Marvin W. Skougstad U.S. Geological Survey Denver, Colo. 80225
Water pollution may be considered to be the addition of some substance or material, or the alteration of some physical, chemical, or biological property of water, which either temporarily or permanently renders that water less suitable for a particular use, such as for industrial, domestic, municipal, agricultural, or recreation purposes. To assess true conditions of water quality, specified chemical, physical, and biological measurements and tests are made on the water body or, commonly, on representative samples of that body of water. It is essential that the best available analytical techniques be used so as to accurately reflect the true condition of the water body. Through continuous monitoring and testing over a period of time, it is possible to determine whether a discharge of wastes has resulted in deterioration of the general condition of the water, or whether appropriate control and management of effluent discharges have resulted in nondeterioration of the water quality. Moreover, effective cooperation between government regulatory agencies, or between state environmental agencies, and industrial, municipal, agricultural, and other organizations depends on an agreement as to the ap-
propriate analytical method that should be used in order that all parties may have confidence in the results as being a true evaluation of the actual condition of a stream or other body of water. The desirability of such agreements naturally leads to attempts to standardize the analytical methods used. Standardization is obviously desirable on a national basis so that all interested and concerned parties may accept the water-quality data with confidence. It is also desirable internationally, especially when two or more nations share an interest in a single water system or a part of that system. The need for uniformity in analytical and test methods and for standardization in all aspects of waterquality monitoring has frequently been included within the scope of national standards bodies, such as the American National Standards Institute (ANSI) and the American Society for Testing and Materials (ASTM) in the United States. Technical Committee D-19 of ASTM currently has more than 350 professional people working on the development of standard methods of tests for water-quality data, water characteristics, and water-related materials. The Committee has published more than 135 standard meth-
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ods and is continually expanding its efforts to meet new needs and conditions. Organization for Economic Cooperation and Development Early interests in the development and international standardization of analytical methods for assessing conditions of water quality were evidenced in the late 1950's within the Committee for Applied Research of the Organization for Economic Cooperation and Development (OECD) and the Organization for European Economic Cooperation (OEEC). The first meeting under the sponsorship of this agency was held in 1960 and was titled "The First International Meeting on Scientific Research into Water Pollution." Their initial efforts were directed toward coordinating research on water pollution and "preparing a list of research subjects which could usefully be studied on a cooperative basis." At that time, 22 different laboratories indicated an interest in "methods for the determination of pollution of watercourses and estuaries; standardization of sampling methods and analysis by chemical, biological, or other means."
Report
International Standardization for Water-Quality Evaluation
At the first plenary session of a group of experts to study the methods of determining the "Composition and Condition of the Water of Streams," eight subgroups or working groups were established. Among these was Subgroup No. 8, whose assignment included the preparation of recommendations for the establishment of general sampling criteria and a comparative study of methods of analysis. The subgroup held several meetings, including two general meetings in Paris in December 1962 and in December 1964. The group's activities were terminated in April 1965, and a final report of their activities was prepared in December of that year. During Subgroup No. 8's tenure, a number of matters were investigated by the participating countries, including dissolved oxygen, biochemical oxygen demand (BOD s ), chemical oxygen demand, chloride, nitrite, nitrate, copper, zinc, residual chlorine, phosphates, and cyanide. Their final report ended with two general conclusions: "(a) Sampling. There is a growing tendency to use sampling systems relying more on statistical principles, either based on a grid of adjacent sections or the speed of the current. More and more automatic sampling and re-
cording stations are being installed for research on major waterways. (b) Methods of analysis. The group compared a large number of tests. Several types of determinations are still under study with a view to improvement or even fundamental modification, but in the great majority of cases the more accepted methods are now practiced. Many laboratories are tending increasingly to exchange the results of the methods in question." With the report of Subgroup 8, one of the early efforts toward international standardization of water-analysis methods had begun. Nordic Standards A few years later, in 1968, the four Scandinavian countries organized among themselves a working group with the aim of developing methods for air and water analysis that would be acceptable to the four countries. The working group consisted initially of experts from leading water-analysis laboratories in Norway, Sweden, Denmark, and Finland. Their activities have been supported by the standards associations in their respective countries. Their early efforts resulted, in October 1970, in the formation of a Nordic Standardization Committee
for analytical methods for air and water. Water-analysis methods were given priority, and it was decided to select a limited number of determinations to work on first and to divide the responsibility for developing methods among the four countries. As a result, efforts are being made to agree on methods for determining such quality factors as calcium, chloride, hardness, pH, specific conductance, color, turbidity, ortho- and total-phosphorus, chemical oxygen demand, suspended matter, and a number of others. A given method for a determination is recommended as a Nordic standard only after cooperative testing of the method and after general agreement and acceptance of the method by the four countries. As with other analytical problems, the water analyst is usually faced with a choice of methods for a particular determination. The Nordic standards generally stress the simpler methods requiring a minimum of instrumentation and expensive equipment. To this end, even atomic absorption spectrophotometric methods are at this time omitted, an omission which may be unfortunate in view of the fact that many toxic metals which occur in water, often at vanishingly small con-
