Index

Absorption 333, 459 Acetone 95 Acetylene 272 Adsorption 333, 432

water 376

water in glass 22 Aluminosilicate glass, see Glass, alu-

minosilicate

American Chemical Society 511 American Society for Testing and Ma-

terials, see ASTM American Vacuum Society 515 Annealing (glass) 4, 6 Aristotle 325

Aspirator 341-343 ASTM 85, 177

Avogadro's Law, see Gas law

B

Back diffusion 377,432 Back migration 378, 432 Back streaming 377 Backflow 368, 387, 432, 433

Backstreaming, see also Leak detection 441

Baeyer, von 327 Baffles 386 Balances 118-144

accuracy 123

air buoyancy 120-122 analytical 132-136 beam 131

buoyancy 120 calibration 139-144 density 119

inertia 119

lever Arm 128-131 linearity 123

location 123 mass 119 null-type 131

off-center errors 123 precision 122 readability 122 reading 125-127 Roberval principle 130 scale intervals 118 spring 127-128 top-loading 136-137 true mass 122 verification 137-139 weight 119

Barbs 480

Base bath, see also Cleaning, base bath 240

Bayard-Alpert (gauge) 327 Boyle, Robert 327

Boyle's Law, see Gas laws Brazing 488

Buckley 327

Buna-N 460 Bunsen burner 477 Burettes 113-118

automatic 116 Class A 113 cleaning 118 dispensing 116 Geissler 115 Mohrll5 student grade 113

Teflon stopcocks 117

Cajon® Ultra-Torr 405 Calibrated weights 119, 139 Caliper 80

dial 82

518

electronic 83

Canadian Chemical Producer's Association 273

Canadian Transport Commission 255 Centigrade 147

CGA Fittings 256

Charles' Law, see Gas laws ChemCapl91 Chemisorption 432 Chromic acid 244

alternatives 245 Clamp supports 470 Cleaning

acids and oxidizers 242-244 albuminous materials 250 bacteriological material 250 base baths 92, 240-242 carbonaceous materials 250 chromic acid 244-245 cuvetts 233

fritted filters 248 glass strippers 232

hydrofluoric acid 245-247 iron stains 249

last resort cleaning solutions 250- 251

magnesium oxide stains 250 mercury residue 249 mineral deposits 232

NMR tubes 233

organic solvents 239-240 permanganate stains 250

polar and nonpolar solvents 234 rinsing 232

safety 234

soap and water 236-238

tar from distillation flasks 249 tungsten from glassware 248 ultrasonic 238

Cleaning, see also Hydrofluoric acid 92

Coaxial traps

see Traps, coaxial Cold traps

Index

see Traps, cold Compressed gas

cap removal 257 emergency 272 finding leaks 283 safety 254-256 tanks 253-278

color coding 268 marking 272 safety 269-272 storage 271

Compressed Gas Association (CGA) 256

Compression ratio (re. mechanical pumps) 432

Condensable gases

see Condensable vapors Condensable vapors 340, 352, 353,

354, 355, 384, 386, 416, 427, 464

Conductance (gas flow) 338 Conduction 287 Convection 287

Cooling 301-318 containment 309-313

beakers and flasks 313 dewars 310

foam insulated containers 312 dry ice 303

ice 302

ice with salts 302 liquid nitrogen 303 slush baths 304-309 tap water 302

Corks 49 Crawford 327

Crookes, Sir William 327 Cryogenic gas tanks 313-318

gas dispensing tank 316 liquid dispensing tank 313

D

Dalton's Law, see Gas law

Index

Degassing 431

Density, see Balances, density Department of Transportation 255 Desorption431

Detector-probe technique, see Helium leak detection

Dewar, Sir James 327 Dewars 310 Diffusion 431

Diffusion pumps 365-384 arrangement on vacuum lines 370-

372 cleaning

fluorinated oil 383 glass 381 mercury 384 metal pump 381

diagnosis and correction 375 draining 381

glass versus metal 367 limitations 377 maintenance 380-384 oils 378-379, 381, 382 pumping speed 366 safety 377

