《CHEMICAL ANALYSIS OF INDUSTRIAL SOLVENTS》求取 ⇩

Ⅰ.Introduction and Sampling1

1.Introduction1

(a)Definitions2

(b)Classification3

2.Sampling4

(a)Accuracy of Sampling4

(b)Sampling Instruments5

(c)Sampling Methods8

From Loaded Tank Car or Other Large Vessel8

From Barrels and Drums8

Sampling Data9

(d)Preparation of Sample9

(e)Final Disposition of Sample10

3.Amount of Solvent in a Tank Car or Drum10

Gauging of Quantity of Solvent in a Tank Car10

Volume of Solvent in 55-Gallon Drum13

Ⅱ.Physical and General Methods17

1.Determination of Specific Gravity17

(a)Balances18

Westphal Balance18

Specific Gravity Balance20

(b)Pycnometers20

Pycnometer20

(c)Specific Gravity Spindles24

Hydrometer24

(d)A.P.I.Gravity28

2.Boiling Point and Boiling Range29

At Barometric Pressure30

At Reduced Pressure32

U.S.P.Method Ⅰ33

U.S.P.Method Ⅱ34

3.Vapor Pressure and Evaporation Rate35

(a)Vapor Pressure35

Reid Method36

(b)Evaporation Rate38

Watch Glass Method41

Dietrich Variation41

Porcelain Dish Method41

Hofmann Dish Method41

Filter Paper Method42

Bent and Wik Method42

Jolly Balance Method42

Evap-O-Rotor45

4.Nonvolatile Matter45

5.Water46

Turbidity Method46

Immiscible Solvent Distillation Method47

Refractometer Method48

Smith and Bryant Method48

Fischer Method49

6.Solubility of Water in Solvent and of Solvent in Water53

Solubility of Water in Solvent53

Solubility of Solvent in Water54

7.Acidity54

(a)Total Titratable Acidity54

(b)pH55

8.Total Titratable Alkalinity55

9.Ash56

10.Residual Odor56

11.Extractions and Separations57

(a)Partition Law57

(b)Apparatus58

Jacobs-Singer Separatory Flask58

Continuous Extractors60

Countercurrent Distribution61

12.Iodine Value62

Hanus Iodine Value62

Wijs Iodine Value63

13.Bromine Number64

Lewis and Bradstreet Modification64

Electronic Method65

14.Sulfur Test66

15.Doctor Test67

16.Corrosion Tests68

Copper Corrosion Test69

Copper Strip Corrosion Test for Oils69

Copper Strip Corrosion Test for Gasoline70

Copper Strip Corrosion Test for Petroleum Naphtha70

Steel Strip Corrosion Tests for Steam-Turbine Oils70

Mercury Corrosion Test71

17.Acid Heat Test71

18.Aniline Point and Mixed Aniline Point71

Mixed Aniline Point71

19.Kauri Butanol Number72

20.Dimethyl Sulfate Value72

21.Butyl Acetate Dilution Ratio73

22.Heptane Number74

Ⅲ.Physical Chemical Methods75

1.Refractometry75

Abbe Refraetometer75

Dispersion78

Immersion Refraetometer79

Molecular Refraction80

2.Color and Colorimetry83

(a)Color84

Hue84

Brightness84

Saturation84

(b)Color Measurement85

Nessler Tubes85

Tag-Robinson Colorimeter85

Union Colorimeter86

Hellige Comparator86

Saybolt Chromometer86

Klett Colorimeter86

Lovibond Tintometer87

3.Folarimetry87

Polarimeter89

Angular Rotation90

Specific Rotation90

Molecular Rotation91

4.Viscometry92

Absolute Viscosity92

Kinematic Viscosity92

Fluidity93

Viscometcrs93

(a)Capillary Tube Viscometers93

Ostwald Viscometers94

Bingham and Jackson Method94

Ubbelhode Yiscometer97

(b)Orifice Viscometers98

(c)Falling Weight Viscometers99

Falling Ball Viscometer99

(d)Torsion Viseometers100

(e)Bubble Viscometers102

5.Surface Tension and Interfacial Tension102

Types of Measurement103

Ring Method103

