IS 15621: Terabromobisphenol-A

2005·1.3 MB·English

by  Bureau of Indian Standards

इंटरनेट मानक
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in order to promote transparency and accountability in the working of every public authority,
and whereas the attached publication of the Bureau of Indian Standards is of particular interest
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education and knowledge, the attached public safety standard is made available to promote the
timely dissemination of this information in an accurate manner to the public.
“जान1 का अ+धकार, जी1 का अ+धकार” “प0रा1 को छोड न’ 5 तरफ”
Mazdoor Kisan Shakti Sangathan Jawaharlal Nehru
“The Right to Information, The Right to Live” “Step Out From the Old to the New”
IS 15621 (2005): Terabromobisphenol-A [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””ै”
Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”

IS 15621:2005

Indian Standard
TETRABROMOBISPHENOL-A —
SPECIFICATION
ICS 71.080.90

0 BIS 2005
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

Price Group 4
September 2005
;,
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Plastics Sectional Committee, PCD 12
FOREWORD
This Indian Standard was adopted by the Bureau of Indian Standards, after the dratl finalized by the Plastics
Sectional Committee had been approved by the Petroleum, Coal and Related Products Division Council.
Tetrabromobisphenol-A is used for flame retardant applications in polymeric resin such as thermoplastics,
thermosetting, rubber foams, coatings, etc and other products like textiles, etc.
For the purpose of deciding whether aparticular requirement ofthis standard iscomplied with, the final value,
observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance with
IS2:1960 ‘Rules for rounding off numerical values (revised)’. Thenumber ofsignificant places retained inthe
rounded off value should be the same asthat of the specified value inthis standard.

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IS 15621:2005
Indian Standard
TETRABROMOBISPHENOL-A —
SPECIFICATION
1SCOPE liner and finally packed in plastic woven sack of
sizes as agreed to between the purchaser and the
This standard prescribes requirements and methods
supplier.
of sampling and test for Tetrabromobisphenol-A.
5.2 Marking
2 REFERENCES
The material shall be marked with the following
The following standards contain provisions which,
information:
through reference inthe text, constitute provisions of
this standard. At the time of publication, the editions a) Name of the material;
indicated were valid. All standards are subject to b) Manufacturer’s name, initials or trade-mark, if
revision and parties to agreements based on this any;
standard are encouraged to investigate the possibility ,.. .
c) Net mass of material; and
of applying the most recent editions of the standards 1 “,
;; ,
indicated below: d) Identification incode orotherwise toenable the !
$’:
lotof consignment ormanufacture to be traced
IS No. Title ii ‘i
back from records.
264:1976 ‘ Nitric acid (second revision) /;\,: ‘;
?,,
265:1993 Hydrochloric acid (fiourth 5.2.1 BIS Certzfzcation Marking
revision)
The container may also be marked with the Standard
517:1986 Specification for methanol Mark.
(second revision) $
5.2.1.1 The use of Standard Mark isgoverned by the ,..?
1070:1992 Reagent grade water (third provisions o~theBureau ofIndian Standar& Act, 1986 ‘.#
revision)
and the Rules and Regulations made thereunder. The
2828:2001 Plastics — Vocabulary details of conditions under which the licence for the
)
4905:1968 Methods for random sampling use of the Standard Mark may be granted to
manufacturers orproducers maybe obtained from the
3 TERMINOLOGY Bureau of Indian Standards.

For the purpose of this standar d, definitions given in 6 SAMPLING AND CRITERIA FOR
IS2828 shall apply. CONFORMITY
4 REQUIREMENTS Representative samples ofthe material shall be drawn .
and conformity of the material to the requirement of
4.1 Description
this s~ecification shallbe determined according—to the ,.
,?
The material shall be inthe form of awhite powder. proc~dure prescribed in Annex M.
4.2 The material shall also comply with the 7 TESTS
requirements given in Table 1when tested according
7.1 Tests shall be carried out as given in CO14 of t
to the methods given in CO14of Table 1.
Table 1.
5 PACKING AND MARKING
7.2 Quality of Reagents
5.1 Packing i
Unless specified otherwise, A.R. grade chemicals and
The material shall be packed in polyethylene inner distilled water shall be used intests (see IS 10’70).

