1、Designation: D 5256 05 (Reapproved 2009)An American National StandardStandard Test Method forRelative Efficacy of Dynamic Solvent Systems forDissolving Water-Formed Deposits1This standard is issued under the fixed designation D 5256; the number immediately following the designation indicates the yea
2、r oforiginal adoption or, in the 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 relati
3、veefficacy of dynamic solvent systems for dissolving water-formed deposits that have been removed from the underlyingmaterial or deposits attached to the underlying material.1.2 The nature of this test method is such that statements ofprecision and bias as determined by round robin tests couldmislea
4、d users of this test method (see Sections 11 and 12).Therefore, no precision and bias statements are made.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concern
5、s, 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 regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 887 Practices for Sampling Water-Formed
6、DepositsD 1129 Terminology Relating to WaterD 1193 Specification for Reagent WaterD 2331 Practices for Preparation and Preliminary Testing ofWater-Formed DepositsD 2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD 3263 Test Methods for Corrosi
7、vity of Solvent Systemsfor Removing Water-Formed Deposits3D 3483 Test Methods for Accumulated Deposition in aSteam Generator Tube3. Terminology3.1 Definitions:3.1.1 water-formed depositsany accumulation of in-soluble material derived from water or formed by the reactionof water upon the surface in c
8、ontact with the water.3.1.1.1 DiscussionDeposits formed from or by water inall its phases may be further classified as scale, sludge,corrosion products, or biological deposits. The overall compo-sition of a deposit or some part of a deposit may be determinedby chemical or spectrographic analysis; th
9、e constituents actu-ally present as chemical substances may be identified bymicroscope or x-ray diffraction studies. Organisms may beidentified by microscopical or biological methods.3.1.2 For definitions of other terms used in this test method,refer to Terminology D 1129.3.2 Definitions of Terms Sp
10、ecific to This Standard:3.2.1 dynamic solvent systemany closed loop system inwhich the solvent is in motion across the deposit surface.3.2.2 single and multiple solvent systemsa single solventsystem is a one-solution treatment.Amultiple solvent system isa treatment using two or more solutions in seq
11、uence.3.2.3 solvent systemspecified chemicals or combinationof chemicals, that may include corrosion inhibitors, formulatedto react with and remove deposits.4. Summary of Test Method4.1 This test method consists of determining the ability of adynamic solvent system to dissolve deposits.1This test me
12、thod is under the jurisdiction of ASTM Committee D19 on Waterand is the direct responsibility of Subcommittee D19.03 on Sampling Water andWater-Formed Deposits, Analysis of Water for Power Generation and Process Use,On-Line Water Analysis, and Surveillance of Water.Current edition approved May 1, 20
13、09. Published June 2009. Originallyapproved 1992. Last previous edition approved in 2005 as D 5256 05.2For 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
14、Document Summary page onthe ASTM website.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4.2 For the unattached deposits, this test method
15、 consists ofexposing weighed amounts of deposit to the dynamic solventsystems and determining the weight loss of the exposeddeposit, thereby determining the efficacy of the solvent system.4.3 For the attached deposits, the amount and time requiredto yield a constant amount of certain loss of interes
16、t and theamount of deposit not removed determines the relative efficacyof the dynamic solvent system.5. Significance and Use5.1 This test method is useful because the choice of asolvent system for removing water-formed deposits dependsupon the ability of the dynamic solvent system to dissolve bothun
17、attached and attached deposits.6. Apparatus6.1 Common Equipment:NOTE 1The equipment listed in this section is basic and serves thefunction of this test method. This basic test procedure could be modifiedto meet the specific needs of a particular investigation. The test apparatus,however, must be ide