swamped 441 use 372

Wheeler design 370

Disposable glass (student glassware) 11

Drying ovens 299 Duran 13

Durometer (on flexible tubing) 43

E

Engineering resins 495 nylon 495 polycarbonate 495 polysulfone 495

EPR 483 Evaporation 431 Exax 12, 92

519

Faraday, Michael 327 Film enclosures 58 Filters 386

Fire-polish (glass) 56, 477, 482, 487 Fisher burner 477

Flanges, glass to metal 367 Flask stoppers (stopper plug) 178 Flexible tubing 4 1 ^ 8

dimensions 42 pressure 44

Fluorocarbons 496 ethylenechlorotrifluoroethylene

496 ethylenetetrafluoroethylene 496 perfluoroalkoxy 496 polyvinylidene fluoride 496 tetrafluoroethylene 496

Flux 488

Fore pumps, see also Mechanical pumps, fore pumps 346

G

Gaede 327 Gas

compatibility 273 cryogenic 253 definition 253 dissolved 253 solidified 253 volume in tank

by regulator 279 by tarring 254

Gas ballast

see Mechanical pumps, gas ballast Gas discharge tube 449

Gas flow 335-338

effects of tube diameter versus length on pumping speed 338

molecular 336 turbulent 335 viscous 335

520

Gas laws 329, 329-331

Exceptions to Ideal gas law 331 Gases versus vapors 329

Gasket materials aluminum 468 conflat 468

copper (OFHC) 468 gold 468

indium wire 468 Gas-oxygen torches 477 Glass 1-41

aluminosilicate 14,431 annealing point 4 apparatus (accuracy) 492 apparatus drawing 489-492 borosilicate glass 5, 13

breakage (preventing) 22-25 devitrification 7, 10

silica 8 8-cristobalite 8

faults (in glass) 40 faults (manufacturer) 40 fused quartz 2

fused silica 2, 15 graded seals 18 grading glass 18 hard glass 9, 13-15 heat-strengthening 31

high temperature and UV-trans- mission 9, 15-18

joints 491 lead glass 5

flint 12

marking (on) glass 38 melting point 3 phase separation 6 properties of 1 quartz

four types 16 quartz crystal 2 quartz glass 2, 5, 15 recycling 10 refractive index 12

separating (types of glass) 19

Index

checking the sodium content of the glass 21

linear expansion 22

logical deduction and observation 19

matching the index of refraction 21

sighting down the end of a glass tube or rod 20

SiO22

soda-lime 10, 477 crown 12 sodium silicate 11 soft glass 9,10-13 softening point 4

storage 37 strain point 4 strength of 22

structural properties 1 surface check 24 techniques for heating 30 tempered

ion exchange 32 laminated 33 rapid cooling 31

tubing 490 Vycor 6, 16 waterglass 11 working point 4

Glass strippers 232 Glass tubing 56, 212-228

basics 212

inside diameter 213 volume calculations 215

Glass vacuum system, see Vacuum system, design (glass)

Glassblowing 372,488 see also Chapter 8

Glassware anneal 488

cleaning 231-251 Glyptol 466

Graded seal 367 Graduated cylinder 87

Index

Graduated cylinders 104-107 EX 88

IN 88 pharmaceutical 105 Style 1 105

Style 2 105

Style 3 105 TC87 TD87

Tolerances 106

Ground joints (standard taper) 173 Ground joints, see Joints Guericke, Otto von 326

H

Halar 496 Halocarbons 239

methylene chloride 239 perchloroethylene 239 trichloroethylene 239 trichlorotrifluoroethane 239

Heating 287-301

advantages of open flames 289 drawbacks to open flame 289 electrical resistance heaters 296-

