1、Designation: D4453 11Standard Practice forHandling of High Purity Water Samples1This standard is issued under the fixed designation D4453; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in paren
2、theses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This practice2covers concepts for handling high puritywater samples needed for the measurement of ever-decreasinglevels of specified impurities that a
3、re encountered in theoperation of modern high-pressure boilers and turbines. Thehandling of blanks associated with the analysis of high puritywater samples is also covered by this practice. The techniquespresented can help the investigator increase the accuracy ofanalyses performed.1.2 This practice
4、 is applicable to water and steam samplesfrom “zero solids treated” once-through or drum-type boilers,reactor coolant water, electronic grade water, or any otherprocess water where analyte concentrations are in the low partsper billion (micrograms per litre) range.1.3 The values stated in SI units a
5、re 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 concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practice
6、s and determine the applica-bility of regulatory limitations prior to use. Specific hazardsstatements are given in 6.2.3.5, 6.1, and 6.3.7.2. Referenced Documents2.1 ASTM Standards:3D1066 Practice for Sampling SteamD1129 Terminology Relating to WaterD1193 Specification for Reagent Water3. Terminolog
7、y3.1 DefinitionsFor definitions of terms used in these testmethods, refer to Terminology D1129.4. Significance and Use4.1 The determination of trace impurities (on the order ofparts per billion) in high purity water places extreme require-ments on all aspects of the analytical system. This is partic
8、u-larly true when ubiquitous species such as sodium and chlorideare of interest because they can potentially be introduced ascontaminants at almost every step of an analytical procedure.Contamination can occur during sample collection, duringsample storage by leaching of improperly cleaned container
9、s,during sample transfer, and by handling with pipets, syringes,etc., and during the actual analysis by contaminated reagentsand sample cells and loop systems. It is also possible that tracecontaminants can be lost from samples by volatilization orprecipitation, by diffusion into the matrix of the c
10、ontainermaterial, and by “plating out” on the walls of sampling lines byflow phenomena.4.2 Strict adherence to a given procedure is necessary toachieve good results at trace levels of analysis because verysmall differences in procedure execution will affect precisionand the addition or loss of nanog
11、ram amounts of analyte mayaffect the accuracy of a determination.5. Reagents and Materials5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. It is intended that all reagents shall conform tothe specifications of the Committee on Analytical Reagents ofthe American Chemical Socie
12、ty, where such specifications areavailable.4Other grades may be used, provided it is firstascertained that the reagent is of sufficiently high purity topermit its use without lessening the accuracy of the determi-nation.5.2 Purity of Water Reference to water that is used forreagent preparation, rins
13、ing or dilution shall be understood tomean water that conforms to the quantitative specifications ofType II reagent water of Specification D1193.5.3 Hydrochloric Acid (1 + 1)Dilute concentrated hydro-chloric acid with an equal volume of water.5.4 Nitric Acid (1 + 1)Dilute concentrated nitric acid wi
14、than equal volume of water.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 Analysis, and Surveillance of Wat
15、er.Current edition approved Feb. 1, 2011. Published April 2011. Originallyapproved in 1985. Last previous edition approved in 2006 as D4453 02(2006).DOI: 10.1520/D4453-11.2This practice suggests the use of specific techniques. As new techniques aredeveloped or required by lower limits, revision of t
16、his practice will likely be needed.3For 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.4“Reagent Chemicals,Americ
17、an Chemical Society Specifications,”Am. Chemi-cal Soc., Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see “Analar Standards for Laboratory Chemicals,”BDH Ltd., Poole, Dorset, U.K., and the “United States Pharmacopeia.”1Copyright ASTM Internati
18、onal, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.5 Nitric Acid, ultra-pure.5.6 Methanol.5.7 n-hexane.5.8 Nitrogen, organic-free.6. Procedure6.1 Environmental ConditionsAny processes that mightcontaminate the analytes should be excluded from the samplingand
19、handling area, e.g., smoke, volatile organic solvents, etc.(Warningwhen performing trace organic analyses, do notallow the use of volatile organic solvents or smoking at thesame time and within the area.)6.2 Sample Containers and Their Treatment:6.2.1 Analysis of Trace Metals:56.2.1.1 Bottles made f
20、rom the following materials should beadequate: TFE-fluorocarbon FEP, HDPE, LDPE, Polypropy-lene, and polycarbonate. Caps should be made of the samematerial or, if not available, the caps should be lined with oneof the suggested materials.6.2.1.2 Fill the bottle with HCl (1 + 1) and allow to stand fo
21、r48 h at room temperature (80C for TFE-fluorocarbon), thenempty and rinse with water.6.2.1.3 Fill the bottle with HNO3(1 + 1) and allow to standfor 48 h at room temperature (80C for TFE-fluorocarbon),then empty and rinse with water.6.2.1.4 Fill the bottle about one third full with water, cap,shake,
22、and empty. Wear disposable polyethylene gloves whenhandling the bottles from this point onward. If a contaminatedsurface is touched, remove and replace the glove.6.2.1.5 Repeat 6.2.1.4.6.2.1.6 Completely fill the bottle with water, cap, and allowto soak for 48 h.After filling, place the bottle in a
23、polyethylenebag and seal the bag during the storage period. The watershould be changed at weekly intervals during long storageperiods.6.2.2 Analysis of Other Trace Ions:66.2.2.1 Containers made from the following materialsshould be adequate: HDPE, LDPE, polysulfone, polycarbon-ate, polystyrene, poly