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chapter on interlaboratory calibrations. International Standards Organization
centrations, can conveniently be determined by atomic absorption spectrophotometry. These metals have become increasingly important factors in water-quality characterization; consequently, their determination has also become important and common in many water-analysis laboratories. Because this technique is so useful for the determination of minor constituents, it becomes almost an essential part of the equipment for a laboratory. In light of this, it would seem that atomic absorption spectrophotometric methods might also be specified for the common constituents, too. The group, however, recognizes the necessity of preparing methods using special equipment and also the urgent need for methods for additional constituents and parameters. Presumably, their work will expand to include these other areas; the start they have made represents an important step in the development of water-analysis methods that can be accepted internationally. World Health Organization Other international organizations have, in recent years, given attention to the development and publication of methods for international acceptance. Notable among these is the World Health Organization which has gathered a number of water-analysis methods which are useful in water-quality investigations and in programs of water-pollution assessment. Currently, they are preparing a "Manual on Analysis for Water-Pollution Control," a manual "intended to provide governmental and other agencies, and particularly health administrations, with information and recommendations to assist them in setting up of water-pollution control programmes and the establishment of a unified system for fresh water analysis and recording of results." The manual will include procedures for the determination of a great number of significant water-quality constituents and parameters, including certain radiochemical measurements, and will include a
The International Standards Organization (ISO), with headquarters in Geneva, is the international specialized agency for standardization, comprising the national standards bodies of 73 countries. Its work, which covers many fields, is carried out by more than 150 technical committees. The results of ISO technical work are published as International Standards, which represent a global consensus of opinion. ISO initiated activity in the fields of air and water quality in 1971, and the first meeting of two new technical committees (TC 146 and TC 147) organized to deal with these problems was held in Geneva at the end of April 1972. The establishment of these committees was evidence of the growing worldwide interest and concern for the condition of the human environment and the conviction that something must be done to preserve and improve its quality. About 80 representatives from 19 countries attended this first organizing meeting of the water committee of ISO, which is identified as Technical Committee 147 on Water Quality. Liaison observers from several international organizations attended that first meeting and have continued to offer cooperation in the designation and preparation of urgently needed standards. These include observers from the World Health Organization (WHO), the Food and Agriculture Organization (FAO), the International Union of Pure and Applied Chemistry (IUPAC), and the Economic Commission for Europe (ECE). The Technical Committee on Water Quality was established by ISO on the premise that major environmental problems are by their very nature international in scope, and that they can, therefore, best be solved at the international level. All national and international regulations relating to water quality should be founded on the same scientific and technological base. By developing the needed, appropriate international standards for pollution assessment, the proper scientific base can be established. Furthermore, it was reasonable that ISO, as the dominant agency for establishing international standards, would be the logical organization to provide the mechanism for preparing and publishing standards that could be accepted worldwide. The American National Standards Institute (ANSI) serves as Secretariat for ISO Technical Committee 147. The Committee on Water Quality held a second meeting in Washington,
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D.C., in September 1973, in connection with the Ninth Triennial Meeting of ISO. As a result of these two meetings, the committee has defined the scope of its responsibilities as follows: "Standardization in the field of water quality, including definition of terms, sampling of waters, and the measuring and reporting of water characteristics. Standards of acceptability for water are excluded." The committee subsequently approved a program of work within the scope established for the committee. The program of work is in two parts, consisting of a preamble and a tabulation of priority work items. The preamble seems worth examining, for it demonstrates the broad categories with which the committee plans to become involved as it pursues its work. "The program of work of ISO/TC 147 on Water Quality shall include, but shall not necessarily be limited to, the following: 1. Standardization of terminology dealing with all aspects of water-quality characterization, including definition of relevant terms, units of measurement, and reporting results of water analysis. 2. Standardization of general methods for collecting samples of water, sludges, and bottom materials for various purposes, including selection of proper sampling sites, frequency of sampling, appropriate sampling equipment, treatment, preservation, and special handling of samples as may be required, and adequate identification and labeling of samples collected. 3. Standardization of methods for the measurement of water-quality properties and characteristics, including both chemical and physical properties, as well as radiological, microbiological, biological, and biochemical quality factors. Consideration will be given to the analysis and examination of all types of waters, including natural fresh and brackish water, sea water and brines, drinking water, industrial water, municipal and industrial wastewaters, and also sludges and bottom materials.