300 hot air guns 295

microwave 294-295 safety precautions 288

safety with open flames 290-292 six ways in laboratory 287 steam 292-294

thermal radiation 294 Helium 261, 262, 275 Helium leak detection

calibration 466 clean-up time 464 complications 461

detector-probe technique 456,457, 463

inside-out technique 456, 458 maintenance 465

outside-in technique 456,458

521

response time 464 techniques 457-459

tracer-probe technique 456,463 spraying pattern 463

Hose connection 480 Hydrochloric acid 242 Hydrofluoric acid 245 Hydrogen 261, 262, 276

Ideal Gas Law, see Gas law Implosion 469

Inside-out technique, see Helium leak detection

Ionization gauge

as getter pump 423 cold-cathode ion gauge 429

cleaning 430

hot and cold ion gauge 423 hot-cathode ion gauge 424

cleaning 428 filaments 426 suggested rules 426

safety 424 ISO 402

ISO (International Standards Organization) 85

ISO 9000 71

J

Joints

ball-and-socket 178 Cajon Ultra-Torr 182 Clear-Seal 176 European sizes 177

glass-threaded connections 183 inner 174

mercury seal 176 O-ring ball joint 180 O-ring joint 179 outer 174

preparations for use 196 Solv-Seal 181

522

storage and use 192, 194-196 Swagelok 181

K

Kelvin 147

Kevlar471

Kimax 13

Kovar 19, 367

Krytox 200

L

Langmuir 327 Lead crystal 2, 11

Leak detection 431^467 determination of a leak 433 false leaks 433^35

helium leak detection, see also Helium leak detection 454- 466

isolation 442-444

Pirani or thermocouple gauges 452 probe gases and liquids 444

real leaks 435-442 repairing leaks 466 seven sources 431—432 soap bubbles 451 Tesla coil 446-451

limitations 447

using probe gases 450 virtual leaks 396, 436, 438,442,

467

Left-handed thread fittings 256 Length 71

krypton-86 72 meter 71 ruler 79

Liquid nitrogen 394, 484

M

Magdeburg hemispheres 326 Manometer 401, 407

reading 407

Index

Mass 72 kilogram 72

Prototype Kilogram 73 Mass, see Balances, mass McLeod gauge 325, 401, 409

advantages and disadvantages 409 cleaning 417

condensable vapors 416 reading 411-413 tipping 414

use 413

Mean free path 335 Measurement 65

accuracy 66 reliability 66 significant figures 77 uniformity 65

Measurement rules 76 Measuring (pipettes) 107 Mechanical pumps 343-354

backstreaming 390 belt-driven 346 belts and pulleys 354 changing oil 352

condensable vapors, see Condensable vapors

condensate trap 350 connection 349 direct-drive 346, 360

double-stage, see Mechanical pumps, two-stage

double-vane, see Mechanical pumps, two-stage

dry 347

dry nitrogen purge 356 efficiency and speeds 363 exhaust 350, 387

filter traps 350 fore pumps 371

gas ballast 345, 350, 356 maintenance 351

motor types 347 oils 358-362

chlorofluorocarbon oils 362

Index

perfluorinated polyether oils 362

phosphate ester oils 361 properties 358

piston pump 343 pump size 347 roughing pumps 371 scroll pump 347 single-stage 344, 346 single-vane 343 storage 362

