ASTM D5463-18

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it 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 version
of the standard as published by ASTM is to be considered the official document.
Designation: D5463 − 13 D5463 − 18
Standard Guide for
Use of Test Kits to Measure Inorganic Constituents in
Water
This standard is issued under the fixed designation D5463; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope*
1.1 This guide covers general considerations for the use of test kits for quantitative determination of analytes in water and
wastewater. Test kits are available from various manufacturers for the determination of a wide variety of analytes in drinking water,
surface or ground waters, domestic and industrial feedwaters and wastes, and water used in power generation and steam raising.
See Table 1 for a listing of some of the types of kits that are available for various inorganic analytes in water.
1.2 Ranges, detection limits, sensitivity, accuracy, and susceptibility to interferences vary from kit to kit, depending on the
methodology selected by the manufacturer. In some cases, kits are designed to replicate exactly an official test method of a
standard-setting organization such as the Association of Official Analytical Chemists (AOAC), American Public Health Association
(APHA), ASTM, or the U.S. Environmental Protection Agency (USEPA). In other cases, minor modifications of official test
methods are made for various reasons, such as to improve performance, operator convenience, or ease of use. Adjustments may
be made to sample size, reagent volumes and concentrations, timing, and details of the analytical finish. In yet other cases, major
changes may be made to the official test method, such as the omission of analytical steps, change of the analytical finish, omission
of reagents, or substitution of one reagent for another. Reagents in test kits are often combined to obtain a fewer number and make
the test easier to use. Additives may also be used to minimize interferences and to make the reagent more stable with time. A kit
test method may be based on a completely different technology, not approved by any official or standard-setting organization.
Combinations of test kits—multi-parameter test kits—may be packaged to satisfy the requirements of a particular application
conveniently. The test kits in such combination products may be used to make dozens of determinations of several parameters.
1.3 Test kit reagent refills are commonly available from manufacturers. Refills permit cost savings through reuse of the major
test kit components.
1.4 Because of the wide differences among kits and methodologies for different analytes, universal instructions cannot be
provided. Instead, the user should follow the instructions provided by the manufacturer of a particular kit.
1.5 A test kit or kit component should not be used after the manufacturer’s expiration date; it is the user’s responsibility to
determine that the performance is satisfactory.
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. For specific precautionary statements, see Section 10.
1.8 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
This guide is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents in Water.
Current edition approved Jan. 1, 2013May 1, 2018. Published February 2013May 2018. Originally approved in 1993. Last previous edition approved in 20082013 as
D5463 – 08.D5463 – 13. DOI: 10.1520/D5463-13.10.1520/D5463-18.
Test kits for determining inorganic analytes in water are available from various United States and foreign manufacturers, as well as from laboratory supply companies.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*A Summary of Changes section appears at the end of this standard
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D5463 − 18
TABLE 1 Availability and Types of Test Kits
A
Analyte Kit Methodology
Acidity T
Alkalinity C, P, T
Aluminum C, P
Ammonia C, P
Boron C, P
Bromine C, P, T
Cadmium C
Calcium P, T
Carbon dioxide T
Chloride A, C, P, T
Chlorine C, P, T
Chlorine dioxide C, P, T
Chromium (III) C
Chromium (VI) C, P, T
Cobalt C
Copper C, P, T
Cyanide C, P, T
Fluoride P
Hardness C, GNG, P, T
Hydrazine C, P
Hydrogen peroxide C, P, T
Iodine C, P, T
Iron C, P
Lead C, P
Manganese C, P
Magnesium C, T
Molybdate C, P, T
Nickel C, P
Nitrate C, P
Nitrite C, P, T
Oxygen (dissolved) C, P, T
Ozone C, P
Permanganate C, T
pH C, P
Phosphate C, P
Silica C, P
Silver P
Sulfate A, C, P, T
Sulfide C, P, T
Sulfite C, P, T
Thiocyanate C
Tin C
Vanadium C
Zinc C, P, T
A
Kit Methodology: A = appearance ⁄turbidity, C = visual colorimetric, GNG = go no
go, P = photometric, and T = titrimetric.
D3370 Practices for Sampling Water from Closed Conduits
D4453 Practice for Handling of High Purity Water Samples
D4691 Practice for Measuring Elements in Water by Flame Atomic Absorption Spectrophotometry
D5810 Guide for Spiking into Aqueous Samples
D5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
E178 Practice for Dealing With Outlying Observations
E275 Practice for Describing and Measuring Performance of Ultraviolet and Visible Spectrophotometers
E958 Practice for Estimation of the Spectral Bandwidth of Ultraviolet-Visible Spectrophotometers
3. Terminology
3.1 Definitions—Definitions: For definitions of terms used in this guide, refer to Terminology D1129 and Practice D4691.
3.1.1 For definitions of terms used in this standard, refer to Terminology D1129 and Practice D4691.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 analyte, n—the chemical or constituent being determined.
3.2.2 carryover, n—the contamination of a subsequent sample by a previous sample, typically due to incomplete cleaning of a
reused test kit component.
3.2.3 expiration date, n—a date applied by the manufacturer after which an accurate result is not ensured by the manufacturer.
3.2.4 finish (usually analytical finish), n—the analytical methodology used for the measuring step of the analysis.
D5463 − 18
3.2.5 kit (or test kit), n—a commercially-packaged collection of components intended to simplify the analytical-testing function.
3.2.6 interference, n—a matrix component’s effect that might cause an analytical bias or that might prevent a successful analysis.
3.2.7 material safety data sheet, n—a federally-mandated, safety-related document that must be made available to kit-chemistry
users.