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IS 15621:2005
Table 1 Requirements for Tetrabromobisphenol
(Clause 4.2)
S1No, Characteristics Requirements Method ofTest,
ReftoAnnex
(1) (2) (3) (4)
i) Assay,percent,Mirr 99.0 A
ii) Meltingpoint,‘C,&fin 180.0 B
iii) Colour,APHA,Mu-x 20.0 c
iv) [onisablebromide,ppm,Max 50.0 D
v) Hydrolyzablebromide,ppm,J44izx 50.0 E
vi) pH 6.0-7.0 F
vii) Turbidity,NTU,Max 5.0 G
viii) Ironcontent,ppm,Max 1.0 H
ix) Moisturecontent ppm,A&c 1000 J
x) Volatilecontent,ppm,Mu-x 500 K’
xi) Brominecontent,perceng&fin 58.0 L
ANNEX A
[Table 1,S1No. (i)]
DETERMINATION OF ASSAY BY CHROMATOGRAPHIC ANALYSIS
.,
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A-1 APPARATUS A-3.2 Mobile Phase
A-1.l High Performance Liquid Chromatograph Mobile phase is 80 (methanol): 20 (15 percent acetic
(Isocratic) acid inwater). Flow rate: 1.0mllmin.

A-1.2 UV-VIS Detector A-3.3 Run Time
.
A-1.3 Data Station 10.0min.
A-1.4 Printer A-4 PROCEDURE
A-1.5 Micro Litre Syringe Switch on the mains and start the instrument. Prime
thepump for about 5.0min and flush the system with
A-1.6 Volumetric Flask, 100ml.
100percent methanol for half an hour, then flush the
A-1.7 Column, C18 micro Bondapak. systemwiththemobile phase for half anhour. Setthe
detector at 290 nm. Check the base line, if a steady
A-2 REAGENTS base line isobserved then inject 20 VIstandard tetra-
bromobisphenol-A andrun the instrument for 10min.
A-2.1 Methanol
Note down the retention time. Then inject 20 pl test
A-2.2 Water sampleandnotedowntheretention time.Asharppeak
appears at about 6.8 min is tetrabromobisphenol-A.
A-2.3 Acetic Acid (An impurity peak, tribromobisphenol-A peak
appears at about 5.4 rein, bisphenol-A peak appears
A-3 SAMPLE PREPARATION
at about 3.7 rein). Note down the area percent of
A-3.1 Weigh accurately about 0.100 g of sample in each peak from the chromatogram and report
100ml volumetric flask and dissolve inmethanol and (100 percentage of corqponents other than tetra-
make up to volume with methanol. Filter through bromobisphenol-A is the chromatographic purity of
Whatman filter paper No. 42. TBBA).
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IS 15621:2005
ANNEX B
[Table 1,S1No. (ii)]
DETERMINATION OF MELTING POINT
B-1 APPARATUS B-2 PROCEDURE
B-1.l Glass Heating Vessel —Suitable construction B-2.1 Dry a small quantity of the finely powdered
andcapacitycontaining oneofthefollowingoranother substance at 105+2°Cfor2h. Transfer aportion to a
suitable liquid, to aheight of not lessthan 14cm. dry capillary tube andpack the powder by tapping on
a hard surface so asto form atightly packed column
B-1.1.1Liquid Paraffin — Having sufficiently high
4 to 6 mm in height. Heat a suitable liquid in the
boiling point
heating vessel and regulate the rate of rise of
B-1.1.2 Silicone Fluid — Having sufficiently high temperature prior to the introduction of the capillary
boiling point. tube to 1°/min, when the temperature reaches 10°
below the lowest figure ofthe range for the substance
B-1.2 Suitable Stirring Device— Capable ofrapidly
being tested insertthe capillary tube. The temperature
mixing the liquid.
at which the lastparticle disappear isregarded as the
B-1.3 Calibrated Thermometer — Suitable for the melting point of the substance, for substances that
substance being carried complying with the decomposes thetemperature atwhich frothing begins.
requirements. Correct the observed temperature for any error in the
calibration of the thermometer and of the difference,
B-1.4 Thin Walled Capillary, of hard glass, closed
if any.
at one end, with awall thickness of 0.10 to 0.15 mm
atleast 12cm inlength andof internal diameter 0.9to B-2.2 The apparatus should be periodically calibrated
1.1mm. Thetubes should bepreferably bekeptsealed using certified reference substances of declared
at both ends and cuts asrequired. melting point.
ANNEX C
[Table 1,Sl No. (iii)] 1:
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DETERMINATION OF COLOUR (APHA)
C-1 APPARATUS C-2.2 Methanol ‘,)

