Safety valve, 391
Salicylic acid, use of, in Kjeldahl nitrogen determination, 191
S-alkyl groups (see also Alkyl groups), determination of, 438
Salt(s) of alkali and alkaline earth metals, determination of carbon-hydrogen in, 222, 250-255
Salts, use of, as source of carbon dioxide, 180
Sample,
introducing of, into Dumas tube, 181 preparation of, for analysis, 83-101 size of, practical, 2, 31
theoretical minimum, 31 weighing of, 73
Sample containers, 88
Saponification equivalent, determination of (see saponification number)
Saponification number, determination of, 516, 518
Sargent combustion apparatus, 236 Sargent manometric apparatus, 459 Scale, of balance, various, 32
Scale indicating reaction period required for complete decomposition of al-pha-amino acids, 478
Schôniger combustion (see also Flask com
bustion), 291-295, 331, 332 Scrubber solutions, various, for alkoxyl de
termination, 439
Scrubbing towers (bottles), use of, 379, 496
Selenium, determination of, 143,
use of, in Kjeldahl determination, 188, 214
Semicarbazide(s), determination of, 520 Semicarbazide, determination of nitrogen
in, 152, 189
Semimicrochemical balances, 30, 45
Sensitivity of microchemical balances, 30, 38, 39, 55-57
Separation, 97
Shot, lead, use of, for tare purposes, 71, 244
Signer (isothermal distillation) apparatus, 536, 537
Signer method for determination of molec
ular weight, 535-539 additional information related to,
table of, 543, 544 Silica, determination of, 143 Silicon, determination of, 143
determination of alkoxyl on compounds containing, 438
Silver, determination of, 133, 143
use of, for determination of alkoxyl, 439 for determination of sulfur, 307 Silver, use of, in determination of carbon
and hydrogen, 223, 230-235 Silver condenser t u b e ( s ) , 204
Silver halide precipitate(s), dissolving of, 322
drying of, 322 filtering of, 321, 322
treatment of (silver iodide) with nitric acid, 436
weighing of, 322
Silver iodide, treatment of, in alkoxyl de
termination, 423, 433-437
Silver nitrate, alcoholic (see Alcoholic sil
ver nitrate)
use of, in determination of halogen, 317, 324
Silver perchlorate, use of, in determination of fluorine, 328, 332
Silver permanganate, use of, in carbon-hy
drogen determination, 259 Silver s a l t ( s ) , analysis of, for carbon-hy
drogen, 223 Silver sulfate,
use of, in determination of acetyl, 444, 447
in determination of formyl, 444, 447 Silver wire,
use of, in carbon-hydrogen determination, 230-235
Simultaneous determinations (see tables on additional information on references related to the various chapters), 139, 179, 264, 306, 336, 340, 362, 373, 405, 438
Simultaneous determination of alkoxyl and alkimide, 438, 509
Simultaneous determination of barium and phosphorus, 361, 362
Simultaneous determination of chlorine and bromine, 326, 336
Simultaneous determination of ethoxyl and methoxyl, 438
Siphon receiver and inner container, 289 Small mercury bottle with capillary, 464 Soda-lime, use of, as absorbent, 457, 461 Sodium, determination of, 133, 143 Sodium acetate solution, 424
use of, in alkoxyl determination, 424 in oxygen determination, 398 Sodium-alcohol (and other solvents) meth
od for determination of halogens, 338
Sodium alizarin sulfonate, 103 Sodium fluoride, 112
standard solution, O.OlN, 112 standardization of, 112
Sodium hydroxide, carbonate free, 111, 456, 457
on asbestos (see Ascarite) 223
