United States Environmental Protection Agency Environmental Monitoring Systems •• Laboratory * r t \ \ Research Triangle Park NC 27711 Research and Development EPA-600/S4-81-074 Sept. 1981 Project Summary Air Quality Data for IMonmetallic Inorganic Ions: Nitrate and Sulfate for 1977 and 1978 from the National Air Surveillance Networks Gary F. Evans, John C. Puzak, John E. Frazer, and Allan Riley The National Air Surveillance Net- works provide information on air quality for many urban and nonurban Jocations within the United States. This report summarizes the network data for two nonmetallic inorganic ions (nitrate and sulfate) determined from high volume samples collected during 1977 and 1978. Concentration values are presented in the form of cumulative frequency distributions. Arithmetic and geometric sample statistics are also reported, as are measures of the precision and bias associated with the analytical methods employed. This Project Summary was devel- oped by EPA's Environmental Moni- toring Systems Laboratory, Research Triangle Park, NC. to announce key findings of the research project that is fully documented in a separate report of the same title (see Project Report ordering information at back). Introduction The U.S. Environmental Protection Agency (EPA) conducts a variety of air sampling activities to obtain information about the quality of the nation's air. Often this work is accomplished with the assistance and cooperation of state and local government agencies. One such program consists of the National Air Surveillance Networks (NASN) which have reported air quality data for more than 20 years. Although the operation of the sampling sites is decentralized, the determination and publication of trace pollutant concen- trations remains the responsibility of EPA's Environmental Monitoring Sys- tems Laboratory at Research Triangle Park (EMSL/RTP). The air quality monitoring stations of the NASN are located throughout the country in areas originally classified as urban or nonurban. Urban-classified sites were generally located within a city, town, or adjacent suburb. Non- urban-classified sites were originally located in rural or remote areas; but, over time, many of these areas became more heavily populated and subjected to the influences of spreading urban- ization. This report summarizes the 1977 and 1978 network data for nitrate and sulfate ions. Procedure Laboratory Methods Preweighed glass-fiber filters were distributed to the cooperating local ------- agencies for sample collection. After high volume sampling, the filters were returned to the EPA for final weighing and chemical analysis. Analyses for inorganic ions during 1977 and 1978 were performed by Northrop Services, Incorporated - Environmental Sciences, under Contract No. 68-02-2566. An 8.3 percent section of each particulate filter was cut and extracted in water for autoanalysis. The analytical procedure for each ion was as follows: 1. The aqueous extract was analyzed for nitrate ion by reduction of the nitrate to nitrite by a copper-cadmium reduction column. The nitrate was reacted with sulfanilamide in acidic solution to form a diazo compound. This compound then coupled with N- 1 -naphthylene diamine dihydrochlor- ide to form a reddish-purple azo dye which was determined colorimetri- cally at a wavelength of 520 to 540 nm. 2. The extract was analyzed for sulfate ion by the methylthymol blue (MTB) method using a single channel Technicon Autoanalyzer II system equipped with a linearizer. The MTB method is based on the spectral difference which exists in basic solution (pH 12.5 to 13.0) between the barium complex of MTB and free MTB. At this pH, the barium complex is blue and free MTB is brownish-red (absorbs light at 460 nm). Thus, the color of solutions containing both the free MTB and the complex appears as gray. The amount of free MTB, monitored colorimetrically at wave- lengths of 460 to 480 nm, was the measure of the amount of sulfate in the sample. Quality Assurance Methods Independent estimates of laboratory precision and bias were determined for these data to aid in interpreting analyt- ical results. However, several potential sources of measurement error associ- ated with sample collection and handling procedures (flow control, artifact forma- tion, shipping and storage losses, etc. that were not directly controlled by EMSL/RTP) were not considered in the estimates of data quality presented here. Analytical precision estimates are based upon percent differences deter- mined from analyses of two filter strips taken from the same filter. Thus, the measure of precision includes variation caused by cutting, extracting, and analytical processing as well as any actual differences which may exist between filter strips. Duplicate strips of every 20th sample were analyzed for the purpose of estimating precision. Analytical bias estimates were ob- tained through an audit program in which "spiked" filter strips were introduced into the ambient air sample group for routine ana lysis. These quality assurance samples contained known quantities of each ion and thus provided a measure of analytical recovery and its complement, bias. Every 2 weeks a set of 10 audit samples was provided to the analytical laboratory for inclusion in the routine sample processing. Estimates of bias and precision for the 1977 and 1978 analytical results are given by concentration range in Table 1. Results and Conclusions Data are presented in Tables 2 and 3 in the form of annual cumulative frequency distributions by ion for urban and nonurban locations, respectively. In the first line of Table 2, the number 3900 is the number of valid 24-hr samples analyzed for nitrate in 1971. The next entry is the minimum value detected that year, and "LD" means below the minimum detectable level of the instrument. The next seven entries are the 10 through 99 percentile values. For example, the 90 percentile value of 5.02 indicates that 90 percent of the 3900 values, i.e., 0.90 x 3900 = 3510, were equal to or less than 5.02 pg/m3. The next entry is the maximum annual value. Arithmetic means and standard deviations, and geometric means and geometric standard deviations are presented in the lastfour columns in the table. Comparison among years for a given pollutant provides a relative Table 1. Analytical Precision and Bias indication of national trends. Nitrate ion concentrations, for example, have apparently increased over the 8-year period in both urban and nonurban areas, while sulfate ion concentrations have remained relatively consistent. Since typical levels of these pollutants may be geographically dependent, the national frequency distribution is not helpful for judging the localized contri- bution and relative severity of these pollutants for an individual site. There- fore, local site analyses should be performed with data from surrounding sites within the same general geo- graphical area. Data for each site are presented in the project report. Also, some of the variability from year to year in the national summary tables may be attributed to different sets of sites being used in the summarization. A. 1977 B. 1978 Ion Nitrate Sulfate Nitrate Sulfate Concentration Range (ug/m3) <3 3-6 >6 <6 6-20 >20 <3 3-6 >6 <6 6-20 >20 Bias (%l +0.7 -5.6 -2.8 -6.8 -5.3 -5.9 +6.8 -4.5 -1.2 -7.3 -3.7 -5.5 Precision (%) 12 8 8 9 5 3 21 11 24 11 9 4 ------- Table 2. Urban National Cumulative Frequency Distributions Number Percent of time concentration (fjg/m3) is equal to or less than Arithmetic statistics Geometric statistics of Ion Year Samples Min. NO1 1971 3900 LD 1972 5519 LD 1973 4775 LD 1974 4562 LD 1975 4113 0.20 1976 3817 0.08 1977 4531 0.07 1978. 