Laboratory Experiments in Trace Environmental Quantitative Analysis

Cover
Half Title
Title Page
Copyright Page
Dedication
Table of Contents
Preface
About the Author
Photos
Chapter 1 Introduction
1.1 What Might a Typical Laboratory Schedule Look Like?
1.2 How Is the Instructional Laboratory Configured?
1.3 How to Weigh the Right Way
Chapter 2 An Introduction to pH Measurement: Estimating the Degree of Purity of Snow, Measuring Soil pH: Introduction to Ion Chromatography
2.1 Background and Summary of Method
2.2 Experiment
2.2.1 Glassware Needed per Student
2.2.2 Chemical Reagents/pH Meter Needed per Student Workstation
2.2.3 Ion Chromatograph
2.2.4 Procedure
2.3 Suggested Reading
Chapter 3 Introduction to the Visible Spectrophotometer
3.1 Background and Summary of Method
3.2 Experiment
3.2.1 Glassware Needed per Student or Group
3.2.2 Chemical Reagents Needed per Student or Group
3.2.3 Miscellaneous Item Needed per Student or Group
3.2.4 Spectrophotometer
3.2.5 Product Line History of the Spec 20
3.2.6 Troubleshooting the Spec 20
3.2.7 Procedure
3.3 For the Report
3.4 Suggested Reading
Chapter 4 Visible Spectrophotometric Determination of Trace Levels of Iron in Groundwater
4.1 Background and Summary of Method
4.2 Experiment
4.2.1 Volumetric Glassware Needed per Student
4.2.2 Gravity Filtration Setup
4.2.3 Chemical Reagents Needed per Student or Group
4.2.4 Spectrophotometer
4.2.5 Procedure
4.2.6 Determination of Total Fe by FLAA or ICP-AES
4.3 For the Notebook
4.4 Suggested Reading
Chapter 5 Spectrophotometric Determination of Phosphorus in Eutrophicated Surface Water
5.1 Background and Summary of Method
5.2 Experiment
5.2.1 Preparation of Chemical Reagents
5.2.1.1 5 M Sulfuric Acid
5.2.1.2 Molybdate Reagent
5.2.1.3 1% Ascorbic Acid
5.2.1.4 Preparation of Stock Phosphorus
5.2.2 Procedure
5.3 For the Notebook
5.4 Suggested Reading
Chapter 6 Determination of Anionic Surfactants by Mini-Liquid–Liquid Extraction (MINI-LLE) in an Industrial Wastewater Effluent Using Ion Pairing with Methylene Blue
6.1 Background and Summary of Method
6.2 Experiment
6.2.1 Preparation of Chemical Reagents
6.2.1.1 Methylene Blue (MB)
6.2.1.2 3 M Sulfuric Acid
6.2.1.3 To Prepare a 0.5 M Sulfuric Acid Solution
6.2.1.4 To Prepare a 0.1 M Sodium Hydroxide Solution
6.2.1.5 To Prepare the Wash Solution
6.2.1.6 To Prepare the MB Reagent
6.2.2 Preparation of the 100 ppm Surfactant Stock Solution and General Comments on Standards
6.2.3 Operation and Calibration of the Orion SA 720A pH Meter
6.2.4 Procedure to conduct a miniaturized liquid-liquid extraction (LLE)
6.3 For the Report (a Written Laboratory Report Due on This Experiment)
6.4 Suggested Reading
Chapter 7 Comparison of Ultraviolet and Infrared Absorption Spectra of Chemically Similar Organic Compounds
7.1 Background and Summary of Method
7.1.1 UV-Vis Absorption Spectroscopy
7.1.2 Mid-Infrared Absorption Spectroscopy
7.2 Experiment
7.2.1 Items/Accessories Needed per Student or Group
7.2.2 Preparation of Chemical Reagents
7.2.3 Procedure to Obtain UV Absorption Spectra for Two Sets of Chemically Similar Organic Compounds: (1) Alkane Sulfonates vs. Alkyl Sulfates and (2) Two Esters with Different Carbon Backbones
7.2.4 Procedure to Obtain FTIR Absorption (Transmission) Spectra for Various Organic Compounds
7.3 For the Report
7.4 Suggested Reading
Chapter 8 Determination of Oil and Grease and of Total Petroleum Hydrocarbons in Wastewater via Reversed-Phase Solid-Phase Extraction Techniques (RP-SPE) and Quantitative Fourier-Transform Infrared (FTIR) Spectroscopy
8.1 Background and Summary of Method
8.2 Experiment
8.2.1 Preparation of Chemical Reagents
8.2.2 Reagents Needed per Student or Group of Students
8.2.3 Apparatus Needed per Group
8.2.4 Procedure
8.2.5 Percent Recovery Study
8.2.6 Probe Sonication: Liquid–Solid Extraction
8.2.7 Calibration of the FTIR Spectrophotometer
