1、Designation: D 6301 08Standard Practice forCollection of On-Line Composite Samples of SuspendedSolids and Ionic Solids in Process 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
2、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 practice is applicable for sampling condensedsteam or water, such as boiler feedwater, f
3、or 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
4、 practice iscommonly 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-bilit
5、y of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1066 Practice for Sampling SteamD 1129 Terminology Relating to WaterD 1193 Specification for Reagent WaterD 1971 Practices for Digestion of Water Samples for De-termination of Metals by Flame Atomic Absorption,Grap
6、hite 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 Bias ofApplicable Test Methods of Committee D19 on WaterD 3370 Pr
7、actices 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 of Terms Specific to This Standard:3.2.1 corrosion product s
8、ampler, na device used to col-lect integrated samples of suspended solids and (as an option)ionic solids. It consists of a flow totalizer that accuratelymeasures the amount of sample passing through the device anda 0.45-m pore size membrane filter. Adding a second filter forion exchange resin impreg
9、nated membranes allows for collect-ing 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 exchange membranes, or both.3.2.3 suspended solids, nincludes all matter that is re-moved by a 0.45-m pore size filt
10、er.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 0.45-m membranefilter and ion exchange membranes. The sampling is accom-plished at system operating pressure or aft
11、er 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 suspended solids) and ifdesired, ion exchange membranes (for ionic solids). Thesample collection system (corrosion product
12、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 determines thetotal volume of sample that has passed through the sampler,regardless of changes in flowrate or pr
13、essure during thecollection period. Control and pressure reducing valves andmetering devices are downstream of the filter housing toeliminate the possible contribution of suspended solids andionic solids from these components to the sample stream.1This practice is under the jurisdiction of ASTM Comm
14、ittee 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 Analysis, and Surveillance of Water.Current edition approved Oct. 1, 2008. Published October 2008. Originallyappr
15、oved in 1998. Last previous edition approved in 2003 as D 6301 03.2For 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 Document Summary page onthe ASTM web
16、site.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.FIG. 1 Simplified Flow Diagram for Corrosion Product SamplerD6301082Additional flow may bypass the filter housing, so that flowswithin the sample lines are maintained within requir
17、ed range(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. Significance and Use5.1 The transport of any suspended solids or corrosionproducts from the preboiler cyc
18、le 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 corrosion products on PWR steam generatortubes can reduce heat transfer, and, if the deposit is suffic
19、ientlythick, 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, out of core radiation problems from activation reac-tions, and other material related problems.5.3 In f
20、ossil 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 expensive and potentially harmful to theboiler tubes.5.4 Normally, grab samples are not sensitive enough t
21、odetect 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 fordetecting the corrosion products and provide a better under-standing of the total corrosion product transport t
22、o 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 exchange media isflowrate and matrix dependent and could show variations fromlot to lot.6.3 Sample temperature
23、 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 Due to settling, or deposition, or both, in sampling lineswith low velocity, flow in sampling lines mu
24、st be turbulent andmaintained at a velocity of 1.8 m/s (6 ft/s) (see also PracticesD 3370).7. Apparatus7.1 Sample heat exchanger, made of such material that fullsystem pressure can be maintained within the coil, and of suchcapacity that the water being sampled will be cooled to lessthan 50C when the
25、 sampling flow rate is established (seePractices D 3370).7.2 Corrosion Product SamplerSee Fig. 1, SimplifiedFlow Diagram.7.3 Flow TotalizerWater meter that will maintain 6 5%accuracy over full range.8. Reagents and Materials8.1 Reagent WaterReferences to water shall be under-stood to mean water that
26、 meets or exceeds the quantitativespecifications for Type III reagent water conforming to Speci-fication D 1193, Section 1.1.8.2 Anion resin impregnated membranes (47-mm diameter),optional.8.3 Cation resin impregnated membranes (47-mm diam-eter), optional.8.4 Membrane Filters, (47-mm diameter), 0.45
27、-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 suspendedsolids/ionic solids is desired, record the lot numbers o
28、f 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 ensure that they are centered. If necessary, use afew drops of water to wet the membranes to help h
29、old 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, slowly open the sample is
30、olation 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 using Practices D 1066 o
31、r 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 bydraining it or by purg
32、ing 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 cation ion exchange
33、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 thespecific analyte collec
34、ted on the 0.45-m pore size filter or onthe resin impregnated membranes. Preparation should beD6301083consistent with the method of analysis. Refer to the specificmethod of analysis for specific guidance and information onpreparation, sample storage, etc. For the usual corrosionproducts of interest
35、(iron, copper, and zinc collected as eithersuspended solids or ionic solids), refer to Practices D 1971. Forelements above atomic weight 11, particularly chlorine andsulfur, contained in anions collected as ionic solids andconcentrated above 0.1%, Practice D 2332 might be used.11. Calculation11.1 A
36、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 filter /total flow in liters.12.
37、 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 will be determined on the type
38、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, such as Practices D 1971 or Prac
39、tice D 2332 refer-enced 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 membranes will be governed by
40、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 Water Quality(2) Solomon, Y., Ed.
41、, 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,Electric Power Research Institute, R
42、eport 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, “Automated Corrosion Produc
43、tSampling 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, December, 1981.(7) Emory, B. B.
44、, “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 Cycle Chemistry, ElectricPow
45、er 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 mentionedin this standard. Users of
46、 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 must be reviewed every five
47、 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 ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical co
48、mmittee, 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 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).D6301084
