1、Designation: D 6301 03Standard Practice forthe Collection of Samples of Filterable and NonfilterableMatter in Water1This standard is issued under the fixed designation D 6301; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the yea
2、r 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 practice is applicable for sampling condensedsteam or water, such as boiler feedwater, for the collection o
3、ffilterable and (optional) nonfilterable matter using 0.45-mmembrane filter (filterable matter) and ion exchange media(nonfilterable matter). As the major filterable containmentfound in most boiler feedwaters is some form of corrosionproduct from the preboiler system, the device used for thispractic
4、e is commonly called a corrosion product sampler.1.2 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 re
5、gulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1066 Practice for Sampling SteamD 1129 Terminology Relating to WaterD 1192 Guide for Equipment for Sampling Water andSteam in Closed ConduitsD 1193 Specification for Reagent WaterD 1971 Practices for Digestion of Water Sa
6、mples for De-termination of Metals by Flame Atomic Absorption,Graphite Furnace Atomic Absorption, Plasma EmissionSpectroscopy, or Plasma Mass SpectrometryD 2332 Practice for Analysis of Water-Formed Deposits byWavelength-Dispersive X-Ray FluorescenceD 2777 Practice for Determination of Precision and
7、 Bias ofApplicable Methods of Committee D19 on WaterD 3370 Practice for Sampling Water from Closed ConduitsD 3864 Guide for Continual On-Line Monitoring Systemsfor Water Analysis3. Terminology3.1 DefinitionsFor definitions of terms used in this prac-tice, refer to Terminology D 1129.3.2 Definitions
8、of Terms Specific to This Standard:3.2.1 corrosion product sampler, na device used to col-lect integrated samples of filterable and (as an option) nonfil-terable matter. It consists of a flow totalizer that accuratelymeasures the amount of sample passing through the device anda 0.45-m pore size memb
9、rane filter. Adding a second filter forion exchange resin impregnated membranes allows for collect-ing nonfilterable matter.3.2.2 filterable matter, nincludes all matter that is re-moved by a 0.45-m pore size filter.3.2.3 nonfilterable matter, nincludes all matter that willpass through a 0.45-m pore
10、 size filter and may be captured onanion, or cation ion exchange membranes, or both.4. Summary of Practice4.1 A typical sampling apparatus, or corrosion productsampler, is used to obtain integrated, representative samples offilterable and nonfilterable matter using a 0.45-m membranefilter and ion ex
11、change membranes. The sampling is accom-plished at system operating pressure or after pressure reduc-tion, and sample temperature of#50C. The practice utilizes amodified stainless steel high pressure filter housing to accom-modate a 47-mm diameter filter (for filterable matter) and ifdesired, ion ex
12、change membranes (for nonfilterable matter).The sample collection system (corrosion product sampler) isdesigned and operated specifically for quantitative collection offilterable and nonfilterable matter. An important feature of thesampler is the flow totalizer, which accurately determines thetotal
13、volume of sample that has passed through the sampler,regardless of changes in flowrate or pressure during thecollection period. Control and pressure reducing valves andmetering devices are downstream of the filter housing toeliminate the possible contribution of filterable and nonfilter-able matter
14、from these components to the sample stream.Additional flow may bypass the filter housing, so that flowswithin the sample lines are maintained within required range1This practice is under the jurisdiction of ASTM Committee D19 on Water andis the direct responsibility of Subcommittee D19.03 on Samplin
15、g of Water andWater-formed Deposits, Analysis of Water for Power Generation and Process Use,On-Line Water Analysis, and Surveillance of Water.Current edition approved Aug. 10, 2003. Published September 2003. Originallyapproved in 1998. Last previous edition approved in 1998 as D 6301 98.2For referen
16、ced 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, West C
17、onshohocken, PA 19428-2959, United States.FIG. 1 Simplified Flow Diagram for Corrosion Product SamplerD6301032(see Guide D 3864). If a single sampling point is not represen-tative due to lack of homogeneity in the process fluid (the waterbeing sampled), multiple point sampling may be required.5. Sig