3.2.8 matrix, n—sample contents other than the target analyte.
3.2.9 offıcial method, n—an analytical test method officially approved by an industry consensus organization (such as ASTM,
AOAC, or APHA) or by a government entity such as the USEPA.
3.2.10 refill, n—a replacement package of test kit components used in testing.
3.2.11 spike, n—a small-volume, high relative concentration aliquot of analyte added quantitatively to a split sample as a quality
check.
3.2.12 split sample, n—a sample that is split into sub-samples that are intended to have the same composition as the original
sample.
4. Summary of Guide
4.1 Analytical test kits simplify the operational procedures necessary to perform an analysis. This guide includes general
considerations relating to the procedures to be followed in order to ensure an accurate determination. This guide also describes,
in general terms, the characteristics of some kit types and kit components and includes some comments on their capabilities,
benefits and, where appropriate, their limitations.
5. Significance and Use
5.1 Inorganic constituents in water and wastewater must be identified and measured to support effective water quality
monitoring and control programs. Currently, one of the simplest, most practical and cost effective means of accomplishing this is
through the use of chemical test kits and refills. A more detailed discussion is presented in ASTM STP 1102.
5.2 Test kits have been accepted for many applications, including routine monitoring, compliance reporting, rapid screening,
trouble investigation, and tracking contaminant source.
5.3 Test kits offer time-saving advantages to the user. They are particularly appropriate for field use and usually are easy to use.
Users do not need to have a high level of technical expertise. Relatively unskilled staff can be trained to make accurate
determinations using kits that include a premixed liquid reagent, premeasured reagent (tablets, powders, or glass ampoules), and
premeasured sample (evacuated glass ampoules).
6. General Considerations
6.1 Personnel—The selection of a test kit and determination that the test kit analysis is appropriate should be conducted by a
responsible chemist. The development of suitable protocols and conditions for safe use should be conducted by the responsible
chemist with the assistance of an industrial hygienist. The kit user may be a relatively unskilled staff person but must be trained
to an appropriate level of proficiency.
6.2 Completeness of Kits—The kit’s components may or may not be complete for the required determination. The user must
assemble all instruments and materials necessary for the determination. For example, if the test kit is used for field screening to
indicate the need for samples requiring a high accuracy measurement, the user may need to provide a means of preserving a sample
for later measurements at a laboratory.
6.3 Protocol Established by a Responsible Chemist—A responsible chemist must determine whether the sample can be analyzed
correctly by a particular kit chemistry. The responsible chemist should determine whether matrix factors, interferences, and
temperature are handled correctly by the kit chemistry. Questions to be answered include the following: Has the kit chemistry
previously given satisfactory results under the proposed conditions? What changes have occurred that must be taken into account?
For example, the chemist should consider seasonal changes, new interferences, sample pH changes, new dischargers upstream, and
new process wastes in the sample. The responsible chemist must also decide whether the proposed kit chemistry is applicable to
the particular circumstances. For example, it is necessary to determine whether the test range is appropriate, ensure that a
colorimetric test kit that compensates for color is used with a highly colored sample, and ensure that a colorblind user is able to
run a test requiring visual color comparisons accurately. The chemist must also ensure that an officially approved kit chemistry is
used when an official method is required.
Other documents: Offıcial Methods of Analysis of the Association of Offıcial Analytical Chemists, 15th Ed., AOAC, Arlington, VA, 1990. Changes are published in annual
supplements. Standard Methods for the Examination of Water and Wastewater, 17th Ed., APHA, AWWA, and WPCF. Washington, DC, 1989. Methods for the Chemical
Analysis of Water and Wastes, USEPA, Cincinnati, OH, March 1983.Other documents: Offıcial Methods of Analysis of the Association of Offıcial Analytical Chemists, 15th
ed., AOAC, Arlington, VA, 1990. Changes are published in annual supplements. Standard Methods for the Examination of Water and Wastewater, 17th ed., APHA, AWWA,
and WPCF. Washington, DC, 1989. Methods for the Chemical Analysis of Water and Wastes, USEPA, Cincinnati, OH, March 1983.
Spokes, G. Neil, and Bradley, Julie A., “Performance Testing of Selected Test Kits for Analysis of Water Samples,” ASTM STP 1102, ASTM, Philadelphia, PA, 1991.
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6.4 Technical Support—In case of difficulties, many kit manufacturers may provide technical assistance.
7. Interferences
7.1 Kit chemistries that are based on an official test method are subject to the same interferences as that test method. If the kit
manufacturer uses a revised version of the official test method, the revision may increase or decrease interference effects.
7.2 Sample carryover effects may occur if a common sampling cup or tube is used. Appropriate care is necessary under such
conditions in order to prevent sample carryover. The carryover may be prevented or reduced by either cleaning the reused item
or rinsing with fresh sample several times. Aggressive cleaning action may be necessary after a sample containing a high
concentration is tested.
7.3 Careful note should be made of the manufacturer’s comments concerning interferences, and appropriate action should be
taken.
7.4 Temperature may affect kit performance.
8. Apparatus
8.1 Colorimetric Determinations —Determinations—Many procedures depend on color determination with a color comparator,
photometer, or spectrophotometer. The manufacturer may offer a color comparator for visual comparisons based on liquid, glass,
plastic, or printed color standards. The manufacturer may offer a photometer or may recommend the use of a spectrophotometer
for photo-electric color determinations. The manufacturer’s photometer may be based on optical filters using either colored glass
or plastic, or on interference filters or LEDs. The filter bandwidth may be wide (up to 100-nm full width half maximum height)
for colored glass
...