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South Asian Petrochem Limited

Customer Interaction Program

@
ASPET
Edited by:

Y.Somasundaram, B.E, PGD-PE, PGD-EE, PGD-TQM, PGD-MM

First Edition: 12/03/2005


Second Edition: 20/10/2005
Third Edition: 20/03/2006
Fourth Edition: 20/12/2006
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Preface
The aim of this technical guide is to provide our customers with thorough expertise in PET
processing to Preforms & Bottles. The experience accumulated by various Resin
Manufacturers, Preform Makers, and Bottle Blowers, has been collected and assimilated
into this technical guide.

PET resin to package encounters three unique factors in the polymer industry, the Intrinsic
Viscosity (IV) drop, Residual Acetaldehyde (AA) during Preform making and the Strain
hardening during blowing of preform, these needs to be effectively controlled during the
process to get a perfect package, the guide will throw some light in these topics, to help to
process PET better into a ideal package.

The guide starts with the basics of Polyesters, Zimmers manufacturing technology. The
main focus of this technical guide is to provide the Preform Makers and the Bottle Blowers
adequate technical background for various processes during conversion of PET resin to a
bottle. To enable them take decision, when they encounter processing problems, and
solve it with easy.

The guide also provides tips in design of preforms and bottles in the development of new
preform / bottle designs for new packaging applications.

Hope this will be an informative resource for engineers in the PET industry.

In this fourth edition, we have added Single stage blow molding, based on the interest
from our single stage customers. We thank all our customers, who have provided their
valuable comments for improvement.

We also thank Dr. Sushil K.Verma, Director General, CIPET for his comments for
improvement, accordingly, we are also added a topic on Product testing.

Please let me know your suggestion for improvement for this guide in terms of new topics
to be added, which will help us in bring out our fifth edition more informative.

Fourth Edition
Date: 20/12/2006 Y.Somasundaram
Customer Technical Service
ysomasundaram@aspetindia.com
South Asian Petrochem Limited

Content
1 Polyesters 4

2 Zimmer Technology 5

3 ASPET resin grades 6

4 ASPET 21CF: Energy saving & Easy blow 7

5 ASPET 19C: Low AA applications 10

6 Quality Parameters 12

7 PET Drying 14

8 PET Injection Molding 22

9 Stretch Blow Molding of PET 30

10 Single stage Injection Stretch Blow Molding 37

11 Product testing Preform / Bottle 41

Annexure 1: PET Injection Stretch Blow Molding Thermal history 49

Annexure 2: IV of Preform / Bottle 51

Annexure 3: Definition of Natural Stretch Ratio 53

Annexure 4: PET Injection Molding Screws 54

Annexure 5: PET Preform Design 57

Annexure 6: PET Bottle Design 61

Annexure 7: ASPET 22CJ 62

Annexure 8: Coloring of PET 63

Annexure 9: Trouble shooting in Injection Molding 67

Annexure 10: Trouble shooting in Stretch Blow Molding 71

Annexure 11: Trouble shooting in ISBM 77


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Polyesters have hydrocarbon backbones with ester linkages, hence called polyesters.

The structure above is called poly(ethylene terephthalate), or PET for short, as it contains ethylene groups
and terephthalate groups.

The ester groups in chain are polar, with the carbonyl oxygen atom having a negative charge and the
carbonyl carbon atom having a positive charge. The positive and negative charges of different ester groups
are attracted to each other, allowing nearby chains to align up in crystal form, so they can form strong fibers.
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2. Zimmer technology
Pure Terephthalic acid (PTA) is reacted with ethylene glycol (EG) in the presence of catalyst, to form
ethylene terephthalate, which is polymerized in melt and further in SSP (Solid State Process) to form
Polyethylene terephthalate in form of pellets suitable for bottle grade application.

Paste preparation: PTA is mixed with Ethylene Glycol and catalyst into a paste

Esterification: The paste is fed to esterification reaction system consisting of two-esterification


reactor. Esterification is carried out at atmospheric pressure. Water is the byproduct of the reaction.
The byproduct is rectified and expelled.

Pre-poly-condensation: Esterified product from esterification stage is fed to Pre Poly-condensation


where poly-condensation reaction takes place under vacuum. The pre-poly-condensation takes
place in two reactors.

