IS 15030: Terephthalic Acid

19 Pages·2001·1.7 MB·English

by  Bureau of Indian Standards

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and whereas the attached publication of the Bureau of Indian Standards is of particular interest
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timely dissemination of this information in an accurate manner to the public.
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“The Right to Information, The Right to Live” “Step Out From the Old to the New”
IS 15030 (2001): Terephthalic Acid [PCD 9: Organic
Chemicals Alcohols and Allied Products and Dye
Intermediates]
“!ा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 15030:2001 &a
W7mTWFF
NF1—Rmqftl-s-fafmz

Indian Standard
TEREPHTHALIC ACID — SPECIFICATION
ICS71.080.40

0 BIS2001
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

November2001 Price Group 7
-.-q
OrganicChemicals (Miscellaneous) SectionalCommittee,PCD9
FOREWORD
This Indian Standard was adopted by the Bureau of Indian Standards, after the draft finalized by the Organic
Chemicals(Miscellaneous) SectionalCommitteehadbeenapprovedbythePetroleum, CoalandRelatedProducts
DivisionCouncil. 1
*
Terephthalicacid(C8HC0,)isderivedbyoxidationofpara-xylene. Itisalsocommercially knownaspara-phthalic
acid;benezene-para-dicarboxylic acidor1,4benzenedicarboxylicacid. Itisrepresentedbythefollowingstructural
andmoleculw forrnuale:
COOH

y-“-
(MOLECULAWREIGHT- 176) ,!.
fy: ’
[MolecularFormula: C,H,(COOH),]
.
Itisused intheproduction ofsynthetic resins, fibers and filmsbycombination withglycols.
Composition oftheCommittee responsible forformulation ofthisstandard isgiven inAnnex K.
For thepurpose ofdeciding whether aparticular requirement ofthisstandard iscomplied with, thefinal value,
observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance with
IS2:1960 ‘Rulesforrounding offnumerical values(revised). Thenumberofsignificant placesretained inthe
rounded off value should bethe same asthat of the specified value inthis standard.
_
Is 15030:2001
,
Indian Standard
TEREPHTHALIC ACID — SPECIFICATION
1 SCOPE Table 1Requirements For Terephthalic Acid
This standardprescribes requirements andmethodsof (Clause3.2)
sampling andtestforpure terephthalic acid.
S1 Characteristic Requirement Method of Test
No. (Ref to Annex)
2 REFERENCES
(1) (2) (3) (4)
The following Indian Standards contain provisions i) Moisture content, 0.2 A
percent by mass, Max
which through reference in this text, constitute the
ii) Colour, in Hazen 10 B
provisions ofthisstandard. Atthetimeofpublication, units, Mu
the editions indicated were valid. All standards are iii) Ash content, 10 c
subject torevision andparties toagreements based on ppm,Max
iv) Acid value, 675*2 D
this standard are encouraged to investigate the
mgKOFf/g
possibility of applying the most recent editions ofthe v) Total of iron, cobalt, 8(each not E
standard indicated below: manganese and greater than
chromium 2 ppm)
ISNo. Title vi) Total of sodium, iO(each not F
magnesium, potassium, greater than
265:1993 Hydrochloricacid~ourthrevision) calcium and Nickel 2 ppm)
ppm, Max
266:1993 Sulphuric acid(third revision)
vii) 4-carboxybenzaldehy de, 20 G (Method A,
460(Patt1):1985 Specification for test sieves : ppm, Max andMethod C)
Part 1 Wire cloth test sieves viii) p-toluic acid, ppm, 150 G(Method A
(third revision) Max and Method B)
915:1975 One-mark volumetric flasks 4 PRECAUTIONS IN HANDLING
(’@Wrevision)
Terephthalic acid has very low toxicity. The use of
1070:1992 Specification forwaterforgeneral
dust masks is advisable when handling terephthalic
laboratory use (third revision)
acid. Finely divided organic products which are
2362:1993 Determination of water by Karl
combustible are liable to explosion should the dust
Fisher method (firstrevision)
contentoftheatmospherebehighandif ignitionoccurs.
4161:1967 Nessler cyli nders

