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TESTING TECHNIQUES II

(Permenance properties:
WA, Chemical resistance, Weathering
properties)
Dr S Soundararajan
PTC

Water absorption
Test specimen 50 x50 mm square

50 mm dia disc

3-3.2 mm thick
Def:
The percentage of water absorbed by a test
specimen at 23 c for 24 hours
Materials like nylons, cellulosics, Absorb more 2-6%
PE, PP, less <0.02%
Polar materials absorb moisture/ water.
Materials containing Oxygen, OH, COOH, NHCO..absorp moisture/ water

Polymers containing halogens CL, F, not absorb water- water


repellent.
Hydrocarbon polymers C & H - PE, PP, - less

Weight before immersion (a)


Weight after immersion (b)
% of water absorption = (b-a)/a * 100

IMMERSION TEMP AND TIME


24 HRS / 23C Average materials
2 HRS / 23C - High Rate of Absorption
Long term / 23c - UNTIL Specmn saturation
( nylons ..90 days)
2 HRS / 100 C - At elevated
temperature
HRS / 100C - For high absorption materials
CYCLIC IMMERSION 23C/100C
Dinnerwares, washing m/c Agitators, Irrigation
valves, sprinklers.

EFFECT OF WA

Loss of ELECTRICAL RESISTANCE


Decrease in MECH STRENGTH IMP
Change in DIMENSION DURING SERVICE
Difficulty in processing, Voids, Foaming
Loss OF CLARITY

WATER SOLUBLE MATTER


Instability OF THE MATERIAL
Increase OF BRITTLENESS
Not Prefered FOR FOOD, MEDICAL &
PHARMACEUTICAL APPLICATIONS

Permanence properties
Chemical Resistance of plastics
Immersion test method ASTMD 543
Specimen size : 50 x 50 mm or

any shape & size


Time of Exposure: 7 days min, s\
standard lab atm or desired Temp
Parameters to study: weight & volume
change
Other observations to be notede:
Loss os Gloss, swelling, Tackiness, crazing
& bubbling

short term tests are useful only for


screening out the unsuitable materials for
applications involving continuous
immersion
Also useful for solvent stress cracking
resistance test i.e under stressed
conditions

Stain resistance
Resistance staining of plastics is determined
Staining agents: coffee, tea, lipstick, nail polish,
shoe polish, bevarages, medicine,
pharmaceuticals, etc
Specimen size : 50 x 50 mm or any shape and
size
Apply the staining agents as thin coating on the
surface on the specimen
Keep in oven at 50 c for 48 hrs
After washing check for residual staining

Sulfide staining resistance


Make H2S solution
Immerse part of the sample in the solution
After the specified time or 30 min
remove the sample and wash it and compare it with
unexposed area of the sample or with controlled sample
one
When one types of PVC are mixed with PVC containig
tin and lead compounds like sulfides, staining may
evident. Also PVC used near by Sulfur based industries
or rubber industries, S fumes may attack PVC and stain.

SSCR Solvent stress cracking resistance


When solvent is exposed to plastics specimen polymer
polymer cohesive bond may be replaced by polymer solvpolymer bond and progressive weaken the polymer
Below a critical limit the polymer will not fail
This critical stress limit is obtained by two methods
1) UTM Tensile test method
apply the solvent on the specimen in the test chamber by a
wig or by spraying for one minute
Stretch the tensile specimen to a known level of stress
And check for cracking
Repeat until failure occurs with fresh specimens
If cracking occurs that is the limit of Stress for which platics
can be useful in that chemical environment.

Elliptical Jig method


In the jig at higher end when a sample in attached , will have
lower stress
At the lower end higher stress because of more bending
moment.
Sp 4/1/0.1 inches rectangular
Immerse in the solvent or chemical
for specified time
Observe the point at which cracking ceases
i.e critical stress limit
stress on the curvatured specimen can be measurable
at any point
Adv : only one test specimen required

ESCR- environmentally stress cracking resistance


Def : surface initiated under poly axial stress of a
rectangular specimen under bent conditions (180 ) in
presence an environment medium without which no
failure occurs even the same conditions are present.
Temp 50 C
Time 48 hrs or F50% or F10%
Envi medium :Igepol Co 630
If 10% fails repeat it with fresh 10 specimens
Notch is made with nicking Jig
STD ; ASTM D 1693 Sample size 38/13/33.2mm

STANDARD TEST METHOD FOR


OUTDOOR WEATHRING OF PLASTICS
ASTM D 1435
SAMPLES ARE OF SUTIABLE SHAPE/
SIZE (TENSILE , IMPACT , DISC )
MOUNTED ON HOLDER ATTACHED TO
RACKS
RACKS ARE POSITIONED 45 ANGLE &
FACING THE EQUATOR

