EUROPEAN PHARMACOPOEIA 8.

Application : 0.5 mL of solution A1 obtained during the

identication as a band 30 mm by 3 mm and 5 L of each
reference solution.
Development : over a path of 15 cm.
Drying : in air.
Detection A : examine in ultraviolet light at 254 nm.
Locate the zone corresponding to plastic additive 01 (RF about
0.4). Remove the area of silica gel corresponding to this zone
and shake with 40 mL of ether R for 1 min. Filter, rinse with
2 quantities, each of 10 mL of ether R, add the rinsings to the
ltrate and evaporate to dryness. The residue C weighs not
more than 40 mg.
Detection B : expose the plate to iodine vapour for 5 min.
Examine the chromatogram and locate the band corresponding
to plastic additives 04 and 05 (RF = 0). Remove the area of
silica gel corresponding to this zone. Similarly remove a
corresponding area of silica gel as a blank reference. Separately
shake both samples for 15 min with 40 mL of methanol R.
Filter, rinse with 2 quantities, each of 10 mL of methanol R,
add the rinsings to the ltrate and evaporate to dryness. The
difference between the masses of both residues is not more
than 10 mg.
Plastic additive 03. Infrared absorption spectrophotometry
(2.2.24).
Preparation. Wash precipitate B2 obtained during the
identication and contained in the tared sintered-glass lter
(40) (2.1.2) with anhydrous ethanol R. Dry to constant mass
over diphosphorus pentoxide R and weigh the lter. The
residue weighs not more than 20 mg.
Comparison : plastic additive 03 CRS.
Barium : maximum 5 ppm.
Inductively coupled plasma-atomic emission spectrometry
(2.2.57).
Test solution. Ignite 1.0 g of the substance to be examined in a
silica crucible. Take up the residue with 10 mL of hydrochloric
acid R and evaporate to dryness on a water-bath. Take up the
residue with 20 mL of 0.1 M hydrochloric acid.
Reference solution. A solution containing 0.25 ppm of barium
prepared by dilution of barium standard solution (50 ppm
Ba) R with 0.1 M hydrochloric acid.
Wavelength : use the emission of barium at 455.40 nm, the
spectral background being taken at 455.30 nm.
Verify the absence of barium in the hydrochloric acid used.
Cadmium : maximum 0.6 ppm.
Atomic absorption spectrometry (2.2.23, Method I).
Test solution. Evaporate 10 mL of solution S1 to dryness.
Take up the residue using 5 mL of a 1 per cent V/V solution
of hydrochloric acid R, lter and dilute the ltrate to 10.0 mL
with the same acid.
Reference solutions. Prepare the reference solutions using
cadmium standard solution (0.1 per cent Cd) R, diluting with a
1 per cent V/V solution of hydrochloric acid R.
Source : cadmium hollow-cathode lamp.
Wavelength : 228.8 nm.
Atomisation device : air-acetylene ame.
Verify the absence of cadmium in the hydrochloric acid used.
Calcium : maximum 0.07 per cent.
Inductively coupled plasma-atomic emission spectrometry
(2.2.57).
Test solution. Use the test solution prepared for the
determination of barium.
Reference solution. A solution containing 50.0 ppm of calcium
prepared by dilution of calcium standard solution (400 ppm
Ca) R with 0.1 M hydrochloric acid.
Wavelength : use the emission of calcium at 315.89 nm, the
spectral background being taken at 315.60 nm.
General Notices (1) apply to all monographs and other texts

3.1.15. Polyethylene terephthalate for containers

Verify the absence of calcium in the hydrochloric acid used.

Tin : maximum 20 ppm.
Inductively coupled plasma-atomic emission spectrometry
(2.2.57).
Test solution. Dilute solution S1 10 times with water R
immediately before use.
Reference solution. Introduce 2 mL of tin standard solution
(5 ppm Sn) R into a 50 mL ask containing 5 mL of a 20 per
cent V/V solution of sulfuric acid R and dilute to 50 mL with
water R immediately before use.
Wavelength : use the emission of tin at 189.99 nm, the spectral
background being taken at 190.10 nm.
Verify the absence of tin in the hydrochloric acid used.
Zinc : maximum 0.2 per cent.
Atomic absorption spectrometry (2.2.23, Method I).
Test solution. Dilute solution S1 100 times with 0.1 M
hydrochloric acid.
Reference solutions. Prepare the reference solutions using
zinc standard solution (100 ppm Zn) R, diluting with 0.1 M
hydrochloric acid.
Source : zinc hollow-cathode lamp.
Wavelength : 213.9 nm.
Atomisation device : air-acetylene ame.
Verify the absence of zinc in the hydrochloric acid used.
Heavy metals (2.4.8): maximum 50 ppm.
To 10 mL of solution S1 add 0.5 mL of phenolphthalein
solution R and then strong sodium hydroxide solution R until
a pale pink colour is obtained. Dilute to 25 mL with water R.
12 mL of solution complies with test A. Prepare the reference
solution using lead standard solution (2 ppm Pb) R.
Water extractable substances : maximum 0.3 per cent.
Evaporate 50.0 mL of solution S2 to dryness on a water-bath
and dry at 100-105 C until constant mass. Carry out a blank
titration with 50.0 mL of water for injections R. The residue
weighs not more than 7.5 mg taking into account the blank
test.
ASSAY
Carry out the oxygen-ask method (2.5.10) using 50.0 mg.
Absorb the combustion products in 20 mL of 1 M sodium
hydroxide. To the solution obtained add 1 mL of dibutyl
phthalate R, 2.5 mL of nitric acid R, 5 mL of ferric ammonium
sulfate solution R2 and 10.0 mL of 0.1 M silver nitrate. Titrate
with 0.05 M ammonium thiocyanate until a reddish-yellow
colour is obtained. Carry out a blank test.
1 mL of 0.1 M silver nitrate is equivalent to 6.25 mg of
poly(vinyl chloride).
01/2008:30115
corrected 7.5

