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PRACTICAL LABORATORY INFORMATION 11.31 11.4.2.7 Time of Analysis. The retention time required to perform a separation is given by t 16Rs 2 R 2 (1 k) 3 H 2 1 (k) u Now t R is a minimum when k 2, that is, when tR 3t M. There is little increase in analysis time when k lies between 1 and 10. A twofold increase in the mobile-phase velocity roughly halves the analysis time (actually it is the ratio H/u which influences the analysis time). The ratio H/u can be obtained from the experimental plate height/velocity graph. 11.4.2.8 High-Performance Liquid Chromatography. Typical performances for various experimental conditions are given in Table 11.15. The data assume these reduced parameters: h 3, v 4.5. The reduced plate height is The reduced velocity of the eluent is H L h d Nd ud v D p p p Ldp t D M M M In these expressions, d p is the particle diameter of the stationary phase that constitutes one plate height. D M is the diffusion coefficient of the solute in the mobile phase. TABLE 11.15 Typical Performances in HPLC for Various Conditions Performances N t M ,s Column parameters L, cm d p , m P, atm (psi) 2 500 30 2.3 3 18.4 (270) 2 500 30 3.7 5 18.4 (270) 2 500 30 7.5 10 18.4 (270) 5 000 30 4.5 3 74 (1088) 5 000 30 7.5 5 74 (1088) 5 000 30 15.0 10 74 (1088) 10 000 30 9.0 3 300 (4410) 10 000 30 15.0 5 300 (4410) 10 000 30 30.0 10 300 (4410) 10 000 30 9.0 3 300 (4410) 10 000 60 9.0 3 150 (2200) 10 000 90 9.0 3 100 (1470) 15 000 90 2.3 3 223 (3275) 15 000 120 2.3 3 167 (2459) 11 100 30 10.0 3 369 (5420) 11 100 37 10.0 3 300 (4410) 11 100 101 10.0 3 100 (1470) 27 800 231 25.0 3 300 (4410) Assumed reduced parameters: , These are optimum values from a graph of reduced plate height versus reduced h 3 v 4.5. linear velocity of the mobile phase.
11.32 SECTION 11 11.4.3 Ion-Exchange (Normal Pressure, Columnar) Ion-exchange methods are based essentially on a reversible exchange of ions between an external liquid phase and an ionic solid phase. The solid phase consists of a polymeric matrix, insoluble, but permeable, which contains fixed charge groups and mobile counter ions of opposite charge. These counter ions can be exchanged for other ions in the external liquid phase. Enrichment of one or several of the components is obtained if selective exchange forces are operative. The method is limited to substances at least partially in ionized form. 11.4.3.1 Chemical Structure of Ion-Exchange Resins. An ion-exchange resin usually consists of polystyrene copolymerized with divinylbenzene to build up an inert three-dimensional, crosslinked matrix of hydrocarbon chains. Protruding from the polymer chains are the ion-exchange sites distributed statistically throughout the entire resin particle. The ionic sites are balanced by an equivalent number of mobile counter ions. The type and strength of the exchanger is determined by these active groups. Ion-exchangers are designated anionic or cationic, according to whether they have an affinity for negative or positive counter ions. Each main group is further subdivided into strongly or weakly ionized groups. A selection of commercially available ion-exchange resins is given in Table 11.16. The cross-linking of a polystyrene resin is expressed as the proportion by weight percent of divinylbenzene in the reaction mixture; for example, “8” for 8 percent cross-linking. As the percentage is increased, the ionic groups come into effectively closer proximity, resulting in increased selectivity. Intermediate cross-linking, in the range of 4 to 8 percent, is usually used. An increase in cross-linking decreases the diffusion rate in the resin particles; the diffusion rate is the ratecontrolling step in column operations. Decreasing the particle size reduces the time required for attaining equilibrium, but at the same time decreases the flow rate until it is prohibitively slow unless pressure is applied. In most inorganic chromatography, resins of 100 to 200 mesh size are suitable; difficult separations may require 200 to 400 mesh resins. A flow rate of 1 mL · cm 2 · min 1 is often satisfactory. With HPLC columns, the flow rate in long columns of fine adsorbent can be increased by applying pressure. 11.4.3.1.1 Macroreticular Resins. Macroreticular resins are an agglomerate of randomly packed microspheres which extend through the agglomerate in a continuous non-gel pore structure. The channels throughout the rigid pore structure render the bead centers accessible even in nonaqueous solvents, in which microreticular resins do not swell sufficiently. Because of their high porosity and large pore diameters, these resins can handle large organic molecules. 11.4.3.1.2 Microreticular Resins. Microreticular resins, by contrast, are elastic gels that, in the dry state, avidly absorb water and other polar solvents in which they are immersed. While taking up solvent, the gel structure expands until the retractile stresses of the distended polymer network balance the osmotic effect. In nonpolar solvents, little or no swelling occurs and diffusion is impaired. 11.4.3.1.3 Ion-Exchange Membranes. Ion-exchange membranes are extremely flexible, strong membranes, composed of analytical grade ion-exchange resin beads (90%) permanently enmeshed in a poly(tetrafluoroethylene) membrane (10%). The membranes offer an alternative to column and batch methods, and can be used in many of the same applications as traditional ion exchange resins. Three ion-exchange resin types have been incorporated into membranes: AG 1-X8, AG 50W-X8, and Chelex 100. 11.4.3.2 Functional Groups Sulfonate exchangers contain the group 9SO , which is strongly acidic and completely disso- 3 ciated whether in the H form or the cation form. These exchangers are used for cation exchange.
