Universitäts- und Landesbibliothek Tirol

A handbook of chemical manipulation

Williams, Charles Greville

London, 1857

Contents

urn:nbn:at:at-ubi:2-3808 vii

CONTENTS .

Section I . Gas-furnace page 28 Gas sand-bath 29 Experimental Laboratory page l Bunsen’s burner 29 Oil- and spirit-lamps . . . . 30 Section II . Circular spirit-lamps . . . . 31 Stoneware wick-holders . . . 31 Furnaces . Berzelius’s lamp 32 Athanor 10 Crucible jacket 32 Brande’s Table-furnace . . . 11 Furnace -rings 11 Section IV . Supports for furnace-bars 12 Hood of furnace 12 Blowpipe Apparatus . Sand-pots 13 Combustion-furnace for tube Black’s blowpipe 33 operations 14 Wollaston’s ditto 34 Luhme’s furnace 15 Cronstedt’s ditto 34 Sefstrom’s blast-furnace . . . 16 Blowpipe-lamp 34 Staffordshire coke as fuel 17 Continuous blast kept up . . 36 Platinum crucibles protected . 18 Oxidizing and reducing flame . 36 Precautions with blast-furnace . 18 Supports for substances before Wind -furnace for various opera¬ the blowpipe 37 tions 19 Platinum wire and spoons . . 38 Furnace -bars for wind-furnace . 19 Handle for ditto 39 Fused products, precautions in Removal of fused mass from wire making 20 and spoons 39 Chauffer (sheet-iron) . . . . 21 Platinum foil 40 Cupelling furnace 22 Clay supports 40 Muffle 23 Forceps 41 Cupel mould 23 Self-acting blowpipes . . . . 41 Maximum heat, position of, in Table blowpipes 43 furnaces 24 Large sand-bath 24 Section Y . Section III . Baths. Lamps. Spirit-bath 45 Argand gas-burner . . . . 25 Water - and oil-baths . . . . 46 Mixed air and gas-lamp . . . 26 Table of boiling-points of satu¬ Remington's burner . . . . 27 rated solutions of various salts 49 Beale’s burner 27 Kemp’s gas-regulator . . . . 49 viii CONTENTS.

Section YI . Section IX . Heat Measurers. Specific Gravity. Specific gravity in general page 83 Construction of thermometerspage 51 of solids 83 Examination of thermometers . 54 of substancesin grains . . 84 Thermometersgraduated on stem 56 tube apparatus for taking . 85 Varieties of thermometers . . 57 of solids lighter than water 86 Leslie’s differentialthermometer 58 of substances soluble in water 87 Melloni’s thermo-electric multi¬ of liquids 87 plier 58 bottle 88 Self-registering thermometers . 58 at standard temperature . 89 Daniell's pyrometer . . . . 59 Hydrometers 90 Wedgwood’s ditto 59 Urinometer 91 Regnault’s air-thermometer . . 60 Twaddell’s scale 91 Beaume’s, Cartier’s, Gay-Lus¬ sac’sand Tralles’ hydrometers 91 Section YU . Hydrometers for hot climates . 92 Nicholson’s hydrometer . . . 92 Operations preparatory to Specific gravity bottle dried . . 93 Weighing. Perforated stoppers to be avoided 93 States in which substances are Vapour densities 94 as check on analytical results 95 to be weighed 65 Dumas’ method of taking . 95 Crucibles cooled 66 balloons for 96 Desiccating media 66 balloons for, dried . . . 96 Watch -glasses 67 balloons for, the point made 96 Ignition of precipitates . . . 67 quantity of fluid to be used 96 Apparatus to contain substances fluid inserted in balloon . 97 while being weighed . . . 71 fusible solids inserted . . 97 Counterpoises 72 nature of bath for . . . 97 supports for balloon . . 97 bath heated 98 Section VIII . balloon inserted in bath . 99 The Balance . balloon sealed . . . . 99 volume of vapour ascertained 100 Proofs of good instrument . . 73 residual air ascertained . . 100 Robinson’s balance . . . . 75 formula for calculation of . 101 Determination of platinum and fusible metal baths for . . 101 silver in organic compounds . 75 Table of density of acetic aeid at Error caused by hook-ends . . 76 varying temperatures . . . 101 Rider for balance 76 Vapour densities under dimi¬ Oertling’s balances 77 nished pressures 102 Weights 78 Gay-Lussac’smethod of de¬ Method of weighing . . . . 78 termining . . . . . 102 Double weighing 79 Formula for calculation of, Weighing of bulky apparatus . 80 at various pressures . 104 Weighing of deliquescent sub¬ Densities of gases, Regnault’s stances 81 method of determining . . 105 Crucibles, &c. cooled before balloons weighed . . . . 105 weighing 82 balloons balanced . . . 106 Substances which emit corrosive balloons exhausted . . . 107 vapours weighed . . . . 82 barometric manometer . . 108 Weighing gases 82 Frankland &Kolbe’smethod 110 CONTENTS. ix

