I • <$• I 55 V ^ LLl O CENTRAL REGIONAL LABORATORY REGION V ------- :RONMENTAL PROTECTION AGEK< ------- aboratory Introduction and Background The Central Regional Laboratory (CRL), located on Chicago's near south side, provides scientific expertise for the U.S. Environmental Protection Agency as well as State and local pollution control agencies in Region V (Illinois, Indiana, Michigan, Minnesota, Ohio and Wisconsin). In EPA's early days, shortly after it was established in December, 1970, there were five laboratories in Region V. One located at each of five District Offices in Evansville, IN; Minneapolis, MN; Grosse lie, Ml; Cleveland, OH; and, Chicago, IL. The purpose of these laboratories was to test environmental samples collected by District Office field operations teams. Although this laboratory system served an important function, it soon became apparent that such a method of organization was not economical ly sound nor did it provide a scientific base to support the more difficult, expensive and unusual tests required by the Region. On Feb. 5, 1973, Francis T. Mayo, Midwest Regional Administrator of the U.S. EPA, reorganized the Region's laboratory operations to create the Central Regional Labo- ratory, a major environmental testing facility, in the Surveil- lance and Analysis Division (S&AD). District offices will continue to maintain small scientific staffs to perform time dependent analyses and ship samples to the CRL for all other analyses. r ------- Francis T. Mayo—Regional Administrator Valdas V. Adamkus—Deputy Regional Administrator Christopher Timm—Director, Surveillance & Analysis Division Through the work of the scientists and staff personnel, the CRL is accomplishing its prime mission—performing and evaluating environmental measurements for regulatory actions, evaluating ambient environmental quality and sup- porting State and local government environmental agencies in the Region. In late 1974 and early 1975, the CRL performed over 100,000 chemical and biological analyses. The source of samples for analysis ranged from the open waters of the Great Lakes to the bottom sediments of the Mahoning River in Ohio. On many occasions, CRL has been requested to analyze samples for which accurate analytical methods do not exist, such as organics in bottom sediments. To meet this de- mand, the CRL is actively developing analytical procedures to better support existing environmental programs, as well as developing the capability to handle new programs. In order to efficiently handle the heavy routine workload, the CRL continually investigates methods for automating existing analytical procedures. During FY75, automated methods for analysis of mercury and chemical oxygen demand were developed and approved for use with the National Pollutant Discharge Elimination System (NPDES) by the Regional Administrator. Two gas chromatographs were automated and compu- terized to allow unattended analyses of 55 pesticides. In addition, a new plasma source emission spectrometer was placed in operation which performs 20 metal analyses simultaneously. Another very important function at the CRL is conducting training seminars for State and local agencies. In methods development, the CRL gives considerable attention to the possibility that the new techniques can be adopted and used by other EPA, State, local, and private laboratories. These seminars serve to transfer the latest technology de- veloped at the CRL to these environmental agencies for their application. The CRL staff presently numbers about 30 and is divided into four major sections: 1. Administration; 2. Chemistry Branch; 3. Biology Branch; and 4. Quality Assurance Branch. Art direction and photography by the Graphic Arts Section, U.S. EPA, Region V. ------- ADMINISTRATION The Director's office, which is responsible for the admin- istration of the CRL, consists of a Director, Deputy Director and a Program Technician. The Director and Deputy Direc- tor provide coordinated program development, direction and control. They formulate and execute short and long range plans for optimum utilization of resources to insure meeting the responsibilites, obligations and commitments of the CRL. Day-to-day laboratory operations are delegated to the Branch Chiefs. The Program Technician is responsi- ble for fiscal, procurement, property, personnel and other administrative matters that support the operation of the CRL. John Quarles—Deputy Administrator, U. S. EPA; Dr. Abbas E/-Awady—Chemist; Thomas Yeates—Director, Central Regional Laboratory; and, Christopher Timm—Director, Surveillance & Analysis Division, discuss the development of the automated cyanide analysis system (l-r). ------- A sample is injected into a total organic carbon analyzer. A gas chromatograph equipped with flame photometric detectors sensitive to phosphorus and sulfur is used to identify oil pollutants. A water blank is aspirated into the flame of an atomic absorption spectrometer to insure that the instrument is operating properly. J ------- CHEMISTRY BRANCH The Chemistry Branch, by far the largest division in the CRL, is comprised of the Inorganic, Metals and Organic Sections. It has the capability to routinely perform over 100 different parameter analyses on each sample submitted. The samples consist of industrial and domestic waste- waters; lake, river