Table I. Subcommittees of ISO/TC 147 on Water Quality (1) Terminology (2) Physical, chemical, biochemical methods (3) Radiological methods (4) Microbiological methods (5) Biological methods (6) Sampling
4. Standardization of procedures for determining and expressing the comparative precision and accuracy of all test methods proposed as standards." To accomplish this program of work, the committee established six subcommittees, five of which have been activated and are pursuing their assigned activities. The designated subcommittees are given in Table I. Only Subcommittee 3 on Radiological Methods has not yet been activated. In addition, a Preliminary Study Group was organized to make recom mendations concerning committee policies in the matters of precision and accuracy of water-analysis standards. This study group has since become a work group, charged with the responsibility of specifying (1) minimum requirements for determining the precision of a method, (2) minimum requirements for determining the accuracy of a standard method, (3) means of expressing precision and accuracy, and (4) the relationship between significant figures and accuracy. Subcommittee 1, for which South Africa holds the Secretariat, is preparing a compilation of definitions of terms relating to five categories: (1) types of water, (2) water treatment and storage, (3) water sampling, (4) water analysis, and (5) miscellaneous terms. Subcommittee 2, for which the United States holds the Secretariat, has addressed itself to the preparation of standard methods in three broad categories: (1) physical properties of water and wastewater, (2) individual inorganic chemical constituents, and (3) individual or groups of organic constituents. Twelve work groups
have been established under Subcommittee 2, according to determined priorities of work. These work groups are actively developing methods which can be considered by representatives of the participating member nations for adoption as ISO international standards. The work groups presently working on individual methods include those on nitrogen compounds (United Kingdom), phosphorus compounds (Germany), calcium (Sweden), cadmium (USA), mercury (France), cyanides (Germany), dissolved oxygen (Belgium), biochemical oxygen demand (Belgium), chemical oxygen demand-dichromate (Sweden), total organic carbon (Netherlands), and halogenated hydrocarbons (USA). Other determinations were also assigned high priority, but these twelve were considered urgent and most in need of immediate attention. Subcommittees 4, 5, and 6, and Work Group A on Precision and Accuracy met in London in March 1974, during which meeting additional work groups under each of these subcommittees were set up to begin preparation of standards. Seven work groups were established under Subcommittee 4 on Microbiological Methods: (1) aerobic mesophilic viable bacteria (France), (2) coliforms, including E. Coli and others (France), (3) pseudomonas including fluorescents and aeruginosa (United Kingdom), (4) fecal streptococci (Netherlands), (5) sulfite-reducing Clostridium (Germany), (6) nitrogen-cycle bacteria (Sweden, tentatively), and (7) salmonellae (Hungary). Subcommittee 5 on Biological Methods now includes three work groups: (1) toxicity-bacteria (Germany), (2) toxicity-daphnia (Hungary), and (3) toxicity-fish (United Kingdom). Subcommittee 6 on Sampling has divided its activities into three categories and assigned them to work groups as follows: (1) sampling programs (United Kingdom), (2) sampling techniques (USA), and (3) sample handling and preservation (France). The next meeting of ISO/TC 147 will be in Budapest, Hungary, in the spring of 1975. Presumably, the subcommittees will schedule meetings in the same week as the committee and during the days immediately preceding those on which the full committee will meet. By the time of the planned third meeting of ISO/TC 147, many of the subcommittees and work groups will have significant accomplishments to report, and a number of methods will be ready for consideration and approval as international standards. Technical Advisory Group As Secretariat for ISO/TC 147, the
American National Standards Institute (ANSI) is responsible to the ISO Council and to the members of the committee, for all the activities of the Technical Committee including its subcommittees and working groups. To assist ANSI in carrying out these responsibilities, a United States Technical Advisory Group (USA-TAG) was organized early in 1972. This TAG provides input to the Secretariat in the matter of proposals for organizing TC 147 and for conducting its work. As Secretariat for TC 147, ANSI acts as an international Secretariat and must not be influenced by national considerations. The Secretariat does rely, however, on counsel and advice from the USA-TAG for guidance in policy matters which are subject to consideration and adoption by all ISO/TC 147 member nations. The USA-TAG is composed of representatives from organizations and professional societies who have an interest in promoting international standardization in water-quality measurements. Presently active on the USATAG are representatives from federal agencies, including the Geological Survey, Environmental Protection Agency, the National Bureau of Standards, Atomic Energy Commission, and the Naval Ship Engineering Center. Several professional societies and organizations are represented, including the American Society of Civil Engineers, American Society of Mechanical Engineers, Manufacturing Chemists Association, Water Pollution Control Federation, American Water Works Association, and the American Society for Testing and Materials. Membership and participation in USA-TAG activities are not restricted but are open to any organization or agency that has an interest in participating in the development of international standards in the area of water-quality assessment. The group ordinarily holds three meetings a year. The USA-TAG also functions to advise ANSI as Secretariat of TC 147 Subcommittee 2 on Physical, Chemical, and Biochemical Methods, and
