
Basic Laboratory Procedures for the Operator-Analyst, 6th Edition
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Content
- Intro
- Title Page
- Copyright
- Contents
- List of Figures
- List of Tables
- Preface
- Chapter 1 Introduction to the Laboratory
- 1.0 Background
- 2.0 Wastewater Constituents
- 2.1 Components
- 2.2 Relationships between Different Wastewater Components
- 2.2.1 Per Capita Generation Rates
- 2.2.2 Ratios Between Wastewater Constituents in Domestic Wastewater
- 2.3 Mass Balance
- 3.0 Sampling
- 3.1 Representative Sampling
- 3.2 Purposes of Sampling
- 3.2.1 Regulatory Requirements
- 3.2.2 Process Control
- 3.2.3 Determine Process and Facility Efficiency
- 3.2.4 Support or Refute Future Capital Expenditures
- 3.2.5 Historical Records
- 3.3 Sample and Measurement Collection
- 3.3.1 Continuous Measurements
- 3.3.2 Grab Samples
- 3.3.3 Composite Samples
- 3.3.3.1 Fixed-Volume Composite Samples
- 3.3.3.2 Flow-Proportional Composite Samples
- 3.3.3.2.1 Variable-Volume Technique
- 3.3.3.2.2 Variable-Frequency Technique
- 3.4 Use of Automatic Samplers
- 3.4.1 Programming
- 3.4.2 Cleanliness
- 3.4.3 Materials of Construction
- 3.5 Sample Hold Time
- 3.6 Sample Containers
- 3.7 Preservatives
- 3.8 Samples Requiring Special Consideration
- 3.9 Recommended Sampling Locations for Process Control
- 4.0 References
- Chapter 2 Laboratory Basics
- 1.0 Laboratory Safety
- 1.1 Personal Protective Equipment
- 1.2 Chemical Storage
- 1.3 Chemical Handling
- 1.4 Chemical Spills
- 1.5 Fire
- 1.6 Ingestion Hazards
- 2.0 Laboratory Analysis
- 2.1 Volumetric Analyses (Titrations)
- 2.2 Gravimetric Analysis
- 2.3 Colorimetric Analysis
- 2.4 Electrometric Analysis
- 3.0 Laboratory Equipment
- 3.1 Glassware
- 3.1.1 Volumetric Glassware
- 3.1.2 Using Volumetric Glassware
- 3.1.3 Other Glassware
- 3.2 Miscellaneous Laboratory Equipment
- 4.0 Housekeeping
- 4.1 Laboratory Environment
- 4.1.1 Climate
- 4.1.2 General Cleanliness
- 4.2 Washing Dishes
- 4.2.1 Acid Washes
- 4.2.2 Oxidizers
- 5.0 Basic Chemistry
- 5.1 Using the Periodic Table of the Elements
- 5.2 Atoms
- 5.3 Elements
- 5.4 Atomic Numbers
- 5.5 Molecules and Compounds
- 5.6 Moles
- 5.7 Atomic Weight
- 5.8 Formula Weight
- 5.9 Ions
- 5.10 Molar Solutions
- 5.11 Normal Solutions
- 5.12 Milligrams per Liter Solutions
- 5.13 Determining Percent Weight of Atoms in Molecules
- 6.0 Weighing
- 6.1 Analytical Balances and Weighing Conditions
- 6.2 Weighing Containers and Accessories
- 6.3 Drying Dishes and Reagents
- 6.4 Weighing Procedures for Reagents
- 7.0 Reagents
- 7.1 Laboratory-Grade Water
- 7.2 Reagent Grades
- 7.3 Mixing Reagents
- 8.0 Making Acids and Bases
- 9.0 Stock, Standards, and Standard Dilutions
- 9.1 Stock Solutions
- 9.2 Standard Solutions
- 9.3 Standard Dilutions
- 10.0 Accuracy, Precision, and Error
- 10.1 Accuracy and Precision
- 10.2 Error and Uncertainty
- 10.2.1 Determinate Errors
- 10.2.2 Indeterminate Errors
- 10.3 Significant Figures
- 11.0 Quality Assurance and Quality Control
- 11.1 Quality Assurance System
- 11.2 Measures of Precision
- 11.2.1 Mean
- 11.2.2 Relative Percent Difference
- 11.2.3 Standard Deviation
- 11.2.4 Relative Standard Deviation
- 11.3 Measures of Accuracy
