title: Determination of mercury in carbon black by cold vapor atomic absorption spectrometry.
abstract: Recently, a new color additive, D&C Black No. 2, a high-purity furnace black in the general category of carbon blacks, was listed as a color subject to batch certification by the U.S. Food and Drug Administration. A simple procedure was developed to determine mercury (Hg) in D&C Black No. 2, which is limited by specification to not more than 1 ppm Hg. The method uses partial acid digestion followed by cold vapor atomic absorption and was developed by modifying a method used for other color additives. The carbon black samples are treated with a mixture of nitric and hydrochloric acids and heated by microwave in sealed Teflon vessels. The resulting solutions, which are stable to Hg loss for at least 1 week, are diluted and analyzed for Hg using cold vapor atomic absorption spectrometry. Validation was performed by spiking carbon black samples with inorganic Hg (HgNO3) at levels from 0.1 to 1.5 microg/g, and by analyzing 2 standard reference materials. At the specification level of 1 ppm Hg (1 microg Hg/g), the 95% confidence interval was +/-0.01 ppm Hg (0.01 microg Hg/g). The method developed in this study gave good results for very difficult-to-analyze materials, such as coal standard reference materials and carbon black. By eliminating volatility and adsorption factors through the formation of HgCl4(-2) complexes, one can avoid using extremely hazardous acids such as HF and HClO4.
authors.affiliation: U.S. Food and Drug Administration, Office of Cosmetics and Colors, 5100 Paint Branch Pkwy, College Park, MD 20740, USA. nhepp@cfsan.fda.gov
authors.forename: Nancy M
authors.initials: NM
authors.lastname: Hepp
mesh_terms: D002138:Calibration; D002244:Carbon / Q000737:chemistry*; D002623:Chemistry Techniques, Analytical / Q000379:methods*; D005740:Gases; D008628:Mercury / Q000032:analysis*; D008872:Microwaves; D017942:Nitric Acid / Q000737:chemistry; D011138:Polytetrafluoroethylene; D015203:Reproducibility of Results; D013054:Spectrophotometry, Atomic / Q000379:methods*
chemical_list: D005740:Gases; D017942:Nitric Acid; D002244:Carbon; D011138:Polytetrafluoroethylene; D008628:Mercury