Stalagmometer105

6.Flash Point105

Tag Closed Tester106

Tag Open Cup Tester109

Pensky-Martens Closed Tester110

Cleveland Open-Cup Tester111

7.Congealing Point111

8.Melting Point111

9.Blush Resistance113

10.Dilution Ratio114

Ⅳ.Physiological Effects of Industrial Solvents117

1.Effect of Solvents on the Human System117

Saturated Hydrocarbons118

Unsaturated Aliphatic Hydrocarbons118

Cyclic Hydrogenated Hydrocarbons118

Aromatic Hydrocarbons119

Chlorinated Hydrocarbons119

Alcohols119

Glycols and Alcohol-Ethers119

Aldehydes and Ketones119

Ethers119

Acids119

Esters119

Aniline and Coal-Tar Derivatives120

2.Organic Solvents as Agents causing Dermatitis120

3.Toxicity of Organic Solvents121

4.Probable Safe Concentration Limits of Exposure for Solvent Vapors122

Ⅴ.General Methods for the Determination of Solvent Vapors131

1.Explosive Limits132

2.Detectors133

(a)Combustion Type Detector133

Jones Gas Detector133

(b)Catalytic Type Detectors133

U.C.C.Methane Detector133

M.S.A.Detectors134

Davis Vapotester135

3.Adsorption Methods135

(a)Adsorption by Silica Gel135

(b)Adsorption on Equilibrated Activated Charcoal138

(c)Adsorption and Distillation140

(d)Adsorption and Extraction140

4.Physical Chemical Methods140

(a)Gas Interferometer140

(b)Conductivity Methods142

(c)Absorption of Radiant Energy142

Quartz Spectrophotometer143

(d)Vapor Pressure144

(e)Other Physical Methods145

Ⅵ.General Methods for the Analysis of Solvent Mixtures147

1.Fractional Distillation147

2.Analysis of Solvent Mixtures149

Goldman Method150

Volatile Solvents and Thinners of Lacquers154

Weber's Method156

I.G.Method159

3.Analysis by Functional Groups163

(a)Chemical Methods163

(b)Physical Methods164

Electrical Measurements165

Polarographic Methods165

Amperometric Measurements166

Potentiometric Measurements166

Conductometric Measurements168

Polarized Electrode Titrations168

High-Frequency Titrations169

Ⅶ.Paraffin and Unsaturated Aliphatic Hydrocarbons and Turpentine171

A.Paraffin Hydrocarbons and Petroleum Distillates171

1.Flammability and Vapor Pressure171

(a)Flammability Ratings171

(b)Vapor Pressure171

2.Gasoline173

3.Petroleum Benzine174

(a)A.S.C.Requirements175

(b)U.S.P.Requirements175

4.Petroleum Distillates176

(a)Petroleum Spirits or Mineral Spirits177

(b)White Spirit178

(c)Paint Benzine179

(d)Stoddard Solvent179

(e)Varnish Makers' and Painters'Naphtha179

(f)Heavy Petroleum Spirits179

(g)Kerosene180

(h)Other Petroleum Distillates180

(i)Benzene Substitute180

5.Analysis of Petroleum Products and Significance of Various Tests180

(a)Gravity A.P.I.181

(b)Specific Gravity181

(c)Flash and Fire Points181

(d)Sulfur Test181

(e)Doctor Test182

(f)Odor Test182

(g)Color Test182

(h)Copper Strip Corrosion Test182

(i)Steel Strip Corrosion Test183

(j)Acid Heat Test183

(k)Aniline Point183

(l)Kauri Butanol Number184

(m)Distillation Test184

(n)Dimethyl Sulfate Value184

(o)Butyl Acetate Dilution Ratio184

(p)Evaporation Test185

(q)Iodine Number185

(r)Bromine Number185

(s)Standard Distillation Method185

(t)Separation of Paraffin from Aromatic Hydrocarbons192

(u)Aromatic Compounds in Benzine194

6.Mineral Oil195

(a)Light Mineral Oil196

B.Turpentine and Terpene Hydrocarbons196