- 12.0 Elements of Quality Control
- 12.1 Method Blank
- 12.2 Laboratory-Fortified Blank
- 12.3 Laboratory-Fortified Matrix and Laboratory-Fortified Matrix Duplicate
- 12.4 Duplicates
- 12.5 Calibration
- 12.6 Continuing Calibration Verification
- 12.7 Initial Demonstration of Capability
- 12.8 Quality Control Sample
- 12.9 Control Charts
- 12.10 Limits and Levels
- 12.10.1 Instrument Detection Limit
- 12.10.2 Method Detection Level
- 12.10.3 Quantitation Limits
- 12.10.4 Reporting Limits
- 13.0 References
- Chapter 3 Physical and Chemical Examination
- 1.0 pH
- 1.1 General Description
- 1.2 Application
- 1.3 Interferences
- 1.4 Apparatus and Materials
- 1.5 Stock and Standards
- 1.6 Quality Assurance and Quality Control
- 1.7 Sample Collection, Preservation, and Holding Times
- 1.8 Procedure
- 1.9 Reporting
- 1.10 Troubleshooting and Tips
- 1.11 Benchsheet
- 2.0 Total Alkalinity of Wastewater and Sludge
- 2.1 General Description
- 2.2 Application
- 2.3 Interferences
- 2.4 Apparatus and Materials
- 2.5 Reagents
- 2.6 Quality Assurance and Quality Control
- 2.7 Sample Collection, Preservation, and Holding Times
- 2.8 Procedure
- 2.9 Calculations
- 2.10 Reporting
- 2.11 Troubleshooting and Tips
- 2.12 Benchsheet
- 3.0 Volatile Organic Acids in Wastewater Sludge
- 3.1 General Description
- 3.2 Application
- 3.3 Interferences
- 3.4 Apparatus and Materials
- 3.5 Reagents
- 3.6 Sample Collection, Preservation, and Handling
- 3.7 Quality Assurance and Quality Control
- 3.8 Procedure
- 3.9 Calculations
- 3.10 Reporting
- 3.11 Benchsheet
- 4.0 Solids Procedures
- 5.0 Settleable Solids
- 5.1 General Description
- 5.2 Application
- 5.3 Apparatus and Materials
- 5.4 Sample Collection, Preservation, and Holding Times
- 5.5 Quality Assurance and Quality Control
- 5.6 Procedure
- 5.7 Calculations
- 5.8 Reporting
- 5.9 Troubleshooting and Tips
- 5.10 Benchsheet
- 6.0 Total Fixed and Volatile Solids in Solid and Semisolid Samples
- 6.1 General Description
- 6.2 Application
- 6.3 Interferences
- 6.4 Apparatus and Materials
- 6.5 Stock and Standards
- 6.6 Quality Assurance and Quality Control
- 6.7 Sample Collection, Preservation, and Holding Times
- 6.8 Procedure
- 6.9 Calculations
- 6.10 Reporting
- 6.11 Troubleshooting and Tips
- 7.0 Total Solids Dried at 103 to 105 °C
- 7.1 General Description
- 7.2 Application
- 7.3 Interferences
- 7.4 Apparatus and Materials
- 7.5 Reagents
- 7.6 Stock and Standards
- 7.7 Quality Assurance and Quality Control
- 7.8 Sample Collection, Preservation, and Holding Times
- 7.9 Procedure
- 7.10 Calculations
- 7.11 Reporting
- 7.12 Troubleshooting and Tips
- 7.13 Benchsheet
- 8.0 Total Suspended Solids (Total Nonfilterable Residue)
- 8.1 General Description
- 8.2 Application
- 8.3 Interferences
- 8.4 Apparatus and Materials
- 8.5 Reagents
- 8.6 Stock and Standards
- 8.7 Quality Assurance and Quality Control
- 8.8 Sample Collection, Preservation, and Holding Times
- 8.9 Procedure
- 8.10 Calculations
- 8.11 Reporting
- 8.12 Troubleshooting and Tips
- 8.13 Benchsheet
- 9.0 Total Dissolved Solids Dried at 180 °C
- 9.1 General Description
- 9.2 Application
- 9.3 Interferences
- 9.4 Apparatus and Materials
- 9.5 Reagents
