1、Designation: D 5217 91 (Reapproved 2009)Standard Guide forDetection of Fouling and Degradation of Particulate IonExchange Materials1This standard is issued under the fixed designation D 5217; the number immediately following the designation indicates the year oforiginal adoption or, in the case of r
2、evision, 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 guide presents a series of tests and evaluationsintended to detect fouling and degradation o
3、f particulate ionexchange materials. Suggestions on reducing fouling and oncleaning resins are given.1.2 This guide is to be used only as an aid in the evaluationof particulate ion exchange material performance and does notpurport to address all possible causes of unsatisfactory perfor-mance. The ev
4、aluations of mechanical and operational prob-lems are not addressed.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 a
5、pplica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1129 Terminology Relating to WaterD 1782 Test Methods for Operating Performance of Par-ticulate Cation-Exchange MaterialsD 2187 Test Methods for Physical and Chemical Propertiesof Particulate Ion-Exchan
6、ge ResinsD 2332 Practice for Analysis of Water-Formed Deposits byWavelength-Dispersive X-Ray FluorescenceD 2687 Practices for Sampling Particulate Ion-ExchangeMaterialsD 3087 Test Method for Operating Performance of Anion-Exchange Materials for Strong Acid RemovalD 3375 Test Method for Column Capaci
7、ty of ParticulateMixed Bed IonExchange MaterialsD 3682 Test Method for Major and Minor Elements inCombustion Residues from Coal Utilization ProcessesD 3683 Test Method for Trace Elements in Coal and CokeAsh by Atomic AbsorptionD 5042 Test Method for Estimating the Organic Fouling ofParticulate Anion
8、 Exchange ResinsE 830 Test Method for Ash in the Analysis Sample ofRefuse-Derived Fuel3. Terminology3.1 Definitions: For definitions of terms used in this guide,refer to Terminology D 1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 organic foulingthe buildup of organic material in oron
9、 anion exchange resins by sorption during the service cycleand incomplete removal during normal regeneration.4. Significance and Use4.1 Resins used in demineralization systems may deterioratedue to many factors including chemical attack, fouling byorganic and inorganic materials, mishandling, or the
10、 effects ofaging. Detection of degradation or fouling may be important indetermining the cause of poor demineralizer performance.5. Sampling5.1 Follow the recommendations of Practices D 2687 forobtaining samples of particulate ion exchange materials. Coresamples are important for obtaining represent
11、ative samples;however, special problems may dictate other sampling require-ments, such as surface, interface, or other samples.6. Preliminary Examination6.1 Examine the sample visually or with the aid of amagnifier for any abnormalities. Note any unusual color,precipitates, biological material (slim
12、e), particulate matter, orsmall pieces or fragments of resin. Note that the color of resinmay vary from lot to lot or with normal use and would not beconsidered unusual.6.2 Note any peculiar odor associated with the sample, suchas from oil, solvents, or biological activity.1This guide is under the j
13、urisdiction of ASTM Committee D19 on Water and isthe direct responsibility of Subcommittee D19.08 on Membranes and Ion ExchangeMaterials.Current edition approved May 1, 2009. Published June 2009. Originallyapproved in 1991. Last previous edition approved in 2004 as D 5217 91 (2004).2For referenced A
14、STM standards, visit the 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 Consho
15、hocken, PA 19428-2959, United States.7. Moisture and Particule Size Distribution7.1 Follow procedures given in Test Methods D 2187,MethodsA, B, and D for determining moisture (water retentioncapacity) and particle size distribution.7.2 Compare the values obtained in 7.1 to those expected forthe resi
16、n when in good condition. It is preferred that new resin,treated in the same way, be used for this comparison, butmanufacturers specifications can also be used.8. Mixed-Bed Resin Separation8.1 Observe resin during separation according to Test Meth-ods D 2187, MethodA.Adjust backwash rate to give opt
17、imiumseparation, then let resin settle and observe interface and notedegree of cross-mixing.9. Ash Content and Metals Analysis9.1 Follow the procedure given in Test Method E 830 fordetermining the ash content of the pretreated and dried sample.A larger sample portion may be used for low-ash resins.9
18、.2 Analyze the ash for silica or metals such as iron, copper,manganese, barium, aluminum, calcium, magnesium, or otherswhich might be suspected as contaminants. Use X-ray fluores-cence analysis to determine major elements (see PracticeD 2332). Employ digestion, fusion, and analysis techniques aswoul
