1、Designation: D4266 96 (Reapproved 2009)1D4266 17Standard Test Methods forPrecoat Capacity of Powdered Ion-Exchange Resins1This standard is issued under the fixed designation D4266; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, th
2、e year 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.1 NOTEUpdated 5.2 editorially in June 2009.1. Scope1.1 These test methods cover the determination of the operating ion-e
3、xchange capacity of both powdered cation-exchange resins(hydrogen form) and powdered anion-exchange resins (hydroxide form). These test methods are intended for use in testing newpowdered ion-exchange resins when used for the treatment of water. The following two test methods are included:SectionsTe
4、st Method 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 the standard. The inch-pound units given in parentheses are forinformation only.1.3 This standa
5、rd does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.1.4 This international standard
6、was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Reference
7、d Documents2.1 ASTM Standards:2D1125 Test Methods for Electrical Conductivity and Resistivity of WaterD1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD2687 Practices for Sampling Particulate Ion-Exchange MaterialsD4456 Test Methods for Physical and Chemical Properties of Powd
8、ered Ion Exchange ResinsD5391 Test Method for Electrical Conductivity and Resistivity of a Flowing High Purity Water SampleE200 Practice for Preparation, Standardization, and Storage of Standard and Reagent Solutions for Chemical Analysis3. Terminology3.1 Definitions:3.1.1 For definitions of other t
9、erms used in this standard, refer to Terminology D1129.3.2 Definitions of Terms Specific to This Standard:3.1.1 For definitions of other terms used in these test methods, refer to Terminology D1129.3.2.1 powdered ion-exchange material, nan ion-exchange resin that has undergone post-manufacturing siz
10、e reduction to lessthan 300 m.1 These test methods are under the jurisdiction of ASTM Committee D19 on Water and are the direct responsibility of Subcommittee D19.08 on Membranes and IonExchange Materials.Current edition approved May 1, 2009June 1, 2017. Published June 2009 June 2017. Originally app
11、roved in 1983. Last previous edition approved in 20072009 asD4266 96 (2007).(2009)1. DOI: 10.1520/D4266-96R09E01.10.1520/D4266-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume informati
12、on, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict
13、 all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428
14、-2959. United States13.2.2 resin dosage, nthe weight of mixed resin applied per unit area of precoatable filter surface. This is expressed as drypounds per square foot.3.2.3 resin floc, nthat voluminous aggregate formed when powdered anion-exchange resin and powdered cation-exchangeresin are slurrie
15、d together in an aqueous suspension.3.2.4 resin ratio, nthe ratio of the weights of powdered cation-exchange resin to powdered anion-exchange resin used toprepare a resin slurry. If not otherwise indicated, it is understood to be the ratio of the dry resin weights.4. Significance and Use4.1 The salt
16、 removal capacity of a powdered resin precoat is limited by the capacity of either the anion-exchange resin or thecation-exchange resin contained in it.Applications include condensate polishing in fossil-fueled electric generating plants, as wellas condensate polishing, spent fuel pool water treatme
17、nt, reactor water treatment, and low-level radioactive liquid waste treatmentin nuclear-powered electric generating plants.4.2 By determining the ion-exchange capacity profile of either a cation exchange resin or an anion-exchange resin (capacityexpended per unit of time under specific conditions),
18、it is possible to estimate runlength and remaining capacity when treating aliquid of the same makeup. Although they cannot accurately predict performance during condenser leaks, these test methods areuseful for determining operating capacities as measured under the test conditions used.4.3 These tes
19、t methods may be used to monitor the performance of either powdered anion-exchange resin or powderedcation-exchange resin. The total capacity of either resin depends primarily upon the number density of ion-exchange sites withinthe resin. The operating capacity is a function of the total capacity, d
20、egree of conversion to the desired ionic form when received,and properties of the resin and the system that affect 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 shall conformto the speci
21、fications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications areavailable.35.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean Type II reagent water,Specification D1193.6. Sampling6.1 Obtain a representative
22、sample of the powdered ion-exchange resin in accordance with Practices D2687 but substituting a12.5-mm (12-in.) inside diameter tube.TEST METHOD AOPERATING CAPACITY,ANION-EXCHANGE RESIN, HYDROXIDE FORM7. Scope7.1 This test method covers the determination of ion-exchange capacity, on a dry weight bas
23、is, of new powderedanion-exchange resins in the hydroxide form.7.2 The ion-exchange capacity obtainable in commercial installations depends not only upon the initial state of thepowdered resin, but also on how the resin floc is prepared and applied, on the condition of the equipment on which it is t
24、o be used,and the pH and general chemistry of the water system being treated. Thus, this test method has comparative rather than predictivevalue and provides an upper limit on exchange capacity that may be expected.8. Summary of Test Method8.1 The powdered anion-exchange resin to be tested is slurri
25、ed with an appropriate amount of powdered cation-exchange resinin the hydrogen form, and the resulting floc is precoated onto a filter disk. Then a dilute standardized solution of a strong acid isfed to the precoat while monitoring the effluent stream conductometrically.3 Reagent Chemicals, American
26、 Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary,