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LANGE'S HANDBOOK OF CHEMISTRY John
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Grateful acknowledgment is hereby m
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PREFACE TO FIFTEENTH EDITION This n
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PREFACE TO FIFTEENTH EDITION ix inv
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xii PREFACE TO FOURTEENTH EDITION l
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PREFACE TO FIRST EDITION This book
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For the detailed contents of any se
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1.2 SECTION 1 is derived from the G
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1.4 SECTION 1 rather than methylide
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1.6 SECTION 1 Styrene Toluene Xylen
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1.8 SECTION 1 TABLE 1.2 Fused Polyc
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1.10 SECTION 1 1.1.1.6 Bridged Hydr
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1.12 SECTION 1 TABLE 1.4 Suffixes f
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1.14 SECTION 1 TABLE 1.5 Trivial Na
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1.16 SECTION 1 TABLE 1.6 Trivial Na
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1.18 SECTION 1 Selection of the pri
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1.20 SECTION 1 attached to one anot
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1.22 SECTION 1 When side chains of
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1.24 SECTION 1 heterocyclic structu
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1.26 SECTION 1 Bivalent radicals of
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1.28 SECTION 1 Complex linear polya
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1.30 SECTION 1 TABLE 1.11 Names of
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1.32 SECTION 1 hydroxyamino- to the
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1.34 SECTION 1 may be named (1) by
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1.36 SECTION 1 Examples are methyl
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1.38 SECTION 1 tuted acid, respecti
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1.40 SECTION 1 FIGURE 1.2 Newman pr
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1.42 SECTION 1 from the ring are kn
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1.44 SECTION 1 FIGURE 1.11 Two isom
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1.46 SECTION 1 Chiral Center. The c
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1.48 SECTION 1 FIGURE 1.15 Isomers
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1.50 SECTION 1 entries to bring tog
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1.52 SECTION 1 TABLE 1.13 Names and
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1.60 SECTION 1 TABLE 1.14 Empirical
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2.2 SECTION 2 2.3.6 Student’s Dis
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2.4 SECTION 2 TABLE 2.1 Fundamental
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2.6 SECTION 2 TABLE 2.1 Fundamental
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2.8 SECTION 2 TABLE 2.2 Physical an
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2.10 SECTION 2 TABLE 2.2 Physical a
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2.24 SECTION 2 TABLE 2.3 Mathematic
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2.26 SECTION 2 TABLE 2.6 Abbreviati
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2.36 SECTION 2 TABLE 2.7 Conversion
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2.54 SECTION 2 TABLE 2.8 Temperatur
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2.66 SECTION 2 2.1.1 Conversion of
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2.68 SECTION 2 Oleometer. A hydrome
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2.70 SECTION 2 Example 3. 25 1.2500
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2.72 SECTION 2 TABLE 2.9 Barometer
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2.74 SECTION 2 TABLE 2.9 Barometer
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2.76 SECTION 2 TABLE 2.10 Barometri
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2.78 SECTION 2 TABLE 2.12 Reduction
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2.80 SECTION 2 TABLE 2.12 Reduction
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2.82 SECTION 2 TABLE 2.13 Viscosity
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2.84 SECTION 2 TABLE 2.14 Conversio
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2.86 SECTION 2 TABLE 2.15 Hydromete
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2.88 SECTION 2 TABLE 2.17 Correctio
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2.90 SECTION 2 TABLE 2.18 Pressure
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2.96 SECTION 2 TABLE 2.20 Values of
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2.98 SECTION 2 TABLE 2.21 Transmitt
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2.100 SECTION 2 TABLE 2.21 Transmit
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2.102 SECTION 2 2.2 MATHEMATICAL TA
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2.104 SECTION 2 TABLE 2.23 Derivati
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2.106 SECTION 2 TABLE 2.24 Integral
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2.108 SECTION 2 TABLE 2.24 Integral
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2.110 SECTION 2 Regular Polygon of
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2.112 SECTION 2 A h[0.4(y y ) 1.
