Modern methods in organic microanalysis:
Gespeichert in:
| Beteilige Person: | |
|---|---|
| Format: | Buch |
| Sprache: | Englisch |
| Veröffentlicht: |
London [u.a.]
Van Nostrand
1968
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| Schriftenreihe: | The Van Nostrand series in analytical chemistry
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| Schlagwörter: | |
| Links: | http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=002858043&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
| Umfang: | XV S., 1 Bl., 301 S. |
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Datensatz im Suchindex
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|---|---|
| adam_text | MODERN METHODS IN
V ORGANIC MICROANALYSIS
JEAN P DIXON
Senior Scientist
Shell Research Limited
Chester
LONDON
PRINCETON,NEWJERSEYTORONTO
CONTENTS
PREFACE
CHAPTER 1 A NEW PHILOSOPHY
Introduction
Arrangement and Contents of the Text
Training in Microchemical Procedure
Customer Relationship
CHAPTER 2 LABORATORY DESIGN AMD LABORATORY EQUIPMENT
Laboratory Design
The balance room
Benches and bench services
Safetyscreens
Fume cupboards
Heating
Water supply
Laboratory Equipment
In the balance room
Microchemical balances
The quartz fibre microgram balance
Static eliminators
Drybox
Fume chamber
Inthelaboratory
Microchemical combustion furnaces
Apparatus for combustion in an oxygen-filled flask
Parr micro bomb
Sample mixer
BIBLIOGRAPHY
REFERENCES
CHAPTER 3 SAMPLING PROCEDURES
Introduction
Operation of the balance
Manipulative tools
Weighing Vessels
Combustion boats
viiiMODERNMETHODSINORGANICMICROANALYSIS
Weighing cups
Weighing handles
Melting-point tubes
Sealed tubes
Paper supports and Sellotape packets
Additional Devices
Inert gas blanket
Weighing pig
Pyrolysis tube cooling device
Weighing Vessels for the Transfer of Microgram Samples
Weighinghandleforsolidsamples
Transfer of liquid samples
REFERENCES
CHAPTER 4 DETERMINATION OF CARBON AND HYDROGEN
Introduction
Micro Determination of Carbon and Hydrogen by Ignition in
Oxygen
Principle
Apparatus
Rotameter
Quartz tube
Purification tubes
Ignition tube
Adsorption tubes and counterpoises
Manganese dioxide adsorber
Reagents
Preparation of the apparatus
Preliminary notes on procedure
Procedure
Problems associated with weighing adsorption tubes
Static interference
Time conditioning
Modifications to the Method
Tungstic oxide as a sample flux
Analysis of mercury compounds
Analysis of compounds with high sulphur contents
Summary of Sampling Procedures
Comments and Typical Results
Application to the Determination of Carbon-to-Hydrogen Ratios
Application to the Determination of Carbon in Iron and Steel
Separationofcarbon
Determination of carbon by ignition
REFERENCES
CHAPTER 5 DETERMINATION OF NITROGEN
Introduction
The Pregl-Dumas method
The micro Kjeldahl method
The micro Ter Meulen method
CONTENTSix
The Structure of Nitrogen Compounds and the suitability of the
Micro Kjeldahl and Micro Ter Meulen Methods of Analysis 59
Notes on the choice of the method 60
Determination of Nitrogen by the Micro Kjeldahl Method 60
Principle60
Apparatus60
Reagents66
Procedure67
Determination of Nitrogen by the Micro Ter Meulen Method 67
Principle67
• vApparatus67
Reagents68
Preparation of the apparatus 69
Notes on procedure 69
Procedure69
The use of nickel powder 70
Determination of Small Quantities of Ammonia with Sodium Hypo-
bromite70
Principle71
Apparatus71
Reagents71
Procedure72
Determination of Traces (ppm) of Nitrogen by a Concentration
Procedure73
Principle74
Suitability test 75
Apparatus75
Reagents76
Procedure76
Percolation procedure for samples containing less than 5 ppm
ofnitrogen77
Principle77
Preparation of the column 78
Determination of Basic Nitrogen 79
Principle80
Apparatus80
Reagents80
Procedure81
REFERENCES 83
CHAPTER 6 DETERMINATION OF OXYGEN 84
Introduction84
Method Development 85
The carbon conversion 85
Carbon monoxide oxidation 86
Determination of carbon dioxide 86
Other developments 87
Interferences87
Micro Determination of Oxygen 89
xiiMODERNMETHODSINORGANICMICROANALYSIS
Methods of decomposition 155
Wet oxidation 155
Fusion with sodium peroxide in a Parr bomb 156
Heatingwithzincoxide156
Decompositionwithahydriodicacidreagent156
Decompositioninanoxygen-filledflask156
Methodsofdetermination157
Volumetric 158
Colorimetric 158
Determination of Phosphorus by Combustion in an Oxygen-filled
Flask 160
Principle160
Apparatus160
Reagents160
Preparation of calibration curve 161
Procedure 161
Determination of Phosphorus by Wet Oxidation in a Volumetric
Flask162
Principle162
Apparatus163
Reagents 164
Preparation of calibration curve 164
Procedure 164
Determination of Phosphorus on the Microgram Scale 165
Principle 166
Apparatus166
Reagents168
Preparation of calibration curve 168
Procedure169
REFERENCES 170
CHAPTER 10 DETERMINATION OF BORON 172
