[(C+C2)-(B) +B2)] AOX(ug/L)=

V Cirug Cl- from micro-coulometer for first

column from the sample C2=ug Cl- from micro-coulometer for second

column from the sample B;=ug from micro-coulometer for first col

umn from the reagent water blank (Sec

tion 9.4.1) B2=ug Cl - from micro-coulometer for second

column from the reagent water blank (Sec

tion 9.4.1) V=volume of sample in liters

12.3 Percent breakthrough: For each sample analyzed by the column method, calculate the percent breakthrough of halide from the first column to the second column, using the following equation:

has been diluted, analyze a less dilute aliquot of sample.

12.6.3 If the instrument response of an undiluted sample containing AOX above the minimum level is less than three times the instrument response for the blank, the result is suspect and may not be used for regulatory compliance purposes. In this case, find the cause of contamination, correct the problem, and reanalyze the sample under the corrected conditions.

12.7 Report results that meet all of the specifications in this method as the mean of the blank-subtracted values from Section 12.1 or 12.2 for the two analyses at different dilution levels, in ug/L of Cl- (not as 2,4,6trichlorophenol), to three significant figures. Report the RPD of the two analyses. For samples analyzed by the column procedure, also report the percent breakthrough.

13.0 Method Performance The specifications contained in this method are based on data from a single laboratory and from a large-scale study of the pulp and paper industry.

(C2-B2)(100) % Breakthrough =

[(C, -B.)+(C2-B2) 12.3.1 For samples to be reported for regulatory compliance purposes, the percent breakthrough must be less than or equal to 25% for both of the two analyses performed on each sample (see Section 11.5).

12.3.2 If the breakthrough exceeds 25%, dilute the affected sample further, maintaining the amount of halide at least three times higher than the level of blank, and reanalyze the sample. Ensure that the sample is also analyzed at a second level of dilution that is at least a factor of 2 different (and still higher than three times the blank).

12.4 Relative percent difference (RPD): Calculate the relative percent difference between the results of the two analyses of each sample, using the following equation:

14.0 Pollution Prevention 14.1 The solvents used in this method pose little threat to the environment when recycled and managed properly.

14.2 Standards should be prepared in volumes consistent with laboratory use to minimize the volume of expired standards to be disposed.

12.5 High concentrations of AOX: If the amount of halide from either analysis exceeds the calibration range, dilute the sample and reanalyze, maintaining at least a factor of 2 difference in the dilution levels of the two portions of the sample used.

12.6 Low concentrations of AOX: The blank-subtracted final result from the batch procedure or the sum of the blank-subtracted results from the two carbon columns should be significantly above the level of the blank.

12.6.1 If the instrument response for a sample exceeds the instrument response for the blank by a factor of at least 3, the result is acceptable.

12.6.2 If the instrument response for a sample is less than three times the instrument response for the blank, and the sample

15.0 Waste Management 15.1 It is the laboratory's responsibility to comply with all federal, state, and local regulations governing waste management, particularly the hazardous waste identification rules and land disposal restrictions, and to protect the air, water, and land by minimizing and controlling all releases from fume hoods and bench operations. Compliance with all sewage discharge permits and regulations is also required.

15.2 Samples preserved with HCl or H2SO. to pH <2 are hazardous and must be neutralized before being disposed, or must be handled as hazardous waste. Acetic acid and silver acetate solutions resulting from cell flushing must be disposed of in accordance with all applicable federal, state, and local regulations.

15.3 For further information on waste management, consult “The Waste Management Manual for Laboratory Personnel," and “Less is Better: Laboratory Chemical Management for Waste Reduction,” both available from the American Chemical Society's Department of Government Relations and Science Policy, 1155 16th Street NW., Washington, DC 20036.

16.0 References 16.1 Total Organic Halide, Methods 450.1–Interim," Prepared by Stephen Billets and James J. Lichtenberg, USEPA, Office of Research and Development, Physical and Chemical Methods Branch, EMSL-Cincinnati, Cincinnati, OH 45268, EPA 600/4-81056 (1981).

16.2 Method 9020, USEPA Office of Solid Waste, Test Methods for Evaluating Solid Waste, SW-846." Third Edition, 1987.

16.3 "Determination of Adsorbable Organic Halogens (AOX)," "German Standard Methods for the Analysis of Water, Waste Water and Sludge-General Parameters of Effects and Substances," Deutsche Industrie Norm (DIN) Method 38 409, Part 14, DIN German Standards Institute, Beuth Verlag, Berlin, Germany (1987).

16.4 "Water Quality: Determination of Adsorbable Organic Halogens (AOX)." International Organization for Standard/Draft International Standardization (ISO/DIS) Method 9562 (1988).

16.5 "Organically Bound Chlorine by the AOX Method." SCAN-W 9:89, Secretariat, Scandinavian Pulp, Paper and Board Testing Committee, Box 5604, S-11486, Stockholm, Sweden (1989).

16.6 Method 5320, "Dissolved Organic Halogen," from "Standard Methods for the

Examination of Water and Wastewater," 5320, American Public Health Association, 1015 15th St. NW, Washington, DC 20005 (1989).

16.7 "Canadian Standard Method for the Determination of

Adsorbable Organic Halides (AOX) in Waters and Wastewaters," Environment Canada and The Canadian Pulp and Paper Association (1990).

16.8 40 CFR Part 136, Appendix B.

16.9 “Working with Carcinogens," DHEW, PHS, CDC, NIOSH, Publication 77–206, (Aug 1977).

16.10 “OSHA Safety and Health Standards, General Industry” OSHA 2206, 29 CFR 1910 (Jan 1976).

16.11 "Safety in Academic Chemistry Laboratories," ACS Committee on Chemical Safety (1979).

16.12 “Methods 330.4 and 330.5 for Total Residual Chlorine," USEPA, EMSL-Cincinnati, Cincinnati, OH 45268, EPA-479-020 (March 1979).

16.13 “Validation of Method 1650: Determination of Organic Halide,” Analytical Technologies Inc., ERCE Contract 87-3410, November 15, 1990. Available from the EPA Sample Control Center, DynCorp, 300 N. Lee St., Alexandria, VA 22314 (703-519-1140).

17.0 Figures