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2.114 SECTION 2 2.2.3.1 Signs of th
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2.116 SECTION 2 x2 x3 x4 x5 ln(1 x
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2.118 SECTION 2 2.3.2 Errors in Qua
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2.120 SECTION 2 The breadth or spre
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2.122 SECTION 2 TABLE 2.26b Areas U
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2.124 SECTION 2 The distribution of
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2.126 SECTION 2 Should there be mor
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2.128 SECTION 2 Example 10 Six samp
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2.130 SECTION 2 2.3.9 The F Statist
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TABLE 2.29 F Distribution (Continue
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2.134 SECTION 2 mathematical treatm
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2.136 SECTION 2 The confidence limi
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2.138 SECTION 2 situation where rel
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3.2 SECTION 3 The alphabetical orde
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3.4 SECTION 3 When it is required t
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3.6 SECTION 3 PO phosphoryl SeO sel
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3.8 SECTION 3 3.1.5 Acids 3.1.5.1 A
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3.10 SECTION 3 3.1.6.6 Multiplicati
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3.12 SECTION 3 3.2 PHYSICAL PROPERT
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TABLE 3.2 Physical Constants of Ino
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3.62 SECTION 3 TABLE 3.3 Synonyms a
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SECTION 4 PROPERTIES OF ATOMS, RADI
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4.3 Fermium Fm 100 [Rn] 5f 12 7s 2
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Silver (argentum) Ag 47 [Kr] 4d 10
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PROPERTIES OF ATOMS,RADICALS,AND BO
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PROPERTIES OF ATOMS, RADICALS, AND
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SECTION 5 PHYSICAL PROPERTIES 5.1 S
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PHYSICAL PROPERTIES 5.3 5.1 SOLUBIL
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TABLE 5.1 Solubility of Gases in Wa
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TABLE 5.1 Solubility of Gases in Wa
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TABLE 5.2 Solubilities of Inorganic
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formateBa(CHO 2 ) 2 26.2 28.0 29.9
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(III) sulfateCe 2 (SO 4 ) 3 ·9H 2
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iodidePbI 2 0.044 0.056 0.069 0.090
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Nickel sulfateNiSO 4 ·6H 2 O (pale
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Praseodymium bromatePr(BrO 3 ) 3 55
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formate NaCHO 2 43.9 62.5 81.2 102
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Uranyl nitrate UO 2 (NO 3 ) 2 98 10
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PHYSICAL PROPERTIES 5.25 TABLE 5.3
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PHYSICAL PROPERTIES 5.57 5.3 BOILIN
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TABLE 5.12 Ternary Azeotropic Mixtu
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TABLE 5.12 Ternary Azeotropic Mixtu
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PHYSICAL PROPERTIES 5.83 5.4 FREEZI
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PHYSICAL PROPERTIES 5.87 5.5 DENSIT
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PHYSICAL PROPERTIES 5.89 dt Dt P
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PHYSICAL PROPERTIES 5.135 5.6.1 Ref
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PHYSICAL PROPERTIES 5.137 where the
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PHYSICAL PROPERTIES 5.139 5.7 COMBU
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Temperature, C Substance 40 20 0 20
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PHYSICAL PROPERTIES 5.171 This equa
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SECTION 6 THERMODYNAMIC PROPERTIES
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THERMODYNAMICPROPERTIES 6.3 6.1.1.2
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THERMODYNAMICPROPERTIES 6.5 A gener
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THERMODYNAMICPROPERTIES 6.7 TABLE 6
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THERMODYNAMICPROPERTIES 6.9 TABLE 6
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THERMODYNAMICPROPERTIES 6.11 TABLE
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THERMODYNAMIC PROPERTIES 6.21 TABLE
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THERMODYNAMIC PROPERTIES 6.101 TABL
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THERMODYNAMIC PROPERTIES 6.143 The
