API 4694 : 1999

LABORATORY ANALYSIS OF PETROLEUM INDUSTRY WASTEWATERS - ARRANGING FOR ANALYSIS AND UNDERSTANDING LABORATORY REPORTS

American Petroleum Institute

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Introduction
- Types of Wastewater Covered
- Purpose of This Manual
- What's in This Manual
      - Overview of Manual
      - Quick Start
Part I - Essential Information
         Chapter 1 - Setting Objectives
         Chapter 2 - Planning Analyses
                     - Methods Specified by Regulatory
                     - Detection and Quantification Limits
                     - Matrix Interferences
                     - Quality Assurance/Quality Control
                     - Developing an Analytical Schedule
         Chapter 3 - Selecting a Laboratory
                     - Required Analyses
                     - In-House or Commercial Laboratory
                     - Capabilities
                     - Support Services
                     - Reputation and Size
                     - Costs
                     - Site Visit
                     - Evaluating Laboratory Performance with
                       Test Samples
                     - Getting Help from Consultants
         Chapter 4 - Reviewing Laboratory Reports
                     - Report Contents
                     - Reviewing Reports
Part II - Additional Detail and Special Topics
          Chapter 5 - Detection and Quantification Limits
                      - Definitions
                      - Application and Interpretation
          Chapter 6 - Quality Assurance/Quality Control
                      - Common Terms
                      - Requirements in Analytical Methods
                      - Laboratory Requirements
                      - Checking Performance with QA/QC
                        Criteria
          Chapter 7 - Method References
                      - NPDES Method References
                      - SW-846
          Chapter 8 - Method-Defined Analytes
                      - Biochemical Oxygen Demand
                      - Chemical Oxygen Demand
                      - Total Organic Carbon
                      - Oil and Grease
                      - Total Petroleum Hydrocarbons
                      - Phenols
                      - Total Solids
                      - Total Suspended Solids
                      - Total Dissolved Solids
                      - Surfactants
                      - Whole Effluent Toxicity
          Chapter 9 - Statistical Calculations
                      - Data Distributions
                      - Precision
                      - Bias
                      - Accuracy and Recovery
                      - Relationships Among Precision, Bias,
                        and Accuracy
                      - Outliers
                      - Nondetects and Censored Data
                      - EPA Method Detection Limit
Part III - References and Acronyms
           - References
           - Acronyms and Abbreviations
Part IV - Checklists
          - Checklists
Table 1-1 - Example of General DQO Statements for Analytical
            Data
Table 2-1 - Description of Analytical Specifications at 40
            CFR 136
Table 2-2 - Analytical Method References at 40 CFR 136
Table 2-3 - Examples of Water Quality Criteria that are Below
            Analytical Method Detection and Quantification
            Capabilities
Table 2-4 - Example Elements of Quality Control Program
Table 2-5 - Example Elements of Quality Assurance Program
Table 2-6 - Common Types of Sample Spikes
Table 2-7 - Sample Questions on QA/QC for Initial Discussion
            with Laboratory
Table 3-1 - Example Elements of a Good Laboratory Record-
            keeping System
Table 3-2 - Example Items that may be Included in an Onside
            Laboratory Evaluation
Table 3-3 - Examples of Sample Types Used to Evaluate
            Laboratory Performance
Table 4-1 - Items Typically Included in Analytical Laboratory
            Report
Table 4-2 - Sample Questions to Perform Initial Review of
            Laboratory Report
Table 4-3 - Required Containers, Preservation Techniques, and
            Holding Times from 40 CFR 136 for Selected
            Analytes
Table 4-4 - Examples of Alternate Names for Some Common
            Wastewater Analytes
Table 4-5 - Example of Notations Qualifying Analytical Results
Table 4-6 - Examples of Method-Defined Analytes for Wastewater
Table 5-1 - Definitions of Terms Commonly Used in Reference to
            Detection and Quantification Limits
Table 6-1 - Example of Analytes Used for Matrix Spikes for
            Organic Analyses
Table 6-2 - Example of Analytes Used for Surrogate Spikes for
            Organic Analyses
Table 6-3 - Example of Analytes Used for Internal Standard
            Spikes for Organic Analyses
Table 6-4 - Example QA/QC Requirements in Analytical Methods
Table 6-5 - Example Elements of QA/QC Program
Table 6-6 - Recommended Minimum QA/QC Information
Table 6-7 - Additional QA/QC Specifications to Consider
Table 6-8 - Analytical Method Performance Equations for
            Selected Analytes
Table 9-1 - Examples of Sources of Bias in Sample Measurement
Table 9-2 - Situations that May Indicate Sample Analysis Bias
Table 9-3 - Examples of Errors that Can Result in Outliers
Figure 2-1 - Different Types of Sample Spikes
Figure 4-1 - Example of Analytical Information in Laboratory
             Report
Figure 4-2 - Example Laboratory Report for QA/QC Data
             (Detailed Data)
Figure 4-3 - Example Laboratory Report for QA/QC Data
             (Less Detail)
Figure 9-1 - Bell-Shaped Normal Distribution
Figure 9-2 - Probability Plot (Normal Scale)
Figure 9-3 - Probability Plot (Long Scale)
Figure 9-4 - Comparing Precision of Dataom Two Different
             Laboratories
Figure 9-5 - Relative and Constant Bias in Sample Analyses
Figure 9-6 - Relationships Among Precision, Accuracy, and Bias

Abstract

To aid in understanding the following: technical and regulatory issues associated with obtaining analytical data on wastewater samples; data quality objectives, selecting analytical methods; specifying method detection limits, quantification limits, reporting levels, minimum levels and other related terms.