1、Designation: D4456 17Standard Test Methods forPhysical and Chemical Properties of Powdered IonExchange Resins1This standard is issued under the fixed designation D4456; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of la
2、st revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () 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 exchangeresins and are
3、 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. The values given in parentheses are mathematicalconversions t
4、o inch-pound units that are provided for informa-tion only and are not considered standard.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 establish appro-priate safety, health and envir
5、onmental practices and deter-mine the applicability of regulatory limitations prior to use.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standar
6、ds, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD2687 Practices for Sampling Particulate Ion-Exchange Ma-terialsD2777 P
7、ractice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterF322 Test Method for Determining the Quality of Calibra-tion Particles for Automatic Particle Counters (Withdrawn1990)3F651 Method for Particle Counter Single-Point Calibrationby the Median Method (Wit
8、hdrawn 1987)3F658 Practice for Calibration of a Liquid-Borne ParticleCounter Using an Optical System Based Upon LightExtinction (Withdrawn 2007)33. Terminology3.1 Definitions:3.1.1 For definitions of terms used in these standards, referto Terminology D1129.3.2 Definitions of Terms Specific to This S
9、tandard:3.2.1 Certain terms that relate specifically to these standardsare described as follows:3.2.2 powdered ion exchange resinan ion exchange resinthat has undergone post-manufacturing size reduction to lessthan 30 m.3.2.3 resin flocthat voluminous aggregate formed whenpowdered anion exchange res
10、in 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 th
11、e 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.1These test methods are under the jurisdiction of ASTM
12、Committee D19 onWater and are the direct responsibility of Subcommittee D19.08 on Membranes andIon Exchange Materials.Current edition approved Aug. 1, 2017. Published August 2017. Originallyapproved in 1985. Last previous edition approved in 2009 as D4456 99 (2009)1.DOI: 10.1520/D4456-17.2For refere
13、nced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onw
14、ww.astm.org.4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions 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 State
15、s Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized prin
16、ciples on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.14.2 Purity of WaterUnless otherwise indicated, referencesto water shall be
17、 understood to mean Type III reagent water,Specification D1193.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 ion exchange resin
18、 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 aremade of mean particle size, percent below a specified smallersize limit, and percent above a specifie
19、d larger size limit.6.2 The analyst should be aware that adequate collaborativedata for precision and bias statements as required by PracticeD2777 are not provided. See Section 15 for details.7. Significance and Use7.1 The particle size distribution of powdered ion exchangeresins and, more important
20、ly, the derived parameters of meanparticle size and percent above and below specified size limitsare useful for determining batch to batch variations and, insome cases, can be related to certain aspects of productperformance.7.2 Although automatic multichannel particle sizeanalyzers, of the type des
21、cribed in Section 9, yield informationon the entire distribution of sizes present in a given sample, ithas been found that, for this application, the numerical value ofthree derived parameters may adequately describe the particlesize characteristics of the samples: the mean particle diameter(in micr
22、ometres), the percent of the sample that falls belowsome size limit, and the percent of the sample that falls abovesome 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 instru
23、ments not requiring an elec-trolyte.9. Apparatus9.1 Instruments for Measuring Particle Size Distribution,from 2 to 300 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 o
24、peration. Instruments from other manufacturersmay be suitable but have not been evaluated.9.1.1 Optical Particle Counters, 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 pa
25、sses through the sensing zone.9.1.2 Electrical Resistance Particle Counters, that set up avoltage difference across 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
26、Light-Scattering Instruments, that view a flowingstream of particles with a laser beam and produce a Fraunhofferdiffraction 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
27、 Auxiliary Equipment, as specified by the manufacturerof the instrument being used.10. Material10.1 Nonionic Wetting 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
28、(with wetting agent) does not exceed 1 %of the total count during analysis of the resin sample.11. Calibration and Standardization11.1 Calibrate the instrument over the size range to bemeasured following either the manufacturers instructions orMethod F651, Practice F658, or Test Method F322.12. Proc
29、edure12.1 Into a clean sample container, add measured quantitiesof clean liquid, clean wetting agent, and a sample of 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
30、 used for thesize range to be measured.12.2 Agitate the resulting suspension to break up aglomer-ates and create a uniform 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 par
31、ticles not exceeding the maximum specifiedfor proper instrument performance.12.4 If the sample is diluted, the diluted 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
32、.12.6 Record the results.13. Calculation13.1 From the information provided, calculate the meanvalue and the percent above 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 be
33、low and above certainspecified values.D4456 17215. Precision and Bias15.1 Because of the improbability of a single laboratoryhaving all three types of particle size analyzers described inthis test method, round-robin testing is not feasible. Also, sincethe three instruments measure different propert
34、ies, completeagreement is not expected. However, for aliquots of a singlesample of powdered ion exchange resin sent to owners of 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 t
35、ypes of instruments are involved. Morefundamentally, however, powdered resin particle size distribu-tion measurements are statistical measurements on irregularlyshaped particles, and an absolute, or true, value is not possible.TEST METHOD BSOLIDS CONTENT16. Scope16.1 This test method covers the dete
36、rmination of thepercent solids in new powdered ion exchange resins. Bothanion resin and cation resin may be tested by this test method.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 hydrox
37、ide form, aresubject to thermal degradation under the conditions of this test.Therefore, volatile degradation products are released 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 sampl
38、es.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. Significance 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
39、 that the actual solidscontent of the resin be determined.19. Sampling19.1 Obtain a representative sample of the powdered ionexchange resin in accordance with Practices D2687, PracticeA, but substitute a 12.5-mm inside diameter tube.20. Procedure20.1 Weigh three approximately 15-g representativesamp
40、les 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 the 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:Sol
41、ids content, % 5 B/A! 3100where:A = wet sample used, g, andB = dry sample obtained, g.22. Report22.1 Reject and repeat any sample 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
42、.23. Precision and Bias523.1 The overall precision of this test method may beexpressed as follows:SA5 1.43SC5 0.391where:SA= overall precision for powdered anion exchange resinsin hydroxide form expressed as weight percent solids,andSC= overall precision for powdered cation exchange resinsin hydroge
43、n or ammonium forms expressed as weightpercent solids.NOTE 1Using this test method with resins in different ionic formsother than 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 laborator
44、ies.Two samples each of hydrogen form, ammonium form, hy-droxide form and hydrogen/hydroxide mixed beds with fibers,were evaluated. The mixed sample results were not included inthe precision calculations. Results of this collaborative studymay not be typical of results for matrices other than thoses
45、tudied.23.3 BiasIon Exchange resins are the product of acomplex, multiple step synthesis involving a polymerizationreaction followed 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
46、and a bias statement cannot be given.24. Quality Control24.1 In the analysis of ion exchange resins, it is not possibleto prepare a known standard resin for comparison with theactual samples. Therefore, it is impossible to test the accuracyof the results, and these test methods do not include a bias
47、statement.24.2 Analysts are expected to replicate samples to deter-mine if the results are within the expected precision stated inSection 23.25. Keywords25.1 floc; ion exchange; particle size; powdered resin; solidscontent5Supporting data have been filed at ASTM International Headquarters and maybe
48、obtained by requesting Research Report RR:D19-1084. ContactASTM CustomerService at serviceastm.org.D4456 173ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised t
49、hat 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 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 committee,
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