دانلود کتاب Trace environmental quantitative analysis : including student-tested experiments

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Cover
Half Title
Title Page
Copyright Page
Dedication
Table of Contents
Preface to the Third Edition
About the Author
Contributors
1 Introduction to Trace Environmental Quantitative Analysis (TEQA)
1.1 What Caused the Birth of the Environmental Movement in the U.S.?
1.2 What Happened When Flame Retardant Chemicals Were Inadvertently Substituted in Cattle Feed in Michigan?
1.3 What Was the Government Response to the Mix-up?
1.4 Was Analytical Testing for PBBs Established Within the State?
1.5 What Were the Most Significant Analytical Results from the PBB Crisis?
1.6 What Happened in Flint, Michigan? is it Important to Lower Detection Limits for Quantitating Blood PB?
1.7 What Other Endeavors Require Trace Analysis?
1.8 Can Examples Provide Insight into Trace Environmental Health and Environmental Chemical Quantitative Analysis?
1.9 To What Extent Do Environmental Contaminants Enter Humans?
1.10 What Might an Analytical Chemistry Approach to Biomonitoring Look Like?
1.11 What Kind of Chemistry is This?
1.12 Who Needs Environmental Testing?
1.13 Who Requires Industry to Perform TEQA?
1.14 How Does One Make Sense of All the “REGS”?
1.15 What Analytical Methods Satisfy These Regulations?
1.16 How Are the Regulatory Methods for TEQA Identified?
1.17 Why is It Considered a Challenge to Implement an EPA Method?
1.18 What Made EPA Method 625 So Unique?
1.19 What About Methods for the Analysis of Air and Other Methods?
1.20 What is the Physical/chemical Basis of the EPA’s Organics Protocol?
References
2 Calibration, Verification, Quantification, Statistical Treatment of Analytical Data, Detection Limits, and Quality ...
2.1 What Is Good Laboratory Practice?
2.2 Can Data Reduction, Interpretation, and Statistical Treatment Be Summarized Before We Plunge into Calibration?
2.2.1 How is Measurement Error Defined?
2.2.2 Are There Laboratory-Based Examples of How Δ andD δ are U Used?
2.3 How Important is Instrument Calibration and Verification?
2.3.1 How Does the External Mode of Instrument Calibration Work?
2.3.2 How Does the IS Mode of Instrument Calibration Work and Why is It Increasingly Important to TEQA?
2.3.2.1 What Is Isotope Dilution?
2.3.2.2 Can a Fundamental Quantification Equation Be Derived from Simple Principles?
2.3.2.3 What is Organics IDMS?
2.3.3 How Does the SA Mode of Instrument Calibration Work?
2.3.3.1 Can We Derive a Quantification Equation for SA?
2.4 What Does Least Squares Regression Really Mean?
2.4.1 How Do You Derive the Least Squares Regression Equations?
2.4.2 To What Extent Are We Confident in the Analytical Results?
2.4.3 How Confident Are We of an Interpolated Result?
2.5 How Do You Derive Equations to Find Instrument Detection Limits?
2.5.1 Can We Derive Equations for Confidence Intervals About the Regression? Will These Equations Lead to Calculating IDLs?
