1、Designation: D5627 94 (Reapproved 2009)1D5627 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
2、revision, 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.1 NOTEAdded research report information to Section 13 editorially in November 2010.1. Scope1.1 This test met
3、hod covers the measurement of water soluble extractable residue from particulate ion-exchange resins basedon elevated temperature extraction and gravimetric determination of residue.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this s
4、tandard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of regulatory limit
5、ations prior to use.1.4 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Tech
6、nical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD2187 Test Methods and Practices for Evaluating Physical and Chemical Properties of Particulate Ion-Exchange ResinsD2687 Practices for Sampling P
7、articulate Ion-Exchange MaterialsD2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water3. Terminology3.1 DefinitionsDefinitions: For definitions of terms used in this test method, refer to Terminology D1129.3.1.1 For definitions of terms used in t
8、his standard, refer to Terminology D1129.4. Summary of Test Method4.1 A sample of particulate ion exchange material is contacted with water at an elevated temperature. After a specified contacttime, the concentration of soluble material in the aqueous phase is measured gravimetrically after filtrati
9、on.5. Significance and Use5.1 The presence of water extractables in ion-exchange resins can cause fouling of other materials downstream andcontamination of process water. The quantity of water extractables is sometimes used as a specification to indicate resin quality,and typical values are 0.01 to
10、0.1 %.5.2 It is recognized that this test method may not remove all potential sloughage products and does not measure volatilecompounds. More extensive extraction and identification of compounds may be needed in specific cases.1 This test method is under the jurisdiction of ASTM Committee D19 on Wat
11、er and is the direct responsibility of Subcommittee D19.08 on Membranes and Ion ExchangeMaterials.Current edition approved May 1, 2009Nov. 1, 2017. Published June 2009November 2017. Originally approved in 1994. Last previous edition approved in 20042009 asD5627 94 (2009)1 (2004). . DOI: 10.1520/D562
12、7-94R09E01.10.1520/D5627-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM stan
13、dard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all case
14、s only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16. Interferences6.1 The hygroscopic nature of some extracted compounds can make i
15、t difficult to obtain a constant weight. Other extractiontimes and temperatures may give results that are not comparable to these.7. Apparatus7.1 Funnel, 60 mL with coarse frit.7.2 Filtration assembly.7.3 Glass fiber filters, without binder, pre-rinsed with water.37.4 Weighing vesselPlatinum, nickel
16、, or aluminum may be used so long as there is no attack by the sample and constant weightcan be achieved.7.5 Water bath, for use at 60 6 1C.8. Reagents8.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall conform t
17、o the specifications of the Committee on Analytical Reagents of the American Chemical Society, wheresuch specifications are available.4 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently highpurity to permit its use without lessening the accuracy of the de
18、termination.8.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water conforming toSpecification D1193, Type I or lI.II.9. Sampling9.1 Collect the sample in accordance with Practices D2687. In-service resins are taken after regeneration and rinse.10
19、. Procedure10.1 Drain the sample, if necessary, with the draining apparatus described in the draining apparatus section of Test MethodsD2187 to remove free water. Do not wash.10.2 Weigh (to the nearest 0.1 g) two 50-g portions of the drained sample into clean, dry, 250-mL Erlenmeyer flasks (withstop
20、pers) or BOD bottles.Also weigh (to the nearest 5 mg) a 5-g portion of the drained sample for percent water retention capacityaccording to Test Methods D2187, Test Method B.10.3 Transfer 200 mL of water by graduate to each of the two flasks containing sample. (Alternatively, measure the 200 mLof wat
21、er by weight into each flask.) Prepare another flask and add 200 mL of water to serve as a blank. Stopper the flasks andmaintain them at 60 6 1C for 18 6 2 h using a water bath.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
22、. (Platinum is preferred, but nickel or aluminum may be used.)10.5 Filter the entire volume of each extract using either a coarse fritted funnel or filter assembly with glass fiber filter.Withdrawa 100-mL aliquot and transfer to a tared weighing vessel. (The remainder of the filtered extracts can be
23、 tested for total organiccarbon or other parameters as desired.)10.6 Evaporate the water and then dry the weighing vessels to constant weight (61 mg) at 104 6 2C (which can be doneovernight). A hot plate can be used to evaporate nearly all the water so long as a layer of water covers the bottom of t
24、he vessel.Final drying is to be done in an oven. Weigh to the nearest 0.1 mg.11. Calculation11.1 Calculate the water extractable residue, in percent, for each of the two sample portions as follows:Water Extractable Residue,%wet basis5A 2B!3200CWater Extractable Residue,%dry basis5A 2B!3200SC 3 D100D
25、3 Gelman Type A/E, Millipore Type AP40, Whatman GF/C, or equivalent, have been found suitable for this purpose.4 Reagent Chemicals, American Chemical Society Specifications, , American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Soc
26、iety, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville, MD.D5627 172where:A = residue from sample, in g,B = residue from blank, in g,C = drained sample used,
27、in g, andD = percent solids, calculated as 100 % water retention capacity (from Test Methods D2187, Test Method B).(These calculations assume a 100-mL aliquot out of 200 mL 200-mL extract.)12. Report12.1 Report the percent water extractable residue as the average of the two values obtained, using th
28、e wet or dry, reporting basisor both, as required.13. Precision and Bias513.1 Single-operator precision was determined using a composite sample of aged but unused strong acid, gel-type cation resinwith an average solids content of 48.6 % by weight. The sample was analyzed in triplicate by six operat
29、ors in one laboratory. Theoperators who participated represented a wide range of experience levels. Since other sources of variability should be relativelysmall (such as from the analytical balances), the multiple laboratory variability is expected to mimic the single-operator precisionand is not se
30、parately determined.All determinations were made using disposable aluminum weighing dishes. The following resultswere obtained:x = 0.393 % by weight, wet basis,So = 0.019 % by weight, wet basis,x = 0.812 % by weight, dry basis, andSo = 0.039 % by weight, dry basisx = 0.393 % by weight, wet basis,So
31、= 0.019 % by weight, wet basis,x = 0.812 % by weight, dry basis, andSo = 0.039 % by weight, dry basis.where x is the arithmetic mean of the 18 determinations and So is the single-operator precision calculated in accordance withPractice D2777.13.2 Since known standards are not available, bias cannot
32、be determined.14. Quality Control14.1 In the analysis of ion exchange resins, it is not possible to prepare a known standard resin for comparison with actualsamples. Therefore it is impossible to test the accuracy of the results, and this test method does not include a bias statement.14.2 Analysts a
33、re expected to run replicate samples to determine if the results are within the expected precision stated inSections 13.15. Keywords15.1 extractables; fouling; ion exchange; residue; sloughageASTM International takes no position respecting the validity of any patent rights asserted in connection wit
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