AFTER THE EXPOSURE PERIOD 1-2 YEARS


Appearance, mech & electrical properties to be
determined & compared with control. Control samples
to be covered with black covers.
FACTORS AFFECT
Climate
Time of year seasons / no of years
Industrial atmosphere.
TEST SITES :
Where the product will be used

RESISTANCE TO FUNGI ASTM


G21
Specimens are placed on petri dishes, &
covered with nutrients salt agar, and then
sprayed with fungus spore suspension.
INCUBATOR Temp : 28-30 c

RH : 85%

TIME : 21 DAYS
Effect of physical, optical, electrical
properties were studied.

RESISTANCE TO BACTERIA
ASTM G22
SAMPLES SANDWICTHED WITH SALTS
AGAR.
BACTERIAL CELL SUSPENSION SPRAYED
TESTING AS MENTIONED BELOW
INCUBATOR Temp : 28-30 c

RH : 85%

TIME : 21 DAYS

LIMITATIONS OF ACCELERATED TESTS OF MICROORGANISMS


HIGH LEVEL TOXIC COMPOUNDS MAY OVER-KILL IN
COMMERCIAL APPLICATIONS
EXPOSURE LIMITED TO SMALL NO OF SPECIES OF
DIFFERENT MICRO ORGANISMS
EXPOSURE TIME & CONDITIONS ARE LIMITED
NON-EXPERT MAY MIS INTERPRET DATA
MAY BE DEGRADED BY UV OR WASHED BY
RAIN/OR DEW OR VOLATILIZED BY HOT WEATHER

LIMITATION OF OUT-DOOR TESTS FOR


RESISTANCE OF P.M. TO MICRO
ORGANISMS
Time: 4 weeks
Can be directly exposed to micro
organisms or buried in the soil
Favorable conditions for growth of MO
should be present Temp & Humidity
Observe the effect on specimens

Limitations
Chemical compositions of products
Angle exposure ( 40 C south)
Time of year of exposures, seasons , no of years
Geographic location of exposure
(warm & humid conditions are favourable)
Good water resistance like PE, PP products have
greater resistance to microbial attack unlike ppvc
(no exudation of plasticizer)

Ablation
Decomposition of FRP product when used as
nose cones for rockets and missiles.
Erosion
Destructive effect of water droplets impinging
on articles at high speeds
e.g Air screws of rotating arms, wings in air-craft
Loss of weight & depth of erosion will be
evaluated.

Salt spray resistance


BS 2011-1963
Marine atmosphere may degrade the plastics
Formulations
Nacl
27 parts Distilled water 1 litre
Mgcl2(anh) 6 ,,
Cacl2 ( ,, )
1 part
Kcl ( ,, )
1 part

Irradiation effects
Astm E 1027
Application of plastics in
Nuclear plant- may degrade
During radiation cross-linking
During strerilization e.g. PP syringes
needles, PES medical trays

Accelerated weathering
Weathering properties
The major environmental factors which affect the properties
of plastics
1 Solar Radiation UV, IR, X-rays
2 micro organisms- bacteria, fungii
3 high humidity
4 ozone, oxygen
5 water; vapour, liquid or solid
6 thermal energy
7 Pollution : industrial chemicals

Due to ageing due to above mentioned factors, plastics


may degrade.
Hence become brittle & prop will be lowered. TS, Eb,
FM,IMP st, DST, HDT,VR/SR, Clarity, Gloss, Haze
may varry.
UV radiation
Most destructive of all radiations, Uv energy is strong to
break down main chain c-c bonds
Thermal oxidative degradation results in embrittlement,
discolouration and reduction in physical & electrical
properties

Sources of UV
xenon lamps
Flourescent lighting
Carbon arc lamps

Stabilization : UV absorbers or UV stabilizers


E.g Carbon blackl
Hydroxy benzo phenone, Hydroxy benzo triazole.
Mechanism: converts high energy waves into low energy
waves & emit in a harmless manner.