2.5.2 What is Weighted Least Squares and How Does This Influence IDLS?
2.5.3 Is There a “roadmap” We Can Use to Find X_c and X_d Based on WLS-CBCS?
2.5.3.1 Finding the Critical Instrument Response Y_c and Critical Concentration X_c While Minimizing ...
2.5.3.2 Estimating the Instrument Response Limit y[D]., the Instrument Detection Limit x[D] and Calculating the ...
2.5.4 How Do MDLs Differ from IDLs?
2.5.5 How Do I Obtain MDLs for My Analytical Method?
2.6 Why So Many Replicate Measurements?
2.6.1 How Do Analytical Chemists Deal with Replicate Analytical Data?
2.7 How Do I Find the Limit of Quantitation?
2.7.1 Is There a Way to Couple the Blank and Calibration Approaches to Find X_loq?
2.8 Can Important Terms Be Clarified?
2.9 What Does It Mean for a Laboratory to Have a Quality Assurance Program?
2.10 Are There Definitions of QC Standards Used in the Lab?
2.11 What QC Specs Must a Lab Meet?
2.11.1 Minimum Demonstration of Capability
2.11.2 Laboratory Background Contamination
2.11.3 Assessing Targeted and Surrogate Analyte Recovery
2.11.4 Assessing Goodness of Fit of the Experimental Calibration Data and the Range of Linearity
2.11.5 Assessing ICV Precision and Accuracy
2.11.6 Assessing Sample Results
2.12 How is an Environmental Testing Lab Organized?
2.13 Which Lab Would You Choose?
2.14 How Does the CDC Evaluate a Method Validation?
2.14.1 Evaluation Criteria
2.14.2 Multi-rule QC (Westgard)
2.14.3 Additional Cdc Validation Criteria
2.15 From Transducers to Spreadsheets: What Does This Mean?
2.15.1 How Does Analog Become Digital?
2.15.2 How Does the 900 Series® Interface Convert Analog Signals to Digital Values?
2.15.3 What Are Integration Parameters?
2.15.4 How Are Analytical Results Reported?
2.16 What Do I Need to Know About Sampling?
2.16.1 What Happened When Frozen Blood Specimens Were Thawed Repeatedly?
2.16.2 Can We Predict How Many Samples Must Be Taken When Sampling the Environment?
2.16.3 How Might We Obtain a Representative Sample from a Large Environmental Location?
2.16.4 What Factors Need to Be Considered in Obtaining Representative Samples?
References
3 Sample Preparation Techniques to Isolate and Recover Organics and Inorganics
3.1 What Are the Principles Underlying LLE?
3.2 Does Thermodynamics Explain Differences in NaCl Vs. HOAc Partitioning?
3.3 What Are Solute Activities Anyway?
3.4 Can the Difference Between K⁰ Values for Nacl and Hoac Be Shown Graphically?
3.5 Can We Relate K⁰ to Analytically Measurable Quantities?
3.6 Is Lle a Useful Cleanup Technique?
3.7 How Do We Account for Secondary Equilibria in LLE?
3.8 What If the Chemical Form of HOAc Changes in the Organic Phase?
3.9 If We Know D, Can We Find the Percent Recovery?
3.10 Are Organics the Only Analytes That Will Extract?
3.11 Can Organic Cations or Anions Be Extracted?
3.12 Is There an Important Application of IP-LLE to TEQA?
3.13 Are There Other Examples of Nonspecific LLE Pertinent to TEQA?
3.14 Can Lle Be Downsized?
3.15 Does the Rate of Mass Transfer Become Important in µLLE?
3.16 Is There Any Other Way to Perform LLE?
3.17 What is Soxhlet Extraction Anyway?
3.18 Are There Alternatives to S-LSE?
3.19 What is Ultrasonic Liquid–Solid Extraction?
3.20 Can Phase Diagrams Help to Explain These Alternative Sample Prep Techniques?
3.21 What is Microwave-accelerated LSE?
3.22 Have There Been Studies Applying MAE to Environmental Samples?
3.23 Automated Liquid-solid Extraction (A-LSE)
3.24 How Does ASE Work?
3.25 What Samples Has Ase Been Applied To?
3.26 Can Volatile Organics Be Isolated from Contaminated Water Using LLE?
3.27 On What Basis Can VOCs Be Quantitated Using Static Headspace Techniques?
3.28 What Happens When Gaseous SO₂ is Dissolved in Water, Then Placed in a Vessel and Sealed?
3.29 On What Basis Can We Quantitate TCE in Groundwater by HS-GC?
3.30 On What Basis Does K^TCE Depend?
3.31 Must We Always Heat a Sample in HS-GC to Conduct TEQA?
3.32 Is There an Example That Illustrates the Concept in Equation (3.31)?
3.33 What Happens When KHSVOC Values Vary Significantly?
3.34 Why is Static Headspace Sampling Not More Acceptable to the EPA?
3.35 What If We Could Concentrate the Analyte in the Headspace Onto a Nonpolar Coated Fiber and Then Thermally Desorb ...
3.36 Is There a Recently Updated EPA Method for VOCs Using Static HS Techniques?
3.37 How Should I Proceed to Quantitate VOCs?
3.38 What is Hexadecane Screening?
3.39 What Are EPA’s Sample Prep Approaches to Trace VOCs?
3.40 What is the P&T Technique?
3.41 How Does One Go About Conducting the P&T Technique?
3.42 Do All VOCs Purge with the Same Rate?
3.43 What is Cleanup?
3.44 Can Adsorption Chromatography Be Used to Achieve Compound Class Fractionation in Addition to Cleanup?
3.45 How Does GPC Clean Up Oily Sample Extracts?
3.46 How is Saponification Used to Clean Up Rat Feed to Isolate PCBs?
3.47 How Do I Get Started Doing SFE?
3.48 What Liquids and Gases Can Be Used to Conduct SFE?
3.49 What Other Physico-chemical Properties Are of Interest in SFE?
3.50 What Does an SFE Instrument Look Like?
3.51 Is There an Epa Method That Requires SFE? If So, Please Describe
3.52 Have Comparative Studies for SFE Been Done?
3.53 What Is Solid-phase Extraction?
3.54 How Is SPE Done?
3.55 How Can I Learn More About SPE Techniques?
3.56 How Does SPE Work?
3.57 Is SPE a Form of Column Chromatography?
3.58 Can SPE Breakthrough Be Predicted?
3.59 What is Solvent Polarity?
3.60 Can a Solute’s Aqueous Solubility or Octanol–Water Partition Coefficient Be Used to Predict RP-SPE Percent Recoveries?