Final Poly-condensation: Polymer from pre-poly-condensation reactor is fed to the final poly-
condensation reactor where desired viscosity is achieved by temperature and vacuum. Final polymer
is filtered though polymer filters and granulated by cutters.

Solid State Poly-condensation (SSP): The chips produced from melt phase poly-condensation are
amorphous in nature with lower IV. The low IV amorphous chips are converted to bottle grade chips
in solid-state poly-condensation reactor.

In solid-state poly-condensation process, amorphous PET chips are crystallized in Crystallizer 1 and
Crystallizer 2 and then fed to SSP reactor. Desired molecular weight is achieved by temperature and
residence time in a Nitrogen atmosphere. The reaction products and volatile impurities such as
Acetaldehyde are removed by diffusion to gas stream. Chips from reactor out let are cooled and de -
dusted and conveyed to the storage silo for bagging.

2.1: Key Features of ASPET resin:

One largest Poly condensation melt line producing 500 MT/day.


Two SSP reactors working in tandem with Poly condensation line, ensures two product IVs
at same time.

Zimmers low temperature profile and high residence time ensures low residual AA in resin.

Zimmers technology ensures better L color.

Low oligomer & Vinyl ester content ensures, lower AA generation in down stream injection
molding process.
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3. ASPET Resin Grades
3.1: General grades:
Parameter Units ASPET 19C ASPET 20C ASPET 21C
Intrinsic Viscosity .dl/g 0.76 +/- 0.02 0.80 +/- 0.02 0.84 +/- 0.02
Carboxyl end .meq/Kg 30 max 30 max 30 max
group
Acetaldehyde PPM 1 1 1
Crystallinity % 50 50 50
Dust content PPM 100 max 100 max 100 max
Moisture content 2500 max 2500 max 2500 max
PPM
Weight / 100 chips Gms 1.7 1.7 1.7
o
Melting point C 248 +/- 2 248 +/ 2
L Color CIE 90 90 90
.b color CIE -0.5 to 1.2 -0.5 to 1.2 -0.5 to 1.2
Low AA Package General purpose High strength /
Applications pressure applications
Flat / Mineral water Pharmaceutical Carbonated soft drinks
container
Liquor bottles Sparkling water
Wide mouth containers Beer Packaging
APET sheet
Strapping

3.2: Special grades:


Parameter Units ASPET 20 HF ASPET 21CF ASPET 22CJ
Intrinsic .dl/g 0.78 + / - 0.02 0.84 +/- 0.02 0.90 +/- 0.02
Viscosity
Carboxyl end .meq/Kg 30 max 30 max 30 max
group
Acetaldehyde PPM 1 1 1
Crystallinity % 50 50 50
Dust content PPM 100 max 100 max 100 max
Moisture 2500 max 2500 max 2500 max
content PPM
Weight / 100 Gms 1.55 ~ 1.7 1.7 1.7
chips
o
Melting point C 253 ~ 255 248 +/- 2 244 +/- 2
L Color CIE 90 82 90
.b color CIE -0.5 to 1.2 -1.5 to 0.5 -0.5 to 1.2
Hot fill bottles CSD + Power Saving Thick wall containers
Carbonated soft drinks 20 ltr water bottles.
Applications Beer packaging Thick wall cosmetic
bottles.
25% power saving in blow Clear preforms for wall
molder thickness up to 10 mm
Performance Low blowing temperature,
o
Low processing
Highlights less by 8 C temperature.
High co-polymer content,
5.5%
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4. ASPET 21CF
Power Saving & Easy Blow

ASPET 21CF has inbuilt additive, to enhance absorption of Infra red radiation from IR lamps, during the Re-
heat Blow Molding Process. Enhance IR absorption of preform during re-heat provides following advantages;

Lower preform temperature during blowing.


Lower oven temperature & less oven ventilation.
Heating energy saving of 18 ~ 24 % in CSD preforms (High wall thickness).
Heating energy saving of 14 ~ 18 % in water preforms (Low wall thickness).
Increase in machine speed possible to a tune of 3 ~ 5 %.
Better stretching of material around gate, due to better heat absorption, enhancing the stress
cracking resistance.
Wider process window due to uniform heat distribution across the wall thickness of the preform.
Better wall thickness distribution and lower temperature processing, improves the overall strain
hardening of the bottle wall and hence better gas barrier properties.