3.1.15. POLYETHYLENE
TEREPHTHALATE FOR CONTAINERS
FOR PREPARATIONS NOT FOR
PARENTERAL USE

DEFINITION
Polyethylene terephthalate is obtained from the
polymerisation of terephthalic acid or dimethyl
terephthalate with ethylene glycol. Isophthalic acid,
dimethyl isophthalate, 1,4-bis(hydroxymethyl)cyclohexane

403

3.1.15. Polyethylene terephthalate for containers

(cyclohexane-1,4-dimethanol) or diethylene glycol may be

used in the polymerisation. It may contain not more than
0.5 per cent of silica or silicates and colouring matter approved
by the competent authority.
PRODUCTION
The manufacturing process is validated to demonstrate that
the residual acetaldehyde content is not greater than 10 ppm
in the granules.
CHARACTERS
Appearance : clear or opaque granules.
Solubility : practically insoluble in water, in ethanol (96 per
cent) and in methylene chloride. It is hydrolysed by strong
bases.
IDENTIFICATION
A. Place 0.10 g of the material to be examined into a
borosilicate glass ask with a ground-glass neck. Add
25 mL of a 200 g/L solution of potassium hydroxide R in a
50 per cent V/V solution of anhydrous ethanol R. Reux for
30 min. Allow to cool and dilute to 100 mL with water R.
Filter if necessary. Dilute 1.0 mL of the ltrate to 100 mL
with water R. Examined between 210 nm and 330 nm
(2.2.25), the solution shows an absorption maximum at
240 nm.
B. Dissolve 0.05 g of the material to be examined in 2 mL
of 1,1,1,3,3,3-hexafluoropropan-2-ol R. Apply to a glass
plate on a water-bath in a fume cupboard several drops of
the solution to produce a lm of about 15 mm by 15 mm.
Allow the solvent to evaporate and remove the lm using a
stream of water and a scraper. Dry in an oven at 100-105 C
for 1-2 h. Examine the lm by infrared absorption
spectrophotometry (2.2.24). The spectrum of the material
to be examined shows maxima in particular at 1725 cm 1,
1410 cm 1, 1265 cm 1, 1120 cm 1, 1100 cm 1, 1020 cm 1,
875 cm 1, 725 cm 1. The spectrum obtained, in addition, is
identical to that of the material selected for the type sample.
TESTS
If necessary, cut out samples for testing to a maximum size of
1 cm per side.
Solution S1. Place 10.0 g of the material to be examined in a
borosilicate glass ask with a ground-glass neck. Add 200 mL
of water R and heat at 50 C for 5 h. Allow to cool and decant
the solution. Use solution S1 within 4 h of its preparation.
Solution S2. Place 10 g of the material to be examined in a
borosilicate glass ask with a ground-glass neck. Add 100 mL
of ethanol (96 per cent) R and heat at 50 C for 5 h. Allow to
cool and decant the solution. Use solution S2 within 4 h of its
preparation.
Solution S3. Place 20 g of the material to be examined in a
borosilicate glass ask with a ground-glass neck. Add 50 mL
of 0.1 M hydrochloric acid and heat at 50 C for 5 h. Allow
to cool and decant the solution. Use solution S3 within 4 h
of its preparation.
Solution S4. Place 20 g of the material to be examined into a
borosilicate glass ask with a ground-glass neck. Add 50 mL
of 0.01 M sodium hydroxide and heat at 50 C for 5 h. Allow to
cool and decant. Use solution S4 within 4 h of its preparation.
Appearance of solution S1. Solution S1 is clear (2.2.1).
Appearance of solution S2. Solution S2 is clear (2.2.1) and
colourless (2.2.2, Method II).
Acidity or alkalinity. To 50 mL of solution S1 add 0.15 mL
of BRP indicator solution R. The solution turns yellow. Not
more than 0.5 mL of 0.01 M sodium hydroxide is required
to change the colour of the indicator to blue. To another
50 mL of solution S1 add 0.2 mL of methyl orange solution R.

