2.9.11. Test for methanol and 2-propanol EUROPEAN PHARMACOPOEIA 10.

A1 ´ I 2 ´ 100 Temperature :
A 2 ´ I1 ´ V1 Time Temperature
(min) (°C)
A1 = area of the peak due to ethanol in the chromatogram
Column 0 - 1.6 40
obtained with the test solution ;
A2 = area of the peak due to ethanol in the chromatogram 1.6 - 9.9 40 → 65
obtained with reference solution (c) ; 9.9 - 13.6 65 → 175
I1 = area of the peak due to the internal standard in the
13.6 - 20 175
chromatogram obtained with the test solution ;
I2 = area of the peak due to the internal standard Injection port 200
in the chromatogram obtained with reference Detector 200
solution (c) ;
V1 = volume of the preparation to be examined in the Detection : flame ionisation.
test solution, in millilitres. Injection : 1.0 mL of the gaseous phase of the test solution and
reference solution (c), at least 3 times.
Elution order : methanol, ethanol, 2-propanol, 1-propanol.
Relative retention with reference to ethanol (retention
time = about 5.3 min) : methanol = about 0.8 ;
2-propanol = about 1.2 ; 1-propanol = about 1.6.
07/2019:20911 System suitability : reference solution (c) :
corrected 10.0 – resolution : minimum 5 between the peaks due to methanol
and ethanol.
Calculate the methanol content in per cent V/V using the
following expression :
A1 ´ I 2
2.9.11. TEST FOR METHANOL AND A 2 ´ I1 ´ 40
2-PROPANOL
A1 = area of the peak due to methanol in the
METHOD A chromatogram obtained with the test solution ;
A2 = area of the peak due to methanol in the
Head-space gas chromatography (2.2.28).
chromatogram obtained with reference
Internal standard solution. Dilute 1.0 mL of propanol R1 solution (c) ;
to 100.0 mL with water R. Dilute 1.0 mL of the solution to I1 = area of the peak due to the internal standard in the
20.0 mL with water R. chromatogram obtained with the test solution ;
Test solution. Mix 1.0 mL of the internal standard solution I2 = area of the peak due to the internal standard
and 4.0 mL of the preparation to be examined and dilute to in the chromatogram obtained with reference
20.0 mL with water R. Transfer 2.0 mL of this solution into solution (c).
an injection vial.
Reference solution (a). Mix 1.0 mL of methanol R2 and 1.0 mL Calculate the 2-propanol content in per cent V/V using the
of 2-propanol R2 and dilute to 100.0 mL with water R. Dilute following expression :
1.0 mL of the solution to 20.0 mL with water R.
A3 ´ I 2
Reference solution (b). Dilute 5.0 mL of anhydrous ethanol R
to 100.0 mL with water R. Dilute 25.0 mL of the solution A 4 ´ I1 ´ 40
to 100.0 mL with water R. Dilute 1.0 mL of this solution to
20.0 mL with water R. A3 = area of the peak due to 2-propanol in the
chromatogram obtained with the test solution ;
Reference solution (c). Mix 1.0 mL of the internal standard A4 = area of the peak due to 2-propanol in the
solution, 2.0 mL of reference solution (a) and 2.0 mL of
chromatogram obtained with reference
reference solution (b) and dilute to 20.0 mL with water R.
solution (c) ;
Transfer 2.0 mL of this solution into an injection vial.
I1 = area of the peak due to the internal standard in the
Close the vials immediately with a tight rubber membrane chromatogram obtained with the test solution ;
stopper coated with polytetrafluoroethylene and secure with an
aluminium crimp cap. I 2 = area of the peak due to the internal standard
in the chromatogram obtained with reference
Column : solution (c).
– material : fused silica ;
METHOD B
– size : l = 30 m, Ø = 0.53 mm ; Gas chromatography (2.2.28).
– stationary phase : cyanopropyl(3)phenyl(3)methyl(94)polysi- Internal standard solution. Dilute 1.0 mL of propanol R1 to
loxane R (film thickness 3 μm). 100.0 mL with water R.
Carrier gas : helium for chromatography R. Test solution. Mix 1.0 mL of the internal standard solution
and 4.0 mL of the preparation to be examined and dilute to
Flow rate : 3 mL/min. 20.0 mL with water R.
Split ratio : 1:50. Reference solution (a). Mix 1.0 mL of methanol R2 and 1.0 mL
Static head-space conditions that may be used : of 2-propanol R2 and dilute to 100.0 mL with water R. Dilute
1.0 mL of the solution to 20.0 mL with water R.
– equilibration temperature : 85 °C ; Reference solution (b). Dilute 1.0 mL of anhydrous ethanol R
– equilibration time : 20 min. to 50.0 mL with water R.

