Method CARB 429

Determination of Polycyclic Aromatic Hydrocarbon (PAH) Emissions from Stationary Sources


This method applies to the determination of nineteen polycyclic aromatic hydrocarbons (PAHs) in emissions from stationary sources.  The method calls for use of isotope dilution LRMS (low resolution mass spectrometry) or HRMS (high resolution) for PAH determination.   Since the method was written, the HRMS analysis is typically the option of preference in order to achieve the lowest detection limits possible. 

Particulate and gaseous phase PAHs are extracted isokinetically from the stack and collected using a modified Method 5 sampling train consisting of a heated probe and filter holder, Teflon coated glass fiber filter, XAD-2 resin trap and a series of impingers. 

Particulate and gaseous phase PCDD,s PCDFs and PCBs are extracted isokinetically from the stack and collected using a modified Method 5 sampling train consisting of a heated probe and filter holder, glass fiber or quartz filter,  XAD-2 resin trap, and a series of impingers.  The first and second impingers are filled with 100mL of a 3mM sodium bicarbonate/2.4 sodium carbonate solution to neutralize any acids in the gas stream.  The third impinger is left empty and the fourth impinger is filled 200-300g of silica gel. 

After collection, the filter is placed in glass petri dish or bottle.  The method states to not wrap the filter in aluminum foil.  The probe, nozzle and front half of the filter holder (front half of sampling train) is rinsed with acetone, hexane and  methylene chloride (3x each) and placed in an amber glass jar.  The back half of the sampling train (back half of filter holder, transfer lines, connecting glassware) is rinsed with the same solvents and can be combined with the front half rinse.  The contents of each impinger are weighed and can be combined in a single amber glass container.  The impingers are rinsed with acetone, hexane and methylene chloride (3x each).  The rinse can be combined with the impinger contents.  The silica gel can be weighed in the field.

Upon return to the laboratory, the sample components are spiked and extracted with methylene chloride.  The method states that the impinger contents can be processed separately from the other components of the train if a breakthrough check is needed.  Typically, all components of the train are combined for analysis.


(CARB Stationary Source Test Methods, Volume 3)

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Method Data

Hold Times, Preservatives, Preps, Collection, Analytical & Documentation
Holding Time:   The XAD-2 resin must be used for sampling within 21 days of cleaning per the method. Samples must be extracted as soon as practically feasible but within 21 days of collection. Sample extracts must be analyzed as soon as practically feasible but within
Preservatives:   Keep all sample fractions and filters at 4°C and protected from light.
Required Preps:   Teflon coated glass fiber filter without organic binders and XAD resin trap
Collection Method:   Modified Method 5 sampling train following CARB 429 procedures.
Analytical Methodology:   HRGC/HRMS
Documentation:   CARB 429

Analyte List*

Analyte Formula CAS Number Detection Limit
Anthracene
C14H10
120-12-7
5
 ng
Pyrene
C16H10
129-00-0
5
 ng
Benzo(g,h,i)perylene
C22H12
191-24-2
5
 ng
Benzo[e]pyrene
C20H12
192-97-2
5
 ng
Indeno(1,2,3-cd)pyrene
C22H12
193-39-5
5
 ng
Perylene
C20H12
198-55-0
5
 ng
Benzo[b]fluoranthene
C20H12
205-99-2
5
 ng
Fluoranthene
C16H10
206-44-0
5
 ng
Benzo[k]fluoranthene
C20H12
207-08-9
5
 ng
Acenaphthylene
C12H8
208-96-8
5
 ng
Chrysene
C18H12
218-01-9
5
 ng
Benzo[a]pyrene
C20H12
50-32-8
5
 ng
Dibenz[a,h]anthracene
C22H14
53-70-3
5
 ng
Benzo(a)anthracene
C18H12
56-55-3
5
 ng
Acenaphthene
C12H10
83-32-9
5
 ng
Phenanthrene
C14H10
85-01-8
22
 ng
Fluorene
C13H10
86-73-7
16.5
 ng
Naphthalene
C10H8
91-20-3
480
 ng
2-Methylnaphthalene
C11H10
91-57-6
66
 ng

* 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.