18、ntified and reported with the results. For comparativetype tests, as described in the procedure, it is important that all tests be runin an identical manner.6.2 Unattached Deposit Removal (See Fig. 1 and Fig. 2):6.2.1 Balance, capable of weighing to the nearest 0.1 mg.6.2.2 Heating Bath, thermostati
19、cally controlled to 61C.6.2.3 Stirrer, controlled agitation.6.2.4 Temperature Indicator.6.2.5 Reaction Flask, stirred tests are best accomplished inround bottom flasks.6.2.6 Condenser.6.2.7 Glass Filter Crucibles, Gooch 30-mL low form coursefritted disc crucibles.6.2.8 Vacuum Oven, for drying residu
20、al deposits.6.2.9 Desiccator.6.3 Attached Deposit Removal (See Fig. 3):6.3.1 Solvent Heater/Solvent Reservoir.6.3.2 Sample Holder.6.3.3 Flow Controller.6.3.4 Sample System (usually with cooler).6.3.5 Pressure Relief.6.3.6 Pump.6.3.7 Flow Meter.6.3.8 Temperature Controller.A: Condenser, B: Temperatur
21、e Measurement, C: Stirrer, D: Heated ReactionFlaskFIG. 1 Low Temperature Test EquipmentA: Stirrer, B: Pressure Control (Gauge, Vent and Relief), C: Temperature Mea-surement, D: Temperature Control, E: Heated AutoclaveFIG. 2 High Temperature Test EquipmentA: High Point Pressure Relief, B: Pressure Ga
22、uge, C: Vent, D: Solvent AdditionValve, E: Temperature Measurement, F: Flow Measurement, G: Tube SampleHolder, H: Variable Speed Pump, I: Sample Valve With Integral Cooler, J: Regu-lated Heat SourceFIG. 3 Dynamic Test EquipmentD 5256 05 (2009)27. Reagents7.1 Purity of ReagentsAll solvent materials s
23、uch as acids,inhibitors, and other additives shall be of the grade normallyemployed in chemical cleaning practices for the removal ofwater-formed deposits. Unless otherwise indicated, it is in-tended that all chemicals shall conform to the specifications ofthe Committee onAnalytical Reagents of theA
24、merican Chemi-cal Society,4where such specifications are available.7.2 Purity of WaterUnless otherwise indicated referencesto water shall be understood to mean reagent water conformingto Type IV of Specification D 1193.8. Sampling8.1 Collect and preserve the sample in accordance withPractices D 887
25、(see Note 2).NOTE 2If Method A of Test Methods D 3483 is being used, thedeposit removed in that test can be used in this test method.8.2 Collect and preserve the sample(s) obtained during thecleaning of attached deposit sample.9. Procedure9.1 Prepare a water solution of the solvent systems to betest
26、ed using a weight percentage basis for the acid or otheractive material including any additives. Add only inhibitorssupplied in liquid form on a volume basis as prescribed by themanufacturer.9.2 Unattached Deposits:9.2.1 Preparation of Sample:9.2.1.1 Preliminary ExaminationExamine the sample ascolle
27、cted, using a microscope if available, for structure, color,odor, oil matter, appearance of mother liquor if any, and othercharacteristics of note (for example, attraction to magnet).Record the results for future reference. Further informationabout examination and documentation of the nature of depo
28、sitscan be found in Practices D 2331.(1) Filtration and other steps in the preparation of thesample may frequently be bypassed; for example, a moistsample that contains no separated water or an apparent drysample shall be started in accordance with 9.2.1.3(1), and a drysample shall be started in acc
29、ordance with 9.2.1.4.9.2.1.2 Filtration of SampleIf the sample includes anappreciable quantity of separated water, remove the solidmaterial by filtration. Save the filtrate, undiluted, pendingdecision as to whether or not its chemical examination isrequired. Transfer all of the solid sample to the f
30、ilter, using thefiltrate to rinse the sample container if necessary. Air-drying orpartial air-drying of the filter is frequently helpful towardeffecting a clean separation of the deposit.9.2.1.3 Sample DryingRemove the drained solid samplefrom the filter, being careful to avoid gross contamination w
31、ithfilter paper. Spread the entire quantity of sample in a thin layeron a nonreactive, impervious surface.(1) Oven DryingDry the sample using a vacuum oven ata temperature that will not degrade the deposit. A commonchoice is 52C (125F) and 34 kPa (absolute) (20 in. ofmercury). Place the sample in a
32、desiccator and allow it to coolto room temperature. Weigh the sample to the nearest 0.01 g.Repeat until constant weight is obtained.Arecord of the weightloss during drying is often used.(2) Air DryingAir dry the entire quantity of solid, spreadit in a thin layer on a nonreactive impervious surface.