five % solution, use of, in pressure regu
lators, 223, 226
standard solution, O.OlN, 111 standardization of, 111
Sodium hydroxide-thiosulfate solution, 192 use of, in Kjeldahl method, 192
Sodium nitrite, 475
use of, in manometric determination of alpha-amino nitrogen, 478, 479 Sodium nitroprusside test for acetone, 93 Sodium peroxide, use of, in determination
of fluorine, 327
Sodium thiosulfate, crystalline, use of, in Kjeldahl nitrogen determination, 191 Sodium thiosulfate, standard solution,
O.OlN, 108 standardization, 108
use of, in alkimide determination, 508, 509
in acyl (acetyl, formyl) determination, 445
in alkoxyl determination, 424, 434 in arsenic determination, 368 in oxygen determination, 398 Solid(s), drying of, 91-93, 97
weighing of, 73-76
Soltys active hydrogen apparatus, 515
Solvent(s),
for molecular weight determination, by isothermal distillation, 536, 542 by Rast (cryoscopic), 529, 535 of crystallization, 92
determination of, 92
Solvents, various, for alkoxyl determina
tion, 439
Spatula(s) (microspatulas), 66, 67
Specific gravity, determination of, 554-559, 561
additional information related to, table of, 561, 562
using gravitometer, 554-558
using micro weighing pipettes, density type (pycnometers), 558, 559 Spectrophotometric equipment, 125 Spectrophotometric methods, 139, 214, 308,
338, 339, 341, 342, 363, 414, 415, 439, 451, 505, 544
Stand, for manometric apparatus, 460 illuminated titration (see Illuminated
titration stand assembly) Standard solution(s), 102-115, 126
additional information, 115-126 table of, 124-126
barium chloride, O.OlN, 110 hydrochloric acid, O.OlN, 112, 126 iodine, O.OlN, 109
potassium biiodate (biniodate), 102 potassium sulfate, O.OlN, 110, 126 sodium fluoride, O.OlN, 112, 126 sodium hydroxide, O.OlN, 111 sodium thiosulfate, O.OlN, 108, 126 thorium nitrate, O.OlN, 112
Standard(s), use of, in molecular weight determination (see also Test sub
stances, compounds, samples), 536 Standard deviation of balance, 56 Standardization, 2-5
Standardization program(s), 2
Standards (see Test compounds, samples, substances)
Starch indicator, 103 use of, in determination of,
acyl groups, 445 arsenic, 368 oxygen, 398
Static charge(s) (see Electrostatic charges), effect of, 74
elimination of, 12, 74, 253, 259
Statistical studies, 260
Steam generator, 196-199, 201, 328 Steam trap, 199-202
Steaming apparatus, 123 Stirring devices, 125
Stirrup(s) (suspensions), of balance, 33, 35
Stopcock, three-way, for use in Dumas method, 171
Stopcock cylinder, 461, 464 Stopcock grease, 152, 488
Stopcock grease for manometric apparatus, 488
Stopcock pipette, 464
Storm window, heated, for balance room, 13
Strontium, determination of, 133, 143
Strychnine phosphomolybdate, phosphorus determined as, 363
Sublimation,
during carbon-hydrogen determination, 251
use of, for purification, 84, 96 Sublimation apparatus, vacuum, 84, 96 Submicro methods (see Ultramicro-,
sub-micro methods)
Submicrogram methods (see Ultramicro-, submicro methods)
Succinyl chloride, use of, in determination of moisture, 97
Sulfate, titration of, 110, 126
Sulfhydryl group(s), determination of (see Mercapto, Mercaptans )
Sulfonamide(s), Dumas modification for analyzing, 152
Sulfur, detection of elementary, 549 determination of, 276-315 (see also nu
merous items regarding determina
tion, such as apparatus, types of compounds, modifications, interfer
ences, etc.)
