Analytical Methods for Glycerol

Contents

Preface


1. Glycerol 1


1.1 Oxidation Methods .


1.1.1 Bromine


1.1.2 Cerium(IV)


1.1.3 Chloramine T


1.1.4 Chromium(VI)


1.1.5 Copper(III)


1.1.6 Gold(III)


1.1.7 Hypohalite


1.1.8 Iodate


1.1.9 Iodine


1.1.10 Lead(IV)


1.1.11 Manganate


1.1.12 Mercury(II)


1.1.13 Oxygen


1.1.14 Periodate


1.1.15 Permanganate


1.1.16 Silver


1.1.17 Vanadate


1.2 Esterification Methods


1.2.1 Identification of Glycerol


1.2.2 Quantitative Determination


1.3 Ether Formation


1.3.1 Trimethylsilylation


1.3.2 Other Ether Formation Procedures


1.4 Dehydration and Detection Or Determination of the Acrolein Formed


1.4.1 Pungent Odour of Acrolein


1.4.2 Reaction of the C = C Group to Form Epihydrinaldehyde


1.4.3 Aldehyde Reducing Reactions


1.4.4 Reaction With Nitroprusside-Base


1.4.5 Condensation Reactions of the C = 0 Group


1.5 Reaction With Hydriodic Acid Yielding Isopropyl Iodide


1.6 Reaction With Inorganic Cations and Anions


1.6.1 With Copper(II)


1.6.2 With Other Cations


1.6.3 With Borate


1.6.4 With Other Anions


1.7 Purely Physical Methods


1.7.1 Refractive Index


1.7.2 Density, Surface Tension, and Critical Solution Temperature


1.7.3 Viscosity


1.7.4 Infrared Spectrophotometry


1.7.5 Nuclear Magnetic Resonance


1.8 Non-Chromatographic Separation Methods


1.8.1 Solvent Extraction


1.8.2 Distillation


1.9 Chromatographic Methods


1.9.1 Gas Chromatography


1.9.2 Paper Chromatography


1.9.3 Thin Layer Chromatography


1.9.4 Column and Liquid Chromatography


1.9.5 Paper Electrophoresis


1.9.6 Ion Exchange

References


2. Glycerol Compounds: Introduction, and Methods Based On Residual Hydroxyl Groups


2.1 Oxidation With Periodate


2.1.1 Use of Excess Reagent and Detection Or Determination of the Unused Reagent


2.1.2 Isomerisation of Glycerol 2-Monoesters


2.1.3 Detection and Determination of Aldehyde Reaction Products


2.2 Oxidation With Lead(IV)


2.3 Formation of Isopropylidene Derivatives


2.4 Complex Formation With Boron Compounds


2.5 Esterification


2.6 Ether Formation


2.6.1 Trimethylsilylation


2.6.2 Other Ether Formation Reactions


2.7 Infrared Spectrophotometry


2.8 Nuclear Magnetic Resonance


2.9 Other Oxidations


2.10 Thermogravimetry


2.11 Non-Chromatographic Separation Methods


2.11.1 Thermal Diffusion


2.11.2 Urea Complexes


2.11.3 Fractional Distillation and Extraction


2.12 Chromatography of Mixtures of Glycerol Mono-, Diand Tri-Esters Or -Ethers


2.12.1 Thin Layer Chromatography


2.12.2 Paper Chromatography


2.12.3 Column and Liquid Chromatography


2.12.4 Gas Chromatography

References


3. Glycerol Compounds: Methods Based On Release of Glycerol From The Sample


3.1 Hydrolysis


3.1.1 Oxidation with Periodate


3.1.2 Formation of Isopropylidene Groups


3.1.3 Other Oxidations


3.1.4 Dehydration


3.1.5 Esterification


3.1.6 Ether Formation


3.1.7 Reaction With Hydriodic Acid


3.1.8 Infrared Spectrophotometry


3.1.9 Chromatographic Methods


3.2 Aminolysis


3.3 Reduction


3.4 Thermal Cleavage

References


4. Glycerol Compounds: Methods Based On Probable Participation of the Complete Molecules of the Sample


4.1 Nephelometry


4.2 Critical Solution Temperature


4.3 Differential Thermal Analysis


4.4 Mass Spectrometry


4.5 Infrared Spectrophotometry


4.6 Solvent Extraction


4.7 Chromatography


4.7.1 Gas Chromatography


4.7.2 Paper Chromatography


4.7.3 Thin Layer Chromatography


4.7.4 Column Chromatography


4.8 Lipid Reagents


4.8.1 Charring Procedures


4.8.2 Iodine


4.8.3 Iodine-A-Cyclodextrin Or Starch


4.8.4 Molybdo-And Tungsto-Phosphoric Acids


4.8.5 Fluorescent Detecting Agents


4.8.6 Other Dyes and Indicators

References


5. Analysis of Glycerol


5.1 Pharmacopoeia Tests


5.1.1 Chloride Ion


5.1.2 Sulphate Ion


5.1.3 Total (Including Organic) Chlorine


5.1.4 Arsenic


5.1.5 Heavy Metals


5.1.6 Acidity, Alkalinity


5.1.7 Reducing Properties, Materials, Impurities; Glucose


5.1.8 Ammonium Compounds


5.1.9 Sugars


5.1.10 Esters


5.1.11 Behaviour Towards Sulphuric Acid


5.1.12 Sulphate Ash


5.1.13 Oxalate


5.1.14 Calcium, Magnesium, Barium Ions


5.1.15 Oxidizing Substances


5.1.16 Test For Glycerol Itself


5.2 Determination of Water In Glycerol


5.2.1 Chemical Methods


5.2.2 Purely Physical Methods


5.2.3 Separation Techniques


5.3 Assay of Glycerol In Pharmacopoeias

References


6. The Enzymic Determination of Glycerol


6.1 Basic Reactions..


6.1.1 The GK-GPDH Method


6.1.2 The GDH Method


6.1.3 The GK-GDH Method


6.1.4 The GK-PK-LDH Method


6.1.5 The GK-GPDH-TIM-GAPDH Method


6.1.6 Differences Between The Various Methods


6.1.7 The Enzymic-Radiometric Method


6.2 Modes of Determination of NADH


6.3 Method of Calculation


6.4 Nature and Origin of the Samples


6.5 Preliminary Treatment of the Samples


6.5.1 Anticoagulation Treatment


6.5.2 Deproteinization


6.5.3 Liberation of Bound Glycerol


6.6 Interfering Substances


6.6.1 In The Enzymes


6.6.2 In The Substrate


6.7 Chronological Literature


6.7.1 The GK-GPDH Method


6.7.2 The GDH Method


6.7.3 The GK-GDH Method


6.7.4 The GK-PK-LDH Method


6.7.5 The GK-GPDH-TIM-GAPDH Method


6.7.6 The GPDH Method For GP


6.7.7 The Enzymic-Radiometric Method

References

Index