1、Designation: D 3087 91 (Reapproved 2009)Standard Test Method forOperating Performance of Anion-Exchange Materials forStrong Acid Removal1This standard is issued under the fixed designation D 3087; the number immediately following the designation indicates the year oforiginal adoption or, in the case
2、 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 oper-ating capacity of anion-exchange mater
3、ials when used for theremoval of hydrochloric and sulfuric acid from water. It isdesigned to simulate operating conditions for strong acidremoval and is intended for use in testing both new and usedmaterials.1.2 The values stated in SI units are to be regarded as thestandard. The inch-pound units gi
4、ven 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 health practices and determine the applica-bility of regulato
5、ry limitations prior to use. Specific precau-tionary statements are given in Note .2. Referenced Documents2.1 ASTM Standards:2D 1067 Test Methods for Acidity or Alkalinity of WaterD 1125 Test Methods for Electrical Conductivity and Re-sistivity of WaterD 1129 Terminology Relating to WaterD 1193 Spec
6、ification for Reagent WaterD 2687 Practices for Sampling Particulate Ion-ExchangeMaterials3. Terminology3.1 Definitions: For definitions of terms used in this testmethod, refer to Terminology D 1129.4. Summary of Test Method4.1 The test method consists of repeated cycles of back-wash, base regenerat
7、ion, rinse, and exhaustion of the sample inthe form of a bed in a transparent column. The exhaustionmedium used is an ion-exchange test water.5. Significance and Use5.1 This test method can be used for evaluating performanceof commercially available anion-exchange materials regardlessof the basic st
8、rength of the ion exchange groups. Whenprevious operating history is known, a good interpretation ofresin fouling or malfunction can be obtained by comparisonagainst a reference sample of unused ion-exchange materialevaluated in the same way.5.2 While resistivity has been chosen as the preferredanal
9、ytical method for defining the exhaustion end point, withtitration as the alternative, it is understood that observation ofpH during rinse and the service run can yield useful informa-tion. The variations in pH observed with an ion exchangematerial suspected of having degraded, can be helpful ininte
10、rpretation of performance when compared with similar datafor a reference sample of unused material exhausted in thesame way.6. Apparatus6.1 Test Assembly (see Fig. 1), consisting of the following:6.1.1 Column, transparent, vertically supported, 25.4 62.5-mm (1.0 6 0.1-in.) inside diameter and approx
11、imately 1.5m (60 in.) long. The bottom of the column shall be closed andprovided with an outlet of approximately 6-mm (14-in.) insidediameter. Connections shall be provided at the top and bottomfor the admission and removal of the solutions described inSection 7. Adequate means for measuring and reg
12、ulating theflow shall also be provided. The column shall be calibrated insuch a manner that the volume readings required by the methodcan be made (see Section 9). All measurements shall be madeat 25 6 5C.6.1.2 Support the sample at least 50 mm (2 in.) above thebottom of the column outlet using quart
13、z, gravel, glass beads orother material from 1.5 to 3.5 mm (116 to18 in.) in diameter,insoluble in the reagents used, and retained on a corrosion-resistant screen. However, other supports may be used at thediscretion of the interested parties.1This test method is under the jurisdiction of ASTM Commi
14、ttee D19 on Waterand is the direct responsibility of Subcommittee D19.08 on Membranes and IonExchange Materials.Current edition approved May 1, 2009. Published June 2009. Originallyapproved in 1978. Last previous edition approved in 2004 as D 3087 91 (2004).2For referenced ASTM standards, visit the
15、ASTM website, www.astm.org, orcontact ASTM Customer Service 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, Un
16、ited States.7. Reagents7.1 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 avai
17、lable.3Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high puritity to permit its use without lessening theaccuracy of the determination.7.2 Purity of Water Unless otherwise indicated, refer-ences to water shall be understood to mean reagent waterconform
18、ing to Specification D 1193, Type III.7.3 Acidity Test ReagentsFor reagents used in determin-ing acidity, refer to Test Methods D 1067.7.4 Anion Exchange Test Water C (10 meq/L)Carefullyadd 18.1 mL of sulfuric acid (H2SO4, sp gr 1.84) and 27.5 mLof hydrochloric acid (HCl, sp gr 1.19) to 500 mL of wa
19、ter anddilute to 1 L. Prepare the test water by adding 1 volume of themixed acid solution to 99 volumes of water. Determine theacidity of the test water in accordance with Test MethodsD 1067, titrating to the methyl purple end point. The acidityshall be 10.0 6 0.5 meq/L (epm).7.5 Base Regenerants:7.
