1、Designation: D6301 13Standard Practice forCollection of On-Line Composite Samples of SuspendedSolids and Ionic Solids in Process Water1This standard is issued under the fixed designation D6301; the number immediately following the designation indicates the year oforiginal adoption or, in the case of
2、 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 practice is applicable for sampling condensedsteam or water, such as boiler feedwater, for
3、 the collection ofsuspended solids and (optional) ionic solids using a 0.45-mmembrane filter (suspended solids) and ion exchange media(ionic solids). As the major suspended component found inmost boiler feedwaters is some form of corrosion product fromthe preboiler system, the device used for this p
4、ractice iscommonly called a corrosion product sampler.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is therespons
5、ibility 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:2D1066 Practice for Sampling SteamD1129 Terminology Relating to WaterD1193 Specification for Re
6、agent WaterD1971 Practices for Digestion of Water Samples for Deter-mination of Metals by FlameAtomicAbsorption, GraphiteFurnace Atomic Absorption, Plasma EmissionSpectroscopy, or Plasma Mass SpectrometryD2332 Practice for Analysis of Water-Formed Deposits byWavelength-Dispersive X-Ray FluorescenceD
7、2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD3370 Practices for Sampling Water from Closed ConduitsD3864 Guide for On-Line Monitoring Systems for WaterAnalysis3. Terminology3.1 DefinitionsFor definitions of terms used in thispractice, refe
8、r to Terminology D1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 corrosion product sampler, na device used to collectintegrated samples of suspended solids and (as an option) ionicsolids.3.2.1.1 DiscussionIt consists of a flow totalizer that accu-rately measures the amount of sample p
9、assing through thedevice and a 0.45-m pore size membrane filter. Adding asecond filter for ion exchange resin impregnated membranesallows for collecting ionic solids.3.2.2 ionic solids, nincludes all matter that will passthrough a 0.45-m pore size filter and may be captured onanion, or cation ion ex
10、change membranes, or both.3.2.3 suspended solids, nincludes all matter that is re-moved by a 0.45-m pore size filter.4. Summary of Practice4.1 A typical sampling apparatus, or corrosion productsampler, is used to obtain integrated, representative samples ofsuspended solids and ionic solids using a 0
11、45-m membranefilter and ion exchange membranes. The sampling is accom-plished at system operating pressure or after pressurereduction, and sample temperature of 50C. The practiceutilizes a modified stainless steel high pressure filter housing toaccommodate a 47-mm diameter filter (for suspended sol
12、ids)and if desired, ion exchange membranes (for ionic solids). Thesample collection system (corrosion product sampler) is de-signed and operated specifically for quantitative collection ofsuspended solids and ionic solids. An important feature of thesampler is the flow totalizer, which accurately de
13、termines thetotal 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 suspended solids an
14、dionic solids from these components to the sample stream.1This practice is under the jurisdiction of ASTM Committee D19 on Water andis 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 Ana
15、lysis, and Surveillance of Water.Current edition approved July 15, 2013. Published August 2013. Originallyapproved in 1998. Last previous edition approved in 2008 as D6301 08. DOI:10.1520/D6301-13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service a
16、t serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1FIG. 1 Simplified Flow Diagram for Corrosion Produ
17、ct SamplerD6301 132Additional flow may bypass the filter housing, so that flowswithin the sample lines are maintained within required range(see Guide D3864). If a single sampling point is not represen-tative due to lack of homogeneity in the process fluid (the waterbeing sampled), multiple point sam
18、pling may be required.5. Significance and Use5.1 The transport of any suspended solids 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 generator
19、s performance.5.2 Deposited 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 produ
20、cts can cause fuelfailure, out of core radiation problems from activationreactions, 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 b
21、ychemical cleaning is expensive 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 th
22、e sensitivity fordetecting 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 effi
23、ciency of the ion exchange 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 p
24、revent loss of sample.6.5 Due to settling, or deposition, or both, in sampling lineswith low velocity, flow in sampling lines must be turbulent andmaintained at a velocity of 1.8 m/s (6 ft/s) (see also PracticesD3370).7. Apparatus7.1 Sample heat exchanger, made of such material that fullsystem press
25、ure can be maintained within the coil, and of suchcapacity that the water being sampled will be cooled to lessthan 50C when the sampling flow rate is established (seePractices D3370).7.2 Corrosion Product SamplerSee Fig. 1.7.3 Flow TotalizerWater meter that will maintain 65%accuracy over full range.
