1、Designation: D5463 13Standard Guide forUse of Test Kits to Measure Inorganic Constituents inWater1This standard is issued under the fixed designation D5463; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision.
2、 A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () 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 andwastewater.
3、 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 ofkits
4、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 test
5、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, such
6、 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 steps,
7、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 kit t
8、est 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 products
9、 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 analytes
10、, 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 is s
11、atisfactory.1.6 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.7 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 es
12、tablish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specificprecautionary statements, see Section 10.2. Referenced Documents2.1 ASTM Standards:3D1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD3370 Prac
13、tices for Sampling Water from Closed ConduitsD4453 Practice for Handling of High Purity Water SamplesD4691 Practice for Measuring Elements in Water by FlameAtomic Absorption SpectrophotometryD5810 Guide for Spiking into Aqueous SamplesD5847 Practice for Writing Quality Control Specificationsfor Stan
14、dard Test Methods for Water AnalysisE178 Practice for Dealing With Outlying ObservationsE275 Practice for Describing and Measuring Performance ofUltraviolet and Visible SpectrophotometersE958 Practice for Estimation of the Spectral Bandwidth ofUltraviolet-Visible Spectrophotometers1This guide is und
15、er the jurisdiction of ASTM Committee D19 on Water and isthe direct responsibility of Subcommittee D19.05 on Inorganic Constituents inWater.Current edition approved Jan. 1, 2013. Published February 2013. Originallyapproved in 1993. Last previous edition approved in 2008 as D5463 08. DOI:10.1520/D546
16、3-13.2Test kits for determining inorganic analytes in water are available from variousUnited States and foreign manufacturers, as well as from laboratory supplycompanies.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annu
17、al Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13. Terminolo
18、gy3.1 DefinitionsFor definitions of terms used in this guide,refer to Terminology D1129 and Practice D4691.3.2 Definitions of Terms Specific to This Standard:3.2.1 analyte, nthe chemical or constituent being deter-mined.3.2.2 carryover, nthe contamination of a subsequentsample by a previous sample,
19、typically due to incompletecleaning of a reused test kit component.3.2.3 expiration date, na date applied by the manufacturerafter which an accurate result is not ensured by the manufac-turer.3.2.4 finish (usually analytical finish), nthe analyticalmethodology used for the measuring step of the anal
20、ysis.3.2.5 kit (or test kit), na commercially-packaged collec-tion of components intended to simplify the analytical-testingfunction.3.2.6 interference, na matrix components effect thatmight cause an analytical bias or that might prevent a success-ful analysis.3.2.7 material safety data sheet, na fe
21、derally-mandated,safety-related document that must be made available to kit-chemistry users.3.2.8 matrix, nsample contents other than the target ana-lyte.3.2.9 offcial method, nan analytical test method officiallyapproved by an industry consensus organization (such asASTM, AOAC, or APHA) or by a gov
22、ernment entity such asthe USEPA.43.2.10 refill, na replacement package of test kit compo-nents used in testing.3.2.11 spike, na small-volume, high relative concentrationaliquot of analyte added quantitatively to a split sample as aquality check.3.2.12 split sample, na sample that is split into sub-s
23、amples that are intended to have the same composition as theoriginal sample.4. Summary of Guide4.1 Analytical test kits simplify the operational proceduresnecessary to perform an analysis. This guide includes generalconsiderations relating to the procedures to be followed inorder to ensure an accura
24、te determination. This guide alsodescribes, in general terms, the characteristics of some kit typesand kit components and includes some comments on theircapabilities, benefits and, where appropriate, their limitations.5. Significance and Use5.1 Inorganic constituents in water and wastewater must bei
25、dentified and measured to support effective water qualitymonitoring and control programs. Currently, one of thesimplest, most practical and cost effective means of accom-plishing this is through the use of chemical test kits and refills.A more detailed discussion is presented in ASTM STP 1102.55.2 T
26、est kits have been accepted for many applications,including routine monitoring, compliance reporting, rapidscreening, trouble investigation, and tracking contaminantsource.5.3 Test kits offer time-saving advantages to the user. Theyare particularly appropriate for field use and usually are easy tous
27、e. Users do not need to have a high level of technicalexpertise. Relatively unskilled staff can be trained to makeaccurate determinations using kits that include a premixed4Other documents: Offcial Methods of Analysis of the Association of OffcialAnalytical Chemists, 15th Ed., AOAC, Arlington, VA, 1