342 See the information section on general monographs (cover pages)

EUROPEAN PHARMACOPOEIA 10.0 2.9.14. Specific surface area by air permeability

Reference solution (c). Mix 1.0 mL of the internal standard
solution, 1.0 mL of reference solution (b) and 2.0 mL of
reference solution (a) and dilute to 20.0 mL with water R.
Column :
– material : fused silica ;
– size : l = 30 m, Ø = 0.53 mm ;
– stationary phase : cyanopropyl(3)phenyl(3)methyl(94)polysi-
loxane R (film thickness 3 μm).
A3 = area of the peak due to 2-propanol in the
chromatogram obtained with the test solution ;
A4 = area of the peak due to 2-propanol in the
chromatogram obtained with reference
solution (c) ;
I1 = area of the peak due to the internal standard in the
chromatogram obtained with the test solution ;
I2 = area of the peak due to the internal standard
in the chromatogram obtained with reference
solution (c).

Carrier gas : helium for chromatography R.

Flow rate : 3 mL/min.
Split ratio : 1:50. 01/2008:20912
Temperature :

Time Temperature
(min) (°C)
Column 0 - 1.6 40 2.9.12. SIEVE TEST
1.6 - 9.9 40 → 65 The degree of fineness of a powder may be expressed by
9.9 - 13.6 65 → 175 reference to sieves that comply with the specifications for
non-analytical sieves (2.1.4).
13.6 - 20 175
Where the degree of fineness of powders is determined by
Injection port 200 sieving, it is defined in relation to the sieve number(s) used
Detector 200
either by means of the following terms or, where such terms
cannot be used, by expressing the fineness of the powder as a
percentage m/m passing the sieve(s) used.
Detection : flame ionisation. The following terms are used in the description of powders :
Injection : 1.0 μL of the test solution and reference solution (c), Coarse powder. Not less than 95 per cent by mass passes
at least 3 times. through a number 1400 sieve and not more than 40 per cent
by mass passes through a number 355 sieve.
Elution order : methanol, ethanol, 2-propanol, 1-propanol.
Moderately fine powder. Not less than 95 per cent by mass
Relative retention with reference to ethanol (retention passes through a number 355 sieve and not more than 40 per
time = about 5.3 min): methanol = about 0.8 ; cent by mass passes through a number 180 sieve.
2-propanol = about 1.2 ; 1-propanol = about 1.6. Fine powder. Not less than 95 per cent by mass passes
through a number 180 sieve and not more than 40 per cent by
System suitability : reference solution (c) : mass passes through a number 125 sieve.
– resolution : minimum 5 between the peaks due to methanol Very fine powder. Not less than 95 per cent by mass passes
and ethanol. through a number 125 sieve and not more than 40 per cent by
mass passes through a number 90 sieve.
Calculate the methanol content in per cent V/V using the If a single sieve number is given, not less than 97 per cent of
following expression : the powder passes through the sieve of that number, unless
otherwise prescribed.
A1 ´ I 2 Assemble the sieves and operate in a suitable manner until
A 2 ´ I1 ´ 40 sifting is practically complete. Weigh the separated fractions
of the powder.
A1 = area of the peak due to methanol in the
chromatogram obtained with the test solution ;
A2 = area of the peak due to methanol in the
chromatogram obtained with reference 04/2017:20914
solution (c) ;
I1 = area of the peak due to the internal standard in the
chromatogram obtained with the test solution ;
I2 = area of the peak due to the internal standard
in the chromatogram obtained with reference 2.9.14. SPECIFIC SURFACE AREA BY
solution (c). AIR PERMEABILITY
The test is intended for the determination of the specific
Calculate the 2-propanol content in per cent V/V using the surface area of dry powders expressed in square metres per
following expression : gram in the sub-sieve region. The effect of molecular flow
(“slip flow”) which may be important when testing powders
consisting of particles less than a few micrometres is not taken
A3 ´ I 2 into account in the equation used to calculate the specific
A4 ´ I1 ´ 40 surface area.

General Notices (1) apply to all monographs and other texts 343