19、d be used for other types of ash. (See Test MethodsD 3682 and D 3683.) Note that some elements may be lostduring the 575C ashing, and spike recoveries must bechecked.10. Detection of Organic Fouling of Anion Resins10.1 Follow procedures given in Test Methods D 5042 forestimation of the degree of org
20、anic fouling of anion resins.10.2 For a more rapid, but less reliable evaluation of theresin, the caustic-brine extract from Test Methods D 5042 maybe judged by color rather than by total organic carbonmeasurement: the darker the color, the heavier the organicfouling. Note that colorless foulants su
21、ch as detergents orsynthetic polyelectrolytes will not be detected.11. Column Performance Testing11.1 Follow procedures given in Test Methods D 3375,D 3087, or D 1782 as needed to evaluate the performance ofmixed bed, anion, or cation exchange materials, respectively.12. Kinetics Testing12.1 The eva
22、luation of the kinetics properties of ion-exchange resins is especially important for anion resins used inhigh flow rate applications such as condensate polishing.12.2 Test the resins kinetics properties according to pub-lished procedures such as those by the Central ElectricityGenerating Board3and
23、Rohm fouling; ion exchange; kinetics; resin3Harris, R. R., “Anion Exchange Kinetics in Condensate Purification MixedBeds-Assessment and Performance Prediction,” Proceedings of EPRI CondensatePolishing Workshop, October 1985, pp. 3140.4McNulty, J. T., et al., “Anion Exchange Resin Kinetic Testing: An
24、 Indispens-able Diagnostic Tool for Condensate Polisher Troubleshooting,” Proceedings ofInternational Water Conference, October, 1986.TABLE 1 Detection of Fouling and Degradation of Particulate Ion Exchange MaterialsSectionNo.Property Tested Test Results Possible Indications6 Visual appearance Unusu
25、al color or precipitates Coating on beads from foulants or improper regenerationPieces/fragments present Physical degradation6 Odor Unusual odor Fouling of resin by oil, solvents, etc. or biological activity7 Moisture Higher than expected (10 % above) Degradation of resin causing decrosslinkingLower
26、 than expected Fouling of resin by heavy materials, such as metal oxides7 Particle size distribution Smaller sizes than expected Physical degradation or non-representative sampleLarger sizes than expected Loss of smaller beads by backwash or through strainers8 Mixed bed resin separation Poor separat
27、ion Ionic form of resin may not be correctResin may be fouledParticle size distribution of beads may be incorrect9 Ash content and metals Higher than expected Fouling of resin by expected metal oxides or silica (from corrosion products,influent water, or regenerants)10 Organic fouling of anion resin
28、s Moderate to severe Presence of sufficient organic fouling to affect performance11 Column performance Poorer than expected Degradation or fouling sufficient to affect performance12 Kinetics Poorer than expected Degradation or fouling sufficient to affect performanceD 5217 91 (2009)2APPENDIXES(Nonma
29、ndatory Information)X1. METHODS FOR PREVENTING OR REDUCING FOULANTS TO ION EXCHANGE RESINS5X1.1 These are only suggested treatments; the resin sup-plier should be consulted before any new treatment process isused.Suspected Contaminant or Foulant OrganicsHumic or fulvic solubles in waterHumic or fulv
30、ic leakage from pretreatment-coagulation or organic trapsColloidal color from influent waterCation degradation productsOil, soluble or greaseOrganic or vegetable fibersFilter media, celite/siliceousFilter media, cellulose (solka floc)Micro-organisms, algae, bacteria, slime, etc.Detergents, ABS/LAS,
31、anionicDetergents, cationicAir-borne dusts, micro-organismsSolvents/detergents from new resinsAmines from anion resinsSloughage from aged exhausted activated carbonOrganic leakage from weak/Type IIResin leakage, fines or beadsPolyelectrolytes/coagulation aidsMetals or Non-Metals:Silt, clay, turbidit
32、y (colloidal)Colloidal silica (insoluble)Silica gelation (due to high soluble silica and strong caustic)Manganese on cation resin with HCl regeneration causing oxidative attack bychlorineIron, soluble or insoluble, influent (greater than 0.5 mg/L per 24-h run)Iron, soluble, to 30 mg/L (no air)Corros
33、ion products, iron, copper, etc., in cation water or regeneration dilutionwaterIron in caustic, above 10 mg/L (50 % sodium hydroxide basis)Sulfur precipitate, above 0.5 mg/L per 24-h runAluminum floc/aluminum precipitation (above 0.3 mg/L per 24 h)Barium, strontium, calcium forming sulfate precipita
34、teChlorine, ozone, oxidationPhysical/Radiological:High operating water temperatureRadiation (less than 1 r/day)Osmotic regeneration shocksAir mixing in mixed beds/oxidation of cation resinsX1.2 WarningTreatments used on potable water produc-tion systems must meet all applicable safety and healthregu
