2017_Book_FoodAnalysisLaboratoryManual.pdf - Food Science Text Series S Suzanne Nielsen Food Analysis Laboratory Manual Third Edition Food Science Text

2017_Book_FoodAnalysisLaboratoryManual.pdf - Food Science...

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Unformatted text preview: Food Science Text Series S. Suzanne Nielsen Food Analysis Laboratory Manual Third Edition Food Science Text Series Third Edition For other titles published in this series, go to Series editor: Dennis R. Heldman Heldman Associates Mason, Ohio, USA The Food Science Text Series provides faculty with the leading teaching tools. The Editorial Board has outlined the most appropriate and complete content for each food science course in a typical food science program and has identified textbooks of the highest quality, written by the leading food science educators. Series Editor Dennis R. Heldman, Professor, Department of Food, Agricultural, and Biological Engineering, The Ohio State University. Editorial Board; John Coupland, Professor of Food Science, Department of Food Science, Penn State University, David A. Golden, Ph.D., Professor of Food Microbiology, Department of Food Science and Technology, University of Tennessee, Mario Ferruzzi, Professor, Food, Bioprocessing and Nutrition Sciences, North Carolina State University, Richard W. Hartel, Professor of Food Engineering, Department of Food Science, University of Wisconsin, Joseph H. Hotchkiss, Professor and Director of the School of Packaging and Center for Packaging Innovation and Sustainability, Michigan State University, S. Suzanne Nielsen, Professor, Department of Food Science, Purdue University, Juan L. Silva, Professor, Department of Food Science, Nutrition and Health Promotion, Mississippi State University, Martin Wiedmann, Professor, Department of Food Science, Cornell University, Kit Keith L. Yam, Professor of Food Science, Department of Food Science, Rutgers University Food Analysis Laboratory Manual Third Edition edited by S. Suzanne Nielsen Purdue University West Lafayette, IN, USA S. Suzanne Nielsen Department of Food Science Purdue University West Lafayette Indiana USA ISSN 1572-0330 ISSN 2214-7799 (electronic) Food Science Text Series ISBN 978-3-319-44125-2 ISBN 978-3-319-44127-6 (eBook) DOI 10.1007/978-3-319-44127-6 Library of Congress Control Number: 2017942968 © Springer International Publishing 2017, corrected publication 2019 This work is subject to copyright. All rights are reserved by the Publisher, whether the whole or part of the material is concerned, specifically the rights of translation, reprinting, reuse of illustrations, recitation, broadcasting, reproduction on microfilms or in any other physical way, and transmission or information storage and retrieval, electronic adaptation, computer software, or by similar or dissimilar methodology now known or hereafter developed. The use of general descriptive names, registered names, trademarks, service marks, etc. in this publication does not imply, even in the absence of a specific statement, that such names are exempt from the relevant protective laws and regulations and therefore free for general use. The publisher, the authors and the editors are safe to assume that the advice and information in this book are believed to be true and accurate at the date of publication. Neither the publisher nor the authors or the editors give a warranty, express or implied, with respect to the material contained herein or for any errors or omissions that may have been made. The publisher remains neutral with regard to jurisdictional claims in published maps and institutional affiliations. Printed on acid-free paper This Springer imprint is published by Springer Nature The registered company is Springer International Publishing AG The registered company address is: Gewerbestrasse 11, 6330 Cham, Switzerland Preface and Acknowledgments This laboratory manual was written to accompany the textbook, Food Analysis, fifth edition. The laboratory exercises are tied closely to the text and cover 21 of the 35 