IS 13360-10-6: Plastics - Methods of testing, Part 10: Resin (thermosetting properties), Section 6 Phenol-formaldehyde mouldings - Determination of free ammonia and ammonium compounds - colorimetric comparison method

2004·0.99 MB·English

by  Bureau of Indian Standards

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IS 13360-10-6 (2004): Plastics - Methods of testing, Part
10: Resin (thermosetting properties), Section 6
Phenol-formaldehyde mouldings - Determination of free
ammonia and ammonium compounds - colorimetric comparison
method [PCD 12: Plastics]
“!ान $ एक न’ भारत का +नम-ण”
Satyanarayan Gangaram Pitroda
““IInnvveenntt aa NNeeww IInnddiiaa UUssiinngg KKnnoowwlleeddggee””
“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता हहहहै””ै”
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IS 13360 (Part 10/See 6) :2004
1s0
120:1977

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Indian Standard
PLASTICS — METHODS OF TESTING
PART 10 RESIN (THERMOSETTING PROPERTIES )
Section 6 Phenol-Formaldehyde Mouldings — Determination of Free Ammonia and
Ammonium Compounds — Calorimetric Comparison Method
ICS 83.080.10

Q BIS 2004
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

December 2004 Price Group 1
Plastics Sectional Committee, PCD 12
NATIONAL FOREWORD
This Indian Standard (Part 10/See 6) which is identical with ISO 120 : 1977 ‘Plastics — Phenol-
formaldehyde mouldings — Determination of free ammonia and ammonium compounds —
Calorimetric comparison method’ issued by the International Organization for Standardization (ISO)
was adopted by the Bureau of Indian Standards on the recommendations of the Plastics Sectional
Committee and approval of the Petroleum, Coal and Related Products Division Council.
The text of ISO Standard has been proposed to be approved as suitable for publication as an Indian
Standard without deviations. Certain conventions are, however, not identical to those used in Indian
Standards. Attention is particularly drawn to the following:
a) Wherever the words ‘International Standard’ appear referring to this standard, they should be
read as ‘Indian Standard’.
b) Comma (,) has been used as a decimal marker, while in Indian Standards, the current
practice is to use a point (.) as the decimal marker.
CROSS REFERENCES
In this adopted standard reference appears to certain International Standards listed below for which
Indian Standards also exist. The corresponding Indian Standards, which are to be substituted in their
place, are given below along with their degree of equivalence for the editions indicated. However, that
\nternatlonal Standard cross-referred in this adopted Iso standardwhich has subsequently been
revised, position in respect of latest ISO Standard has been given:
International Standard Corresponding Indian Standard Degree of

Equivalence

ISO 565 : 1990 Test sieves — metal IS 460 (Part 1) :1985 Test sieves: Part 1 Technically
wwe cloth and perforated metal plate — Wire cloth test sieves (third revision) equivalent
Nominal sizes of apertures with minor
IS 460 (Part 2 ) :1985 Test sieves: Part 2
deviations
Perforated plate test sieves (third
revision)
ISO 648 : 1977 Laboratory glasswares IS 1117 : 1975 One-mark pipettes (first do
--- One-mark pipettes revision)
For tropical countries like India, the standard temperature and the relative humidity shall be taken as
27 t 20C and 65 ~ 5 percent respectively.
In reporting the results of a test or analysis made m accordance with this standard, if the final value,
observed or calculated, is to be rounded off, it shall be done in accordance with IS 2: 1960 ‘Rules for
rounding off numerical values (revised)’.
IS 13360 (Part 10/See 6) :2004
1s0 120: 1977
Indian Standard
PLASTICS — METHODS OF TESTING
PART 10 RESIN (THERMOSEITING PROPERTIES )
Section 6 Phenol-Formaldehyde Mouldings — Determination of Free Ammonia and
Ammonium Compounds — Calorimetric Comparison Method
1 SCOPE AND FIELD OF APPLICATION 5 APPARATUS
This International Standard specifies a calorimetric Ordinary laboratory apparatus, and
comparison method for the semi-quantitative determination
of the amount of ammonia in phenol-formaldehyde 5.1 Means for reducing the mouldings to apowder.
mouldings.
5.2 Sieve, with nominal apertures of 250 pm, conform-
NOTE – This international Standard does not provide an absolute
measure of the ammonia present. ing to ISO 565.
The amount of ammonia in a moulded article is of 5.3 Salance, accurate to 0,01 g.
importance when corrosion of metal inserts or contami-
nation of foodstuffs in contact with the article has to be
5.4 Glass-stoppered flask, 250 ml capacity.
considered.
5.5 Distillation apparatus, comprising a flask of 250 ml
2 REFERENCES capacity, splash head and acondenser.
ISO 565, Test sieves – Woven metal wire cloth and
5.6 Filter funnel, with hardened medium speed filter
perforated plate – Nominal sizes of apertures.
paper.
ISO 648, Laboratory glassware – One-mark pipettes. 1)
5.7 Pipettes, capacities 2 and 10 ml, complying with the
requirements of ISO 648.
3 PRINCIPLE
Hot aqueous extraction of free ammonia from apowdered 5.8 Nessler cylinders, 50 ml capacity.
test portion. Distillation of the aq ueous extract in the