28、990. Changes are publishedin annual supplements. Standard Methods for the Examination of Water andWastewater, 17th Ed.,APHA,AWWA, and WPCF. Washington, DC, 1989. Methodsfor the Chemical Analysis of Water and Wastes, USEPA, Cincinnati, OH, March1983.5Spokes, G. Neil, and Bradley, Julie A., “Performan
29、ce Testing of Selected TestKits for Analysis of Water Samples,” ASTM STP 1102, ASTM, Philadelphia, 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,
30、C, P, TChlorine C, P, TChlorine dioxide C, P, TChromium (III) CChromium (VI) C, P, TCobalt CCopper 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
31、, P, TOxygen (dissolved) C, P, TOzone C, PPermanganate C, TpH C, PPhosphate C, PSilica C, PSilver 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 = go nogo, P = photometric, and T = titr
32、imetric.D5463 132liquid 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 conducted bya responsib
33、le chemist. The development of suitable protocolsand conditions for safe use should be conducted by theresponsible chemist with the 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 Completene
34、ss of KitsThe kits components may ormay not be complete for the required determination. The usermust assemble all instruments and materials necessary for thedetermination. For example, if the test kit is used for fieldscreening to indicate the need for samples requiring a highaccuracy measurement, t
35、he user may need to provide a meansof preserving a sample for later measurements at a laboratory.6.3 Protocol Established by a Responsible ChemistAresponsible chemist must determine whether the sample can beanalyzed correctly by a particular kit chemistry. The respon-sible chemist should determine w
36、hether matrix factors,interferences, and temperature are handled correctly by the kitchemistry. Questions to be answered include the following:Has the kit chemistry previously given satisfactory resultsunder the proposed conditions? What changes have occurredthat must be taken into account? For exam
37、ple, the chemistshould consider seasonal changes, new interferences, samplepH changes, new dischargers upstream, and new processwastes in the sample. The responsible chemist must also decidewhether the proposed kit chemistry is applicable to theparticular circumstances. For example, it is necessary
38、todetermine whether the test range is appropriate, ensure that acolorimetric test kit that compensates for color is used with ahighly 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 a
39、pproved kitchemistry is used when an official method is required.6.4 Technical SupportIn case of difficulties, many kitmanufacturers 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
40、. If thekit manufacturer uses a revised version of the official testmethod, the revision may increase or decrease interferenceeffects.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 carryove
41、r.The carryover may be prevented or reduced by either cleaningthe reused item or rinsing with fresh sample several times.Aggressive cleaning action may be necessary after a samplecontaining a high concentration is tested.7.3 Careful note should be made of the manufacturerscomments concerning interfe
42、rences, and appropriate actionshould be taken.7.4 Temperature may affect kit performance.8. Apparatus8.1 Colorimetric Determinations Many procedures de-pend on color determination with a color comparator,photometer, or spectrophotometer. The manufacturer may offera color comparator for visual compar
43、isons based on liquid,glass, plastic, or printed color standards. The manufacturermay offer a photometer or may recommend the use of aspectrophotometer for photo-electric color determinations. Themanufacturers photometer may be based on optical filtersusing either colored glass or plastic, or on int
44、erference filters orLEDs. The filter bandwidth may be wide (up to 100-nm fullwidth half maximum height) for colored glass or plastic filtersand LEDs or quite narrow (10 nm) with interference filters. Thelaboratory spectrophotometer may have a 1- to 20-nm band-width and is typically more accurate tha
45、n a kit photometer orcolorimeter. Refer to Practices E275 and E958 for additionaldiscussion of colorimetry.NOTE 1Visual comparator kits may require the use of a particular typeof background illumination. The user should use the light source thatproduces the correct color or spectrum of background il
46、lumination, asspecified by the manufacturer.NOTE 2Color standards may not be permanent; reference should bemade to the manufacturers recommendations.8.2 Titrimetric Determinations Many procedures dependon measuring the volume of a standard solution required toreact with an analyte completely. The ma
47、nufacturer may offera buret, digital titrator, drop-test, or calibrated sample containerto dispense and measure the volume 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 Reagent
48、sReagent grade or better chemicalsshall be used in all tests. Unless otherwise indicated, it isintended that all reagents shall conform to the specifications ofthe Committee onAnalytical Reagents of theAmerican Chemi-cal Society, where such specifications are available.6However,these reagents may no
49、t be of sufficient purity in some cases dueto the sensitivity of the technique. It is the responsibility of themanufacturer 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 impr