Section X . Filters , weight of . . . page 138 shape of 139 Solution. estimation of ash . . . . 139 folded 139 Varieties of solvents . 2)a9e 11- cut 141 Solvents selected 113 weighed 141 Apparatus for solution . . . 116 supported 141 Test-tubes, flasks, retorts . . . 116 G-melin’s washing-bottle . . . 142 Capsules 117 Berzelius’s ditto 142 Beakers 118 Wash -water tested 143 Infusion , decoction, percolation 119 Continuous wasliing of precipi¬ Payen’sapparatus for continuous tates 143 distillation 120 by inverted flask . . . . 143 Transference of fluids . . . . 121 by Gay-Lussac’s method . 144 Pouring down a rod . . . . 121 by Berzelius’s method . . 145 Transference of solids into flasks 122 by double siphon . . . . 146 Solubility modified by presence Double filter 147 of organic matter . . . . 122 Quadrants of tin for cutting cir¬ Separation of bodies by differ¬ cular filters 148 ence of solubility in certain Splashing avoided 148 menstrua 123 Clearness of filtrate observed . 148 Non-miscible fluids separated by Section XI . filtration 148 Calico filters 148 Precipitation. Filtration of corrosive liquids . 148 at high temperatures . . 150 Precipitation induced by lieat . 124 of volatile liquids . . . 151 by gases 125 of small quantities . . . 151 in analysis 126 out of contact of air . . . 152 influence of heat on . . . 127 special instances of . . . 128 of organic bodies . . . . 129 Section XIII . electro-chemical . . . . 130 incomplete, how remedied 130 Supports for Apparatus. state of solution altered pre¬ vious to 131 Supports for filtration . . . . 153 for pulverization . . . . 155 retarded by organic matter 131 for thermometers . . . . 155 Action of certain reagents . . 130 Wire triangle 156 Lime as a precipitant . . . . 133 156 Precipitation facilitated by heat 134 Supports for evaporation . . . of valuable substances . . 135 Table support 157 fractional 135 Support for reduction-tube . 157 Sefstrom’s holder 157 apparatus for 135 Wooden vice 158 Retort -stands 159 Section XII . Test-tube holder 159 Tripod stand 159 Filtration and Washing of Vertical support 160 Precipitates. Supports for burettes . . . . 161 Grahn’s cylinder-holder . . . 161 Precipitates washed by decanta- Blocks 162 tion 137 Supports for U-tubes . . . . 163 Filtration in general . . . . 138 Support for thermometer and Filtering -paper 138 vapour-flask 163 X CONTENTS.

