Final Report. Analysis of Heavy Metals in Cleaning Products. for The Soap and Detergent Association 475 Park Avenue South New York, NY 10016
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1 Final Report Analysis of Heavy Metals in Cleaning Products for The Soap and Detergent Association 475 Park Avenue South New York, NY by Corning Hazleton 3301 Kinsman Boulevard Madison. WI Author Robert G. Allen June 8, 1995
2 2 CONTENTS Page INTRODUCTION SAMPLE COLLECTION COMPOSITING PROCEDURE MATERIALS SAMPLE ANALYSIS SIGNATURE TABLES 1. Product Brands to be Collected and Composited 6 2. Sample Collection 7 3. Compositing Procedure 8 4. Instrument Parameters Atomic Absorption 9 5. Analytical Results Method References 11
3 3 INTRODUCTION Composite samples of powder laundry detergent were analyzed for arsenic, cadmium, chromium, copper, lead, mercury, nickel, silver, and zinc to develop background information on the potential contribution of these products to the heavy metal contamination of municipal sewage. The Soap and Detergent Association (SDA) previously sponsored a study in which the concentrations of these same heavy metals were measured in composite samples of seven categories of cleaning products which are known to be disposed into sewage. Since the completion of this study, powder laundry detergents have undergone widespread reformulation. This matrix was reexamined to determine if the heavy metal content was altered. SAMPLE COLLECTION Eleven different brands of powder laundry detergent were collected from stores in three California cities: Sunnyvale, Palo Alto, and San Jose. A ounce container was to be purchased in each municipality. Table I was reprinted from The Soap and Detergent Association scope of work and lists the product brands to be collected and composited. Table 2 lists the container size collected in each area. COMPOSITING PROCEDURE Eleven within-brand composites were prepared by combining each of the single containers from each of the three cities. From these composites, a subsample was removed based on the market share to prepare the between-brand composite (Table 3). A total of 600 grams was prepared and subdivided into three acid-washed polyethylene bottles (amber, wide-mouthed, 250 ml size). Two of these samples were used for analysis and the third was kept as a reserve sample. Reagents MATERIALS Water, double-deionized, in-house Nitric acid, Mallinckrodt Chemical, Inc., Paris, Kentucky Sulfuric acid, Fisher Scientific, Pittsburgh, Pennsylvania Sodium borohydride, Aldrich Chemical Company, Milwaukee, Wisconsin Stock standard solutions, Fisher Scientific, Pittsburgh, Pennsylvania Equipment General laboratory glassware, Coring Glassworks, Corning, ~ew York Instrumentation Spectrophotometer, Models 3300 and 5000, Perkin Elmer Mercury/hydride system, Perkin Elmer Model MHS-20
4 4 SAMPLE ANALYSIS Cadmium. Chromium. Copper. Lead. Nickel. Silver. and Zinc The samples were digested with nitric acid in glass beakers on a hot plate, transferred to 50 ml volumetric flasks, filtered, and analyzed by atomic absorption spectroscopy. Arsenic The samples were digested with a mixture of sulfuric and nitric acids, transferred to 25 ml volumetric flasks, and analyzed by hydride generation. Mercury The samples were digested with a mixture of sulfuric and nitric acids, transferred to 100 ml volumetric flasks, and analyzed by cold vapor atomic absorption spectroscopy. All of the analyses were performed using atomic absorption spectroscopy. The instrument operating parameters are included in Table 4. Analytical results are listed in Table 5. Spikes were prepared to test for matrix effects. The amount of each analyte added and the respective percent recovery are listed in Table 5. Recoveries ranged from %.
5 5 SIGNATURE ~~ ~ l. Robert G. Allen Supervisor Inorganic Chemistry QU..I.olOo-~- Date by and for Corning Hazleton
6 6 Table I Product Brands To Be Collected and Composited 4 Powder Laundry Detergents Market Cumulative Density2 Weighting Brand Manufacturer Share! Share (gm/l) Factor3 Tide Procter & Gamble Tide with bleach Procter & Gamble Surf Lever Brothers Cheer Procter & Gamble Arm & Hammer Church & Dwight Wisk Lever Brothers Purex Dial All Lever Brothers Bold Procter & Gamble Gain Procter & Gamble Fab Colgate-Palmolive !Information Resources, Inc., personal communication, Personal communications with manufacturers. 3Weighting factor = [Powder detergent market share x Density] / E[Powder detergent market share x Density] x 100 4Reprinted from The Soap and Detergent Association scope of work.