chapters in the textbook. Compared to the second edition of this laboratory manual, this third edition contains four introductory chapters with basic information that compliments both the textbook chapters and the laboratory exercises (as described below). Three of the introductory chapters include example problems and their solutions, plus additional practice problems at the end of the chapter (with answers at the end of the laboratory manual). This third edition also contains three new laboratory exercises, and previous experiments have been updated and corrected as appropriate. Most of the laboratory exercises include the following: background, reading assignment, objective, principle of method, chemicals (with CAS number and hazards), reagents, precautions and waste disposal, supplies, equipment, procedure, data and calculations, questions, and resource materials. Instructors using these laboratory exercises should note the following: 1. Use of Introductory Chapters: • Chap. 1, “Laboratory Standard Operating Procedures” – recommended for students prior to starting any food analysis laboratory exercises • Chap. 2, “Preparation of Reagents and Buffers” – includes definition of units of concentrations, to assist in making chemical solutions • Chap. 3, “Dilution and Concentration Calculations” – relevant for calculations in many laboratory exercises • Chap. 4, “Use of Statistics in Food Analysis” – relevant to data analysis 2. Order of Laboratory Exercises: The order of laboratory exercises has been changed to be fairly consistent with the reordering of chapters in the textbook, Food Analysis, fifth edition (i.e., chromatography and spectroscopy near the front of the book). However, each laboratory exercise stands alone, so they can be covered in any order. 3. Customizing Laboratory Procedures: It is recognized that the time and equipment avail- able for teaching food analysis laboratory sessions vary considerably between schools, as do student numbers and their level in school. Therefore, instructors may need to modify the laboratory procedures (e.g., number of samples analyzed, replicates) to fit their needs and situation. Some experiments include numerous parts/methods, and it is not assumed that an instructor uses all parts of the experiment as written. It may be logical to have students work in pairs to make things go faster. Also, it may be logical to have some students do one part of the experiment/one type of sample and other students to another part of the experiment/type of sample. 4. Use of Chemicals: The information on hazards and precautions in the use of the chemicals for each experiment is not comprehensive but should make students and a laboratory assistant aware of major concerns in handling and disposing of the chemicals. 5. Reagent Preparation: It is recommended in the text of the experiments that a laboratory assistant prepare many of the reagents, because of the time limitations for students in a laboratory session. The lists of supplies and equipment for experiments do not necessarily include those needed by the laboratory assistant in preparing reagents for the laboratory session. 6. Data and Calculations: The laboratory exercises provide details on recording data and doing calculations. In requesting laboratory reports from students, instructors will need to specify if they require just sample calculations or all calculations. Even though this is the third edition of this laboratory manual, there are sure to be inadvertent omissions and mistakes. I will very much appreciate receiving suggestions for revisions from instructors, including input from lab assistants and students. I maintain a website with additional teaching materials related to both the Food Analysis textbook and laboratory manual. Instructors are welcome to contact me for access to this website. To compliment the laboratory manual, the website contains more detailed versions of select introductory chapters and Excel sheets related to numerous laboratory exercises. v vi I am grateful to the food analysis