1、Designation: D 5463 03Standard Guide forUse of Test Kits to Measure Inorganic Constituents inWater1This standard is issued under the fixed designation D 5463; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisio
2、n. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This guide covers general considerations for the use oftest kits for quantitative determination of analytes in water andwastewat
3、er. Test kits are available from various manufacturersfor the determination of a wide variety of analytes in drinkingwater, surface or ground waters, domestic and industrialfeedwaters and wastes, and water used in power generation andsteam raising. See Table 1 for a listing of some of the types ofki
4、ts that are available for various inorganic analytes in water.21.2 Ranges, detection limits, sensitivity, accuracy, and sus-ceptibility to interferences vary from kit to kit, depending onthe methodology selected by the manufacturer. In some cases,kits are designed to replicate exactly an official te
5、st method ofa standard-setting organization such as the Association ofOfficial Analytical Chemists (AOAC), American Public HealthAssociation (APHA), ASTM, or the U.S. Environmental Pro-tection Agency (USEPA). In other cases, minor modificationsof official test methods are made for various reasons, s
6、uch as toimprove performance, operator convenience, or ease of use.Adjustments may be made to sample size, reagent volumes andconcentrations, timing, and details of the analytical finish. Inyet other cases, major changes may be made to the official testmethod, such as the omission of analytical step
7、s, change of theanalytical finish, omission of reagents, or substitution of onereagent for another. Reagents in test kits are often combined toobtain a fewer number and make the test easier to use.Additives may also be used to minimize interferences and tomake the reagent more stable with time. A ki
8、t test method maybe based on a completely different technology, not approved byany official or standard-setting organization. Combinations oftest kitsmulti-parameter test kitsmay be packaged tosatisfy the requirements of a particular application conve-niently. The test kits in such combination produ
9、cts may be usedto make dozens of determinations of several parameters.1.3 Test kit reagent refills are commonly available frommanufacturers. Refills permit cost savings through reuse of themajor test kit components.1.4 Because of the wide differences among kits and meth-odologies for different analy
10、tes, universal instructions cannotbe provided. Instead, the user should follow the instructionsprovided by the manufacturer of a particular kit.1.5 A test kit or kit component should not be used after themanufacturers expiration date; it is the users responsibility todetermine that the performance i
11、s satisfactory.1.6 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-bility of regulatory limitations prior to use.
12、 For specificprecautionary statements, see Section 10.2. Referenced Documents2.1 ASTM Standards:D 1129 Terminology Relating to Water3D 1192 Guide for Equipment for Sampling Water andSteam in Closed Conduits3D 1193 Specification for Reagent Water3D 3370 Practices for Sampling Water from Closed Con-du
13、its3D 4453 Practice for Handling of Ultra-Pure Water Samples3D 4691 Practice for Measuring Elements in Water by FlameAtomic Absorption Spectrophotometry3D 5810 Guide for Spiking into Aqueous Samples3D 5847 Practice for Writing Quality Control Specificationsfor Standard Test Methods for Water Analysi
14、s4E 178 Practice for Dealing with Outlying Observations5E 275 Practice for Describing and Measuring Performanceof Ultraviolet, Visible, and Near Infrared Spectrophotom-eters6E 958 Practice for Measuring Practical Spectral Bandwidthof Ultraviolet-Visible Spectrophotometers61This guide is under the ju
15、risdiction of ASTM Committee D19 on Water and isthe direct responsibility of Subcommittee D19.05 on Inorganic Constituents inWater.Current edition approved June 10, 2003. Published July 2003. Originallyapproved in 1993. Last previous edition approved in 1998 as D 546398.2Test kits for determining in
16、organic analytes in water are available from variousUnited States and foreign manufacturers, as well as from laboratory supplycompanies.3Annual Book of ASTM Standards, Vol 11.01.4Annual Book of ASTM Standards, Vol 11.02.5Annual Book of ASTM Standards, Vol 14.02.6Annual Book of ASTM Standards, Vol 03
17、.06.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3. Terminology3.1 DefinitionsFor definitions of terms used in this guide,refer to Terminology D 1129 and Practice D
18、 4691.3.2 Definitions of Terms Specific to This Standard:3.2.1 analytethe chemical or constituent being deter-mined.3.2.2 carryoverthe contamination of a subsequent sampleby a previous sample, typically due to incomplete cleaning ofa reused test kit component.3.2.3 expiration datea date applied by t