3.61 What is Aqueous Solubility Anyway?
3.62 What Does a Plot of K_ow vs. Aqueous Solubility Tell Us?
3.63 Can We Predict Values for K_ow from Only a Knowledge of Molecular Structure?
3.64 Are Values for K_ow Useful to Predict Breakthrough in RP-SPE?
3.65 Where Can One Obtain K_ow Values?
3.66 Can Breakthrough Volumes Be Determined More Precisely?
3.67 Does an SPE Cartridge or Disk Have a Capacity Factor and If So, How Do We Calculate It?
3.68 How Did RP-SPE Once Solve an Analytical Laboratory Dilemma in Enviro-Chemical TEQA?
3.69 What Role Does RP-SPE Have in TEQA?
3.70 Should I Use RP-SPE to Measure OCs in Drinking Water? How Could I Use RP-SPE to Isolate and Recover These Selected OCs ...
3.71 Can Lindane, Endrin, and Methoxychlor Be Isolated and Recovered Using RP-SPE?
3.72 Was Lindane Isolated and Recovered from a Biological Matrix Using RP-SPE? If So, How?
3.73 What Does a Sample Analysis Report Using RP-SPE Techniques Look Like?
Report on the Quantitative Determination of Lindane in Myometrial Tissue Suspended Cells in Saline
Summary of Method
Calibration
Sample Analysis
Method Evaluation
3.74 Does It Matter Which Elution Solvent is Used in RP-SPE?
3.75 How Can PCBs Be Isolated and Recovered from Serum, Plasma, or Organ for Trace Enviro-health QA?
3.76 PBDEs, Used as Flame Retardants, Are More Contemporary Pollutants. Have These Organic Compounds Been Studied by ...
3.77 What Is Matrix Solid-phase Dispersion and Is It Applicable to Biological Tissue?
3.78 What Factors Influence Percent Recoveries in MSPD?
3.79 What Is Microextraction by Packed Sorbent (MEPS)?
3.80 Can an Spme Fiber Extract SVOCs from Aqueous Samples?
3.81 Can We Quantitate Before We Reach Equilibrium in Spme?
3.82 What Factors Need to Be Considered When Using Spme to Isolate PCBs from Contaminated Groundwater?
3.83 Might the Sample Matrix Influence SPME Efficiency?
3.84 What is This Solid-Phase Extraction That Uses a Stir Bar?
3.85 What Instrument Accessories Are Needed to Conduct SBSE?
3.86 How is SBSE Performed?
3.87 Can SPE, SPME, and SBSE Be Automated?
3.88 Are There Examples of Automated SPE Out There?
3.89 What is This Sample Prep Technique Called Quechers?
3.90 Have Bloodspots Been Isolated and Recovered Using These Mini-extraction Techniques?
3.91 How Are Heterogeneous Magnetic Materials Based on Metal-organic Frameworks (MOFS) Used to Isolate and Recover ...
3.92 How Are the Methods Categorized for Trace Inorganics Analysis?
3.93 How Do You Prepare an Environmental Sample to Measure Trace Metals?
3.94 What is Matrix Modification in GFAA?
3.95 How Do I Prepare a Solid Waste, Sludge, Sediment, Biological Tissue, or Soil Sample?
3.96 What Are the EPA’s Microwave Digestion Methods?
3.97 What is Done to Prepare a Blood, Serum, or Urine Specimen for Trace Metals Analysis?
3.98 What Can I Do to Preconcentrate a Sample for Trace Metal Analysis?
3.99 How Do I Preconcentrate Cr(VI) from a Leachate Using Coprecipitation?
3.100 To What Extent Can a Given Metal Chelate Be Recovered by LLE?
3.101 How Do You Derive a More Useful Relationship for Metal Chelates?
3.102 Can We Derive a Working Expression for the Distribution Ratio?
3.103 Are There Other Ways to Preconcentrate Metal Ions from Environmental Samples?
3.104 Can We Isolate and Recover a Neutral Metal Chelate from an Environmental Sample Using Bonded Silicas?
3.105 How Does the Fraction of Cadmium Free or Complexed Vary?
3.106 Can an Equation Be Derived Using These Δ Values to Find D?
3.107 How Good is the Prediction of Equation (3.73)?
3.108 How Are Other Toxic Metals/metalloids, Cyanide, and Phenols (often Found in Hazardous Waste Samples) Prepared for ...
