API DR 148 : 1997
API DR 148 : 1997
IDENTIFICATION OF ORGANIC TOXICANTS IN TREATED REFINERY EFFLUENTS
American Petroleum Institute
IDENTIFICATION OF ORGANIC TOXICANTS IN TREATED REFINERY EFFLUENTS
American Petroleum Institute
Section
EXECUTIVE SUMMARY
1 INTRODUCTION
BACKGROUND
OBJECTIVES AND SCOPE
2 METHODS
GENERAL APPROACH
INITIAL TOXICITY SCREENS
Fathead Minnow Tests
Mysid Tests
PHASE I METHODS
PHASE II C18 SPE METHODS
C18 SPE Sorption and Elution
Concentration of Toxic Phase II Fractions
HPLC Separation Techniques
GC/MS Methods
3 RESULTS
PHASE I RESULTS FOR SELECTED REFINERY EFFLUENTS
PHASE II NONPOLAR ORGANIC TOXICITY IDENTIFICATION
pH Modifications of the Effluent Prior to C18
Sorption
Modification of the Standard Phase II Elution
Sequence
PHASE III TOXICITY CONFIRMATION
Toxicant Variability
4 SUMMARY
REFERENCES
Figure
3-1 GC/MS Scans of pHi, pH 3.0 and pH 9.0 100% Methanol
Toxic Phase II Fraction Concentrates, Refinery 1 -
Sample I
3-2 Comparison of U.S. EPA and Modified Scheme Used in
This Study for Identification of Nonpolar Toxicants
3-3 GC/MS Total Ion Chromatogram of Toxic 100% Methanol
Fraction Concentrate, Refinery 1 - Sample I
3-4 GC/MS Total Ion Chromatogram for the First Toxic 100%
Methanol Fraction Concentrate, Refinery 1 - Sample I
3-5 GC/MS Total Ion Chromatogram for the Second Toxic 100%
Methanol Fraction Concentrate, Refinery 1 - Sample I
3-6 GC/MS Chromatogram for 58 mg/L 2,4 ditert-butyl phenol
and Toxic Fraction Concentrate, Refinery 1 - Sample I
3-7 HPLC Chromatogram for 58 mg/L 2,4 ditert-butyl phenol
and Toxic Fraction Concentrate, Refinery 1 - Sample I
3-8 GC/MS Total Ion Chromatogram of the 90% Methanol Fraction
Concentrate of Jet Fuel Additive A and Identified Peaks
3-9 GC/MS Total Ion Chromatogram of the 95% Methanol Fraction
Concentrate of Jet Fuel Additive A and Identified Peaks
3-10 GC/MS Total Ion Chromatogram of the Combined 95% and
100% Methanol Fraction Concentrate of Jet Fuel Additive
B and Tentatively Identified Peaks
3-11 GC/MS Total Ion Chromatogram of Simplified Toxic C18
SPE Fraction Concentrate, Refinery 1 - Sample II
3-12 GC/MS Total Ion Chromatogram of Simplified Toxic C18
SPE Fraction Concentrate, Refinery 1 - Sample III
3-13 GC/MS Total Ion Chromatogram of Toxic Eluates Before
and After Phase II Separation, Refinery 1 - Sample I
3-14 GC/MS Total Ion Chromatogram of Toxic Eluates Before
and After Phase II Separation, Refinery 1 - Sample I
3-15 GC/MS Total Ion Chromatogram of the Concentrated
Toxic HPLC Fraction Concentrate, Refinery 1 - Sample I
3-16 Mass Spectrum of Peak at 25.301 Minutes, Refinery 1
Sample IV
3-17 Mass Spectrum of Peak at 26.350 Minutes, Refinery 1
Sample IV
3-18 Mass Spectrum of Peak at 31.066 minutes, Refinery 1
Sample IV
3-19 Mass Spectrum of Peak at 31.835 Minutes, Refinery 1
Sample IV
3-20 Mass Spectrum of Peak at 44.587 Minutes, Refinery 1
Sample IV
3-21 GC/MS Total Ion Chromatogram of HPLC Fraction 11,
Refinery 1 - Sample V
3-22 GC/MS Total Ion Chromatogram of HPLC Fraction 12,
Refinery 2 - Sample V
3-23 Mass Spectrum of Peak at 25.384 Minutes with Breakdown
of Chemical Components
3-24 Mass Spectrum of Peak at 31.042 minutes with Breakdown
of Chemical Components
3-25 Structures of Brominated Compounds in Refinery 1 -
Samples IV and V
Table
3-1 Chronic Phase I Toxicity Characterization Results
for Fathead Minnows Exposed to Refinery 1 Final
Effluent
3-2 Chronic Phase I Toxicity Characterization Results
for Fathead Minnows Exposed to Refinery 2 Final
Effluent
3-3 Chronic Phase I Toxicity Characterization Results
for Mysids Exposed to Refinery 3 Final Effluent
3-4 Chronic Phase I Toxicity Characterization Results
for Mysids Exposed to Refinery 4 Final Effluent
3-5 Percentage Survival of Fathead Minnows in C18
Concentrate Made from Effluent That Had Aged for
12 and 19 Days
3-6 Refinery 1, Fathead Minnow Survival from C18
SPE Tests Employing pH Adjustment Before Extraction
3-7 Refinery 3, Mysid Percent Survival in C18 Eluate
Employing pH Adjustment Before Elution
3-8 Mysid Percent Survival in Eight Fractions Eluated
from C18 SPE Columns Using Effluent from Refinery 3
3-9 Fathead Minnow Percent Survival in Eight Eluates
from C18 SPE Columns Using Effluent from Refinery 3
3-10 Fathead Minnow Percent Survival in Five Eluate
from a C18 SPE Column That Had Previously Been
Eluted with 25 and 50% Methanol Using Refinery 1
Gives procedures for toxicity characterization in treated refinery effluents.
Document Type | Standard |
Status | Current |
Publisher | American Petroleum Institute |