Introduction172
Methods of decomposition 172
(a) Wet oxidation 172
(b) Decomposition in a bomb 173
(c) Fusion with sodium carbonate 173
(id)Combustioninanoxygen-filledflask173
Methods of separation 174
Methods of determination 174
The sodium hydroxide-mannitol method 174
Colorimetricmethods175
Determination of Boron 179
Principle179
Apparatus179
Reagents180
Procedure180
(a) Standardization of sodium hydroxide 180
(b) Sample procedure 180
CONTENTSXiii
Note on the determination of boron trifluoride 181
REFERENCES 182
CHAPTER 11 DETERMINATION OF METALS IN ORGANIC COMPOUNDS 184
Introduction 184
Composition of Combustion Residues 184
Apparatus 185
Micro muffle 185
Platinum boats 186
Reagents186
Procedure186
NotesonProcedure187
Supplementary Methods for the Determination of Metals 188
REFERENCES 190
CHAPTER 12 POTENTIOMETRY IN NON-AQUEOUS MEDIA 191
Introduction 191
Acidity and solvent media 191
Titrants and standards for acidity determinations 192
Applications of tetrabutyl ammonium hydroxide (TBAH) in
selected potentiometric systems 193
Determination of Organic Acids 195
Principle 195
Apparatus 195
Reagents196
Preparation of TBAH 196
Procedure197
Determination of Combined Acids 198
Principle198
Additional apparatus 199
Additional reagents 199
Preparationofcolumn199
Procedure 199
Titrations with Silver Nitrate 200
Thiols and disulphides 200
Hydrolysable chlorine 202
a-Epoxy groups 202
REFERENCES 203
CHAPTER 13 MISCELLANEOUS DETERMINATIONS 204
Introduction204
Acetyl, Benzoyl and C-Methyl Groups 206
Procedure for hydrolysis 207
Procedure for oxidation of C-methyl groups 208
Acetylenic Hydrogen 208
Procedure for titration with sodium hydroxide 209
Active Hydrogen 210
Alkoxy Groups 212
Procedure213
Notes on the procedure 214
Amino Groups , , 215
XivMODERNMETHODSINORGANICMICROANALYSIS
Titrimetric determination of amines 216
Acetylation 217
Reaction with an aldehyde 217
Reactionwithnitrousacid217
CarbonylGroups218
a-Epoxy Groups 219
Hydroxy Groups 220
Micro esterification of hydroxyl groups 221
Procedure 222
Micro determination of 1,2-diols 222
Procedure223
Nitro, Nitroso, Azo and Hydrazo Groups 224
Procedure225
Peroxy Groups 225
Procedure226
Sulphur Groups 227
Unsaturation 229
Procedure for bromine number determination 229
Procedure for iodine number determination 230
Water231
(a) Removal of water 231
(b) Determination of active hydrogen 232
(c) Determination by Karl Fischer reagent 232
(d) Coulometric determination 234
(e) Spectrophotometric determination 235
REFERENCES 235
CHAPTER 14 QUANTITATIVE ASPECTS OF PAPER AND THIN-LAYER
CHROMATOGRAPHY 238
Introduction238
Physical methods 238
Comparison of spot or zone-strip sizes 239
Determination of the area of the spot 240
Photographic recording 240
Optical measurement 240
Radioactivecounting241
Chemical methods 241
Decomposition and the determination of an element 241
Titrimetric procedures 242
Colorimetric methods 243
Sample sizes 244
Determinations involving Combustion in an Oxygen-filled Flask 245
Analysis via sulphur content 246
Analysis via chlorine content 247
Screening Samples before Microanalysis 248
Preparation of chromatograms 250
REFERENCES 250
CHAPTER 15 THROUGH INSTRUMENTATION TO AUTOMATION 252
Introduction 252
CONTENTSXV
Carbon, Hydrogen and Nitrogen 253
Instrumental approach 253
Mechanization of the combustion 253
Manometric determination 254
Electrical conductivity 254
Thermal conductivity 256
Coulometric determination 258
Commercial analysers 260
Nitrogen 267
The Pregl-Dumas method 267
The Micro Kjeldahl method 267
VOxygen268
Instrumental approach 269
The Coleman Analyzer 269
Autoanalysis270
Principle of operation 270
REFERENCES 272
CHAPTER 16 ACCURACY AND SOURCES OF PRACTICAL ERROR 275
Introduction275
Gravimetric Errors 278
Volumetric Errors 280
Methods of measurement 280
(a) The sample 280
(b) The reagents 280
(c) The titrant 280
Chemical errors 287
Colorimetric Errors 288
The theory and practice of a spectrophotometric procedure 290
Experimental variables 292
REFERENCES 293
INDEX295
|
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| spellingShingle | Dixon, Jean P. Modern methods in organic microanalysis Chemistry, Organic Microchemistry |
| title | Modern methods in organic microanalysis |
| title_auth | Modern methods in organic microanalysis |
| title_exact_search | Modern methods in organic microanalysis |
| title_full | Modern methods in organic microanalysis Jean P[ickering] Dixon |
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| title_full_unstemmed | Modern methods in organic microanalysis Jean P[ickering] Dixon |
| title_short | Modern methods in organic microanalysis |
| title_sort | modern methods in organic microanalysis |
| topic | Chemistry, Organic Microchemistry |
| topic_facet | Chemistry, Organic Microchemistry |
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