IS 13948: Textile auxiliaries - Urea-formaldehyde resin

10 Pages·1994·1.2 MB·English

by  Bureau of Indian Standards

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IS 13948 (1994): Textile auxiliaries - Urea-formaldehyde
resin [TXD 7: Textile Sizing and Finishing Materials]
“!ान $ एक न’ भारत का +नम-ण”
Satyanarayan Gangaram Pitroda
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IS 13948 : 1994

Indian Standard
TEXTILE AUXILIARIES - UREA
FORMALDEHYDERESIN-SPECIFICATION
UDC 677*047 : 678.652 “41” 21

BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MAKG
NEW DELHI 110002
March 1994 ecirP puorG 3
Textile Sizing and Finishing Materials Sectional Committee, TX 07
FOREWORD
This Indian Standard was adopted by the Bureau of Indian Standards, after the draft finalized by the
Textile Sizing and Finishing Materials Sectional Committee had been approved by the Textile Division
Council. .
For guidance oC the users, the various advantages and disadvantages associated with the use of urea-
formaldehyde resin used in textile industry are given in Annex A.
For the purpose of deciding whether a particular requirement of this standard is complied with, the final
value, observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance
with IS :! : 1960 ‘Rules for rounding off numerical values ( revised )‘. The number of significant places
retained in the rounded off value should be the same as that of the specified value in this standard.
IS 13948 : 1994
Indian Standard
TEXTILE AUXILIARIES- UREA
FORMALDEHYDERBSIN-SPECllFICATION
1 SCOPE 4 CREASE RECOVERY ANGLE
1.1 sihT dradnats seificeps eht stnemeriuqer and
The crease recovery angle of bleached, mercerized
methods of test for dimethylol dihydroxy ethylene white cotton poplin conforming to IS 188 : 1980
urea ( DMDHEU ) reactant solution used in
treated with the reactant solution by the method
textile industry. It also specifies details of
prescribed in Annex G shall be 240’ Min when
measurement of crease recovery angle to check tested by the method given in IS 4681 : 1981.
its effectiveness as cross-linking agent.
2 REFERENCES 5 PACKING
2.1 The following Indian Standards are necessary
The material shall be suitably packed in
adjuncts to this standard:
waterproof packages as detailed in the contract or
IS No. Title order.
188 : 1980 nottoC snilpop ( second revision )
6 MARKING
1070 : 1992 retaW rof lareneg yrotarobal esu
( driht noisiver )
6.1 Each package shall be legibly and indelibly
1390 : 1983 sdohteM rof noitanimreted fo /IH marked with the following:
eulav fo suoeuqa stcartxe fo
elitxet slairetam tsriJ( revision ) )a Net mass of the resin solution;
4681 : 1981 dohteM rof noitanimreted fo b) Name of the material namely dimethylol
yrevocer morf gnisaerc fo elitxet dihydroxy ethylene urea;
scirbaf yb gnirusaem eht elgna fo
yrevocer ( jrst revision ) Cl Solid content of the material;
)d
Indication of source of the manufacture;
3 REQUIREMENTS
and
3.1 General Requirements e>
Month and year of manufacture.
The tnatcaer llahs eb raelc tnerapsnart noitulos
eerf morf ytidibrut dna llahs eb fo etihw ot elap
6.2 BIS Certification Marking
yellow colour.
2.3 Specific Requirements hcaE package may also be marked with the
Urea-formaldehyde ( UF ) shall meet the require- Standard Mark.

