Environmental Sampling and Analysis: Lab Manual

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ISBN: 9781566701785 | 1566701783
Cover: Paperback
Copyright: 3/24/1997

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This manual covers the latest laboratory techniques, state-of-the-art instrumentation, laboratory safety, & quality assurance & quality control requirements. In addition to complete coverage of laboratory techniques, it also provides an introduction to the inorganic nonmetallic constituents in environmental samples, their chemistry, & their control by regulations & standards. Environmental Sampling & Analysis Laboratory Manual is perfect for college & graduate students learning laboratory practices, as well as consultants & regulators who make evaluations & quality control decisions. Anyone performing laboratory procedures in an environmental lab will appreciate this unique & valuable text.

Chapter 1 INTRODUCTION TO CHEMICAL ANALYSIS

(8)

1.1 The Nature of Analytical Chemistry

(1)

1.2 General Direction of Chemical Analysis

(8)

1.2.1 The Responsibility and Psychology of the Analyst

(1)

1.2.2 Cleanliness in the Laboratory

(1)

1.2.3 Recording Analyltical Data

(1)

1.2.4 Planning Laboratory Work

(3)

1.2.5 Documents to be Saved

(2)

Chapter 2 SAFETY AND LABORATORY WORK

(12)

2.1 Laboratory Hazards

(5)

2.1.1 Chemical Hazards

(4)

2.1.2 Fire Hazards

(1)

2.1.3 Careless Habits

(1)

2.2 Safe Handling of Compressed Gases

(1)

2.2.1 General Precautions When Working with Compressed Gases

(1)

2.2.2 Hazardous Properties of Compressed Gases

(1)

2.3 Stockroom Safety Rules

(3)

2.3.1 Cheklist for Safety Room

(2)

2.3.2 Storage of Chemicals

(1)

2.4 Laboratory Safety Rules

(3)

Chapter 3 QUALITY ASSURANCE OF CHEMICAL MEASUREMENTS

(18)

3.1 Introduction

(2)

3.1.1 Quality Assurance (QA)

(1)

3.1.2 Quality Control (QC)

(1)

3.1.3 Quality Assessment

(1)

3.2 Laboratory Quality Assurance Program

(16)

3.2.1 Sampling

(4)

3.2.2 Sample Custody

(1)

3.2.3 Sample preparation for Analysis

(1)

3.2.4 Analytical Methodology

(2)

3.2.5 Analytical System Calibration

(1)

3.2.6 Detection Limits

(2)

3.2.7 Statistics in Chemical Analysis

(2)

3.2.8 Quality Control Charts

(1)

3.2.9 Items for the Essential Control of Chemical Measurements

(3)

Chapter 4 LABORATORY APPARATUS AND GLASSWARE

(12)

4.1 Labware Materials

(1)

4.1.1 Soft Laboratory Glassware vs. Heat-Resistant Glassware

(1)

4.1.2 Plastic Labware

(1)

4.1.3 Porcelain Labware

(1)

4.1.4 Plantinum Crucible

(1)

4.1.5 Nickel Crucible

(1)

4.2 Volumetric Glassware

(8)

4.2.1 Volumetric Flask

(3)

4.2.2 Pipets and Their Use

(2)

4.2.3 Burets and Their Use

(2)

4.2.4 Cleaning of Volumetric Glassware

(1)

4.3 The Analytical Balance

(2)

4.4 Desiccator

(1)

Chapter 5 CHEMICALS, REAGENTS, AND STANDARDS

(16)

5.1 Chemicals

(1)

5.1.1 Grades and Purity of Chemicals

(1)

5.1.2 Proper Storage of Chemicals and Standards

(1)

5.2 Laboratory Pure Water

(2)

5.2.1 Methods for Preparation of Laboratory Pure Water

(1)

5.3 Reagents and Solutions

(13)

5.3.1 Expressing Concentration of a Solution

(4)

5.3.2 Diluting Solutions

(1)

5.3.3 Handling Reagents and Solutions

(7)

