Qualitative Organic Microanalysis: Cognition and Recognition of Carbon Compounds

ISBN-13: 9783709158296 / Angielski / Miękka / 2012 / 536 str.

Jr. Frank Schneider

Opis

The most important task of the analytical chemist, aside from the acquisition of experimental data, is the coordination and interpretation of such data in terms of the qualitative and quantitative composition of the test substance. As in the old tale of the blind men and the elephant, a single observation or test, not considered in conjunction with others, may lead to entirely erroneous conclusions. On the other hand, mere in crease in the number of such tests, without regard to their need or to their relationship to each other, also may not suffice for drawing the correct inferences from the experimental evidence. The deductive reasoning which is usually associated with the analy tical chemist finds its greatest opportunity for application in the problems of cognition and recognition of carbon compounds. Since a rigid scheme of procedure tends to produce a corresponding rigidity of thought, the intent of the present book is to outline approaches which will minimize the chances of misinterpretation without restricting the analytical chemist in his choice of tests. The selection of subsequent tests or reactions should be governed by the results of the preceding ones rather than by an arbi trary list. The relationships of the various approaches (and the information derived from each) to the composition and constitution of the test sub stance are brought out in the discussion with the hope that they may serve as guide lines for such selection."

Spis treści

I Fundamental Techniques and Preparation of Sample.- I. Fundamental Apparatus and Operations.- Capillaries.- Microscope Slides.- Microcones.- Spot Plates.- Reflex Tubes.- Microbeakers.- Determination of Weight.- The Microscope.- Reagents.- II. Preparation of the Sample.- Tests for Purity.- Separation of Minor Components and Impurities.- Mechanical Separation.- Distillation.- Fractional Distillation.- Recrystallization.- Zone Melting.- Extraction.- Sublimation.- Drying and Removal of Solvent.- Separation of Mixtures.- Heterogeneous Mixtures.- Homogeneous Mixtures.- II Preliminary Examination.- III. Elementary Analysis.- Carbon.- Water.- Oxygen.- Other Elements.- Decomposition of the Substance.- Nitrogen.- Halogens.- Other Tests for Halogens.- Sulfur.- Phosphorus.- Arsenic.- Silicon.- Metals.- Quantitative Elementary Analysis.- IV. Determination of Physical Constants.- Melting Point.- Boiling Point.- Density.- Refractive Index.- Solids.- Liquids.- Crystallographic Properties.- Crystal Optical Properties.- Molecular Weight Determination.- Specific Rotation.- V. Solubility.- Solvents.- Determination of Solubility.- Application of Solubility Data.- III Systematic Analysis.- VI. Compounds of Order I.- Aldehydes.- Generic Test.- Classification Tests for Aldehydes.- Derivatives of Aldehydes.- Degradative Procedures.- Chemical Separation of Aldehydes.- Quantitative Determination of Aldehydes.- Carbohydrates.- Generic Test.- Supplementary Tests.- Sectional Tests.- Classification Tests for Carbohydrates.- Crystallization Test.- Degradative Procedures.- Chemical Separation of Carbohydrates.- Quantitative Analysis of Carbohydrates.- Acids.- Generic Test.- Divisional Test.- Sectional Tests.- Classification Tests.- Derivatives of Acids.- Degradative Procedures for Acids.- Chemical Separation of Acids.- Quantitative Analysis of Acids.- Phenols.- Generic Tests.- Classification Tests for Phenols.