1、Designation: D4453 16D4453 17Standard 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 Definitions: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 billion) in high purity water places extreme requirementson all aspects of the analytical syst
8、em. 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. Contamination canoccur during sample collection, during sample storage by leaching of improperl
9、y 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 trace contaminants can be lost from samples by volatilization or precipitation, by diffusion in
10、to 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 analysis because very smalldifferences in procedure execution will affect precision and the
11、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 Subcommittee D19.03 on Sampling Water and Water-FormedDeposits, Analysis of Water for Power Generation
12、 and Process Use, On-Line Water Analysis, and Surveillance of Water.Current edition approved Feb. 15, 2016Feb. 1, 2017. Published March 2016February 2017. Originally approved in 1985. Last previous edition approved in 20112016 asD4453 11.D4453 16. DOI: 10.1520/D4453-16.10.1520/D4453-17.2 This practi
13、ce 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 website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM St
14、andardsvolume 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 of what changes have been made to the previous version. Becauseit may not be technically possib
15、le 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 considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West
16、 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 thespecifications of the Committee on Analytical Reagents of the American Chemical Society, where such spec
17、ifications 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 Purity of WaterReference to water that is used for reagent preparation, rinsing or dilution sh
18、all 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 equal volume of water.5.4 Nitric Acid (1 + 1)Dilute concentrated nitric acid with an equal volume
19、 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 the sampling andhandling area, for example, smoke, volatile organic solvents, etc. (WarningWhen
20、 performing trace organic analyses, do notallow the use 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 Metals:56.2.1.1 Bottles made from the following materials should be adequate: TFE-fluorocarbon FEP,
21、HDPE, LDPE, Polypropylene,and polycarbonate. Caps 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 r
22、inse with water.6.2.1.3 Fill the bottle with HNO3 (1 + 1) and allow to stand for 48 h at room temperature (80C for TFE-fluorocarbon), thenempty 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 bo
23、ttles from this point onward. If a contaminated 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
24、water should be changed at weekly intervals during long storage periods.6.2.2 Analysis of Other Trace Ions: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 sampl
25、es should not be above 50C when taken 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 surf
26、ace 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 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
27、be changed at 5 dayintervals 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 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
28、 Rinse three times with water.6.2.3.4 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 co
29、ntainplasticizers (phthalates) that may cause contamination. Polyurethane, polyethylene, or nitrile rubber gloves are not likely to havephthalates and should be used. (WarningWhen rinsing with solvents, use a fume hood with proper exhaust flow.)4 “Reagent Chemicals, American Chemical Society Specifi
30、cations,” Am. Chemical Soc., Washington, DC. For suggestions on the testing of reagents not listed by theAmerican Chemical Society, see “Analar Standards for Laboratory Chemicals,” BDH Ltd., Poole, Dorset, U.K., and the “United States Pharmacopeia.”5 Except alkali and alkali earth metals.6 Ions such
31、 as Na+, K+, Cl, Ca2+, Mg2+, F, Br, NH4+, NO3, SO42, and PO43.D4453 1726.2.3.6 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 cleanedusing the same method.6.2.4 Analysi
32、s 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 three times with water.6.2.4.4 Heat the vial
33、s 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 measurement technique. A proper choice ofmaterials
34、 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 samples (see above). It is recommended that sam
35、ple 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 24 h should be refrigerated (4C). (above f
36、reezing and 6C). Samples requiring tracePO4 3, NO3, NH4+, and SO42- determinations should be refrigerated at 4C above freezing and 6C 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
37、 not 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 th
38、e outside 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 sampl
39、e bottle 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
40、meniscus 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.)6.3.8 In the event an automatic sampler is being used, care must be taken during set-up, and blank water
41、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 traceelement analysis. Often it is the variability in the b
42、lank 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 estimated with some degree of reliability. It is a
43、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 sampling of water shall also be observed for bott
44、les 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 1737. Keywords7.1 analysis; container; contamination; ion; sam
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