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Solvent Drying and Drying Agents

Related link :
Drying with sodium wire :
Disposal of spent sodium, magnesium and calcium hydride

On this page : Properties of solvents

and methods used for drying them with specific drying agents

Removing water from Solvents

There are various ways of removing water and other impurities from a solution. This can become
a major task once the used reagents are also sensitive towards water e.g. Grignard reagents or
enolates. If water is one of the products, it also has a detrimental effect on the yield and/or
reaction rate. In those cases, drying agents like activated alumina¹, calcium hydride (CaH2),
sodium metal (in combination with benzophenone which forms a dark blue ketyl radical), lithium
aluminum hydride (LiAlH4) or phosphorous pentoxide (P4O10) are used to chemically destroy the
water.
The drying agents commonly used in the organic laboratories are calcium chloride (CaCl2),
sodium sulfate (Na2SO4) Calcium sulfate (CaSO 4, as Drierite (R)) and magnesium sulfate
(MgSO4), all in their anhydrous form.
Listed below are the drying agents that are commonly used.Organic liquids are considered to be
wet if they contain water. Realize that the organic liquid will still be a liquid after it is dried.

Activated alumina ¹ is a very porous form of aluminum oxide of high surface area which adsorbs
liquids and gases without any change in form. Activated alumina will not soften or disintegrate
when immersed in liquids. Activated alumina may be regenerated to its original adsorption
efficiency by heating to a temperature between (177-316°C).
Reconditioning of mineral oils like transformer or insulating oils. Removal of oil vapor mist from
compressed air. Drying of organic liquids to a moisture level of 10 ppm or below. Drying of
various liquids such as Benzene, Carbon, Tetrachloride, Chlorobenzene, Ethyl Acetate,
Transformer oil, Vegetable oils etc.

Solvents drying guide

TO DRY USE ONE OF THE FOLLOWING DRYING AGENTS

Anhydrous forms of potassium carbonate; anhydrous magnesium or

Alcohols
calcium sulphate; quicklime.
Alkyl halides Anhydrous calcium chloride; anhydrous forms of sodium sulphate,
Aryl halides magnesium sulphate, or calcium sulphate; sodium pentoxide.
Saturated and
Anhydrous calcium chloride or sulphate; metallic sodium; phosphorus
Aromatic
pentoxide.
hydrocarbons
Aldehydes Anhydrous sodium sulphate; anhydrous magnesium or calcium sulphate.
Anhydrous sodium sulphate; anhydrous magnesium or calcium sulphate;
Ketones
anhydrous potassium carbonate.
Organic bases
Solid potassium or sodium hydroxide; quicklime; barium oxide.
(amines)
Organic acids Anhydrous sodium sulphate; anhydrous magnesium or calcium sulphate.

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Solvents: Properties and Drying agents