26、8. Reagents and Materials8.1 Reagent WaterReferences to water shall be under-stood to mean water that meets or exceeds the quantitativespecifications for Type III reagent water conforming to Speci-fication D1193, Section 1.1.8.2 Anion resin impregnated membranes (47-mm diameter),optional.8.3 Cation
27、resin impregnated membranes (47-mmdiameter), optional.8.4 Membrane Filters, (47-mm 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 subsequen
28、t chemical analysis of collected suspendedsolids/ionic solids is desired, record the lot numbers of the ionexchange membranes. Prepare sample blanks from same lot.10.2 Install filter and optional ion exchange membranes infilter holder so that the sample goes through the filter first,taking care to e
29、nsure that they are centered. If necessary, use afew drops of water to wet the 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
30、 membranes.10.4 With the sample “indicating controller rotameter”closed, slowly 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, i
31、f used (the normal flow range is 80to 200 mL/min).10.6 Collect the sample using Practices D1066 or D3370.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
32、finaltotalizer reading.10.8 Remove excess water from the filter housing bydraining 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.D6301 13310.10 Remove membranes from filter housing. Use
33、Petridishes to store membranes. Membrane filters, anion ion ex-change membranes, and 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 p
34、reparation technique,depending on the analytes of interest and the quantity of thespecific analyte collected on the 0.45-m pore size filter or onthe resin impregnated membranes. Preparation should beconsistent with the method of analysis. Refer to the specificmethod of analysis for specific guidance
35、 and information onpreparation, sample storage, etc. For the usual corrosionproducts of interest (iron, copper, and zinc collected as eithersuspended solids or ionic solids), refer to Practices D1971. Forelements above atomic weight 11, particularly chlorine andsulfur, contained in anions collected
36、as ionic solids andconcentrated above 0.1 %, Practice D2332 might 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 expres
37、s ppb results:ppb of analyte in sample stream5g of analyte on filtertotal flow in litres(1)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 c
38、heck on the operation of the totalizer.12.2 Initially, a blank 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 A
39、ny additional quality control (QC) practices requiredby the method of analysis, such as Practices D1971 or PracticeD2332 referenced above, if used will be followed.13. Precision and Bias13.1 Practice D2777 is not applicable to this practicebecause it includes methodology involving continuous sam-pli
40、ng.13.2 The precision and bias of the analysis of the filters orion exchange membranes 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
41、) ASTM STP-742, Power Plant Instrumentation for Measurement ofHigh-Purity Water Quality(2) Solomon, Y., Ed., Proceedings: Workshop Corrosion Product Sam-pling from Hot Water Systems, Electric Power Research Institute,Report NP-3402-Sr, March 1984.(3) Berry, W. E. and R. B. Diegle, Survey of Corrosio
42、n ProductGeneration, Transport, and Deposition in Light Water Reactors,Electric 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 An
43、alysis , Vol. 30,Plenum Publishing, 1987.(5) Connolly, D. J. and N. J. Mravich, “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 Prod-uct Transpor
44、t in PWR Secondary Systems, Electric Power Re-search Institute, Report NP-2149, December, 1981.(7) Emory, B. B., “Theoretical Considerations in the Design of CrudSample Systems for Nuclear Power Plants”, NACE Corrosion 79-Corrosion Product Sampling Symposium, Atlanta, GA., March,1979.(8) Aschoff, A.
45、 F., Y. H. Lee, D. M. Sopocy, O. Jonas, Interim Con-sensus Guidelines on Fossil Plant Cycle Chemistry, Electric PowerResearch Institute, Report CS-4629, June 1986.(9) Tucker, P.A., “Best Practices in Corrosion Product Sampling”,EPRI PWR Chemistry Meeting 1995.D6301 134ASTM International takes no pos
46、ition respecting the validity of any patent rights asserted in connection with any item mentionedin 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 responsibil
47、ity.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to AS
48、TM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address
49、 shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D6301 135
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