3.109 How Do You Prepare a Sample for Hg Determination?
3.110 Could HS-SPME Combined with an Element-specific GC Be Used to Speciate HG?
3.111 Can Arsenic Be Speciated?
3.112 How is a Wastewater Sample Prepared in Order to Quantitate Trace Cyanide? What About Sulfides? What About Phenols?
3.113 What is Chemical Derivatization and Why is It Still Important to TEQA?
3.114 How Do You Make a PFB Derivative of Some Butyric Acids?
3.114.1 To Prepare the Reagents
3.114.2 To Synthesize and Extract the PFB Ester
3.115 How Do You Prepare a P-bromophenacyl Ester of N-butyric Acid as a Chromotag and Conduct a Quantitative Analysis?
3.115.1 Preparation of Mixed Alkylating (ALK RGT) Reagent
3.115.2 Preparation of Fatty Acid Stock Reference Standard
3.115.3 Preparation of 1 M Aqueous KHCO₃
3.115.4 To Prepare the Potassium Salt of Butyric Acid (n-BuOOH)
3.115.5 Preparation of Working Calibration Standards
3.115.6 Derivatization
3.116 What is the Sample Prep Approach to Placing a Fluorotag on a Carboxylic Acid?
3.117 What About Sample Prep Techniques Applicable to Ambient Air Analysis?
3.118 What Commmon Sample Prep Devices Are Used to Obtain a Suitable Air Sample?
3.119 What Can We Conclude About Sample Prep?
References
4 Determinative Techniques to Measure Organics and Inorganics
4.1 How Do You Know Which Determinative Technique to Use?
4.2 What is Differential Migration Anyway?
4.3 What Causes the Bands to Separate?
4.4 What Happens If We Really Increase the Number of Craig Tubes?
4.5 What is Chromatography?
4.6 Why is Gc So Dominant in TEQA?
4.7 Why is HPLC More Universal in TEQA?
4.8 Can We Visualize a Chromatographic Separation?
4.9 Can We Develop Useful Mathematical Relationships for Chromatography?
4.10 How Does One Control the Chromatographic Peak Width?
4.11 Is There a More Practical Way to Define H?
4.12 What Factors Contribute to Chromatographic Peak Broadening?
4.13 How Does Longitudinal Diffusion Contribute to H?
4.14 How Does All of This Fit Together?
4.15 How Do We Distinguish Between Linear and Volumetric Flow Rates?
4.16 What is Chromatographic Resolution?
4.17 How Do You Derive This Fundamental Equation?
4.18 What is Equation (4.30) Really Telling Us?
4.19 How Does a GC Work?
4.20 What Are External Gas Pneumatics and Are They Important in GC?
4.20.1 The Safe Handling of Compressed Gases is Very Important!
4.21 What About Gc Inlets? What Do I Need to Know?
4.22 What is a Split Ratio and What Does Splitless Really Mean?
4.23 What Does It Mean to Overload a Chromatographic Column?
4.24 What is So Important About GC Columns?
4.25 What GC Columns Are Used in TEQA?
4.26 What is the Kovats Retention Index?
4.27 Why Do I Not See Mcreynolds/rohrschneider Constants in Current Chromatography Catalogs?
4.28 What Are Fused-silica Polysiloxane WCOTs?
4.29 Why is Wcot Film Thickness Important?
4.30 How Does Column Temperature Influence K\'?
4.31 What is PTGC Anyway?
4.32 Can We Find How Retention Time Varies with Tc?
4.33 This is All Well and Good, but Do I Not Find Temperature Programs Already Provided in EPA Methods?
4.34 What Role Does Cryogenics Play in GC?
4.35 What Are the Common GC Detectors and How Do They Work?
4.36 How Does a Fid Work?
4.37 What Are the Optimum Gas Flow Rates and Operating Characteristics of a FID?
4.38 How Do a PID and an ELCD Work?
4.39 What is an ECD, How Does It Work, and Why is It So Important to TEQA?
4.40 How Responsive Are ECDs?
4.41 Are There Other Element-Specific Detectors?
4.42 What About Any Recently Developed Element-specific GC Detectors?
4.43 Ok, but What About Chemiluminescence?
4.44 Atomic Spectrometric Emission as a GC Detector: What Was It Anyway?
4.45 Is It Possible to Prepare Environmental Samples and Quantitate Analytes of Interest Using GC-AED as the Determinative ...
