1、Designation: D 4266 96 (Reapproved 2001)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 Form7-15Test Method BOperating Capacity, Cation-ExchangeResin, Hydrogen Form16-241.2 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 concerns,
5、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:D 1125 Test Methods for Electrical Conductivit
6、y and Re-sistivity of Water2D 1129 Terminology Relating to Water2D 1193 Specification for Reagent Water2D 2687 Practices for Sampling Particulate Ion-ExchangeMaterials3D 4456 Test Methods for Physical and Chemical Propertiesof Powdered Ion-Exchange Resins3E 200 Practice for Preparation, Standardizat
7、ion, and Storageof Standard and Reagent Solutions for Chemical Analysis43. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 powdered ion-exchange material, nan ion-exchange resin that has undergone post-manufacturing sizereduction to less than 300 m.3.1.2 resin dosage, nthe weight
8、 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 ratio
9、, 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 Terminol
10、ogy 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 conden
11、sate 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 sites1These test methods are under the
14、 jurisdiction of ASTM Committee D19 onWater and are the direct responsibility of Subcommittee D19.08 on Membranes andIon-Exchange Materials.Current edition approved July 10, 1996. Published November 1996. Originallypublished as D 4266 83. Last previous edition D 4266 83 (1990)e1.2Annual Book of ASTM
15、 Standards, Vol 11.01.3Annual Book of ASTM Standards, Vol 11.02.4Annual Book of ASTM Standards, Vol 15.05.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.within the resin. The operating capacity is a function of thetotal capacity, de
16、gree of conversion to the desired ionic formwhen received, and properties of the resin and the system thataffect ion exchange kinetics.5. Purity of Reagents5.1 Reagent grade chemicals shall be used in all tests.Unless otherwise indicated, it is intended that all reagents shallconform to the specific
17、ations of the Committee on AnalyticalReagents of the American Chemical Society, where suchspecifications are available.55.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean Type II reagent water,Specification D 1193.6. Sampling6.1 Obtain a representative samp
18、le 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,ANIONEXCHANGE RESIN, HYDROXIDE FORM7. Scope7.1 This test method covers the determination of ion-exchange capacity, on a dry weight basis,
19、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 thepowdered resin, but also on how the resin floc is prepared andapplied, on the condition of the equipment on which it is to beus
20、ed, 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 exchangecapacity that may be expected.8. Summary of Test Method8.1 The powdered anion-exchange resin to be tested isslurried with a
21、n 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 strong acid is fed to the precoat while monitoring theeffluent stream conductometrically.9. Apparatus9.1 Test apparatus, as show
22、n 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.69.1.2 Pressure Gages (2), 0 to 4.137 3 105Pa (0 to 60psig) with appropriate snubbers.9.1.3 Disk Filter Holder, 142-mm diameter with sufficientclearance abo
23、ve the filter disk to allow for uniform applicationof resin precoat.79.1.4 Filter-Disk, 142-mm diameter, with nominal retentionrating of 25 to 30 m and absolute retention rating of 40 to60m.89.1.5 Flow Metre, 0 to 1.89 L/min (0 to 30 gal/h) withregulating valve.9.1.6 Beaker, stainless steel, 4 L to
24、volume with bulkheadfittings installed at tubing penetrations.9.1.7 Chemical Pump, with pumping rate between8.33 3 10 6and 8.33 3 10 5L/s (30 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
25、 (116-in.) outside diameter stainlesssteel.99.2 Electrical Conductivity Measurement Apparatus, con-forming to the requirements given in Test 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 A
26、cid Solution, Standard (1 + 99)Pipet 1mL of polyacrylic acid10(25 weight % solids, MW 50 000)into a 100 mL volumetric flask and dilute to 100 mL 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/ft
27、2) 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 plant, then the capacity test may beperformed using the same wet resin ratio and the same resindosage as is used in the com
28、mercial 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 dry weights to use are10.3 g of cation and 5.2 g of anion exchange resins. The solidscontents should be determined by Meth
29、od B of Test MethodsD 4456.11.1.3 From the known solids content of the resins, 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 1005Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, W