20、5.1 For Weak Base Ion-Exchange Materials:7.5.1.1 Ammonium Hydroxide (40 g NH3/L)Dilute 155mL of ammonium hydroxide (NH4OH sp gr 0.90) to 1 L withwater. The solution should be freshly prepared to avoidabsorption of carbon dioxide (CO2) from the air.7.5.2 For Weak, Intermediate, and Strong Base Ion-Ex
21、change Materials:7.5.2.1 Sodium Hydroxide Solution (40 g/L)Dissolve 40 gof sodium hydroxide (NaOH) in 800 mL of water and dilute to1 L. The solution should be freshly prepared to avoid absorp-tion of carbon dioxide (CO2) from the air.8. Sampling8.1 For sampling procedures refer to Practices D 2687.9
22、. Procedure9.1 Adjust temperature of the water and all solutions to beused in this procedure to 25 6 5C and maintain thistemperature throughout the test.9.2 Fill the column approximately half full of water and addsufficient sample to give a bed height of 750 6 75 mm (30 63 in.) above the top of the
23、support. To avoid drying out of theion-exchange material, maintain a layer of liquid at least 20 to30 mm (0.8 to 1.2 in.) deep above the top of the bed at all timesduring the procedure.9.3 Backwash with water for 10 min using a flow rate thatwill maintain a 50 % expansion of the bed. If the supernat
24、antliquid is clear at this point, proceed to 9.4. If the supernatantliquid is cloudy (indicating the presence of light, insoluble,extraneous material), adjust the backwash outlet tube to aheight above the bed equal to 75 % of the bed height. Continuebackwashing at the same rate until the effluent is
25、 clear.9.4 Allow the bed to settle and then drain at a rate ofapproximately 100 mL/min until the water level is 20 to 30 mm(0.8 to 1.2 in.) above the top of the bed. Record the volume, inmillilitres, of ion-exchange material for use in the followingpretreatment. Regenerate the sample with the approp
26、riatedilute sodium hydroxide solution (see Note 1) for 90 min at aflow rate of 0.11 mL/min for each millilitre of ion exchanger inthe column. This corresponds to a regeneration level of 400 g/L(25 lb/ft3) of ion exchange material.9.5 When only a 20 to 30-mm (0.8 to 1.2-in.) layer of liquidremains ab
27、ove the bed, rinse with water using the same flowrate, until a volume equal to the volume of resin has beendisplaced (one bed volume). Increase the rinse rate to approxi-mately 100 mL/min and continue the rinse until a total of tenbed volumes liquid have been used.9.6 Backwash with water for 10 min
28、using a flow rate thatwill maintain a 50 % expansion of the bed. Allow the bed tosettle and then drain at rate of approximately 100 mL/min untilthe water is 20 to 30 mm (0.8 to 1.2 in.) above the top of thebed. Record the volume in millilitres, of ion-exchange mate-rial. Repeat the foregoing procedu
29、re until two successivevolume readings agree within 5 mL. Take the average of thesetwo readings as the sample volume used in calculating thecapacity of the ion-exchange material under test.9.7 Exhaust the ion exchange material with the anion-exchange test water C at a flow rate of 0.33 mL/min/mL of
30、ionexchange material as measured in 9.6. Maintain a head ofliquid not less than 50 mm (2 in.) above the top of the bed3“Reagent Chemicals, American Chemical Society Specifications,” Am. Chemi-cal Soc., Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Soci
31、ety, see “Analar Standards for Laboratory Chemicals,”BDH Ltd., Poole, Dorset, U.K., and the “United States Pharmacopeia.”FIG. 1 Typical Arrangement of Apparatus for Performance Testingof Ion-Exchange MaterialsD 3087 91 (2009)2during the exhaustion. During the run, test the effluent periodi-cally by
32、one of the methods given in Table 1. Continue the rununtil the designated end point is reached, and record thevolume of test water used.9.8 Repeat the backwash and drain in accordance with 9.6,omitting the determination of bed volume.9.9 Regenerate the sample with the appropriate NaOHsolution (see N
33、ote 1), maintaining a flow rate through the bedof 0.054 mL/min/mL of ion-exchange material based on thesample volume determined in 9.6. Continue the flow for 30min, leaving a 20 to 30-mm (0.8 to 1.2-in.) layer of liquidabove the bed. This corresponds to a regeneration level of 64.1g/L (4 lb/ft3) of
34、ion-exchange material.NOTE 1Alternative regenerant solutions, ammonia and soda ash, maybe used in place of caustic for evaluation of weak base ion-exchangematerial; however, the operating capacity results based on these regener-ants may be different than the operating capacity results based on caust
