1、Designation: D 1782 95 (Reapproved 2009)Standard Test Methods forOperating Performance of Particulate Cation-ExchangeMaterials1This standard is issued under the fixed designation D 1782; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revisi
2、on, 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 theoperating capacity of particulate cation-exchange mat
3、erialswhen used for the removal of calcium, magnesium, and sodiumions from water. It is intended for use in testing both new andused materials. The following two test methods are included:SectionsTest Method ASodium Cycle 8 to 14Test Method BHydrogen Cycle 15 to 211.2 The values given in SI units ar
4、e 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 this standard to establish appro-priate safety and healt
5、h practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1067 Test Methods for Acidity or Alkalinity of WaterD 1126 Test Method for Hardness in WaterD 1129 Terminology Relating to WaterD 1193 Specification for Reagent WaterD 268
6、7 Practices for Sampling Particulate Ion-ExchangeMaterials3. Terminology3.1 Definitions:3.1.1 For definitions of terms used in these test methods,refer to Terminology D 1129.3.2 Definitions of Terms Specific to This Standard: Certainterms in these test methods that relate specifically to ionexchange
7、 are defined as follows:3.2.1 free mineral aciditythe quantitative capacity ofaqueous media to react with hydroxyl ions to pH 4.3.3.2.2 hydrogen cyclethe operation of a cation-exchangecycle wherein the removal of specified cations from influentwater is accomplished by exchange with an equivalent amo
8、untof hydrogen ion from the exchange material.3.2.3 theoretical free mineral aciditythe free mineralacidity that would result from the conversion of the anions ofstrong acids in solution to their respective free acids.4. Summary of Test Methods4.1 Test Method A consists of repeated cycles of backwas
9、h,brine regeneration, rinse, and exhaustion of the sample in theform of a bed in a transparent column. The exhausting mediumused is an ion-exchange test water.4.2 Test Method B consists of repeated cycles of backwash,acid regeneration, rinse, and exhaustion of the sample in theform of a bed in a tra
10、nsparent column. The exhausting mediumused is an ion-exchange test water.5. Apparatus5.1 Test Assemble (see Fig. 1), consisting of the following:5.1.1 Column, transparent, vertically supported, 25.4 6 2.5mm (1.0 6 0.1 in.) in inside diameter and approximately 1500mm (60 in.) long. The bottom of the
11、column shall be closed andprovided with an outlet of approximately 6-mm inside diam-eter. Connections shall be provided at top and bottom 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
12、 manner that thevolume readings required by the test method can be made.Make all measurements at 25 6 5C.5.1.2 Support, for the sample, so designed that the distancefrom the sample to the column outlet is at least 50 mm. Asuggested supporting bed utilizes quartz, glass beads, or othermaterial 1.5 to
13、 3.5 mm in diameter, insoluble in the reagentsused, and retained on a corrosion-resistant screen. However,1These test methods are under the jurisdiction of ASTM Committee D19 onWater and are the direct responsibility of Subcommittee D19.08 on Membranes andIon Exchange Materials.Current edition appro
14、ved May 1, 2009. Published June 2009. Originallyapproved in 1960. Last previous edition approved in 2007 as D 1782 95 (2007).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information,
15、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.other supports such as fritted glass or polyester screens may beused at the discretion of the interested parties.6. Reage
16、nts6.1 Purity of ReagentsReagent grade chemicals shall beused 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,where such specifications are available.3Other grades
17、may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.6.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water, Type IV,conforming to Specific
18、ation D 1193.7. Sampling7.1 To obtain a representative sample of particulate ion-exchange material, either from a shipment of new product inthe manufacturers original packages or from a bed of usedmaterial, refer to Practices D 2687.7.2 Transfer the laboratory sample to a 2-L beaker and addenough wa
19、ter to bring the water level up to that of theion-exchange material and soak for 1 h (see Note 1). Mix thesample thoroughly and transfer a sufficient representativeportion to fill a 400-mL beaker. Use this portion of sample inthe procedure.NOTE 1Where new materials are shipped dry, follow the manufa