C-3 PROCEDURE
C-1.1 Spectrophotometer

Prepare standards of 10, 20 and 30 Hazen units in .
C-1.2 Cuvettes, 1cm.
methanol using the 500 Hazen unit stock solution. )
Prepare a20 percent sample solution in methanol by
C-2 REAGENTS
dissolving 4.0 g sample in 20 ml of methanol. Filter %
C-2.1 Standard 500 Hazen Unit Solution thesolutionthrough Whatman filter paper No. 42. Set
the UV-VIS spectropkotometer at 385 nm, use
Prepare 500 Hazen unit standard solution by methanol as blank, make auto zero, using methanol.
f
dissolving 0.25 g of cobalt chloride and 0.2625 g of Put the standard 10hazen unit standard solution and
chloroplatinic acid (or 0.311 3 g of potassium make auto concentration 10.0 and check the
chloroplatinate) with 25 ml of concentrated concentration for 20and 30hazen standard solutions.
hydrochloric acid in a 250 ml volumetric flask and Now putthe sample solution, record the concentration
I
dilute it up to the mark with demineralized water. and report the colour asAPHA.

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1S 15621:2005
ANNEX D
[~dze 1, (iv)]
.y] N().
DETERMINATION OF IONIZABLE BROMIDE
D-1 APPARATUS and 10-15drops offerroin indicator andtitrate against
0.0lN ammonium thiocyanate solution till pale brick
D-1.l Conical Flask, 250 ml.
red coloured end point is obtained. Carry out a blank
titration without the sample. Note down the volume
D-2 REAGENTS
ofammonium thiocyanate solutionaddedandcalculate
D-2.1 Nitric Acid, Concentrated, see IS264. the ionic bromide content as given below.
D-2.2 Silver Nitrate Solution, 0.0lN. D-4 CALCULATION
D-2.3 Ammonium Thiocynate Solution, O.OIN. (B-A) XNX 79.904 ~ ~03
Ionic bromide, ppm =
M
D-2.4 Nitro Benzene
where
D-2.5 Ferroin Indicator
A. volume of standard ammonium thiocyanate
solution used intitration of sample, in ml;
D-3 PROCEDURE
B. volume of standard ammonium thiocyanate
Take 10.0 g of sample in a 250 ml conical flask and
solution used for blank, in ml;
add 100ml water, mix properly and acidi~ with lml
of concentrated nitric acid and add 10 ml of 0.0lN A/f. mass of sample, in g; and
silver nitrate solution. Add 2-3 drops of nitrobenzene N. normality of ammonium thiocyanate solution.
ANNEX E
[Table 1,S1No. (v)]
DETERMINATION OF HYDROLYZABLE BROMIDE
E-1 APPARATUS of nitrobenzene and 10-15 drops of ferroin indicator
and titrate against 0.01 N ammonium thiocyanate
E-1.1 Round Bottom Flask, 250 ml. solution till pale brick red coloured end point is
obtained. Carry out a blank titration without the
E-1.2 Reflux Condenser
sample. Note down the volume of ammonium
E-2 REAGENTS thiocyanate solution added and calculate the .
hydrolyzable bromide content as given below.
E-2.1 Concentrated Nitric Acid
E-4 CALCULATION
E-2.2 Silver Nitrate Solution, 0.01 N.
(B-A) x NX 79.904 x lo,
Hydrolyzable =
