1、Designation: D3087 91 (Reapproved 2009)D3087 17Standard Test Method forOperating Performance of Anion-Exchange Materials forStrong Acid Removal1This standard is issued under the fixed designation D3087; the number immediately following the designation indicates the year oforiginal adoption or, in th
2、e case of 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 This test method covers the determination of the operating capacity of anion-exchange
3、materials when used for the removalof hydrochloric and sulfuric acid from water. It is designed to simulate operating conditions for strong acid removal and is intendedfor use in testing both new and used materials.1.2 The values stated in SI units are to be regarded as the standard. The inch-pound
4、units given in parentheses are forinformation only.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 and health practices and determine the applicability of r
5、egulatorylimitations 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 Org
6、anization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1067 Test Methods for Acidity or Alkalinity of WaterD1125 Test Methods for Electrical Conductivity and Resistivity of WaterD1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD2687 P
7、ractices for Sampling Particulate Ion-Exchange Materials1 This test method is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.08 on Membranes and Ion ExchangeMaterials.Current edition approved May 1, 2009June 1, 2017. Published June 2009June
8、 2017. Originally approved in 1978. Last previous edition approved in 20042009 asD3087 91 (2004).(2009). DOI: 10.1520/D3087-91R09.10.1520/D3087-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standard
9、svolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard 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
10、adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases 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 Consh
11、ohocken, PA 19428-2959. United States1D5391 Test Method for Electrical Conductivity and Resistivity of a Flowing High Purity Water Sample3. 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 this
12、 standard, refer to Terminology D1129.4. Summary of Test Method4.1 The test method consists of repeated cycles of backwash, base regeneration, rinse, and exhaustion of the sample in the formof a bed in a transparent column. The exhaustion medium used is an ion-exchange test water.5. Significance and
13、 Use5.1 This test method can be used for evaluating performance of commercially available anion-exchange materials regardless ofthe basic strength of the ion exchange groups. When previous operating history is known, a good interpretation of resin foulingor malfunction can be obtained by comparison
14、against a reference sample of unused ion-exchange material evaluated in the sameway.5.2 While resistivity has been chosen as the preferred analytical method for defining the exhaustion end point, with titration asthe alternative, it is understood that observation of pH during rinse and the service r
15、un can yield useful information. The variationsin pH observed with an ion exchange material suspected of having degraded, can be helpful in interpretation of performance whencompared with similar data for a reference sample of unused material exhausted in the same way.6. Apparatus6.1 Test Assembly (
16、see Fig. 1), consisting of the following:6.1.1 Column, transparent, vertically supported, 25.4 6 2.5-mm (1.0 6 0.1-in.) inside diameter and approximately 1.5 m (60in.) long. The bottom of the column shall be closed and provided with an outlet of approximately 6-mm (14-in.) inside diameter.Connection
17、s shall be provided at the top and bottom for the admission and removal of the solutions described in Section 7.Adequate means for measuring and regulating the flow shall also be provided. The column shall be calibrated in such a mannerthat the volume readings required by the method can be made (see
18、 Section 9). All measurements shall be made at 25 6 5C.FIG. 1 Typical Arrangement of Apparatus for Performance Testing of Ion-Exchange MaterialsD3087 1726.1.2 Support the sample at least 50 mm (2 in.) above the bottom of the column outlet using quartz, gravel, glass beads or othermaterial from 1.5 t
19、o 3.5 mm (116 to 18 in.) in diameter, insoluble in the reagents used, and retained on a corrosion-resistant screen.However, other supports may be used at the discretion of the interested parties.7. Reagents7.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise ind
