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Laboratory Tips Safety proceedures, test reagents, drilling rubber stoppers, bending glass tubes, etc. Contributed to by chemists.

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 #1 
Old 2003-10-03, 04:19
super manic soul super manic soul is offline
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Default fractional distillation

what temperatures should starter fluid be heated at when performing fractional distillation to extract ether?
 #2 
Old 2003-10-03, 09:55
mnm mnm is offline
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Default Re: fractional distillation

This has been discussed before...

But ask and ye shall recieve.



3852. Ethyl Ether.

1,1'-Oxybisethane; ethoxyethane; ether; diethyl ether; ethyl oxide; diethyl oxide; sulfuric ether; anesthetic ether. C4H10O; mol wt 74.12. C 64.82%, H 13.60%, O

21.58%. C2H5OC2H5. Produced on a large scale by dehydration of ethanol or by hydration of ethylene, both processes being carried out in the presence of sulfuric

acid. Review of mfg processes: Himmler in Ullmann's Encyklopdie der Technischen Chemie, vol. 5 (1954) pp 777-782; D. E. Keeley in Kirk-Othmer Encyclopedia of

Chemical Technology vol. 9 (Wiley-Interscience, New York, 3rd ed., 1980) pp 381-393.

Mobile, very volatile, highly flammable liq. Explosive! Vapor heavier than air. Characteristic, sweetish, pungent odor, more agreeable than chloroform. Burning

taste. Tends to form explosive peroxides under the influence of air and light, esp when evaporation to dryness is attempted. Peroxides may be removed from ether by

shaking with 5% aq ferrous sulfate soln. Addition of naphthols, polyphenols, aromatic amines, and aminophenols has been proposed for the stabilization of ethyl ether.

d40 0.7364; d410 0.7249; d420 0.7134; d430 0.7019. Vapor density 2.55 (air = 1.0). mp -116.3 deg (stable crystals); mp -123.3 deg (metastable crystals). bp760 34.6 deg; bp400

17.9 deg; bp200 +2.2 deg; bp100 -11.5 deg; bp10 -48.1 deg; bp1.0 -74.3 deg. Satd vapor press. at 0 deg: 184.9 mm; at 10 deg: 290.8 mm; at 20 deg: 439.8 mm; at 50 deg: 1276 mm; at 70 deg: 2304

mm. Critical temp 192.7 deg; crit press. 35.6 atm. Flash pt, closed cup: -49 degF (-45 degC). Air-ether mixtures containing more than 1.85 volume-% of ether vapor, are

explosive hazards. Autoignition temp 180-190 deg. nD15 1.35555. Dielectric constant at 26.9 deg and 85.8 kilocycles = 4.197; good insulator. When shaken under absolutely

dry conditions ether can generate enough static electricity to start a fire. Surface tension at 20 deg: 17.06 dynes/cm. Viscosity at 20 deg: 0.2448 cp. Heat of vaporization at

30 deg: 89.80 cal/g. Produces considerable coldness on quick evaporation. Heat of formation -907 cal/g; heat of combustion -8.807 kcal/g. Ether is slightly sol in water

and water is slightly sol in ether. A satd water soln contains 8.43% (w/w) of ether at 15 deg and 6.05% (w/w) at 25 deg. Ether satd with water contains 1.2% H2O at 20 deg.

Soly in water increased by HCl. Sol in concd hydrochloric acid. May explode when brought in contact with anhydr nitric acid. Miscible with lower aliphatic alcohols,

benzene, chloroform, petr ether, other fat solvents, many oils. Azeotrope with water (1.3%), bp 34.2 deg.

 Caution: Potential symptoms of overexposure are dizziness; drowsiness; headache, excitedness and narcosis; nausea, vomiting; irritation of eyes, upper

respiratory system and skin. See NIOSH Pocket Guide to Chemical Hazards (DHHS/NIOSH 90-117, 1990) p 112.

USE: Solvent for waxes, fats, oils, perfumes, alkaloids, gums. Excellent solvent for nitrocellulose when mixed with alc. Important reagent in organic syntheses,

esp in Grignard and Wurtz type reactions. Easily removable extractant of active principles (hormones, etc.) from plant and animal tissues. In the manuf of gun

powder. As primer for gasoline engines.

THERAP CAT: Anesthetic (inhalation).

THERAP CAT (VET): Anesthetic (inhalation). Has been used orally in colic, subcutaneously as a stimulant.

4694. n-Heptane.

C7H16; mol wt 100.20. C 83.91%, H 16.09%. CH3(CH2)5CH3. A hydrocarbon from petroleum.

Volatile, flammable liquid. d420 0.684. bp 98.4 deg. mp -90.7 deg. Flash pt, open cup: 30 degF (-1 degC); closed cup: 25 degF (-4 degC). nD25 1.3855. Insol in water; sol in

alcohol, chloroform, ether. Lethal concn for mice in air: 15900 ppm, Handbook of Toxicology vol 1, W. S. Spector, Ed. (Saunders, Philadelphia, 1956) pp 338-339.

Caution: Potential symptoms of verexposure are lightheadedness, giddiness and stupor; no appetite, nausea; dermatitis; chemical pneumonia;

unconsciousness. See NIOSH Pocket Guide to Chemical Hazards (DHHS/NIOSH 90-117, 1990) p 120.

USE: As standard in testing knock of gasoline engines.



Goods Luck...
 #3 
Old 2003-10-03, 16:42
tryptamine tryptamine is offline
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Default Re: fractional distillation

The top of your column should be 35 degrees, but depending on the column you use you could be heating the reaction flask quite strongly. This is a very basic question, are you sure you want to be distilling ether? Are you sure you have an adequate setup?

Make sure the water in your condenser is 0 degrees C, with a serious ice bath in the reservoir. You also need your receiving flask cooled in an ice bath. And keep a few extra bags of ice in the freezer for replenishing while in progress.
 
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