and ground waters; and, drinking water supplies. Other samples include sludges, soils and sedi- ments, biological specimens, solid and liquid fuels and gaseous and impinged air. The bulk of the workload, at this time, consists of con- ducting analyses on water samples obtained from industrial and municipal discharges. By analyzing for the amounts of various substances present in these effluent waters, it is possible to determine whether a given facility is meeting the conditions for discharge set forth in its NPDES permit. The permit is, in essence, a contract between the Govern- ment and the facility, which defines maximum amounts of each chemical that can be discharged to a receiving stream and still maintain good water quality. The branch is currently very active in developing and implementing an automated computerized laboratory system in cooperation with the EPA Environmental Moni- toring and Support Laboratory in Cincinnati, Ohio. In July, 1975, the CRL began installing a new NOVA 840 computer system which will enter data from the lab instru- ments directly into a national EPA data bank for future retrieval. This will eliminate the need to keypunch data for the Washington computer and will reduce turn-around time for users. Software for this new data processing system is being written at the Lawrence Livermore Laboratory at the Univer- sity of California, Berkeley. This system in Region V, when operable, will serve as a pilot for other EPA Regional labs. The new computer system is being designed to handle: • data listing related to samples to be collected for analyses • data storing of all measured values • operation of laboratory instruments including calibration and statistical analysis on instrument variables and finished data • production of comprehensive labels for samples • multiple typing projects • other routine computer functions At the present time, the CRL manually processes data to support over 125,000 analyses per year. With the new computer system, it will be able to handle 1000 pieces of data per day. A gas chromatograph and associated equipment in operation to measure the amount of chloroform and related pollutants in drinking water. ------- The technicon Auto Analyzer II system automatically determines the concentration of ammonia, nitrate and nitrite and ortho phosphate at the rate of forty samples per hour. Inorganic Section J Scientists of the Inorganic Section of the Chemistry Branch analyze surface and wastewaters, air, fuel and sediment samples for nutrient, oxygen demand, mineral, physical and air pollution parameters. Approximately 2/3 of the resources of the Inorganic Section are devoted to water and sediment testing for about 30 parameters. Automated methods using Technicon Auto Analyzer equipment are used to test for the frequently-run parame- ters, such as ammonia, nitrate plus nitrite, total phosphorus, chemical oxygen demand, mercury, chloride and sulfate at an average rate of 30 samples per hour. Since instruments perform the repetitive and more tedious tasks in the testing procedures, scientists have more time to interpret the data and develop new procedures. In order to analyze large numbers of difficult samples such as Great Lakes' waters, sediments and industrial wastes, the Inorganic Section has developed several new analytical methods. Automated methods for the analysis of chemical oxygen demand and mercury were developed in FY75 and approved for use with the NPDES permits. In addition, micro methods for the analysis of dissolved and suspended solids were also developed. In addition to devising new and more efficient methods of performing sample tests, the Section is conducting preser- vation studies on samples so that they can be held for longer periods than are now allowed. At present, some of the water samples collected in the field must be tested almost imme- diately in order for the results to be valid. When implemented, the efficiency of the District Office sampling teams could be greatly increased. Teams could stay in the field for longer periods, collecting additional samples and the samples could then be held until there is a large enough number for analyses to make automation more efficient. Any headway in this area will have a tremen- dous effect on how the CRL and the S&AD operate, as well as State Pollution Control agencies. More air testing is done in thisSection than in any other section of the Chemistry Branch—about 1 /3 of their total testing time is spent with air samples. Ambient air samples are collected every 12 days by equipment set up and cali- brated by other offices. These samples are then sent to the CRL and analyzed for total particulates, sulfur dioxide and nitrogen dioxide. The analytical results which determine the trend of air quality in Region V are stored in an EPA national air data bank located in North Carolina. The Inorganic Section routinely participates with EPA and ------- The measurement of total organic carbon, an important pollution indicator. other governmental agency air pollution control laboratories in special analytical studies. The scope of studies includes evaluating methods of sampling and analysis for mercury in stack and ambient air samples and the effect of shelter size on the collection efficiency of suspended particulate matter in the air. A