Goodhousekeepingis,thete.fore,advisabletominimize

3 REQ~ theamount ofdust when terephthalic acid ishandled.
The atmosphere of any silo or pneumatic transfer
3.1 Description
equipment where dust explosions could occur should
beblanketedwithinertgastobelow 10volumepercent
The material shall be in the form of white crystalline
oxygen content.
freeflowingpowderandfreefromextraneous impurities
like dust and dirt. Terephthalic is insoluble in water, 5 PACKING AND MARKING
chloroform, ether, acetic acid but slightly soluble in
5.1 The material shall be supplied in bulk containers
alcohol andcompletely solubleinalkalis.
of 1000 kg in flexible woven plastic or packages as
3.2 The material shall also comply with the agreed tobetween the purchaser and the supplier.
requirements given in Table 1, when tested in
5.2 Marking
accordance to the methods referred in CO14 of the
Table1. Thepackages shallbemarked withthefollowing:
a) Nameofthematerial,
3.3 Particle Size
b) Indication ofthe source of manufacture,
Notmorethan36percent bymassofthematerial shall c) Netmassofthematerial inthecontainer, and
pass through 56micron IS sieve [seeIS 460 (Part 1)] d) Lotorbatch number.
and not more than 6 percent by mass of the material
5.2.1 BIS Certification Marking
shallberetainedon250micronISSievewhentestedin
accordance tomethod given inAnnex H, Thecontainers may alsobemarked withthe Standard
Mark.

1
.
IS 15030:2001 .—
5.2.1.1 The useof the Standard Mark isgoverned by 6.1 Testsshall beconducted according tothemethod
theprovisions ofBureau ofIndianStandardsAct, 1986 oftestreferred inCOI4of Table 1.
—+J
“..
and the rules and regulations made thereunder. The
6.2 Quality ofReagents
details of conditions under which the licence for the
use of the Standard Mark may be granted to Unlessspecifiedotherwise,purechemicalsanddistilled
manufacturers orproducers maybe obtained from the water(seeIS 1070)shallbeusedintests.
Bureau ofIndian Standards.
NOTE — ‘Pure chemicals’ shall mean chemicals that do
6 TESTMETHODS not contain impurities, which affect the results of analysi.
ANNEX A
[Table 1,S1No. (i)]
DETERMINATION OF MOISTURE CONTENT
A-1 GENERAL A-1.l Takeabout2gofthematerialanddetermine the
moisture content by-KarlFischer method asdescribed
Moisture content is determined by using the Karl inIs 2362
Fischer method.
ANNEX B
[Table 1,S1No. (ii)]
DETERMINATION OF COLOUR — HAZEN
B-1 GENERAL on a water-bath. When the metal has dissolved,
evaporate the solution to dryness. Add 1 ml of
Twomethods, namely,Method AandMethod Bhave
hydrochloric acid and again evaporate to dryness.
beenprescribed. Incaseofdispute, Method Ashallbe
Repeat thisoperation twice.
treated asreferee method.
B-2 METHOD A B-2.3.4 N,N-Ditnethy~ormamide
B-2.1 Outline oftheMethod B-2.4 Preparation of Colour Standard
The co[our of a 5% solution of terephthalic acid in
Dissolve0.50gofthecobah chloride hexahydrate and
.N,N-Dimethylformamide iscom pared withthatofthe wholeofthechloroplatinic acid(seeB-2.3.3) in50ml ,.