Micro organisms
polymeric materials are not attacked .
Only additives are susceptible

Plasticizers,
Lubricants,
Stabilizers,
Antioxidants.

| Migrate to surface
| and act as food
|
|

Oxygen : Hydrogen abstraction and


oxidative degradation
Ozone : Peroxide linkage forms , unstable,
degrades, dec Mol. Wt. mostly on
double bonds, like in ABS
Thermal energy : Accelerates oxidative
degradation at elevated
Temps.
Water : all forms : liquid, solid, vapour
a) hydrolysis effect
b) chalking effect
c) Photo chemical effect

Pollutants
H2S, Sulfur, from chemical industries
staining
smog and fog, dirt like
aesthetic quality decreases

Accelerated Weathering
Exposure of plastics test specimens or products cut
pieces in a chamber known
As accelerated weather-o-meter
As per Different STDs
ASTM G 53 Flourescent lamps
ASTM G 154, G155- Xenon lamps
ISO 4892
IS 14889. Flourescent
SAE 1960, 1888
Equipment Suppliers: Atlas Ci 65, Ci 5000, Quv 2000

heraeus alpha ,

Chamber Temp 45 +/-5 C

55+/-5 C

63+/-3 C
Black panel Temp 80 C
RH %- 50 0r 65 in Phase I (only Light)

95%
in phase II ( Raining)

Phsae I 102 min Phase II 18 min


Energy .53 w/m 2
irradiance light source : 5000-8000 watts
Depends upon energy requirements at sample absorption wave
lengths

Exposure Time should match with outdoor energy


accumulated per year
South india :500- 600 KJ/sqm per year

North India : 350-400 Kj/sqm per year


Europe, USA(Florida, california north) , canada : 200-250
Kj/sqm
Africa, Mexico May higher than south india
Depends upon Temp and Humidity
Depends upon location of the country & city at which the
Plastics to be used in the out door

In India H irradiation dose 1248 Kj/sqm


at 0.53 watts/sqm
Every 50 hours in the Accelerated Weatherometer = one month exposure in india in the outdoor
So 600 hrs = 1 year exposure
At regular interval of time say 100, 200, 300,
500, 600hrs, samples to withdrawn and some
properties like Tensile St, Flexural st, Impact st
may determined. Time for 50 % lowering of any
property may be determined.

Very fastly determined in the weathero-meter. 1:10-15 times indoor to out


door ratio depends upon the type of
Plastics materials and exposure
conditions.
The Spectral wave lengths distribution
made similar to outdoor radiation in
the UV& Visible regions (295-380 &
380 -720nm)

IS 14889
For woven sack photo resistance
Time 240 hrs
8 hrs uv /60 deg C Fluores light cycle
4hrs water condensation / 50 C dark

cycle

Photo degradation Studies


time for brittleness of the photo-Degradable films
Time 144 hrs ( approx. 3 months in the out door
for packagings like PE, PP, HIPS, PVC)

PRODUCT TESTINGS
PIPE TESTING
HDPE PIPE TESTING IS 4984

INTERNAL PRESSURE CREEP RUPTURE TEST


L = 10 D =>250 <750 mm
Temp 80 C

Apparatus: Pipe Tester equipment for application of


controlled Internal hydraulic pressure immersed in
thermostatically controlled water bath
Pressure 10-30 Seconds
Test pressure P should be calculated from dimensions
given in tables 3, 4, or 5 (OD & t) and corresponding

Induced stress values given in Table 6


P = 2 S. t /(OD-t)
where
P = test pressure in MPa
OD = outside dia
t = wall thickness
S = design stress , circumferential stress or
induced stress
S= P (OD-t) /2t

Nominal Dia 16 - 1000 mm


Pressure rating
Mpa
0.25, 0.4, 0.6, 1.0, 1.25, 1.6
Kg/sqcm PN 2.5, 4, 6, 10, 12.5, 16

Material PE 63, 80, 100 ( minimum reqd Tensile St

Kg/sqcm)
Designation:

Grade, pressure rating, nominal dia

Visual appearance
-free from groves, clean, smooth internal &
external surfaces & other defects
Wall thickness
Slight shallow longitudinal grooves or
irregularity in the wall thickness
permissible if wall thickness remains
within the permissible limits

Table 3 for grade 63, for each Class of PN & with Dia
nominal dia min &max & the thickness min and max
will be given
Table 4 for grade 80
Table 5 for grade 100 material
Table 6

Type test
80 c/165 hrs
Aceptance Test 80 c/48 hrs

Induced stress MPa


PE63 80
100
3.5
4.6
5.5
3.8
4.9
5.7

DN, dia nominal, mm


16, 20, 25, 32, 40, 50, 63, 75, 90, 110, 140,
160,180, 200, 225, 250, 315, 355, 400, 450,
500, 630, 800, 900,1000
Tolerances 0.3 9.0 mm
Ovality 1.2-35 mm
For each grade, class pressure rating & DN, the
thickness min & max will be given
Ovalty Differcences between Min & max OD in
mm from 300 mm away from cut ends
Coiling 25 X Dia

