1、Designation: D 4456 99 (Reapproved 2009)1Standard Test Methods forPhysical and Chemical Properties of Powdered IonExchange Resins1This standard is issued under the fixed designation D 4456; the number immediately following the designation indicates the year oforiginal adoption or, in the case of rev
2、ision, the 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.1NOTEUpdated 4.2 editorially in June 2009.1. Scope1.1 These test methods cover the determination of thephysical
3、 and chemical properties of powdered ion exchangeresins and are intended for use in testing new materials. Thefollowing test methods are included:SectionsTest Method AParticle Size Distribution 5 to 15Test Method BSolids Content 16 to 231.2 The values stated in SI units are to be regarded asstandard
4、. No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to consult andestablish appropriate safety and health practices and deter-mine t
5、he applicability of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1129 Terminology Relating to WaterD 1193 Specification for Reagent WaterD 2687 Practices for Sampling Particulate Ion-ExchangeMaterialsD 2777 Practice for Determination of Precision and Bias ofApplic
6、able Test Methods of Committee D19 on WaterF 322 Method of Test for Amount of Nonvolatile Residue(NVR) in Trichlorotrifluouroethane (Meseran Procedure)3F 651 Method for Particle Single-Point Calibration by theMedian Method3F 658 Practice for Calibration of a Liquid-Borne ParticleCounter Using an Opt
7、ical System Based Upon LightExtinction33. Terminology3.1 Definitions: For definitions of terms used in this prac-tice, refer to Terminology D 1129.3.2 Definitions of Terms Specific to This Standard: Certainterms that relate specifically to these test methods are describedas follows:3.2.1 powdered io
8、n exchange resinan ion exchange resinthat has undergone post-manufacturing size reduction to lessthan 30 m.3.2.2 resin flocthat voluminous aggregate formed whenpowdered anion exchange resin and powdered cation exchangeresin are slurried together in an aqueous suspension.4. Purity of Reagents4.1 Reag
9、ent 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,4where suchspecifications are available. Other grades may be used, pro-vided it is fi
10、rst ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.1These test methods are under the jurisdiction of ASTM Committee D19 onWater and are the direct responsibility of Subcommittee D19.08 on Membranes andIon Exchange Mater
11、ials.Current edition approved May 1, 2009. Published June 2009. Originallyapproved in 1985. Last previous edition approved in 2005 as D 4456 99 (2005).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStan
12、dards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.4Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For Sugges
13、tions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.1Copyright ASTM International,
14、100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean Type III reagent water,Specification D 1193.TEST METHOD APARTICLE SIZEDISTRIBUTION5. Scope5.1 This test method covers the
15、instrumental determinationof the particle-size distribution of powdered ion exchangeresins.6. Summary of Test Method6.1 A sample of powdered ion exchange resin is disperseduniformly in a suitable aqueous liquid. The resulting suspen-sion is passed through an instrument for measuring particle sizedis
16、tribution by weight, number, or volume. Determinations aremade of mean particle size, percent below a specified smallersize limit, and percent above a specified larger size limit.6.2 The analyst should be aware that adequate collaborativedata for precision and bias statements as required by Practice
17、D 2777 are not provided. See Section 15 for details.7. Significance and Use7.1 The particle size distribution of powdered ion exchangeresins and, more importantly, the derived parameters of meanparticle size and percent above and below specified size limitsare useful for determining batch to batch v
18、ariations and, insome cases, can be related to certain aspects of productperformance.7.2 Although automatic multichannel particle size analyz-ers, of the type described in Section 9, yield information on theentire distribution of sizes present in a given sample, it hasbeen found that, for this appli
19、cation, the numerical value ofthree derived parameters may adequately describe the particlesize characteristics of the samples: the mean particle diameter(in micrometres), the percent of the sample that falls belowsome size limit, and the percent of the sample that falls abovesome size limit.8. Inte
20、rferences8.1 Instruments requiring the use of an aqueous electrolytefor sample suspension, such as described in 9.1.2, may giveresults different than those instruments not requiring an elec-trolyte.9. Apparatus9.1 Instruments for Measuring Particle Size Distribution,from 2 to 300 m in size, although
21、 it may not be necessary tocover this entire range for any one sample. Satisfactory resultshave been obtained from instruments with three differentprinciples of operation. Instruments from other manufacturersmay be suitable but have not been evaluated.9.1.1 Optical Particle Counters, that pass a col
22、limated lightbeam through a flowing stream of particles to measure andcount each individual particle according to the reduction inlight intensity created as it passes through the sensing zone.9.1.2 Electrical Resistance Particle Counters, that set up avoltage difference across an aperture through wh
23、ich a conduc-tive liquid flows to measure and count each particle in theliquid by the change in conductivity or resistance as it passesthrough the aperture.9.1.3 Light-Scattering Instruments, that view a flowingstream of particles with a laser beam and produce a Fraunhofferdiffraction pattern from w
24、hich a thirteen-segment histogram ofvolume size distribution is obtained.9.2 Sample Handling System, compatible with the particle-sizing instrument being used.9.3 Auxiliary Equipment, as specified by the manufacturerof the instrument being used.10. Material10.1 Nonionic Wetting Agent, to assist in t