8.2.8 Isolation, Recovery, and Quantitation of Oil and Grease from Wastewater Samples
8.3 Calculations
8.4 Suggested Reading
Chapter 9 Determination of the Degree of Hardness in Various Sources of Groundwater Using Flame Atomic Absorption Spectroscopy
9.1 Background and Summary of Method
9.2 Experiment
9.2.1 Preparation of Chemical Reagents
9.2.2 Chemicals/Reagents Needed per Student or Group
9.2.3 FLAA Operating Analytical Requirement
9.2.4 Preparation of the Calibration Curve
9.2.5 Procedure
9.3 For the Lab Notebook (No Report Necessary)
9.4 Suggested Reading
Chapter 10 Determination of Lead in Drinking Water Using Graphite Furnace Atomic Absorption Spectroscopy (GFAA): External Standard vs. Standard Addition Calibration Mode
10.1 Background and Summary of Method
10.2 Experiment
10.2.1 Preparation of Chemical Reagents
10.2.2 Reagents Needed per Student or Group
10.2.3 Procedure
10.2.4 Using the WinLab® Software
10.2.5 Preparation of the Stock Reference Pb Standard and Start of the Autosampler
10.3 For the Notebook
10.4 Suggested Readings
Chapter 11 A 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 Spectrometry
11.1 Background and Summary of Method
11.2 Experiment
11.2.1 Chemical Reagents Needed per Student or Group
11.2.2 Procedure for Alkaline Digestion
11.2.3 Procedure for Conducting Visible Spectrophotometric Analysis
11.2.4 Procedure for Atomic Absorption Spectrophotometric Analysis or ICP-AES
11.3 For the Report
11.4 Suggested Reading
Chapter 12 Data Acquisition and Instrument Control Using the Turbochrom Chromatography Software: An Introduction to High-Performance Liquid Chromatography (HPLC): Evaluating Those Experimental Parameters That Influence Separations
12.1 Background and Summary of Method
12.1.1 HPLC and TEQA
12.1.2 Flow-through Packed Columns
12.1.3 HPLC Also Refers to an Instrument That Is a High-Pressure Liquid Chromatograph
12.2 Experiment
12.2.1 Preparation of Chemical Reagents
12.2.2 Accessories to Be Used with the HPLC per Group
12.2.3 Procedure
12.2.3.1 Initial Observations of a Computer-Controlled High-Performance Liquid Chromatograph
12.2.3.2 Creating a QuickStart Method, Acquiring Data, Optimizing, Calibrating, and Conducting Analysis Using the QuickStart Method
12.2.3.3 Effect of Solvent Strength on k’
12.2.3.4 Effect of Mobile-Phase Flow Rate on Resolution
12.3 For the Lab Notebook
12.4 Suggested Reading
Chapter 13 Identifying the Ubiquitous Phthalate Esters in the Environment Using HPLC, Photodiode Array Detection, and Confirmation by GC-MS
13.1 Background and Summary of Method
13.1.1 Analytical Method Development Using HPLC
13.1.2 GC-MS Using a Quadrupole Mass Spectrometer
13.2 Of What Value Is This Experiment?
13.3 Experiment
13.3.1 Preparation of Chemical Reagents
13.3.2 Accessories to be Used With the HPLC per Student or Group
13.3.3 Procedure
13.4 For the Report
13.5 Suggested Reading
Chapter 14 An Introduction to Gas Chromatography: Evaluating Experimental Parameters That Influence Gas Chromatographic Performance
14.1 Background and Summary of Method
14.2 Brief Description of Gas Chromatographs Located in the Hazardous Waste Analysis Lab at Michigan State University
14.3 Principle of Separation in GC
14.4 Experiment
14.4.1 Preparation of Chemical Reagents
14.4.2 Accessories to Be Used with the GC per Group
14.4.2.1 Summary of Turbochrom Methods to Be Used in this Experiment
14.4.3 Procedure
14.4.3.1 Measurement and Adjustment of Carrier Gas Flow Rate and Split Ratio
14.4.3.2 Comparison of the FID vs. the ECD Sensitivity
14.4.3.3 Injection Volume vs. GC Peak Shape
14.4.3.4 Flow Rate vs. Capillary Column Efficiency
14.4.3.5 Column Temperature vs. Capacity Factor
14.5 For the Lab Notebook
14.6 Suggested Readings
Chapter 15 Screening for the Presence of BTEX in Wastewater Using Liquid–Liquid Extraction (LLE) and Gas Chromatography: Screening for THMs in Chlorine-Disinfected Drinking Water Using Static Headspace (HS) Gas Chromatography