7 7 Table 2 Sample Collection Brand City Sunnyvale Palo Alto San Jose Tide 420z 420z 420z Tide with Bleach 470z 470z 470z Surf 420z 420z 420z Cheer 420z 420z 420z Arm & Hammer 4.51b 4.51b 4.51b Wisk 420z 420z 420z Purex 66 oz 66 oz 660z All 480z 480z 480z Bold 420z 420z 420z Gain 420z 420z 420z Fab 6 lb 2 oz 1 420z 1 This brand could not be located in Palo Alto.
8 8 Table 3 Compositing Procedure Power Laundry Detergent Tide Tide with Bleach Surf Cheer Arm & Hammer Wisk Purex All Bold Gain Fab Weight (grams)
9 9 Table 4 Instrument Parameters Atomic Ahsorption Element Techniaue Instrument Analytical Wavelength ~nm) Silt (nm) Gases Standard Solutions Range!mmll Arsenic Cadmium Chromium Copper Lead Mercury Nickel Silver Zinc Hydride Flame Flame flame Flame Hydride Flame Flame Flame PE 5000/MHS-20 PE 3300 PE 5000 PE 3300 PE 5000 PE 5000/MHS-20 PE 3300 PE 5000 PE Argon (carrier) Air/acetylene N]O/acetylene Air/acetylene Air/acetylene Argon (carrier) Air/acetylene Air/acetylene Air/acetylene PE Perkin Elmer Corp., Norwalk, CT MHS-20 QP Perkin Elmer Mercury/Hydride System
10 10 Table 5 Analytical Results Analyte Concentration (mg/kg) Powder Laundry Detergent Assay I As Cd <0.20 Cr < 1.00 Cu 1.52 Pb 0.18 Hg <0.025 Ni < 1.00 Ag 1.01 Zn 4.02 Assay <0.20 < <0.025 < Analyte Added (llg) Recovery (%) lot
11 11 Table 6 Method References Arsenic by Hydride Generation Digestion: Analytical Methods Committee, The Analyst, Volume 85, Pages (1960) (Modified). Perkin Elmer, Analytical Methods Using the MHS Mercury/Hydride System, Norwalk, CT., January, 1981 (Modified). Cadmium Official Methods of Analysis of the Association of Official Analytical Chemists, 15th Edition, Method , Arlington, VA., (1990) (Modified). Perkin Elmer, Analytical Methods for Atomic Absorption Spectrophotometry, Norwalk, Ct., January 1982 (Modified) Methods for Chemical Analysis of Water and Wastes (1979), Metals 1-19 and Method 213.1, U.S. EPA, Cincinnati, OH (Modified). Chromium Perkin Elmer, Analytical Methods for Atomic Absorption Spectrophotometry, Norwalk, CT, January 1982 (Modified). Methods for Chemical Analysis of Water and Wastes (1979), Metals 1-19 and Method 218.1, U.S. EPA, Cincinnati, OH (Modified). Lead Official Methods of Analysis of the AOAC, 15th Edition, Methods , and , AOAC, Arlington, VA. (1990) (Modified). Friend, M.T., Smith, C. A., and Wishart, D., Atomic Absorption Newsletter, Volume 16, No.2, Pages (1979) (Modified) Mercury Digestion: Analyst, Volume 86, Page 608 (1961) (Modified). Determination: Analytical Chemistry, Volume 40, Page 2085 (1968) (Modified). Nickel Perkin Elmer, Analytical Methods for Atomic Absorption Spectrophotometry, Norwalk, CT, January 1982 (Modified). Methods for Chemical Analysis of Water and Wastes (1979), Metals 1-19 and Method 249.1, U.S. EPA, Cincinnati, OH (Modified).
12 12 Table 6 (Continued) Silver Perkin Elmer, Analytical Methods for Atomic Absorption Spectrophotometry, Norwalk, CT, January 1982 (Modified). Methods for Chemical Analysis of Water and Wastes (1979), Metals 1-19 and Method 272.1, U.S. EPA, Cincinnati, OH (Modified). Zinc Official Methods of Analysis of the Association of Official Analytical Chemists, 15th Edition, Methods , , and , Arlington, Virginia (1990) (Modified).
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