1、Designation: D5627 94 (Reapproved 2009)1Standard 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
2、, 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.1NOTEAdded research report information to Section 13 editorially in November 2010.1. Scope1.1 This test method cover
3、s the measurement of watersoluble extractable residue from particulate ion-exchange res-ins based on 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
4、 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 and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Docu
5、ments2.1 ASTM Standards:2D1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD2187 Test Methods for Physical and Chemical Propertiesof Particulate Ion-Exchange ResinsD2687 Practices for Sampling Particulate Ion-ExchangeMaterialsD2777 Practice for Determination of Precision and Bi
6、as ofApplicable Test Methods of Committee D19 on Water3. Terminology3.1 Definitions:3.1.1 For definitions of terms used in this test method, referto Terminology D1129.4. Summary of Test Method4.1 A sample of particulate ion exchange material is con-tacted with water at an elevated temperature. After
7、 a specifiedcontact time, the concentration 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
8、quantity of water extract-ables is sometimes 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 identifi
9、cation ofcompounds may be needed in specific 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 coars
10、e frit.7.2 Filtration assembly.7.3 Glass fiber filters, without binder, pre-rinsed with wa-ter.37.4 Weighing vesselPlatinum, nickel, or aluminum maybe used 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.8. Reagents8.1 Purity of Reage
11、ntsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended that1This test method is under the jurisdiction of ASTM Committee D19 on Waterand is the direct responsibility of Subcommittee D19.08 on Membranes and IonExchange Materials.Current edition approved May 1
12、, 2009. Published June 2009. Originallyapproved in 1994. Last previous edition approved in 2004 as D5627 94 (2004).DOI: 10.1520/D5627-94R09E01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards vo
13、lume 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 suitable for this purpose.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United S
14、tates.all reagents shall 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
15、 lessening theaccuracy 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 lI.9. Sampling9.1 Collect the sample in accordance with Practices D2687.In-service resins are taken afte
16、r regeneration and rinse.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 Er
17、lenmeyer flasks(with stoppers) 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, m
18、easure the 200mL of water 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
19、to the nearest 0.1mg. (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 filter
20、ed extracts can be tested 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
21、 the bottom of thevessel. 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! 3 200CWater Extractable Residue, % dry bas
22、is 5A 2 B! 3 200SC 3D100Dwhere: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, Method B).(These calculations assume a 100-mL aliquot out of 200 mLextract.)12. Report
23、12.1 Report the percent 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 wi
24、th an average solids 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 analytical bal-ances),
25、 the multiple laboratory variability is expected to mimicthe single-operator precision and is not separately determined.All determinations were made using disposable aluminumweighing dishes. The following results were obtained:x = 0.393 % by weight, wet basis,So= 0.019 % by weight, wet basis,x = 0.8
26、12 % by weight, dry basis, andSo= 0.039 % by weight, dry basiswhere x is the arithmetic mean of the 18 determinations andSois the single-operator precision calculated in accordancewith D2777.13.2 Since known standards are not available, bias cannotbe determined.14. Keywords14.1 extractables; fouling
27、; ion exchange; residue; sloughage4Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, 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
28、., and the United States Pharmacopeiaand National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D19-1159.D5627 94 (2009)12ASTM International takes no positio
29、n respecting the validity of any patent rights asserted in connection with any item 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.
30、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 I
31、nternational Headquarters. Your comments will receive careful consideration at a meeting 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 sho
32、wn 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D5627 94 (2009)13
