ASTM D3375-2018 Standard Test Method for Column Capacity of Particulate Mixed Bed IonExchange Materials.pdf

1、Designation: D3375 16D3375 18Standard Test Method forColumn Capacity of Particulate Mixed Bed IonExchange Materials1This standard is issued under the fixed designation D3375; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year

2、 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 performance of particulate mixed bed ion exchange materials in th

3、eregenerated form when used for deionization. It is intended for use in testing unused mixed bed materials and samples ofregenerated mixed beds from operating units.1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses are mathematical conversionsto inch-p

4、ound units that are provided for information only and are not considered standard.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 health

5、environmental practices and determine theapplicability of regulatory limitations 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 Standa

6、rds, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1125 Test Methods for Electrical Conductivity and Resistivity of WaterD1129 Terminology Relating to WaterD1193 Specification for Reagent Water

7、D1293 Test Methods for pH of WaterD1782 Test Methods for Operating Performance of Particulate Cation-Exchange MaterialsD2687 Practices for Sampling Particulate Ion-Exchange Materials3. Terminology3.1 DefinitionsFor definitions of terms related to water, refer to Terminology D1129.4. Summary of Test

8、Method4.1 This test method consists of exhausting a column of regenerated mixed bed ion exchange material to a specific end pointwith an influent solution of known composition and volume.5. Significance and Use5.1 This test method can be used to evaluate unused mixed bed ion exchange materials for c

9、onformance to specifications. Whena representative sample of the mixed bed can be obtained from an operating unit, this test method can be used to evaluate theregeneration efficiency by comparison with the same data obtained with new material from the same manufactured lots, or retainedsamples of th

10、e in-place products.5.2 This test method provides for the calculation of capacity in terms of the volume of water treated to a conductivity end point.1 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 I

11、on ExchangeMaterials.Current edition approved July 1, 2016May 1, 2018. Published July 2016May 2018. Originally approved in 1975. Last previous edition approved in 20072016 asD3375 95a (2007).D3375 16. DOI: 10.1520/D3375-16.10.1520/D3375-18.2 For referencedASTM standards, visit theASTM website, www.a

12、stm.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 standard and is intended only to provide the user of an ASTM standard an indication of what

13、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 cases only the current versionof the standard as published by ASTM is to be considered the o

14、fficial document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.3 The test method as written assumes that the cation exchange material has been regenerated to the hydrogen form with acidand the anion exchange material has been rege

15、nerated with alkali to the hydroxide or free-base form. In certain applications acation exchange material in the potassium, ammonium, or other monovalent form may be encountered. Such materials may betested following this procedure using Test Water A (Test Methods D1782) as the influent and substitu

16、ting the hardness end point(Test Methods D1782) for the end points prescribed herein.5.4 In most cases the product tested will be properly mixed and will contain the correct proportions of anion and cationexchange materials. However, if the pH as well as the conductivity of the effluent is measured,

17、 the test method will indicate whichof the components is present in excess; an acid effluent at breakthrough indicating an excess of regenerated cation exchange groupsand an alkaline effluent an excess of regenerated anion exchange groups. In such cases the volumes of the two components obtainedin t

18、he final backwash will indicate whether this imbalance arises from improper regeneration or from an improper ratio of the twocomponents. It should be noted, however, that not all units are charged with a balanced ratio of anion-exchanging andcation-exchanging groups. Hence, wherever possible, a fiel

19、d sample should be evaluated in comparison with a retained sample ofthe original charge.5.5 This test method provides for the calculation of capacity on either a wet weight basis or a volume basis. Although suchmaterials are normally bought and sold in terms of cubic feet, they are actually packaged

20、 in wet pounds.Therefore, it is the capacityon a wet weight basis that is directly correlatable to the amount of material in a given shipment.5.6 Calculation of a volume capacity is based on the exhausted, separated volume of the components after backwashing andresettling the bed. This volume is cho

21、sen because it is difficult, if not impossible, to pack a sample of regenerated mixed bedmaterial in a small-diameter column reproducibly.5.7 This test method may be used to test mixed bed resin cartridges. In such cases the flow rate of test water and the frequencyof sampling must be varied to comp