ASPET 21 CF Performance in Sidel SBO 20


Trial conducted at Partex Beverages, Dhaka
Preform 29.3 gms 500 ml Contoured Rc Cola Bottles Date 17/06/2005
Parameters for
No. comparison Unit ASPET 21C ASPET 21 CF Advantage
1 Oven temperatures % Kw % Kw
Zone 7 % 7.40 3.70 6.70 3.35 9.46
Zone 6 % 28.40 14.20 18.60 9.30 34.51
Zone 5 % 13.20 6.60 13.10 6.55 0.76
Zone 4 % 20.50 10.25 17.70 8.85 13.66
Zone 3 % 51.20 25.60 36.70 18.35 28.32
Zone 2 % 54.00 27.00 40.70 20.35 24.63
Zone 1 % 32.30 19.38 29.50 17.70 8.67
106.73 84.45 20.88
o
2 Oven Temperature C 254 216 38
o
3 Preform Temperature C 94.3 84 10.3
o
4 Delta (Preform Vs Oven) C 159.7 132 27.7
5 Power meter (Total) Amp 311 245 21.22
6 Blowing Rate % 100 100 0
7 Blower Throughput BPH 30682 30682 0

Table 3: Power saving achieved in ASPET 21CF resin in SIDEL SBO20, with 29.3gms preform.
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4.1: ASPET21CF - Injection Molding

Preform processing conditions are very much similar to processing of ASPET 21C. The additive does not
play any role in the injection molding process.

The preforms made with ASPET 21CF are dark in color due to the presence of IR heat absorbing additive.
Normally it is not distinctly visible, when blown into a bottle.

Recipe file Date 17/06/2005


Product 500 ml contour - Rc Cola Place Partex
Preform Partex - ASPET 21C Size 29.3 gms
Box. No. Date 15/06/2005

Oven settings
Penetration Oven % Distribution Oven % overall
Zone 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 Heating
9 0.00
8 0.00
7 80 1 1 1 1 7.40
6 1 1 1 1 60 1 1 1 1 1 1 28.40
5 1 1 35 1 1 1 1 13.20
4 1 1 75 1 1 1 1 1 1 20.50
3 1 1 1 1 1 1 1 1 80 1 1 1 1 1 1 51.20
2 1 1 1 1 1 1 1 1 75 1 1 1 1 1 1 1 1 54.00
1 1 1 1 1 1 1 50 1 1 32.30

o
Preform temperature 94 C Production start up 80 %
o
Oven Temperature 254 C Ventilation 80 %
o
Room Temperature 32 C Correction frequency 50
Relative Humidity 65 % Correction coefficient 0.3

Process Time, in Seconds Angular position, in degrees


Preblow 0.150 Point 0 55.9
Exhaust 0.400 Point 10 67.95
Blowing 0.960 Start of preblow 55.31 -0.5/10
Compensation 1.560 Nozzle down 26
Process 1.630 Nozzle up 293.8
Stretching up 180
Stretching Speed 1.059 m/s

Stretching Pressures
Diameter 14.00 mm Preblow 13 bar
Shoulder diameter 8.00 mm Preblow rate 3 rev
Shoulder height 120.00 mm Blow pressure 39 bar
Gap between rod and mold base 2.50 mm Min Max
Stretching Speed 1.06 m/s Blowing SV control pressure 5.7 6.7 bar

Preform Capacity 500 ml


Material ASPET 21C Type Standard
Resin color Clear Shape Contour - Rc Cola Partex
Type of neck 28PCO VXBO 7126
Weight 29.30 gms
Total length 100.00 mm On mold - Neck & Bases 12 degC
Preform Neck height 21.00 mm On mold - Bodies degC
Exterior diameter 23.00 mm
Neck diameter 25.00 mm Blowing rate 30682 bph

Table 1: SIDEL SBO20 blow molder setting for ASPET 21C, with 29.3gms preforms for
500ml Carbonated Beverages.
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4.2: ASPET 21CF - Blow Molding

The blow parameters need to be retuned to reduce heat input by 14 ~ 24 % depending on the wall thickness
of the preforms. High wall thickness preforms (4 mm), will require switching off of heaters in the first column
of Penetration Zone & last column of Distribution Zone of the oven in Sidel machines, in machines like SIG
all ovens are integrated together, hence switching of heater may be tried in the first column. Subsequently
the heater percentages may be tuned to match the blowing condition of preforms.

