ASTM D2187-1994(2009) Standard Test Methods for Physical and Chemical Properties of Particulate Ion-Exchange Resins.pdf

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1、Designation: D 2187 94 (Reapproved 2009)Standard Test Methods forPhysical and Chemical Properties of Particulate Ion-Exchange Resins1This standard is issued under the fixed designation D 2187; 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. Scope1.1 These test methods cover the determination of thephysical and chemical properties of ion-exchang

3、e resins whenused for the treatment of water. They are intended for use intesting both new and used materials. The following thirteen testmethods are included:SectionsTest Method APretreatment 6-10Test Method BWater Retention Capacity 11-17Test Method CBackwashed and Settled Density 18-24Test Method

4、 DParticle Size Distribution 25-32Test Method ESalt-Splitting Capacity of Cation-Exchange Resins33-41Test Method FTotal Capacity of Cation-ExchangeResins42-50Test Method GPercent Regeneration of Hydrogen-Form Cation-Exchange Resins51-58Test Method HTotal and Salt-Splitting Capacity ofAnion-Exchange

5、Resins59-66Test Method IPercent Regeneration of AnionExchange Resins67-75Test Method JIonic Chloride Content of Anion-Exchange Resins76-83Test Method KCarbonate Content of Anion-Exchange Resins84-91Test Method LSulfate Content of Anion ExchangeResins92-99Test Method MTotal Anion Capacity of Anion-Ex

6、change Resins100-1081.2 The values stated in SI units are to be regarded as thestandard. The inch-pound units given in parentheses are forinformation only.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

7、this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific precau-tionary statements are given in Section 10.8.2. Referenced Documents2.1 ASTM Standards:2D 1129 Terminology Relating to WaterD 1193 Specificatio

8、n for Reagent WaterD 1293 Test Methods for pH of WaterD 2687 Practices for Sampling Particulate Ion-ExchangeMaterialsD 2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterE11 Specification for Woven Wire Test Sieve Cloth andTest Sieves3. Terminolo

9、gy3.1 DefinitionsFor definitions of terms used in these testmethods refer to Terminology D 1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 anion-exchange materialan ion-exchange materialcapable of the reversible exchange of negatively charged ions.3.2.2 cation-exchange materialan ion-e

10、xchange materialcapable of the reversible exchange of positively charged ions.3.2.3 ion-exchange resina synthetic organic ion-exchangematerial.3.2.4 mixed beda physical mixture of anion-exchangematerial and cation-exchange material.4. Reagents4.1 Purity of ReagentsReagent grade chemicals shall beuse

11、d in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,1These test methods are under the jurisdiction of ASTM Committee D19 onWater and are the direct responsibility of

12、Subcommittee D19.08 on Membranes andIon Exchange Materials.Current edition approved May 1, 2009. Published June 2009. Originallyapproved in 1963. Last previous edition approved in 2004 as D 2187 94 (2004).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer S

13、ervice at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.where such specifications are available.3

14、Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.4.2 Purity of Water Unless otherwise indicated, refer-ences to water shall be understood to mean Type IV reagentwater describe

15、d in Specification D 1193.5. Sampling5.1 Obtain a representative sample of the ion-exchangeresin in accordance with Practices D 2687.5.2 A minimum sample size of 1 L is recommended for acomplete testing program.TEST METHOD APRETREATMENT6. Scope6.1 This test method covers the conversion of ion-exchan

16、geresins to a known ionic form and is intended for application toboth new and used material.7. Significance and Use7.1 The ionic form of an ion-exchange material affects bothits equivalent mass and its equilibrium water content. These inturn influence the numerical values obtained in exchangecapacit

17、y determinations, in density measurements, and in thesize of the particles. To provide a uniform basis for compari-son, therefore, the sample should be converted to a knownionic form before analysis. This procedure provides for theconversion of cation-exchange materials to the sodium formand anion-e

18、xchange materials to the chloride form prior toanalysis. These forms are chosen since they permit samples tobe weighed and dried without concern for air contamination ordecomposition. If other ionic forms are used this fact should benoted in reporting the results.8. Apparatus8.1 Pretreatment Apparat

19、us (See Fig. 1):8.1.1 Column, transparent, vertically-supported, 25 6 2.5mm (1.0 6 0.1 in.) inside diameter and approximately 1500mm (60 in.) long.The bottom of the column shall be closed andprovided with an outlet of approximately 6-mm inside diam-eter. Connections shall be provided at top and bott

