Trace Environmental Quantitative Analysis: Including Student-Tested Experiments


What Caused the Birth of the Environmental Movement in the U.S.?What Happened When Flame Retardant Chemicals Were Inadvertently Substituted in Cattle Feed in Michigan?What Was the Government Response to the Mix-up?Was Analytical Testing for PBBs Established Within the State?What Were the Most Significant Analytical Results from the PBB Crisis?What Happened in Flint, Michigan? is it Important to Lower Detection Limits for Quantitating Blood PB?What Other Endeavors Require Trace Analysis?Can Examples Provide Insight into Trace Environmental Health and Environmental Chemical Quantitative Analysis?To What Extent Do Environmental Contaminants Enter Humans?What Might an Analytical Chemistry Approach to Biomonitoring Look Like?What Kind of Chemistry is This?Who Needs Environmental Testing?Who Requires Industry to Perform TEQA?How Does One Make Sense of All the “REGS”?What Analytical Methods Satisfy These Regulations?How Are the Regulatory Methods for TEQA Identified?Why is It Considered a Challenge to Implement an EPA Method?What Made EPA Method 625 So Unique?What About Methods for the Analysis of Air and Other Methods?What is the Physical/chemical Basis of the EPA’s Organics Protocol?ReferencesCalibration, Verification, Quantification, Statistical Treatment of Analytical Data, Detection Limits, and Quality Assurance/Quality ControlWhat Is Good Laboratory Practice?Can Data Reduction, Interpretation, and Statistical Treatment Be Summarized Before We Plunge into Calibration?How is Measurement Error Defined?Are There Laboratory-Based Examples of How Δ and δ are Used?How Important is Instrument Calibration and Verification?How Does the External Mode of Instrument Calibration Work?How Does the IS Mode of Instrument Calibration Work and Why is It Increasingly Important to TEQA?What Is Isotope Dilution?Can a Fundamental Quantification Equation Be Derived from Simple Principles?What is Organics IDMS?How Does the SA Mode of Instrument Calibration Work?Can We Derive a Quantification Equation for SA?What Does Least Squares Regression Really Mean?How Do You Derive the Least Squares Regression Equations?To What Extent Are We Confident in the Analytical Results?How Confident Are We of an Interpolated Result?How Do You Derive Equations to Find Instrument Detection Limits?Can We Derive Equations for Confidence Intervals About the Regression? Will These Equations Lead to Calculating IDLs?What is Weighted Least Squares and How Does This Influence IDLS?Is There a "Roadmap" We Can Use to Find Xc and Xd Based on WLS-CBCS?Finding the Critical Instrument Response yc and Critical Concentration xc While Minimizing Type 1 (False Positive) Errors for WLS/CBCSEstimating the Instrument Response Limit y[D], the Instrument Detection Limit x[D] and Calculating the Instrument Detection Limit x[D] While Minimizing Type 2 (False Negative) ErrorsHow Do MDLs Differ from IDLs?How Do I Obtain MDLs for My Analytical Method?Why So Many Replicate Measurements?How Do Analytical Chemists Deal with Replicate Analytical Data?How Do I Find the Limit of Quantitation?Is There a Way to Couple the Blank and Calibration Approaches to Find Xloq?Can Important Terms Be Clarified?What Does It Mean for a Laboratory to Have a Quality Assurance Program?Are There Definitions of QC Standards Used in the Lab?What QC Specs Must a Lab Meet?Minimum Demonstration of CapabilityLaboratory Background ContaminationAssessing Targeted and Surrogate Analyte RecoveryAssessing Goodness of Fit of the Experimental Calibration Data and the Range of LinearityAssessing ICV Precision and AccuracyAssessing Sample ResultsHow is an Environmental Testing Lab Organized?Which Lab Would You Choose?How Does the CDC Evaluate a Method Validation?From Transducers to Spreadsheets: What Does This Mean?How Does Analog Become Digital?How Does the 900 Series® Interface Convert Analog Signals to Digital Values?What Are Integration Parameters?How Are Analytical Results Reported?What Do I Need to Know About Sampling?ReferencesSample Preparation Techniques to Isolate and Recover Organics and InorganicsWhat Are the Principles Underlying LLE?Does Thermodynamics