27、U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.D4266 1729. Apparatus9.1 Test apparatus, as shown in Fig. 1, with the following components:9.1.1 Water Pumpadjustable between 0 to 7.57 L/min (0 to 2 gal/min) at 2.76 105 Pa (40 psig) pressure.49.1.2 Pressure Gauges (two), 0 to 4.137 105 Pa (
28、0 to 60 psig) with appropriate snubbers.4 The sole source of supply of the Millipore pump (ZPN100400) apparatus known to the committee at this time is the Millipore Corporation, 290 Concord Rd., Billerica,MA 01821. If you are aware of alternative suppliers, please provide this information to ASTM In
29、ternational Headquarters. Your comments will receive careful considerationat a meeting of the responsible technical committee,1 which you may attend.(A) Pump, adjustable between 0 to 2 gal/min at 40 psig (0.27 MPa) pressure. Millipore pump (ZPN100400) has been found satisfactory for this use.(B) Gau
30、ges, 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 a 12 in. (12.5 mm) powdered resin precoat.Millipore filter holder (YY2214230) with acrylic cylinder (XX4214201) and accessories has been
31、 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 between 30300 mL/h at 100-psig pressure. Pr
32、ovide 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) Tubing,116 in (1.6 mm), including three-w
33、ay 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 measurement apparatus, including tempera
34、ture measurement.FIG. 1 Equipment Layout for Precoat Capacity DeterminationD4266 1739.1.3 Disk Filter Holder, 142-mm diameter with sufficient clearance above the filter disk to allow for uniform application ofresin precoat.59.1.4 Filter-Disk, 142-mm diameter, with nominal retention rating of 25 to 3
35、0 m and absolute retention rating of 40 to 60m.69.1.5 Flow Meter, 0 to 1.89 L/min (0 to 30 gal/h) with regulating valve.9.1.6 Beaker, stainless steel, 4 L to volume with bulkhead fittings installed at tubing penetrations.9.1.7 Chemical Pump, with pumping rate between 8.33 106 and 8.33 105 L/s (30 to
36、 300 mL/h) at 3.45 10 6 Pa (500 psig)pressure. Suction tubing should be 3.2-mm (18-in.) outside diameter stainless steel and discharge tubing should be 1.6-mm (116-in.)outside diameter stainless steel.79.2 Electrical Conductivity Measurement Apparatus, conforming to the requirements given in Test Me
37、thods D1125, TestMethod B.B, and D5391.10. Reagents10.1 Hydrochloric Acid Solution, Standard (0.10 N)Prepare and standardize as described in Practice E200.10.2 Polyacrylic Acid Solution, Standard (1+99)Pipet 1 mL of polyacrylic acid8 (25 weight % solids, MW 50 000) into a100 mL volumetric flask and
38、dilute to 100 mL with water. Mix well. Prepare this solution fresh daily.11. Sample Preparation11.1 Selection of Proper Sample WeightUse a resin dosage 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 the resin as a consideration in a situat
39、ion involving a performanceproblem in a commercial plant, then the capacity test may be performed using the same wet resin ratio and the same resin dosageas is used in the commercial equipment.11.1.2 Using a resin dosage of 1 kg/m2 (0.2 lb/ft2), the correct dry weight of resin to be used on a 142-mm
40、 diameter filter is15.5 g. At a resin ratio of 2+1, the dry weights to use are 10.3 g of cation and 5.2 g of anion exchange resins. The solids contentsshould be determined by Test Method B of Test Methods D4456.11.1.3 From the known solids content of the resins, and the dry weight of resin desired f
41、or the test, calculate the weight of wetresin to be taken for analysis as follows:5 The sole source of supply of the Millipore filter holder (YY2214230) with acrylic cylinder (XX4214201) and accessories apparatus known to the committee at this timeis the Millipore Corporation, 290 Concord Rd., Bille
42、rica, MA 01821. If you are aware of alternative suppliers, please provide this information to ASTM InternationalHeadquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee,1 which you may attend.6 The sole source of supply of the BG or DG filter
43、 apparatus known to the committee at this time is the Pall Corporation, 30 Sea Cliff Ave., Glen Cove, NY 11542. Ifyou are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meetingof the responsibl
44、e technical committee,1 which you may attend.7 The sole source of supply of the Milton Roy pump (1960066002) apparatus known to the committee at this time is Milton Roy USA, 201 Ivyland Rd., Ivyland, PA18974.If you are aware of alternative suppliers, please provide this information toASTM Internatio
45、nal Headquarters. Your comments will receive careful consideration at a meetingof the responsible technical committee,1 which you may attend.8 The sole source of supply of the Accumer (1510) apparatus known to the committee at this time is the Rohm and Haas Company, 100 Independence Mall West,Philad
46、elphia, PA 19106. If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive carefulconsideration at a meeting of the responsible technical committee,1 which you may attend.D4266 174W 5B/S! 3100where:W = weight of wet res
47、in, g,B = weight of 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-mL beakers and place each beaker on a magnetic stirrer. Adjust thestirring speed to as high as possible without appreciable vortex formation.11.2.2
48、Accurately weigh three portions each of the cation resin and the anion resin, using the wet weights as determined in 11.1.Place the proper amount of cation resin and anion resin in each of the three beakers and stir gently for 5 min.11.2.3 For each beaker, after mixing for five min, turn off the mag
49、netic stirrer and allow the floc to settle for 5 min. The desiredfloc density is obtained if the top surface of the settled floc appears flat and uniform.11.2.4 If the desired settled floc density is not obtained after the initial 5 min settling time, turn the magnetic stirrer on and add1 mL of the polyacrylic acid solution. Mix for 5 min, allow the floc to settle an additional 5 min, and check the settled floc densityagain. Continue with 1 mL incremental additions of the polyacrylic acid solution until the desired floc density is o