20、icated, it is intended that allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, wheresuch specifications are available.3 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently highpuritity t
21、o permit its use without lessening the accuracy of the determination.7.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water conforming toSpecification D1193, Type III.7.3 Acidity Test ReagentsFor reagents used in determining acidity, refer to Tes
22、t Methods D1067.7.4 Anion Exchange Test Water C (10 meq/L)Carefully add 18.1 mL of sulfuric acid (H2SO4, sp gr 1.84) and 27.5 mL ofhydrochloric acid (HCl, sp gr 1.19) to 500 mL of water and dilute to 1 L. Prepare the test water by adding 1 volume of the mixedacid solution to 99 volumes of water. Det
23、ermine the acidity of the test water in accordance with Test Methods D1067, titrating tothe methyl purple end point. The acidity shall be 10.0 6 0.5 meq/L (epm).7.5 Base Regenerants:7.5.1 For Weak Base Ion-Exchange Materials:7.5.1.1 Ammonium Hydroxide (40 g NH3/L)Dilute 155 mL of ammonium hydroxide
24、(NH4OH sp gr 0.90) to 1 L with water.The solution should be freshly prepared to avoid absorption of carbon dioxide (CO2) from the air.7.5.2 For Weak, Intermediate, and Strong Base Ion-Exchange Materials:7.5.2.1 Sodium Hydroxide Solution (40 g/L)Dissolve 40 g of sodium hydroxide (NaOH) in 800 mL of w
25、ater and dilute to 1L. The solution should be freshly prepared to avoid absorption of carbon dioxide (CO2) from the air.8. Sampling8.1 For sampling procedures refer to Practices D2687.9. Procedure9.1 Adjust temperature of the water and all solutions to be used in this procedure to 25 6 5C and mainta
26、in this temperaturethroughout the test.9.2 Fill the column approximately half full of water and add sufficient sample to give a bed height of 750 6 75 mm (30 6 3in.) above the top of the support. To avoid drying out of the ion-exchange material, maintain a layer of liquid at least 20 to 30 mm(0.8 to
27、 1.2 in.) deep above the top of the bed at all times during the procedure.9.3 Backwash with water for 10 min using a flow rate that will maintain a 50 % expansion of the bed. If the supernatant liquidis clear at this point, proceed to 9.4. If the supernatant liquid is cloudy (indicating the presence
28、 of light, insoluble, extraneousmaterial), adjust the backwash outlet tube to a height above the bed equal to 75 % of the bed height. Continue backwashing at thesame rate until the effluent is clear.9.4 Allow the bed to settle and then drain at a rate of approximately 100 mL/min until the water leve
29、l is 20 to 30 mm (0.8 to1.2 in.) above the top of the bed. Record the volume, in millilitres, of ion-exchange material for use in the following pretreatment.Regenerate the sample with the appropriate dilute sodium hydroxide solution (see Note 1) for 90 min at a flow rate of 0.11 mL/minfor each milli
30、litre of ion exchanger in the column. This corresponds to a regeneration level of 400 g/L (25 lb/ft3) of ion exchangematerial.9.5 When only a 20 to 30-mm (0.8 to 1.2-in.) layer of liquid remains above the bed, rinse with water using the same flow rate,until a volume equal to the volume of resin has
31、been displaced (one bed volume). Increase the rinse rate to approximately 100mL/min and continue the rinse until a total of ten bed volumes liquid have been used.9.6 Backwash with water for 10 min using a flow rate that will maintain a 50 % expansion of the bed. Allow the bed to settleand then drain
32、 at rate of approximately 100 mL/min until the water is 20 to 30 mm (0.8 to 1.2 in.) above the top of the bed. Recordthe volume in millilitres, of ion-exchange material. Repeat the foregoing procedure until two successive volume readings agreewithin 5 mL. Take the average of these two readings as th
33、e sample volume used in calculating the capacity of the ion-exchangematerial under test.3 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC, www.chemistry.org. For suggestions on the testing ofreagents not listed by theAmerican Chemical Society, s
34、ee the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD, http:/www.usp.org.“Reagent Chemicals, American Chemical Society Specifications,” Am. Chemical Soc., Washington, DC. For suggestions on the testing of reagents not listed by theAmerican
35、 Chemical Society, see “Analar Standards for Laboratory Chemicals,” BDH Ltd., Poole, Dorset, U.K., and the “United States Pharmacopeia.”D3087 1739.7 Exhaust the ion exchange material with the anion-exchange test water C at a flow rate of 0.33 mL/min/mL of ion exchangematerial as measured in 9.6. Mai