Water preforms and other preforms with ~ 3mm wall thickness; the preform blowing conditions may be
achieved by reducing the heater percentages.

Recipe file Date 17/10/2005


Product 500 ml contour Rc Cola Place Partex
Preform Partex - ASPET 21CF Size 29.3gms
Box. No. Date 15/06/2005

Oven settings
Penetration Oven Distribution Oven %
Zone 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 Heating
9
8
7 1 1 1 1 6.70
6 1 1 1 1 1 1 18.60
5 1 1 1 1 13.10
4 1 1 1 1 1 1 17.70
3 1 1 1 1 1 1 1 1 1 1 36.70
2 1 1 1 1 1 1 1 1 1 1 1 1 40.70
1 1 1 1 1 1 1 1 1 29.50

Oven Temperature 216 oC Production start up 95 %


Preform temperature 84 oC Ventilation 70 %

Process Time, in Seconds Angular position, in degrees


Preblow 0.150 Point 0 55.9
Exhaust 0.400 Point 10 67.95
Blowing 0.960 Start of preblow 55.31 -0.2/10
Compensation 1.560 Nozzle down 26
Process 1.630 Nozzle up 293.8
Stretching up 180
Stretching Speed 1.059 m/s

Stretching Pressures
Diameter 14.00 mm Preblow 13 bar
Shoulder diameter 8.00 mm Preblow rate 3 rev
Shoulder height 120.00 mm Blow pressure 39 bar
Gap - rod and mold base 2.50 mm Min Max
Stretching Speed 1.06 m/s Blowing SV control pressure 5.7 6.7 bar

Preform Capacity 500 ml


Material ASPET 21CF Type Standard
Resin color Grey Shape Contour - Rc Cola Partex
Type of neck 28PCO VXBO 7126
Weight 29.30 gms
Total length 100.00 mm On mold - Neck & Bases 12 degC
Preform Neck height 21.00 mm On mold - Bodies degC
Exterior diameter 23.00 mm
Neck diameter 25.00 mm Blowing rate 30682 bph
Preform age 48.00 hrs

Table 2 SIDEL SBO20 blow molder setting for ASPET 21CF with 29.3gms preforms for
500ml Carbonated Beverages.
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5. ASPET 19C
Low AA in Preform / Bottle
Acetaldehyde commonly known as AA, is present in all citric juices, and is not harmful to humans for
consumption. AA normally gives off taste and flavor to flat water.

AA (Acetaldehyde) is generated during the melt polymerization and most AA generated during the melt
phase is driven out during the SSP (Solid State Polymerization) process and the net resultant AA in PET
chips of water grade resin is less than 0.60 PPM.

Major portion of AA in preform / bottle is generated during the melt processing of SSP chips in extruder to
make preforms. Since, the functional end groups in PET are highly sensitive to temperature. The high
temperature and shear in screw / barrel, breaks Hydroxyl groups to vinyl ester groups. The reaction is as
below.

R-CO-O-CH2-CH2-OH R-CO-O-CH=CH2 + H2O

The new vinyl ester groups, further degrades to produce AA (Acetaldehyde) in the preforms.

H2O+ R0-CO-O-CH=CH2 AA + R0-COOH

The AA thus generated remains in the preform / bottle wall, after the processing is completed. This residual
AA in the container, migrate slowly into the content of the container, when the temperature is above the
boiling point.

The AA in the bottle is reduced in long-term storage, by migration to air. But, there will hardly any change in
AA during the Stretch Blow Molding of Preform to Bottle.
o
The boiling point of AA at normal pressure is 21 C.

5.1: ASPET 19C High Lights

Manufactured in latest Zimmer Technology with low temperature profile ensures low vinyl
ester & oligomer content.
Low residual AA in pellets around 0.6PPM.
Low temperature processing due to higher copolymer content, so low AA generation, easy
blow-ability.
Low AA generation in molding due to low vinyl ester content.
Low fines content.
Low catalyst
Low Global Migration.
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5.2: Tips for low AA in Preform / Bottle:

Reduce the barrel set temperature.

