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7/23/2019 5.c.Raw material testing.ppt
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COMPOUNDING
The mixture of rubber and ingredients used for
manufacture of any rubber product is called compound and
the art of maing such a compound is called compounding!
Ingredients for product manufacture
"! Polymer or rubber
#! Crosslining agents$! %ccelerators for crosslining reaction
&! %ccelerator modifiers '%cti(ator and retarders)
*! %ids to processing
+! ,einforcing fillers '-lac. mineral and organic)
/! %ntidegradants
0! %ids to (olume cost 'inert fillers)
1! Colouring materials
"2! 3pecific additi(es
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Different stages of 4uality control
"! ,a5 material testing
#! In process testing
$! Product testing
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Important polymers
Natural rubber 'N,)
3tyrene butadiene rubbers '3-,) Polyisoprene rubbers 'I,)
Isobutene isoprene '-utyl) rubbers 'II,)
Chloroprene 'Neoprene) rubbers 'C,)
%crylonitrile butadiene 'Nitrile) rubbers 'N-,)
6thylene propylene rubbers '6PM and 6PDM)
Chlorosulphonated polyethylene rubbers 'C3P6)
'7ypalon) 3ilicone rubbers '8)
Polysulphide rubbers 'Thiools)
Polyurethane rubbers
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Polymer 6lements present %ppearance
N, C.7 Translucent. stra5 colour
3-, C.7 Opa4ue. 5hite-, C.7 Translucent
C, C.7.Cl Opa4ue. 5hite
N-, C.7.N Opa4ue. cream colour
II, C.7 Translucent. cream colour
C3M C.7.Cl.3.O Opa4ue. 5hite
T, C.7.3 Opa4ue. cream
8 C.7.3i.O Translucent. soft
6PDM C.7 Translucent
PU C.7.N.O Can be transparent or
5ide range of colour
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Polymer identification
"! -urning test
#! 6lemental analysis$! 3olubility test
&! Colour reactions
*! Instrumental analysis
-urning test
Polymers
Materials burn and continues to
burn on remo(al from the flame
eg! N,. 3-,. I,.-,. etc!
Materials burn but
extinguishes itself on
remo(al from the flame
eg! C,. C3P6
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Polymer 9lame colour Odour
N, and I, :ello5. smoy Pungent
3-, :ello5. (ery smoy 3tyrene
N-, :ello5. smoy 35eet
-, :ello5 5ith blue base.
smoy
35eet
6PDM ; 6PM :ello5 5ith blue base ,esembles burning
candle 5ax
II, :ello5.smoy <ight s5eet
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6lemental analysis '<assaigne=s test)
3odium fusion extract
Nitrogen
Nitrile rubber.
Polyurethane
Chlorine
Neoprene.
7ypalon
3ulphur
Thiool.
7ypalon
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7eat the polymer 5ith con! Nitric acid
Disintegration
N,. I,. 3-,. -,
No disintegration
II,. 8. 6PDM
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>et Tests?
9or 5et test. ra5 rubber is pyrolised and out coming (apour is
tested by solution "!
Preparation of solution "?
"g of p@dimethyl aminobenAaldehyde and 2!2" g of hydro4uinone
are dissol(ed in "22 cc of absolute methanol! To this * cc of 7C<
and "2 cc of ethylene glycol is added!
Procedure?
,ubber is cut into small pieces and is placed in the test tube
containing side arm! The test tube is cored and heated 5ith
micro burner until it is decomposed and (apour appears at themouth of side arm! Bapour is introduced into the test tube
containing solution ". and the change of colour is noted!
Next this solution is transferred into bigger test tube and to it *
cc of methanol is added and heated on 5ater bath! %fter * min!
heating. colour change is noted!
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6xperiment Initial colour Colour after heating5ith methanol Inference
Pyrolised
(apour is
passed
through the
solution
Pale yello5 Pale yello5 -lan
Pale yello5 Pale blue or bluish C,
Pin to red -lue N-,
Pale blue Green 3-,
Pinish (iolet Biolet blue N, or I,
Pale blue Pale blue II,
Pyrolysis Test 5ith solution "
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6xtraction sol(ent for (ulcaniAed ,ubber
6lastomer ,a5 (ulcaniAed
N, %cetone. Methanol.#@propanol 'iso@propyl alcohol)
%cetone. Methanol.M6 'Methyl ethyletone)
-,. 3-,.I, %cetone. #@propanol %cetone. M6
II, %cetone. M6 %cetone. M6
C, <ight petroleum'+2 @ 02C)
#@propanol. Methanol
<ight petroleum'+2 @ 02C).
#@propanol. Methanol
N-, <ight petroleum'+2 @ 02C)
<ight petroleum'+2 @ 02C)
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I, 3pectrum
The absorption peas
Isoprene ,ubber 3-, ,ubber
>a(e number cm@" Intensity >a(e number cm@" Intensity
022 m +11 (s
0$+ (s /*0 s
00* s 121 m
121 s 1+# s
"$/2 s 112 m"+&2 m "&12 M
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I, 3pectrum
The absorption peas
N-, ,ubber C,
>a(e number cm@" Intensity >a(e number cm@" Intensity
121 m 0#2 s
1+# s """2 s
"$22 m "$"* m
###2 (s "++* (s
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I, 3pectrum
The absorption peas
-utyl ,ubber Polybutadiene ,ubber
>a(e number cm@" Intensity >a(e number cm@" Intensity
00* 3 /&" (s
"##2 m 0"$ 5
"#*2 m 121 s
"$/2 s 1+# s
"$12 s 112 m
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6PDM ,ubber ChlorosulphonatedPolyethylene ,ubber
'C3P6)
>a(e number cm@" Intensity >a(e number cm@" Intensity
/"2 m /$2 m
/+2 m 0"$ 5
121 3 121 s
"20$ 3 112 m
""&* m ""*2 s
"$/2 s "#+* m
"$/2 (s
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8uantitati(e analysis
9or N, –
estimate the hydrocarbon content 9or each & isoprene units in the rubber hydrocarbon
$ moles of acetic acid are produced!