Class 1
PE 63 2.5
PE80
-PE100 --

2
4
---

3 4
5 6 Kg/sqcm
6 10 12.5 16
6 10 12.5 16
-- 10 12.5 16

Reversion < 3%
200 mm long 100 mm references marks
8 mm t Temp 110 c
oven 1 hr 1min
8-16 mm
110 c
2 hr 2min
Cool it measure the distance between the two
marks
l0-l1/l0 * 100
Overall migration IS 9845 (gen) IS 10146 specfic
38 c /10 days in distilled water < 10 mg/deci lit

Density IS 7328

940.5 kg/m2 946.4 kg/m2

3 Kg/m2

MFI at 190 /5 Kg 0.41 -1.10 gms/10 min


CBC 2.5 0.5 %
CBD satisfactorily
Anti oxidants 0.3% by UV, IR spectra

Pipes and Pipe joints


Burst strength
pipes should not burst/break
No bulging/expanding
no pressure leakage
Pipe Joints

After Joining to m length pipes with solvent cement ,


similar burst st test is done
No leakage of pressure
No breakage of Pipe joints
Dimensions & min max tolerances
Visual appearnce

Containers for water storage

HMHDPE / HDPE /LLDPE IS12701


Dimensions as per standardss Tables & figures
Deformation after filling the tank & PE film covered on the
surface
Change in circumferential dimension
<2% maintained for 3 days >15 c
<3%
,,
,, 7 days > 15 c

Width w.r.to 2L

L w.r.to 2W

For rectangular

tanks & closed with lid

Tensile strength As per IS 8543 P4 Sec 1


IS 13360
> 12N/mm2
Flexural modulus as per IS 13360 P5/S7-95
> 300 N/mm2
Resistance to Impact

Striker Weight 2.5KG


Nose cone Dia 25 mm hemi spherical
Drop height 3 Meters from the bottom surface of inverted tank
No of drops 1 at centre 3 at near by edges or close to corners
No deshaping or punchuring of the tank

Test For TOP Load resistance


Tank Fill 98%
100 kg Load for 4 hrs on the horizontal top
surfaces
Remove the load & allow for another 4 hrs
To recover to normal position
No deformation and cracks should be observed

Overall migration as per 10146


38 C/10 days
10mg/DL
Anti oxidants Thermal stabilizer 0.3%
MFI raw material 0.2 -6 gm/10 min
TOP lid and tank
CBC 2.5 0.5 %
CBD satisfactorily
6mm wire should not pass thro lid and container
gap.

Foams tests

IS 7888 PU foam -flexible foam


Dimension
Density 100 x 100 x 50 mm
M/V * 1000 Kg/m3
Tensile St 10- 20 mm thick 0.7 Kg/m2
Eb % 150 min
Hardness No 380 x380x100 with deflection 25, 40, 50,
65 %
Load quotient > 1.9 min
ratio of hardness number of 65% Def to 25% Def

Tensile strength after heat ageing 70 c/16 hrs - 1


Kg/mm2 ( 70 % of initial Tensile St)
Overall length 152 mm, Ow 38/25mm
t -10-15 mm gauge length 50 mm
Test speed 500mm/min
Ts at break Force/Area
Compression set at 70 C/ 22 hrs
50x50x25
CS 50% h0-h50/h0 x 100
Flammability Flame spread /depth of erosion due
burning

FRP raw materials /products

FRP DMC, SMC


DMC IS 13411 standard
E Glass fibre , 6746
Grades D1, D2,
D3
GP, Mech, Electrical
compression moulding(for raw materials)
J for Inj
J D1 GP by Inj
S- Special purpose for Chemical, thermal, electrical &
Mech

Processability
120- 160 C 3-15 MPa 30-60 Sec/mm t
Thermal Endurance
20000 hrs IS 8504 Part1/2 -1977
Temp/time prop (any) change(50%)
Test specimen-electrical / Water absorption by
inj moulding
Cutting & machining for remaining tests(for
Products)

DMC specifications

D1

Glass content min 15

shrinkage max
Flow mm , min
density gm/cc
WA
%, max
Izod,notch Kj/m2
Flex St
Mpa
Modulus
,,

D2
20

D3 Annex
procedure
20 Type test

0.2 0.2 0.2 Acce test


170 170 170
1.6 2.0 2.0
0.2 0.2 0.2
15 20 18
60 80 70
<- 12000 ->

D1
Surface resist. ohm 1E10
24/water
CTI
600
Arc Resist min s 120
DS at 90 c Kv/mm 8
Dissi factor 1kHz
4 days /80% RH
HDT
C min
125
LOI
% min
23

