1、Designation: D 5217 91 (Reapproved 2004)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 (e) 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
3、of 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 e
4、valuations 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
5、applica-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 Excha
6、nge 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 Capac
7、ity of ParticulateMixed Bed Ion Exchange 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 the Atomic Absorption MethodD 5042 Test Methods for Estimating the Organic Fouling ofPar
8、ticulate Anion Exchange ResinsE 830 Test Method for Ash in the Analysis Sample ofRefuse-Derived Fuel3. Terminology3.1 DefinitionsFor 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 mate
9、rial in oron 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, mishand
10、ling, or the 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 obtaini
11、ng representative 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 ma
12、terial (slime), 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
13、 under the jurisdiction of ASTM Committee D19 on Water and isthe direct responsibility of Subcommittee D19.08 on Membranes and Ion ExchangeMaterials.Current edition approved June 1, 2004. Published June 2004. Originallyapproved in 1991. Last previous edition approved in 1998 as D 5217 91 (1998).2For
14、 referenced ASTM 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
15、, West Conshohocken, 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 expecte
16、d forthe resin 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 rat
17、e to give optimiumseparation, 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
18、-ash resins.9.2 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 tech
19、niques aswould 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
20、degree of organic 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 colorles
21、s foulants such 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 Testin
22、g12.1 The evaluation 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 ElectricityGenerati
23、ng Board3and 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 Kineti
24、c Testing: An 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 app
25、earance Unusual 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 decros
26、slinkingLower 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
27、 Poor separation 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 o
28、f anion resins 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 (2004)2APP
29、ENDIXES(Nonmandatory 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 water
30、Humic or fulvic 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.Detergen
31、ts, ABS/LAS, 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, c
32、lay, turbidity (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 (
33、no air)Corrosion 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 sulf
34、ate precipitateChlorine, ozone, oxidationPhysical/Radiological:High operating water temperatureRadiation (less than 1 r/day)Osmotic regeneration shocksAir mixing in mixed beds/oxidation of cation resinsX1.2 Warning: Treatments used on potable water produc-tion systems must meet all applicable safety
35、 and healthregulations.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 o
36、f filter operationBetter 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/coagulat
37、ion/caustic-salt treatmentsImprove underdrain collectorReduce dosage of aidsCoagulation/filtration pretreatmentCoagulation/filtrationReduce temperature, sodium hydroxide strength, step regenerationAeration/filtration, with or without coagulationAeration/coagulation/filtrationBrine regeneration with
38、reducing agentsUse 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 radiat
39、ion versus resin 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
40、 Warning: Treatments 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
41、soak isrecommended.X2.3.4 Always backwash thoroughly after treatment, for atleast 30 min.X2.3.5 For softener after acid treatments, always brinetwice.5Crits, G. J., “The Prevention of Organics and Other Foulants in Ion ExchangeResins,” 24th Annual Liberty Bell Corrosion Course, April 1986.6Crits, G.
42、 J., “Resin Cleaning Methods and Are They Effective,” 24th AnnualLiberty Bell Corrosion Course, April, 1986.D 5217 91 (2004)3X2.4 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 the org
43、anics orcolor.Equipment 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
44、, or oxalic acid per 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
45、1.2 oz. sodium hypochloritesolution (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. App
46、ly 0.5 to 1 mg/L chlorine (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
47、 surfactantAir lanceAir 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 ac
48、id or weakacid cationOrganic 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 magnesiu
49、m, apply 3 % HClFor 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 dropsbe