Chapter 6 STANDARD SOLUTIONS

(8)

6.1 Stock Standard Solutions

(1)

6.2 Standardization of Solutions

(1)

6.3 Preparation and Standardization of Common Standard Solution

(7)

6.3.1 Sulfuric Acid (H2SO4) Solution 0.1 N

(1)

6.3.2 Hydrochloric Acid (HCl) Solultion 0.1 N

(1)

6.3.3 Sodium Hydroxide (NaOH) Solution 0.1 N

(1)

6.3.4 Iodine (I2) Solution 0.1 N

(1)

6.3.5 Sodium Thiosulfate (Na2S2O3) Solution 0.1 N

(1)

6.3.6 Potassium Permanganate (KMnO4) Solution 0.1 N

(2)

Chapter 7 COMMON LABORATORY TECHNIQUES

(22)

7.1 Filtration

(6)

7.1.1 Filtration Methods

(1)

7.1.2 Filter Media

(4)

7.1.3 Gravity Filtration

(1)

7.1.4 Vacuum Filtration

(1)

7.2 Centrifugation

(3)

7.2.1 Using a Common Laboratory Centrifuge

(1)

7.2.2 Centrifuge Safety Rules

(1)

7.3 Distillation

(4)

7.3.1 Simple Distillation

(2)

7.3.2 Fractional Distillation

(1)

7.3.3 Vacuum Distillation

(1)

7.4 Refluxing

(1)

7.5 Ion Exchange

(1)

7.6 Drying and Ashing Samples

(1)

7.6.1 Drying Samples

(1)

7.6.2 Ashing

(1)

7.7 Dissolving the Sample

(1)

7.7.1 Decomposition under Pressure in a Closed System

(1)

7.7.2 Decomposition in an Open System

(1)

7.7.3 Digestion

(1)

7.7.4 Fusion

(1)

7.8 Extraction

(5)

7.8.1 Liquid-Liquid Extraction by Separatory Funnel

(2)

7.8.2 Continuous Liquid-Liquid Extraction

(1)

7.8.3 Sohxlet Extraction

(2)

Chapter 8 GRAVIMETRIC METHODS OF ANALYSIS

(8)

8.1 General Principles

(3)

8.1.1 Types of Precipitate

(1)

8.1.2 Aging and Digestion of the Precipitate

(1)

8.1.3 Manipulations Associated with the Filtration Process

(2)

8.2 Gravimetric Calculation

100

(2)

8.2.1 Utilization of the Gravimetric Factor

101

(1)

8.3 Gravimetric Analysis and Modern Analyltical Chemistry

102

(3)

Chapter 9 TITRIMETRIC ANALYSIS

105

(6)

9.1 General Principles

105

(2)

9.1.1 Chief Requirements for a Titration

105

(1)

9.1.2 Indicators

106

(1)

9.1.3 Volumetric Glassware

106

(1)

9.1.4 Reactions Used for Titration

106

(1)

9.1.5 Performing a Titration

107

(1)

9.2 Calculating the Result of a Titration

107

(1)

9.2.1 Results Given in the Same Concentration a the Titrant

107

(1)

9.2.2 Results Given in Concentrations, Using Normality

108

(1)

9.3 Back-Titration

108

(3)

Chapter 10 ACID-BASE TITRATION

111

(12)

10.1 Acids and Bases

111

(1)

10.1.1 Arrhenius Theory of Acids and Bases

111

(1)

10.1.2 Bronsted-Lowry Concept of Acids and Bases

112

(1)

10.2 Basic Concept of Chemical Equilibrium

112

(5)

10.2.1 Acid-Base Equilibrium

112

(1)

10.2.2 Self-Ionization of Water

113

(1)

10.2.3 pH Calculations

114

(3)

10.2.4 Measurement of pH

117

(1)

10.2.5 Buffers

117

(1)

10.3 Acid-Base Titration

117

(6)

10.3.1 Acid-Base Titration Curves

117

(3)

10.3.2 Acid-Base Indicators

120

(3)