- Derivatives of Phenols.- Degradative Procedures.- Chemical Separation of Phenols.- Quantitative Determination of Phenols.- Esters.- Generic Test.- Derivatives of Esters.- Degradative Procedures.- Chemical Separation of Esters.- Quantitative Determination of Esters.- Acid Anhydrides and Lactones.- Titration of Anhydrides and Lactones.- 2,4-Dichloroanilides of Anhydrides.- Degradative Procedures.- Chemical Separation.- Quantitative Determination.- Ketones.- Generic Test.- Derivatives of Ketones.- Degradative Procedures.- Chemical Separation of Ketones.- Quantitative Determination of Ketones.- Alcohols.- Generic Test.- Classification Test for Alcohols.- Derivatives of Alcohols.- Degradative Procedures for Alcohols.- Chemical Separation of Alcohols.- Quantitative Determination of Alcohols.- Hydrocarbons and Ethers.- Sectional Tests.- Classification Tests.- Derivatives of Hydrocarbons and Ethers.- Degradative Procedures for Hydrocarbons and Ethers.- Chemical Separation of Hydrocarbons and Ethers.- Quantitative Determination of Hydrocarbons.- Ethers.- VII. Compounds of Order II.- Genus 1. Acidic Species.- Classification Reactions.- Derivatives of Amino Acids.- Degradative Procedures for Acidic Nitrogen Compounds.- Chemical Separation of Acidic Nitrogen Compounds.- Genus 2. Basic Species.- Classification Reactions.- Derivatives of Amines.- Degradative Procedures.- Chemical Separation.- Quantitative Determination.- Genus 3. Neutral Species.- Classification Tests.- Derivatives of Neutral Species.- Degradative Procedures for Neutral Species.- Quantitative Determination of Neutral Species.- VIII. Compounds of the Higher Orders.- Halogen Compounds.- Classification Test.- Derivatives of Halogen Compounds.- Degradative Procedures for Halogen Compounds.- Chemical Separation of Halogen Compounds.- Quantitative Determination of Halogen Compounds.- Sulfur Compounds.- Classification Test.- Derivatives of Sulfur Compounds.- Degradative Procedures for Sulfur Compounds.- Chemical Separation of Sulfur Compounds.- Quantitative Determination of Sulfur Compounds.- Literature Cited.- Tables of Physical Constants of Compounds and Derivatives Classified by Orders, Genera, Divisions, and Sections.- Arrangement of Tables and Data.- Notes on the Use of the Tables.- Table 1–1-A. Aldehydes, Solid.- Table 1–1-B. Aldehydes, Liquid.- Table 1–2-A. Carbohydrates.- Table 1–3-A. Acids, Solid.- Table 1–3-B. Acids, Liquid.- Table 1–4-A. Phenols, Solid.- Table 1–4-B. Phenols, Liquid.- Table 1–5-A. Esters, Solid.- Table 1–5-B. Esters, Liquid.- Table 1–6-A. Anhydrides, Solid.- Table 1–6-B. Anhydrides, Liquid.- Table 1–7-A. Ketones, Solid.- Table 1–7-B. Ketones, Liquid.- Table 1–8-A. Alcohols, Solid.- Table 1–8-B. Alcohols, Liquid.- Table 1–9-A-1. Hydrocarbons, Solid, Non-Aromatic.- Table 1–9-A-2. Hydrocarbons, Solid, Aromatic.- Table 1–9-A-3. Ethers, Solid.- Table 1–9-B-l. Hydrocarbons, Liquid, Aromatic.- Table 1–9-B-2. Ethers, Liquid.- Table 1–9-B-3. Hydrocarbons, Liquid. Alkynes, Terpenes, etc.- Table 1–9-B-4. Hydrocarbons, Liquid. Alkenes.- Table 1–9-B-5. Hydrocarbons, Liquid. Alkanes.- Table 2–1–1. Acid Nitrogen Compounds. Amino Acids.- Table 2–1–2. Acid Nitrogen Compounds. Other Acids and Anhydrides.- Table 2–1–3. Acid Nitrogen Compounds. Nitrophenols.- Table 2–1–4. Acid Nitrogen Compounds, Azophenols.- Table 2–1–5. Acid Nitrogen Compounds. Other Nitrogen Phenols.- Table 2–2–1. Basic Nitrogen Compounds. Primary and Secondary.- Table 2–2–2. Basic Nitrogen Compounds. Primary and Secondary Amines. Liquid.