35、icregeneration.9.10 Rinse the bed with anion-exchange test water C (seeNote 2) at the same rate until one bed volume of liquid hasbeen displaced, then increase the rate to 0.33 mL/min/mL ofion-exchange material as measured in 9.6. The liquid levelabove the top of the bed should be maintained at 50 m
36、m (2 in.).During the rinse, determine the effluent resistivity at least every15 min, until the resistivity is greater than 20 000 V-cm andrecord the volume of rinse water.NOTE 2Test water C is used for the rinse step to simulate the use ofcation bed effluent for anion bed rinse which is typical in m
37、any industrialdemineralizer systems. Alternative rinse solutions, such as water, may beused in the evaluation of other types of systems; however, the operatingcapacity results based on these rinse solutions may be different than thoseusing test water C as required in 9.10.9.11 Exhaust the ion-exchan
38、ge material by maintaining theflow of test water until the effluent resistivity is less than20 000 V-cm. Record the total volume of test water.9.12 Repeat the cycle, beginning with the backwash (see9.8) followed by the regeneration (see 9.9). Continue with therinse (see 9.10) and end with the servic
39、e run (see 9.11). Repeatuntil each of three successive runs agrees within 6 5 % of theaverage capacity as calculated in accordance with Section 10.10. Calculation10.1 Calculate the operating capacity, C8, in milliequiva-lents per millilitre of ion-exchange material as follows:C8 5 B 2 A! 3 F/Swhere:
40、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 = millilitres of ion-exchange material used (see 9.6).10.2 Calculate the operating capacity, C9, in kilograins ofcalcium carbonate per cubic foot, as foll
41、ows:C9 5 C8 3 21.810.3 Calculate the rinse value, R, in litres of rinse water perlitre of bed volume, as follows:R 5 A 3 1000!/Swhere:A = litres of rinse water (see 9.10), andS = millilitres of ion-exchange material used (see 9.6).10.4 Calculate the rinse value, R8, in gallons of rinse waterper cubi
42、c foot of bed volume, as follows:R8 5 R 3 7.4811. Report11.1 Report the capacity of test material as the average ofthree successive service runs that agree within 6 5 % of theaverage.12. Precision and Bias412.1 PrecisionThe Referenced Documents show thatseven laboratories participated in a round rob
43、in test of theoperating performance of anion-exchange materials of fourresins using two different regenerants, sodium hydroxide, andammonium hydroxide. Each of the four resin samples wereevaluated by at least three different labs and in some cases fourdifferent labs. Each lab evaluated the assigned
44、resin samples atleast once, with three labs doing the assigned samples induplicate, and one lab doing the assigned samples in triplicate.Separate evaluations of two resin samples were made by twopeople in one lab.12.1.1 The precision of the values obtained by this testmethod is dependent upon the ma
45、gnitude of the observedvalues and can be estimated from the following relationships:12.1.1.1 For rinse values in litre of rinse per litre of resinbed (see 10.3):log SR5 0.0267R 2 0.523where:SR= the absolute value of the standard deviation, andR = rinse value in L of rinse/L of resin bed.12.1.1.2 For
46、 capacity values in kilograins per cubic foot asCaCO3(see 10.2):Sc5 0.0481 C9 2 0.1641where:Sc= the absolute value of the standard deviation, andC9 = operating capacity in kilograins/ft3.12.2 BiasBecause no materials with known operatingcapacity can be prepared, calculation of bias is impossible.13.
47、 Keywords13.1 anion resin; ion exchange; operating performance4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D191011.TABLE 1 Test Methods for Anion-Exchanger EffluentStatus ASTMDesignationRinse EndPointService EndPointPreferre
48、d D 1125 20 000 V-cm 20 000 V-cmAlternative D 1067 0.1 meq/L phenol-phthalein0.1 meq/L methylpurpleD 3087 91 (2009)3ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly a
49、dvised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.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 International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical
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