traps

avoiding danger 357 traps, see also Traps two-stage 344, 346, 371 use 350

Meter stick 79 Metric System

Base units 68 Derived units 68

International Bureau of Weights

and Measures 68 international commerce 68 King Louis XVI 67 MKSA 68

Supplementary base units 68 Metric system (history) 66 Micrometer 80, 83-84

Micron (unit of vacuum measurement) 328

Millimeters of mercury (unit of vacuum measurement) 328

Millitorr (unit of vacuum measurement) 328

Mist traps, see Traps, mist Mohs' scale of hardness 23

Molecular sieves, see Traps, molecular Momentum transfer gauge 430

N

National Institute of Standards and Technology, see NIST

Natural rubber 459

523

Neon 12 Neoprene 460 Newman 327

NIST (National Institute of Standards

and Technology) 85 Nitrogen 253, 261, 262, 276 Nitrogen leak (dry) 356 NMR 483

Nollet 327

Noncondensable gases 385, 416, 455, 464

Non-polar solvents 239 Nonpolar solvents 234

benzene 239 ethane 239 hexane 239

o

Organic solvents 239 O-ring461

O-rings 58-63, 179 chemical Resistance 59 sizes 60

Outgassing 378, 431, 442

Outside-in technique, see Helium leak detection

Oxygen 253, 256, 261, 262, 269, 271, 276, 283

condensing within cold trap 394

PARAFILM "M"® 58

Parallax 78, 79, 93, 94

Partial pressure versus total pressure 363

Paniculate traps, see Traps, particulate Pascal, Blaise 326

Penning 327

Penning gauge, see also Ionization gauge 429

Pennyhead stoppers storage 195 Permeability 460, 461

524

Permeation 432 Pharmaceutical cylinder 87 Phase separation 5-7, 8

Philips gauge, see also Ionization gauge 429

Photosensitive glass 5

PIG (Philips Ionization Gauge), see also Ionization gauge 429

Pipettes 107-113

color coded bands 108 cotton plug 108 measuring 107, 111 non-blowout 108 serological 107, 112

volumetric transfer 107, 109 Pirani 327

Pirani gauge 420, 452 safety concerns 419

Polar solvents 234, 239 acetone 239 ethanol 239 isopropanol 239 methanol 239

methyl ethyl ketone 239 Polariscope 23, 36 Polycarbonate 90

Polymer resistance 493 Polymers

Effects of chemicals upon 497 Polyolefins 493

polyethylene 494 polyethylene, high-density 494 polyethylene, low-density 494 polymethylpentene 494 polypropylene/polyallomer 494 polystyrene 495

polyvinyl chloride 494 Pressure release valves 254

Probe gases and liquids 444-446, 455 Propane 253, 256, 261, 262, 269, 276,

279 Propane tank 480 Pumping speed 338 Pyrex 13

Index

Pyroceramic material 6

Q

Quartz, see Glass, quartz

R

Radiation/Absorption (temperature) 287

Reagent bottle (stopper plug) 178 Redhead 327

Regional Control Centers (RCCs) (Canadian) 273

Regulator 278-285 instillation 281 parts 278-281 purchasing 284 safety 283

single-stage 280, 284 two-stage 280, 283, 284

Rotary valves 189-191 storage 194

Roughing pumps, see also Mechanical pumps, roughing pumps 346

Round bottom flask support 470 Rubber stoppers 50

drilling 51-55

inserting glass tubing 56 removing glass tubing 57

Screw clamp 480 Seals

demountable 436 Separation traps (cross ref) 400 Serological (pipettes) 107 Silicon grease 27

Silicone 459

Silver soldering 488

Slush baths 304-309, 394,484 safety 306

Soft glass, see also Glass, soft glass 10 Stainless steel

Index

(type) 303 468 (type) 304L 468 Standard leak 457, 459

Stopcock grease 117, 196-203 (silicon-based) 117 applying 203

fluorocarbon (cleaning) 236 hydrocarbon 198 hydrocarbon (cleaning) 236 Krytox 200-203

