Method 12

Determination of Inorganic Lead Emissions From Stationary Sources


This method is applicable for the determination of inorganic lead emissions from stationary sources. Particulate and gaseous lead emissions are withdrawn isokinetically from the source and are collected on a filter and in dilute nitric acid.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 analyzed by atomic absorption spectrophotometry. 

Samples are collected isokinetically using Method 5 train which consists of a heated probe and glass fiber filter containing no organic binders and a series of impingers.  The 1st and 2nd impingers are filled with 100mL of 01.N HNO(nitric) .  The 3rd impinger is left empty and the 4th impinger is filled with 200-300g of silica gel.

After collection, the filter is folded with the collected particulate to the inside and place in a glass bottle.  A separate glass container (container 2 per the method) is used for the 0.1N HNO3 rinses of the probe, nozzle, and liner.  Take care to not include any dust on the outside of the probe in the container.  The silica gel is weighed to determine the percent moisture in the stack.  This step can be performed in the field.  The contents of the impingers are measured and then combined with the impinger rinses, and rinse of the connecting glassware and combined into one container (container 4 per the method).

 

Prior to analysis the filter is cut into strips and quantitatively transferred to a flask.  The probe rinse and impinger contents/rinses are combined, evaporated to dryness.  The solution is then combined with the filter, digested in nitric acid and analyzed.  Three readings from the spectrophotometer are required for each analysis.

 


(EPA 40CFR Part 60 Appendix A)

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Method Data

Hold Times, Preservatives, Preps, Collection, Analytical & Documentation
Holding Time:   None specified in method
Preservatives:   None specified in method.
Required Preps:   Glass fiber filter
Collection Method:   Modified Method 5 train following Method 12 procedures.
Analytical Methodology:   Atomic absorption spectrophotometry
Documentation:   12

Analyte List*

Analyte Formula CAS Number Detection Limit
Lead
Pb
7439-92-1
100
 ug

* The analytes and detection limits listed for each method represent the typical detection limits and analytes reported for that particular method. Keep in mind that analyte lists may vary from laboratory to laboratory. Detection limits may also vary from lab to lab and are dependent upon the sample size, matrix, and any interferences that may be present in the sample.