1、Designation: D4453 11D4453 16Standard 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
2、in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This practice2 covers concepts for handling high purity water samples needed for the measurement of ever-decreasing levelsof specified impurit
3、ies that are encountered in the operation of modern high-pressure boilers and turbines. The handling of blanksassociated with the analysis of high purity water samples is also covered by this practice. The techniques presented can help theinvestigator increase the accuracy of analyses performed.1.2
4、This practice is applicable to water and steam samples from “zero solids treated” once-through or drum-type boilers, reactorcoolant water, electronic grade water, or any other process water where analyte concentrations are in the low parts per billion(micrograms per litre) range.1.3 The values state
5、d in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety an
6、d health practices and determine the applicability of regulatorylimitations prior to use. Specific hazards statements 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 Wa
7、ter3. Terminology3.1 DefinitionsDefinitions: For definitions of terms used in these test methods, refer to Terminology D1129.3.1.1 For definitions of terms used in this standard, refer to Terminology D1129.4. Significance and Use4.1 The determination of trace impurities (on the order of parts per bi
8、llion) in high purity water places extreme requirementson all aspects of the analytical system. This is particularly true when ubiquitous species such as sodium and chloride are of interestbecause they can potentially be introduced as contaminants at almost every step of an analytical procedure. Con
9、tamination canoccur during sample collection, during sample storage by leaching of improperly cleaned containers, during sample transfer, andby handling with pipets, syringes, etc., and during the actual analysis by contaminated reagents and sample cells and loop systems.It is also possible that tra
10、ce contaminants can be lost from samples by volatilization or precipitation, by diffusion into the matrixof the container material, and by “plating out” on the walls of sampling lines by flow phenomena.4.2 Strict adherence to a given procedure is necessary to achieve good results at trace levels of
11、analysis because very smalldifferences in procedure execution will affect precision and the addition or loss of nanogram amounts of analyte may affect theaccuracy of a determination.1 This practice is under the jurisdiction ofASTM Committee D19 on Water and is the direct responsibility of Subcommitt
12、ee D19.03 on Sampling Water and Water-FormedDeposits, Analysis of Water for Power Generation and Process Use, On-Line Water Analysis, and Surveillance of Water.Current edition approved Feb. 1, 2011Feb. 15, 2016. Published April 2011March 2016. Originally approved in 1985. Last previous edition appro
13、ved in 20062011 asD4453 02D4453 11.(2006). DOI: 10.1520/D4453-11.10.1520/D4453-16.2 This practice suggests the use of specific techniques. As new techniques are developed or required by lower limits, revision of this practice will likely be needed.3 For referencedASTM standards, visit theASTM websit
14、e, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication
15、of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be consider
16、ed the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15. Reagents and Materials5.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. It is intended that all reagents shall conform to thespecifica
17、tions of the Committee on Analytical Reagents of the American Chemical Society, where such specifications areavailable.4 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its usewithout lessening the accuracy of the determination.5.2
18、 Purity of WaterReference to water that is used for reagent preparation, rinsing or dilution shall be understood to meanwater that conforms to the quantitative specifications of Type II reagent water of Specification D1193.5.3 Hydrochloric Acid (1 + 1)Dilute concentrated hydrochloric acid with an eq
19、ual volume of water.5.4 Nitric Acid (1 + 1)Dilute concentrated nitric acid with an equal volume of water.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 might contaminate the analytes should be excluded from
20、the sampling andhandling area, e.g., for example, smoke, volatile organic solvents, etc. (WarningWhen performing trace organic analyses, donot allow the use of volatile organic solvents or smoking at the same time and within the area.Warning)when performing traceorganic analyses, do not allow the us
21、e of volatile organic solvents or smoking at the same time and within the area.)6.2 Sample Containers and Their Treatment:6.2.1 Analysis of Trace MetalsMetals:56.2.1.1 Bottles made from the following materials should be adequate: TFE-fluorocarbon FEP, HDPE, LDPE, Polypropylene,and polycarbonate. Cap
22、s should be made of the same material or, if not available, the caps should be lined with one of the suggestedmaterials.6.2.1.2 Fill the bottle with HCl (1 + 1) and allow to stand for 48 h at room temperature (80C for TFE-fluorocarbon), then emptyand rinse with water.6.2.1.3 Fill the bottle with HNO
23、3 (1 + 1) (1 + 1) and allow to stand for 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, and empty. Wear disposable polyethylene gloves whenhandling the bottles from this point onward. If a conta
24、minated surface 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 allow to soak for 48 h.After filling, place the bottle in a polyethylene bagand seal the bag during the storage period. The water should be changed at weekly interv
25、als during long storage periods.6.2.2 Analysis of Other Trace IonsIons:66.2.2.1 Containers made from the following materials should be adequate: HDPE, LDPE, polysulfone, polycarbonate,polystyrene, polypropylene, and polymethyl pentene. The temperature of the samples should not be above 50C when take
26、n orduring the storage period to prevent leaching from the containers. (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 handling thebottles from this point onward. If a contaminated surface is touched, remove and replace t
27、he glove.6.2.2.3 Repeat 6.2.2.2.6.2.2.4 Completely fill the bottle with water, cap, and allow to soak for a minimum of 1 day and a maximum of 5 days. Afterfilling, place the bottle in a polyethylene bag and seal the bag during the storage period. The water should be changed at 5 dayintervals during
28、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 a TFE-fluorocarbon-lined or aluminum-lined cap.6.2.3.2 Wash in hot detergent water and rinse with tap water three times.6.2.3.3 Rinse three times with water.6.2.3.
