Table Of Contentइंटरनेट मानक
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Whereas the Parliament of India has set out to provide a practical regime of right to
information for citizens to secure access to information under the control of public authorities,
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
to the public, particularly disadvantaged communities and those engaged in the pursuit of
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 538 (2000): Phenol (Carbolic Acid) [PCD 3: Petroleum,
Lubricants and their Related Products]
“!ा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”
l
IS 538:2000
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Indian Standard
PHENOL ( CARBOLIC ACID) — SPECIFICATION
(Second Revision )
ICS71.080.90
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002
November 2000 Price Group 5
Aromatic Hydrocarbons and Related Products Sectional Committee, PCD 8
—
FOREWORD
This Indian Standard (Second Revision) wasadopted bythe Bureau of Indian Standards after the draft finalized
byAromatic Hydrocarbons and Related Products Sectional Committee had been approved bythe Petroleum Coal
and Related Products Division Council.
Phenolisobtained fromcoaltar.inthefraction distilling between 170“Cand230“C.Thereaction ofsodium hydroxide
isapplied inthe recov~~, fo!lowed bytreatment with carbon dioxide and distillation ofthe separated phenol, Itis
alsoobtained from benzene sulphonic acid (C~H5S01H)byheating with sodium hydroxide or calcium hydroxide:
or from chlorobenzene byheating under pressure with sodium hydroxide in the presence of diphenyl oxide.
Phenol isused asan antiseptic, germicide and disinfectant. It isalso used in the manufacture ofcertain dyes and
picric acid.
This standard was first issued in 1955and revised in 1968. Inthe revised version requirement for boiling point was
omitted and use ofadehydrated sample in the determination ofcrystallization point was stipulated. However, the
committee responsible forpreparation ofthis standard decided torevise itagain inaccordance with thedevelopment
inand growing demand bythe petrochemical industry. Cognizance hasbeen taken ofthe developments inoverseas
specifications vis-a-vis requirements inIndian conditions. Thus thepresent standard hasbeen updated inaccordance
\viththe need of the industry and in the light ofthe past experience gained.
Therefore inthepresent version (Second Revision) ofthe standard twogrades ofthe material have been introduced
onthe basis ofassay and crystallization point. The grades are also meant for specific uselike pharmaceuticals and
forgeneral industrial purposes. The GCanalysis has been included asan alternative method for determination of
purity.
In the preparation ofthis standard, considerable assistance has been derived from the following publications:
1S01897:1977 Phenol, o-cresol, m-cresol,p-cresol, cresylic acid and xylenols for industrial use— Methods
of test
1S01S97-1 :1977 Part 1:General
1S01897-2:1977 Part 2:Determin ation ofwater-Dean and Stark method
1S0 1897-3:1977 Part 3:Determination ofneutral ails and pyridine bases
Iso 1897-4:1977 Part 4:Visual test for impurities insoluble insodium hydroxide solution (Excluding cresylic
acid and xylenols )
1S0 1897-5:1977 Part 5:Visual test for impurities insoluble inwater (Phenol only)
1S0 1897-10:1982 Part 10:Determination ofdry residue after evaporation onawater bath (Excluding cresylic
acid and xylenols )
1S0 1897-11:1983 Part 11:Determination.of crystallizing point (Excluding cresylic acid and ?@enols )
ASTM4961:1993 Gaschromatographic analysis ofmajor organic impurities inphenol produced bythe cumene
process
BS523:1964 Specification forphenol (withdmwn )
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 offnumerical values (revised )’. The number ofsignificant places retained inthe
rounded offvalue should be the same asthat of the specified value in this standard.
..—
IS538:2000
Indian Standard
PHENOL ( CARBOLIC ACID) — SPECIFICATION
(Second Revision )
1 SCOPE asagreed tobetween the purchaser and the supplier.
Insuchcasesthephenol content ofthehydrated phenol
This standard (Second Revision) prescribes the
shall be determined bythe Bromination method and
requirements and the methods of sampling and test
water content bythe method ofIS 1448[P: 40] :1967
forphenol (carbolic acid).
using 2or 10mlreceiver depending onwater content
2NORMATIVE REFERENCES and toluene ascarrier liquid.
The fotlowing standards contain provisions which 4.2 Volubility inWater
through, reference inthis textconstitute theprovisions
When10gofthematerialis tuixedwith 120rnlofdistilled
ofthestandard. Atthetime ofpublication, theeditions
water, the solution shall be complete and clear, and
indicated were valid. All standards are subject to
shall remain soafter standing for 30minutes at27“C.
revision and parties to agreements based on this
standard are encouraged toinvestigate the possibility 4.3’Thematerialshallalsocomplywiththerequirements
of applying the most recent edition of the standard prescribed in Table 1when tested according to the
indicated below: methods given in Annex Ato D.
