ASTM D5627-17 Standard Test Method for Water Extractable Residue from Particulate Ion-Exchange Resins.pdf

1、Designation: D5627 17Standard Test Method forWater Extractable Residue from Particulate Ion-ExchangeResins1This standard is issued under the fixed designation D5627; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last

2、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 This test method covers the measurement of watersoluble extractable residue from particulate ion-exchange res-ins based on

3、elevated temperature extraction and gravimetricdetermination of residue.1.2 The values stated in SI units are to be regarded asstandard. 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

4、. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental 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

5、 on standard-ization established in the Decision on Principles for theDevelopment of International Standards, 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 WaterD1

6、193 Specification for Reagent WaterD2187 Test Methods and Practices for Evaluating Physicaland Chemical Properties of Particulate Ion-ExchangeResinsD2687 Practices for Sampling Particulate Ion-Exchange Ma-terialsD2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Comm

7、ittee D19 on Water3. Terminology3.1 Definitions:3.1.1 For definitions of terms used in this standard, refer toTerminology D1129.4. Summary of Test Method4.1 A sample of particulate ion exchange material is con-tacted with water at an elevated temperature. After a specifiedcontact time, the concentra

8、tion of soluble material in theaqueous phase is measured gravimetrically after filtration.5. Significance and Use5.1 The presence of water extractables in ion-exchangeresins can cause fouling of other materials downstream andcontamination of process water. The quantity of water extract-ables is some

9、times used as a specification to indicate resinquality, and typical values are 0.01 to 0.1 %.5.2 It is recognized that this test method may not remove allpotential sloughage products and does not measure volatilecompounds. More extensive extraction and identification ofcompounds may be needed in spe

10、cific cases.6. Interferences6.1 The hygroscopic nature of some extracted compoundscan make it difficult to obtain a constant weight. Otherextraction times and temperatures may give results that are notcomparable to these.7. Apparatus7.1 Funnel, 60 mL with coarse frit.7.2 Filtration assembly.7.3 Glas

11、s fiber filters, without binder, pre-rinsed with wa-ter.37.4 Weighing vesselPlatinum, nickel, or aluminum may beused so long as there is no attack by the sample and constantweight can be achieved.7.5 Water bath, for use at 60 6 1C.1This test method is under the jurisdiction of ASTM Committee D19 on

12、Waterand is the direct responsibility of Subcommittee D19.08 on Membranes and IonExchange Materials.Current edition approved Nov. 1, 2017. Published November 2017. Originallyapproved in 1994. Last previous edition approved in 2009 as D5627 94 (2009)1.DOI: 10.1520/D5627-17.2For referenced ASTM standa

13、rds, 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.3Gelman Type A/E, Millipore Type AP40, Whatman GF/C, or equivalent, havebeen found suita

14、ble for this purpose.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 principles on standardization established in the Decision on Principles for th

15、eDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.18. Reagents8.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shal

16、l conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.4Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy

17、of the determination.8.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water conformingto Specification D1193, Type I or II.9. Sampling9.1 Collect the sample in accordance with Practices D2687.In-service resins are taken after regeneration and rins

18、e.10. Procedure10.1 Drain the sample, if necessary, with the drainingapparatus described in the draining apparatus section of TestMethods D2187 to remove free water. Do not wash.10.2 Weigh (to the nearest 0.1 g) two 50-g portions of thedrained sample into clean, dry, 250-mL Erlenmeyer flasks(with st

19、oppers) or BOD bottles. Also weigh (to the nearest 5mg) a 5-g portion of the drained sample for percent waterretention capacity according to Test Methods D2187, TestMethod B.10.3 Transfer 200 mL of water by graduate to each of thetwo flasks containing sample. (Alternatively, measure the 200mL of wat

20、er by weight into each flask.) Prepare another flaskand add 200 mL of water to serve as a blank. Stopper the flasksand maintain them at 60 6 1C for 18 6 2 h using a waterbath.10.4 Dry three weighing vessels to constant weight (61 mg)at 104 6 2C, cool in a desiccator and weigh to the nearest 0.1mg. (

21、Platinum is preferred, but nickel or aluminum may beused.)10.5 Filter the entire volume of each extract using either acoarse fritted funnel or filter assembly with glass fiber filter.Withdraw a 100-mL aliquot and transfer to a tared weighingvessel. (The remainder of the filtered extracts can be test

22、ed fortotal organic carbon or other parameters as desired.)10.6 Evaporate the water and then dry the weighing vesselsto constant weight (61 mg) at 104 6 2C (which can be doneovernight). A hot plate can be used to evaporate nearly all thewater so long as a layer of water covers the bottom of thevesse

23、l. Final drying is to be done in an oven. Weigh to thenearest 0.1 mg.11. Calculation11.1 Calculate the water extractable residue, in percent, foreach of the two sample portions as follows:Water Extractable Residue, % wet basis 5A 2 B! 3200CWater Extractable Residue, % dry basis 5A 2 B! 3200SC 3D100D

24、where:A = residue from sample, in g,B = residue from blank, in g,C = drained sample used, in g, andD = percent solids, calculated as 100 % water retentioncapacity (from Test Methods D2187, Test Method B).(These calculations assume a 100-mL aliquot out of 200-mLextract.)12. Report12.1 Report the perc

25、ent water extractable residue as theaverage of the two values obtained, using the wet or dry,reporting basis or both, as required.13. Precision and Bias513.1 Single-operator precision was determined using a com-posite sample of aged but unused strong acid, gel-type cationresin with an average solids

26、 content of 48.6 % by weight. Thesample was analyzed in triplicate by six operators in onelaboratory. The operators who participated represented a widerange of experience levels. Since other sources of variabilityshould be relatively small (such as from the analyticalbalances), the multiple laborato

27、ry variability is expected tomimic the single-operator precision and is not separatelydetermined. All determinations were made using disposablealuminum weighing dishes. The following results were ob-tained:x = 0.393 % by weight, wet basis,So= 0.019 % by weight, wet basis,x = 0.812 % by weight, dry b

28、asis, andSo= 0.039 % by weight, dry basis.where x is the arithmetic mean of the 18 determinations andSois the single-operator precision calculated in accordancewith Practice D2777.13.2 Since known standards are not available, bias cannotbe determined.14. Quality Control14.1 In the analysis of ion ex

29、change resins, it is not possibleto prepare a known standard resin for comparison with actualsamples. Therefore it is impossible to test the accuracy of theresults, and this test method does not include a bias statement.4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical S

30、ociety, Washington, 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. Pharmaceutical Convention, Inc. (USPC), Rockville

31、,MD.5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D19-1159. ContactASTM CustomerService at serviceastm.org.D5627 17214.2 Analysts are expected to run replicate samples todetermine if the results are within the expected precisi

32、on statedin Sections 13.15. Keywords15.1 extractables; fouling; ion exchange; residue; sloughageASTM 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 that determin

33、ation 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 wit

34、hdrawn. 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, which you may attend. If you feel that yo

35、ur 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 (sin

36、gle 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). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 173