Explain Differences in NaCl Vs. HOAc Partitioning?What Are Solute Activities Anyway?Can the Difference Between K0 Values for Nacl and Hoac Be Shown Graphically?Can We Relate K0 to Analytically Measurable Quantities?Is Lle a Useful Cleanup Technique?How Do We Account for Secondary Equilibria in LLE?What If the Chemical Form of HOAc Changes in the Organic Phase?If We Know D, Can We Find the Percent Recovery?Are Organics the Only Analytes That Will Extract?Can Organic Cations or Anions Be Extracted?Is There an Important Application of IP-LLE to TEQA?Are There Other Examples of Nonspecific LLE Pertinent to TEQA?Can Lle Be Downsized?Does the Rate of Mass Transfer Become Important in µLLE?Is There Any Other Way to Perform LLE?What is Soxhlet Extraction Anyway?Are There Alternatives to S-LSE?What is Ultrasonic Liquid–Solid Extraction?Can Phase Diagrams Help to Explain These Alternative Sample Prep Techniques?What is Microwave-accelerated LSE?Have There Been Studies Applying MAE to Environmental Samples?Automated Liquid-solid Extraction (A-LSE)How Does ASE Work?What Samples Has Ase Been Applied To?Can Volatile Organics Be Isolated from Contaminated Water Using LLE?On What Basis Can VOCs Be Quantitated Using Static Headspace Techniques?What Happens When Gaseous SO2 is Dissolved in Water, Then Placed in a Vessel and Sealed?On What Basis Can We Quantitate TCE in Groundwater by HS-GC?On What Basis Does KTCE Depend?Must We Always Heat a Sample in HS-GC to Conduct TEQA?Is There an Example That Illustrates the Concept in Equation (3.31)?What Happens When KHSVOC Values Vary Significantly?Why is Static Headspace Sampling Not More Acceptable to the EPA?What If We Could Concentrate the Analyte in the Headspace Onto a Nonpolar Coated Fiber and Then Thermally Desorb ...Is There a Recently Updated EPA Method for VOCs Using Static HS Techniques?How Should I Proceed to Quantitate VOCs?What is Hexadecane Screening?What Are EPA’s Sample Prep Approaches to Trace VOCs?What is the P&T Technique?How Does One Go About Conducting the P&T Technique?Do All VOCs Purge with the Same Rate?What is Cleanup?Can Adsorption Chromatography Be Used to Achieve Compound Class Fractionation in Addition to Cleanup?How Does GPC Clean Up Oily Sample Extracts?How is Saponification Used to Clean Up Rat Feed to Isolate PCBs?How Do I Get Started Doing SFE?What Liquids and Gases Can Be Used to Conduct SFE?What Other Physico-chemical Properties Are of Interest in SFE?What Does an SFE Instrument Look Like?Is There an Epa Method That Requires SFE? If So, Please DescribeHave Comparative Studies for SFE Been Done?What Is Solid-phase Extraction?How Is SPE Done?How Can I Learn More About SPE Techniques?How Does SPE Work?Is SPE a Form of Column Chromatography?Can SPE Breakthrough Be Predicted?What is Solvent Polarity?Can a Solute’s Aqueous Solubility or Octanol–Water Partition Coefficient Be Used to Predict RP-SPE Percent Recoveries?What is Aqueous Solubility Anyway?What Does a Plot of KОW vs. Aqueous Solubility Tell Us?Can We Predict Values for KОW from Only a Knowledge of Molecular Structure?Are Values for KОW Useful to Predict Breakthrough in RP-SPE?Where Can One Obtain KОW Values?Can Breakthrough Volumes Be Determined More Precisely?Does an SPE Cartridge or Disk Have a Capacity Factor and If So, How Do We Calculate It?How Did RP-SPE Once Solve an Analytical Laboratory Dilemma in Enviro-Chemical TEQA?What Role Does RP-SPE Have in TEQA?Should I Use RP-SPE to Measure OCs in Drinking Water? How Could I Use RP-SPE to Isolate and Recover These Selected OCs from SoilCan Lindane, Endrin, and Methoxychlor Be Isolated and Recovered Using RP-SPE?Was Lindane Isolated and Recovered from a Biological Matrix Using RP-SPE? If So, How?What Does a Sample Analysis Report Using RP-SPE Techniques Look Like?Does It Matter Which Elution Solvent is Used in RP-SPE?How Can PCBs Be Isolated and Recovered from Serum, Plasma, or Organ for Trace Enviro-health QA?PBDEs, Used as Flame Retardants, Are More Contemporary Pollutants. Have These Organic Compounds Been Studied by RP-SPE Sample Prep Techniques?What Is Matrix Solid-phase Dispersion and Is It Applicable to Biological Tissue?What Factors Influence Percent Recoveries