1.Turpentine196

(a)N.F.Requirements197

(b)Analysis198

2.Dipentene204

Ⅷ.Benzene,Aromatic and Hydrocyclic Hydrocarbons205

A.Benzene Homologues205

1.Benzene205

(a)Properties205

(b)A.C.S.and U.S.P.Requirements206

(c)Industrial Benzol207

(d)Separation and Detection211

(e)Determination213

2.Toluene221

(a)A.C.S.and U.S.P.Requirements221

(b)Industrial Toluene223

(c)Detection224

(d)Determination224

3.Xylene227

(a)A.C.S.and U.S.P.Requirements227

(b)Industrial Xylene228

(c)Detection and Determination228

4.Solvent Naphtha229

5.Ethylbenzene232

6.Cumene232

7.Mixtures232

(a)Aromatic Hydrocarbons232

(b)Paraffins in Aromatic Hydrocarbons233

(c)Benzene and Toluene234

(d)Benzene and Toluene in Solvent Mixtures236

(e)Toluene-n-Butyl Alcohol-Water Mixtures238

B.Cyclic Hydrocarbons240

1.Cyclohexane240

2.Cyclohexene240

3.Styrene240

C.Condensed Ring Hydrocarbons241

1.Tetralin241

2.Decalin242

3.Mixtures243

Ⅸ.Halogenated Hydrocarbons247

Beilstcin Test247

Sulfur Lamp Method248

Fajans Method250

Goldman Modification251

A.Chlorinated Hydrocarbons252

1.Dichloromethane252

(a)U.S.P.Requirements252

(b)Detection and Determination253

2.Chloroform253

(a)A.C.S.and U.S.P.Requirements253

(b)Detection and Determination255

3.Carbon Tetrachloride256

(a)A.C.S.and U.S.P.Requirements257

(b)Detection and Determination258

4.Ethylene Dichloride(1,2-Dichloroethane)261

5.Tctrachloroethane261

6.Pentachloroethane262

7.Dichloroethylene263

8.Trichloroethylene263

(a)U.S.P.Requirements264

(b)Detection and Determination264

9.Tetrachloroethylene267

(a)U.S.P.Reqnirements267

(b)Detection and Determination268

10.Allyl Chloride269

11.Chloroprene270

12.Mixtures270

(a)Chlorinated Hydrocarbons and Alcohol-Ester Mixtures270

(b)Carbon Tetrachloride,Dichloromethane,and Trichloro-ethylene271

(c)Chlorinated Hydrocarbons and Benzine and Benzene271

(d)Carbon Tetrachloride in Chloroform272

(e)Dichloroethylene in other Chlorinated Hydrocarbons273

(f)Trichloroethylene in other Chlorinated Hydrocarbens273

13.Chlorobenzene273

14.Dichlorobenzene274

B.Brominated Hydrocarbons275

1.Methyl Bromide275

(a)Detection275

(b)Determination275

2.Ethyl Bromide277

3.Ethylene Dibromide278

(a)Detection278

(b)Determination278

C.Chlorine-Bromine Compounds278

Monobromomonochloromethane278

D.Oxyhalogenated Hydrocarbons279

1.Dichloroethyl Ether279

Detection and Determination279

2.Ethylene Chlorohydrin280

3.Propylene Chlorohydrin281

4.Mixtures281

Ethylene and Propylene Chlorohydrins281

Ⅹ.Alcohols283

Acethydroxamic Acid Test283

p-Nitrobenzoie Acid Esters283

Xanthate Reaction284

Acetyl Value286

Smith and Bryant Method288

Hydroxyl Value289

Primary Alcohols290

Oxidation to Acid291

Nonaqueous Solvent Titration292

1.Methyl Alcohol293

(a)A.C.S.and U.S.P.Requirements293

(b)Detection295

(c)Determination297

2.Ethyl Alcohol298

(a)A.C.S.and U.S.P.Requirements298

(b)Detection300

(c)Determination302

3.n-Propyl Alcohol304

(a)U.S.P.Requirements304

(b)Detection304

4.Isopropyl Alcohol305

(a)U.S.P.Requirements305

(b)A.S.T.M.Specifications305

(c)Detection306

(d)Determination307

5.n-Butyl Alcohol307

(a)U.S.P.Requirements308

(b)A.S.T.M.Requirements308

(c)Detection and Determination308