Section XIV . Section XYI . Disintegration. Pressnre-Tube Operations. General remarks . . . page 1G4 Pestles and mortars of various Pressure-tubes heated . . page 189 kinds 164 constructed 190 Reduction of substances to pow¬ labelled 190 der 165 Bath for pressure-tubes kept at Pestle in one piece 166 constant level 191 Mortars tested and preserved . 166 Precautions in operations with Refractory silicates pulverized . 167 pressure-tubes 191 Agate mortar 168 Pressure-tubes opened . . . 192 Agate mortar examined . . . 169 Substitutes for pressure-tubes . 193 Agate mortar used in blowpipe operations 169 Iron mortar 169 Section XVII . Pulverization of camphor and Evaporation. chloride of ammonium . . 170 Metals obtained in powder . . 170 Evaporation over naked fire . 194 Diamond mortar 170 Bayeux and Meissen dishes . . 195 Necessity for stirring . . . . 196 Section XV . Access of dust prevented . . . 197 Evaporation over desiccating Crucibles and Operations at media 198 High.Temperatures. Precautions in drying substances 199 Cornish crucibles 171 171 English crucibles Section XVIII . Skittle-pots 172 Hessian crucibles 173 Distillation. Blue-pots 173 Porcelain crucibles 174 Alembic 202 Platinum crucibles 175 Retorts 203 Platinum capsules 176 Substances added during distil¬ Precautions in using platinum lation 204 vessels 177 Receivers 205 Gold crucibles 178 Substitutes for retorts . . . . 206 Silver crucibles 178 Tube-retorts 207 Iron crucibles 178 Distillation with tube-retorts . 209 General remarks on crucible Alembics, tube condenser, com¬ operations 178 mon still 211 Crucible tongs 179 Distillation with common still . 213 Terms used to denote high tem¬ Concussiveebullition . . . . 214 peratures 179 Worm cleaned 215 Charcoal crucibles 179 Precautions in distilling with Crucibles heated 180 retorts 216 Crucible operations, special cases 182 Liebig’s condenser 217 Reductions in platinum and por¬ Adapters 218 celain crucibles 185 Adapters used as condensers . 219 Operations at high temperatures Distillation of very volatile fluids 220 in tubes 185 Adapters cooled 221 Gun-barrels 186 Fractional distillation . . . . 221 Reductions in tubes . . . . 187 Special cases of distillation . . 226 Tubes luted 188 Distillation of sulphuric acid . 227 Illustrations of processes in tubes 188 of hydrofluoric acid . . . 227 CONTENTS. XI

Preparation of hydrochloric Decomposition induced by ten¬ acid page 229 dency to crystallize . page 253 Distillation of fluids which ex¬ Water of crystallization . . . 253 plode at 212° 230 Water mechanically contained Distillation of mercury . . . 230 between layers of crystals . . 254 Distillation in a current of hy¬ Crystallization from alcohol and drogen 231 mixtures of alcohol and water 254 Distillation of spontaneouslyin¬ Crystallization of substances flammable fluids 232 equally soluble in hot and Fluids requiring digestion pre¬ cold water 255 vious to distillation . . . 233 Slow cooling of solutions to be Stoneware still 234 crystallized 255 Chloride-of-calcium bath . . . 235 Vibration prevented during cry¬ Destructive distillation . . . 235 stallization 255 Distillation of wood and coal . 236 Removal of resinous and oily Apparatus for destructive distil¬ impurities from organic bodies 255 lation 237 Variations in tendency to as¬ Iron alembics 238 sume crystalline state with Hot -air bath 239 different members of homolo¬ Stone alembic 239 gous series 256 Distillation under diminished Special instances of crystalliza¬ pressure 240 tion 257 Separation of bodies of different Crystallization at high tempe¬ degrees of volatility by double¬ ratures ...... 258 headed still 241 Coloured crystals bleached by Distillatory apparatus coated animal charcoal 259 with copper 242 Crystallization of benzole . . 259 Small retorts for fractional di¬ Crystallization of substances stillation 243 from a solution in benzole . 260 Very volatile fluids condensed . 243 Apparatus for cohobation over sodium, &c 244 Section XXI .