instructors identified in the text who provided complete laboratory experiments or the materials to develop the experiments. For this edition, I especially want to thank the authors of the new introductory chapters who used their experience from teaching food analysis to develop what I hope will be very valuable chapters for students and instructors alike. The input I received from other food analysis instructors, their students, and mine who reviewed these new introductory chapters was extremely valuable and very Preface and Acknowledgments much appreciated. Special thanks go to Baraem (Pam) Ismail and Andrew Neilson for their input and major contributions toward this edition of the laboratory manual. My last acknowledgment goes to my former graduate students, with thanks for their help in working out and testing all experimental procedures written for the initial edition of the laboratory manual. West Lafayette, IN, USA The original version of this book was revised. The correction to this book can be found at DOI 10.1007/978-3-319-44127-6_32 S. Suzanne Nielsen Contents Preface and Acknowledgments Part 1 1 2 3 4 v 4.6 4.7 4.8 4.9 4.10 Introductory Chapters Laboratory Standard Operating Procedures 1.1 Introduction 5 1.2 Precision and Accuracy 5 1.3 Balances 6 1.4 Mechanical Pipettes 7 1.5 Glassware 9 1.6 Reagents 16 1.7 Data Handling and Reporting 18 1.8 Basic Laboratory Safety 19 Preparation of Reagents and Buffers 21 2.1 Preparation of Reagents of Specified Concentrations 22 2.2 Use of Titration to Determine Concentration of Analytes 24 2.3 Preparation of Buffers 25 2.4 Notes on Buffers 30 2.5 Practice Problems 31 Dilutions and Concentrations 33 3.1 Introduction 34 3.2 Reasons for Dilutions and Concentrations 34 3.3 Using Volumetric Glassware to Perform Dilutions and Concentrations 34 3.4 Calculations for Dilutions and Concentrations 34 3.5 Special Cases 40 3.6 Standard Curves 41 3.7 Unit Conversions 44 3.8 Avoiding Common Errors 45 3.9 Practice Problems 46 Statistics for Food Analysis 49 4.1 Introduction 50 4.2 Population Distributions 50 4.3 Z-Scores 51 4.4 Sample Distributions 54 4.5 Confidence Intervals 55 3 Part 2 t-Scores 58 t-Tests 59 Practical Considerations Practice Problems 62 Terms and Symbols 62 61 Laboratory Exercises 5 Nutrition Labeling Using a Computer Program 65 5.1 Introduction 67 5.2 Preparing Nutrition Labels for Sample Yogurt Formulas 67 5.3 Adding New Ingredients to a Formula and Determining How They Influence the Nutrition Label 68 5.4 An Example of Reverse Engineering in Product Development 69 5.5 Questions 70 6 Accuracy and Precision Assessment 6.1 Introduction 72 6.2 Procedure 73 6.3 Data and Calculations 74 6.4 Questions 74 7 High-Performance Liquid Chromatography 77 7.1 Introduction 79 7.2 Determination of Caffeine in Beverages By HPLC 79 7.3 Solid-Phase Extraction and HPLC Analysis of Anthocyanidins from Fruits and Vegetables 81 8 Gas Chromatography 87 8.1 Introduction 89 8.2 Determination of Methanol and Higher Alcohols in Wine by Gas Chromatography 89 8.3 Preparation of Fatty Acid Methyl Esters (FAMEs) and Determination of Fatty Acid Profile of Oils by Gas Chromatography 91 71 vii viii 9 Contents Mass Spectrometry with High-Performance Liquid Chromatography 97 9.1 Introduction 98 9.2 Procedure 100 9.3 Data and Calculations 101 9.4 Questions 102 9.5 Case Study 102 10 Moisture Content Determination 105 10.1 Introduction 107 10.2 Forced Draft Oven 107 10.3 Vacuum Oven 109 10.4 Microwave Drying Oven 110 10.5 Rapid Moisture Analyzer 111 10.6 Toluene Distillation 111 10.7 Karl Fischer Method 112 10.8 Near-Infrared Analyzer 114 10.9 Questions 114 11 Ash Content Determination 117 11.1 Introduction 118 11.2 Procedure 118 11.3 Data and Calculations 118 11.4 Questions 119 12 Fat Content Determination 121 12.1 Introduction 123 12.2 Soxhlet Method 123 12.3 Goldfish Method 125 12.4 Mojonnier Method 125 12.5 Babcock Method 127 13 Protein Nitrogen Determination 131 13.1 Introduction 132 13.2 Kjeldahl Nitrogen Method 132 13.3 Nitrogen Combustion Method 135 14 Total Carbohydrate