6.Isobutyl Alcohol309

(a)U.S.P.Requirements309

(b)Detection310

7.sec-Butyl Alcohol310

8.Amyl Alcohol and Isoamyl Alcohol311

(a)U.S.P.and A.C.S.Requirements311

(b)Synthetic Amyl Alcohol312

(c)Detection312

(d)Determination313

9.Higher Alcohols315

10.Capryl Alcohol316

11.Allyl Alcohol316

12.Cyclohexanol317

(a)Detection317

(b)Determination318

13.Methylcyclohexanol319

14.Benzyl Alcohol319

15.Alcohol Mixtures320

(a)Ethyl and Methyl Alcohol320

(b)Ethyl and Isopropyl Alcohol322

(c)Ethyl and Butyl Alcohol323

(d)Methyl Alcohol and Formaldehyde324

(e)Alcohols and Aldehydes324

(f)Alcohols in Motor Fuel325

Ⅺ.Glycols,Polyhydroxy Compounds,and Ethers327

A.Glycols327

Cyclopentanol Reaction327

Acetyl Value327

1.Ethylene Glycol328

(a)Specifications329

(b)Detection329

(c)Determination330

2.Propylene Glycol330

(a)U.S.P.Requirements330

(b)Specifications331

(c)Detection and Determination332

3.Butylene Glycol332

4.Mixtures332

(a)Ethylene Glycol and 1,2-Propylene Glycol332

B.Alcohol-Ethers333

Dichromate Oxidation333

1.Ethylene Glycol Monomethyl Ether335

2.Ethylene Glycol Monoethyl Ether336

3.Ethylene Glycol Monobutyl Ether337

4.Diethylene Glycol337

5.Diethylene Glycol Monoethyl Ether338

6.Methoxybutanol339

7.Mixtures339

(a)Glycol and Glycol Ethers339

(b)Glycol,Propylene Glycol,Glycerol,and Diethylene Glycol340

(c)Glycol,Glycerol,and Propylene Glycol342

C.Polyhydroxy Alcohols343

1.Glycerol343

(a)U.S.P.and A.C.S.Requirements344

(b)Detection346

(c)Determination346

D.Ethers353

1.Ethyl Ether353

(a)A.C.S.and U.S.P.Requirements354

(b)Absolute Ether355

(c)Determination356

(d)Ether and Ethyl Alcohol356

2.Isopropyl Ether357

3.Vinyl Ether358

(a)U.S.P.Requirements358

(b)Detection and Determination359

4.Dioxane360

(a)U.S.P.Requirements and Commercial Specifications360

(b)Detection360

Ⅻ.Acids and Esters363

A.Acids363

1.Acetic Acid363

(a)U.S.P.and A.C.S.Requirements364

(b)Detection365

(c)Determination366

2.Acetic Anhydride366

(a)A.C.S.and U.S.P.Requirements367

(b)Detection and Determination368

3.Formic Acid368

(a)A.C.S.and U.S.P.Requirements369

(b)N.F.Requirements370

(c)Detection371

(d)Determination372

4.Propienic Acid372

5.Butyric Acid373

6.Lactic Acid373

(a)N.F.Requirements374

(b)Detection375

(c)Determination376

7.Mixtures376

(a)Fatty Acid Mixtures376

(b)Acids and Aldehydes377

B.Esters377

General Saponification Method377

Saponifieation Value378

Ester Value379

By Electrical Methods380

Special Procedures381

Saponification Equivalents of High-Boiling381

1.Methyl Acetate383

2.Ethyl Acetate384

(a)U.S.P.Requirements384

(b)85 to 88 Per Cent Grade385

(c)N.F.Requirements385

(d)Detection and Determination386

3.Propyl Acetate386

4.Isopropyl Acetate386

(a)95 Per Cent Grade387

(b)85 to 88 Per Cent Grade387

(c)Detection and Determination388

5.Butyl Acetate388

(a)88 to 92 Per Cent Grade388

(b)Determination389

6.Isobutyl Acetate389

7.see-Butyl Acetate389

8.Amyl Acetate and Isoamyl Acetate390

(a)U.S.P.Requirements391

(b)Synthetic Amyl Acetate391

(c)Fusel Oil Amyl Acetate392

(d)Determination392

9.see-Amyl Acetate392

10.Butyl and Amyl Acetate Mixtures393

11.Methyl Formate393

12.Ethyl,Butyl,and Amyl Formates394

13.Butyl Propionate395