20、c-turers instructions for preconditioning.TEST METHOD ASODIUM CYCLE8. Scope8.1 This test method is designed to simulate operatingconditions on a sodium cycle used for the removal of calciumand magnesium and other divalent ions from water.9. Significance and Use9.1 Cation exchange materials are frequ
21、ently used in thesodium form to exchange divalent and trivalent ions in theinfluent water for sodium ions on the resin sites. This processis commonly referred to as softening water since it removesthose ions that form a “hard” curd of insoluble salts with thefatty acids used in some soaps and that a
22、lso precipitate when3Reagent 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., and the Uni
23、ted States Pharmacopeiaand National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.FIG. 1 Typical Arrangement of Apparatus for Performance Testing of Ion-Exchange MaterialsD 1782 95 (2009)2water is boiled. In such a process, sodium chloride is used asthe regenerant to return th
24、e cation-exchanging groups to thesodium form.9.2 This test method is intended to simulate the performanceof such materials in actual usage. It may be used either tocompare the performance of new materials or to compare theperformance of a material that has been used with its originalperformance.9.3
25、Regenerant concentrations and dosages used herein aretypical for the types of materials used in this application. Ifdifferent concentrations or amounts of regenerant are agreedupon by parties using this test method, this fact should bestated when the results are reported. Similarly, the test watersp
26、ecified is the agreed upon standard. Where other test watersor the water to be treated are used in the test, the analysis of thewater in terms of total solids, sodium, calcium, magnesium,other di- or trivalent metals as well as the major anions presentshould be reported with the test results.10. Rea
27、gents and Materials10.1 Brine Regenerants:10.1.1 For synthetic organic ion-exchange materials:10.1.1.1 Sodium Chloride (100 g/L)Dissolve enough so-dium chloride (NaCl) in water to make a solution containing ineach litre 100.0 g of NaCl.10.1.2 For all other ion-exchange materials:10.1.2.1 Sodium Chlo
28、ride (50 g/L)Dissolve enough NaClin water to make a solution containing in each litre 50.0 g ofNaCl.10.2 Cation-Exchange Test Water A (10 meq/L)Dissolveenough calcium chloride (CaCl22H2O) and magnesium sulfate(MgSO47H2O) in water to make a solution containing, in eachlitre, 0.49 g of CaCl22H2O and 0
29、.415 g of MgSO47H2O.Adjust the pH to 7.5 by the addition of Na2CO3(30 g/L) anddetermine the hardness of the solution in accordance with TestMethod D 1126. The hardness of the test water will be 10.0 60.5 meq/L. Use the determined hardness in calculating operat-ing capacity as indicated in 12.1. This
30、 test water shall be usedfor all tests.10.3 Hardness Test ReagentsFor reagents used in deter-mining hardness, refer to Test Method D 1126. This reagent isused only in preparation of test water (see 10.2).10.4 Sodium Carbonate Solution (30 g/L)Dissolve 30 g ofsodium carbonate (Na2CO3) in water and di
31、lute to 1 L.11. Procedure11.1 Adjust the temperature of the water and all solutions tobe used in this procedure to 25 6 5C and maintain thistemperature throughout the test.11.2 Fill the column approximately half full of water andadd sufficient sample to give a bed height of 750 6 75 mmabove the top
32、of the support. To avoid drying out of theion-exchange material, maintain a layer of liquid at least 20 to30 mm deep above the top of the bed at all times during theprocedure.11.3 Backwash with water for 10 min using a flow rate thatwill maintain a 50 % expansion of the bed. If the supernatantliquid
33、 is clear at this point, proceed to 11.4. If the liquid iscloudy (indicating the presence of light, insoluble, extraneousmaterial), adjust the backwash outlet tube to a height above thebed equal to 75 % of the bed height. Continue backwashing atthe same rate until the effluent is clear.11.4 Allow th
34、e bed to settle and then drain at a rate ofapproximately 100 mL/min until the water level is 20 to 30 mmabove the top of the bed. Do not jar. Record the volume, inmillilitres, of ion-exchange material. Repeat the 10-min back-wash until two successive readings of volume agree within 5mL. The average
35、of these two readings shall be the samplevolume for new materials shipped in the sodium form.11.5 Exhaust the ion exchanger with cation-exchange testwater A at a flow rate of 0.33 mL/min/mL of exchanger, asmeasured in 11.4. Maintain a head of liquid not less than 50mm above the top of the bed. Conti
