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Ethanol, Anhydrous

This document provides information on anhydrous ethanol, including its definition, characteristics, identification tests, purity tests, and storage requirements. It defines anhydrous ethanol as a colorless, volatile, flammable liquid that is miscible with water and methylene chloride, with a boiling point of around 78°C and minimum purity of 99.5% v/v ethanol. Identification tests include relative density, infrared spectroscopy, and chemical reactions. Purity tests include clarity, acidity, relative density, absorbance in UV, gas chromatography for volatile impurities including methanol, acetaldehyde, acetal and benzene, and residue on evaporation.

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Miroslav Ilic
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310 views2 pages

Ethanol, Anhydrous

This document provides information on anhydrous ethanol, including its definition, characteristics, identification tests, purity tests, and storage requirements. It defines anhydrous ethanol as a colorless, volatile, flammable liquid that is miscible with water and methylene chloride, with a boiling point of around 78°C and minimum purity of 99.5% v/v ethanol. Identification tests include relative density, infrared spectroscopy, and chemical reactions. Purity tests include clarity, acidity, relative density, absorbance in UV, gas chromatography for volatile impurities including methanol, acetaldehyde, acetal and benzene, and residue on evaporation.

Uploaded by

Miroslav Ilic
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Ethanol, anhydrous

EUROPEAN PHARMACOPOEIA 5.0

V. hexan-3-ol.
01/2005:1318

ETHANOL, ANHYDROUS
Ethanolum anhydricum
C2H 6O

Mr 46.07

DEFINITION
Content : not less than 99.5 per cent V/V of C2H6O (99.2 per
cent m/m), at 20 C, calculated from the relative density
using the alcoholimetric tables (5.5).
CHARACTERS
Appearance : colourless, clear, volatile, flammable liquid,
hygroscopic.
Solubility : miscible with water and with methylene chloride.
It burns with a blue, smokeless flame.
bp : about 78 C.
IDENTIFICATION
First identification : A, B.
Second identification : A, C, D.
A. It complies with the test for relative density (see Tests).
B. Infrared absorption spectrophotometry (2.2.24).
Comparison : Ph. Eur. reference spectrum of anhydrous
ethanol.
C. Mix 0.1 ml with 1 ml of a 10 g/l solution of potassium
permanganate R and 0.2 ml of dilute sulphuric acid R
in a test-tube. Cover immediately with a filter paper
moistened with a freshly prepared solution containing
0.1 g of sodium nitroprusside R and 0.5 g of piperazine
hydrate R in 5 ml of water R. After a few minutes, an
intense blue colour appears on the paper and becomes
paler after 10-15 min.
D. To 0.5 ml add 5 ml of water R, 2 ml of dilute sodium
hydroxide solution R, then slowly add 2 ml of 0.05 M
iodine. A yellow precipitate is formed within 30 min.
TESTS
Appearance. It is clear (2.2.1) and colourless (2.2.2,
Method II) when compared with water R. Dilute 1.0 ml to
20 ml with water R. After standing for 5 min, the dilution
remains clear (2.2.1) when compared with water R.
Acidity or alkalinity. To 20 ml add 20 ml of carbon
dioxide-free water R and 0.1 ml of phenolphthalein
solution R. The solution is colourless. Add 1.0 ml of 0.01 M
sodium hydroxide. The solution is pink (30 ppm, expressed
as acetic acid).
Relative density (2.2.5) : 0.790 to 0.793.
Absorbance (2.2.25) : maximum 0.40 at 240 nm, 0.30
between 250 nm and 260 nm, and 0.10 between 270 nm
and 340 nm.
Examined between 235 nm and 340 nm in a 5 cm cell using
water R as the compensation liquid. The absorption curve
is smooth.
Volatile impurities. Gas chromatography (2.2.28).
Test solution (a). The substance to be examined.
General Notices (1) apply to all monographs and other texts