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SECTION 7 SPECTROSCOPY 7.1 X-RAY ME
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SPECTROSCOPY 7.3 TABLE 7.1 Waveleng
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SPECTROSCOPY 7.9 TABLE 7.3 Critical
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SPECTROSCOPY 7.11 TABLE 7.4 X-Ray E
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SPECTROSCOPY 7.13 Emission line K 1
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SPECTROSCOPY 7.15 TABLE 7.7 Analyzi
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SPECTROSCOPY 7.17 TABLE 7.8 Mass Ab
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SPECTROSCOPY 7.19 TABLE 7.9 Electro
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SPECTROSCOPY 7.21 TABLE 7.11 Absorp
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SPECTROSCOPY 7.23 TABLE 7.13 Solven
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SPECTROSCOPY 7.25 7.3 FLUORESCENCE
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SPECTROSCOPY 7.27 TABLE 7.16 Fluore
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SPECTROSCOPY 7.29 TABLE 7.18 Detect
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SPECTROSCOPY 7.35 TABLE 7.19 Sensit
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SPECTROSCOPY 7.37 TABLE 7.19 Sensit
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SPECTROSCOPY 7.39 In terms of m ,
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SPECTROSCOPY 7.41 The ionization co
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SPECTROSCOPY 7.67 TABLE 7.28 Infrar
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7.69
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SPECTROSCOPY 7.71 7.6 RAMAN SPECTRO
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SPECTROSCOPY 7.73 TABLE 7.30 Raman
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SPECTROSCOPY 7.89 7.7 NUCLEAR MAGNE
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SPECTROSCOPY 7.91 TABLE 7.41 Nuclea
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SPECTROSCOPY 7.93 TABLE 7.42 Proton
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SPECTROSCOPY 7.95 TABLE 7.44 Estima
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SPECTROSCOPY 7.97 TABLE 7.46 Proton
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SPECTROSCOPY 7.99 TABLE 7.48 Solven
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SPECTROSCOPY 7.101 TABLE 7.49 Carbo
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SPECTROSCOPY 7.107 TABLE 7.56 One-B
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SPECTROSCOPY 7.113 TABLE 7.63 Nitro
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SPECTROSCOPY 7.115 TABLE 7.64 Nitro
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SPECTROSCOPY 7.117 TABLE 7.69 Fluor
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SPECTROSCOPY 7.119 TABLE 7.72 Silic
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SPECTROSCOPY 7.121 TABLE 7.73 Phosp
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SPECTROSCOPY 7.123 TABLE 7.74 Phosp
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SPECTROSCOPY 7.125 when z 3 and y
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SPECTROSCOPY 7.127 Masses 19 and 31
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SPECTROSCOPY 7.129 TABLE 7.76 Conde
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SECTION 8 ELECTROLYTES, ELECTROMOTI
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ELECTROLYTES, EMF, AND CHEMICAL EQU
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TABLE 8.7 Proton Transfer Reactions
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TABLE 8.7 Proton Transfer Reactions
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TABLE 8.9 Selected Equilibrium Cons
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8.75 3-tert-Butylbenzoic acid (0) 4
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4-Hydroxyproline (1) 1.900 1C 1.850
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N-Propionylglycine (1) 3.728 3.723
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TABLE 8.14 National Bureau of Stand
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1 part 0.1% neutral red in alc. * V
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3,3-Dimethoxybenzidine dihydrochlor
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TABLE 8.35 Equivalent Conductivitie
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KCl 127.3 124.4 122.4 115.8 112.0 1
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NaIO 3 75.2 72.6 70.9 64.4 60.5 1
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9.2 SECTION 9 9.1 LINEAR FREE ENERG
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9.4 SECTION 9 TABLE 9.1 Hammett and
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9.6 SECTION 9 TABLE 9.1 Hammett and
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9.8 SECTION 9 TABLE 9.3 pK a and Rh
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10.2 SECTION 10 10.4.6 Polyacrylate
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10.4 SECTION 10 10.2 ADDITIVES TO P
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10.6 SECTION 10 injection molding.