ments given in Table 1.
6.2.1 The use of the Standard Mark is governed
Table 1 Urea-Formaldehyde - Specific by the provisions of Bureau of Indian Standards
Requirements Act, 1986 and the Rules and Regulations made
( Clause 3.2 ) thereunder. The details of conditions under
which the licence for the use of Standard Mark
Sl Characteristic Requirement Method of may be granted to manufacturers or producers
tseT
NO. may be obtained from the Bureau of Indian
(1) (2) (3) (4) Standards.
i) Total solid content 45 % Annex B
7 SAMPLING
MCI ( m/m )
ii) ,hH of solution 7-8 a tuohtiw nd 4-5 htiw tsylatac SI 1390 : 1983 7.1 Lot
tsylatac
)iii eerF cltyhedlanlrof I’0 % xennA :C The quantity of dimethylol dihydroxy ethylene
,tnetnoc Mm urea solution of one definite composition delivered
Total edyhedlamrof 33’7 f 2 */Q xennA D to a buyer against one despatch note. shall
iv)
tnetnoc constitute ~1l ot.
)v n)cgortiN tnetnoc 15’7 f 2 ‘>; xennA il
)i~, negortiN ot formal- I’rl - I.3 xennA ;I 7.2 Unless otherwise agrred to brtwecn the buyer
edyhed
IllOh and the seller, the .number of packages to be
ratio detceles tiom each lot at random llahs eb sa
1
IS 13948 : 1994
given below: different parts of each container and mix them
Lot Sire Sample Size thoroughly so as to get a composite sample of
desired mass.
up to 15 3
16 to 25 4
8 CRITERIA FOR CONFORMITY
2561 ttoo 15000 7”
8.1 The lot shall be considered conforming to the
101 and above 10
requirements of this standard if the composite
7.3 Draw small quantities of the resin solution by sample meets the various requirements specified
suitable sampling instrument from at least three under 3 and 4.
ANNEX A
( Foreword )
COMMONLY USED RESINS/REACTANTS AND ADVANTAGES AND
DISADVANTAGES OF UREA-FORMALDEHYDE RESIN
A-l A large number of resins/reactants are avail- A-3 The most widely used resins for imparting
able in the market, each one having some advan- wash-and-wear properties to textile fabrics are
tages and disadvantages. In India, these are based on urea-formaldehyde adducts inspite of
mainly based on the following five chemical stiff competition from other resins/reactions. The
types: advantages of urea-formaldehyde adducts are the
low cost and high efficiency. Their main draw-
a) Methyl01 urea, popularly known as urea- backs are the poor stability of the product, poor
formaldehyde resin ( UF );
durability of the finish towards laundering and
b) ( Tri ) Methylol Melamine, popularly susceptibility of the fiuished fabric to rlllorine
known as melamine-formaldehyde resin damage after hypochlo~ ite bleaching. The urea-
formaldehyde resins are, therefore, recommended
( MF );
only for finishing coloured goods which are not
c) ( Di) Methyl01 Ethylene Urea, popularly subjected to hypochlorite bleaching during laun-
known as DMEU resin; dering. Urea-forma!dehyde resins are not suitable
for post-cure ( also called the deferred cure )
d) p( oDpiu la) rlMy ethkynl0o1w n Daihsy dDr Mo xDyH EUEt hylerneesi n; Uarenad, finishing process because the resin cures very
easily and the treated fabric would not remain