Chapter 11 COMPLEXOMETRIC, OXIDATION-REDUCTION, AND OTHER TIRRATIONS

123

(10)

11.1 Complexometric Titration

123

(4)

11.1.1 Complex Formation

123

(3)

11.1.2 Compleometric Titration

126

(1)

11.2 Oxidation-Reduction Titration

127

(4)

11.2.1 Theory of Oxidation-Reduction

127

(2)

11.2.2 Redox Titrations

129

(2)

11.3 Precipitation Formation Titration

131

(2)

11.3.1 Mohr Method for Halides

131

(1)

11.3.2 Volhard Method

131

(1)

11.3.3 The Use of Adsorption Indicators: The Fajans Method

132

(1)

Chapter 12 SPECTROPHOTOMERY

133

(20)

12.1 Fundamentals of Spectroscopy

133

(6)

12.1.1 Early History of the Nature of Light

133

(1)

12.1.2 Electromagnetic Radiation

134

(2)

12.1.3 Continuous and Line Spectra

136

(2)

12.1.4 Beer's Law

138

(1)

12.2 Molecular Spectrophotometry

139

(8)

12.2.1 Molecular Absorption and Color

139

(1)

12.2.2 Molecular Absorption Spectrophotometry

139

(1)

12.2.3 Basic Components of Spectrophotometers

140

(2)

12.2.4 Single-Beam and Double-Beam Spectrophotometer

142

(2)

12.2.5 UV, Visible, and Infrared Spectrophotometers

144

(3)

12.3 Calibration of Spectrophotometers

147

(6)

12.3.1 General Rules in Preparation of Calibration Curves

148

(1)

12.3.2 Linear Regression Calculation

148

(1)

12.3.3 Performance Check of UV / VIS and IR Spectrophotometers

149

(1)

12.3.4 Maintenance of UV / VIS and IR Spectrophotometers

150

(3)

Chapter 13 POTENTIOMETRY AND ION-SELECTIVE ELECTRODES

153

(12)

13.1 Principles of Electrochemistry

153

(3)

13.1.1 Galvanic Cell

153

(2)

13.1.2 Dependence of EMF on Concentration

155

(1)

13.1.3 The Nernst Equation

155

(1)

13.2 Determining Concentrations from Cell Potential

156

(9)

13.2.1 The Saturated Calomel Reference Electrode

156

(1)

13.2.2 Potentiometer and Electronic Voltmeter

157

(1)

13.2.3 Ion-Selective Electrodes (ISEs)

158

(7)

Chapter 14 ENVIRONMENTAL TESTING LABORATORIES

165

(16)

14.1 Environmental Regulations

165

(3)

14.1.1 Overview of Federal Regulations

165

(3)

14.1.2 Overview of State Programs

168

(1)

14.2 Laboratory Operations for the Analysis of Regulated Substances

168

(3)

14.2.1 Methodology

169

(1)

14.2.2 EPA-Approved Methods and References for Analayzing Water Samples

169

(1)

14.2.3 EPA-Approved Methods and Reference for Analyzing Soils, Sediments, and Residuals

170

(1)

14.2.4 Approved Modifications of EPA Methods

171

(1)

14.2.5 EPA Contract Laboratory Protocol

171

(1)

14.3 Laboratory QA / QC

171

(1)

14.4 Standards

172

(6)

14.4.1 Drinking Water Standards

172

(1)

14.4.2 Waste Characterization

172

(4)

14.4.3 Irrigation Water Quality

176

(2)

14.5 Analytical Departments in Environmental Testing Laboratories

178

(3)

Chapter 15 RAW DATA CONVERSION INTO REPORTABLE RESULTS

181

(10)

15.1 Raw Data and Reportable Data

181

(1)

15.2 Calculations for Final Values

181

(6)

15.2.1 Temperature Correction for pH Values

181

(1)

15.2.2 Temperature Compensation for Conductivity

182

(1)

15.2.3 Solids, Moisture, and Ash Calculation

182

(1)

15.2.4 Calculations Related to Titrimetric Analysis

183

(1)

