Identification of Materials : Via Physical Properties Chemical Tests and Microscopy

This book has been written for the practicing chemist whose occasional task may be qualitative analysis. It deals with the investigation of things as they are without any limitations to the scope. It emphasizes the identification of materials - inorganic, organic, organized (biological), common, rare, described or not described in the accessible literatur- as they actually occur in nature and industry, or are met in the investigation of mishaps and crime. The description of techniques - macro to submicro - and the practice exercises have been included since the teaching of these arts is rarely a part of academic curricula and it happens with increasing frequency that chemists have to acquire them "on the job". In the systematic procedure given, emphasis is placed upon the investiga­ tion of minute specimens and upon acute reasoning that continuously weighs all accumulating evi9.ence. The work begins with the consideration of the history of the material under investigation. Especially when specks of all organic substance shall be identified, it should be realized that the discovery of the source - and consequently of the possibilities involve- may be the most valuable clue to an efficient solution of the problem.

The Task of Qualitative Analysis.- Principles and Definitions.- Specificity and Sensitivity.- The Method of Qualitative Analysis.- The Minimum Size of the Sample for Chemical Analysis.- Properties Affected by the Size of the System.- Apparatus, Technique, and Scale of Work.- Observation of Properties.- Selection of Procedure.- I: Technique of Observation and Manipulation.- Use of Optical Aids.- The Microscope.- Experiment 1. Inspecting and Cleaning the Microscope.- Illumination of the Specimen.- Experiment 2. Illumination of Microscopical Specimens.- Experiment 3. Calibration of Eyepiece Micrometer; Working Distances and Fields of Vision.- The Immersion Method for the Determination of Refraction.- Experiment 4. Phenomena Caused by Differences in Refraction.- Observation of Schlieren.- Experiment 5. Visual Observation of Schlieren.- Use of Polarized Light.- Experiment 6. Testing and Adjusting a Polarizing Microscope.- Experiment 7. Isotropic and Anisotropie Substances in Polarized Light.- Experiment 8. Determination of Vibration Directions in Relation to Profile.- Experiment 9. Use of Compensators.- Experiment 10. On the Determination of the Refractive Indices of Anisotropie Materials.- Experiment 11. Observation of Pleochroism.- Experiment 12. Observation of Axial Figures.- Experiment 13. Transition Phenomena in Polarized Light.- Experiment 14. Preserving Microscopical Preparations.- Technique of Experimentation and Observation.- Basic Rules.- Work on the Gram Scale.- Experiment 15. Phenomena Observed Upon Heating in an Inert Atmosphere.- Experiment 16. Phenomena Observed Upon Heating in a Stream of Air.- Experiment 17. Heating Upon the Charcoal Block.- Experiment 18. Performance of Flame Tests.- Work on the Centigram Scale.- Experiment 19. Preparation of Capillaries, Capillary Pipets, and Microburners.- Experiment 20. Emich’s Method of Fractional Distillation.- Experiment 21. Emich’s Method for the Determination of Boiling Points.- Work on the Milligram Scale.- Experiment 22. Calibration of Capillary Pipets and Centrifugal Pipets.- Experiment 23. Preparation and Calibration of Platinum Loops and Hooks.- Techniques of the Submilligram Scale.- Spot Tests.- Experiment 24. Test for Mercuric Mercury and Lead.- Experiment 25. Chromate Test for Silver.- Experiment 26. Tests for Bismuth and Antimony.- Experiment 27. Test for Copper, Nickel, and Cobalt.- Experiment 28. Test for Cadmium.- Experiment 29. Precipitation of Silver Arsenate.- Experiment 30. Molybdenum Blue Test for Tin.- Slide Tests.- Experiment 31. Silver Dichromate.- Experiment 32. Recrystallization of Silver Chloride.- Experiment 33. Lead Iodide.- Experiment 34. Potassium-Lead-Copper Nitrite.