ASTM D4266-1996(2007) Standard Test Methods for Precoat Capacity of Powdered Ion-Exchange Resins.pdf

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1、Designation: D 4266 96 (Reapproved 2007)Standard 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 (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 These test methods cover the determination of theoperating ion-exchange capacity of both powdered cation-exchange

3、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 AOperating Capacity, Anion-ExchangeResin,

4、 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 not purport to address all of thesafety conc

5、erns, 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 Standards:2D 1125 Test Methods for Electrical Cond

6、uctivity 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 ResinsE 200 Practice for Preparation, Standardiz

7、ation, and Stor-age of Standard and Reagent Solutions for ChemicalAnalysis3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 powdered ion-exchange material, nan ion-exchangeresin that has undergone post-manufacturing size reduction toless than 300 m.3.1.2 resin dosage, nthe weigh

8、t 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 formed whenpowdered anion-exchange resin and powdered cation-exchange resin are slurried together in an aqueous suspension.3.1.4 resin rati

9、o, nthe ratio of the weights of powderedcation-exchange resin to powdered anion-exchange resin usedto prepare a resin slurry. If not otherwise indicated, it isunderstood to be the ratio of the dry resin weights.3.2 DefinitionsFor definitions of other terms used in thesetest methods, refer to Termino

10、logy D 1129.4. 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 electric generating plants,as well as conde

11、nsate 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 anion-exchange resin(capacity expended

12、 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 determining operating capaci-ties as measured

13、 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 siteswithin the resin. The operating

14、capacity is a function of thetotal capacity, degree of conversion to the desired ionic formwhen received, and properties of the resin and the system thataffect ion exchange kinetics.1These test methods are under the jurisdiction of ASTM Committee D19 onWater and are the direct responsibility of Subc

15、ommittee D19.08 on Membranes andIon Exchange Materials.Current edition approved Dec. 1, 2007. Published January 2008. Originallyapproved in 1983. Last previous edition approved in 2001 as D 4266 96 (2001).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer S

16、ervice at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Purity of Reagents5.1 Reagent grade ch

17、emicals 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 WaterUnless otherwise indicated, reference

18、sto 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 AOPERATING CAPACITY,ANION-EXCHANGE

19、 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 only upon the initial state of thepo

20、wdered 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 provides an upper limit on exchan

21、gecapacity 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 dilute standardized solutionof a str

22、ong 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) pressure.49.1.2 Pressure Gages (two), 0

23、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 25 to 30 m and absolute retention ra

24、ting of 40 to60m.69.1.5 Flow Metre, 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 (30 to 300 mL/h) at3.45 3 106Pa (500

25、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 Methods D 1125,Method B.10. Reagen

26、ts10.1 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 mL withwater. Mix well. Prepare this

27、 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 performanceproblem in a commercial p

28、lant, 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 diameterfilter is 15.5 g. At a resin ratio of 2+1, the

29、 dry weights to use3Reagent Chemicals, 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 Unite

30、d States Pharmacopeiaand National 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 alter

31、native suppliers, please provide 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 (XX

32、4214201) and accessories apparatus 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 a

33、meeting of the responsible technical 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 informati

34、on toASTM International Headquarters. 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

35、 Rd., Ivyland,PA 18974. If you 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

36、(1510) apparatus known to thecommittee 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 meet

37、ing of the responsible technical committee,1which you may attend.D 4266 96 (2007)2are 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, and thedry weight of resin desired

38、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, %.(A) Pump, adjustable between 0 to 2 gal/min at 40 psig (0.27 MPa) pressure. Millipore pump (ZPN100400) has b

39、een found satisfactory for this use.(B) Gages, 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 resin precoat.Millipore filter holder (YY2214230) with acrylic cyli

40、nder (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) Magnetic stirrer and hotplate.(G) Instrument Pump, with pumping rate be

41、tween 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. (6.4 mm), including regulating valve.(J) Tubing,18 in. (3.2 mm).(K)

42、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 found satisfactory for this use.(M) Electrical conductivity cell and

43、 measurement apparatus, including temperature measurement.FIG. 1 Equipment Layout for Precoat Capacity DeterminationD 4266 96 (2007)311.2 Resin Slurry Preparation:11.2.1 Measure 300 mL of water into each of three 500-mLbeakers and place each beaker on a magnetic stirrer.Adjust thestirring speed to a

44、s 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 beakers and stir gently for 5 min.11.2.3

45、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 obtained afterthe initial 5 min settli

46、ng 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 the desired floc density isobtained. U

47、se 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 too voluminous and precoatingdifficul

48、ties 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 142-mm diameter disk filter (C) into the

49、 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 N HCl to approximately 5 mL above the250-mL