15.2.5 Calculations Related to Spectrophotometric and Potentiometric Analytical Performances

183

(1)

15.2.6 Calculating the Results for Solid Matrixes

183

(1)

15.2.7 Calculation of Total Hardness from Calcium and Magnesium Values

184

(1)

15.2.8 Calculation of Magnesium Values from Total Hardness as CaCO3 and Calcium as CaCO3

185

(1)

15.2.9 Calculation of Carbonate, Bicarbonate, and Hydroxide from Alklinity

185

(2)

15.3 Calculation of Calcium Carbonate Saturation, Corrosivity

187

(1)

15.4 Dilutions and Concentrations

188

(1)

15.5 Significant Figures

189

(2)

15.5.1 Exponential Notation

189

(2)

Chapter 16 EVALUATION AND APPROVAL OF ANALYTICAL DATA

191

(8)

16.1 Validation of Analytical QC Checks

191

(3)

16.1.1 Documentation of the Out-of-Control Condition

194

(1)

16.2 Checking the Correctness of the Analysis

194

(5)

16.2.1 Calculation of TDS

195

(1)

16.2.2 TDS and Electrical Conductance Ratio

195

(1)

16.2.3 Anion-Cation Balance

195

(1)

16.2.4 Relation between Conductivity and Total Cations and Anions

196

(1)

16.2.5 Relation between Total Hardness and Calcium and Magnesium Values

196

(1)

16.2.6. Relation of the Different Forms of Nitrogens

197

(1)

16.2.7 Relation of the Different Form of Phosphorus

197

(2)

Chapter 17 REPORTING ANALYTICAL DATA

199

(4)

17.1 Required Documentation

199

(1)

17.1.1 Documentation Required to Approve and Defend Reported Data

199

(1)

17.2 Significant Figures in Analytical Reports

200

(1)

17.3 Units used to Express Analytical Results

200

(1)

17.4 Report with Confidence Interval

201

(1)

17.5 Report Format

201

(2)

Chapter 18 DETERMINATION OF COLOR, ODOR, AND CONDUCTIVITY

203

(8)

18.1 Introduction to the Physical Properties

203

(1)

18.2 Color

203

(2)

18.2.1 General Discussion

203

(1)

18.2.2 Sample Collection and Storage

203

(1)

18.2.3 Sample Pretreatment

204

(1)

18.2.4 Color Determination by Platinum-Cobalt Method

204

(1)

18.3 Odor

205

(1)

18.3.1 General Discussion

205

(1)

18.3.2 Sample Collection and Handling

205

(1)

18.3.3 Sample Pretreatment

205

(1)

18.3.4 Measurement of Odor with Threshold Odor Test

206

(1)

18.4 Conductivity

206

(5)

18.4.1 General Discussion

206

(2)

18.4.2 Sample Collection and Handling

208

(1)

18.4.3 Measurement

208

(3)

Chapter 19 ANALYSIS OF SOLIDS AND TURBIDITY

211

(10)

19.1 Solids

211

(7)

19.1.1 General Discussion

211

(1)

19.1.2 Sample Collection and Handling

211

(1)

19.1.3 Sample Pretreatment

211

(1)

19.1.4 Determination of Total Solids (TS) Dried at 103-105C

211

(1)

19.1.5 Determination of Total Dissolved Solids (TDS) Dried at 180 C

212

(3)

19.1.6 Determination of Total Suspended Solids (TSS) Dried at 103-105C

215

(1)

19.1.7 Fixed and Volatile Solids Ignited at 500C

216

(1)

19.1.8 Total, Fixed, and Volatile Solids in Solid and Semisolid Samples

217

(1)

19.1.9 Settleable Fluids

218

(1)

19.2 Turbidity

(3)

19.2.1 General Discussion

218

(1)

19.2.2 Sample Collection and Handling

219

(1)

19.2.3 Measurement of Turbidity by Nephelometric Method

219

(2)

Chapter 20 ALKALINITY AND pH CALCIUM CARBONATE SATURATION

221

(10)