Section XIX . Volumetric Manipulation. Sublimation. Gray-Lussac’s burette . . . . 262 Mohr’s alkalimeter 262 Sublimationinplatinum crucibles 245 Binks’ alkalimeter 262 in porcelain crucibles . . 245 in porcelain basins . . . 245 precautions in using . . 264 of iodine 245 part of curve of fluid to be read from ...... 265 of naphthaline , &c. . . . 246 French alkalimeter . . . . 265 of indigo 247 Volumetric determination of of biniodide of mercury . 247 Change of colour in substances acids 266 by sublimation 247 Lime-syrup , . 266 Sublimation in current of air . 248 Compression-bottle for filling in tubes 248 burettes 267 in crucibles 249 Strength of standard solutions . 268 Volumetric determination of al¬ Section XX . kalies 271 Volumetric methods in general 271 Crystallization. Volumetric estimation of bromine 271 Large crystals formed . . . 251 Volumetric estimation of chlo¬ Fractional crystallization . . 252 rine, uranium , urea, silver . 272 XU CONTENTS .

Test-papers page 273 Experiments with gas-jars page 300 Litmus-papers 274 Gases collected by displacement 302 Turmeric ditto 274 Kerr’s gas-tube 304 Lead ditto 274 Solution of gases 305 Logwood 275 Safety-tubes 307 Fir -wood 275 Gasometer 309 Guaiacum 275 Glass gasometer 313 Experiments showing accuracy Transference of gases at the of the methods given . . . 275 pneumatic trough . . . . 314 Alkalimetry 275 Manipulation with gases over Estimation of silver by standard mercury 316 solution of common salt . . 276 Mercurial troughs 317 Estimation of free bromine by Cooper’s mercurial receiver . . 320 oil of turpentine . . . . 277 Transference of gases . . . . 321 Results of analysis of some car¬ Transferring pipette . . . . 322 bonates of potash . . . . 278 Miller’s transferring pipette . 323 Regnault’s gas analysing appa¬ Section XXII . ratus 324 Franklandand Ward ’s gas ana¬ Gas Manipulation. lysing apparatus . . . . 332 Sulphuretted hydrogen . . . 279 Eudiometers 337 Preparation of sulphuretted hy¬ Mixture of gases exploded . . 338 drogen from sulphide of iron 280 Gay-Lussac’s eudiometer . . 339 Kemp’s sulphuretted hydrogen Mitscherlich’s eudiometer . . 339 apparatus 281 Ure’s eudiometer 340 Bunsen’s eudiometer . . . . 342 Uses of sulphuretted hydrogen . 283 Carbonic acid 284 Reading-off of volumes . . . 343 Error of meniscus 343 Sulphuretted hydrogen and car¬ Estimation of carbonic acid in bonic acid prepared on large scale 285 carbonates by weight . . . 344 Hydrogen 286 Parnell ’s method 344 Reductions in hydrogen . . . 287 Fresenius and Will ’s apparatus 345 Other uses of hydrogen in re¬ search 288 Section XXIII . Hydrogen lamp 289 Oxygen prepared 291 Manipulation connected with Chlorine prepared 292 Organic Analysis . Chlorine prepared in large Analysis with chromate of lead 349 quantities 292 Potash-tube 350 Sulphurous acid prepared . . 293 Chloride-of-calcium tube . . 351 Sulphite and hyposulphite of Suction-tube 352 soda prepared 294 Tube to contain substance . . 353 Cyanogen prepared . . . . 294 Corks for combustions 354 Nitrous acid prepared . . . 295 Corks prepared for combustions 355 Muriatic acid gas prepared . . 295 Combustion-tubes 356 Collection and retention of Combustion-tubes made . . . 357 gases 295 Reduced copper turnings . . 358 Pneumatic trough 296 Caoutchouc-tubes 358 Bee-hive shelf 297 Combustion-furnace . . . . 359 Manipulation with gas-jars . . 298 Operations previous to all ana¬ Gas-jars required in experi¬ lyses 360 ments 299 Analysis of substances free from Deflagrating jar 299 nitrogen 361 CONTEXTS. xiii