Boiling Flash
Solvent Pt. Density Pt. Drying agent
°C °C
Acetone 56 0.791 -18 K2CO3; Molecular sieve 0.3nm; CaCl2
Acetic acid 118 1.049 +40 P2O5; CuSO4
Acetic anhydride 136 1.082 +49 CaCl2
CaCl2; P2O5; K2CO3; calcium hydride;
Acetonitrile 82 0.782 +6
Molecular sieve 0.3nm
Aniline 184 1.022 +76 KOH; BaO
Anisole 154 0.995 +51 CaCl2; Na; distillation
CaCl2; distillation; Na; Pb/Na; ; calcium
Benzene 80 0.879 -10
hydride; Na wire; Molecular sieve 0.4nm
1-Butanol 117 0.810 +29 K2CO3; distillation
2-Butanol 100 0.808 +24 K2CO3; distillation
tert-Butanol 82 0.882 +11 CaO; Freezing
n-Butyl acetate 127 0.882 +33 MgSO4;
Carbon disulphide 46 1.263 -30 CaCl2P2O5;
distillation; P2O3; Pb/Na; Molecular sieve
Carbon tetrachloride 77 1.594 none
0.4nm
Chlorobenzene 132 1.106 +29 CaCl2; distillation;P2O5
CaCl2; P2O5; Pb/Na; Molecular sieve
Chloroform 62 1.486 none
0.4nm
Na; Na/Pb; LiAlH4; Molecular sieve
Cyclohexane 81 0.799 none
0.4nm
Cyclohexanone 155 na na Distillation
Decahydronaphthalene
~190 0.886 <54 CaCl2; Na; Pb/Na
(Dekalin)
CaCl2; Pb/Na; calcium hydride;
Dichloromethane 40 1.325 none
Molecular sieve 0.4nm
Refractionation: distillate at 40 - 42°C.
Dicyclopentadiene:
170 na na (Use at once! or keep in dry ice/acetone
(cyclopentadiene dimer)
bath no longer than 1 Hr.)
Diethyl carbonate 126 0.975 +25 Na2SO4; K2CO3
Diethylene glycoldibutyl
225 0.885 +118 CaCl2; Na
ether
Diethylene glycol 155
0.906 +70 CaCl2; Na
dimethyl ether 165
CaCl2; Na; Pb/Na; LiAlH4; Na
Diethyl ether 34 0.714 -40 wire/benzophenone; Molecular sieve
0.4nm
Di-isopropyl ether 68 0.726 -23 CaCl2; Na; Molecular sieve 0.4nm
Dimethyl formamide 153 0.950 +62 distillation; Molecular sieve 0.4nm
Dimethyl sulfoxide 189 1.101 +95 distillation; Molecular sieve 0.4nm
1,4 Dioxane 101 1.034 +11.8 CaCl2; Na; Molecular sieve 0.4nm
Ethanol 79 0.791 +12 CaO; Mg; MgO; Molecular sieve 0.3nm
K2CO3; P2O5; Na2SO4; calcium hydride;
Ethyl acetate 77 0.901 -4
Molecular sieve 0.4nm
Ethylenediamine:
118 na na Simple distillation.
(1-2 diaminoethane)

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Boiling Flash
Solvent Pt. Density Pt. Drying agent
°C °C
Ethylene glycol 197 1.109 +111 distillation; Na2SO4
Ethylene glycol monoethyl
135 0.930 +41 distillation
ether
Ethylene glycol
125 0.965 +52 distillation
monomethyl ether
Ethyl formate 54 0.924 -20 MgSO4; Na2SO4;
Formamide 211 1.134 155 Na2SO4; CaO
Glycerol 290 1.260 +176 distillation
Heptane 98 0.684 -4 calcium hydride; Na wire
Na; Pb/Na; LiAlH4; calcium hydride;
n-Hexane 69 0.659 -23 Na wire/benzophenone; Molecular
sieve 0.4nm
Isobutanol 108 0.803 +28 K2CO3; CaO; Mg;
Isobutyl methyl ketone 117 0.801 +15.5-4 K2CO3;
Methanol 65 0.792 +11 Mg; CaO; Molecular sieve 0.3nm
Methyl acetate 57 0.933 -10 K2CO3; CaO;
Na2SO4; distillation; Molecular sieve
1-Methyl-2-pyrrolidone 202 1.026 +95
0.4nm
Methyl Ethyl ketone 80 0.806 -44 K2CO3;
Nitrobenzene 211 1.204 +92 CaCl2; P2O5; distillation;
n-Pentane 36 0.626 -49 Na; Pb/Na;calcium hydride; Na wire
calcium hydride; Na
Pet ether mixture na na wire/benzophenone; Molecular sieve
type 4A
1- Propanol 97 0.804 +15 CaO; Mg
2-Propanol 82 0.785 +12 CaO; Mg; Molecular sieve 0.3nm
Pyridine 116 0.982 +20 KOH; BaO; Molecular sieve 0.4nm
Tetrahydrofuran 66 0.887 -17.5 Molecular sieve 0.4nm
Tetrahydronaphthalene
208 0.973 CaCl2; Na
(Tetralin)
Thionyl chloride 48 na na Redistill.
distillation; Ca; CaCl2; Na; Molecular
Toluene 111 0.867 +4
sieve 0.4nm
Trichloroethylene 87 1.462 none distillation; Na2SO4; K2CO3
distillation; Na; CaCl2; Molecular sieve
Xylene 137/140 -0.86 +25
0.4nm

Reference: http://www.deltaadsorbents.com/activated_alumina_2.php

delloyd.50megs.com

Signature: Dhanlal De Lloyd, Chem. Dept, The University of The West Indies, St. Augustine campus
The Republic of Trinidad and Tobago.
Copyright: delloyd2000© All rights reserved.

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