4.45.1 Calibration Considerations
4.45.2 Quantitative Analysis of the Biolatex Based on the Calibrated Response Factor (RF)
4.46 Of the Plethora of Mass Specs, Which Are Most Useful to Quantitate Vocs/svocs by TEQA?
4.47 Can We Predict What M/Z Values Are Stable Through the Quadrupole Rods?
4.48 What is Mass Spectrometric Resolution Anyway?
4.49 The Math is Ok, but What Really Happens to M·⁺ When It is Propelled into the Center of the Quadrupole?
4.50 Is the MSD the Only Mass Spec Used in TEQA?
4.51 Again, the Math is Ok, but This Time, What About Some Applications of C-GC-MS(ITD)?
4.52 I Hear That a Mass Spec Must Be Tuned: How is This Done?
4.53 What’s the Difference Between So-Called Soft vs. Hard Mass Spec?
4.54 How Do Negative Ions Get Detected in GC-MS That Benefits TEQA?
4.55 How Does GC-MS Using a Single Quadrupole Relate to TEQA?
4.56 How Does a Time-of-Flight Mass Spectrometer Work?
4.57 What Are We Really Seeing When We Peer into a Computer Screen While Acquiring GC-MS Data?
4.58 How Are These Quant Ions Found?
4.59 What is Tandem Mass Spectrometry and What Role Does It Play in TEQA?
4.60 Is GC-MS-MS Used in TEQA?
4.61 Where Does HPLC Play a Role in TEQA?
4.62 What is HPLC?
4.63 How Did the Name Reversed-phase HPLC Come About?
4.64 Why Does the Mobile Phase Exert So Much Influence on R_s?
4.65 Are All Octadecyl-Bonded Silica HPLC Columns the Same?
4.66 How Do Hplc Detectors Work?
4.67 How Do You Go About Doing Quantitative Analysis Using HPLC with UV Detection?
4.68 How Does the Absorbance of a Solute Get Measured?
4.69 What is an HPLC Fluorescence Detector?
4.70 How Is It That Fluorescence Can Be Quantitated?
4.71 How Do UV Absorption and Fluorescence Emission HPLC Chromatograms Compare?
4.72 Can a Mass Spec Be Used as a Detector for HPLC?
4.73 Is LC-MS-MS Used in TEQA?
4.74 How Did Ic Make It to the Forefront in Trace Inorganics Analysis?
4.74.1 Chemical Reactions Used in This Demonstration
4.75 How Does an IC Work?
4.76 Is There a Theoretical Basis for Conductivity Measurements?
4.77 If IC is Not the Principal Determinative Technique to Measure Metals in the Environment, What Is?
4.78 How Do I Choose Which Atomic Spectral Method to Use?
4.79 What Happens When Various Inorganic Salts Are Thrust into Flames?
4.80 How Does the Design of AA, AE, and AF Instruments Fundamentally Differ?
4.81 What is ICP-AES?
4.82 How Have Icp-aes Instruments Evolved?
4.83 What Happens to Argon Gas (Ar) and to a Metal Analyte (M) in the Plasma?
4.84 Can the Intensity of an Atomic Emission Line Be Predicted?
4.85 Why do the AE Lines Broaden?
4.86 What is ICP-MS and How Does This Determinative Technique Complement and Compete with ICP-AES?
4.87 What Interferences Are Present and How Are These Overcome?
4.88 How Is ICP-MS Used in Trace Metals Speciation?
4.89 What Is Atomic Absorption?
4.90 What Elements of the AA Spectrophotometer Do I Need to Know More About?
4.91 Why is the GFAA a Suitable Trace Determinative Technique?
4.92 What Determines the Strength of Absorption for a Given Metal Analyte?
4.93 Why is It Important to Correct for Background Absorption?
4.94 In What Ways Does IR Absorption Spectroscopy Contribute to TEQA?
4.95 How Do I Quantitate Oil and Grease in Wastewater Using IR Absorption?
4.96 What is TOC and How is IR Absorption Used?
4.97 How Do the Two Types of TOC Analyzers Work?
4.98 What is Capillary Electrophoresis and What Role Does It Have in TEQA?
4.99 What Factors Influence Separations in CE?
4.100 How Does Electrode Polarity Influence CE?
4.101 What is Vacancy or Indirect UV Absorption Detection?
4.102 How Important is Buffer pH in CE?
4.103 I Understand There is Something New in Enviro-chemical TEQA When the Sample Matrix is Polluted Air: What is It?
4.104 I Understand There is Something Called “ion Chemistry” in SIFT-MS. What is This?
4.105 What Does the Future Hold for Determinative Techniques?