- Table 2–2–3. Basic Nitrogen Compounds. Tertiary Amines, Solid.- Table 2–2–4. Basic Nitrogen Compounds. Tertiary Amines, Liquid.- Table 2–2–5. Basic Nitrogen Compounds. Aminophenols.- Table 2–3–1. Neutral Nitrogen Compounds. Aldehydes.- Table 2–3–2. Neutral Nitrogen Compounds. Carbohydrates.- Table 2–3–3. Neutral Nitrogen Compounds. Nitriles, Solid.- Table 2–3–4. Neutral Nitrogen Compounds. Nitriles, Liquid.- Table 2–3–5. Neutral Nitrogen Compounds. Esters.- Table 2–3–6. Neutral Nitrogen Compounds. Ketones.- Table 2–3–7. Neutral Nitrogen Compounds. Quinones.- Table 2–3–8. Neutral Nitrogen Compounds. Alcohols.- Table 2–3–9. Neutral Nitrogen Compounds. Ethers.- Table 2–3–10. Neutral Nitrogen Compounds. Nitrohydrocarbons, Solid.- Table 2–3–11. Neutral Nitrogen Compounds. Nitrohydrocarbons, Liquid.- Table 2–3–12. Neutral Nitrogen Compounds. Miscellaneous.- Table 3–1-A. Chlorine Compounds. Aldehydes, Solid.- Table 3–1-B. Chlorine Compounds. Aldehydes, Liquid.- Table 3–2. Chlorine Compounds. Acids and Anhydrides.- Table 3–3. Chlorine Compounds. Acyl Chlorides.- Table 3–4. Chlorine Compounds. Phenols.- Table 3–5. Chlorine Compounds. Esters.- Table 3–6. Chlorine Compounds. Ketones.- Table 3–7. Chlorine Compounds. Alcohols.- Table 3–8. Chlorine Compounds. Ethers.- Table 3–9-A. Chlorine Compounds. Hydrocarbons, Solid.- Table 3–9-B. Chlorine Compounds. Hydrocarbons, Liquid.- Table 4–1. Bromine Compounds. Aldehydes.- Table 4–2. Bromine Compounds. Acids and Anhydrides.- Table 4–3. Bromine Compounds. Acyl Bromides.- Table 4–4. Bromine Compounds. Phenols.- Table 4–5. Bromine Compounds. Esters.- Table 4–6. Bromine Compounds. Ketones.- Table 4–7. Bromine Compounds. Alcohols.- Table 4–8. Bromine Compounds. Ethers.- Table 4–9. Bromine Compounds. Hydrocarbons.- Table 5–1. Iodine Compounds. Aldehydes and Ketones.- Table 5–2. Iodine Compounds. Acids and Anhydrides.- Table 5–3. Iodine Compounds. Acyl Iodides.- Table 5–4. Iodine Compounds. Phenols.- Table 5–5. Iodine Compounds. Ethers.- Table 5–6. Iodine Compounds. Hydrocarbons.- Table 6–1. Fluorine Compounds. Aldehydes and Ketones.- Table 6–2. Fluorine Compounds. Acids and Anhydrides.- Table 6–3. Fluorine Compounds. Acyl Fluorides.- Table 6–4. Fluorine Compounds. Esters.- Table 6–5. Fluorine Compounds. Alcohols.- Table 6–6. Fluorine Compounds. Ethers.- Table 6–7. Fluorine Compounds. Hydrocarbons.- Table 7–1. Sulfur Compounds. Aldehydes and Ketones.- Table 7–2. Sulfur Compounds. Carboxylic Acids.- Table 7–3. Sulfur Compounds. Thiols and Thiophenols.- Table 7–4. Sulfur Compounds. Sulfides and Disulfides.- Table 7–5. Sulfur Compounds. Cyclic Thioethers.- Table 7–6. Sulfur Compounds. Esters.- Table 8–1. Silicon Compounds. Silicates.- Table 8–2. Silicon Compounds. Alkoxy Silanes.- Table 8–3. Silicon Compounds. Alkoxy Siloxanes.- Table 8–4. Silicon Compounds. Silanols.- Table 8–5. Silicon Compounds. Silanes.- Table 9–1. Higher Orders. Acids.- Table 9–2. Higher Orders. Phenols.- Table 9–3. Higher Orders. Amino Compounds.- Table 9–4. Higher Orders. Acyl Halides.- Table 9–5. Higher Orders. Halides and Nitro Compounds.- Table 9–6. Higher Orders. Sulfonamides.- Table 9–7. Higher Orders. Nitriles.- Table 9–8. Higher Orders. Chlorosilanes.- Table 9–9. Higher Orders. Miscellaneous.

O autorze

Prof. Dr. med. Dr. rer. soc. Frank Schneider, Jahrgang 1958, war Präsident der Deutschen Gesellschaft für Psychiatrie, Psychotherapie und Nervenheilkunde (DGPPN) und arbeitet als Direktor der Klinik für Psychiatrie, Psychotherapie und Psychosomatik am Universitätsklinikum Aachen.