in MSPD?What Is Microextraction by Packed Sorbent (MEPS)?Can an Spme Fiber Extract SVOCs from Aqueous Samples?Can We Quantitate Before We Reach Equilibrium in Spme?What Factors Need to Be Considered When Using Spme to Isolate PCBs from Contaminated Groundwater?Might the Sample Matrix Influence SPME Efficiency?What is This Solid-Phase Extraction That Uses a Stir Bar?What Instrument Accessories Are Needed to Conduct SBSE?How is SBSE Performed?Can SPE, SPME, and SBSE Be Automated?Are There Examples of Automated SPE Out There?What is This Sample Prep Technique Called Quechers?Have Bloodspots Been Isolated and Recovered Using These Mini-extraction Techniques?How Are Heterogeneous Magnetic Materials Based on Metal-organic Frameworks (MOFS) Used to Isolate and Recover Priority Pollutant Organics from Comtaminated Waters Drawn from the Environment?How Are the Methods Categorized for Trace Inorganics Analysis?How Do You Prepare an Environmental Sample to Measure Trace Metals?What is Matrix Modification in GFAA?How Do I Prepare a Solid Waste, Sludge, Sediment, Biological Tissue, or Soil Sample?What Are the EPA’s Microwave Digestion Methods?What is Done to Prepare a Blood, Serum, or Urine Specimen for Trace Metals Analysis?What Can I Do to Preconcentrate a Sample for Trace Metal Analysis?How Do I Preconcentrate Cr(VI) from a Leachate Using Coprecipitation?To What Extent Can a Given Metal Chelate Be Recovered by LLE?How Do You Derive a More Useful Relationship for Metal Chelates?Can We Derive a Working Expression for the Distribution Ratio?Are There Other Ways to Preconcentrate Metal Ions from Environmental Samples?Can We Isolate and Recover a Neutral Metal Chelate from an Environmental Sample Using Bonded Silicas?How Does the Fraction of Cadmium Free or Complexed Vary?Can an Equation Be Derived Using These Δ Values to Find D?How Good is the Prediction of Equation (3.73)?How Are Other Toxic Metals/metalloids, Cyanide, and Phenols (often Found in Hazardous Waste Samples) Prepared for ...How Do You Prepare a Sample for Hg Determination?Could HS-SPME Combined with an Element-specific GC Be Used to Speciate HG?Can Arsenic Be Speciated?How is a Wastewater Sample Prepared in Order to Quantitate Trace Cyanide? What About Sulfides? What About Phenols?What is Chemical Derivatization and Why is It Still Important to TEQA?How Do You Make a PFB Derivative of Some Butyric Acids?How Do You Prepare a P-bromophenacyl Ester of N-butyric Acid as a Chromotag and Conduct a Quantitative Analysis?What is the Sample Prep Approach to Placing a Fluorotag on a Carboxylic Acid?What About Sample Prep Techniques Applicable to Ambient Air Analysis?What Commmon Sample Prep Devices Are Used to Obtain a Suitable Air Sample?What Can We Conclude About Sample Prep?ReferencesDeterminative Techniques to Measure Organics and InorganicsHow Do You Know Which Determinative Technique to Use?What is Differential Migration Anyway?What Causes the Bands to Separate?What Happens If We Really Increase the Number of Craig Tubes?What is Chromatography?Why is Gc So Dominant in TEQA?Why is HPLC More Universal in TEQA?Can We Visualize a Chromatographic Separation?Can We Develop Useful Mathematical Relationships for Chromatography?How Does One Control the Chromatographic Peak Width?Is There a More Practical Way to Define H?What Factors Contribute to Chromatographic Peak Broadening?How Does Longitudinal Diffusion Contribute to H?How Does All of This Fit Together?How Do We Distinguish Between Linear and Volumetric Flow Rates?What is Chromatographic Resolution?How Do You Derive This Fundamental Equation?What is Equation (4.30) Really Telling Us?How Does a GC Work?What Are External Gas Pneumatics and Are They Important in GC?The Safe Handling of Compressed Gases is Very Important!What About Gc Inlets? What Do I Need to Know?What is a Split Ratio and What Does Splitless Really Mean?What Does It Mean to Overload a Chromatographic Column?What is So Important About GC Columns?What GC Columns Are Used in TEQA?What is the Kovats Retention Index?Why Do I Not See Mcreynolds/rohrschneider Constants in Current Chromatography Catalogs?What Are Fused-silica Polysiloxane WCOTs?Why is Wcot Film Thickness Important?How