19、he manufacturerafter which an accurate result is not ensured by the manufac-turer.3.2.4 finish (usually analytical finish)the analytical meth-odology used for the measuring step of the analysis.3.2.5 kit (or test kit)a commercially packaged collectionof components that is intended to simplify the an
20、alytical testingfunction.3.2.6 interferencean effect of a matrix component thatmight cause an analytical bias or that might prevent a success-ful analysis.3.2.7 material safety data sheeta federally-mandated,safety-related document that must be made available to kitchemistry users.3.2.8 matrixsample
21、 contents other than the target analyte.3.2.9 offcial methodan analytical test method officiallyapproved by an industry consensus organization such asASTM,AOAC, orAPHAor by a government entity such as theUSEPA.73.2.10 refilla replacement package of test kit componentsused in testing.3.2.11 spikea sm
22、all volume, high relative concentrationaliquot of analyte added quantitatively to a split sample as aquality check.3.2.12 split samplea sample that is split into sub-samplesthat are intended to have the same composition as the originalsample.4. Summary of Guide4.1 Analytical test kits simplify the o
23、perational proceduresnecessary to perform an analysis. This guide includes generalconsiderations relating to the procedures to be followed inorder to ensure an accurate determination. This guide alsodescribes, in general terms, the characteristics of some kit typesand kit components and includes som
24、e comments on theircapabilities, benefits and, where appropriate, their limitations.5. Significance and Use5.1 Inorganic constituents in water and wastewater must beidentified and measured to support effective water qualitymonitoring and control programs. Currently, one of the sim-plest, most practi
25、cal and cost effective means of accomplishingthis is through the use of chemical test kits and refills. A moredetailed discussion is presented in ASTM STP 1102.85.2 Test kits have been accepted for many applications,including routine monitoring, compliance reporting, rapidscreening, trouble investig
26、ation, and tracking contaminantsource.5.3 Test kits offer time-saving advantages to the user. Theyare particularly appropriate for field use and usually are easy touse. Users do not need to have a high level of technicalexpertise. Relatively unskilled staff can be trained to makeaccurate determinati
27、ons using kits that include a premixedliquid reagent, premeasured reagent (tablets, powders, or glassampoules), and premeasured sample (evacuated glass am-poules).6. General Considerations6.1 PersonnelThe selection of a test kit and determinationthat the test kit analysis is appropriate should be co
28、nducted bya responsible chemist. The development of suitable protocols7Other documents: Offcial Methods of Analysis of the Association of OffcialAnalytical Chemists, 15th Ed., AOAC, Arlington, VA, 1990. Changes are pub-lished in annual supplements. Standard Methods for the Examination of Water andWa
29、stewater, 17th Ed., APHA, AWWA, and WPCF. Washington, DC, 1989. Methodsfor the Chemical Analysis of Water and Wastes, USEPA, Cincinnati, OH, March1983.8Spokes, G. Neil, and Bradley, Julie A., “Performance Testing of Selected TestKits for Analysis of Water Samples,” ASTM STP 1102, ASTM, Philadelphia,
30、 PA,1991.TABLE 1 Availability and Types of Test KitsAnalyte Kit MethodologyAAcidity TAlkalinity C, P, TAluminum C, PAmmonia C, PBoron C, PBromine C, P, TCadmium CCalcium P, TCarbon dioxide TChloride A, C, P, TChlorine C, P, TChlorine dioxide C, P, TChromium (III) CChromium (VI) C, P, TCobalt CCopper
31、 C, P, TCyanide C, P, TFluoride PHardness C, GNG, P, THydrazine C, PHydrogen peroxide C, P, TIodine C, P, TIron C, PLead C, PManganese C, PMagnesium C, TMolybdate C, P, TNickel C, PNitrate C, PNitrite C, P, TOxygen (dissolved) C, P, TOzone C, PPermanganate C, TpH C, PPhosphate C, PSilica C, PSilver
32、PSulfate A, C, P, TSulfide C, P, TSulfite C, P, TThiocyanate CTin CVanadium CZinc C, P, TAKit Methodology: A = appearance/turbidity, C = visual colorimetric, GNG = gono go, P = photometric, and T = titrimetric.D 5463 032and conditions for safe use should be conducted by theresponsible chemist with t
33、he assistance of an industrial hygien-ist. The kit user may be a relatively unskilled staff person butmust be trained to an appropriate level of proficiency.6.2 Completeness of KitsThe kits components may ormay not be complete for the required determination. The usermust assemble all instruments and
34、 materials necessary for thedetermination. For example, if the test kit is used for fieldscreening to indicate the need for samples requiring a highaccuracy measurement, the user may need to provide a meansof preserving a sample for later measurements at a laboratory.6.3 Protocol Established by a Re