18、nificance and Use5.1 The transport of any filterable matter or corrosionproducts from the preboiler cycle has been shown to bedetrimental to all types of steam generating equipment. Cor-rosion product transport as low as 10 ppb can have significantimpact on steam generators performance.5.2 Deposited
19、 corrosion products on PWR steam generatortubes can reduce heat transfer, and, if the deposit is sufficientlythick, can provide a local area for impurities in the bulk waterto concentrate, resulting in a corrosive environment. In BWRplants, the transport of corrosion products can cause fuelfailure,
20、out of core radiation problems from activation reac-tions, and other material related problems.5.3 In fossil plants, the transport of corrosion products canreduce heat transfer in the boilers leading to tube failures fromoverheating. The removal of these corrosion products bychemical cleaning is exp
21、ensive and potentially harmful to theboiler tubes.5.4 Normally, grab samples are not sensitive enough todetect changes in the level of corrosion product transport.Also,system transients may be missed by only taking grab samples.An integrated sample over time will increase the sensitivity fordetectin
22、g the corrosion products and provide a better under-standing of the total corrosion product transport to steamgenerators.6. Interferences6.1 The ion exchange capacity may be exceeded if anexcessive volume of sample is passed through the ion exchangemedia.6.2 The removal efficiency of the ion exchang
23、e media isflowrate and matrix dependent and could show variations fromlot to lot.6.3 Sample temperature greater than 50C may have delete-rious effects on the ion exchange media.6.4 The corrosion products collected on the 0.45-m filtermay be loose so care should be taken to prevent loss of sample.6.5
24、 Due to settling, or deposition, or both, in sampling lineswith low velocity, flow in sampling lines must be turbulent andmaintained at a velocity of 1.5 2.1 m/s (57 ft/s) (see alsoGuide D 1192).7. Apparatus7.1 Sample heat exchanger, made of such material that fullsystem pressure can be maintained w
25、ithin the coil, and of suchcapacity that the water being sampled will be cooled to lessthan 50C when the sampling flow rate is established (seeGuide D 1192).7.2 Corrosion Product SamplerSee Fig. 1, SimplifiedFlow Diagram.7.3 Flow TotalizerWater meter that will maintain 6 5%accuracy over full range.8
26、. Reagents and Materials8.1 Reagent WaterReference to reagent water shall beunderstood to mean Type I reagent water conforming to GuideD 1193.8.2 Anion resin impregnated membranes (47-mm diameter),optional.8.3 Cation resin impregnated membranes (47-mm diam-eter), optional.8.4 Membrane Filters, (47-m
27、m diameter), 0.45-m poresize, without grid.8.5 Petri Dishes, large enough to hold the 47-mm filters.9. Calibration9.1 Calibrate the flow totalizer following the manufacturersrecommendation.10. Procedure10.1 If subsequent chemical analysis of collected filterable/nonfilterable material is desired, re
28、cord the lot numbers of theion exchange membranes. Prepare sample blanks from samelot.10.2 Install filter and optional ion exchange membranes infilter holder so that the sample goes through the filter first,taking care to ensure that they are centered. If necessary, use afew drops of water to wet th
29、e membranes to help hold them inplace.NOTE 1If two filter holders are used, the filter membrane shouldprecede the ion exchange membranes in the second holder.10.3 Install top of the filter housing, taking care not todisturb membranes.10.4 With the sample “indicating controller rotameter”closed, slow
30、ly open the sample isolation valve. Take the initialflow totalizer reading.10.5 Slowly increase flow through filter holder to thedesired settings. Select the flow rate not to exceed the capacityof the ion exchange papers, if used (the normal flow range is 80to 200 mL/min).10.6 Collect the sample usi
31、ng Practices D 1066 or D 3370.Maintain flow constant throughout the incoming line andthrough the filter holder.10.7 Slowly isolate and depressurize the corrosion productsampler at the end of the collection period. Record the finaltotalizer reading.10.8 Remove excess water from the filter housing byd