20、om foradmission and removal of solutions as described in Section 10.Adequate means for measuring and regulating flow shall beprovided. Calibrate the column in such a manner that thevolume readings required by the method can be made. Make allmeasurements at 25 6 5C.8.1.2 Support, for the sample, so d

21、esigned that the distancefrom the sample to the column outlet is at least 50 mm.Suggested supports are corrosion-resistant screen or porousplate.8.2 Draining Apparatus (Fig. 2):8.2.1 Buchner-Type Funnel, containing a 125-mm filterpaper and supported in a 1-L suction flask.8.2.2 Open-Arm Mercury Mano

22、meter, connected by aT-tube to a vacuum train.8.2.3 Gas-Humidifying Tower, of at least 500 mL capacity,two thirds filled with glass beads or similar material.8.2.4 Vacuum Pump, capable of creating a pressure differ-ential 40 mm Hg below atmospheric pressure.9. Reagents9.1 Hydrochloric Acid (1 + 9)Ca

23、refully pour 100 mL ofhydrochloric acid (HCl, sp gr 1.19) into 900 mL of water,stirring constantly. Cool to 25 6 5C.9.2 Sodium Chloride Solution (100 g/L)Dissolve 100.0 gof sodium chloride (NaCl) in 800 mL of water and dilute to 1L.9.3 Sodium Chloride Solution (240 g/L)Dissolve 240 g ofsodium chlori

24、de (NaCl) in 800 mL of water and dilute to 1 L.9.4 Sodium Hydroxide Solution (40 g/L)Dissolve 40.0 gof sodium hydroxide (NaOH) in 800 mL of water. Cool anddilute to 1 L.9.5 Thymol Blue Indicator SolutionDissolve 0.1 g ofthymol blue (thymol sulfonphthalein) in 10.75 mL of 0.02 NNaOH solution. Dilute

25、to 250 mL with water.9.6 Tropaeolin O Indicator SolutionDissolve 0.10 g oftropaeolin O (p-benzene-sulfonic acid-azoresorcinol) in 50 mLof water and dilute to 100 mL in a volumetric flask.3Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For sugg

26、estions 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,MD.FIG. 1 Typical Arrangement o

27、f Apparatus for Pretreatment of Ion-Exchange MaterialsD 2187 94 (2009)210. Procedure10.1 Adjust the temperature of the water and all solutions tobe used in the procedure to 25 6 5C and maintain thistemperature throughout the test.10.2 Transfer the entire sample as received to a 2-L beakerusing water

28、 to rinse out the container. Adjust the water level tothe sample level. Let stand a minimum of 1 h. Mix thoroughlyand transfer a representative sample to fill a 400-mL beaker.10.3 Fill the pretreatment column one half full of water.Transfer the entire contents of the 400-mL beaker to thecolumn using

29、 additional water if necessary.10.4 Backwash with water using a flow rate that willmaintain a 50 % expansion of the bed. Adjust the backwashoutlet tube to a height above the bed equal to 75 % of the bedheight. Continue backwashing for a minimum of 10 min oruntil the effluent is clear. For mixed bed

30、samples proceed inaccordance with 10.5. For single component samples, proceedin accordance with 10.6.10.5 If the sample is a mixed bed, displace the backwashwater from the bed by slowly introducing NaCl solution (100g/L) at the bottom of the column and allowing it to flowupward through the sample. W

31、hen the water has been dis-placed, increase the flow rate until the anion-exchange resin isseparated from and suspended above the cation-exchangeresin. Lower the backwash outlet tube as required to siphon offthe anion-exchange resin, collecting it in a separate pretreat-ment apparatus. Exercise care

32、 to prevent the removal ofcation-exchange resin in this operation. When the transfer ofthe anion-exchange resin is complete, discontinue the flow ofNaCl solution. If the separation of anion and cation-exchangeresins has not been complete and a mixed band is left in thecenter, repeat the siphoning pr

33、ocedure to remove this bandfrom the cation-portion of the sample. This mixed material thatshould not constitute more than 5 % of the original samplevolume, is not included in subsequent tests. If more than 5 %of the sample remains unseparated, the separation should berepeated using NaCl solution (24

34、0 g/L). In either case proceedwith the separated anion and cation components as separatesamples as described in 10.6.10.6 Allow the resin to settle until the liquid level is 20 to 30mm above the top of the bed, and estimate its volume. PassNaCl solution (100 g/L) downflow through the single compo-ne