- Experiment 35. Cesium Iodobismuthite and Cesium Iodoantimonite.- Experiment 36. Bismuth Cobalticyanide Pentahydrate.- Experiment 37. The Mercurithiocyanates of Copper, Zinc, Cadmium, and Cobalt.- Experiment 38. Test for Cadmium with Brucine and Bromide.- Experiment 39. Test for Mercury with Zinc, Copper, and Thiocyanate.- Experiment 40. Magnesium-Ammonium Arsenate and Silver Arsenate.- Experiment 41. Rubidium Chlorostannate.- Experiment 42. Estimation of the Relative Quantities of the Metals in a Slurry Containing Arsenic, Antimony, Copper, and Silver.- Working Upon the Surface of a Slide.- Experiment 43. Conversion of Silver Chloride to Silver Dichromate. Handling Precipitates and Solutions, Fusion, and Electrolytic Reduction.- Experiment 44. Separation of Bismuth and Lead. Evaporation, Extraction of “Invisible” Residues.- Experiment 45. Separation of Silver, Lead, and Mercurous Mercury, Sublimation, Extraction with Boiling Solutions.- Experiment 46. Test for Ammonium Ion, Use of the Gas Reaction Cell.- Working in Capillaries.- Experiment 47. Lead Sulfate, Triple Nitrite, Lead Chromate The Capillary as Adjunct to Working Upon the Microscope Slide.- Experiment 48. Recrystallization of Lead Iodide.- Experiment 49. Isolation of Metallic Mercury, Conversion to Iodide.- Experiment 50. Bettendorff’s Test for Arsenic.- Experiment 51. Oxidation of Arsenic to Arsenic Acid. Carius’ Treatment in Capillaries.- Experiment 52. Conversion of Aniline to Acetanilide.- Experiment 53. Conversion of Urea to Symmetrical Diphenyl Urea.- Experiment 54. Purification of Benzene; Separation by Partial Melting in the Capillary.- Experiment 55. Cupric Ammonia Complex, Observation of Color in the Capillary.- Working in Filter Paper.- Experiment 56. Ring-Oven Technique for Extraction and Evaporation in Paper.- Particles of Ion Exchange Resins as Reaction Media.- Working on Textile Fibers and Wires.- Experiment 57. Turmeric Test for Boric Acid.- Experiment 58. Test for Bismuth, Precipitation of the Sulfide Upon the Fiber and Conversion to Sulfate, Chromate, and Elemental Bismuth.- Experiment 59. Bead Test for Cobalt.- Experiment 60. Luminescence Test for Bismuth, Antimony, and Manganese.- Work on the Microgram Scale.- Apparatus.- Technique.- Experiment 61. Mechanical Separation of the Components of a Powder.- Experiment 62. Precipitation of Silver Dichromate Upon the Platform of the Condenser Rod.- Experiment 63. Estimation of the Quantities of Arsenic and Antimony in a Solution of Unknown Concentration.- Additional Practice Experiments for the Chosen Scale of Work.- Experiment 64. Study of Chemical Behavior.- Experiment 65. Analysis of Two Unknown Solutions.- Experiment 66. Identification of Simple Compounds of the Common Metals of the Hydrogen Sulfide Group.- Experiment 67. Identification of Simple Inorganic Compounds.- Experiment 68. Identification of Simple Compounds.- Experiment 69. Identification of Simple Compounds.- Experiment 70. Identification of Materials as They Occur in Nature, Industry, and Research.- II: Systematic Analysis: Choice of Materials and Cleaning.- Sampling for Analysis.- Systematic Procedure of Analysis.- The History of the Sample.- Description of Sample and Record of Investigation.- Preliminary Inspection.- The Sample is a Liquid.- Identification of Organized Matter.- Identification of Artifacts.- Well-Developed Crystals.- Solids of Random Shape and Structure.- Non-Destructive Testing.- Action Upon Light, Color.- Investigation of Crystals and Crystal Fragments.- Testing for Radioactive Decay.- Testing for Ferromagnetism.- Odor.- Hardness.- Refractive Index.- Density.- Classification Tests.- Observation of Transition Points Below 350° C.- Ignition Above 300° C.- Solubility.- Performance of Solubility Tests.- Review: Inorganic Substances.- Organic Substances.- Elemental Analysis of Organic Substances.- Testing with Dilute Sulfuric Acid.- Test with Concentrated Sulfuric Acid.- Flame Tests.- Bead Tests.- Review of Findings.- Dissolution of the Sample.