EPA OAR/OAQPS/EMAEMC: OAQPS-12: Lead in Air Emissions by Flame Atomic Absorption

Summary
Analytes
Revision
Data and Sites

Official Method Name

Method 12 - Determination of Inorganic Lead Emissions from Stationary Sources

Current Revision

2000

Media

AIR

Instrumentation

Flame Atomic Absorption

Method Subcategory

Inorganic

Method Source

EPA OAR/OAQPS/EMAEMC

Citation

The official copy of this method is available at 40 Code of Federal Regulations (CFR) 60, Appendix A. The CFR can be accessed on-line at http://www.gpoaccess.gov/cfr/index.html

Brief Method Summary

Particulate and gaseous Pb emissions are withdrawn isokinetically from the source and are collected on a filter and in dilute nitric acid.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.

Scope and Application

This method is applicable for the determination of inorganic lead (Pb) in air emissions from stationary sources.

Applicable Concentration Range

> 100 ug-Pb

Interferences

(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.

Quality Control Requirements

(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.

Sample Handling

Detailed sample collection and handling procedures, including a diagram for the lead sampling train, are provided in the method.

Maximum Holding Time

Not Available

Relative Cost

Unknown

Sample Preparation Methods

This method has 1 analyte associated with it.

Analyte	Detection Level	Bias	Precision	Pct False Positive	Pct False Negative	Spiking Level
Lead(7439-92-1) Lead Lead and compounds (inorganic) Lead and lead compounds Pb	0.200 ug/mL	N/A	N/A

Precision Descriptor Notes:	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.
Detection Level Note:	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.

Precision Descriptor Notes:

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.

Detection Level Note:

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.

Revision	PDF/Link
2000

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EPA OAR/OAQPS/EMAEMC: OAQPS-12: Lead in Air Emissions by Flame Atomic Absorption

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