References
5 Student-Tested Laboratory Experiments
5.1 What Might a Typical Laboratory Schedule Look Like?
5.2 How is the Instructional Laboratory Configured?
5.3 How to Weigh the Right Way
5.4 An Introduction to Ph Measurement: Estimating the Degree of Purity of Snow; Measuring Soil Ph; Introduction to Ion Chromato
5.4.1 Background and Summary of Method
5.4.2 Experimental
5.4.2.1 Glassware Needed per Student
5.4.2.2 Chemical Reagents/pH Meter Needed per Student Workstation
5.4.2.3 Ion Chromatograph
5.4.2.4 Procedure
5.4.3 Suggested Readings
5.5 Introduction to the Visible Spectrophotometer
5.5.1 Background and Summary of Method
5.5.2 Experimental
5.5.2.1 Glassware Needed per Student or Group
5.5.2.2 Chemical Reagents Needed per Student or Group
5.5.2.3 Miscellaneous Item Needed per Student or Group
5.5.2.4 Spectrophotometer
5.5.2.5 Product Line History of the Spec 20
5.5.2.6 Troubleshooting the Spec 20
5.5.2.7 Procedure
5.5.3 For the Report
5.5.4 Suggested Readings
5.6 Visible Spectrophotometric Determination of Trace Levels of Iron in Groundwater
5.6.1 Background and Summary of Method
5.6.2 Experimental
5.6.2.1 Volumetric Glassware Needed per Student
5.6.2.2 Gravity Filtration Setup
5.6.2.3 Chemical Reagents Needed per Student or Group
5.6.2.4 Spectrophotometer
5.6.2.5 Procedure
5.6.2.6 Determination of Total Fe by FLAA or ICP-AES
5.6.3 For the Notebook
5.6.4 Suggested Readings
5.7 Spectrophotometric Determination of Phosphorus in Eutrophicated Surface Water
5.7.1 Background and Summary of Method
5.7.2 Experimental
5.7.2.1 Preparation of Chemical Reagents
5.7.2.1.1 5 M Sulfuric Acid
5.7.2.1.2 Molybdate Reagent
5.7.2.1.3 1% Ascorbic Acid
5.7.2.1.4 Preparation of Stock Phosphorus
5.7.2.2 Procedure
5.7.3 For the Notebook
5.7.4 Suggested Readings
5.8 Determination of Anionic Surfactants by Mini-Liquid–Liquid Extraction (Mini-LLE) in an Industrial Wastewater Effluent …
5.8.1 Background and Summary of Method
5.8.2 Experimental
5.8.2.1 Preparation of Chemical Reagents
5.8.2.1.1 Methylene Blue (MB)
5.8.2.1.2 3m Sulfuric Acid
5.8.2.1.3 To Prepare a 0.5 M Sulfuric Acid Solution
5.8.2.1.4 To Prepare a 0.1 M Sodium Hydroxide Solution
5.8.2.1.5 To Prepare the Wash Solution
5.8.2.1.6 To Prepare the MB Reagent
5.8.2.2 Preparation of the 100 ppm Surfactant Stock Solution and General Comments on Standards
5.8.2.3 Operation and Calibration of the Orion Sa 720A pH Meter
5.8.2.4 Procedure for Mini-LLE
5.8.3 For the Report (A Written Laboratory Report Due on This Experiment)
5.8.4 Suggested Readings
5.9 Comparison of Ultraviolet and Infrared Absorption Spectra of Chemically Similar Organic Compounds
5.9.1 Background and Summary of Method
5.9.1.1 UV-Vis Absorption Spectroscopy
5.9.1.2 Mid-infrared Absorption Spectroscopy
5.9.2 Experimental
5.9.2.1 Items/Accessories Needed per Student or Group
5.9.2.2 Preparation of Chemical Reagents
5.9.2.3 Procedure to Obtain UV Absorption Spectra for Two Sets of Chemically Similar Organic Compounds: (1) An Alkane ...
5.9.2.4 Procedure to Obtain FTIR Absorption (Transmission) Spectra for Various Organic Compounds
5.9.3 For the Report
5.9.4 Suggested Readings
5.10 Determination of Oil and Grease and of Total Petroleum Hydrocarbons in Wastewater Via Reversed-Phase Solid-Phase ...
5.10.1 Background and Summary of Method
5.10.2 Experimental
5.10.2.1 Preparation of Chemical Reagents
5.10.2.2 Reagents Needed per Student or Group of Students
5.10.2.3 Apparatus Needed per Group
5.10.2.4 Procedure
5.10.2.5 Percent Recovery Study
5.10.2.6 Probe Sonication: Liquid–solid Extraction
5.10.2.7 Calibration of the FTIR Spectrophotometer
5.10.2.8 Isolation, Recovery and Quantitation of Oil and Grease from Wastewater Samples
5.10.3 Calculations
5.10.4 Suggested Readings
5.11 Determination of the Degree of Hardness in Various Sources of Groundwater Using Flame Atomic Absorption Spectroscopy