35、nt sample or the separated components of the mixed bedresin at the approximate rate of 0.133 mL/min/mL of samplefor 1 h. Discontinue the flow of NaCl solution. Backwash withwater for 10 min at a flow rate sufficient to maintain a 50 %expansion of the bed. Discontinue the flow of water.10.7 Allow the

36、 bed to settle and then drain off the water ata rate of approximately 100 mL/min until the water level is 20to 30 mm above the top of the bed. Estimate the volume ofion-exchange resin in millilitres.10.8 Determine the amount of reagent and the flow raterequired for the initial pretreatment from Tabl

37、e 1 using thesample volume determined in 10.7. WarningSwelling of theresin in the column may occur in subsequent steps.10.9 Pass the specified volume of reagent through the bed atthe specified rate until only a 20 or 30 mm layer of liquidremains above the bed. Rinse the bed with two sample volumesof

38、 water at the same rate.10.10 Determine the amount of reagent and the flow raterequired for the second pretreatment from Table 2 using theFIG. 2 Typical Arrangement of Water-Draining ApparatusTABLE 1 Requirements for Initial PretreatmentAnion-ExchangeResinsCation-ExchangeResinsReagent NaOH HClConcen

39、tration 40 g/L 1 + 9Volume required 8 sample volumes 8 sample volumesContact time 1 h 1 hFlow rate, mL/min-mL sample 0.133 0.133Regeneration level:lb/ft3g/L20.032021.2340D 2187 94 (2009)3sample volume determined in 10.7. Note that this secondpretreatment is not used for some methods.10.11 Pass the s

40、pecified volume of reagent through a bed atthe specified rate until only a 20 to 30-mm layer of liquidremains above the bed. Rinse the bed with one sample volumeof water at the same rate. Increase the rinse rate to 100 mL/min.Rinse for 15 min. Thereafter test successive 100-mL portionsof the effluen

41、t from anion-exchange resins by adding two dropsof thymol blue indicator solution. Continue rinsing until a 100mL portion of the effluent remains yellow (pH 2.5) on theaddition of the indicator. Test the effluent from the cation-exchange resins in the same manner with two drops oftropaeolin-O indica

42、tor solution. Continue rinsing until a100-mL portion of the effluent remains yellow (pH 11.0)3onthe addition of the indicator.10.12 Remove the ion-exchange resin from the pretreatmentcolumn, discarding any extraneous material that may haveaccumulated at the bottom of the bed. Transfer the resin to t

43、heBuchner funnel of the draining apparatus that has been fittedwith a medium porosity filter paper. Drain the water to the topof the sample using suction if required. Cover the funnel witha suitable vacuum-tight cover, which is fitted with an inlet forair from the water-filled humidifying tower. App

44、ly sufficientsuction to maintain a pressure differential of 40 6 5mmHgbelow atmospheric pressure. Continue passing humidified airthrough the sample for 10 min.10.13 Transfer the entire drained sample to a clean, dry, 1-L(1-qt.), wide-mouthed bottle with a screw top or other vapor-tight closure.TEST

45、METHOD BWATER RETENTION CAPACITY11. Scope11.1 This test method covers the determination of theamount of water retained by ion-exchange resins and isintended for testing both new and used materials.12. Summary of Test Method12.1 This test method consists of the determination of theloss of mass on dry

46、ing at 104 6 2C.13. Significance and Use13.1 The water retention capacity of an ion-exchange ma-terial is proportional to its pore volume. For new materials ofthe same functionality and polymer type, higher values indicatelower effective crosslinking. Increases in water retention ca-pacity of used m

47、aterials as compared with the values for newmaterial serve as an indicator of polymer decrosslinking:decreases may indicate either loss of functionality or fouling ofthe ion-exchange material. Since the numerical value is di-rectly dependent on the ionic form of the material, carefulpreconditioning

48、of both original and used samples to knownionic forms as outlined in Section 7 is essential when suchcomparisons are made.14. Procedure14.1 Weigh three approximately 5-g representative samplesof material pretreated in accordance with Section 10 to thenearest 1 mg into previously tared weighing vesse

49、ls.14.2 Dry the samples for 18 6 2hat1046 2C.14.3 Remove the samples from the oven. Cool 30 min in adesiccator, and reweigh.15. Calculation15.1 Calculate the water retention capacity, in percent, asfollows:water retained, % 5 A 2 B!/A 3 100 (1)where:A = amount of wet sample used, g, andB = amount of dry sample obtained, g.16. Report16.1 Report the percent water retained as the average of thethree values obtained.17. Precision and Bias417.1 PrecisionThe precision of this test method of deter-mining water retention capacity of ion exchange resin