ANALYSIS OF ALCOHOL LEVEL IN EFFLUENT

1.0 PURPOSE

The purpose of this SOP is to ensure reliable and reproducible analytical results of tert-butanol and hexanol in effluent from the cosolvent flood by Clemson University NAPL group for laboratory-based or on-site (field-based) GC-FID analyses, and to permit traceability of possible causes of error in analytical results.

2.0 SCOPE

This SOP describes the analytical procedures used by Clemson University (CU) for analysis of tert-butanol and hexanol, in both laboratory and field studies. This SOP may not be specifically applicable to the activities of other organizations.

This SOP was written by John Coates, Patrick Haskell, and Cindy Lee at Clemson University.

The method involves gas chromatography (GC) techniques for estimation of concentrations of tert-butanol and hexanol; a flame-ionization detector (FID) is used to quantify the analyte con-centrations in the sample. The method has been found to provide reliable and reproducible quantitation of target compounds for concentrations >1%; this value is then considered to be the Method Detection Level (MDL). The standards calibration curve for FID response was found to be linear up to 15% for hexanol and 95% for tert-, and it may be linear even beyond these values, but was not tested.

Samples selected for GC-FID analysis may be chosen on the basis of preliminary screening to determine approximate concentration ranges, and select appropriate GC parameters (e.g., sample injection volumes; concentration range for standard curves, etc.) However, strategies for sample screening themselves are outside the scope of this SOP.

Water samples from laboratory and field experiments may be sub-samples into 2-ml GC vials for analysis.

3.0 RESPONSIBILITIES

All NAPL project staff, faculty, and students are responsible for knowing the procedures outlined below for analysis of tert-butanol and hexanol.

4.0 PROCEDURES

4.1 Sample Containers, Collection, Transportation and Storage

Sample Containers. Samples are contained in 4-ml glass sample vials (Fisher Catalog # 03-393G or equivalent) or 20 ml glass vials (Fisher # 03-339-14C) with open caps and Teflon-faced

septa. The glass vials or the caps are not reused.

Sample Collection. Each sample vial is completely filled with samples, such that no headspace of air exists, and capped. The vials are not opened until the time of subsampling or analysis.

Transportation and Storage. For field studies, the samples are stored in coolers containing "blue ice", and later stored in refrigerators in a trailer located on the site. Samples may be subjected to on-site GC analysis, and/or shipped back to CU laboratories; samples are packed in coolers and shipped via overnight air express (e.g., Fed. Ex.). The samples are stored in a refrigerator at 4C, until they are ready for GC analysis. After subsampling, the samples are returned to cold storage. For laboratory studies, the samples are stored in a refrigerator if the period prior to analysis is expected to exceed eight hours.