colourstandardandexpressedintermsof Hazencolour
ofthehydrochloric acid. Warm,ifnecessary,toobtain

units. TheHazencolour whichisdefinedasthecolour
aclearsolutionandaftercooling, pour intothe500-ml
ofanaqueoussolution,containing 1partpermillionof
one-markgraduatedflask.Dilutewithwatertothemark.
platinum intheformofchloroplatinic acidand2parts
This solution hasacolour of500Hazen colour units.
permillionofcobaltchloride(COCI,.6H,0).
B-2.4.1 Pipette 5mlofthesolution (seeB-2.4) intoa
B-2.2 Apparatus
250-mlone-mark graduated flaskanddilutewithwater
B-2.2.1 Nessler Cylinder — two, 100 ml capacity to the mark. The diluted solution corresponds to a
each(seeIS4161). colourof 10Hazen unitsandshould alwaysbefreshly
B-2.2.2 One Mark Volumetric Flasks — 250 ml and prepared.
500mlcapacities(seeIS915).
B-2.5 Procedure
B-2.2.3 Erlenmeyer Fiask— 250ml.
Weighaccurately 5.0 g of the material into a250-ml
B-2.3 Reagents
Erlenmeyer flask and add 100 * 0.5ml of N,
B-2.3.1 Cobaltous Chloride Hexahydrate — solid. N-Dimethylformamide. Shakethestopperedflaskuntil
all of the sample is dissolved. Transfer the solution
B-2.3.2 Concentrated Hydrochloric Acid —
intoaNesslercylinder andcompare thecolour against
conforming toIS265.
awhite background with thecolour standard taken in
B-2.3.3 Chloroplatinic Acid theotherNesslercylinder. Thematerial shallbetaken
Dissolve 250mgofplatinum insmallquantity ofaqua to have passed the test if the colour of the sample
solution isnotdarker thanthat ofthecolour standard.
regiacontained inaglassorprocelain basisbyheating

2
Is 15030:2001
B-3 METHOD B B-3.4.3 HazenDiscs— 0.70and70-250 Hazenunits.
B-3.1 General B-3.5 Procedure
Themethod isforthedetermination ofthecolour ofa
Measure 75 ml of 2N potassium hydroxide solution
solution of pure terephthalic acid in potassium
into a 100ml beaker. Whh constant stirring carefully
hydroxide.
add 10.0 g of sample. When dissolved fill a 50 ml
Nessletiser cylinder tothemark with thesolution and
B-3.20 utline of the Method
place inthe right hand compartment of the Lovibond
The sample is dissolved in aqueous potassium
Nessleriser cylinder tothe mark with thesoh.ttionand
hydroxide and thecolour of the solution measured in
place inthe right hand compartment of the Lovibond
Hazenunits.
Nessleriser. Fill the second Nessleriser tube to the
B-3.3 Reagents markwith2Npotassium hydroxide solution andplace
inthelefthandcompartment oftheNessleriser. Stand
Potassium hydroxide sohttion — 2Naqueous.
theNessleriser before auniform source of white light
B-3.4 Apparatus andcompare thecolour ofthesample withthecolours
inthestandardHazendisc;rotatethediscuntilacolour
B-3.4.1 Lwibond Nessleriser
match isobtained.
B-3.4.2 Nessleriser Cylinders— onematchedpairof
Report thecolour inHazen units.
50mlcylinders(seeIS4161).
ANNEXc
[Table 1,SINO.(iii)]
DETERMINATION OF ASH
C-1 APPARATUS (see Note 1) by means of a suitable burner. Afger
ignition, placethedishinthemuffte furnace at550 C
C-1.l Muffle Furnace
andremovethesamefromthefurnacewhenallcarbon
C-1.2 Blast Burner isremoved (seeNote2). Placethedishwithashinthe
desiccator for 30 minutes. Take the massof thedish
C-1.3 Platinum Dish — 50 ml.
and its contents. ,.. -
C-1.4 Micro Balance NOTES
1 A minimum of 304)g of sample is to be incinerated.
,.
C-1.5 Crucible Tongs —madeofstainlesssteel 2 Once the sample has been reduced to a carbonaceous
ash,extremecaremustbeexercisedinhandlingthedish. If
withplatinum tips.
the dish is handled in the usual manner with the tongs,

