EPA Method 12
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EPA Method 12:
DETERMINATION OF INORGANIC LEAD EMISSIONS FROM STATIONARY SOURCES
Particulate and gaseous Pb emissions are withdrawn isokinetically from the source and are collected on a filter and in dilute nitric acid. The collected samples are digested in acid solution and are analyzed by atomic absorption spectrophotometry using an air/acetylene flame.
This method is applicable for the determination of inorganic lead emissions from stationary sources, only as specified in an applicable subpart of the regulations.
The official copy of this method is available at 40 Code of Federal Regulations (CFR) 60, Appendix A.
(A) Copper. High concentrations of copper may interfere with the analysis of Pb at 217.0 nm. This interference can be avoided by analyzing the samples at 283.3 nm.(B) Matrix Effects. Analysis for Pb by flame atomic absorption spectrophotometry is sensitive to the chemical composition and to the physical properties (e.g., viscosity, pH) of the sample. The analytical procedure requires the use of the Method of Standard Additions to check for these matrix effects, and requires sample analysis using the Method of Standard Additions if significant matrix effects are found to be present.
(A) Sampling equipment leak-checks and calibration -- This is done to ensure accuracy and precision of sampling measurements.(B) Spectrophotometer calibration -- This is done to ensure linearity of spectrophotometer response to standards.(C) Check for matrix effects -- This is done to help identify and eliminate matrix effects.
Maximum Holding Time:
> 100 ug-Pb
The within-laboratory precision, as measured by the coefficient of variation, ranges from 0.2 to 9.5 percent relative to a run-mean concentration. These values were based on tests conducted at a gray iron foundry, a lead storage battery manufacturing plant, a secondary lead smelter, and a lead recovery furnace of an alkyl lead manufacturing plant. The concentrations encountered during these tests ranged from 0.61 to 123.3 mg Pb/m3. For a minimum analytical accuracy of +/- 10 percent, the lower limit of the range is 100 ug. The upper limit can be extended considerably by dilution.
Typical sensitivities for a 1-percent change in absorption (0.0044 absorbance units) are 0.2 and 0.5 ug Pb/ml for the 217.0 and 283.3 nm lines, respectively.
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