33、A recordof the loss of weight during air drying is often used.9.2.1.4 Choose a representative portion of the dried samplefor testing.9.2.2 Pour a measured volume of the test solvent (see 9.1)into the chosen test apparatus (see Section 6).9.2.2.1 The weighed deposit can be added to the solventprior t
34、o heating the solvent; however, a controlled and reportedtemperature must be maintained so that the results betweentests can be readily compared.9.2.3 Heat the solvent to the test temperature while stirringat the specified RPM (see Note 3).NOTE 3A stir rate of 60 to 90 RPM is commonly used.9.2.4 Tak
35、e a portion of the deposit (see 9.2.1), weigh to thenearest 0.01 g and record an original deposit weight. Thedeposit weight should meet a solvent volume/deposit weightratio for this specified application (see Note 4).NOTE 4A solvent volume/deposit weight ratio of 100 mL solvent/1 gdeposit is commonl
36、y used.9.2.5 After the solvent has stabilized at the test temperature,draw a sample for analysis, then add the deposit to the solvent.This is considered as “time zero.”9.2.6 If required, samples can be drawn at periodic timeintervals. Maintain strict control of all sample weights (tonearest 0.01 g).
37、9.2.7 At the termination of the test, cool and filter thesolvent.9.2.7.1 Weigh a clean, dry filter crucible to the nearest0.01 g. Record the weight as original crucible weight.9.2.7.2 Filter the solvent-deposit mixture through theweighed filter crucible. Vacuum filtration increases the filtra-tion r
38、ate.9.2.7.3 Rinse the filter crucible and residual deposit withwater.9.2.7.4 Dry the crucible and residual deposit in the vacuumoven. Choose a temperature and vacuum that will not degradethe residual deposit. A common choice is 52C (125F) and 34kPa (absolute) (20 in. of mercury).9.2.7.5 Place the dr
39、ied crucible and residue in the desiccatorand allow them to cool to room temperature.9.2.7.6 Weigh the crucible plus residue to the nearest 0.01 g.9.2.7.7 Repeat 9.2.7.4 to 9.2.7.6 until a constant weight isobtained. Record this weight as the final crucible weight.9.3 Attached Deposit (Comparative T
40、ests):9.3.1 Establish accumulated deposition in accordance withTest Methods D 3483 on a portion of the sample adjacent toand representative of the section to be tested below. Further4Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For Suggestio
41、ns on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D 5256 05 (2009)3information about
42、 examination and documentation of thenature of deposits can be found in Practices D 2331.9.3.2 The ratio of the weight of attached deposit on the testspecimen to test apparatus volume must be recorded andshould be appropriate for the application (see Note 5).NOTE 5Due to the constraints imposed by t
43、he solvent circulationsystem, the solvent volume/deposit weight ratio on attached deposits isoften larger than desired. This excess capacity can be partially compen-sated by reducing the concentration of the active components of thesolvent. However, in all cases the actual cleaning operation should
44、bedesigned and controlled according to the accepted practice for theparticular solvent system being applied and not according to the valuesgenerated by this test method.9.3.3 Use a measured volume of test solvent to fill the testapparatus.9.3.4 Establish solvent flow in the test apparatus. Thesolven
45、t flow should bypass the test specimen until the properflow rate, system pressure, and solvent temperature is reached.9.3.4.1 Establish and record the solvent flow rate based onthe cross section area of the test specimen.9.3.5 Heat the solvent to the appropriate test temperature.After the solvent te
46、mperature and flow rate have stabilized,draw a sample for analysis.9.3.6 Establish flow through the test specimen. This isconsidered as “time zero.”9.3.7 Monitor and record flow rate, pressure and tempera-ture during the test interval.9.3.8 Draw samples at periodic time intervals and analyzefor ions
47、 of choices.9.3.9 If necessary, use intermediate visual examinations todetermine cleaning efficacy.9.3.10 At the completion of the test period, determined by9.3.8 and 9.3.9, determine the remaining deposit accumulationaccording to Test Methods D 3483 (see Note 6). This value aswell as the time requi
48、red to achieve the level of cleanliness isused as the relative measure of cleaning efficacy for attacheddeposit.NOTE 6Since the remaining deposit may be acid insoluble, thepreferred method is Method A of Test Methods D 3483.10. Calculation10.1 Unattached Deposits:10.1.1 Determine the amount of depos
49、it that was dissolvedby subtracting the amount not dissolved (see 9.2.7) from theoriginal deposit weight (see 9.2.4).10.1.2 Express the efficacy of the solvent system as thepercent deposit dissolved, by dividing the amount dissolved(see 10.1.1) by the original amount (see 9.2.4) and convertingthe resultant decimal to a percentage.10.1.3 Use the following formula to calculate solvent effi-cacy:SE 5OS 2 FS!OS3 100 (1)where:SE = solvent efficacy,OS = original deposit weight, g, andFS = final deposit residue weight, g.10.2 For Attached Deposits:10.2.1 Determine
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