5.11.1 Background and Summary of Method
5.11.2 Experimental
5.11.2.1 Preparation of Chemical Reagents
5.11.2.2 Chemicals/reagents Needed per Student or Group
5.11.2.3 Flaa Operating Analytical Requirement
5.11.2.4 Preparation of the Calibration Curve
5.11.2.5 Procedure
5.11.3 For the Lab Notebook (No Report Necessary)
5.11.4 Suggested Readings
5.12 Determination of Lead in Drinking Water Using Graphite Furnace Atomic Absorption Spectroscopy (GFAA): External ...
5.12.1 Background and Summary of Method
5.12.2 Experimental
5.12.2.1 Preparation of Chemical Reagents
5.12.2.2 Reagents Needed per Student or Group
5.12.2.3 Procedure
5.12.2.4 Using the Winlab® Software
5.12.2.5 Preparation of the Stock Reference Pb Standard and Start of the Autosampler
5.12.3 For the Notebook
5.12.4 Suggested Readings
5.13 A Comparison of Soil Types via a Quantitative Determination of the Chromium Content Using Visible Spectrophotometry ...
5.13.1 Background and Summary of Method
5.13.2 Experimental
5.13.2.1 Chemical Reagents Needed per Student or Group
5.13.2.2 Procedure for Alkaline Digestion
5.13.2.3 Procedure for Conducting Visible Spectrophotometric Analysis
5.13.2.4 Procedure for Atomic Absorption Spectrophotometric Analysis or ICP-AES
5.13.3 For the Report
5.13.4 Suggested Readings
5.14 Data Acquisition and Instrument Control Using the Turbochrom Chromatography Software. An Introduction to ...
5.14.1 Background and Summary of Method
5.14.1.1 HPLC and TEQA
5.14.1.2 Flow-through Packed Columns
5.14.1.3 HPLC Also Refers to an Instrument That is a High-Pressure Liquid Chromatograph
5.14.2 Experimental
5.14.2.1 Preparation of Chemical Reagents
5.14.2.2 Accessories to Be Used with the HPLC per Group
5.14.2.3 Procedure
5.14.2.3.1 Initial Observations of a Computer-controlled High-performance Liquid Chromatograph
5.14.2.3.2 Creating a Quickstart Method, Acquiring Data, Optimizing, Calibrating, and Conducting Analysis Using the ...
5.14.2.3.3 Effect of Solvent Strength on K\'
5.14.2.3.4 Effect of Mobile-phase Flow Rate on Resolution
5.14.3 For the Lab Notebook
5.14.4 Suggested Readings
5.15 Identifying the Ubiquitous Phthalate Esters in the Environment Using HPLC, Photodiode Array Detection, and ...
5.15.1 Background and Summary of Method
5.15.1.1 Analytical Method Development Using HPLC
5.15.1.2 GC-MS Using a Quadrupole Mass Spectrometer
5.15.2 Of What Value is This Experiment?
5.15.3 Experimental
5.15.3.1 Preparation of Chemical Reagents
5.15.3.2 Accessories to Be Used with the HPLC per Student or Group
5.15.3.3 Procedure
5.15.4 For the Report
5.15.5 Suggested Readings
5.16 An Introduction to Gas Chromatography: Evaluating Experimental Parameters That Influence Gas Chromatographic Performance