15.1 Background and Summary of Method
15.2 Of What Value Is This Experiment?
15.3 Experimental
15.3.1 Preparation of Chemical Reagents
15.3.2 Chemicals/Reagents Needed per Group
15.3.3 Items/Accessories Needed per Student or per Group
15.3.4 Preliminary Planning
15.3.5 Procedure for BTEX Instrumental Analysis Using Mini-LLE Techniques
15.3.5.1 Selecting the Most Suitable Extraction Solvent
15.3.5.2 Preparation of the Primary Dilution Standard and Working Calibration Standards
15.3.6 Procedure for THM Instrumental Analysis Using HS Techniques
15.3.7 Procedure to Conduct a Screen for BTEXs via Mini-LLE and Subsequent Injection into a GC-FID
15.3.8 Procedure to Conduct Manual Headspace Sampling and Direct Injection into a GC-ECD
15.4 For the Report
15.5 Suggested Readings
Chapter 16 Determination of Priority Pollutant Volatile Organic Compounds (VOCs) in Gasoline-Contaminated Groundwater Using Static Headspace (HS) and Solid-Phase Microextraction Headspace (SPME-HS) and Gas Chromatography
16.1 Background and Summary Method
16.2 Of What Value Is This Experiment?
16.3 Use of t Statistics
16.4 Experimental
16.4.1 Preparation of Chemical Reagents
16.4.2 Chemicals/Reagents Needed per Group
16.4.3 Items/Accessories Needed per Student or per Group
16.4.4 Preliminary Planning
16.4.5 Procedure for BTEX Instrumental Analysis HS Techniques
16.4.6 Technique to Conduct a Manual Headspace Sampling and Direct Injection Using a Gas-Tight Sampling Syringe
16.4.7 Technique to Conduct an SPME Headspace Sampling and Injection/Thermal Desorption Using an SPME Syringe/Fiber Assembly
16.5 For the Report
16.6 Suggested Readings
Chapter 17 Determination of the Herbicide Residue Trifluralin in Chemically Treated Lawn Soil by Gas Chromatography Using Reversed-Phase Solid-Phase Extraction (RP-SPE) Sample Prep Techniques
17.1 Background and Summary of Method
17.1.1 Solid-Phase Extraction
17.1.2 Internal Standard Mode of Calibration
17.2 Experiment
17.2.1 Preparation of Chemical Reagents
17.2.2 Chemicals/Reagents/Accessories Needed per Group
17.2.3 Preparation of the Working Calibration Standards
17.2.4 Establishing the Calibration
17.2.5 Isolating Trifluralin from Lawn-Treated Soil Using RP-SPE Techniques
17.3 For the Report
17.4 Suggested Reading
Chapter 18 Determination of Priority Pollutant Semivolatile Organochlorine Pesticides: A Comparison of Mini-Liquid–Liquid and Reversed-Phase Solid-Phase Extraction Techniques
18.1 Background and Summary of Method
18.2 Experimental
18.2.1 Preparation of Chemical Reagents
18.2.2 Chemicals/Reagents Needed per Group
18.2.3 Preliminary Planning
18.2.4 Selection of a Suitable Internal Standard
18.2.5 Procedure for Calibration and Quantitation of the GC-ECD
18.2.6 Procedure for Performing Mini-LLE and RP-SPE
18.3 For the Report
18.4 Suggested Reading
Chapter 19 Determination of Priority Pollutant Polycyclic Aromatic Hydrocarbons (PAHs) in Contaminated Soil Using RP-HPLC-PDA with Wavelength Programming
19.1 Background and Summary of Method
19.2 Of What Value Is This Experiment?
19.3 Experiment
19.3.1 Preparation of Chemical Reagents
19.3.2 Accessories to Be Used with the HPLC per Group
19.3.3 Procedure
19.3.3.1 Creating the Wavelength Program Method
19.3.3.2 Extraction Procedure for Soil
19.3.3.3 Calculation of the # ppm of Each PAH in Contaminated Soil
19.4 For the Report
19.5 Suggested Reading
Chapter 20 How to Set up and Operate an Ion Chromatograph
20.1 Determination of Inorganic Anions Using Ion Chromatography (IC): Anion Exchange IC with Suppressed Conductivity Detection
20.1.1 Background
20.2 How Do I Operate the Ion Chromatograph?
20.3 Is There a Need for Sample Prep?
20.4 How Do I Prepare a Reference Stock Standard for Each Anion?
20.5 How Do I Prepare the Bicarbonate/Carbonate Eluent from Scratch?
20.6 How Do I Prepare a Mixed Anion Stock Standard for IC?
20.7 How Do I Prepare a Four-Level Set of Calibration Standards for IC?
20.8 What Does the Data Look Like?
20.9 Suggested Reading
Index