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serves to establish the United States position relative to technical documents generated by the subcommittees and work groups. These generally consist of Draft Proposals and Draft International Standards. Liaison Evidence of the widespread interest in, and the urgent need for, international standards for water analysis is amply demonstrated by the number of international organizations with which ISO/TC 147 has established liaison. Active liaison arrangements have been established with 17 international organizations or agencies, including the World Health Organization, Food and Agriculture Organization of the UN, Economic Commission for Europe, Committee of the European Communities, Inter-Governmental Maritime Consultative Organization, World Meteorological Organization, Council for Mutual Economic Assistance, the International Organization for Hydraulic Research, and the Nordic Standardization Committee for Air and Water. All of these organizations have an interest in standards for water analysis, and active liaison efforts involving at least the exchange of pertinent documents and information have been initiated. In addition, whenever possible, a representative of each of the liaison organizations attends meetings of ISO/TC 147 as observers, and ISO representatives attend meetings of the other agencies in order to maintain an active exchange of information and to keep each other up-to-date on the activities of each relating to water and pollution analysis. In addition, to facilitate the work of TC 147, liaison has been established and is maintained with nine other ISO and IEC (International Electrotechnical Commission) Technical Committees. These inlcude TC 28 on Petroleum Products, TC 47 on Chemistry, TC 69 on Application of Statistical Methods, TC 113 on Measurement of Liquid Flow in Open Channels, and TC 146 on Air Quality. The output of ISO and its Technical Committee 147 on Water Quality shows promise of fulfilling an urgent need for international standardization for water pollution assessment. International Association of Hydrologie Sciences Still another international organization has recently involved itself in matters relating to agreement on uniformity of methods for water analysis. The International Association of Hydrologie Sciences (IAHS) recently organized a subcommittee on water quality. One of this subcommittee's first actions was to recognize the possibility of discrepancies when data
Marvin W. Skougstad of the Water Resources Division of the U.S. Geological Survey, Denver, Colo., received his BS in chemistry and his PhD in chemistry and metallurgy in 1939 and 1949, respectively, from the University of Wisconsin. He served in chemistry and teaching positions at Washburn Co., Rockford, 111.; Fairbanks-Morse and Co., Beloit, Wis.; and St. Olaf College, Northfield, Minn., before joining the U.S. Geological Survey in 1958. His research interests are centered on the occurrence and distribution of minor elements in water, development and standardization of methods for water analysis, and methods of determining minor elements in water. He is active in professional societies, including the ACS, SAS, ASTM, and is chairman of Technical Committee 147 on Water of the International Standards Organization.
from different laboratories are used to evaluate theoretical hydrogeochemical principles. As a part of a program for evaluating the various analytical methods used by leading analytical laboratories around the world, as many as 25 or 30 worldwide laboratories are conducting a round-robin analysis program involving seven natural water samples of widely different types, including both surface and ground waters, and for both common and unusual constituents. The results of this testing program will be summarized and presented at a Symposium on the Geochemistry of Natural Waters to be held in Burlington, Ont., Canada, in the summer of 1975. Data have already been submitted by participating laboratories for the analysis of three samples, and other samples are being prepared for distribution. Prominent water analysis laboratories in Canada, United Kingdom, Australia, New Zealand, Sweden, Norway, Japan, USA, USSR, and
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other countries are involved in this round-robin study. This cooperative program should lead to a revelation of interesting facts concerning interlaboratory test data and the reliability of various analytical methods applied to different types of waters. National and International Standardization With so many agencies and organizations involved and with so many technical experts participating, both in this country and worldwide, there can be real hope that truly national and international agreement can eventually be reached on standardization of methods and techniques for assessing the real condition of national and international waters. The exchange of technical experience and information that takes place as a consequence of these efforts at standardization serves to assist the member countries in their efforts to deal with water-pollution problems that are common to all.