IS No. Title Table 1Requirements for Phenol (-Carbolic Acid)
265:1993 Specification for hydrochloric acid S1 Characteristic Requirement Method
No. . ofTest,
(fourth revision )
GradeA GradeB Ref to
1070:1992 Reagent grade water (third Annex
revision )
(1) (2) (3) (4) (5)
1260(Part 1): Pictorial.marking for handling and i) Crystallization 40.3 39.5 A
1973 labeling ofgoods: Part 1Dangerous point,“C,&fin
goods (first revision )
ii) Moisture, percent 0.1 0.1 B
2362:-1973 Determination ofwater bythe Karl by mass, Max
Fischer method (jlrst revision) iii) Residueon 0.05 0.05 c
evaporation by
4905:1968 Methods for random sampling
mass, Max
5296:1995 Chloroform, pure and technical iv) Assay, percent 99.5 98.5 D
(second revision) bymess,Min
1448[P:40 ]: Methods oftest for petroleum and
5 PACKING AND MARKING
1987 its products [P:40] water by
distillation (first revision ) 5.1 Packing
3 GRADES
Thematerial shallbepacked inamber coloured ordark
blue glass bottles fitted with ground glass stopper
The material shall beoftwo grades, namely:
orasagreed tobetween thepurchaser and thesupplier.
a) Grade A, and
5.2 Marking
b) GradeB.
5.2.1 Each container shallbe securelyclosed and shall
4REQUIREMENTS
bear legibly and indelibly-the following information:
4.1 Description
a) Name and grade ofthe material;
The material shall be colorless to light pink liquid b) Lot orbatch number and date ofmanufacture:
and freefrom suspended matter at41 “C.Phenol may
c) Tare, gross and net mass; and
also be supplied as hydrated phenol containing a
specified quantity ofwater (4to 10percent by mass) d) Indication ofthe source ofmanufacture.
1
IS538:2000
5.2.2 Each container shall also be marked with 6 SAMPLING
Fig, 11ofIS 1260 (Part 1)along with the following
The method ofdrawing representativesamples ofthe
information printed in the space provided:
material and the criteria for conformity shall be as
POISON
prescribed in Annex E.
‘PROTECTFROMLIGHTANDMOISTURE’
7 TEST METHODS
5.2.3 BIS Certi@cation Marking
The container may also be marked with the BIS 7.1 Tests shall be conducted as prescribed in
Certification Mark. Annex Ato D.
5.2.3.1 The use ofthe Standard Mark isgoverned by 7.2 Quality ofReagents
the provisions of Bureau of Indian Standards Aet,
Unlessotherwisespecified,purechemicals anddistilled
1986and the Rulesand Regulations made thereunder.
water (see IS 1070 )shall be employed in the tests.
The details ofconditions under which the licence for
the use of the Standard Mark may be granted to NOTE—‘Pure chemicals’ shall mean chemicais that
manufacturers orproducers maybe obtained from the do not contain impurities, which affect the results of
Bureau of Indian Standards. analysis.
ANNEX A
[ Table 1, S1No. (i)]
DETERMINATIONOFCRYSTALLIZATIONPOINT
A-1 APPARATUS NOTES
1Any thermometer of’similar requirements and accuracy
A-1.1 Crystallization-Point Apparatus
may beused.
The apparatus is illustrated in Fig. 1. Aglass tube 2 The thermometer shall bear a certification from the
150 x 25-mm nominal size isplaced inside a 175 x National Physical Laboratory, New Delhi or any other
institution authorized bythe Government ot’klia to issue
38-mm test tube. The latter tube isflanged sothat it
such a certificate.
maybesupported centrally byametal cover plate, in
a 1000-ml tall-form beaker filled w ith water towithin
20 mm of the top. The wider tube is weighed with
leadshotsorsimilarmaterial andtheinnertubeisclosed
bymeans ofa cork which carries a glass stirrer and
through itscentre astandard thermometer. The stirrer
hasaloopofoutsidediameter ofabout 18mm,surround ~
the thermometer. The thermometer issofixed inthe
corkthat thebottom ofthe bulb isabout 15mm from
the bottom ofthe inner tube. Athermometer forthe -=---=--.----..
----.
-----
water-bath passes through a hole in the cover plate
-----
and is held by arubber ring.