30、ashington, 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 National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.6Milli
31、pore pump ZPN100400, or equivalent, has been found satisfactory for thisuse.7Millipore filter holder YY22 14230 with acrylic cylinder XX42 14201 andaccessories, or an equivalent, has been found satisfactory for this use.8BG or DG filters, available from Pall Corporation, 30 Sea Cove, NY, 11542, oreq
32、uivalent, have been found satisfactory for this use.9Milton Roy pump 1960066002, or an equivalent, has been found satisfactoryfor this use.10Accumer 1510 obtainable from Rohm and Haas Co., Philadelphia, Pa., or anequivalent, is suitable.D 4266 96 (2001)2where:W = weight of wet resin, g,B = weight of
33、 dry resin, g, andS = solids content of resin, %.11.2 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 as high as possible without appreciable vortexformation.11.2.2 Accurately weigh three
34、 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 For each beaker, after mixing for 5 min, turn off themagnetic stirrer and allow the
35、floc to settle for 5 min. Thedesired floc density is obtained if the top surface of the settledfloc appears flat and uniform.(A) Pump, adjustable between 0 to 2 gal/min at 40 psig (0.27 MPa) pressure. Millipore pump ZPN1 004 00 or equivalent has been found satisfactory for thisuse.(B) Gages, 0 to 60
36、 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 a 1/2 in. (12.5 mm) powdered resin precoat.Millipore filter holder YY22 142 30 with XX42 142 01 acrylic cylinder and accessories has been found sati
37、sfactory 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 between 30300 mL/h at 100-psig pressure. Provide exter
38、nal pressure relief protection set for 100 psig.Milton Roy pump model 1960066002 has been found satisfactory for this use.(H) Tubing, 3/8 in. (9.5 mm), precoat circuit(I) Tubing, 1/4 in. (6.4 mm) Including regulating valve(J) Tubing, 1/8 in. (3.2 mm)(K) Tubing, 1/16 in (1.6 mm) Including three-way b
39、all valve and flushing line.(L) Graduated Cylinder, 250 mL.Disk Filters, 142 mm either polypropylene or celluloseNominal rating 2530 mAbsolute rating 4060 mThe Pall Corp has disk filters that have been found satisfactory for this use.(M) Electrical conductivity cell and measurement apparatus, includ
40、ing temperature measurement.FIG. 1 Equipment Layout for Precoat Capacity DeterminationD 4266 96 (2001)311.2.4 If the desired settled floc density is not obtained afterthe initial 5 min settling time, turn the magnetic stirrer on andadd 1 mLof the polyacrylic acid solution. Mix for 5 min, allowthe fl
41、oc 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. Use the minimum required amount of polyacrylicacid solution.The function of the polyacrylic acid is to partial
42、lydeclump 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 precoatingdifficulties and too porous a precoat will result. Conversely, anexcess of polyacrylic acid solution will declump the
43、 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 filterholder and arrange the apparatus as shown in Fig. 1.812.2 Add water to the beaker (E) as required to m
44、aintain 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 a
45、dditions 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 mark in a graduated cylinder (L).12.6 Adjust the chemical pump (G) to12-full stroke, openthe three-way valve to the vent position and operate the pumpto v
46、ent the pump and tubing. Shut off the pump when ventedand adjust the volume of 0.10 N HCl to exactly 250 mL in thegraduated cylinder, if required. Adjust the three-way valve tofeed into the filter circulation pump suction.12.7 Maintain the filter circulation flow rate at 1.406 0.05L/min (22 6 0.5 ga
47、l/h) and maintain the filter inlet pressure at2.07 Pa (30 psig) by adjusting the water pump output and theflowmeter regulating valve (D).12.8 Turn on the magnetic stirrer (F) under the stainlesssteel beaker and adjust the speed so that minimal vortexformation occurs.12.9 Transfer the contents of one
48、 of the resin slurry beakersinto the stainless steel beaker and allow the resin to precoatonto the disk filter. Continue circulation until the water abovethe filter appears clear.12.10 Open and adjust the inlet valve. Start the chemicalpump and adjust the pump rate to maintain a 25C conductivityof 5
49、0 6 2 S/cm at the inlet sample point.12.11 Monitor and record the filter inlet and outlet conduc-tivities (M), the stream temperature, and volume of 0.10 N HClconsumed as a function of time. When the filter outletconductivity rises to 0.2 S/cm (25C), or other desiredconductivity endpoint, record the volume of 0.10 N HClconsumed, and shut down the chemical pump.12.12 Turn off the water pump and vent, drain, and clean thefilter holder and tubing.12.13 Repeat 12.1 through 12.12 on each of the remainingtwo resin slurry samples.13. Calculation and Inter