presence of potassium permanganate and sodium hydroxide

solution. Coloration of the distillate by reaction with 6 PREPARATION OF TEST SAMPLE
Nessler reagent and comparison of the colour with that
obtained in each of aseries of standard matching solutions. Reduce a fully representative sample of the mouldings to
powder by filing, milling, grinding, turning or drilling,
taking care that no undue heating of the material occurs.
4 REAGENTS Sieve this powder, using the sieve (5.2), and use for the test
that portion passing through the sieve. Keep the sample
During the analysis, use only ammonia-free reagents of
in atightly stoppered flask until required.
recognized analytical grade, and only ammonia-free distilled
water or water of equivalent purity. The extraction with water (see 7.2) shall begin within 1 h
of grinding the moulding.
4.1 Potassium permanganate.
NOTE – The method of reduction to powder can affect the results.
In cases of dispute, or for referee purposes, the method should be
4.2 Sodium hydroxide, 2 % (m/m) solution. agreed between the interested parties.
4.3 Standard matching stock solution, containing 10 mg
of NH3 per Iitre. 7 PROCEDURE
Dissolve 31,5 mg of ammonium chloride in 1000 ml of
7.1 Test portion
water.
Weigh, to the nearest 0,01 g, 5 k 0,1 gof the sieved material
4.4 Nessler reagent. (see clause 6).
1) At present at the stage of draft. (Revision of lSO/R 648. )
IS 13360 (Part 10/Sec 6) :2004
1s0 120: 1977
7.2 Preparation of the test solution 8 EXPRESSION OF RESULTS
Place the test portion (7.1 ) in the flask (5.4) and cover it The amount of free ammonia and ammonium compounds,
with ten times its mass of water at a temperature of 90 to expressed as a percentage by mass of ammonia (NH3 ), is
100 “C. Stopper the flask and shake it so that the powder is given by the formula
thoroughly wetted. Allow it to cool at room temperature,
mxD
for 1 h, with occasional shaking. Then filter the contents of
10
the flask, without suction, through the filter funnel (5.6).
Transfer, with a pipette (5.7), 10 ml of the filtered extract,
where
corresponding to 1g of the powder, into the flask of the
distillation apparatus (5.5). m is the mass, in milligrams, of ammonia contained in
the appropriate standard matching solution from the
NOTE – Before using the distillation apparatus, it isrecommended
series (see 7.3);
that it should be freed from any ammonia which may be present by
distilling a quantity of distilled water in it until the ,xJditio” of z ml
D is the dilution factor in the case where the filtrate is
of Nessler reagent (4.4) to 50 ml of distillate does not give rise to
any colour. diluted before distillation :
Add to the flask 0,1 gof potassium permanganate (4.1) and
10 ml of the sodium hydroxide solution (4.2). Slowly distil
the mixture; collect the first 15 ml of the distillate in a
Nessler cylinder (5.8) and dilute to 50 ml with water. where
V, is the volume in millilitres of the portion of the
7.3 Determination
filtered extract before dilution (VI = 10 ml);
Transfer, with a pipette (5.7), 2 ml of the Nessler reagent
Vz is the volume in millilitres of this 10 ml portion
(4.4) into the Nessler cylinder and determine the ammonia
of the filtered extract after dilution.
content by matching the colour of the test solution (7.2)
with that of one of a series of standard matching solutions
9 TEST REPORT
to which Nessler reagent has been added at the same time as
to the test solution. To make the standard matching The test report shall include the following particulars :
solutions transfer, with a pipette, 1, 2, 3, 4, 5 and 6 ml
portions of standard matching stock solution (4.3) into a) reference to this International Standard;
each of a series of six Nessler cylinders (5.8) and dilute
b) full details necessary for the identification of the
to 50 ml with water. These correspond to 0,01, 0,02, 0,03,
sample;
0,04, 0,05 and 0,06 mg of ammonia.
c) the method used for reducing the mouidings to
NOTE – If the 15 ml of distillate is found to contatin more than powder;
0,06 mg of ammonia, a 10 ml portion of th e filtered extract shall be

suitably diluted and a 10 ml portion of this dil uted solut!on used in d) amount of free ammonia;
the distillation. An appropriate dilution facto r should be used in
the calculation. e) date of the test.

2
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ments or edition by referring to the latest issue of ‘BIS Catalogue’ and ‘Standards: Monthly Additions’.
This Indian Standard has been developed from Doc : No. PCD 12 (1797).
Amendments Issued Since Publication
Amend No. Date of Issue Text Affected
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