A-1.2 Thermometer
Conforming tothe following essential requirements:
Range 15t0450c
Graduation 0,1“c
Longer lines, at each 0.5and 1‘C
Fully figured, at each 2‘c
Overall length, Max 430mm ~ SHOTS
Lengthofmain scale, Min 260mm
FIG.1 APPARATUFSORTHEDETERMINATIOONF
Error,Max +0.4“c CRYSTALLIZINPGQINT
2
IS 538:2000
A-1.3 Water-Bath the sample gently and continuously and record
A-1.4 Measuring Cylinders thermometer readingsat30s intervals. Thecwstallizing
point corresponds to the highest of the first five
50 mland 10mlcapacities,
consecutive readings during which the temperature
A-2PROCEDURE remains constant within 0.1 “C.
A-2.1Determination of Crystallization Point
If supercooling occurs, as shown by a rise in
Remove the inner tube from the c~stallization point temperature, observe the constant temperature after
apparatus and directly,pour aboutOOml ofthe sample the rise. Atemperature rise of 1‘C isthe maximum
(in liquid form )into it.Insert the cork carrying the allowable. Iffive consecutive readings within 0.i “C
thermometer and stirrer. Ifthesample hascommenced arenotobtained, record sixreadings commencing wth
tocrystallize, heat gently until itbecomes liquid and the point at which the maximum temperature isfirst
then cool Tapidly to determine the approximate attained. Plotthecompletecoolingcurveoftemperature
crystallizing point. Warm the tube in the water-bath against time and draw a straight line to lie evenly
at about 5 OCabove this point, so that the crystals between the first and second and between the fifth
melt, except for a trace necessary for seeding. and sixth points mentioned above. Extend this line
Replace the inner tube in itsjacket with the water in to meet the section of the cooling curve before the
theapparatus maintained at atemperature between 6 temperature rise. Reportthetemperature corresponding
and 8“Cbelow the expected crystallizing point. Stir tothe point ofintersection asthe crystallizing point.
ANNEX B
[ Table 1, 5’1No. (ii) ]
DETERMINATIONOFMOJSTIJRE
B-1 PROCEDURE
Determine the moisture content inphenol byKarl-Fischer method asprescribed in IS 2362,
ANNEX C
[( Table l, SINO. (iii)]
DETERMINATIONOFRESIDUEONEVAPORATION
C-1 -APPARATUS Overall length, Max 430 mm
C-1.l U-1’hbe-Stopperd Length ofmain scale, Min 240 mm
Error, Max +0.8 “c
Withlimbsabout 125x 15mm. Each limb isprovided
with a side tube as shown in Fig. 2. The stoppers NOTE--–The thermometer shall bear a certificate from
the NationaI Physical Laboratory, New Delhi orany other
shall not be greased.
institution authorized bythe Government ofIndia toissue
C-1.2 Air Bath such a certificate.
Acopper air bath about 150 x150 x150mm. C-1.4 Calcium Chloride ‘Ibbe
C-1.3Thermometer C-1.5 Conical Safety Flask
Conforming tothe following essential requirements: C-1.6 Suction Pump
Range 5oto210°c C-2 PROCEDURE
Graduation 0.5 “c C-2.1 Assemble the apparatus as shown in Fig. 2
Longer lines, ateach 1and 5“C without the U-tube. Heat the air bath to 150* 5‘C.
Fully figured, at each 10“c and maintain it at this temperature. Connect the
3
IS538:2000
U-tube and draw agentle stream ofair through it for andmaintain theair-bathat 150*5 ‘Cuntilevaporation
approximately half an-hour. Remove the U-tube, is complete. Disconnect the U-tube, fit the calcium
connect it byaside arm tothe calcium chioride tube chloride tube to one side arm and close the other to
andclosetheother sidearm totheatmosphere. When the atmosphere. When the tube is cool, weigh it as
cool,remove the calcium chloride tube and weigh the before. Repeat-theheating, cooling andweighing until
U-tube towithin 0.0001 gwith both stoppers closed. a constant mass is obtained.
C-2.2 Weighaccurately about 10gofthe sample into C-3 CALCULATION
M,
the U-tube, at the lowest temperature for complete
Residue onevaporation, percent bymass =~ x 100
liquidity. Reconnect the U-tube tothe train and make
where
sure that the bottom ofthe thermometer bulb islevel
with the bottom ofthe U-tube. Ml =massing of the residue left, and
C-2.3Drawagentlestreamofairthrough theapparatus A42=mass in gofthe sample taken for the test.
FM.2 APPA RATUFSORTHEDETERMINATIOONFRESIDUEONEVAPORATION
ANNEX D
[ Ta31e 1, S1No. (iv)]
DETERMINATIONOFASSAY
D-1GENERAL bromine and ifthese are present they will invalidate
the results.
Two methods have been specified for determination
of assay of phenol Method A is bromide-bromate D-2.2 Reagents
volumetric method while Method B is the gas
D-2.2.1Chloroform (see 1S5296 ).
chromatographic method. In case ofdispute method
Ashall be the referee method. D-2.2.2 Concentrated [{vdrochloric acid ( see
D-2BROMIDEBROMATE SOLUTION METHOD 1S265).