- 9.6 Stock and Standards
- 9.7 Sample Collection, Preservation, and Holding Times
- 9.8 Quality Assurance and Quality Control
- 9.9 Procedure
- 9.10 Calculations
- 9.11 Reporting
- 9.12 Troubleshooting and Tips
- 9.13 Benchsheet
- 10.0 Volatile and Fixed Solids Ignited at 550 °C
- 11.0 Settleability
- 11.1 General Description
- 11.2 Apparatus and Materials
- 11.3 Sample Collection, Preservation, and Holding Times
- 11.4 Procedure
- 11.5 Special Variations or Applications
- 11.5.1 Rise Test
- 11.5.2 Dilution Test
- 11.6 Calculations
- 11.7 Benchsheets
- 12.0 Sludge Volume Index
- 12.1 General Description
- 12.2 Application
- 12.3 Interferences
- 12.4 Required Data
- 12.5 Calculations
- 12.6 Reporting
- 13.0 Centrifuge Method for Estimating Suspended Matter
- 13.1 General Description
- 13.2 Application
- 13.3 Interferences
- 13.4 Apparatus and Materials
- 13.5 Sample Collection, Preservation, and Holding Times
- 13.6 Quality Assurance and Quality Control
- 13.7 Procedure
- 13.8 Calculations
- 13.9 Reporting
- 14.0 Oxygen Uptake Rate and Specific Oxygen Uptake Rate
- 14.1 General Description
- 14.2 Application
- 14.3 Apparatus and Materials
- 14.4 Procedure
- 14.5 Calculations
- 14.6 Benchsheet
- 15.0 Dissolved Oxygen, Winkler Method Azide Modification
- 15.1 General Description
- 15.2 Application
- 15.3 Interferences
- 15.4 Apparatus and Materials
- 15.5 Reagents
- 15.6 Sample Collection, Preservation, and Holding Times
- 15.7 Procedure
- 15.8 Calculations
- 15.9 Reporting
- 16.0 Biochemical Oxygen Demand (5-Day Biochemical Oxygen Demand)
- 16.1 General Description
- 16.2 Application
- 16.3 Interferences
- 16.4 Apparatus and Materials
- 16.5 Reagents
- 16.6 Stock and Standards
- 16.7 Quality Assurance and Quality Control
- 16.7.1 Prepare a Standard
- 16.7.2 Replicates
- 16.7.3 Duplicates
- 16.8 Sample Collection, Preservation, and Holding Times
- 16.9 Procedure
- 16.10 Calculations
- 16.11 Reporting
- 16.12 Benchsheet
- 17.0 Chlorine Residual-Amperometric Titration
- 17.1 General Description
- 17.2 Application
- 17.3 Interferences
- 17.4 Apparatus and Materials
- 17.5 Reagents
- 17.6 Stock and Standards
- 17.7 Sample Collection, Preservation, and Holding Times
- 17.8 Procedure
- 17.9 Calculations
- 17.10 Reporting
- 17.11 Troubleshooting and Tips
- 18.0 Ammonia-Nitrogen-Ion-Selective Electrode Method
- 18.1 General Description
- 18.2 Application
- 18.3 Interferences
- 18.4 Apparatus and Materials
- 18.5 Reagents
- 18.6 Stock and Standards
- 18.7 Sample Collection, Preservation, and Holding Times
- 18.8 Quality Assurance and Quality Control
- 18.9 Procedure
- 18.10 Calculations
- 18.11 Reporting
- 18.12 Troubleshooting and Tips
- 18.13 Benchsheet
- 19.0 Nitrate-Nitrogen-Ion-Selective Electrode Method
- 19.1 General Description
- 19.2 Application
- 19.3 Interferences
- 19.4 Apparatus and Materials
- 19.5 Reagents
- 19.6 Stock and Standards
- 19.7 Sample Collection, Preservation, and Holding Times
- 19.8 Quality Assurance and Quality Control
- 19.9 Procedure
- 19.10 Calculations
- 19.11 Reporting
- 19.12 Troubleshooting and Tips
- 19.13 Benchsheet
- 20.0 Phosphorus
- 20.1 General Description
- 20.2 Application
- 20.3 Interferences
- 20.4 Apparatus and Materials