e) ( Di ) Methyl01 Ethyl Triazone, popularly in the sensitized or uncured state for a long time.
known as triazonc resin ( DMET ).
A-4 Among the quality control tests of resins, one
A-2 The resins/reactants are mainly used in of the most important is obviously the perfor-
durable press finishing of garments, wash-and- mance test. However, it is rather dilhcult to spell
wear finishing or easy care finishing ot textile out the exact improvement/deterioration of the
fabrics. The treatment with these resins/reactants properties for given level of treatment mainly
improves dry wrinkle-resistance, wet wrinkle- because it clppends upon :: number of variables
resistancr, smooth-drying property, drip-dry which differ from mill to mill ~IKI fi,on-1 time to
property, elasticity, dimensional stability, fastness lime. For example, the nature oi fabric aucl the
of many dycstuf’fs, hand and drape 01 fabrics. pretrea.trnent it has receivctl; quality and quantity
There is a reduction in tensile strength ( rayons of catalyst used in trc‘atmcnt; trthcr XccJIIlpmying
gain ) somewhat in dry strength and substantially ausilial ic.s buch as sof~eu~rs: l/T-To f the ]:a&bath;
in wet strength up to cert:rin level of irPatn~ent., ir:.ati~lg tc~chrliqu~: and condilionz used irlclucling
tear strength, abrasion rcsi:,t::nccb, :tlutsium regain \\<‘i: ,ic Ii up, i!Iy’lI< nllfl l)ac~l;in~!/ ,uring ~~IIl~J~~it-
water imbibition, plasticity, flexibility, extensibility Il:ir, tinlc, pO(:i S.; w:rsli ard tupj.~ill,~ c,llcinirals
and elongation properties. etc.
IS 13948 8 1994
ANNEX B
( Clause 3.2.1 and la& 1 )
METHOD FOR DETERMINATION OF TOTAL SOLID CONTENT
OF THE RESIN SOLUTION
El APPARATUS B-2.2 Decant off the upper layer and add about
50 ml of fresh acetone to the oily residue in the
B-l.1 A centrifuge with centrifuge bottles/tubes
centrifuge at 2 500 rev/min for about 10 minutes.
capable of rotating at 2 500 rev/min.
Repeat the process ( 3 to 5 times ) until the resin,
B-1.2 A Weighing Balance free of water, separates out as solid or sticky
Correct up to 1 mg. mass.
B-Z.3 After removal of acetone, weigh the
B-2 PROCEDURE
centrifuge bottle containing the solid resin.
B-2.1 Weigh about 5 g of resin solution exactly
B-2.4 Calculate the total percent solid content (S)
in a tared centrifuge bottle/tube. Add to it about
of the resin by mass of the resin solution by the
50 ml ( or more depending upon the capacity of
formula:
the centrifuge bottle ) of acetone and centrifuge
at 2 500 rev/min for about 10 minutes when the S , percent = Mass of solid resin -.- x 100
solid matter separates out as a viscous oil. Mass of resin solution taken
ANNEX C
( Clause 3.2.1 and Table 1 ) 1
METHOD FOR DETERMINATION OF FREE FORMALDEHYDE
CONTENT OF THE RESIN SOLUTION
C-l PRINCIPLE a) Sodium Sulphite Sulution -- 1 M prepared by
dissolving 12.6 g of anhydrous sodium
C-l.1 A sample of the resin solution is reacted sulphite m 100 ml of water.
with sodium sulphitc when free formaldehyde
b) Hydrochloric Acid Jbiution - 1 N.
present in the solution forms a formaldehyde
bisulphite adduct and sodium hydroxide is libera- c) Thymolphthalein Indicator Solution - l’rrpared
ted. The mixture is then titrated with standard by dissolving 0. I g indicator in 100 ml 01
hydrochloric acid solution. 80 percent rectified spirit.
C-4 PROCEDURE
H
I C-4.1 Take 20 ml of 1 M sodium sulphite solution
HCHO + Na,S03 f Hz0 = H-C-OH + NaOH
in a conical flask previously placed in an ice bath.
I
s Add to it 3 drops of thymolphthalein indicator.