(METHOD A)
D-2.2.3 Potassium Iodide Solution 20percent (mlv)
D-2.1Outline ofthe Method
Dissolve 20 gofpotassium iodide in 10Oml ofwater.
The method isbased onthe reaction between phenol
D-2.2.4 Standard Br(~t~licle-[3r{~rtla(eSolution
andbromine from standard bromide-bromate solution .
Other phenols and unsaturated compounds reactwith ().1N
4
..
Is 538:2000
Dissolve 10.2gofpotassium bromide and 2.784 gof titrate the contents with the standard sodium
potassium bromate inwater and dilute to 1000 ml in thiosulphate solution until only afaint yellow colour
avolumetric flask. remains. Add 10miofchloroform todissolvethebulky
precipitate ofbromophenol which, otherwise, isliable
D-2.2.5 Standard Sodium Thiosulphate Solution
to absorb iodine, and follow by afew drops ofstarch
O.lN solution. Continue titrating and shaking the contents
ofthe flaskuntil the last traces oftheblue colour hafc
Dissolve 25 g of sodium thiosulphate in water and
disappeared. Record the volume of the sodium
dilute to 1000 ml. Itisessential tofind outthefactor thiosulphate solution used.
ofthe sodiumthiosulphate solution immediately before
use, as follows: D-2.5 Calculation
Pipette 25mlofthebromide-bromate solution intothe “Eachmlof0.1 Nbrmnide-brornate solution consumed
iodineflask,add 5mlofthepotassium iodidesolution, isequivalent to0.001568 gofphenol.
followed by 5 ml of hydrochloric acid. Stopper
6.272 (50 -P)
immediatelyand shakethoroughly. Titmtetheliberated Assay, percent by mass=
M
iodine with the sodium thiosulphate solution until the
where
contents ofthe flask become only faintly yellow, add
afewdropsofstarch solutionand continuethetitration -f = factor for the standard sodium thiosolphatc
untilthelasttracesofthebluecolourhavedisappeared. solution (see D-2.2.5 );
The factor ‘~’ofthe sodium thiosulphate solution is v = volume, in ml, of the standard sodium
25/v,wherevisthevolume (ml)ofsodiumthiosulphate thiosulphate solution used; and
solution used.
M= Mass, in g, ofthe sample taken for the test.
D-2.2.6 Starch Solution
D-3 GAS CHROMATOGRAPHIC METHOD
Freshly prepared. (METHOD B)
D-3.1 General
D-2.3Apparatus
This method determines the concentration of major
D-2.3. 1Iodine Flask
impurities such as mesityl ox-ide, cumcnc.
300-ml capacity. cc-methylstyrene, 2-methylbenzofuran, acetophenonc.
and dimethylbenzyl alcohol.
D-2.3.2 Measuring Cylinders
D-3.2 Outline oftheMethod
One of 100ml and three of25ml capacities.
Aknown amount ofinternal standard isadded tothe
D-2.3.3 Pipettes sample. Aportion of the sample is analyzed by gas
chromatography. The concentration ofeach impurit!
50mland 25mlcapacities.
iscalculated relative tothe known amount ofinterns I
D-2.3.4 Burette standard that is added. It is useful for individuill
impurities inthe range 10to 100mg/lcg.
50-ml capacity
-D-3.3Appara@s
D-2.4 Procedure
D-3.3.1 Chromatography
Weighaccuratelyabout2.5gofthesampleanddissolve
Equipped with an on-column injector and flame
itinwate~ diluteto 1000 mlwithwaterinavolumetric
ionization detector.
flask.Pipette25mlofthis solutionintotheiodineflask
andadd?0mlofthebromidehxnate solution,followed D-3.3.2 Recorder
by5ml ofhydrochloric acid. Stopper immediately and
With afull scaleof”1mVand aresponse time of 1sor
sealbyrunning alittleofthepotassium iodidesolution
less.
into the annular space between the stopper and the
funnel-shqedneck ofthe flask. Mix the contents of D-3.3.3 Integrating Device
the flask by occasional swirling during half an hour
Anydevicecapableofintegrating chromatographypeak
and then leave to stand for a further period of 15
areas with arepeatability ofl1percent relative.
minutes. Gradually add 15ml of potassium iodide
solution to the contents of the flask by pouring the D-3.3.4 C’hromatographic Column
solution into the annular spaceonthe neckand gently
Glass (2-mm inside diameter) orNickel 200 (5.3 mm
easing the stopper. Shake the flask thoroughly and
inside diameter by 3mlength). The column may bc
5