E-2.3 Ammonium Thiocynate Solution, 0.01 N.
M
bromide, ppm
E-2.4 Nitro Benzene
where
E-2.5 Ferroin Indicator
A = volume of standard ammonium thiocyanate
solution used intitration of sample, in ml;
E-3 PROCEDURE
B = volume of standard ammonium thiocyanate
Take 10.0gof sample ina250 ml round bottom flask
solution used for blank, in ml;
and add 100 ml demineralized water, reflux for 2 h,
M= mass of sample, ing; and
cool and add 5ml of concentrated nitric acid and add
zo mIof 0.01 N silver nitrate solution. Add 2-3 drops N= normality of ammonium thiocyanate solution.
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IS 15621:2005
ANNEX F
[Table 1,S1No. (vi)]
DETERMINATION OF pH
F-1 APPARATUS F-3 PROCEDURE
F-1.l Digital pH Meter Take 5 g sample in a mortar and grind well. Add 45
ml distilled water and mix thoroughly. Check thepH
F-1.2 Beaker, 50 ml.
using thePI-Imeter and report.
F-2 REAGENTS
F-2.1 Distilled Water, pH 7.0.
ANNEX G
[Table 1,S1No. (vii)]
DETERMINATION OF TURBIDITY
G-1 APPARATUS methanol and dissolve. Using nephelometer, prepare
a calibration curve using 10 NTU, 20 NTU and
G-1.1 Digital Calibrated Turbidity Meter
30 NTU standard turbid solutions. Measure the
turbidity of the sample and report.
G-1.2 Nessler Tube, 50 ml.
NOTE—Take2.5ml4000 NTUsolution anddilute upto
G-2 REAGENTS 100mlwithdistilled/demineralizedwatertomake 100NTU
solution.Nowtake10,20, and30mlofthksolutionanddilute
G-2.1 Methanol — A.R. grade (see IS 517).
up to 100ml with distilled/demineralized water to make
10NTU,20NTUand30NTUsolution.
G-3 PROCEDURE
Weigh4.0 gsample in50mlNessler tube. Add20ml
ANNEX H

[Table 1,S1No. (viii)]

DETERMINATION OF IRON CONTENT
H-1 APPARATUS hydrochloride in 60 ml water, filter and make up to
100ml with water.
H-1.1 Spectrophotometer
H-2.4 1,10Phenanthroline Solution—Dissolve 0.9 g
H-1.2 Round Bottom Flask, 150ml.
1,10phenanthroline monohydrate in30mlofmethanol
H-1.3 Volumetric Flask, 100ml. and dilute to 300 ml with water.
H-1.4 Beaker, 100ml. H-2.5 Ammonium Acetate-Acetic Acid Solution —
Dissolve200 gofammonium acetate in600ml water,
H-1.5 Reflux Condenser
filter and add 50ml of acetic acid and dilute to 1000
ml with water.
H-1.6 Whatman Filter Paper No. 42
H-2 REAGENTS H-2.6 Standard Iron Solution —Dissolve7.02168 g
of ferrous ammonium sulphate (100 percent) in
H-2.1 Concentrated Hydrochloric Acid A.R. 100mlwaterandadd30mlofconcentrated. sulphuric
grade (see IS265). acid and make up to 1000 ml in a volumetric flask
(1 000 ppm). 1ml of this solution contains 1.0 mg.
H-2.2 Water — HPLC grade.
Take 5.0ml anddilute to 500ml inavolumetric flask
H-2.3 10 Percent Hydroxylamine Hydrochloride (10 ppm) .1 ml of this solution is equivalent to
Solution — Dissolve 10gA.R. grade hydroxylamine 10microgram of iron.
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