35、sponsible ChemistAresponsible chemist must determine whether the sample can beanalyzed correctly by a particular kit chemistry. The respon-sible chemist should determine whether matrix factors, inter-ferences, and temperature are handled correctly by the kitchemistry. Questions to be answered includ
36、e the following:Has the kit chemistry previously given satisfactory resultsunder the proposed conditions? What changes have occurredthat must be taken into account? For example, the chemistshould consider seasonal changes, new interferences, samplepH changes, new dischargers upstream, and new proces
37、swastes in the sample. The responsible chemist must also decidewhether the proposed kit chemistry is applicable to theparticular circumstances. For example, it is necessary todetermine whether the test range is appropriate, ensure that acolorimetric test kit that compensates for color is used with a
38、highly colored sample, and ensure that a colorblind user is ableto run a test requiring visual color comparisons accurately. Thechemist must also ensure that an officially approved kitchemistry is used when an official method is required.6.4 Technical SupportIn case of difficulties, many kitmanufact
39、urers may provide technical assistance.7. Interferences7.1 Kit chemistries that are based on an official test methodare subject to the same interferences as that test method. If thekit manufacturer uses a revised version of the official testmethod, the revision may increase or decrease interferencee
40、ffects.7.2 Sample carryover effects may occur if a commonsampling cup or tube is used. Appropriate care is necessaryunder such conditions in order to prevent sample carryover.The carryover may be prevented or reduced by either cleaningthe reused item or rinsing with fresh sample several times.Aggres
41、sive cleaning action may be necessary after a samplecontaining a high concentration is tested.7.3 Careful note should be made of the manufacturerscomments concerning interferences, and appropriate actionshould be taken.7.4 Temperature may affect kit performance.8. Apparatus8.1 Colorimetric Determina
42、tionsMany procedures de-pend on color determination with a color comparator, photom-eter, or spectrophotometer. The manufacturer may offer a colorcomparator for visual comparisons based on liquid, glass,plastic, or printed color standards. The manufacturer may offera photometer or may recommend the
43、use of a spectrophotom-eter for photo-electric color determinations. The manufactur-ers photometer may be based on optical filters using eithercolored glass or plastic, or on interference filters or LEDs. Thefilter bandwidth may be wide (up to 100-nm full width halfmaximum height) for colored glass
44、or plastic filters and LEDsor quite narrow (10 nm) with interference filters. The labora-tory spectrophotometer may have a 1- to 20-nm bandwidth andis typically more accurate than a kit photometer or colorimeter.Refer to Practices E 275 and E 958 for additional discussion ofcolorimetry.NOTE 1Visual
45、comparator kits may require the use of a particulartype of background illumination. The user should use the light source thatproduces the correct color or spectrum of background illumination, asspecified by the manufacturer.NOTE 2Color standards may not be permanent; reference should bemade to the m
46、anufacturers recommendations.8.2 Titrimetric DeterminationsMany procedures dependon measuring the volume of a standard solution required toreact with an analyte completely. The manufacturer may offera buret, digital titrator, drop-test, or calibrated sample containerto dispense and measure the volum
47、e of a standard solution. Aburet or digital titrator typically provides more accuracy than adrop-test or calibrated sample container.9. Reagents and Materials9.1 Purity of ReagentsReagent grade or better chemicalsshall be used in all tests. Unless otherwise indicated, it isintended that all reagents
48、 shall conform to the specifications ofthe Committee onAnalytical Reagents of theAmerican Chemi-cal Society, where such specifications are available.9However,these reagents may not be of sufficient purity in some cases dueto the sensitivity of the technique. It is the responsibility of themanufactur
49、er to provide reagents and accessory solutions ofsufficient quality to meet the performance specification claimsof the test kit. In addition, the manufacturer should specifyacceptable conditions of storage and provide expiration dates,where appropriate. It is the responsibility of the kit user toensure that no unacceptable deterioration has occurred intransit or due to improper storage conditions and that the kitsare not used improperly after their expiration dates (see 9.4).9.2 Purity of WaterWater must be of sufficient purity thatit does not interfere