by Phenol-Sulfuric Acid Method 137 14.1 Introduction 138 14.2 Procedure 139 14.3 Data and Calculations 140 14.4 Questions 141 15 Vitamin C Determination by Indophenol Method 143 15.1 Introduction 144 15.2 Procedure 145 15.3 Data and Calculations 145 15.4 Questions 146 16 Water Hardness Testing by Complexometric Determination of Calcium 147 16.1 Introduction 149 16.2 EDTA Titrimetric Method for Testing Hardness of Water 149 16.3 Test Strips for Water Hardness 151 17 Phosphorus Determination by Murphy-Riley Method 153 17.1 Introduction 154 17.2 Procedure 155 17.3 Data and Calculations 155 17.4 Questions 155 18 Iron Determination by Ferrozine Method 18.1 Introduction 158 18.2 Procedure 158 18.3 Data and Calculations 159 18.4 Question 159 157 19 Sodium Determination Using Ion-Selective Electrodes, Mohr Titration, and Test Strips 161 19.1 Introduction 163 19.2 Ion-Selective Electrodes 163 19.3 Mohr Titration 165 19.4 Quantab® Test Strips 167 19.5 Summary of Results 169 19.6 Questions 170 20 Sodium and Potassium Determinations by Atomic Absorption Spectroscopy and Inductively Coupled Plasma-Optical Emission Spectroscopy 171 20.1 Introduction 173 20.2 Procedure 174 20.3 Data and Calculations 176 20.4 Questions 177 21 Standard Solutions and Titratable Acidity 179 21.1 Introduction 180 21.2 Preparation and Standardization of Base and Acid Solutions 180 21.3 Titratable Acidity and pH 182 22 Fat Characterization 185 22.1 Introduction 187 22.2 Saponification Value 187 22.3 Iodine Value 188 22.4 Free Fatty Acid Value 190 22.5 Peroxide Value 191 22.6 Thin-Layer Chromatography Separation of Simple Lipids 193 ix Contents 23 Proteins: Extraction, Quantitation, and Electrophoresis 195 23.1 Introduction 196 23.2 Reagents 197 23.3 Supplies 198 23.4 Procedure 198 23.5 Data and Calculations 200 23.6 Questions 200 27 CIE Color Specifications Calculated from Reflectance or Transmittance Spectra 27.1 Introduction 221 27.2 Procedure 222 27.3 Questions 224 219 28 Extraneous Matter Examination 225 28.1 Introduction 227 28.2 Extraneous Matter in Soft Cheese 227 28.3 Extraneous Matter in Jam 228 28.4 Extraneous Matter in Infant Food 229 28.5 Extraneous Matter in Potato Chips 229 28.6 Extraneous Matter in Citrus Juice 230 28.7 Questions 230 24 Glucose Determination by Enzyme Analysis 203 24.1 Introduction 204 24.2 Procedure 205 24.3 Data and Calculations 205 24.4 Questions 205 Part 3 Answers to Practice Problems 25 Gliadin Detection by Immunoassay 25.1 Introduction 208 25.2 Procedure 209 25.3 Data and Calculations 210 25.4 Questions 211 207 26 Viscosity Measurements of Fluid Food Products 213 26.1 Introduction 214 26.2 Procedure 214 26.3 Data 216 26.4 Calculations 216 26.5 Questions 217 29 Answers to Practice Problems in Chap. 2, Preparation of Reagents and Buffers 233 30 Answers to Practice Problems in Chap. 3, Dilutions and Concentrations 239 31 Answers to Practice Problems in Chap. 4, Use of Statistics in Food Analysis 247 Correction to: Food Analysis Laboratory Manual C1 Contributors Charles E. Carpenter Department of Nutrition, Dietetics and Food Sciences, Utah State University, Logan, UT, USA Oscar A. Pike Department of Nutrition, Dietetics, and Food Science, Brigham Young University, Provo, UT, USA Young-Hee Cho Department of Food Science, Purdue University, West Lafayette, IN, USA Michael C. Qian Department of Food Science and Technology, Oregon State University, Corvallis, OR, USA M. Monica Giusti Department of Food Science and Technology, The Ohio State University, Columbus, OH, USA Y.H. Peggy Hsieh Department of Nutrition, Food and Exercise Sciences, Florida State University, Tallahassee, FL, USA Baraem P. Ismail Department of Food Science and Nutrition, University of Minnesota, St. Paul, MN, USA Helen S. Joyner School of Food Science, University of Idaho, Moscow, ID, USA Dennis A. Lonergan The Vista Institute, Eden Prairie, MN, USA Lloyd E. Metzger Department of Dairy Science, University of South Dakota, Brookings, SD, USA Andrew P. Neilson Department of Food Science and Technology, Virginia Polytechnic Institute