36、ntain a head of liquid not less than 50 mm (2 in.) above the top of the bed during the exhaustion.During the run, test the effluent periodically by one of the methods given in Table 1. Continue the run until the designated end pointis reached, and record the volume of test water used.9.8 Repeat the
37、backwash and drain in accordance with 9.6, omitting the determination of bed volume.9.9 Regenerate the sample with the appropriate NaOH solution (see Note 1), maintaining a flow rate through the bed of 0.054mL/min/mL of ion-exchange material based on the sample volume determined in 9.6. Continue the
38、 flow for 30 min, leaving a 20to 30-mm (0.8 to 1.2-in.) layer of liquid above the bed. This corresponds to a regeneration level of 64.1 g/L (4 lb/ft3) ofion-exchange material.NOTE 1Alternative regenerant solutions, ammonia and soda ash, may be used in place of caustic for evaluation of weak base ion
39、-exchange material;however, the operating capacity results based on these regenerants may be different than the operating capacity results based on caustic regeneration.9.10 Rinse the bed with anion-exchange test water C (see Note 2) at the same rate until one bed volume of liquid has beendisplaced,
40、 then increase the rate to 0.33 mL/min/mL of ion-exchange material as measured in 9.6. The liquid level above the topof the bed should be maintained at 50 mm (2 in.). During the rinse, determine the effluent resistivity at least every 15 min, untilthe resistivity is greater than 20 000 -cm and recor
41、d the volume of rinse water.NOTE 2Test water C is used for the rinse step to simulate the use of cation bed effluent for anion bed rinse which is typical in many industrialdemineralizer systems.Alternative rinse solutions, such as water, may be used in the evaluation of other types of systems; howev
42、er, the operating capacityresults based on these rinse solutions may be different than those using test water C as required in 9.10.9.11 Exhaust the ion-exchange material by maintaining the flow of test water until the effluent resistivity is less than 20 000-cm. Record the total volume of test wate
43、r.9.12 Repeat the cycle, beginning with the backwash (see 9.8) followed by the regeneration (see 9.9). Continue with the rinse(see 9.10) and end with the service run (see 9.11). Repeat until each of three successive runs agrees within 6 5 % of the averagecapacity as calculated in accordance with Sec
44、tion 10.10. Calculation10.1 Calculate the operating capacity, C, in milliequivalents per millilitre of ion-exchange material as follows:C5B 2A! 3F#/Swhere:A = litres of test water used in rinse (see 9.10),B = total litres of test water used (see 9.11),F = acidity of test water, meq/L, (see 7.4) andS
45、 = millilitres of ion-exchange material used (see 9.6).10.2 Calculate the operating capacity, C“, in kilograins of calcium carbonate per cubic foot, as follows:C“5C321.810.3 Calculate the rinse value, R, in litres of rinse water per litre of bed volume, as follows:R 5 A 31000!/Swhere:A = litres of r
46、inse water (see 9.10), andS = millilitres of ion-exchange material used (see 9.6).10.4 Calculate the rinse value, R , in gallons of rinse water per cubic foot of bed volume, as follows:R5R 37.4811. Report11.1 Report the capacity of test material as the average of three successive service runs that a
47、gree within 65 % of the average.TABLE 1 Test Methods for Anion-Exchanger EffluentStatus ASTMDesignationRinse EndPointService EndPointPreferred D1125(or D5391)20 000 -cm 20 000 -cmAlternative D1067 0.1 meq/L phenol-phthalein0.1 meq/L methylpurpleD3087 17412. Precision and Bias412.1 PrecisionThe Refer
48、enced Documents show that seven laboratories participated in a round robin test of the operatingperformance of anion-exchange materials of four resins using two different regenerants, sodium hydroxide, and ammoniumhydroxide. Each of the four resin samples were evaluated by at least three different l
49、abs and in some cases four different labs. Eachlab evaluated the assigned resin samples at least once, with three labs doing the assigned samples in duplicate, and one lab doingthe assigned samples in triplicate. Separate evaluations of two resin samples were made by two people in one lab.12.1.1 The precision of the values obtained by this test method is dependent upon the magnitude of the observed values andcan be estimated from the following relationships:12.1.1.1 For rinse values in litre of rinse per litre of resin bed (see 10.3):logSR 50.0267R
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