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10.8 SECTION 10 10.3 FORMULAS AND K
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10.10 SECTION 10 Key properties of
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10.12 SECTION 10 10.3.8 Fluorocarbo
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10.14 SECTION 10 10.3.11 Phenolics
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10.16 SECTION 10 The resin has the
Page 1036 and 1037:
10.18 SECTION 10 10.3.19 Polyuretha
Page 1038 and 1039:
10.20 SECTION 10 10.3.22 Sulfones B
Page 1040 and 1041:
TABLE 10.2 Properties of Commercial
Page 1042 and 1043:
Page 1044 and 1045:
Page 1046 and 1047:
Page 1048 and 1049:
Page 1050 and 1051:
Page 1052 and 1053:
Page 1054 and 1055:
Page 1056 and 1057:
Page 1058 and 1059:
Page 1060 and 1061:
Page 1062 and 1063:
Page 1064 and 1065:
Page 1066 and 1067:
Page 1068 and 1069:
Page 1070 and 1071:
Page 1072 and 1073: TABLE 10.2 Properties of Commercial
Page 1074 and 1075: TABLE 10.2 Properties of Commercial
Page 1076 and 1077: 10.58 SECTION 10 10.4 FORMULAS AND
Page 1078 and 1079: 10.60 SECTION 10 10.4.8 Polychlorop
Page 1080 and 1081: 10.62 SECTION 10 Styrene-butadiene
Page 1082 and 1083: 10.5 CHEMICAL RESISTANCE TABLE 10.4
Page 1084 and 1085: 10.6 GAS PERMEABILITY TABLE 10.5 Ga
Page 1086 and 1087: TABLE 10.5 Gas Permeability Constan
Page 1088 and 1089: TABLE 10.7 Constants ofFats and Oil
Page 1090 and 1091: TABLE 10.8 Constants ofWaxes Wax Me
Page 1092: SECTION 11 PRACTICAL LABORATORY INF
Page 1095 and 1096: 11.4 SECTION 11 TABLE 11.2 Molecula
Page 1097 and 1098: 11.6 SECTION 11 A saturated aqueous
Page 1099 and 1100: 11.8 SECTION 11 TABLE 11.6 Relative
Page 1101 and 1102: 11.10 SECTION 11 11.3 BOILING POINT
Page 1103 and 1104: 11.12 SECTION 11 TABLE 11.8 Organic
Page 1105 and 1106: 11.14 SECTION 11 TABLE 11.9 Molecul
Page 1107 and 1108: 11.4 SEPARATION METHODS TABLE 11.11
Page 1109 and 1110: 11.18 SECTION 11 TABLE 11.12 Solven
Page 1111 and 1112: 11.20 SECTION 11 TABLE 11.12 Solven
Page 1113 and 1114: TABLE 11.13 McReynolds’ Constants
Page 1115 and 1116: TABLE 11.13 McReynolds’ Constants
Page 1117 and 1118: 11.26 SECTION 11 11.4.1 McReynolds
Page 1119 and 1120: 11.28 SECTION 11 11.4.2.2 Partition
Page 1121: 11.30 SECTION 11 FIGURE 11.2 Band a
Page 1125 and 1126: 11.34 SECTION 11 TABLE 11.16 Guide
Page 1127 and 1128: 11.36 SECTION 11 TABLE 11.16 Guide
Page 1129 and 1130: 11.38 SECTION 11 TABLE 11.18 Relati
Page 1131 and 1132: 11.40 SECTION 11 distribution coeff
Page 1133 and 1134: 11.42 SECTION 11 TABLE 11.19 Gravim
Page 1159 and 1160: 11.68 SECTION 11 TABLE 11.20 Elemen
Page 1161 and 1162: 11.70 SECTION 11 TABLE 11.22 Common
Page 1163 and 1164: 11.72 SECTION 11 TABLE 11.25 Tolera
Page 1165 and 1166: 11.74 SECTION 11 TABLE 11.26 Heatin
Page 1167 and 1168: 11.76 SECTION 11 TABLE 11.28 Titrim
Page 1173 and 1174:
11.82 SECTION 11 TABLE 11.28 Titrim
Page 1175 and 1176:
11.84 SECTION 11 appears becomes le
Page 1177 and 1178:
11.86 SECTION 11 TABLE 11.29 Equati