D2
E11

D3
E12

600 1000
140 180
8
10
0.03 0.01
135 135
25 25

Contin Use
D1
D2
D3
Temp
120
130
130
Post Shrinkage %
<- 0.01 ->
CLTE cm/cm/ c
<- 20E-6 ->

SMC Panels
Class panels
Type A 3 mm thick
B 4 mm
C 5 mm
Side panels
Bottom panels
Half/quarter panels
Drain panels
Manhole panels

PVC pipe testings


IS 4985
Dimensions
Nominal Dia Designation of a size of a pipe conveniently
rounded to approx manufacturing dimension in mm.
Nominal Outside Dia dn

specified OD in mm
Dia at any point OD at any point
Mean OD
Min mean OD minimum value specified for given
nominal size
Max mean OD ,,

Mean ID at mid point of socket length


dimension . Arithmetic Mean of two ID
Ovalty : Difference between max & min OD
Nominal wall thick en
Wall thickness at any point nearest 0.1mm
Min wall thickness &
Max wall thickness nearest to 0.1 mm
Mean wall thickness mean of six measurements

Classification of Pressure
0.25, 0.4, 0.6, 0.8, 1.0, 1.25 MPa
x 10 = Kg/cm2
Tolerances 6 mm or < y = 0.1e +0.2
> 6mm
min tol y = 0.1en +0.2mm
max
y = 0.15 emin
rounded to nearest 0.1 mm
Effective length 4, 5, or 6 meters

Dimensions in table 1 for Plain Pipes


ND, Mean OD min & max, Od at any pt min &
max, Working pressures / 6 class of pipes wall
thick -Avg max, min & max

1.7 1.3 1.7

2.0 1.6 2.0

2.2 1.8 2.2

. . .

Socket ended pipes


elastomer sealing
Solvent cement sealing
Table 3
Nominal size, socket length min & max
Table 2 Plumbing pipes
Dia nominal, Mean OD, OD at any
Point(min & max) wall thick (min & max)

dn

dn
OD at any Pt wall t
min max
min max min max
-------------------------------------------------------20 20 20.3
19.5 20.5 2.8 3.3 mm
25 25 25.3
24.5 25.5 2.9 3.4 mm
32 32 32.3
31.5 32.5 3.4 3.9 mm
40 40 40.3
39.5 40.5 3.6 4.2 mm
50 50 50.3
49.4 50.6 3.7 4.3 mm

Pipe end e, e/3 , 15


Physical & chemical characteristics
Visual check up
Colour-light grey slight variation may be
permitted
Internal & external surfaces smooth, clean &
free from groovings and other defects
Slightl shallow longitudinal grooves or irregulariti
es-if wall t within permissible limits

Opacity-0.2% visible light IS 12235 part 3

Effect on water IS 9845


Lead I extraction 1.0 mg/l or ppm
Lead III ,,
0.05 ,,
Disalkyl III ,,
0.02 ,,
Cd (for all 3 ext)
0.01 ,,
Hg ( ,,
) 0.001 ,,

Reversion 100mm 0f 200 mm pipe 5%


IS 12235 Part5

VSP 80 c IS 6307
Density 1.40- 14.6 gm/cc
Sulfated ash content with sulfuric acid
at 850 c / 30 min- 3 h until constant residue weight from
2-5 gms PVC resin
Colour of residue: white
Hydrostatic pressure test IS 12235 Part 8
Type test
1000hrs / 65C 1.16 PN (MPa)
Acceptance
1
/27C 4.19 PN (MPa)
Test

Similarly socket pipes


dia <90mm acceptance
Type test
dia >90 mm acc test
Type test

Test 27C / 1hr 2.88PN(MPa)


1000hrs / 27C 2.2 PN(MPa)
27C / 1hr 3.6 PN (MPa)
27C / 1000 hrs 2.74PN(MPa)

Plumbing pipes _Designed with higher working pressure


& wall thickness
27 C/ 1hr 3.6 MPa

Resistance toexternal blow test


At 0 C true impact not more than 10 %
Socket end at least 100 mm away from root of
the socket
25 cm OD 0.25 kg 0.5 m
32-68 mm 0.25 ,, 1.0 m
75
mm
,,
,, 2 m
90-110 mm
0.5 kg 2 m
125 & >mm 1.0 kg 2 mm

Colour of the information markings


Reg manufacturers name or trade marks,
OD, class of Pipe, pressure rating
Batch No,or lot No
Word plumbing in the case of plumbing
pipes(on pink colour)
Marked in Ink/paint or hot embossing on
white base intervals of not more than 3 m

Colour for information


Class 1 Red
Class 2 blue
Class 3 green
Class 4 Brown
Class 5 Yellow
Class 6 black

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