35、lations.Possible Pretreatment or Method to Reduce FoulingCoagulation, lime softening, organic trapsActivated carbon, caustic/salt treatmentCoagulation, lime softening, ultra filterRinse new resins, sulfite/SO2feedsPretreatment, coagulation, filterCoagulation and filterBetter control of filter operat
36、ionBetter control of filter operation (add another filter)Chlorine/coagulation/filtrationActivated carbon, foam fractionationActivated carbonAdd filter to air blowers/compressorsWarm rinse or brine acid treatment, or bothWarm rinseRenew carbon, caustic-salt treatmentsPretreat/coagulation/caustic-sal
37、t treatmentsImprove underdrain collectorReduce dosage of aidsCoagulation/filtration pretreatmentCoagulation/filtrationReduce temperature, sodium hydroxide strength, step regenerationAeration/filtration, with or without coagulationAeration/coagulation/filtrationBrine regeneration with reducing agents
38、Use plastic materials, stainless steelEvaluate resin replacement versus sodium hydroxideAeration and filter, with or without coagulationHigh rate polishing filterLime softening pretreatmentActivated carbon, sulfite/SO2feedEvaluate temperature reduction versus resin costEvaluate radiation versus resi
39、n replacementReduce regenerant strengths, limit exchange capacityRestrict air mixing time to minimumX2. CLEANING AGENTS AND PROCEDURES FOR ION EXCHANGE RESINS6X2.1 These are only suggested treatments; the resin sup-plier should be consulted before any new treatment process isused.X2.2 WarningTreatme
40、nts used on potable water produc-tion systems must meet all applicable safety and healthregulations.X2.3 Procedures:X2.3.1 Brine at least 8 lb/ft3(at 12 to 15 %).X2.3.2 Air scourat minimum 4 ft3/min/ft2with minimum24 in. water above bedX2.3.3 Air lance (at 4 ft3/min/ft2) along with soak isrecommende
41、d.X2.3.4 Always backwash thoroughly after treatment, for atleast 30 min.X2.3.5 For softener after acid treatments, always brinetwice.X2.4 These cyclic caustic/salt applications should be per-formed at regular intervals such as each week, month, and soforth, to prevent the fixing or polymerization of
42、 the organics orcolor.5Crits, G. J., “The Prevention of Organics and Other Foulants in Ion ExchangeResins,” 24th Annual Liberty Bell Corrosion Course, April 1986.6Crits, G. J., “Resin Cleaning Methods and Are They Effective,” 24th AnnualLiberty Bell Corrosion Course, April 1986.D 5217 91 (2009)3Equi
43、pment System Type Resin Suspected Contaminants Possible Cleaning Agents and ProceduresSoftener Strong acid cation Iron, manganese Brine, 8 lb/ft3Air scourBrine with 1 lb, sodium hydrosulfite, soak 2 hSoftener Strong acid cation Iron, manganese BrineAir scour2 lb sulfamic, or citric, or oxalic acid p
44、er ft3at 2.5 %Air lance, soak for 2 to 4 hSoftener Strong acid cation Iron, manganese, silica gels,aluminum flocBrineAir scourCaustic, 2 lb/ft3at2to4%Air lance, soak 2 hSoftener Strong acid cation Slime, iron chrenothrix algae,etc.H + Bedsmust brine firstAir scourBrine with 0.8 to 1.2 oz. sodium hyp
45、ochloritesolution (5 %)/ft3Soak 2 h, air lanceSoftener/Demineralizer/Mixed BedStrong acid cation Slime, bacteria, algae,etc.Brine, 8 lb/ft3Formaldehyde, peracetic, or H2O2at14 to12 %, soak 3 hor moreAir lanceSoftener/Demineralizer Strong acid cation Slime, bacteria, algae, etc. Apply 0.5 to 1 mg/L c
46、hlorine (on line feed) sodium hypochlorite-solutionfor2to5h(also,I2,O3,H2O2, hot 70C watermay be used)Softener/Demineralizer/De-alkalizerStrong acid or cation anionresinOil, fibers, sulfur, algae or-ganicsBrine (to remove acid and hardness)Caustic, 2 lb/ft3(1 to 3 %) with non-ionic surfactantAir lan
47、ceAir scourSoftener/Demineralizer/De-alkalizerStrong acid or weakacid cationCalcium sulfate, iron HCl, 2 to 3 gal. of 30 %/ft3(add extra acid for conversionof resin to H + form); equipment must be HCl corrosion proofSoftener/Demineralizer/De-alkalizer (Problemswithout oil)Strong acid or weakacid cat
48、ionOrganic fibers, cellulose filtermediaAir scourBrine with or without 0.05 to 0.1 % detergent (non-ionicsurfactant)Air lanceDemineralizer/Organic trap/De-alkalizerStrong or weak base anion Iron, calcium, magnesium Exhaust and brineA2 gal of 30 % HCl per ft3For calcium and magnesium, apply 3 % HClFo
49、r iron, apply 15 % HClFlow slowly for 2 hDemineralizer/Organic trap Strong base anion Silica precipitates or gels Regenerate with normal sodium hydroxide, air scour or lanceApply extra 2 lb sodium hydroxide/ft3at 2 to 4 % and air lancefor 1 hRinse, backwash, and regenerate againDemineralizer/Organic trap Strong base anionType 1Organics, color, foulants Cyclic caustic/saltSodium hydroxide (warm 150F) 2 lb/Cu. at 3 %. Displacewith water, 10min. salt (warm), 6 to 8 lb/ft3at 12 %.Displace with water, 10 min. Repeat 3 times or until color ineffluent dropsbelow 20 % of the
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