- 20.5 Reagents
- 20.6 Stock and Standards
- 20.7 Sample Collection, Preservation, and Holding Times
- 20.8 Quality Assurance and Quality Control
- 20.9 Procedure
- 20.10 Calculations
- 20.11 Reporting
- 20.12 Troubleshooting and Tips
- 20.13 Benchsheet
- 21.0 Temperature
- 21.1 General Description
- 21.2 Application
- 21.2.1 Ponds
- 21.2.2 Facility Influent
- 21.2.3 Clarification (Primary and Secondary)
- 21.2.4 Secondary Treatment
- 21.2.5 Filtration
- 21.2.6 Anaerobic Digestion
- 21.2.7 Biosolids Dewatering
- 21.2.7.1 Polymer Makeup
- 21.2.7.2 Centrifuge
- 21.3 Apparatus and Materials
- 21.4 Sample Collection, Preservation, and Holding Times
- 21.5 Procedure
- 21.6 Calculations
- 21.7 Reporting
- 21.8 Benchsheet
- 22.0 Turbidity
- 22.1 General Description
- 22.2 Application
- 22.3 Interferences
- 22.4 Apparatus and Materials
- 22.5 Reagents
- 22.6 Sample Collection, Preservation, and Holding Times
- 22.7 Quality Assurance and Quality Control
- 22.8 Procedure
- 22.9 Calculations
- 22.10 Reporting
- 22.11 Troubleshooting and Tips
- 22.11.1 Troubleshooting
- 22.11.2 Tips
- 22.12 Benchsheet
- 23.0 Ozone: Indigo Colorimetric Method
- 23.1 General Description
- 23.2 Application
- 23.3 Interferences
- 23.4 Apparatus and Materials
- 23.5 Reagents
- 23.6 Stock and Standards
- 23.7 Quality Assurance and Quality Control
- 23.8 Sample Collection, Preservation, and Holding Times
- 23.9 Procedure
- 23.10 Calculations
- 24.0 Activated Sludge System Microscopic Examination
- 24.1 General Description
- 24.2 Application
- 24.2.1 Indicator Organisms
- 24.2.1.1 Amoeboids
- 24.2.1.2 Flagellates
- 24.2.1.3 Ciliates
- 24.2.1.4 Free-Swimming Ciliates
- 24.2.1.5 Stalked Ciliates
- 24.2.1.6 Rotifers
- 24.2.1.7 Nematodes and Worms
- 24.2.1.8 Filaments
- 24.2.2 Relative Dominance
- 24.3 Interferences
- 24.4 Apparatus and Materials
- 24.5 Sample Collection, Preservation, and Holding Times
- 24.6 Quality Assurance and Quality Control
- 24.7 Procedure
- 24.8 Calculations
- 24.9 Reporting
- 25.0 References
- 26.0 Suggested Readings
- Chapter 4 Spectrophotometry
- 1.0 Introduction
- 2.0 Background and Advantages
- 3.0 Fundamentals of the Technology
- 3.1 Terminology
- 3.2 The Advantage in Water Testing
- 3.2 Calibration and Computer-Based Data
- 4.0 Quality Assurance and Quality Control
- 4.1 Interferences
- 4.2 Detection Limits and Quantitation Limits
- 4.2.1 Method Detection Limit or Minimum Detection Limit
- 4.2.2 Instrument Detection Limit
- 4.2.3 Practical Quantitation Limit (Quantitation Limits)
- 5.0 Other Considerations for Tests
- 5.1 Equipment Operation
- 5.2 Tips and Useful Practices
- 5.2.1 Cuvettes
- 5.2.2 Internal (Instrument) Windows
- 5.2.3 Blanks and Background
- 5.2.4 Operational Hints
- 5.2.4.1 New Spectrophotometers
- 5.2.4.2 Zero and Span Adjustment
- 5.2.5 Typical Instrument Operations
- 5.2.6 Example Steps in a Typical Procedure
- 5.2.7 Instrument Designs
- 5.2.7.1 Older Designs
- 5.2.7.2 Newer Designs
- 6.0 Selected Examples of Commonly Used Methods
- 6.1 Chemical Oxygen Demand
- 6.2 Nitrate-Nitrogen
- 6.3 Nitrite-Nitrogen
- 6.4 Ammonia-Nitrogen
- 6.5 "UV 254" Method for Organic Carbon (Dissolved)
- 6.6 Phosphate Phosphorus
- 7.0 Reference