recent study by the Section which shows that two auto- mated methods for the analysis of sulfur dioxide in impinged air samples are equivalent to the EPA approved manual method will result in a substantial increase in efficiency of State and local air pollution control laboratories. The air pollution scientists also maintain a calibration and auditing capability to assist the State and local agencies with continuous sulfur dioxide, nitrogen dioxide and ozone air monitors. Distillation apparatus for manually measuring the cyanide concentration of environmental samples. &m An ultrasensitive Microbalance is used to weigh materials to within one millionth of a gram. Calibration of an ozone monitor with a dynamic calibration system. ------- Samples are digested in concentrated acids before they are analyzed for metals. Metals Section Determination of arsenic using a heated graphite atomizer at 2700° C. A "Lead Free" gasoline sample is analyzed for lead content by an atomic absorption spectrometer. The Metals Section is primarily concerned with the test- ing of water, sediment and air samples for the presence and quantification of metallic elements, compounds and related components. By using chemical and physical methods of analysis and applying various analytical techniques, the scientists rou- tinely test for 30 different metals. The results of many of these tests are used to determine compliance for the dis- charger as defined by his NPDES permit. Currently, most of the metal analyses are performed by atomic absorption spectrophotometry. The sample is atom- ized either in a flame or an electrically heated furnace and monochromatic light is passed through the cloud of neutral atoms. The concentration of a single metal can be deter- mined by the amount of specific light the particles absorb. In flame atomic absorption, the Section has automated alkali and alkaline earth determinations by applying current state-of-the-art automatic sampling techniques. This approach provides for an increase in productivity and a decrease in operator-related errors. Some bodies of water, i.e. the Great Lakes, are so low in metal content that the traditional flame atomic absorption procedures lack the required sensitivity for a meaningful characterization. As a consequence, flameless methods have been devel- oped and are currently being used which are capable of detecting element concentrations in the low part per billion (10~9 grams per liter) range. This generates data that are useful as baseline information for the assessment of envi- ronmental water quality trends. As with all of the testing procedures employed in the CRL, only those that are EPA approved can be used to monitor for permit compliance. The Metals Section is evaluating a new "emission spec- trometer-inductively coupled argon plasma system" which can perform tests for 20 parameters simultaneously, as opposed to one at a time by atomic absorption. Although this is not yet an EPA approved method, prelim- inary data indicate that this approach will justify acceptance and result in substantial time-savings, not only for the CRL, but also for the many environmental laboratories in EPA and State agencies. In the areas relating to air pollution problems, the Metals Section is currently testing levels of lead in gasoline. The District Offices, with the aid of portable testing kits, perform on-site analyses at gas stations. ------- Analysis of a water sample for magnesium by atomic absorption spectrometry. Any samples registering lead contents above 0.04 grams/ gallon are sent to the CRL where rigorous tests are per- formed to determine if the gasoline supply is contaminated. Any level of lead above O.OSgrams/gallon signifies contam- ination, and prohibits the sale of the gasoline. Although smaller in scope, the characterization of air particulate samples for trace metals is an on-going activity. As with all of the Sections in the CRL, the Metals Section develops, implements and maintains a state-of-the-art ana- lytical quality control program to insure that data generated are within the accuracy range of the methods used to pro- duce the results. Simultaneous multielement analysis of twenty metals by direct sample nebulization using an inductively coupled argon plasma optical emission spectrometer. ------- An infra-red spectrometer is calibrated before being used to identify oils and other organic compounds. Organic Section A high pressure liquid chromatograph is used to purify a sample for subsequent analysis. The primary function of the Organic Section, as with the other Sections of the Chemistry Branch, is to test water, air and biological samples for environmental pollutants. Since there is an extremely large number of organic or carbon containing molecules in the environment, the Or- ganic Section must allocate considerable resources just to identify which organic pollutants are present in a sample. Once this qualitative analysis has been completed, the process of measuring the amount of each organic material in the sample can begin. Frequently, over one hundred different organic pollutants are found in a single water or air sample, and there is seldom enough resources to complete quantitative analyses on all compounds. Therefore, emphasis is placed on those materials that are known or suspected to be highly toxic