20.1 Alkalinity

221

(5)

20.1.1 General Discussion

221

(1)

20.1.2 Sample Collection and Storage

221

(1)

20.1.3 Potentiometric Titration Method

222

(2)

20.1.4 Titrimetric Method by Color Change

224

(1)

20.1.5 Calculation of Alkalinity Relationships

225

(1)

20.1.6 Conversion of the Three Forms of Alkalinity Expressed as CaCO3 to Their Ionic Forms

226

(1)

20.2 Determination of pH

226

(3)

20.2.1 General Discussion

226

(1)

20.2.2 Sample Collection and Holding Time

226

(1)

20.2.3 Potentiometric Determination of pH

226

(3)

20.3 Calcium Carbonate Saturation

229

(2)

20.3.1 General Discussion

229

(1)

20.3.2 Calculation of the Saturation Index

230

(1)

Chapter 21 ANALYSIS OF FLUORIDE AND TOTAL HARDNESS

231

(14)

21.1 Fluoride

231

(7)

21.1.1 General Discussion

231

(1)

21.1.2 Sampling and Storage

231

(1)

21.1.3 Determination of Fluoride by Ion-Selective Electrode

231

(7)

21.2 Total Hardness as CaCo3

238

(5)

21.2.1 General Discussion

238

(1)

21.2.2 Sampling and Storage

239

(1)

21.2.3 Determination of Hardness by EDTA Titrimetric Method

239

(3)

21.2.4 Total Hardness by Calculation

242

(1)

21.2.5 Calculation of Carbonate and Noncarbonate Hardness

242

(1)

21.3 Calcium Determination by EDTA Titrimetric Method

243

(1)

21.4 Determination of Magnesium by Calculation

244

(1)

Chapter 22 DETERMINATION OF RESIDUAL CHLORINE, CHLORIDE, AND CYANIDE

245

(14)

22.1 Chlorine Residual

245

(3)

22.1.1 General Disucssion

245

(1)

22.1.2 Sample Collection and Handling

246

(1)

22.1.3 Measurement

246

(1)

22.1.4 Chlorine Determination by Iodmetric Titration Method

246

(2)

22.2 Chloride

248

(3)

22.2.1 General Discussion

248

(1)

22.2.2 Sample Collection and Handling

248

(1)

22.2.3 Analysis by Mercuric Nitrate Titrimetric Method

249

(2)

22.3 Total Cyanide

251

(6)

22.3.1 General Discussion

251

(1)

22.3.2 Sample Collection and Handling

251

(1)

22.3.3 Determination of Cyanide by Colorimetric Method After Distillation

251

(6)

22.4 Cyanides Amenable To Chlorination After Distillation

257

(2)

22.4.1 General Discussion

257

(1)

22.4.2 Analysis

257

(2)

Chapter 23 NITROGEN COMPOUNDS AND ANALYSIS OF AMMONIA NITROGEN

259

(14)

23.1 Nitrogen Compounds and Nitrogen Cycle

259

(1)

23.2 Ammonia-Nitrogen

260

(13)

23.2.1 General Discussion

260

(1)

23.2.2 Sample Collection and Storage

260

(1)

23.2.3 Ammonia-Nitrogen Determination by Nesslerization

260

(4)

23.2.4 Ammonia Determination by Ion-Selective Electrode

264

(4)

23.2.5 Ammonia Determination by Titrimetric Method

268

(1)

23.2.6 Automated Phenate Method

269

(1)

23.2.7 Ammonia Determination in Soil, Sludge, or Sediment Samples

270

(3)

Chapter 24 ANALYSIS OF NITRITE AND NITRATE, AND TOTAL KJELDAHL NITROGEN

273

(14)

24.1 Nitrite-Nitrogen, NO2-N

273

(2)

24.1.1 General Discussion

273

(1)

24.1.2 Sample Collection and Handling

273

(1)

24.1.3 Determination of NO2-N by Colorimetric Method

273

(2)

24.2 Nitrate-Nitrogen, NO3-N

275

(8)