- Chapter 5 Microbiological Examinations
- 1.0 Introduction
- 2.0 Indicator Organisms
- 2.1 The Coliform Group
- 2.2 The Enterococci Group
- 3.0 Methods
- 3.1 General Description
- 3.2 General Laboratory Equipment and Materials
- 3.3 Reagents
- 3.4 Sterilization of Equipment and Materials
- 3.5 Sample and Dilution Bottles
- 3.6 Filter Holders
- 3.7 Alternate Sterilization Procedures
- 4.0 Quality Assurance and Quality Control Requirements for Microbiological Methods
- 4.1 Sampling
- 4.2 Dechlorination
- 4.3 Storage and Holding Times
- 4.4 Sample Containers
- 4.5 Sample Volume and Dilutions
- 4.5.1 Dilutions for Membrane Filtration
- 4.5.2 Dilutions for Membrane Filtration and Most Probable Number (Quanti-Tray® or Equivalent)
- 4.5.2.1 1:10 Dilution
- 4.5.2.2 1:100 Dilution
- 4.5.2.3 Serial Dilutions
- 4.6 Positive and Negative Controls and Blanks
- 4.7 Duplicates
- 4.8 pH Meter and Buffers
- 4.9 Temperature Monitoring
- 5.0 Test Methods
- 5.1 Multiple Tube Fermentation
- 5.1.1 Introduction
- 5.1.2 Apparatus and Materials
- 5.1.3 Reagents
- 5.1.4 Quality Control
- 5.1.5 Procedure
- 5.1.6 Calculations
- 5.2 General Procedure for Membrane Filtration Methods
- 5.2.1 Introduction
- 5.2.2 Apparatus and Materials
- 5.2.3 Reagents
- 5.2.4 Quality Assurance and Quality Control
- 5.2.5 General Procedure
- 5.2.6 Calculations
- 5.3 Specific Membrane Filtration Methods
- 5.3.1 m-Endo Method
- 5.3.1.1 Introduction
- 5.3.1.2 Method-Specific Reagents
- 5.3.1.3 Procedure
- 5.3.1.4 Interpretation
- 5.3.1.5 Verification
- 5.3.1.6 Calculations
- 5.3.2 Membrane Fecal Coliform Method
- 5.3.2.1 Introduction
- 5.3.2.2 Method-Specific Media Preparation
- 5.3.2.3 Procedure
- 5.3.2.4 Interpretation
- 5.3.2.5 Calculations
- 5.3.3 Modified Membrane Thermotolerant Escherichia coli Method
- 5.3.3.1 Introduction
- 5.3.3.2 Method-Specific Reagents
- 5.3.3.3 Procedure
- 5.3.3.4 Interpretation
- 5.3.3.5 Calculations
- 5.3.4 Membrane ColiBlue®
- 5.3.5 Membrane-Enterococcus Indoxyl 1-D Glucoside Agar
- 5.3.5.1 Introduction
- 5.3.5.2 Method-Specific Media Preparation
- 5.3.5.3 Procedure
- 5.3.5.4 Interpretation
- 5.3.5.5 Calculations
- 5.4 Enzymatic Most Probable Number Methods
- 5.4.1 Colilert® and Colilert®-18
- 5.4.1.1 Introduction
- 5.4.1.2 Apparatus and Materials
- 5.4.1.3 Reagents
- 5.4.1.4 Procedure
- 5.4.1.5 Interpretation
- 5.4.1.6 Calculations
- 5.4.2 Enterolert®
- 5.4.2.1 Procedure
- 5.4.2.2 Interpretation
- 5.4.2.3 Calculations
- 6.0 References
- Chapter 6 Data Reporting and Monitoring
- 1.0 Data Recording
- 1.1 Benchsheets
- 1.2 Logbook
- 2.0 Expression of Results
- 2.1 Definitions
- 2.2 Rounding Off Numbers
- 2.3 Rounding Off Single Arithmetic Operations
- 2.3.1 Addition
- 2.3.2 Subtraction
- 2.3.3 Division and Multiplication
- 3.0 Completing the Discharge Monitoring Report
- 3.1 Introduction
- 3.2 Discharge Monitoring Report Hard Copy
- 3.3 Completing U.S. Environmental Protection Agency's NetDMR
- 3.3.1 Creating an Account and Requesting Access
- 3.3.2 My Account
- 3.4 Frequently Asked Questions About Discharge Monitoring Reports
- 3.5 Common Errors When Completing the Discharge Monitoring Report
- 4.0 Reference
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