1、Designation: D 4456 99 (Reapproved 2005)Standard 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 revi
2、sion, the year 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 thephysical and chemical properties of powdered ion e
3、xchangeresins 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 This standard does not purport to address all of thesafety concerns, if any, associated with its use.
4、 It is theresponsibility of the user of this standard to consult andestablish appropriate safety and health practices and deter-mine the applicability of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1129 Terminology Relating to WaterD 1193 Specification for Reagen
5、t WaterD 2687 Practices for Sampling Particulate Ion-ExchangeMaterialsD 2777 Practice for Determination of Precision and Bias ofApplicable Methods of Committee D19 on WaterF 322 Method for Determining Quality of Calibration Par-ticles for Automatic Particle Counters3F 651 Method for Particle Single-
6、Point Calibration by theMedian Method3F 658 Practice for Calibration of a Liquid-Borne ParticleCounter Using an Optical system Based on Light Extinc-tion3. Terminology3.1 DefinitionsFor definitions of terms used in this prac-tice, refer to Terminology D 1129.3.2 Definitions of Terms Specific to This
7、 Standard: Certainterms that relate specifically to these test methods are describedas follows:3.2.1 powdered ion 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 resi
8、n and powdered cation exchangeresin are slurried together in an aqueous suspension.4. Purity of Reagents4.1 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
9、 American Chemical Society,4where suchspecifications are available. Other grades may be used, pro-vided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.4.2 Purity of WaterUnless otherwise indicated, reference
10、sto water shall be understood to mean Type III reagent water,Specification D 1193.TEST METHOD APARTICLE SIZEDISTRIBUTION5. Scope5.1 This test method covers the instrumental determinationof the particle-size distribution of powdered ion exchangeresins.6. Summary of Test Method6.1 A sample of powdered
11、 ion exchange resin is disperseduniformly in a suitable aqueous liquid. The resulting suspen-sion is passed through an instrument for measuring particle sizedistribution by weight, number, or volume. Determinations are1These test methods are under the jurisdiction of ASTM Committee D19 onWater and a
12、re the direct responsibility of Subcommittee D19.08 on Membranes andIon Exchange Materials.Current edition approved June 1, 2005. Published June 2005. Originallyapproved in 1985. Last previous edition approved in 1999 as D 4456 99.2For referenced ASTM standards, visit the ASTM website, www.astm.org,
13、 orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn.4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions
14、 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, 100 B
15、arr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.made 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
16、 required by PracticeD 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 determi
17、ning batch to batch variations 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
18、 that, for this application, 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 aboveso
19、me size limit.8. Interferences8.1 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,5from 2 to 3
20、00 m in size, although 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 Cou
21、nters, that pass a collimated 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
22、an aperture through which 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 Fraunhofferdiff
23、raction pattern from which 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
24、 Agent, to assist in the 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 S
25、tandardization11.1 Calibrate 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
26、powderedion exchange resin. 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 uni
27、form dispersion of particles 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
28、 sample must beagitated 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 ab
29、ove and below the specified 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 laboratoryha
30、ving all three types of particle size analyzers described inthis test method, round-robin testing is not feasible. Also, sincethe three instruments measure different properties, completeagreement is not expected. However, for aliquots of a singlesample of powdered ion exchange resin sent to owners o
31、f eachtype 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 stati
32、stical measurements on irregularlyshaped particles, and an absolute, or true, value is not possible.5Instruments from the following manufacturers have been found to be suitable.Instruments from other manufacturers may be suitable, but have not been evaluated:HIAC/ROYCO Division, Pacific Scientific,
33、141 Jefferson Dr., Menlo Park, CA94025: Coulter Electronics, Industrial Div., 590 West 20 St., Hialeah, FL 33010: andLeeds ion exchange; particle size; powdered resin; solidscontentASTM International takes no position respecting the validity of any patent rights asserted in connection with any item
34、mentionedin this standard. Users of this 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 commit
35、tee and must be reviewed every five years 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 mee
36、ting of theresponsible technical committee, 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,
37、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).6Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D191084.D 4456 99 (2005)3