22、ensate for the approximate volume of resin in the test sample. The test as written assumes aresin volume of approximately 330 mL.6. Apparatus6.1 Test Assembly (Fig. 1), consisting of the following:6.1.1 Column, transparent supported 2.5 6 0.25-cm (1 6 0.1-in.) inside diameter and approximately 150 c

23、m (60 in.) long. Thebottom of the column shall be closed and provided with an outlet of about 6-mm inside diameter. Connections shall be providedat the top and the bottom for the admission and removal of the exhausting solution as described in 7.4. Adequate means ofregulating and measuring flow shal

24、l be provided. Support for the sample shall be provided so that the distance from the sampleto the column outlet is at least 5 cm. Calibrate the column in such a manner that the volume readings required by the test methodcan be made. Make all calibration measurements at 25 6 5C.6.1.2 Sample Support,

25、 so designed that the distance from the sample to the column outlet is at least 5 cm.Asuggested supportingbed utilizes quartz, gravel, glass beads, or other material 1.5 to 3.5 mm in diameter, insoluble in the reagents used, and retainedon a corrosion-resistant screen.6.2 Measuring circuit and in-li

26、ne conductivity cells as described in Test Methods D1125. A continuous recorder isrecommended.6.3 pH Meter, with associated electrodes as described in Test Methods D1293. A continuous recorder is recommended.7. Reagents7.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless

27、otherwise indicated, 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 h

28、ighpurity to permit its use without lessening the accuracy of the determination.7.2 Purity of WaterAll reference to water in this test method shall be understood to mean Reagent Water Type I or IIconforming to Specification D1193, with the additional requirement that the silica concentration is less

29、 than 0.1 mg/L.7.3 Ammonium Hydroxide Solution (1+19)Carefully pour 50 mL of concentrated ammonium hydroxide (NH4OH, sp gr 0.90)into 500 mL of water, stirring constantly. Cool to 25 6 5C and dilute to 1 L with water. Mix well.7.4 Ion Exchange Test Water D (10 meq/L)Prepare a test water containing, i

30、n each litre, 0.585 g of oven-dried (105C) sodiumchloride (NaCl). Approximately 25 L of this solution are required for a single test.7.4.1 To standardize for chloride content, pipet three 100-mL portions. Add one drop of methyl orange indicator solution andone drop of phenolphthalein indicator solut

31、ion to each and neutralize, if required, by dropwise addition of HNO3 (1+9) until the3 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards f

32、or Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville, MD.D3375 182color changes from yellow to orange followed by dropwise addition of NH4OH (1+19) to restore the yellow color. Pipet i

33、n 1 mLof K2CrO4 solution (50 g/L) and titrate each with standard 0.1 NAgNO3 solution until the color of the supernatant solution changesfrom yellow to red-orange and persists for 30 s with vigorous swirling. Record the average number of millilitres ofAgNO3 solutionused to 60.02 mL.7.4.2 Calculate th

34、e strength of the solution in meq of chloride as follows:Chloride,meq/L5V3N310 (1)where:V = millilitres of AgNO3 solution required for titration, andN = normality of the AgNO3 solution.The test solution used should have a concentration of 10 6 0.5 meq/L of chloride.NOTE 1Because of the large quantit

35、ies of this reagent that are required, it is usually made up semi-quantitatively in large batches and thenstandardized per the above procedure. If desired, it is acceptable to prepare this reagent quantitatively (as for a primary standard) and then eliminate theabove standardization.7.5 Methyl Orang

36、e Indicator Solution (1.0 g/L)Dissolve 0.10 g of methyl orange in water and dilute to 100 mL with water.7.6 Nitric Acid (1+9)Pour one volume of nitric acid (HNO3, sp gr 1.42) into nine volumes of water and mix thoroughly.7.7 Phenolphthalein Indicator Solution (10.0 g/L)Dissolve 1.0 g of phenolphthal