25、he dispersion ofthe particles in the liquid. The volume to be added will besmall, but its cleanliness should be such that the total count inthe suspending liquid (with wetting agent) does not exceed 1 %of the total count during analysis of the resin sample.11. Calibration and Standardization11.1 Cal
26、ibrate the instrument over the size range to bemeasured following either the manufacturers instructions orMethod F 651, Practice F 658, or Method F 322.12. Procedure12.1 Into a clean sample container, add measured quantitiesof clean liquid, clean wetting agent, and a sample of powderedion exchange r
27、esin. The size of the sample container and thequantities of each material to be added will be determined fromthe operating instructions for the instrument being used for thesize range to be measured.12.2 Agitate the resulting suspension to break up aglomer-ates and create a uniform dispersion of par
28、ticles using theequipment specified in the operating instructions for theinstrument.12.3 If necessary, dilute this suspension to provide a con-centration of particles not exceeding the maximum specifiedfor proper instrument performance.12.4 If the sample is diluted, the diluted sample must beagitate
29、d in accordance with the instrument operating instruc-tions to create a uniform dispersion of particles.12.5 Pass the sample through the instrument for analysis.12.6 Record the results.13. Calculation13.1 From the information provided, calculate the meanvalue and the percent above and below the spec
30、ified sizes onthe basis of weight, number, or volume.14. Report14.1 Report the mean particle size in micrometres, and thepercent of the sample tested that is below and above certainspecified values.15. Precision and Bias15.1 Because of the improbability of a single laboratoryhaving all three types o
31、f particle size analyzers described inthis test method, round-robin testing is not feasible. Also, sincethe three instruments measure different properties, completeD 4456 99 (2009)12agreement is not expected. However, for aliquots of a singlesample of powdered ion exchange resin sent to owners of ea
32、chtype of instrument, the mean particle size values did not differby more than 20 %.15.2 A statement of bias may not be obtainable for this testmethod, since different types of instruments are involved. Morefundamentally, however, powdered resin particle size distribu-tion measurements are statistic
33、al measurements on irregularlyshaped particles, and an absolute, or true, value is not possible.TEST METHOD BSOLIDS CONTENT16. Scope16.1 This test method covers the determination of thepercent solids in new powdered ion exchange resins. Bothanion resin and cation resin may be tested by this test met
34、hod.Resins are tested in the ionic form in which they are received.16.2 It is important to note that ion exchange resins,particularly anion exchange resins in the hydroxide form, aresubject to thermal degradation under the conditions of this test.Therefore, volatile degradation products are released
35、 alongwith moisture, resulting in a negative error. However, the valueof this test method is that it is simple and reproducible, and itis applicable to as-received samples.17. Summary of Test Method17.1 This test method consists of determining the loss ofmass on drying at 104 6 2C for 18 h.18. Signi
36、ficance and Use18.1 Powdered ion exchange resins are manufactured andshipped in a moist form. However, they are sold and used on adry weight basis. Thus, it is important that the actual solidscontent of the resin be determined.19. Sampling19.1 Obtain a representative sample of the powdered ionexchan
37、ge resin in accordance with Practices D 2687, PracticeA, but substitute a 12.5-mm inside diameter tube.20. Procedure20.1 Weigh three approximately 15-g representativesamples of material to the nearest 1 mg into previously taredweighing vessels.20.2 Heat the samples for 18 h at 104 6 2C.20.3 Remove t
38、he samples from the oven, cool at least 30min in a desiccator to room temperature and reweigh.21. Calculation21.1 Calculate the solids content, in percent, as follows:Solids content, % 5 B/A! 3 100where:A = wet sample used, g, andB = dry sample obtained, g.22. Report22.1 Reject and repeat any sample
39、 analysis in which theresult differs by more than 2 % from either of the other twosamples.22.2 Report the percent solids content as the average of thethree values obtained.23. Precision and Bias523.1 The overall precision of this test method may beexpressed as follows:SA5 1.43SC5 0.391where:SA= over
40、all precision for powdered anion exchange resinsin hydroxide form expressed as weight percent solids,andSC= overall precision for powdered cation exchange resinsin hydrogen or ammonium forms expressed as weightpercent solids.NOTE 1Using this test method with resins in different ionic formsother than
41、 those indicated will, in general, increase the precision.23.2 For the collaborative study, completed in 1982, eightpowdered IEX resin samples were sent to eight laboratories.Two samples each of hydrogen form, ammonium form, hy-droxide form and hydrogen/hydroxide mixed beds with fibers,were evaluate
42、d. The mixed sample results were not included inthe precision calculations. Results of this collaborative studymay not be typical of results for matrices other than thosestudied.23.3 BiasIon Exchange resins are the product of a com-plex, multiple step synthesis involving a polymerization reac-tion f
43、ollowed by one or more additional reactions to putfunctional groups on the polymeric structure. Consequently,the true value for any property of the finished product isunknown and a bias statement cannot be given.24. Keywords24.1 floc; ion exchange; particle size; powdered resin; solidscontent5Suppor
44、ting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D191084.D 4456 99 (2009)13ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this
45、standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years
46、 andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committe
47、e, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D 4456 99 (2009)14