additional information on, 304-308 table of, 305-308
bomb fusion, 307
Carius method, 276-290, 306
catalytic combustion, 295-304, 306, 307 direct titration, 413
fusion in general, 307 gravimetric, 287-290, 308 hydrogénation, 307
manometric method, 307 oxy-hydrogen flame, 306, 307 perchloric acid digestion, 307 Schôniger combustion, 291-295, 306 silver gauze, 307
simultaneous, carbon, hydrogen, halo
gen, sulfur, 264, 306
effect of, on carbon-hydrogen determina
tion, 221, 222, 255
Sulfur compound, interference of, in deter
mination of oxygen, 379, 405 Sulfur compounds, group determinations on,
516, 520 Sulfuric acid, 191
standardization of, 2 0 % excess of S Os, 456
Superoxol (see Hydrogen peroxide) Suspension(s), of balance (see Stirrups) System for filling capillaries, 79
Τ Table ( s ) ,
additional information related to chap
ters, 21, 22, 46, 79, 96, 97, 124-126, 138-143, 178-181, 212-215, 260-264, 305-308, 335-342, 362-364, 373, 374, 404-406, 413-416, 438-440, 450, 451, 490-492, 504, 505, 517-520, 543, 544, 561, 562
atomic and molecular weights and their multiples (some of them), 572,573 balance data (information), 38, 39 calibration of micronitrometers (correc
tion), 169 carbon factors, 474
Carius combustion tube data, 281 combustion boats, 59
empirical formula calculation series, 570 gravimetric factors, 571
historical developments, 1 logarithms, 584-601
nitrogen, alpha-amino, calculation factors, 484
nitrogen reduction, 574-583 precision of balance, 56
precision of balance-sample weight re
lationship, 31
sample size, various determinations, 2, 31
sensitivity of balances, 30, 38, 39, 55
solvents for Rast method, 535 vapor pressure of acetic acid, 503
test substances (test compounds, test samples), 8, 9
volumetric factors, 571 weighing bottles, 61 Table for balance, 13-20, 22
inertia block-isolator type, 14-20 rigid type, 19, 20
Tare flasks (bottles), 65, 244
Temperature correction for Dumas method, 168
Test compounds (samples, substances), 6, 8, 9, 22, 260
additional information related to subject, 21, 22
Tests, blank, (see Blank tests)
Tetrahydroxyquinone indicator ( T H Q ) , 104, 278
Thallium, determination of, 143
Thermal decomposition (combustion or re
action) tube, 377, 391, 392
Thermal decomposition tube fillings, 392, 405
Thermal decomposition tube temperatures, 378-381, 394, 405
Thermistors, use of,
for determination of melting point, 550, 551
for determination of molecular weight, 540-544
Thermometer(s), Auschutz, 552 correction for exposed stem, 554 Thermos flask (bottle), use of, for genera
tion of carbon dioxide, Dumas de
termination, 155
Thiosemicarbazides, determination of, 520 Thiuramdisulfide, determination of, 516,
520
Thomas combustion furnace, 157 Thomas manometric apparatus, 460 Thorium, determination of, 143 Thorium nitrate,
standard solution, O.OlN, 112 standardization of, 112, 113 Thymolphthalein, 103 Tin, determination of, 143
Tin foil, use of, in alkoxyl determination, 434
Titration stand, illuminated (see Illuminated titration stand assembly)
Titration vessel, for Karl Fischer determina
tion, 95 Titrations, 102-132
amperometric, 124, 339, 342 automatic, 124, 332, 333, 339 cerimetry, 124
conductometric, 124, 342, 415
E D T A , complexometric, 124, 139, 308, 339, 342, 416
high-frequency, 124, 339, 342, 416 heterometric, 124, 139
nonaqueous, 124, 339, 416 potentiometric, 124, 140, 339, 415 general applications, 126, 416 oscillometric, 342
ultramicro-, submicro-, 414
Titrimetric procedures, 102-132, 264, 451 p-Toluene sulfonic acid, use of, in acyl de
termination, 445, 448 Trace determinations, 405
Transfer of nitrogen and nitric oxide to Hempel pipette, 479, 480
Transformer, use of, constant voltage, 11 variable auto- 136, 197
Treatment of barium sulfate precipitate, 288-290
T u b e ( s ) (see under individual names) u