Formaldehyde adduct of Na$Js. C-4.2 Neutralize the solution obtained in C-4.1
carefully with 1 N hydrochloric acid until the
C-2 APPARATUS colour disappears.
A conical fla3k -~~ 500-ml capacity. C-4.3 \j\‘eigh accurately 10 g of resin solution in
a beaker and dillltc to 100 ml after neutralizing
A wsighing balance - with an accuracy up
with thymolphthalein.
to 1 mg.
C-4.4 Add the solution obtained in C-4.3 to thr
A jipetls - 25-1111 capacity. so!uliorl obtained in C-4.2.
A lrurettc.
C-3 REAGENTS
C-3.1 Quality of Reagents
Unless specified otherwise pure chemicals sltall 1~:
employed in tests and t!isti!lc.d water ( CES SI 1070 : p = :+*003 x .,V >Z, I<’
2991 ) shall be used nhtrc t!le ust’ of water as where
reagerlt is intended. Jv = normality 0 r Ii! drciclJoric acid used l’or
titration; and
ETtONaht od - ton eruP‘ niatnoc slacimehc s,citirllplrri llahs hcihw naem trrffa slacinrPhr eht tset 1. :-- volume in rui of’ I N Irytlrochloric acitl
.u.t1user required tar titration.
3
IS 13948 : 1994
ANNEX II
( Clause 3.2.1 and T&e 1 )
METHOD FOR DETERMINATION OF TOTAL FORMALDEHYDE
CONTENT OF THE RESIN SOLUTION
D-l REAGENTS D-2.2 Add to this solution 20 ml of 2 N sulphuric
acid and titrate with 0~1 N sodium thiosulphate
a) Sodium Hydroxide Solution -- 2 N. solution, with stirring to the colourless end point.
b) Iodine Solution - 0.1 N. NOTE - The addition of small amount of starch
solution makes the end point easier to detect,
c) Starch Solution
D-2.3 Calculate the total formaldehyde content
d) Sulphuric Acid Solution - 2 N. (X) of the resin solution by the formula:
e) Sodium Thiosulphate Solution - 0.1 N. 0.15 x ( V, - Va_2
X=
m
D-2 PROCEDURE where
V, = volume in ml of 0.1 N iodine solution
D-2.1 Weigh about 0.2 g of resin solution into
taken,
a 250-ml Erlenmeyer flask and add to it 10 ml of
v, = volume in ml of 0.1 N sodium
2 N sodium hydroxide solution and 50 ml 01
thiosulphate required, and
0.1 N iodine solution. Let the mixture stand for
1 to lg hours at 20 f 2’C in the closed flask. m= mass of the resin solution taken in g.
ANNEX E
( Clause 3.2.1 and Table 1 )
METHOD FOR DETERMINATION OF NITROGEN CONTENT
E-l APPARATUS E-3 PROCEDURE
a) A Weighing Bottle E-3.1 Weigh accurately about 0.5 g of the sample
b) Kjeldahl Flask - with a loosely fitting pear in a weighing bottle and transfer it to Kjeldahl
shaped hollow glass stopper. flask. Add to it 25 ml of concentrated sulphuric
acid and 0.5 g of sucrose.
c) A Water Bath - capab le of working at a
temperature of 100 f 2 ° C. E-3.2 Kerp the Kjeldahl flask in a boiling water
bath for one hour and then add 0.1 g selenium,
d) A Volumetric Flask -- 100 ml capacity.
18 g potassium sulphate and 0.3 g of copper
e) A Beaker - 250 ml capacity. sulphate. Keep the flask in an inclined position
f ) Distillation Arsembly and close with a loosely fitting pear shaped hollow
glass stopper to prevent loss of sulphuric acid or
E-2 REAGENTS entry of dust. IIeat the mixture gently in a fume
cupboard until the initial frothing has ceased.
4 Concentrated sulphuric acid
Heat the liquid to boiling point and continue
b) Sucrose boiling until the solution becomes clear. Boil the
lC Selenium catal_yst liquid for a further period of’ 2 hours and then
4 Potassium sulphate cool the contents of the flask.
)e Copper sulphate E-3.3 Transfer the contents of K.jeldahl flask to a
100-ml volumetric flask and make the solution
f-1 A few pzeces of pumice stone
up to the mark. Takr 10 ml of this solution in a
d Slilphuric acid solution - 0.05 N. volumetric flask and add to it a few pieces of
)h Mixed Indicator Solution - obtained by pumice stone.
dissolving 0.2 g methyl red and 0.1 g E-3.4 Take 50 ml of sulphuric acid solution
methylene blue in 100 ml of rectified ( 0.05 N ) and 3 drops of mixed indicator
spirit. [ see E-2 (11) ] in a beaker. Set up a distillation
)i. Sodium hydroxide solution - 0*05 N. assembly. Add excess of sodium hydroxide solution
4
IS 13948 : 4991
( 0.05 N ) through the separating funnel and mix 1.4 ( rra - VI ) x 0.05 100
JV = x-
the contents of the flask by mild shaking. Distill m 10
about one-third of the total volume of the solution
in the flask. Wash the dip tube with water, 1w here
collecting the washing in the beaker.
V, = volume in ml of sodium hydroxide
E-3.5 Titrate the excess of sulphuric acid in the solution ( 0.05 N ) used to neutralize
beaker with sodium hydroxide solution ( 0.05 N ). excess of acid in the determination with
he sample,
E-3.6 Carry out a blank titration without the
sample as described from E-3.1 to E-3.4. V, = volume of sodium hydroxide solution
used in blank titration, and
E-3.7 Calculate the nitrogen, percent by mass (%w)
by the following formula: ~1 - mass in g of the sample taken for test.
ANNEX F
( esualC 3.2.1 dna Tuble 1 )
DETERMINATION OF NITROGEN TO FORMALDEHYDE MOLAR RATIO
where
F-l Calculate the nitrogen to formaldehyde molar
ratio ( N : F ) of the resin solution by the follow- JV = percent nitrogen content of the resin
ing formula: solution and 14 represents molecular
weight of nitrogen, and
X = percent total formaldehyde content of
the resin solution and 30 represents
molecular weight of formaldehyde.
ANNEX G
( Clause 4 )
METHOD FOR TREATMENT FOR COTTON FABRIC WITH UREA-FORMALDEHYDE

G-l APPLICATION OF RESIN Catalyst ( Magnesium chloride ) = 15 g/l

G-l.1 The resin is applied by pad-dry-cure Wet pick up = 80 t/0 with 2 dips and 2 nips
method and following recipe is used:
Fabric is then dried at 80-100°C for 5 minutes
100
Resin = g/l and cured at 150°C for 5 minutes.