Page 1179 and 1180:
11.88 SECTION 11 TABLE 11.29 Equati
Page 1181 and 1182:
11.90 SECTION 11 The more stable th
Page 1183 and 1184:
11.92 SECTION 11 11.6.6.2.5 Buffer
Page 1185 and 1186:
11.94 SECTION 11 TABLE 11.30 Standa
Page 1187 and 1188:
TABLE 11.32 Properties and Applicat
Page 1189 and 1190:
11.98 SECTION 11 TABLE 11.36 Maskin
Page 1191 and 1192:
11.100 SECTION 11 TABLE 11.37 Anion
Page 1193 and 1194:
11.102 SECTION 11 TABLE 11.39 Amino
Page 1195 and 1196:
11.104 SECTION 11 TABLE 11.44 Facto
Page 1197 and 1198:
11.106 SECTION 11 11.7 LABORATORY S
Page 1199 and 1200:
11.108 SECTION 11 TABLE 11.48 Stand
Page 1201 and 1202:
11.110 SECTION 11 Alizarin yellow G
Page 1203 and 1204:
11.112 SECTION 11 Bromchlorophenol
Page 1205 and 1206:
11.114 SECTION 11 p-Ethoxychrysoidi
Page 1207 and 1208:
11.116 SECTION 11 Mercurous nitrate
Page 1209 and 1210:
11.118 SECTION 11 Potassium carbona
Page 1211 and 1212:
11.120 SECTION 11 until the ammoniu
Page 1213 and 1214:
11.122 SECTION 11 TABLE 11.49 TLV C
Page 1215 and 1216:
Page 1217 and 1218:
Page 1219 and 1220:
Page 1221 and 1222:
11.130 SECTION 11 TABLE 11.50 Chemi
Page 1223 and 1224:
Page 1225 and 1226:
Page 1227 and 1228:
Page 1229 and 1230:
11.138 SECTION 11 of water which is
Page 1231 and 1232:
TABLE 11.55 Thermoelectric Values i
Page 1233 and 1234:
TABLE 11.56 Type B Thermocouples: P
Page 1235 and 1236:
TABLE 11.58 Type J Thermocouples: I
Page 1237 and 1238:
TABLE 11.60 Type N Thermocouples: N
Page 1239 and 1240:
TABLE 11.62 Type S Thermocouples: P
Page 1241 and 1242:
11.150 SECTION 11 11.11 CORRECTION
Page 1243 and 1244:
Index Terms Links 2 Acid-base indic
Page 1245 and 1246:
Index Terms Links 4 Alkynes, nomenc
Page 1247 and 1248:
Index Terms Links 6 Aurintricarboxy
Page 1249 and 1250:
Index Terms Links 8 Boron-11 chemic
Page 1251 and 1252:
Index Terms Links 10 Cellulose acet
Page 1253 and 1254:
Index Terms Links 12 Collective ino
Page 1255 and 1256:
Index Terms Links 14 Degree Fahrenh
Page 1257 and 1258:
Index Terms Links 16 Electrical res
Page 1259 and 1260:
Index Terms Links 18 Equivalent wei
Page 1261 and 1262:
Index Terms Links 20 Fluorocarbon p
Page 1263 and 1264:
Index Terms Links 22 Halogenated hy
Page 1265 and 1266:
Index Terms Links 24 Impact strengt
Page 1267 and 1268:
Index Terms Links 26 Kα 1 lines, m
Page 1269 and 1270:
Index Terms Links 28 Melmine phenol
Page 1271 and 1272:
Index Terms Links 30 Neon-neon bond
Page 1273 and 1274:
Index Terms Links 32 One-tailed tes
Page 1275 and 1276:
Index Terms Links 34 Physical chemi
Page 1277 and 1278:
Index Terms Links 36 Polyolefin the
Page 1279 and 1280:
Index Terms Links 38 Pyridine: bina
Page 1281 and 1282:
Index Terms Links 40 Rho values: fo
Page 1283 and 1284:
Index Terms Links 42 Single-bond ra
Page 1285 and 1286:
Index Terms Links 44 Stereoisomers
Page 1287 and 1288:
Index Terms Links 46 Tension, aqueo
Page 1289 and 1290:
Index Terms Links 48 Triethylenetet
Page 1291 and 1292:
Index Terms Links 50 Water (Cont.)
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