32、raining it or by purging it with a small amount of air (see Fig.1, rubber bulb).10.9 Remove the top of the filter housing, taking care not todisturb collected material.10.10 Remove membranes from filter housing. Use Petridishes to store membranes. Membrane filters, anion ion ex-change membranes, and
33、 cation ion exchange membranesshould be stored in separate Petri dishes.10.11 Analyses of the membrane filters or of the ionexchange membranes may be accomplished by a variety ofmethods following appropriate sample preparation technique,depending on the analytes of interest and the quantity of thesp
34、ecific analyte collected on the 0.45-m pore size filter or onthe resin impregnated membranes. Preparation should beD6301033consistent with the method of analysis. Refer to the specificmethod of analysis for specific guidance and information onpreparation, sample storage, etc. For the usual corrosion
35、products of interest (iron, copper, and zinc collected as eitherfilterable or nonfilterable matter), refer to Practices D 1971. Forelements above atomic weight 11, particularly chlorine andsulfur, contained in anions collected as nonfilterable matter andconcentrated above 0.1%, Practice D 2332 might
36、 be used.11. Calculation11.1 A calculation will be required to make the result of theanalysis of the 0.45-m filter or ion exchange membrane relateto the flow totalizer reading and express a meaningful result.11.2 For example, to express ppb results:ppb of analyte in sample stream = g of analyte on f
37、ilter /total flow in liters.12. Quality Control12.1 The accuracy of the flowmeter and agreement with thetotalizer should be checked by timing a measured quantity ofsample through the sampler. This procedure is repeated peri-odically to check on the operation of the totalizer.12.2 Initially, a blank
38、will be determined on the type of 0.45m filter or the type of ion exchange membrane used, or both,that has gone through the complete handling, installation, andremoval procedures, minus the sample flow, for each analyte ofinterest.12.3 Any additional QC practices required by the method ofanalysis, s
39、uch as Practices D 1971 or Practice D 2332referenced above, if used will be followed.13. Precision and Bias13.1 Practice D 2777 is not applicable to this Practicebecause it includes methodology involving continuous sam-pling.13.2 The precision and bias of the analysis of the filters orion exchange m
40、embranes will be governed by those proceduresused for the individual analytes of interest.14. Keywords14.1 corrosion products; corrosion product sampler; filtra-tion; integrated sample; ion exchange membranesBIBLIOGRAPHY(1) ASTM STP-742, Power Plant Instrumentation for Measurement ofHigh-Purity Wate
41、r Quality(2) Solomon, Y., Ed., Proceedings: Workshop Corrosion ProductSampling from Hot Water Systems, Electric Power Research Insti-tute, Report NP-3402-Sr, March 1984.(3) Berry, W. E. and R. B. Diegle, Survey of Corrosion ProductGeneration, Transport, and Deposition in Light Water Reactors,Electri
42、c Power Research Institute, Report NP-522, March, 1979.(4) Bogert, James R., Jack M. Kibler and Jack K. Schmotzer, “Stan-dardless EDXRF Analysis of Cations in Ion-Exchange Resin-Impregnated Membranes”, Advances in X-Ray Analysis, Vol. 30,Plenum Publishing, 1987.(5) Connolly, D. J. and N. J. Mravich,
43、 “Automated Corrosion ProductSampling and X-Ray Fluorescence Analysis”, 1990 InternationalConference on Measuring Waterborne Trace Substances.(6) Swochika, S. G., S. E. Copely, and W. L. Pearl, Corrosion ProductTransport in PWR Secondary Systems, Electric Power ResearchInstitute, Report NP-2149, Dec
44、ember, 1981.(7) Emory, B. B., “Theoretical Considerations in the Design of CrudSample Systems for Nuclear Power Plants”, NACE Corrosion79-Corrosion Product Sampling Symposium, Atlanta, GA., March,1979.(8) Aschoff, A. F., Y. H. Lee, D. M. Sopocy, O. Jonas, InterimConsensus Guidelines on Fossil Plant
45、Cycle Chemistry, ElectricPower Research Institute, Report CS-4629, June 1986.(9) Tucker, P.A., “Best Practices in Corrosion Product Sampling”,EPRI PWR Chemistry Meeting 1995.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mention
46、edin this standard. Users of this standard are expressly advised 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
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49、C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D6301034