Analysis of substances contain¬ Safety-tubes made . . . page 414 ing nitrogen . . . . page 367 Retort and receiver in one piece 415 Analysis of liquids 369 Combustion of fluids easily de¬ Section XXY . composableby heat . . . . 371 Modified process for burning Electrical and Galvanic Mani¬ fluids 372 pulation. Analysis of fusible solids. . . 373 G-lass trays made 373 Electrophorus constructed . . 417 Analysis of substances difficultly Smee’s battery 418 combustible 374 Silver platinized 419 Laurent ’s mode of burning in a Smee’s battery made . . . . 420 current of oxygen . . . . 375 Large binding-serew . . . . 422 Potash-tube with extra tube at¬ Grove’s battery 422 tached 376 Binding-screw for Grove’s bat¬ Analysis of substances contain¬ tery 423 ing sulphur 376 Daniell’s battery 424 Combustion of very volatile li¬ Bunsen’s battery constructed . 425 Miscellaneousgalvanic manipu¬ quids . 377 lation 426 Ultimate analysis of gases con¬ taining carbon 377 Binding-screws and connexions 426 Estimation of nitrogen . . . 380 Apparatus for electrolysis . . 427 Estimation of nitrogen by Will Apparatus for preparing battery and Yarrentrap ’s method . . 380 gas 428 Apparatus for obtaining gas Kemp’s nitrogen-tube . . . 381 from either electrode . . . 429 Nitrogen determinations made in gun-barrel 382 Electrotype 430 Estimation of nitrogen by Lie¬ Glass flasks covered with copper 431 big’s qualitative method . . 383 Copper flasks made by the elec¬ Determination of nitrogen by trotype 432 Bunsen’s method . . . . 384 Absolute method of determining Section XXYI . nitrogen 387 Gas-furnaces for organic analy¬ Miscellaneous Operations. sis 389 Beale’s furnace . . . . 390 List of tools 434 Hofmann ’s furnace . . . 390 Wooden screws made . . . . 435 Metallic screws made . . . . 436 Aspirator for use in combus¬ tions 397 Caoutchouc-tubes 437 Corks and cork-borers . . . 439 Section XXIV . Tubes graduated 440 Stopcocks 445 Glass-working. Exhausted globes filled with gas 447 Tubes bent 400 Knots 448 Herapath ’s jet 401 The barometer > 450 Cutting glass 402 The goniometer 451 Spring-coals or pastilles . . . 403 Haiiy’s goniometer 452 Piercing holes in glass . . . 404 Wollaston’s goniometer . . . 453 Siphons made 406 The air-pump 457 Tubes closed 408 Leak in pump plate found . . 459 Pipettes made 409 Precautions in drying in vacuo 460 Bulbs blown 410 Defects in pump discovered. . 461 Gas-funnel ; 411 Silver salts dried in vacuo in U-tubes made 413 darkness 462 XIV CONTENTS.

Section XXYII . Formation of acids by treat¬ ment of organic substances Processes and Reactions em¬ with nitric acid . . . page 501 ployed in some researches. Treatment with peroxides . . 503 Production of acids by ferment¬ Non-metallic bodies . . page 465 ation 503 Processes of oxidation . . . 466 Treatment of organic bodies Atomic weight of non-metallic with acids to form conjugate element determined . . . 468 acids 504 Determination of vapour volume 469 Acid amides 505 Processes and reactions con¬ Production of acids by destruc¬ nected with metals . . . . 469 tive distillation 505 Stromeyer’s discovery of cad¬ Pyro -acids 506 mium 471 General remarks on organic Phospliuret of iron mistaken for acids 507 new metal by Bergman . . 472 Gerhardt ’s anhydrous acids . . 508 Subphosphate of yttria mis¬ Decomposition of anhydrous taken for new metal . . . 472 acids by metals 509 Thorina mistaken for new me¬ Organic alkaloids 510 tal, and called donarium . . 472 Alkaloids obtained from the ve¬ Physical properties of metals . 473 getable kingdom . . . . 510 Crystallizability of metals . . 474 Bases derived from the animal Tenacity of metals 475 kingdom 513 Chemical properties of metals . 475 Production of bases by the ac¬ Metallic oxides 477 tion of alkalies on the cyanic Ilinenium a mixture of sesqui- and cyanuric ethers . . . 515 oxide and bin oxide of niobium 477 Production of bases by the ac¬ Pelopium a mixture of tantalic tion of ammonia on the hy- acid with niobate of niobous driodic ethers 517 acid 477 Action of reducing agents on Solubility of metals in acids . 478 the nitro -compounds of cer¬ Reduction of oxides to lower tain hydrocarbons . . . . 519 state of oxidation . . . . 479 Action of reducing agents on Solubility of metals in acids. . 481 the nitro -compounds of oxi¬ Peculiarities of various oxides . 483 dized bodies 521 Action of the non-metallic ele¬ Formation of alkaloids by de¬ ments on metallic oxides . . 484 structive distillation . . . 521 Action of chlorine on metallic General remarks on organic oxides 485 alkaloids 523 Methods of determining atomic Some processes and reactions weights 486 connected with neutral bodies 524 General considerations on the Alcohols 524 elements 489 Aldehydes 525 Metallic groups 491 Ethers 527 Processes and reactions used in Compound ethers 528 organic researches . . . . 493 Nature of aldehydes . . . . 529 Volatile acids examined . . . 495 Aldehydes produced by destruc¬ Fixed vegetable acids examined 496 tive distillation 530 Acids derived from the animal Aldehydes found in plants . . 530 kingdom 498 Isomeric aldehydes . . . . 530 Acids produced by treating or¬ Thialdine 530 ganic substances with oxidi¬ Separation of aldehydes from zing agents 500 complex mixtures . . . . 531 CONTENTS . XV