Ultramicro Kjeldahl method(s), 214 Ultramicro-, submicro methods, 179, 214,
259, 263, 306, 336, 340, 362, 373, 414, 438, 490, 491, 504, 517, 543 Ultraviolet light, use of, to eliminate elec
trostatic charges, 74, 259
Unsaturation (double bonds), determina
tion of, 495-507
additional information related to, table of, 504, 505
Uranium, determination of, 143
Urea, decomposition of, manometric deter
mination, 475, 478 V
Vacuum desiccator(s), use of, 357, 358 Vacuum o v e n ( s ) , 91
Vacuum system, use of, for acyl determina
tion, 447
for drying of samples, 88-92
for molecular weight determination, 536 Vanadium pentoxide, 224
use of, in carbon-hydrogen determination, 222, 224, 255
use of, in Dumas nitrogen determination, 152
Vapor pressure, determination of, 561 Vapor pressure, use of liquids with high,
for isothermal distillation method of molecular weight determination, 536 Vapor pressure of acetic acid, table, curve,
503
Vapor pressure comparison method for molecular weight determination, 544 Vaporimetric method(s), for determination
of molecular weight, 544
Vial testing with manometric apparatus, 485-489
Vials, sample containers, 88
Vibration(s), dampening out of, in balance table construction, 13-21
Vibration isolation, efficiency of, calcula
tion, 15
Vinyl ether, determination of, 516, 519 Viscose liquid(s), determination of specif
ic gravity of, 557 Viscosity, determination of, 562
Volatile compounds, determination of un-saturation on, 505
weighing of, in general, 76-78 Voltage regulation, 10
Volume correction for Dumas method, 168 Volumetric factor(s), table of, 571 Volumetric flasks (see Flasks, volumetric) Volumetric procedures,
for acyl (acetyl, formyl) groups, 444-453 for alkoxyl (ethoxyl, methoxyl) groups,
422-432, 439
for arsenic, 367-369, 373-376 for carboxyl groups, 415, 416 for fluorine, 326-332, 341, 342 for halogens, 413
for metals, 139 for oxygen, 396-409 for phosphorus, 363
for sulfur, 276-287, 291-295, 303, 304, 307, 308, 413
Vorisek test, use of, as means of indirect detection of methanol, 93
w ,
Warburg apparatus, 492, 505 Wash bottle(s), 288
Washing extraction chamber, 472
Water, heavy, use of, for active hydrogen determination, 514, 515, 519
Water (moisture), determination of, 91-93, 97
distilled, for neutralization equivalent and carboxyl determinations, 411 Water absorption tube (see Absorption
tubes)
Water suction system, 465 Weatherproofing, 13 Weighing bottle, 60, 61
various types, 60-64
Weighing bottle, outside cap, 60, 61 Weighing bottle, pig-type, metal, 59, 63, 64
size A, 59, 63 size B , 59, 64 size C, 59, 64
Weighing bottle, pig-type, with outside cap, 61, 62
Weighing bottle with two caps, 62, 63 Weighing cup, 60
Weighing on microchemical balance, 50-82 absorption tubes, 253
additional information, 79 charging tube, 70
filter tubes, 318, 319, 322, 358, 359 pig, 74
sample, 73
hygroscopic, 74, 75 liquid, 76-78
non-hygroscopic, 73, 75 solid, 73-76
performance, 79 problems arising, 79, 261 weighing bottles ( p i g s ) , 74 weighing (charging) tubes, 70, 75 Weighing of samples, 73-79 Weighing techniques, 50, 79 Weighing (charging) tubes, 70 Weighing vessels, 60-64, 70, 76, 78, 79 W e i g h t ( s ) , calibration of, 57, 79 Wet combustion(s), for arsenic, 367-376
for carbon, 263, 454-474, 491 for halogens, 316-323, 336-338, 341 for nitrogen (Kjeldahl), 188-220
for phosphorus, 354-366 for sulfur, 276-291, 307
Window, heated storm, for balance room, 13, 14
X
X-ray fluorescence methods, 139, 308, 339, 363
X-ray spectrophotometric methods, 139, 308 X-ray techniques, 308
Ζ Z-tube, 172
Zero point of balance, 50-55 Zero reading of balance, 50-55 Zinc, determination of, 143
use of, in determination of nitrogen, 191 Zinc dust, use of, in Kjeldahl nitrogen de
termination, 191 Zirconium, determination of, 143