Does Column Temperature Influence K'?What is PTGC Anyway?Can We Find How Retention Time Varies with Tc?This is All Well and Good, but Do I Not Find Temperature Programs Already Provided in EPA Methods?What Role Does Cryogenics Play in GC?What Are the Common GC Detectors and How Do They Work?How Does a Fid Work?What Are the Optimum Gas Flow Rates and Operating Characteristics of a FID?How Do a PID and an ELCD Work?What is an ECD, How Does It Work, and Why is It So Important to TEQA?How Responsive Are ECDs?Are There Other Element-Specific Detectors?What About Any Recently Developed Element-specific GC Detectors?Ok, but What About Chemiluminescence?Atomic Spectrometric Emission as a GC Detector: What Was It Anyway?Is It Possible to Prepare Environmental Samples and Quantitate Analytes of Interest Using GC-AED as the Determinative Technique?Calibration ConsiderationsQuantitative Analysis of the Biolatex Based on the Calibrated Response Factor (RF)Of the Plethora of Mass Specs, Which Are Most Useful to Quantitate Vocs/svocs by TEQA?Can We Predict What M/Z Values Are Stable Through the Quadrupole Rods?What is Mass Spectrometric Resolution Anyway?The Math is Ok, but What Really Happens to M·+ When It is Propelled into the Center of the Quadrupole?Is the MSD the Only Mass Spec Used in TEQA?Again, the Math is Ok, but This Time, What About Some Applications of C-GC-MS(ITD)?I Hear That a Mass Spec Must Be Tuned: How is This Done?What’s the Difference Between So-Called Soft vs. Hard Mass Spec?How Do Negative Ions Get Detected in GC-MS That Benefits TEQA?How Does GC-MS Using a Single Quadrupole Relate to TEQA?How Does a Time-of-Flight Mass Spectrometer Work?What Are We Really Seeing When We Peer into a Computer Screen While Acquiring GC-MS Data?How Are These Quant Ions Found?What is Tandem Mass Spectrometry and What Role Does It Play in TEQA?Is GC-MS-MS Used in TEQA?Where Does HPLC Play a Role in TEQA?What is HPLC?How Did the Name Reversed-phase HPLC Come About?Why Does the Mobile Phase Exert So Much Influence on Rs?How Do Hplc Detectors Work?How Do You Go About Doing Quantitative Analysis Using HPLC with UV Detection?How Does the Absorbance of a Solute Get Measured?What is an HPLC Fluorescence Detector?How Is It That Fluorescence Can Be Quantitated?How Do UV Absorption and Fluorescence Emission HPLC Chromatograms Compare?Can a Mass Spec Be Used as a Detector for HPLC?Is LC-MS-MS Used in TEQA?How Did Ic Make It to the Forefront in Trace Inorganics Analysis?Chemical Reactions Used in This DemonstrationHow Does an IC Work?Is There a Theoretical Basis for Conductivity Measurements?If IC is Not the Principal Determinative Technique to Measure Metals in the Environment, What Is?How Do I Choose Which Atomic Spectral Method to Use?What Happens When Various Inorganic Salts Are Thrust into Flames?How Does the Design of AA, AE, and AF Instruments Fundamentally Differ?What is ICP-AES?How Have Icp-aes Instruments Evolved?What Happens to Argon Gas (Ar) and to a Metal Analyte (M) in the Plasma?Can the Intensity of an Atomic Emission Line Be Predicted?Why Do The Ae Lines Broaden?What is ICP-MS and How Does This Determinative Technique Complement and Compete with ICP-AES?What Interferences Are Present and How Are These Overcome?How Is ICP-MS Used in Trace Metals Speciation?What Is Atomic Absorption?What Elements of the AA Spectrophotometer Do I Need to Know More About?Why is the GFAA a Suitable Trace Determinative Technique?What Determines the Strength of Absorption for a Given Metal Analyte?Why is It Important to Correct for Background Absorption?In What Ways Does IR Absorption Spectroscopy Contribute to TEQA?How Do I Quantitate Oil and Grease in Wastewater Using IR Absorption?What is TOC and How is IR Absorption Used?How Do the Two Types of TOC Analyzers Work?What is Capillary Electrophoresis and What Role Does It Have in TEQA?What Factors Influence Separations in CE?How Does Electrode Polarity Influence CE?What is Vacancy or Indirect UV Absorption Detection?How Important is Buffer pH in CE?I Understand There is Something New in Enviro-chemical TEQA When the Sample Matrix is Polluted Air: What is It?I Understand There is Something Called “ion Chemistry” in