Method CTM-032

Draft Method for Sampling and Analysis for High Levels of Phenol and Cresol Emissions From Stationary Sources


This method is applicable to the collection and analysis of high levels (>20 ppmV in the gas phase and/or associated particulates) of phenol and the cresols. This method  was validated for the target compounds at a fiberglass manufacturing process and is believed to be applicable to other processes where phenols and cresols are emitted.  Samples are analyzed using high performance liquid chromatography (HPLC) with UV detection.

The sample is collected isokinetically  using a sampling train that consists of a heated probe, a heated filter, three impingers containing 200 mLs of 2N sodium hydroxide, an empty impinger, and an impinger containing silica gel.  The phenols and cresol react with NaOH to form the corresponding sodium salts.  A typical sample volume to be collected is 1 dry standard cubic meter (dscm) (35.31 dry standard cubic feet [dscf]).  Note that m-Cresol interferes with the determination of p-cresol and vice versa because the two compounds coelute under the HPLC analytical conditions used.

During sample recovery the contents of the probe rinse are put into a container.  The filter and front half filter holder rinses are put into a container.  The rinses of the back half of the filter holder and the contents of impinger one and rinses are put into another container.  The contents of impingers two, three and four and their corresponding rinses are combined into a final container.  An aliquot of the liquid in each of the containers is taken, acidified with sulfuric acid to a pH <2, and analysis by HPLC.  The filter is extract by following method 3542.  The method recommends that 10% of these extracts are analyzed by GC/MS following Method 8270 to assure that the retention of phenol and cresols is <1% of the analyte concentration observed in the first impinger.  If the concentration of analyte observed on the filter is <1% of the concentration of analyte in the first impinger, the remaining filter extracts may be archived. If the concentration of analyte observed on the filter is >1% of the concentration of analyte in the first impinger, the remaining filter extracts should be analyzed by GC/MS and the analyte recovered from the filter should be added to the concentration of analyte from the first impinger.

 

 

 

 

 

 


(EPA-Conditional Test Method)

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Method Data

Hold Times, Preservatives, Preps, Collection, Analytical & Documentation
Holding Time:   None specified in method.
Preservatives:   None
Required Preps:   Glass fiber or quartz filter
Collection Method:   Modified Method 5 sampling train by following CTM-032 procedures
Analytical Methodology:   HPLC/UV
Documentation:   CTM-032

Analyte List*

Analyte Formula CAS Number Detection Limit
p-Cresol
C7H8O
106-44-5
2390
 ppbv
m-Cresol
C7H8O
108-39-4
2390
 ppbv
Phenol
C6H6O
108-95-2
700
 ppbv
o-Cresol
C7H8O
95-48-7
50
 ppbv

* 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.