5.16.1 Background and Summary of Method
5.16.2 Brief Description of Gas Chromatographs Located in the Hazardous Waste Analysis Lab at Michigan State University
5.16.3 Principle of Separation in GC
5.16.4 Experimental
5.16.4.1 Preparation of Chemical Reagents
5.16.4.2 Accessories to Be Used with the GC per Group
5.16.4.2.1 Summary of Turbochrom Methods to Be Used in This Experiment
5.16.4.3 Procedure
5.16.4.3.1 Measurement and Adjustment of Carrier Gas Flow Rate and Split Ratio
5.16.4.3.2 Comparison of the FID vs. the ECD Sensitivity
5.16.4.3.3 Injection Volume vs. GC Peak Shape
5.16.4.3.4 Flow Rate vs. Capillary Column Efficiency
5.16.4.3.5 Column Temperature vs. Capacity Factor
5.16.5 For the Lab Notebook
5.16.6 Suggested Readings
5.17 Screening for the Presence of BTEX in Wastewater Using Liquid–liquid Extraction (LLE) and Gas Chromatography: ...
5.17.1 Background and Summary of Method
5.17.2 Of What Value is This Experiment?
5.17.3 Experimental
5.17.3.1 Preparation of Chemical Reagents
5.17.3.2 Chemicals/Reagents Needed per Group
5.17.3.3 Items/Accessories Needed per Student or per Group
5.17.3.4 Preliminary Planning
5.17.3.5 Procedure for BTEX Instrumental Analysis Using Mini-LLE Techniques
5.17.3.5.1 Selecting the Most Suitable Extraction Solvent
5.17.3.5.2 Preparation of the Primary Dilution Standard and Working Calibration Standards
5.17.3.6 Procedure for Thm Instrumental Analysis Using Hs Techniques
5.17.3.7 Procedure to Conduct a Screen for BTEXs Via Mini-LLE and Subsequent Injection into a GC-FID
5.17.3.8 Procedure to Conduct Manual Headspace Sampling and Direct Injection into a GC-ECD
5.17.4 For the Report
5.17.5 Suggested Readings
5.18 Determination of Priority Pollutant Volatile Organic Compounds (VOCs) in Gasoline-contaminated Groundwater Using …
5.18.1 Background and Summary Method
5.18.2 Of What Value is This Experiment?
5.18.3 Use of T Statistics
5.18.4 Experimental
5.18.4.1 Preparation of Chemical Reagents
5.18.4.2 Chemicals/Reagents Needed per Group
5.18.4.3 Items/accessories Needed per Student or per Group
5.18.4.4 Preliminary Planning
5.18.4.5 Procedure for BTEX Instrumental Analysis HS Techniques
5.18.4.6 Technique to Conduct a Manual Headspace Sampling and Direct Injection Using a Gas-Tight Sampling Syringe
5.18.4.7 Technique to Conduct an SPME Headspace Sampling and Injection/thermal Desorption Using an Spme Syringe/Fiber ...
5.18.5 For the Report
5.18.6 Suggested Readings
5.19 Determination of the Herbicide Residue Trifluralin in Chemically Treated Lawn Soil by Gas Chromatography Using ...
5.19.1 Background and Summary of Method
5.19.1.1 Solid-Phase Extraction
5.19.1.2 Internal Standard Mode of Calibration
5.19.2 Experimental
5.19.2.1 Preparation of Chemical Reagents
5.19.2.2 Chemicals/Reagents/Accessories Needed per Group
5.19.2.3 Preparation of the Working Calibration Standards
5.19.2.4 Establishing the Calibration
5.19.2.5 Isolating Trifluralin from Lawn-Treated Soil Using RP-SPE Techniques
5.19.3 For the Report
5.19.4 Suggested Readings
5.20 Determination of Priority Pollutant Semivolatile Organochlorine Pesticides: A Comparison of Mini-liquid–liquid and Reverse
5.20.1 Background and Summary of Method
5.20.2 Experimental
5.20.2.1 Preparation of Chemical Reagents
5.20.2.2 Chemicals/Reagents Needed per Group
5.20.2.3 Preliminary Planning
5.20.2.4 Selection of a Suitable Internal Standard
5.20.2.5 Procedure for Calibration and Quantitation of the GC-ECD
5.20.2.6 Procedure for Performing Mini-LLE and Rp-spe
5.20.3 For the Report
5.20.4 Suggested Readings
5.21 Determination of Priority Pollutant Polycyclic Aromatic Hydrocarbons (PAHs) in Contaminated Soil Using RP-HPLC-PDA …
5.21.1 Background and Summary of Method
5.21.2 Of What Value is This Experiment?
5.21.3 Experimental
5.21.3.1 Preparation of Chemical Reagents
5.21.3.2 Accessories to Be Used with the HPLC per Group
5.21.3.3 Procedure
5.21.3.3.1 Creating the Wavelength Program Method
5.21.3.3.2 Extraction Procedure for Soil
5.21.3.3.3 Calculation of the # ppm of Each Pah in Contaminated Soil
5.21.4 For the Report
5.21.5 Suggested Readings
5.22 How to Set Up and Operate an Ion Chromatograph
5.23 Determination of Inorganic Anions Using Ion Chromatography (IC): Anion Exchange IC with Suppressed Conductivity ...
5.23.1 Background
5.23.2 How Do I Operate a Typical Ion Chromatograph?
5.23.3 Is There a Need for Sample Prep?
5.23.4 How Do I Prepare a Reference Stock Standard for Each Anion?
5.23.5 How Do I Prepare the Bicarbonate/carbonate Eluent from Scratch?
5.23.6 How Do I Prepare a Mixed Anion Stock Standard for IC?
5.23.7 How Do I Prepare a Four-level Set of Calibration Standards for IC?
5.23.8 What Does the Data Look Like?
5.23.9 Suggested Readings
Appendix A: Glossary
Appendix B QA/QC Illustrated
Appendix C A Primer on the Basics of Probability and Statistics for Some and a Quick Review for Others
References
Appendix D Quality Control for Environmental-health TEQA
Reference
Appendix E Innovative Sample Prep Flow Charts for TEQA
References
Appendix F Quantitating VOCs in Serum Using Automated Headspace-spme/cryo-focusing/isotope Dilution/capillary GC-MS
References
Appendix G Using a Pooled Standard Deviation to Find the Uncertainty in the Percent Recovery for the Priority Pollutant …
References
Appendix H Laboratory Glass & Instrument Designs
Appendix I Useful Potpourri for Environmental Analytical Chemists
Appendix J Contributing Authors
Index