Hydrocarbons . . . . page 531 VII . Correctionto be applied Benzole series 531 to barometers with Derivatives of benzole . . . 533 brass scales extending Alcohol radicals 534 from the cistern to the Hydrocarbons homologous with top of the mercurial olefiant gas 534 column, to reduce the Decomposition of halogen com¬ observation to 32° pounds by sodium . . . . 535 Fahrenheit . . page 556 Naphthaline 536 VIII . Correction to be applied to barometersthe scales Appendix. of which are engraved Lamp for the production of high on glass, to reduce the temperatures 537 observations to 32° Forge for high temperatures 539 Fahrenheit . . . . 562 Crucibles for high temperatures 540 IX . Correction of barome¬ Determination of vapour-densi- ters for capillary ac¬ ties at varying pressures . . 542 tion 562 Lines divided into equal parts . 544 X.&XI . Conversion of the Stills for destructive distilla¬ gramme and its sub¬ tion,&c 545 divisions into grains . 562 Supports for U-tubes . . . . 546 XII . Conversion of millime¬ Compression pipettes . . . . 547 tres into inches, and Simple decanting apparatus 547 inches into millimetres 563 Small press for squeezing fluids XIII . Weights and measures . 563 out of preparations . . . . 548 XIV . Boiling-points of water Cement for glass and metal for at different pressures . 563 temperatures up to 212° . . 548 XV. Expansion of gases by Apparatus for obtaining the elec¬ heat (Regnault) . . 563 tric spark in damp rooms 548 XVI . Specific gravity of liquids Plan of laboratory, and descrip¬ at 55° Fahrenheit , cor¬ tion 549 responding to the de¬ grees of Beaume’s hy¬ TABLES ...... 552 drometer 564 I . For conversion of de¬ XVII . Weight in grammes of grees Centigrade into one cubic centimetre of degrees Fahrenheit 552 air at different tempe¬ II . Elastic force of aque¬ ratures from 0° to 300° ous vapour in inches Centigrade . . . . 564 of mercury for Fahr¬ XVIII . Specific gravity and ab¬ enheit’s thermometer . 554 solute weight of certain III . Elastic force of aque¬ gases 566 ous vapour in milli¬ XIX . Quantity of absolute al¬ metres of mercury for cohol in spirits of dif¬ Centigrade thermome¬ ferent specific gravi¬ ter 555 ties, according to Lo- IV. Comparison of the de¬ witz 566 grees of the mercurial XX. Quantity of absolute al¬ with those of the air- cohol by weight in mix¬ thermometer according tures of alcohol and to Regnault . . . . 555 water of different spe¬ V. Ditto,according to Mag¬ cific gravities, accord¬ nus 554 ing to ill ’. Drinkwater 568 VI . Ditto, according to Du- long and Petit . . . 555 INDEX 569