29、4 Bottles must be either heated to a minimum of 400C in a muffle furnace (or dry heat sterilizer) for at least 30 min orsolvent rinsed as in 6.2.3.5.6.2.3.5 Rinse with solvents in the following order: methanol, n-hexane. Gloves worn during the solvent rinse may containplasticizers (phthalates) that
30、may cause contamination. Polyurethane, polyethylene, or nitrile rubber gloves are not likely to have4 “Reagent Chemicals, American Chemical Society Specifications,” Am. Chemical Soc., Washington, DC. For suggestions on the testing of reagents not listed by theAmerican Chemical Society, see “Analar S
31、tandards for Laboratory Chemicals,” BDH Ltd., Poole, Dorset, U.K., and the “United States Pharmacopeia.”5 Except alkali and alkali earth metals.6 Ions such as Na+, K+, Cl, Ca2+, Mg2+, F, Br, NH4+, NO3, SO42, and PO43.D4453 162phthalates and should be used. (WarningWhen rinsing with solvents, use a f
32、ume hood with proper exhaust flow.Warning)when rinsing with solvents, use a fume hood with proper exhaust flow.)6.2.3.6 Dry with organic-free nitrogen to drive off the volatile solvents.6.2.3.7 Immediately cap the bottle with a TFE-fluorocarbon-lined or aluminum-lined cap which has been previously c
33、leanedusing the same method.6.2.4 Analysis of Trace Volatile Organics:6.2.4.1 The sample container must be glass with a TFE-fluorocarbon-lined septum and screw cap properly tightened to providea hermetic seal.6.2.4.2 Wash in hot detergent water, and rinse with tap water three times.6.2.4.3 Rinse thr
34、ee times with water.6.2.4.4 Heat the vials and septa at 105C for 1 h, then cool to room temperature in an enclosed contaminant-free area. Cap thevials with the TFE-fluorocarbon lining of the septum down.6.3 Sampling:6.3.1 Errors due to the sampling process can be minimized using an on-line measureme
35、nt technique. A proper choice ofmaterials to conduct the sample to the measuring instrument and the samples residence time in transit can affect the final accuracy.6.3.2 Some of the same precautions followed in the preparation of the sample containers must also be followed when collectinggrab sample
36、s (see above). It is recommended that sample conditioning condensers, coolers, and associated fittings and valves beof stainless steel and maintained leak free (See Practice D1066). Condensate temperature should be 50C and preferably nearambient temperature.6.3.3 Any samples to be stored more than 2
37、4 h should be refrigerated (4C). Samples requiring trace PO4 3, NO3, NH4+, andSO42- determinations should be refrigerated at 4C at the time of collection. These species are subject to biological degradation.6.3.4 Establish a continuous flow in a well-flushed sampling line (24 h recommended). Do not
38、readjust the flow rate less than45 min before sampling. (See Practice D1066.)6.3.5 Put on disposable polyethylene gloves before handling the sample bottle. Empty the bottle, rinse with the sample(including cap) three times, fill only to the rim to prevent ionic transport in the water film on the out
39、side of the sample bottle.Replace the bottle in the plastic bag and collect a duplicate sample.6.3.6 Samples collected for the analysis of non-alkali trace metals should be acidified to a pH of 2 with 1 mL of ultrapureHNO3 per 500 mL of sample. The concentrated acid should be added to the sample bot
40、tle so as to keep its contact time with thebottle to a minimum.7 Fill these bottles just to the rim to avoid loss of the acid. Replace the bottle in the plastic bag and collecta duplicate sample.6.3.7 When sampling for volatile organics the vial should be filled to overflowing so that a convex menis
41、cus is formed. The capand septum with the TFE-fluorocarbon side down is placed on the meniscus and sealed allowing no air into the vial.(WarningAvoid warming the bottle to prevent breakage.Warning)avoid warming the bottle to prevent breakage.)6.3.8 In the event an automatic sampler is being used, ca
42、re must be taken during set-up, and blank water must be run throughthe sampler following the initial set-up to assure adequate rinsing prior to use.6.4 Analytical Blank:6.4.1 The ability to control the level of the analytical blank has seriously affected the accuracy of modern methods of traceelemen
43、t analysis. Often it is the variability in the blank correction and not the absolute value of the blank that affects the accuracyof the analysis. As the variability becomes a significant percentage of the sample amount, more determinations of the blank arenecessary so that the variability can be est
44、imated with some degree of reliability. It is a mistake to base the blank correction ona single determination. At least three replicate runs for the blank determination as well as the subsequent analyses of each sampleare recommended.6.4.2 All precautions observed in the preparation of bottles for s
45、ampling of water shall also be observed for bottles used in thepreparation of analytical blanks.6.4.3 When acidifying samples for trace metals, also acidify the blank with the same amount of acid.7 This prevents the formation of ion-exchange sites on the bottles internal surface.D4453 1637. Keywords
46、7.1 analysis; container; contamination; ion; samplingASTM International takes no position 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 ri
47、ghts, 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 years andif not revised, either reapproved or withdrawn.Your comments are invited either for
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