carbonmaybetransferred to the tips of the tongs and may
C-1.6 Glazed Porcelain Plates add carbon to the ash when the dish is removed from the
furnace. In order to prevent this source of serious error,
turn the tongs with tips pointing upward and pick up the
C-2 PROCEDURE
dishbyplacingthearcsof thetongsaroundthe bodyofthe
dish. The dishshould not makecontact with the refractory
Clean theplatinum dish free from grease andsaltsby
lining of the furnace as particles of platinum may be
soaking in hot chromic acid, washing with 1:1 HCi scratched off thus changing its mass.
followedbydistilledwater. Placethedishinthemuffle
C-3 CALCULATION
furnacewiththeOhelpofplatinum tippedcrucibletongs
and heat at500 C for 30 minutes. Remove the dish
fromthefurnaceandplaceitonacleanporcelainplate
which isfreeofdustparticles. Allow thedishtocool
forone minute and transfer ittoadesiccator which is where
placed near the micro balance. Takethe mass of the Ml= massingofempty dish,
emptydishandagainwithsampleofthematerialtothe Mz= massingofempty dish withsample, and
nearest0.1g. Placethedishwithmaterialonatriangle MJ= massingofdish with ash.
supported by a tripod and ignite the sample
IS 15030:2001
,I“
,
ANNEX D ]
[Table 1,S1No. (iv)] -,
DETERMINATION OF ACID VALUE
.,,,,.+,
,,. ,
{.
D-1 GENERAL ofphenolphthaleinindicator. Titratewith0.5Msodium
,,
hydroxide solution to a permanent pink end point.
Thematerialisdissolvedinpyridine,dilutedwithwater {
Carry out a blank determination simultaneously
and titrated with aqueous sodium hydroxide to
excludingthematerial.
phenolphthalein end point.
D4 CALCULATION
D-2 REAGENTS
D-2.1 Pyridine ~1 - V2)xMx56.1
Acidvalue,mgKOH/g =
D-2.2 Phenolphthalein— 1percentsolutioninethanol. w
where
D-2.3 Sodium Hydroxide —0.5Maqueoussolution.
v, = Volumeinmlofsodium hydroxide consumed
D-3 PRmuRE withsample,
V* = Volume inmlofsodiumhydroxide consumed
Weighaccuratelyabout 1gofthematerialintoa100-ml
withblank,
beaker. Add 25 ml of pyridine and stir until all the
M= Molarity ofsodium hydroxide, and
sampleisdissolved. Add25mlofwaterandtwodrops
w= Massof sample taken forthe test.
ANNEX E
[Table 1,SINO.(V)]
DETERMINATION OFIRON, COBALT, MANGANESE ANDCHROMIUM
E-1 PRINCIPLE E3 REAGENTS
Thematerialisashedintwoseparatedishesinpresence E-3.1 Concentrated Hydrochloric Acid—see IS265.
of sulphuric acid. Ash in one dish is dissolved in
E-3.2 Concentrated !3dphuric Acid— seeIS266.
concentrated hydrochloric acid and cobalt and
manganese are determined by atomic absorption E-3.3 Potassium Hydrogen Sulphate —tinepowder.
,.
spectrophotometric method. Ash in the other dish is
E-3.4 Stock Iron Solution — 1000 ppm(rdv).
fused withpotassium hydrogen sulphate, dissolved in