24、propylene, and polymethyl pentene. Thetemperature of the samples should not be above 50C whentaken or during the storage period to prevent leaching from thecontainers. (See 6.3.3.)6.2.2.2 Fill the bottle one third full with water, cap, shake,and empty. Wear disposable polyethylene gloves when han-dl
25、ing the bottles from this point onward. If a contaminatedsurface is touched, remove and replace the glove.6.2.2.3 Repeat 6.2.2.2.6.2.2.4 Completely fill the bottle with water, cap, and allowto soak for a minimum of 1 day and a maximum of 5 days.After filling, place the bottle in a polyethylene bag a
26、nd seal thebag during the storage period. The water should be changed at5 day intervals during long storage periods.6.2.3 Analysis of Trace Organics (Acid and Base Neutrals):6.2.3.1 The sample bottle must be borosilicate glass with aTFE-fluorocarbon-lined or aluminum-lined cap.6.2.3.2 Wash in hot de
27、tergent water and rinse with tap waterthree times.6.2.3.3 Rinse three times with water.6.2.3.4 Bottles must be either heated to a minimum of400C in a muffle furnace (or dry heat sterilizer) for at least 30min or solvent rinsed as in 6.2.3.5.6.2.3.5 Rinse with solvents in the following order: metha-n
28、ol, n-hexane. Gloves worn during the solvent rinse maycontain plasticizers (phthalates) that may cause contamination.Polyurethane, polyethylene, or nitrile rubber gloves are notlikely to have phthalates and should be used. (Warningwhenrinsing with solvents, use a fume hood with proper exhaustflow.)6
29、.2.3.6 Dry with organic-free nitrogen to drive off thevolatile solvents.6.2.3.7 Immediately cap the bottle with a TFE-fluorocarbon-lined or aluminum-lined cap which has beenpreviously cleaned using the same method.6.2.4 Analysis of Trace Volatile Organics:6.2.4.1 The sample container must be glass w
30、ith a TFE-fluorocarbon-lined septum and screw cap properly tightened toprovide a hermetic seal.6.2.4.2 Wash in hot detergent water, and rinse with tap waterthree times.6.2.4.3 Rinse three times with water.6.2.4.4 Heat the vials and septa at 105C for 1 h, then coolto room temperature in an enclosed c
31、ontaminant-free area. Capthe vials with the TFE-fluorocarbon lining of the septum down.6.3 Sampling:6.3.1 Errors due to the sampling process can be minimizedusing an on-line measurement technique. A proper choice ofmaterials to conduct the sample to the measuring instrumentand the samples residence
32、time in transit can affect the finalaccuracy.6.3.2 Some of the same precautions followed in the prepa-ration of the sample containers must also be followed whencollecting grab samples (see above). It is recommended thatsample conditioning condensers, coolers, and associated fit-tings and valves be o
33、f stainless steel and maintained leak free(See Practice D1066). Condensate temperature should be50C and preferably near ambient temperature.6.3.3 Any samples to be stored more than 24 h should berefrigerated (4C). Samples requiring trace PO43,NO3,NH4+, and SO42-determinations should be refrigerated
34、at 4Cat the time of collection. These species are subject to biologicaldegradation.6.3.4 Establish a continuous flow in a well-flushed samplingline (24 h recommended). Do not readjust the flow rate lessthan 45 min before sampling. (See Practice D1066.)6.3.5 Put on disposable polyethylene gloves befo
35、re handlingthe sample bottle. Empty the bottle, rinse with the sample(including cap) three times, fill only to the rim to prevent ionictransport in the water film on the outside of the sample bottle.Replace the bottle in the plastic bag and collect a duplicatesample.6.3.6 Samples collected for the a
36、nalysis of non-alkali tracemetals should be acidified to a pH of 2 with 1 mLof ultrapureHNO3per 500 mL of sample. The concentrated acid should be5Except alkali and alkali earth metals.6Ions such as Na+,K+,Cl,Ca2+,Mg2+,F,Br,NH4+,NO3,SO42, and PO43.D4453 112added to the sample bottle so as to keep its
37、 contact time withthe bottle to a minimum.7Fill these bottles just to the rim toavoid loss of the acid. Replace the bottle in the plastic bag andcollect a duplicate sample.6.3.7 When sampling for volatile organics the vial should befilled to overflowing so that a convex meniscus is formed. Thecap an
38、d septum with the TFE-fluorocarbon side down is placedon the meniscus and sealed allowing no air into the vial.(Warningavoid warming the bottle to prevent breakage.)6.3.8 In the event an automatic sampler is being used, caremust be taken during set-up, and blank water must be runthrough the sampler
39、following the initial set-up to assureadequate rinsing prior to use.6.4 Analytical Blank:6.4.1 The ability to control the level of the analytical blankhas seriously affected the accuracy of modern methods of traceelement analysis. Often it is the variability in the blankcorrection and not the absolu
40、te value of the blank that affectsthe accuracy of the analysis. As the variability becomes asignificant percentage of the sample amount, more determina-tions of the blank are necessary so that the variability can beestimated with some degree of reliability. It is a mistake to basethe blank correctio
41、n on a single determination. At least threereplicate runs for the blank determination as well as thesubsequent analyses of each sample are recommended.6.4.2 All precautions observed in the preparation of bottlesfor sampling of water shall also be observed for bottles used inthe preparation of analyt
42、ical blanks.6.4.3 When acidifying samples for trace metals, also acidifythe blank with the same amount of acid.7. Keywords7.1 analysis; container; contamination; ion; samplingASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentio
43、nedin 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 an
44、d 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 ASTM International Headquarters. Your comments will receive careful consideration at a meeting o
45、f 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 shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box
46、 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/).7This prevents the formation of ion-exchange sites on the bottles internalsurface.D4453 113