silicone 198-200 silicone (cleaning) 236

Stopcocks 184,471 general tips 212 high-vacuum 184-187 leakage 208-211

merthiolate or prussian blue test 210

pencil test 209

rock or jiggle test 209 leaks, dealing with 211-212 misalignment 184

oblique 186 preparations for use 196

preventing from freezing (sticking) 204

regrind 211

storage and use 192-194 Teflon 187-189, 194 three-way 192

two-way 185

unfreezing (unsticking) 205-208 vacuum 193

Stopper plug 178

Stress Concentration Factor 24 Swagelok 405

Swagelok®, see Joints, Swagelok®

T

Teflon 496

Teflon Sleeve 203

Tefzel 496

Temperature 73, 144-170

525

air thermometer 74 calibration 74, 145 Celsius 75 centigrade 147

dilatometer (or bimetal coil) 147 expansion-based 150 Fahrenheit 74

gas or vapor at constant volume 147

Kelvin 75, 146 linear expansion 151

liquid-in-glass thermometer 147 platinum wire 148

Rankine 75

Reaumur 75 thermocouple 148, 161 volumetric expansion 151

Tesla coil, see also Leak detection, Tesla coil 446

Thermocouple gauge 422, 452 advantages and disadvantages 422 cleaning 423

safety concerns 419 Thermocouples 161-167 Thermometers 151

air bubbles 158 calibration 157 complete-immersion 153 expansion-based 150 hysteresis 156

lag 158

linear expansion 151 partial-immersion 153 pressure expansion 160

resistance thermometers 167-170 total-immersion 153

variations 155 volumetric expansion 151

Throughput (gas flow) 338 Time 75

cesium 133 76

Tip off (sample tube) 483-487 Toepler pumps 325, 385-386 Torch

526

gas-oxygen lighting 480 shutting off 482 using 482

poping 478, 481 premix torch 477 surface-mix 479 surfacemix 477 tips 479

Torr (unit of vacuum measurement) 328

Torricelli, Evangelista 325

Total pressure versus partial pressure 363

Tracer-probe technique see Helium leak detection

Transfer of energy 287 Transportation emergency assistance

plan (TEAP) 273 Traps 355, 386-401

coaxial 388, 390 cold 388, 389

dry ice 394

limiting moisture near top 395 maintenance (coolant level)

396

maintenance (emptying and cleaning) 398

orientation 391 proper use 391 condensing oxygen 394

freezing oxygen 372 liquid 401

mist 389, 390 molecular 388, 389 paniculate 388, 390 purposes for 387

separation traps 387, 399 types 388

u

Ultrasonic cleaners 238

Ultra-Torr fittings, see Joints, Cajon

Index

Ultra-Torr

UV-transmission. See Glass, high temperature and UV-transmission

Vacuum creating 333 dynamic 435

leak sources 431 outer space 324 perfect 323 pressure 328 static 435

units of pressure 328

Vacuum equipment, history 325-327 Vacuum gauges 402-431

accuracy 402 inaccuracy 403-404 ionization gauges 423 liquid 406

manometer, see Manometer McLeod gauge, see McLeod gauge mechanical 404

cleaning 405 thermocouple and pirani 419

thermocouple gauge, see Thermocouple gauge

Vacuum line contamination removal 356

Vacuum pumps 340-386 aspirator 341

mechanical, see also Mechanical pumps

Vacuum rack 469

Vacuum stopcocks, see Stopcocks high-vacuum

Vacuum systems aluminum 468 cadmium 468 copper 468 copper OFHC 468

design (glass) 468-472 how to use 325

Index

pricing and costs 324 shutting down 374, 376, 399 starting up 357

system power failure 442 water vapor 377

zinc 468

Valve, see also Stopcocks and Rotational valves

Vapor pressure 332 Vapor pump

see Diffusion pump Vapors versus gases 329 Vernier (calibration) 81

Virtual leaks, see Leak detection, Virtual leaks

Volume 73, 85, 85-118 Archimedes principle 100 buoyancy (effect) 99 calibration 95

Calibration tolerance ware 89 Certified Ware 89

Class A ware 89 Class B ware 89

correcting volumetric readings 97- 101

cubic decimeter 73

527

effects of alkaline materials 95 general purpose ware 89

level of accuracy 96 paper cuff 94 reproducibility 96 special tolerance ware 89 Type I, Class A 91

Type I, Class B 91 Type II91

Volume containers polycarbonate 90 polymethylpentene 90 polypropylene 90 polystyrene 90

Volumetric flasks 101-104 caps 102

tolerances 101

Volumetric transfer (pipettes) 107 Vycor, see Glass, Vycor

w

Weight and mass 118-120 Weight, see Balances, weight Welding (glass) 490