or carcinogenic. The highly competent staff has many sophisticated instru- ments with which to perform these difficult analyses. In addition to a number of gas chromatographs, there is a nuclear magnetic resonance spectrometer, a liquid chro- matograph, a gas chromatograph/mass spectrometer and several infrared spectrometers. The largest class of organic pollutants studied by the Organic Section this past year was pesticides. This class of chemicals include selected chlorinated hydrocarbon, organ- ophosphorus, organosulfur compounds, the phthalates and polychlorinated biphenyls (PCB's). A semiautomated analysis system in which a computer operates and collects data from several different kinds of gas chromatographs was developed to handle the workload for these programs. The system is used to routinely screen samples for 55 pesticides. These analyses are performed at a rate of over 24,000 reported concentration values per year. Pesticides not included in this group of 55 require much more time to identify and quantify. The Section has also developed and implemented a sim- ple, but highly effective, method of measuring the concen- trations of volatile organic compounds such as chloroform in drinking waters. Hundreds of these analyses were per- formed on Region V drinking water supplies to establish baseline concentrations of these materials. Programs to identify causes for taste and odor problems in both air and water have been initiated, and many samples were analyzed during the first program year. New tech- niques are continually being studied to provide more capa- bilities in this area. The Section supports the U.S. Coast Guard, State and ------- A computer is being programmed which is interfaced to four gas chromatographs equipped to analyze pesticides on an around-the-clock basis. other Federal agencies by performing oil and hazardous material identifications. When a spill occurs, samples are sent to the CRL for immediate analysis and the spill is moni- tored to assess damage to the environment. The analytical result will determine the actions to be taken by the govern- ment officials to protect the public and wildlife. In these situations, it is imperative that the CRL be re- sponsive and accurate. If the spilled material is identical to that from a suspected source, the responsible parties can be identified and appropriate enforcement actions taken. The Organic Section scientists pride themselves in often being able to provide technical assistance to other Federal, State, and local environmental regulatory agencies and to analyze some of the most difficult environmental samples. Unknown organic compounds are frequently identified by a gas chromatograph-mass spectrometer-computer system. ------- BIOLOGY BRANCH The Biology Branch provides biological and microbiolog- ical support for the Region. Emphasis is given to the areas of fish, macro-invertebrate and algal bioassays for toxic materials. It is also well equipped to perform detailed tax- onomy on many different kinds of aquatic organisms. V The Biology Branch develops new field and laboratory procedures and guidelines to more effectively evaluate biological conditions in lakes and streams throughout the Region. This includes such aspects as sediment bioassays for determining toxicity levels in the Great Lakes harbor sedi- ments ; on-site adenosine triphosphate (ATP) photometric analysis of biomass in areas of municipal and industrial dis- charges; and, mobile field bioassay testing. It also offers technical support to State and local agencies when re- quested and serves as a member of the National Biological Advisory Committee. The Branch is divided into two sections: a Bioassay-ln- vertebrate Section and a Plankton-Periphyton Section. Analysis of a diatom slide to determine the proportional count of the diatom species. J ------- Pennate diatom—Cymbella sp. ^Cj> •'^ Zooplankton—Daphnia sp. i Assortment ofplanktonic algae. Head capsule of the chironomid larva—Tribelos sp. PHOTOMICROGRAPHS OF PLANCTONIC AND BENTHIC AQUATIC ORGANISMS 'ooplankton—Bpsmina longirostris —Pinnularia sp. ------- Bioassay- Invertebrate Section Major emphasis is given to toxicity testing with fish, macro-invertebrates and algae. Both static and continuous flow tests are run on such organisms as fathead minnows, goldfish, algae and Daphnia—a small crustacean. All test organisms, except goldfish, are hatched, reared or cultured at the CRL in order to maintain an adequate supply of organisms of the highest quality. The minnows are raised in a specially designed system developed at the CRL to operate using dechlorinated tap water and is temperature controlled by a series of solenoid switches working off the regular hot and cold tap water. A total of 400 to 600 min- nows can be hatched weekly. The bioassay experiments consist of observing the re- action of the organisms when placed in water containing varying amounts of specific toxic chemicals or industrial plant effluents. This is done to determine the lethal levels for the organisms in an attempt to understand what effects pollutants discharged in our waterways have on aquatic life. In support of these areas of testing, a 19 foot mobile bio- assay trailer designed for running continuous flow and static bioassays at on-site locations is used. The trailer, manned by CRL