404

EUROPEAN PHARMACOPOEIA 8.0

The solution turns yellow. Not more than 0.5 mL of 0.01 M

hydrochloric acid is required to reach the beginning of the
colour change of the indicator to orange.
Absorbance of solution S1 (2.2.25) : maximum 0.20 between
220 nm and 340 nm. In addition, for coloured polyethylene
terephthalate : maximum 0.05 between 400 nm to 800 nm.
Absorbance of solution S2 (2.2.25) : maximum 0.05 between
400 nm and 800 nm.
Reducing substances. Add 2 mL of 0.5 M sulfuric acid and
20.0 mL of 0.002 M potassium permanganate to 20.0 mL of
solution S1. Boil for 3 min. Cool immediately to ambient
temperature. Add 1 g of potassium iodide R, 0.25 mL of
starch solution R as indicator and titrate with 0.01 M sodium
thiosulfate. Perform a blank titration using 20.0 mL of water R.
The difference in volume used in the 2 titrations is not greater
than 0.5 mL.
Substances soluble in dioxan : maximum 3 per cent.
Place 2 g of the material to be examined in a borosilicate glass
ask with a ground-glass neck. Add 20 mL of dioxan R and
heat under reux for 2 h. Evaporate 10 mL of the solution
to dryness on a water-bath and then dry the residue at
100-105 C. The residue weighs a maximum of 30 mg.
Extractable aluminium : maximum 1 ppm.
Inductively coupled plasma-atomic emission spectrometry
(2.2.57).
Test solution. Solution S3.
Reference solutions. Prepare the reference solutions using
aluminium standard solution (200 ppm Al) R, diluting with
0.1 M hydrochloric acid.
Wavelength : 396.15 nm, the spectral background being taken
at 396.25 nm.
Verify the absence of aluminium in the 0.1 M hydrochloric
acid used.
Extractable antimony : maximum 1 ppm.
Inductively coupled plasma-atomic emission spectrometry
(2.2.57).
Test solution. Solution S4.
Reference solutions. Prepare the reference solutions using
antimony standard solution (100 ppm Sb) R, diluting with
0.01 M sodium hydroxide.
Wavelength : 231.15 nm or 217.58 nm, the spectral background
being taken at 231.05 nm.
Extractable barium : maximum 1 ppm.
Inductively coupled plasma-atomic emission spectrometry
(2.2.57).
Test solution. Solution S3.
Reference solutions. Prepare the reference solutions using
barium standard solution (50 ppm Ba) R, diluting with 0.1 M
hydrochloric acid.
Wavelength : 455.40 nm, the spectral background being taken
at 455.30 nm.
Verify the absence of barium in the 0.1 M hydrochloric acid
used.
Extractable cobalt : maximum 1 ppm.
Inductively coupled plasma-atomic emission spectrometry
(2.2.57).
Test solution. Solution S3.
Reference solutions. Prepare the reference solutions using
cobalt standard solution (100 ppm Co) R, diluting with 0.1 M
hydrochloric acid.
Wavelength : 228.62 nm, the spectral background being taken
at 228.50 nm.
Verify the absence of cobalt in the 0.1 M hydrochloric acid
used.
See the information section on general monographs (cover pages)

EUROPEAN PHARMACOPOEIA 8.0

Extractable germanium : maximum 1 ppm.

Inductively coupled plasma-atomic emission spectrometry
(2.2.57).
Test solution. Solution S4.
Reference solutions. Prepare the reference solutions using
germanium standard solution (100 ppm Ge) R, diluting with
0.01 M sodium hydroxide.
Wavelength : 206.87 nm or 265.12 nm, the spectral background
being taken at 206.75 nm.
Extractable manganese : maximum 1 ppm.
Inductively coupled plasma-atomic emission spectrometry
(2.2.57).
Test solution. Solution S3.
Reference solutions. Prepare the reference solutions using
manganese standard solution (100 ppm Mn) R, diluting with
0.1 M hydrochloric acid.
Wavelength : 257.61 nm, the spectral background being taken
at 257.50 nm.
Verify the absence of manganese in the 0.1 M hydrochloric
acid used.
Extractable titanium : maximum 1 ppm.
Inductively coupled plasma-atomic emission spectrometry
(2.2.57).

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

3.1.15. Polyethylene terephthalate for containers

Test solution. Solution S3.

Reference solutions. Prepare the reference solutions using
titanium standard solution (100 ppm Ti) R, diluting with 0.1 M
hydrochloric acid.
Wavelength : 323.45 nm or 334.94 nm, the spectral background
being taken at 323.35 nm.
Verify the absence of titanium in the 0.1M hydrochloric acid
used.
Extractable zinc : maximum 1 ppm.
Inductively coupled plasma-atomic emission spectrometry
(2.2.57).
Test solution. Solution S3.
Reference solutions. Prepare the reference solutions using
zinc standard solution (100 ppm Zn) R, diluting with 0.1 M
hydrochloric acid.
Wavelength : 213.86 nm, the spectral background being taken
at 213.75 nm.
Verify the absence of zinc in the 0.1 M hydrochloric acid used.
Sulfated ash (2.4.14) : maximum 0.5 per cent determined on
1.0 g.

405