9or Neoprene rubber – estimate the chlorine content
Neoprene content E #!&1 x percentage chlorine content
9or Nitrile rubber – estimate the nitrogen content
Nitrile rubber content E $!1 x percentage nitrogen content
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CharacteriAation of carbon blac
Particle siAe - Microscope or electron microscope
3tructure - D-P absorptometer 'dibutyl phthalate
absorptomer)
p7 - p7 meter
D-P absorption No! is the amount of D-P absorbed by
"22 g of blac to attain the specified tor4ue
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Mineral fillers
• Moisture content
• Particle siAe
• 3pecific gra(ity
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Petroleum oils %romatic. Naphthenic . Paraffinic
Paraffinic oils Good colour. good stability. good
sol(ent po5er for saturated
compounds and higher cost
%romatic oils Poor colour. poor stability. good
sol(ent po5er for polar compounds
and lo5er cost
Naphthenic oils 9all in the middle bet5een these t5o
CharacteriAation of oils
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Oil type %sphaltenes.
F max
Polar compounds.
F max
3aturates.
F
%romatic
"2"
"2#
2!/*
2!*2
#*
"#
#2 'max)
#2 $*
Naphthenic
"2$ 2!$ + $* +*
Paraffinic
"2& 2!" " +* 'min)
Classification of Oils '%3TM D###+)
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Oils are checed for
3pecific gra(ity
9lash point
%niline point
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3pecific gra(ity?
>eight of a gi(en (olume of oil to the 5eight of an e4ual
(olume of 5ater
9lash point?Temperature of the oil 5hen a flame 5ill ignite (apours
%niline point?
The temperature at 5hich e4ual portions of an oil and
aniline are miscible
%niline point decreases 5ith increasing aromatic content!<o5 aniline point oils tend to be compatible 5ith most
rubbers
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Oil Type 3pecificgra(ity
9lash point. C %niline pointrange. C
%romatic "!222 ##2 #/ @ *&
Naphthenic 2!1$& #$# ** @ 1#
Paraffinic 2!0/+ $2# 1$ @ "#*
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Polymer Compatible
N, . -, . II, Naphthenic
3-, %romatic
N-, 7ighly polar esters
'DOP . D-P)
6PDM Paraffinic .Naphthenic
C, %romatic
C3M %romatic
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%ccelerators
Name Melting point.
C
3pecific gra(ity
Diphenyl guanidine'DPG)
"&* H # "!"0 H 2!2#
Mercapto benAothiaAole
'M-T)
"/* H # "!&1 H 2!2#
DibenAothiaAyldisulphide 'M-T3)
"+0 H # "!*$ H 2!2#
Tetra ethyl thiuramdisulphide 'T6TD)
/2 'approx!) "!$
inc diethyl dithio@carbamate 'DC)
"/0 'approx!) "!&0 H 2!2"
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%ntioxidants
Name Melting point.C
3pecificgra(ity
Phenyl@-@naphthylamine'P-N)
"2* 'approx) "!#"
Diphenyl@p@ phenylenediammine 'DPPD)
"$# H # "!#& H 2!2#
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Chemical -urning test 3olubility
3ulphur -urns 5ith a blue flame.
pungent smell. lea(esno residue
Completely soluble in
carbon disulphide
inc oxide -ecomes yello5 5hilehot and 5hite 5hile cold
Completely soluble inhydrochloric acid orsulphuric acid 5ithout
gi(ing anyeffer(escence! 3houlddissol(e completely indil! acetic acid!
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Chemical 3odium
carbonate test
3olubility Melting
point3tearic
acid
%dd fe5 crystals
of stearic acid to a
hot saturated
solution of sodium
bicarbonte!
6ffer(escence
around the crystal
indicates stearic
acid!
>arm about " g of
the sample in about
"2 ml of methanolic
potassium
hydroxide! 3tearic
acid should dissol(e
completely
/2
C
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Chemical p7 3olubility
3ilica orsilicate
Neutral 'bet5een +and 0)
3hould not be solublein con! 7Cl of 7#3O&
and should not gi(e
effer(escence
Clay Neutral >ith dil! 7C<. it shouldnot gi(e effer(escence
-arium
sulphate
Neutral >ith dil! 7Cl. it should
not gi(e effer(escence
9illers
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Chemical 3olubility Test for calcium
>hiting
'Calciumcarbonate)
>ith dil! 7Cl. it
should gi(eeffer(escence andshould be completelysoluble!
7Cl soluble part is
treated 5ith ammoniumhydroxide andammonium oxalate!>hite precipitate isformed!
Chemical 3olubility Test for Magnesium
Magnesiumcarbonate
>ith dil! 7Cl. itshould gi(eeffer(escence and
should be completelysoluble!
7Cl soluble part istreated 5ith ammoniumhydroxide and
diammonium hydrogenphosphate! >hiteprecipitate is formed!
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