Quantitative Organic Microanalysis

Quantitative Organic Microanalysis, Second Edition presents the recommendations of the American Chemical Society group for specification and methods of organic microanalysis.
This book is organized into 23 chapters, and starts with discussions on test samples, blank tests, second type of efficient vibration-absorbing balance table, and microchemical balances. Other general topics covered include the Kjeldahl procedures to determine nitrogen compounds; oxygen flask combustions; determination of fluorine; and microhydrogenation. The final chapters present the modification of the procedure for the determination of oxygen using gravimetry.
This book will be of great value to microanalysts, researchers, and college students who wants to expand their understanding in organic microanalysis.

Preface to Second Edition

Foreword to First Edition

Acknowledgments

1. Introduction

Recommendations, Collaboration, and Standardization

Blank Tests and Corrections

Test Substances

Critical Determinations

Laboratory Report Sheets

Laboratory Set-up

References

2. The Microchemical Balance

Essential Parts

Mounting the Balance

Assembling and Cleaning the Balance

Additional Information

References

3. Weighing on the Microchemical Balance

Determination of Zero Reading and Deflection

Determination of Sensitivity and Precision

Calibration of Weights

Apparatus

Weighing of Samples

Additional Information

References

4. Preparation of Samples for Analysis

Homogeneity of Samples

Apparatus

Determination of Moisture

Additional Information

References

5. Standard Solutions (Microtitration Techniques)

Reagents

Apparatus

Procedures

Additional Information

References

6. Microdetermination of Metals by the Ashing Technique

Reagents

Apparatus

Procedure

Additional Information

References

7. Microdetermination of Nitrogen by the Dumas Method

Reagents

Apparatus

Procedure

Calculation of Results

Additional Information

References

8. Microdetermination of Nitrogen by the Kjeldahl Method

Reagents

Apparatus

Regular Procedure

Procedure for Determination of Nitrogen in Azo and Nitro Compounds, Oximes, Isoxazoles, Hydrazines, and Hydrazones

Procedure for Determination of Nitrogen in Nitrates

Additional Information

References

9. Microdetermination of Carbon and Hydrogen

Reagents

Apparatus

Assembling the Combustion Train

Procedure

Additional Information

References

10. Microdetermination of Sulfur

Carius Combustion

Volumetric Carius Method

Gravimetric Carius Method

Schöniger Combustion

Volumetric Schöniger Method

Pregl Catalytic Combustion

Reagents

Apparatus

Assembly and Gravimetric Procedure

Acidimetric (Direct Neutralization) Procedure

Volumetric Procedure

Additional Information

References

11. Microdetermination of Halogens

Determination of Bromine, Chlorine, and Iodine

Carius Method

Pregl Catalytic Combustion Method

Simultaneous Determination of Chlorine and Bromine

Determination of Fluorine

Reagents

Apparatus

Procedure

Additional Information

References

12. Microdetermination of Phosphorus

Kjeldahl Gravimetric Method

Reagents

Apparatus

Procedure

Carius Gravimetric Method

Reagents

Apparatus

Procedure

Simultaneous Determination of Barium and Phosphorus

References

13. Microdetermination of Arsenic

Carius Volumetric Method

Reagents

Apparatus

Procedure

Carius Gravimetric Method

Reagents

Apparatus

Procedure

References

14. Microdetermination of Oxygen

Gravimetric Method

Reagents

Apparatus

Assembling the Apparatus

Procedure

Volumetric (Iodometric) Method

Reagents

Apparatus

Assembling the Apparatus

Procedure

References

15. Microdetermination of Neutralization Equivalent, Ionic Hydrogen, or Carboxyl Groups

Reagents

Apparatus

Procedure

References

16. Microdetermination of Alkoxyl Groups (Methoxyl and Ethoxyl)

Volumetric (Iodometric) Method

Reagents

Apparatus

Procedure

Gravimetric Method

Reagents

Apparatus

Procedure

References

17. Microdetermination of Acyl Groups (Acetyl and Formyl)

Reagents

Apparatus

Procedure

References

18. Microdeterminations Carried Out on the Van Slyke Manometric Apparatus

Manometric Carbon Determination

Reagents

Apparatus

Procedure

Manometric Determination of Primary Amino Nitrogen in the Aliphatic α-Amino Acids

Reagents

Apparatus

Procedure

Other Determinations Carried out on the Manometric Apparatus

Ampul and Vial Testing with Manometric Apparatus

Manometric Micro-Kjeldahl Determination of Nitrogen

Blood and Urine Analysis

Gas Solubility Studies

Indirect Methods Based on Manometric Combustion of Organic Precipitates

Determination of Phosphorus

Determination of Sulfur

Determination of Magnesium

References

19. Microdetermination of Unsaturation (Double Bonds)—Hydrogen Number

Reagents

Apparatus

Procedure

References

20. Microdetermination of Other Groups

Determination of Alkimide Groups (N-Methyl and N - Ethyl)

Reagents

Apparatus

Procedure

Determination of Hydroxyl Groups

Micromethod

Semimicromethod

References

21. Microdetermination of Molecular Weight

The Rast Method for the Determination of Molecular Weight

Reagents

Apparatus

Procedure

The Signer (Isothermal Distillation) Method for the Determination of Molecular Weight

Reagents

Apparatus

Procedure

Additional Information

References

22. Microdetermination of Some Physical Constants

Microdetermination of Melting Point

Apparatus

Procedure

Microdetermination of Boiling Point

Apparatus

Procedure

Microdetermination of Specific Gravity

Using the Gravitometer

Using Micro Weighing Pipettes, Density-Type (Pycnometers)

Microdetermination of Other Physical Constants

References

23. Calculations

Calculation of Factors

Calculation of Percentages from the Empirical Formula and Vice Versa

References

Author Index

Subject Index