personnel, will be used Region-wide to test the toxicity of industrial effluents in the field for a continuous 96 hour period. It can be moved easily from one location to another and is equipped for use during all seasons of the year. Other functions of this Section include conducting de- tailed identification and enumeration of macroinvertebrate organisms and biomass determinations. In order to perform species identification on some organisms, it is necessary to extractor prepare certain anatomical structures through special techniques. These techniques are being employed routinely at CRL in all phases of taxonomy. All microbiological functions are also a part of the Bio- assay Invertebrate Section, and include bacteriological ex- aminations of freshwater, domestic and industrial effluents. (A) Fathead minnow eggs attached to the underside of spawning tile. (6) Harvesting brine shrimp from a hatcher that will be fed to fathead minnows. (C) Brine shrimp are fed to newly-hatched minnows. (D) Eight-week-old fathead minnows. (£) Static bioassay being conducted on an industrial waste sample in an environmental chamber. ------- ,*. * Male and female fathead minnows under spawning tile. ------- Plankton-Periphyton Section Determination of chlorophyll a by spectrofluorometry. This Section conducts identification and enumeration of phytoplankton, zooplankton and periphyton on samples collected throughout the Region. These organisms are an important group as indicators of the trophic status of a particular body of water and contri- bute significantly to the total productivity of any given aquatic system. Some are also notorious in causing taste and odor problems in municipal water supplies or off-flavors in commercial or sport fishes. DetaNed species identifica- tion is often necessary in order to identify the algae causing these problems and this capability is available at the CRL. Another important function of this Section is in running algal bioassays in conjunction with the Bioassay-lnverte- brate Section. A series of pure cultures of algae are main- tained at CRL as test organisms. The specimens are sub- jected to predetermined concentrations of a known toxicant or to a municipal or industrial effluent and specific observa- tions are then made to determine the effect of these test materials on the algae. In addition, the algalogists also examine the productivity of the water by means of spectrophotometric and fluoro- metric analysis of chlorophyll, ATP photometry, and ash- free dry weight determinations. Photomicrograph of the zooplankton Keratella quadrate. Environmental Protection Agency Region V, Library 230 South Dearbo'rn Street Chicago, Illinois 60604 Pure cultures of algae being grown in an environmental chamber. i *U.S. GOVERNMENT PRINTING OFFICE: 1975—652-998 ------- QUALITY ASSURANCE BRANCH The Quality Assurance Branch is responsible for quality assurance management in the S&AD and draws upon the resources of the S&AD to carry out this function. The Branch develops and implements, on a continuing basis, a quality assurance management plan for the division. The plan sets policy for the quality of the division's moni- toring data; details operating procedures for sample collec- tion, preservation, analysis, and data reporting; and speci- fies calibrations and audits required. The Branch Chief serves as the Regional Analytical Quality Control Coordi- nator to assure implementation of national quality assurance policies of EPA. The Branch recommends approval or disapproval to the Regional Administrator of alternate test procedures for the NPDES. This very important function has considerable impact on the validity of the data generated by the industrial and municipal dischargers. The Branch, in coordination with the U.S. EPA District offices, evaluates State labora- tories. Through the presentation of seminars, the use of refer- ence samples, split samples, and on-site visits, the Branch provides support to the States for upgrading data quality. It assists the States in developing and implementing a quality assurance program to assure that only approved field and laboratory procedures are being used. The Branch also actively works within the Great Lakes monitoring activities of the International Joint Commission Water Quality Board to implement and coordinate interlabo- ratory quality assurance. It is necessary for data provided by Canadian and United States agencies to be of quantified validity so that water quality assessments, such as long-term trends of the Great Lakes, can be made more accurately. The Branch receives hundreds of requests for technical information of a non-routine nature from State and local pollution control agencies, private laboratories and indus- trial and municipal dischargers. It also serves as a distribu- tion point for EPA's publications on analytical methodology and quality assurance. Dr. Mark Carter—Chief, Inorganic Section and David Payne—Chief, Quality Assurance Branch, discuss the Inorganic Section's quality assurance program (l-r). ------- UNITED STATES OF AMERICA ENVIRONMENTAL PROTECTION AGENCY REGION V CENTRAL REGIONAL LABORATORY 1819 W PERSHING RD CHICAGO, ILLINOIS 60609 AN EQUAL OPPORTUNITY EMPLOYER POSTAGE AND FEES PAID ENVIRONMENTAL PROTECTION AGENCY EPA-335 OFFICIAL BUSINESS PENALTY FOR PRIVATE USE. S3OO ------- |