API DR 148 : 1997

API DR 148 : 1997

IDENTIFICATION OF ORGANIC TOXICANTS IN TREATED REFINERY EFFLUENTS

American Petroleum Institute

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Table of Contents

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

Abstract

Gives procedures for toxicity characterization in treated refinery effluents.

General Product Information

Document Type Standard
Status Current
Publisher American Petroleum Institute

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