3610 LD SOI 1971 3916 LD 1972 5519 LD 1973 4774 LD 1974 4564 LD 1975 4110 0.2 1976 3871 0.2 1977 4531 0.7 1978 3610 LD 10 0.69 0.66 0.81 0.83 0.96 1.07 1.07 1.08 3.4 3.9 3.9 3.9 3.5 3.1 3.1 3.1 30 1.55 1.58 1.71 1.74 2.00 1.99 2.09 2.21 5.7 6.7 6.3 6.3 6.1 5.4 5.7 5.7 Table 3. Nonurban National Cumulative 50 2.29 2.47 2.58 2.54 2.91 2.80 2.99 3.24 8.0 9.4 8.1 8.3 8.3 7.4 7.6 7.8 70 3.22 3.55 3.65 3.63 4.12 3.83 4.15 4.56 10.9 12.7 10.9 11.3 11.5 9.9 10.3 10.6 90 5.02 5.90 6.24 6.46 7.18 6.48 6.76 7.78 18.0 20.3 17.5 17.9 18.1 16.5 17.1 16.6 95 6.48 7.88 8.31 8.62 9.90 9.53 10.40 11.18 22.0 25.4 22.7 22.8 23.8 20.0 20.9 20.4 99 11.85 13.50 14.61 17.50 17.07 20.65 20.63 22.91 33.5 37.9 35.4 34.8 35.8 29.2 29.9 34.5 Max. 26.17 24.99 37.36 54.89 33.71 43.16 97.67 56.96 69.2 75.9 162.0 69.1 72.6 66.7 76.4 228.4 Mean 2.77 3.05 3.25 3.36 3.73 3.71 3.89 4.22 9.6 11.1 9.9 10.0 10.O 8.8 9.1 9.4 Std. Dev. Mean 2.30 2.13 2.61 2.32 2.87 2.44 3.40 2.36 3.31 2.79 3.83 2.58 3.97 2.87 4.10 3.07 6.8 7.84 7.7 9.15 7.0 8.06 6.7 8.34 7.0 8.22 5.8 7.33 6. 1 7.44 7.5 7.55 Std. Dev. 2.06 2.10 2.13 2.32 2.15 2.34 2.18 2.26 1.89 1.87 1.89 1.83 1.88 1.83 1.72 1.95 Frequency Distributions Percent of time concentration Number of Ion Year Samples Min. NOl 1971 671 LD 1972 928 LD 1973 831 LD 1974 706 LD 1975 630 0.20 1976 467 LD 1977 681 LD 1978 458 LD SOI 1971 686 0.4 1972 929 LD 1973 831 LD 1974 706 0. 1 1975 630 0.2 1976 493 0.2 1977 681 LD 1978 458 LD is equal to or 10 0.06 LD 0.04 0.12 0.20 0.10 0.17 0.30 1.5 1.4 1.3 1.4 0.7 0.9 1.2 1.2 30 0.31 0.15 0.28 0.37 0.20 0.36 0.55 0.59 3.0 2.9 2.7 2.6 2.1 1.8 2.5 3.0 50 0.71 0.50 0.71 0.83 0.73 0.82 1.05 1.07 4.7 5.2 4.4 4.8 4.0 4.0 4.7 4.9 70 1.20 1.01 1.26 1.37 1.41 1.51 1.81 2.03 7.2 7.8 6.3 7.2 6.4 6.5 7.4 7.2 ffjg/m3) Arithmetic Geometric less than 90 2.19 2.08 2.35 2.52 2.74 2.82 3.07 3.77 11.8 13.7 12.0 12.2 11.6 11.3 12.8 13.4 95 2.67 2.59 2.83 3.16 3.28 3.54 3.84 4.74 15.5 17.4 17.0 16.6 15.2 13.9 17.1 17.0 99 3.81 4.19 4.47 5.13 4.85 4.73 5.22 8.09 23.6 24.8 29.8 27.0 28.7 21.3 24.6 21.0 Max. 6.04 6.59 6.67 6.65 11.85 6.15 11.57 11.77 35.4 42.7 53.2 90.0 48.3 36.3 43.3 38.5 statistics statistics Mean 0.95 0.79 0.99 1.10 1.13 1.18 1.39 1.69 6.0 6.6 6.0 6.2 5.5 5.3 6.1 6.2 Std. Dev. Mean 0.92 0.68 0.92 0.52 1.02 0.69 1.07 0.79 1.16 0.78 1.16 0.84 1.26 0.85 1.72 1.06 4.9 4.7 5.4 5. 1 5.9 4.2 6.2 4.4 5.7 3.8 4.9 3.8 5.4 4.0 5.3 4.2 Std. Dev. 2.26 2.52 2.34 2.25 2.35 2.27 3.21 2.78 2.03 2.05 2.29 2.30 2.36 2.22 2.72 2.71 ------- The EPA authors Gary F. Evans (also the EPA Project Officer, see below). John C. Puzak, John E. Frazer, and Allan Riley, are with the Environmental Monitoring Systems Laboratory, Research Triangle Park, NC 27711. The complete report, entitled "Air Quality Data for Nonmetallic Inorganic Ions: Nitrate and Sulfate for 1977 and 1978 from the National Air Surveillance Networks," (Order No. PB 81 -248 148; Cost: $ 12.50, subject to change) will be available only from: National Technical Information Service 5285 Port Royal Road Springfield, VA 22161 Telephone: 703-487-4650 The EPA Project Officer can be contacted at: Environmental Monitoring Systems Laboratory U.S. Environmental Protection Agency Research Triangle Park, NC 27711 US GOVERNMENT PRINTING OFFICE; 1981 —559-017/7432 United States Environmental Protection Agency Center for Environmental Research Information Cincinnati OH 45268 Postage and Fees Paid Environmental Protection Agency EPA 335 Official Business Penalty for Private Use $300 2 10* ------- |