SIFT-MS. What is This?What Does the Future Hold for Determinative Techniques?ReferencesStudent-Tested Laboratory ExperimentsWhat Might a Typical Laboratory Schedule Look Like?How is the Instructional Laboratory Configured?How to Weigh the Right WayAn Introduction to pH Measurement: Estimating the Degree of Purity of Snow; Measuring Soil pH; Introduction to Ion ChromatographyIntroduction to the Visible SpectrophotometerVisible Spectrophotometric Determination of Trace Levels of Iron in GroundwaterSpectrophotometric Determination of Phosphorus in Eutrophicated Surface WaterDetermination of Anionic Surfactants by Mini-Liquid–Liquid Extraction (Mini-LLE) in an Industrial Wastewater Effluent Using Ion Pairing with Methylene BlueComparison of Ultraviolet and Infrared Absorption Spectra of Chemically Similar Organic CompoundsDetermination of Oil and Grease and of Total Petroleum Hydrocarbons in Wastewater Via Reversed-Phase Solid-Phase Extraction Techniues (RP-SPE) and Quantitative Fourier-Transform Infrared (FTIR) SpectroscopyDetermination of the Degree of Hardness in Various Sources of Groundwater Using Flame Atomic Absorption SpectroscopyDetermination of Lead in Drinking Water Using Graphite Furnace Atomic Absorption Spectroscopy (GFAA): External Standart vs. Standart Addition Calibration ModeA Comparison of Soil Types via a Quantitative Determination of the Chromium Content Using Visible Spectrophotometry and flame atomic absorption spectroscopy or inductively coupled plasma-optical emission spectrometryData Acquisition and Instrument Control Using the Turbochrom Chromatography Software. An Introduction to Аn introduction to high-performance liquid chromatography (HPLC): evaluating those experimental parameters that influence separationsIdentifying the Ubiquitous Phthalate Esters in the Environment Using HPLC, Photodiode Array Detection, and environment using HPLC, photodiode array detection, and confirmation by GC-MSAn Introduction to Gas Chromatography: Evaluating Experimental Parameters That Influence Gas Chromatographic PerformanceScreening for the Presence of BTEX in Wastewater Using Liquid–liquid Extraction (LLE) and Gas Chromatography: screening forthms in chlorine-disinfected drinking water using static headspace (HS) gas chromatographyDetermination of Priority Pollutant Volatile Organic Compounds (VOCs) in Gasoline-contaminated Groundwater Using organic compounds (VOCs) in gasoline-contaminated groundwater using static headspace (HS) and solid- phase microextraction headspace (SPME-HS) and gas chromatographyDetermination of the Herbicide Residue Trifluralin in Chemically Treated Lawn Soil by Gas Chromatography Using reversed-phase solid-phase extraction (RP-SPE) sample prep techniquesDetermination of Priority Pollutant Semivolatile Organochlorine Pesticides: A Comparison of Mini-liquid–liquid and Reverse-Phase Solid-Phase Extraction TechniquesDetermination of Priority Pollutant Polycyclic Aromatic Hydrocarbons (PAHs) in Contaminated Soil Using RP-HPLC-PDA aromatic hydrocarbons (PAHs) in contaminated soil using RP-HPLC-PDA with wavelength programmingHow to Set Up and Operate an Ion ChromatographDetermination of Inorganic Anions Using Ion Chromatography (IC): Anion Exchange IC with Suppressed Conductivity chromatography (IC): anion exchange 1C with suppressed conductivity detectionAppendix A: GlossaryAppendix B: QA/QC IllustratedAppendix C: A Primer on the Basics of Probability and Statistics for Some and a Quick Review for OthersAppendix D: Quality Control for Environmental-health TEQA: Levey-Jennings Plots and Westgard RulesAppendix E: Innovative Sample Prep Flow Charts for TEQAAppendix F: Quantitating VOCs in Serum Using Automated Headspace- SPME/Cryo-Focusing/lsotope Dilution/Capillary GC-MSAppendix G: Using a Pooled Standard Deviation to Find the Uncertainty in the Percent Recovery for the Priority Pollutant Phenol Using Reversed-Phase SPE from Spiked Water by Converting Phenol to its Pyrazol-3-One Complex: Comparing In Situ vs. Synthesized Experimental ApproachesAppendix H: Laboratory Glass & Instrument DesignsAppendix I: Useful Potpourri for Environmental Analytical Chemists
 
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