic stirrer on andadd 1 mLof the polyacrylic acid solution. Mix for 5 min, allowthe floc to settle an additional 5 min, and check the settled flocdensity again. Continue with 1 mLincremental additions of thepolyacrylic acid solution until
47、the desired floc density isobtained. Use the minimum required amount of polyacrylicacid solution.The function of the polyacrylic acid is to partiallydeclump the floc to ensure optimum precoatability of theslurry. The addition of an insufficient amount of polyacrylicacid will result in a floc that is
48、 too voluminous and precoatingdifficulties and too porous a precoat will result. Conversely, anexcess of polyacrylic acid solution will declump the flocexcessively, and may result in the release of resin fines,observed as turbidity, that tend to foul the precoat filter.12. Procedure12.1 Install a 14
49、2-mm diameter disk filter (C) into the filterholder and arrange the apparatus as shown in Fig. 1.612.2 Add water to the beaker (E) as required to maintain a34-full level.12.3 Open the filter inlet sample valve, the flowmeterregulating valve, and the filter holder vent valve.12.4 Start the water pump (A) and fill and vent the filter diskholder and tubing from the beaker. Close the filter vent valveand the filter inlet valve when full. Further additions of waterto the beaker may be required during the filling and ventingprocedures.12.5 Add 0.10
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