concentrated hydrochloric acidand ironandchromium E-3.5 Stock Cobalt Solution-1 000ppm(WV).
aredeterminedbyatomicabsorptionspectrophotometric
E-3.6 Stock Manganese Solution— 1000ppm(rrdv).
method. Inboth cases air/acetylene flame isused.
E-3.7 Stock Chromium Solution —1000ppm(WV).
E-2 APPARATUS
E-4 PREPARATION OFSTANDARD SOLUTIONS
E-2.1 Atomic Absorption Spectrophotometer
(AAS) — For determination of these elements using E-4.1 Standard Working Solutions
AAS,detailsoftestmethodsasgiveninrelevantIndian
Pipette 10.0mlofeachofthestocksolutions(seeE-3.4
Standard(seeAnnexJ)maybe referred.Typicalworking
toE-3.7) intoa1000-ml flaskandmakeup tothemark
conditions ofAASaregiven below forguidance only:
to given 10 ppm (tiv) standard working solutions.
Iron Cobalt Manganese Chromium Theseshallbeprepared fresheverytime before testing.
a) Wave- 248.3 240.7 279.5 357.9
E-4.LI Standard Iron and Chromium Solutions
length, nm
b) HV 700 620 620 460 Take5,10and20mlofbothstandardworkingsolutions
c) Band pass 0.3 0.3 0.3 0.3
ofiron andchromium of 10ppm (tiv) (seeE-4.1) in
d) Air 16 16 16 16
e) Fuel (acetylene) 6 6 6 6 eachoffour100-mlvolumetricflasks.Add1gofground
f) Burner 8 7 5 8 potassiun hydrogen sulphate and 5 percent
height, mm hydrochloric acidandshake todissolve. Dilute tothe
g) Lamp current, 7 7 3 5
mark with 5 percent HCI to give standard solutions
mA
h) Scale expansion 1 2 1 2 containing 0.5, 1.0,1.5and 2.0ppm (m/v)ofiron and
j) Burner Angle O 0 0 0 chromium.

4
_fJ
-a-A
Is 15030:2001
E-4.1.2 Standard Cobalt and Manganese infollowing ordeq respective standards; samples and
Solutions standards againforcobalt and manganese usinggiven
conditions (seeE-2.1).
Take5, 10,15and20mlofboth standard working
solutions ofcobalt and manganese of 10ppm (W E-5.2 Fusetheresidue fromtheotherdishwith 1.00g
v)(seeE-4.1) ineachoffour100-mlvolumetricflasks. ofground potassium hydrogen sulphate (KHSOd)and
:.,,,..”
Makeuptothemarkwith5percent HC1andshake a few drops of concentrated sulphuric acid over a y
well. Thisgivesstandard solutions containing 0.5, Bunsen burner. Cool, add 5 ml of concentrated
1.0,1.5and2.0ppm(m/v)ofcobaltandmanganese. hydrochloric acid, warm, ifnecessary todissolve and
transferquantitatively toa 100mlvolumetric flaskand
E-5 PROCEDURE
make up to the mark with water. Prepare a blank by
Weigh accurately about 25 g of sample into two taking 1.0g of ground potassium hydrogen sulphate
separatesilicadishes. Wetthoroughly with5mlof KHSOqandafewdropsofconcentrated sulphuricacid.
concentrated sulphuric acid and char completely Runthrough infollowing order; respective standards;
under a vertical heater. Place the dishes in the blank samples and standards again for iron and
entrance of a muffle furnace with the door open, chromium, usingthegiven conditions (seeE-2.1).
andfumeuntilmostofthecarbonhasbeenremoved.
E-5.3 Calculation
Move the dishes further into the muffle furnace,
close thedoor gently andleaveuntil allthecarbon The respective metals
Clxloo
has been removed. Care shall be taken that the
(iron,chromium, cobalt, manganese), ppm= ~
sample does not ignite.
where
E-5.1 Add 5mlofconcentrated hydrochloric acid c, = iron,cobalt,chromium, manganesecontentin
tooneofthedkhes, warm,ifnecessary,todissolve solution derived from sample, ppm and
andtransfer quantitatively toa 100-ml volumetric M= massofthe sample taken fortest, g.
flask. Makeuptothemarkwithwater.Runthrough
..~

5