Test solution (b). Add 150 l of 4-methylpentan-2-ol R to


500.0 ml of the substance to be examined.
Reference solution (a). Dilute 100 l of anhydrous
methanol R to 50.0 ml with the substance to be examined.
Dilute 5.0 ml of the solution to 50.0 ml with the substance
to be examined.
Reference solution (b). Dilute 50 l of anhydrous
methanol R and 50 l of acetaldehyde R to 50.0 ml with the
substance to be examined. Dilute 100 l of the solution to
10.0 ml with the substance to be examined.
Reference solution (c). Dilute 150 l of acetal R to 50.0 ml
with the substance to be examined. Dilute 100 l of the
solution to 10.0 ml with the substance to be examined.
Reference solution (d). Dilute 100 l of benzene R to
100.0 ml with the substance to be examined. Dilute 100 l of
the solution to 50.0 ml with the substance to be examined.
Column :
material : fused silica,
size : l = 30 m, = 0.32 mm,
stationary phase : poly[(cyanopropyl)(phenyl)][dimethyl]siloxane R (film thickness 1.8 m).
Carrier gas : helium for chromatography R.
Linear velocity : 35 cm/s.
Split ratio : 1:20.
Temperature :

Column

Time
(min)

Temperature
(C)

0 - 12

40

12 - 32

40 240

32 - 42

240

Injection port

200

Detector

280

Detection : flame ionisation.


Injection : 1 l.
System suitability : reference solution (b) :
resolution : minimum 1.5 between the first peak
(acetaldehyde) and the second peak (methanol).
Limits :
methanol : in the chromatogram obtained with test
solution (a) : not more than half the area of the
corresponding peak in the chromatogram obtained with
reference solution (a) (200 ppm V/V) .
acetaldehyde + acetal : maximum of 10 ppm V/V,
expressed as acetaldehyde.
Calculate the sum of the contents of acetaldehyde and
acetal in parts per million (V/V) using the following
expression :

AE

= area of the acetaldehyde peak in the


chromatogram obtained with test solution (a),

AT

= area of the acetaldehyde peak in the


chromatogram obtained with reference
solution (b),

CE

= area of the acetal peak in the chromatogram


obtained with test solution (a),

CT

= area of the acetal peak in the chromatogram


obtained with reference solution (c).
1547

Ether

EUROPEAN PHARMACOPOEIA 5.0

benzene : maximum 2 ppm V/V.


Calculate the content of benzene in parts per million
(V/V) using the following expression :
L. butan-2-ol,
BE

= area of the benzene peak in the chromatogram


obtained with the test solution (a),

BT

= area of the benzene peak in the chromatogram


obtained with reference solution (d).

M. 2-methylpropanol (isobutanol),

If necessary, the identity of benzene can be confirmed


using another suitable chromatographic system
(stationary phase with a different polarity).
total of other impurities in the chromatogram obtained
N. furane-2-carbaldehyde (furfural),
with test solution (b) : not more than the area of the peak
due to 4-methylpentan-2-ol in the chromatogram obtained
with test solution (b) (300 ppm),
disregard limit : 0.03 times the area of the peak
corresponding to 4-methylpentan-2-ol in the
O. 2-methylpropan-2-ol (1,1-dimethylethyl alcohol),
chromatogram obtained with test solution (b) (9 ppm).
Residue on evaporation : maximum 25 ppm m/V.
Evaporate 100 ml to dryness on a water-bath and dry at
100-105 C for 1 h. The residue weighs a maximum of 2.5 mg.
P. 2-methylbutan-2-ol,
STORAGE
Protected from light.
IMPURITIES

A. 1,1-diethoxyethane (acetal),

B. acetaldehyde,

Q. pentan-2-ol,
R. CH3-(CH2)4-OH : pentanol,
S. CH3-(CH2)5-OH : hexanol,

T. heptan-2-ol,

C. acetone,
U. hexan-2-ol,
D. benzene,
V. hexan-3-ol.
01/2005:0650

E. cyclohexane,

ETHER

F. CH3-OH : methanol,

Aether
G. butan-2-one (methyl ethyl ketone),

H. 4-methylpentan-2-one (methyl isobutyl ketone),


I. CH3-(CH2)2-OH : propanol,
J. propan-2-ol (isopropyl alcohol),
K. CH3-(CH2)3-OH : butanol,
1548

C4H10O

Mr 74.1

DEFINITION
Ether is diethyl ether which may contain a suitable
non-volatile antioxidant at a suitable concentration.
CHARACTERS
A clear, colourless liquid, volatile, highly flammable, soluble
in water, miscible with alcohol, with methylene chloride and
with fatty oils.
See the information section on general monographs (cover pages)

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