37、ein in 100 mL of 95 % ethanol.NOTE 2In most cases certain denatured alcohols such as specially denatured Formula Nos. 3A, 30, or 2B may be substituted for ethanol.7.8 Potassium Chromate Solution (50 g/L)Dissolve 5.0 g of potassium chromate (K2CrO4) in 50 mL of water. Dilute to 100mL with water.7.9 S

38、ilver Nitrate Solution, Standard (0.10 N)Dry crystalline silver nitrate (AgNO3) at 105C for 1 h and cool in a desiccator.Weigh out 17 6 0.05 g. Transfer to a 1-L volumetric flask with water. Dissolve in 500 mL of water and mix thoroughly. Diluteto 1 L with water at 25 6 5C. Mix well. Store the solut

39、ion in a tightly stoppered amber glass bottle.FIG. 1 Typical Arrangement of Apparatus for Performance Testing of Ion Exchange MaterialsD3375 1837.9.1 To standardize, dry approximately 5 g of reagent sodium chloride (NaCl) in a glass container at 105C for 2 h. Cool ina desiccator. Weigh accurately th

40、ree 0.2500 6 0.0100-g portions of the dried NaCl and transfer to separate 250-mL conical flasks.Add 100 mL of water and swirl to dissolve the NaCl. Pipet in 1 mL of K2CrO4 solution (50 g/L) and titrate with the 0.1 N AgNO3solution with vigorous swirling until the color of the solution changes from y

41、ellow to red-orange and persists for 30 s.7.9.2 Calculate the normality of the AgNO3 solution as follows:N5D/0.058453E (2)where:N = normality of the AgNO3 solution,D = actual weight of NaCl used, andE = millilitres of AgNO3 solution used.8. Sampling8.1 For sampling refer to Practices D2687.8.2 When

42、sampling new mixed bed materials the drum-to-drum uniformity of the mixing is an important factor, particularly ifthe material is to be repackaged into small cartridges. Hence, if samples are taken from three or more separate drums or bags ofa given lot a composite sample is not prepared but one col

43、umn is run from each container sampled. Where the sequence of fillingis known such samples should include the first and the last container filled.9. Procedure9.1 Weigh 270 6 1 g of the moist, as received, mixed bed ion exchange material, and record weight to the nearest 0.1 g.Introduce through the b

44、ackwash line about 25 mm of water to the column. Place about 25 mL of the sample in a large-stemmedplastic funnel inserted in the top of the column. Wash the portion of sample into the column with a minimum of water. Repeat untilall the sample is transferred into the column. Care must be exercised t

45、hat no stratification takes place during the filling procedure.Maintain the water level in the column about 10 mm over the bed level to minimize air trapping.9.2 When all the mixed bed ion exchange material has been transferred slowly introduce test water D at the top of the column.Increase the flow

46、 rate to 100 mL/min, adjusting the rate as required with a flow regulator in the effluent line.9.3 Measure and record the effluent conductivity according to Test Methods D1125 every 2 L. Continue until the 1.0S/cmmhos/cm value is passed, then record readings for each 500 mL of effluent until two suc

47、cessive readings greater than 50S/cm (20 000 50 S/cm (20 000 cm) are obtained.9.4 When the effluent conductivity exceeds 1.0 S/cm (1 Mcm), measure the pH of the effluent according to Test MethodsD1293. Continue the pH measurements at the same frequency as the conductivity measurements.9.5 When the c

48、onductivity exceeds 50 S/cm (20 000 cm), has exceeded 50 S/cm (20 000 cm) on two successivereadings, stop the flow of test water and record the total volume (V) of test water used in litres.9.6 Open the backwash valves and backwash the bed with water for 10 min at a flow rate sufficient to maintain

49、a 50 % expansionof the bed. Stop the flow of water and allow the bed to settle. Drain at the rate of 100 mL/min until the water level is 20 to 30mm above the bed. Do not jar. Record the bed volume in millilitres. Repeat the backwash and drain procedure until two successivereadings of the resettled bed volume agree within 5 mL. Record the average volume as S mL.10. Calculation10.1 The operating capacity may be calculated on either a volume or wet weight basis using a conductivity end point.10.2 Calculate the operating capacity to the conductivit