Method 29 Non-Hg Metals

Determination of Metal Emissions from Stationary Sources


This method is applicable for the determination of metals emissions from stationary sources. This method is considered by most as equivalent to the SW-846 0060 / 6010B series of methods. It may be combined with EPA Method 5 for particulate determination. This method also allows for the determination of particulates from the filter and probe rinses using Method 5 procedures if required.  The method allows for the front half and back half of the sampling train to be analyzed separately or combined following SW-846 Methods 6010B or 6020.

Samples are collected isokinetically using Method 29 train (similar to a Method 5 train) consisting of a quartz filter containing no organic binders and a series of impingers.   The 1st and 2nd impingers are filled with 100mL of a HNO3/ H2O2 solution.  The 3rd impinger is filled with 200-300g of silica gel.   The KMnO4 impingers noted in the method are needed only for the collection of mercury (Hg).

It is important that no metal be used in the probe, probe liner, filter support, or in the collection brushes used in sample recovery.  Metal parts could serve as a source of contamination of the sample. 

 

After collection, the contents of all impingers are measured to later assist with the determination of stack moisture.  The filter is folded such that the particulate is on the inside on the filter and placed in a petri dish.  In all the sample collection procedures, it is important to use 100mL of rinsing solution as specified in the method so that the blank correction procedures will be correct.  An acetone rinse of the probe, liner, and front half of the filter holder (if particulates are determined) is collected in a separate container.  This rinse is not collected if particulates are not needed.  The probe, line and front half of the filter holder is rinsed with HNO3 and collected in a separate container.  The contents of the HNO3/H202 impingers and associated HNO3 rinses of the impingers can be combined into one container or multiple containers if needed for volume. 

 

The filter, acetone rinse (if collected), and probe rinse are all digested separately with HNO3 and concentrated HF and then combined for analysis.  This sample represents the front half section of the sampling train.  The HNO3/H202 impingers and rinses are digested with HNO3 and concentrated HF and then analyzed.  Once prepared, the samples can be analyzed using a various techniques including GFAA (graphite furnace atomic absorption), ICP (inductively coupled plasma spectrometry) or ICP-MS.  ICP and ICP-MS are the most common techniques used as they achieve the lowest analyte detection limits and are less time consuming for the laboratory.

 

The analytes listed in the table below are those listed in the method, however, it is possible to collect use this method to collect and analyze for other metals.


(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, however, 6 months from collection to sample preparation is the generally accepted holding time for non-Hg metals.
Preservatives:   None specified in method.
Required Preps:   Quartz filters (a tared filter is needed for particulate determination)
Collection Method:   Method 29 sampling train
Analytical Methodology:   Analysis by ICP using SW-846 Method 6010B or by ICP-MS using SW-846 Method 6020
Documentation:   M 29
6010D
6020B

Analyte List*

Analyte Formula CAS Number Detection Limit
Lead
Pb
7439-92-1
15.1
 µg/m³
Manganese
Mn
7439-96-5
0.7
 µg/m³
Nickel
Ni
7440-02-0
5.4
 µg/m³
Silver
Ag
7440-22-4
2.6
 µg/m³
Thallium
Tl
7440-28-0
14.4
 µg/m³
Antimony
Sb
7440-36-0
11.5
 µg/m³
Arsenic
As
7440-38-2
19.1
 µg/m³
Barium
Ba
7440-39-3
0.8
 µg/m³
Beryllium
Be
7440-41-7
0.11
 µg/m³
Cadmium
Cd
7440-43-9
1.5
 µg/m³
Chromium
Cr
7440-47-3
2.5
 µg/m³
Cobalt
Co
7440-48-4
2.5
 µg/m³
Copper
Cu
7440-50-8
2.1
 µg/m³
Zinc
Zn
7440-66-6
0.8
 µg/m³
Phosphorus
P
7723-14-0
27
 µg/m³
Selenium
Se
7782-49-2
27
 µg/m³

* 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.