and State University, Blacksburg, VA, USA S. Suzanne Nielsen Department of Food Science, Purdue University, West Lafayette, IN, USA Sean F. O’Keefe Department of Food Science and Technology, Virginia Tech, Blacksburg, VA, USA Qinchun Rao Department of Nutrition, Food and Exercise Sciences, Florida State University, Tallahassee, FL, USA Ann M. Roland Owl Software, Columbia, MO, USA Daniel E. Smith Department of Food Science and Technology, Oregon State University, Corvallis, OR, USA Denise M. Smith School of Food Science, Washington State University, Pullman, WA, USA Stephen T. Talcott Department of Nutrition and Food Science, Texas A&M University, College Station, TX, USA Catrin Tyl Department of Food Science and Nutrition, University of Minnesota, St. Paul, MN, USA Robert E. Ward Department of Nutrition, Dietetics and Food Sciences, Utah State University, Logan, UT, USA Ronald E. Wrolstad Department of Food Science and Technology, Oregon State University, Corvallis, OR, USA xi 1 part Introductory Chapters 1 chapter Laboratory Standard Operating Procedures Andrew P. Neilson (*) Department of Food Science and Technology, Virginia Polytechnic Institute and State University, Blacksburg, VA, USA e-mail: [email protected] Dennis A. Lonergan The Vista Institute, Eden Prairie, MN, USA e-mail: [email protected] S. Suzanne Nielsen Department of Food Science, Purdue University, West Lafayette, IN, USA e-mail: [email protected] S.S. Nielsen, Food Analysis Laboratory Manual, Food Science Text Series, DOI 10.1007/978-3-319-44127-6_1, © Springer International Publishing 2017 3 1.1 Introduction 1.2 Precision and Accuracy 1.3 Balances 1.3.1 Types of Balances 1.3.2 Choice of Balance 1.3.3 Use of Top Loading Balances 1.3.4 Use of Analytical Balances 1.3.5 Additional Information 1.4 Mechanical Pipettes 1.4.1 Operation 1.4.2 Pre-rinsing 1.4.3 Pipetting Solutions of Varying Density or Viscosity 1.4.4 Performance Specifications 1.4.5 Selecting the Correct Pipette 1.5 Glassware 1.5.1 Types of Glassware/Plasticware 1.5.2 Choosing Glassware/Plasticware 1.5.3 Volumetric Glassware 1.5.4 Using Volumetric Glassware to Perform Dilutions and Concentrations 1.5.5 Conventions and Terminology 1.5.6 Burets 1.5.7 Cleaning of Glass and Porcelain 1.6 Reagents 1.6.1 Acids 1.6.2 Distilled Water 1.6.3 Water Purity 1.6.4 Carbon Dioxide-Free Water 1.6.5 Preparing Solutions and Reagents 1.7 Data Handling and Reporting 1.7.1 Significant Figures 1.7.2 Rounding Off Numbers 1.7.3 Rounding Off Single Arithmetic Operations 1.7.4 Rounding Off the Results of a Series of Arithmetic Operations 1.8 Basic Laboratory Safety 1.8.1 Safety Data Sheets 1.8.2 Hazardous Chemicals 1.8.3 Personal Protective Equipment and Safety Equipment 1.8.4 Eating, Drinking, Etc. 1.8.5 Miscellaneous Information Chapter 1 • Laboratory Standard Operating Procedures 1.1 INTRODUCTION This chapter is designed to cover “standard operating procedures” (SOPs), or best practices, for a general food analysis laboratory. The topics covered in this chapter include balances, mechanical pipettes, glassware, reagents, precision and accuracy, data handling, data reporting, and safety. These procedures apply to all the laboratory experiments in this manual, and therefore a thorough review of general procedures will be invaluable for successful completion of these laboratory exercises. This manual covers many of the basic skills and information that are necessary for one to be a good analytical food chemist. Much of this material is the type that one “picks up” from experience. Nothing can replace actual lab experience as a learning tool, but hopefully this manual will help students learn proper lab techniques early rather than having to correct improper habits later. When one reads this manual, your reaction may be “is all of this attention to detail necessary?” Admittedly, the answer is “not always.” This brings to mind an old Irish proverb that “the best person for a job is the one that knows what to ignore.” There is much tru...
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