36、nue the run until the effluentshows 0.2 meq/L (or other agreed-upon hardness level) whentested in accordance with Test Method D 1126. Record thevolume of test water used.11.6 Repeat the 10-min backwash and drain as described in11.3 and 11.4. When testing new material shipped in thesodium form, only
37、one backwash is necessary at this pointbecause a determination of volume has already been made.However, used material other than in the sodium form musthave a volume determination made here as described in 11.4.Use this sample volume determined on the exhausted materialin calculating the capacity of
38、 used ion-exchange materials.11.7 Determine the amount of brine regenerant and raterequired, from Table 1. For use with Table 1, the volumesample for new material shall be that determined in accordancewith 11.4 and for used material shall be that determined inaccordance with 11.6.11.8 Pass the speci
39、fied volume of brine regenerant throughthe bed at the specified rate until only a 20 to 30-mm layer ofliquid remains above the bed. Rinse the bed with water, usingthe same rate, until one bed-volume of liquid has beendisplaced. Increase the rinse rate to approximately 100 mL/min. Test for hardness a
40、t 3-min intervals by adding 0.5 mL ofbuffer solution to 50 mL of the effluent followed by three dropsof hardness indicator and 0.5 mL of sodium ethylendiaminetetraacetate solution (1 mL = 1.0 mg CaCO3), with stirring. IfTABLE 1 Amount of Brine Regenerant Required for Use in Test Method AType of Exch
41、angeMaterialBrine Regenerant,g/LRate of Flow, mLbrine/min/mL of ExchangerContact Time,minRegeneration Levellb/ft3g/LSynthetic organic 100 0.032 30 6.00 96.1Greensand 50 0.027 15 1.25 20.0Synthetic siliceous 50 0.080 20 3.00 80.1Carbonaceous 50 0.067 15 3.15 50.5D 1782 95 (2009)3a blue color develops
42、, the effluent contains 0.2 meq/L or lesshardness and the rinse is completed. If the color is red, the endpoint has not been reached. Continue the rinse until the effluentshows 0.2 meq/L or less hardness.11.9 Repeat the service run described in 11.5.11.10 Repeat the cycle, beginning with a single ba
43、ckwash(see 11.6), omitting the determination of bed volume. Continuewith a regeneration and rinse (see 11.8), and end with a servicerun (see 11.5). Repeat the cycle until each of three successiveruns agrees within 65 % of their average capacity as calcu-lated in accordance with Section 12.12. Calcul
44、ation12.1 Calculate the operating capacity, in milliequivalentsper millilitre, of the ion exchange material ascapacity, meq/mL 5 A 3 B! / Swhere:A = hardness of test water, meq/L,B = volume of test water used in service run, L, andS = volume of sample in the bed, mL. For new materials,this refers to
45、 the average volume of the material in thesodium form as determined in 11.4. For used materi-als, it is the average volume of the material in theexhausted form as determined in 11.6.12.2 Calculate the operating capacity, in kilograins of cal-cium carbonate per cubic foot as follows:capacity, kilogra
46、ins of CaCO3/ft35 C 3 21.8where:C = capacity in milliequivalents per millilitre of ion-exchange material (see 12.1).13. Report13.1 Report the capacity of the tested material as theaverage of three successive service runs that agree within65 % of their average capacity.14. Precision and Bias414.1 Pre
47、cisionPrecision was determined from the resultsof the analyses of eight operators in four labs, with triplicatedeterminations on three materials. The average value deter-mined for each material was as follows:New Synthetic Organic 1.15 meq/mLUsed Synthetic Organic 1.03 meq/mLNew Synthetic Siliceous
48、0.43 meq/mL14.2 The precision of the test method varies with theoperating capacity of the material tested and may be expressedas follows:St5 0.058 CSo5 0.024 Cwhere:St= overall precision, meq/mL,So= single operator precision, meq/mL, andC = operating capacity, meq/mL.14.3 BiasBecause materials with
49、known operating capac-ity cannot be prepared, bias cannot be determined.TEST METHOD BHYDROGEN CYCLE15. Scope15.1 This test method is designed to simulate operatingconditions on a hydrogen cycle used for the removal of allother cations from water.16. Significance and Use16.1 Cation exchange materials containing sulfonic acidgroups are frequently used in the hydrogen form to exchangehydrogen ions from the resin sites for all the cations in theinfluent water. They are then regenerated with acid to restorethe sites to the hydrogen form for reuse. This test is