- Treatment of Substances Insoluble in Acids.- Confirmatory Tests.- Group I A: Alkali Metals.- No. 3: Lithium, 6.939.- No. 11: Sodium, 22.9898.- No. 19: Potassium, 39.102.- No. 37: Rubidium, 85.47.- No. 55: Cesium, 132.905.- Group II A: Alkaline Earths.- No.4: Beryllium, 9.0122.- No.12: Magnesium, 24.312.- No. 20: Calcium, 40.08.- No. 38: Strontium, 87.62.- No. 56: Barium, 137.34.- Group III B: Scandium Group.- No. 21: Scandium, 44.956.- No. 39: Yttrium, and the Lanthanides, Nos. 57 to 71.- No. 58: Cerium, 140.12.- No. 63: Europium, 151.96.- No. 70: Ytterbium, 173.04.- Group IV B: Titanium Group.- No. 22: Titanium, 47.90.- No. 40: Zirconium, 91.22.- No. 90: Thorium, 232.038.- Group V B: Vanadium Group.- No. 23: Vanadium, 50.942.- No. 41: Niobium, 92.906.- No. 73: Tantalum, 180.948.- Group VI B: Chromium Group.- No. 24: Chromium, 51.996.- No. 42: Molybdenum, 95.94.- No. 74: Wolfram (Tungsten), 183.85.- No. 92: Uranium, 238.03.- Group VII B: Manganese Group.- No. 25: Manganese, 54.9380.- No. 75: Rhenium, 186.2.- Group VIII: Fe-Ni Triad.- No. 26: Iron, 55.847.- No. 27: Cobalt, 58.9332.- No. 28: Nickel, 58.71.- Group VIII: Ru-Pd Triad.- No. 44: Ruthenium, 101.07.- No. 45: Rhodium, 102.905.- No. 46: Palladium, 105.4.- Group VIII: Os-Pt Triad.- No. 76: Osmium, 190.2.- No. 77: Iridium, 192.2.- No. 78: Platinum, 195.09.- Group I B: Copper Group.- No. 29: Copper, 63.54.- No. 47: Silver, 107.870.- No. 79: Gold, 196.967.- Group II B: Zinc Group.- No.30: Zinc, 65.37.- No.48: Cadmium, 112.40.- No. 80: Mercury, 200.59.- Group III A: Boron-Thallium Group.- No. 5: Boron, 10.811.- No. 13: Aluminium, 26.9815.- No. 31: Gallium, 69.72.- No. 49: Indium, 114.82.- No. 81: Thallium, 204.37.- Group IV A: Carbon-Lead Group.- No.6: Carbon, 12.01115.- No. 14: Silicon, 28.086.- No. 32: Germanium, 72.59.- No. 50: Tin, 118.69.- No.82: Lead, 207.19.- Group V A: Nitrogen-Bismuth Group.- No. 7: Nitrogen, 14.0067.- No. 15: Phosphorus, 30.9738.- No. 33: Arsenic, 74.9216.- No. 51: Antimony, 121.75.- No. 83: Bismuth, 208.980.- Group VI A: Oxygen-Polonium Group.- No. 8: Oxygen, 15.9994.- No. 16: Sulfur, 32.064.- No. 34: Selenium, 78.96.- No. 52: Tellurium, 127.60.- Group VII A: Halogen Group.- No. 9: Fluorine, 18.9984.- No. 17: Chlorine, 35.453.- No. 35: Bromine, 79.909.- No. 53: Iodine, 126.9044.- Separations.- Systematic Schemes for the Detection of Cations.- The Classical Scheme.- Outline for the Separation of the Analytical Groups.- Observations and Notes.- Analysis of Metals and Alloys Attacked by Nitric Acid.- Separation of the Analytical Groups of Novxs and BRAY.- Systematic Search for Anions.- I. Only Alkali Metals or (and) Ammonium Are Present.- II. Nonmetallic Materials Readily Dissolved or Decomposed by Water or Acids.- III. Nonmetallic Refractory Materials.- Final Review of Observations and Report.- Test Solutions.- Preparation of Unknowns.- Reagents.- Table 1. Color of Some Inorganic Substances.- Table 2. Substances Crystallizing in the Cubic System.- Elements.- Inorganic Compounds.- Organic Compounds.- Table 3. Substances Crystallizing in the Hexagonal System.- Elements.- Inorganic Compounds.- Organic Compounds.- Table 4. List of Common Inorganic Compounds in the Order of Their Melting Points.- Table 5. Inorganic Substances that Sublime, Arranged According to Color.- Table 6. Inorganic Solids which Burst into Flame when Heated in Air, Ignition Temperatures in Centigrades.- Table 7. List of Solids which Explode on Heating.- Inorganic Compounds.- Organic Compounds.- Table 8. Inorganic Solids Moderately Soluble in Water at Room Temperature.- Literature.- General Reference Books.- Theory of Chemical Analysis.- Reagents.- Standard Tests and Procedures of Qualitative Analysis.- Chromatography and Ion Exchange.- Instrumental Methods.- Chemical Microscopy.- Slide Tests and Spot Tests.- Micro Analysis and Microtechnique.- Miscellaneous Applications of Microtechnique.- Mineralogy.- Journals.- Reports.- Theses.- Unpublished Experiments.- Private Communications.- Meetings.- Addresses.