24.2.1 General Disucssion

275

(1)

24.2.2 Sample Collection and Handling

276

(1)

24.2.3 Nitrate Analysis by Ion-Selective Electrode Method

276

(3)

24.2.4 Nitrite + Nitrate Nitrogen Determination by Cadmium Reduction Method

279

(3)

24.2.5 Automated Cadmium Reduction Method

282

(1)

24.2.6 Determination of Nitrite-Nitrogen in Soils and Sediments

282

(1)

24.3 Total Kjeldahl Nitrogen (TKN) and Organic Nitrogen

283

(4)

24.3.1 General Discussion

283

(1)

24.3.2 Sample Collection and Handling

283

(1)

24.3.3 Analysis of Total Kjeldahl Nitrogen (TKN)

283

(4)

Chapter 25 DETERMINATION OF PHOSPHORUS

287

(8)

25.1 Phosphate-Phosphorus as PO4-P

287

(1)

25.1.1 General Discussion

287

(1)

25.1.2 Sampling and Storage

288

(1)

Determination of Phosphate, PO4-P

288

(7)

25.2.1 Acid Hydrolysis for Condensed Phosphate

288

(1)

25.2.2 Persulfate Digestion Method for Total Phosphates

289

(1)

25.2.3 Determination of Phosphorus by Asscorbic Acid Method

290

(3)

25.2.4 Automated Ascorbic Aicd Reduction Method

293

(2)

Chapter 26 DETERMINATION OF SULFIDE

295

(10)

26.1 Analysis of Hydrogen Sulfide

295

(4)

26.1.1 General Discussion

295

(1)

26.1.2 Sample Collection and Handling

295

(1)

26.1.3 Sulfide Determination by Iodometric Method

295

(3)

26.1.4 Calculation of Uni-Ionized Hydrogen Sulfide

298

(1)

26.2 Determination of Total Sulfide in Liquid and Solid Wastes

299

(6)

26.2.1 General Discussion

299

(1)

26.2.2 Sample Collection and Handling

300

(1)

26.2.3 Distillation Followed by Iodometric Method

300

(5)

Chapter 27 DETERMINATION OF SULFITE AND SULFATE

305

(8)

27.1 Analysis of Sulfite, So2/3

305

(2)

27.1.1 General Discussion

305

(1)

27.1.2 Sample Collection and Handling

305

(1)

27.1.3 Iodometric Titration Method

305

(2)

27.2 Determination of Sulfate, SO2/4

307

(6)

27.2.1 General Discussion

307

(1)

27.2.2. Sample Collection and Handling

308

(1)

27.2.3 Sulfate Determination with Turbidimetric Method

308

(2)

27.2.4 Automated Methylthymol Blue (MTB) Method

310

(3)

Chapter 28 CATION EXCHANGE CAPACITY

313

(4)

28.1 General Discussion

313

(1)

28.1.1 Sample Collection and Storage

313

(1)

28.2 Cation Exchange Capacity by Ammonium Acetate Method

313

(4)

Appendix A LABORATORY FIRST AID

317

(6)

General Rules

317

(1)

Imporatant Steps

317

(1)

First Aid for Thermal Burns

318

(1)

First Aid for Chemical Burns

318

(1)

Fisrt Aid for Wounds and Fractures

318

(1)

First Aid for Shock

319

(1)

First Aid for Electric Shock

319

(1)

First Aid for Ingested Poisons

320

(1)

First Aid for Inhaled Poisons

320

(1)

Artificial Respiration

320

(1)

First Aid For Foreign Object in the Eye

321

(2)

Appendix B SALINITY DETERMINATION BY HYDROMETRIC METHOD

323

(8)

Appendix C LOGBOOK FORMS AND USEFUL TABLES APPLICABLE IN ANALYTICAL WORK

331

(20)

Appendix D DOCUMENTATION FORMS FOR QUALITY CONTROL DATA

351

(8)

References

359

(2)

Index

361

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Environmental Sampling and Analysis: Lab Manual

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