14.Ethyl Carbonate395

(a)Specifications396

(b)Deternfination396

15.Ethyl Oxalate396

16.Triacetin397

(a)Detection397

(b)Determination398

17.Phthalates399

18.Ester Mixtures400

(a)Esters and Aldehydes401

(b)Esters and Oils402

(c)Esters of Acids not Readily Volatile with Steam403

C.Polyfunctional Esters403

1.Ethyl Acetoacetate403

(a)Specifications404

(b)Determinations404

2.Ethyl Lactate405

3.Ethyl Chloroformate405

4.Ethylene Glycol Monomethyl Ether Acetate406

5.Ethylene Glycol Monoethyl Ether Acetate407

D.Esters of Inorganic Acids407

1.Trio-o-cresyl Phosphate407

(a)A.S.T.M.Specifications408

(b)Determination410

2.Ethyl Silicate411

ⅩⅢ.Ketones and Aldehydes413

(a)Detection413

Hydrazide Reaction413

(b)Determination413

Ripper's Method413

Bisulfite Absorption Method415

Neutral Sulfite Absorption Method417

Hydroxylamine Method417

Stillman-Reed Alkaline Hydroxylamine Method418

Hydroxylamine-Pyridine Method419

Iodometric Phenylhydrazine Method422

Phenylhydrazine Method423

Silver Oxide Method423

A.Ketones423

1.Acetone423

(a)A.C.S.and U.S.P.Requirements424

(b)A.S.T.M.Specifications425

(c)Detection425

(d)Determination426

2.Ethyl Methyl Ketone428

3.Methyl Propyl Ketone429

4.Butyl Methyl Ketone430

5.Isobutyl Methyl Ketone430

6.Mesityl Oxide431

(a)Detection and Determination431

7.Cyclohexanone432

(a)Detection432

(b)Determination433

8.Methylcyclohexanone433

9.Isophorone433

B.Alcohol Ketones434

Diacetone Alcohol434

(a)Detection435

(b)Determination435

C.Dicarbonyls435

1.Acetylacetone435

2.Acetonylacetone437

D.Aldehydes438

1.Formaldehyde438

(a)U.S.P.Requirements for Formaldehyde Solution439

(b)Detection439

(c)Determination440

2.Acetaldehyde445

(a)Specifications446

(b)Detection446

(c)Determination446

3.Furfural447

(a)Detection448

(b)Determination449

4.Benzaldehyde449

(a)N.F.Requirements449

(b)Determination450

5.Mixtures451

(a)Aldehydes and Ketones451

(b)Carbonyl Compounds and Acids452

E.Acetals452

Acetal453

ⅩⅣ.Nitrogen and Sulfur Compounds455

Kjeldahl-Gunning-Arnold Method456

Pregl-Parnas-Wagner Micro Method457

A.Aliphatic Amino Compounds459

Nonaqueous Solvent Titration459

1.Ethylamine460

2.Propylamines461

3.Butylamines461

4.Amylamines462

5.Dialkylamines462

6.Mixtures of Amines463

B.Aminoalcohols(Ethanolamines)465

1.Ethanolamine and Diethanolamine465

2.Triethanolamine466

C.Nitroparaffins467

1.Nitromethane467

2.Nitroethane468

3.Nitropropanes468

D.Chloronitroparaffins469

1.1,1-Dichloro-1-nitroethane469

(a)Determination469

2.1-Chloro-1-nitropropane470

(a)Determination470

E.Nitriles471

Acrylonitrile471

(a)Determination471

F.Aromatic Nitrogen Compounds473

1.Nitrobenzene473

(a)Detection473

(b)Determination474

2.Aniline474

(a)A.C.S.and U.S.P.Requirements475

(b)Detection475

(c)Determination475

G.Heteroeyclic Compounds476

1.Pyridine476

(a)U.S.P.Requirements476

(b)Detection477

(c)Determination477

2.Morpholine480

(a)Detection481

(b)Determination481

3.Ethylenimine481

4.Pyrrole482

H.Sulfur Compounds483

1.Carbon Disulfide483

(a)A.C.S.Requirements483

(b)Detection484

(c)Determination484

2.Thioglyeolic Acid485

3.Allyl Isothiocyanate486

Index489

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