Optimum temperature of processing of PET changes from machine to machine. Suggestion will be to
reduce the temperature, without the haziness or un-melt. While lowering temperature, if you
encounter actual temperature overshooting, more than set temperature, generation of higher shear
heat is indicated, which can induce higher AA generation. Hence lowering can be discontinued.

o
Try inverse barrel temperature profile. .i.e., Feed zone temperature 5 ~ 10 C, higher than metering
zone temperature.
Reduce melt pressure during plasticization (backpressure).

The lowering of backpressure will reduce the shear, but caution should be exercised that bubbles are
not formed in preform. The optimum melt pressure will be 50 ~ 150 bar for low AA processing,
though it may vary from machine to machine.

Reduce the screw speed.

Lower screw speed will reduce the shear and thus reduce the AA generation. Avoid too low speed
leading to increase in cycle time.

Screw idle time should be less than 2 sec, if higher, reduce screw speed to match.
Inject the melt at slower rate. This will help to reduce the shear heating. Ideal injection rate for water
preforms are < 10 g / sec.
Minimum cushion for extruder and shooting pot is 5 mm.
Reduce the manifold and NT temperatures of hot runner to minimum.

The above are some of the tips for reducing the AA, a combination of the same will help to have the AA
under stipulated norms of 4 PPM for water preforms / bottles.

Drying has considerable impact on AA generation. Higher moisture content will lead to hydrolytic
degradation. Hence moisture content to be maintained less than 40 PPM, for lower AA preforms.
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6. Quality Parameters
The vital parameters deciding the quality of PET resin are Intrinsic Viscosity, Brightness (L) and Yellowness
(b) and Residual Acetaldehyde content.

6.1: Intrinsic Viscosity (IV):

Intrinsic Viscosity (IV) is an indirect measure of polymer molecular weight. This characteristic helps
customer to choose the right resin for right application. Resin with higher I.V crystallizes slowly, and has
higher melt viscosity. The preforms from high I.V resin are stiffer and require higher force to stretch blow.
The containers from higher IV resins have better mechanical strength and barrier properties. The properties
are reverse with low IV resin.

IV of PET is determined by solution viscosity techniques, where, a very dilute solution of polymer is passed
through glass capillary viscometer, and time required for specific volume of solution and solvent is measured.
Intrinsic viscosity of resin is computed using formula.

Following are the computation procedure for Intrinsic Viscosity.

Relative viscosity (RV) = Flow Time of Solution / Flow Time of Solvent

Specific Viscosity ( Sp) = RV 1

Reduced Viscosity ( Red )= Sp / c

Intrinsic Viscosity (IV) = Red at Zero Concentration

The intrinsic viscosity value is very specific to a solvent and set of condition, because, interaction of PET with
different solvent is different; there are various solvents and conditions used in the PET industry.

ASPET method

Equipment: Ubbelohde Viscometer


Solvent: Phenol + 1-2 Dichlorobenzene (60 : 40 w/w)
Temperature: 25C

6.2: Color (L, a, b):

L, a, b are the three-dimensional characteristic for appearance of an object, light source. L defines the
lightness, a & b defines the chromaticity.

L denotes - Black to White: 0, for Black, and 100 denotes white.


a denotes - Red to Green: +ve value indicates Red & -ve value indicates Green.
b denotes - Yellow to Blue: +ve value indicates Yellow & -ve value indicates Blue.

The color values are measured using colorimetric spectrophotometer, which measures the wavelength
distribution of reflected or transmitted light by the sample.

Overall appearance of Resin, Preforms & Bottles is based on the various combinations of the above said
color components. These values will vary from technology to technology and recipe to recipe.
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ASPET measures sample in powder form. Measuring color values of resin in ground form helps to get the
true picture of color values for the core polymer / Pellet.

6.3: Acetaldehyde (AA) Content:

Acetaldehyde (CH3CHO) is a colorless liquid below room temperature with a boiling Point of 21C.

In melt phase poly-condensation, AA is produced as by-product and gets entrapped. The concentration is
reduced drastically by diffusion at elevated temperature in SSP.

ASPET method

Gas Chromotograph: Cryogenically ground resin.


Capillary: Carbowax 30 M
Incubation Temperature & Time: 150 oC & 30 minutes

ASPET resin has residual Acetaldehyde around 0.60 PPM, ensured by Zimmers process.

6.4: Typical Value for PET

Bulk Density(kg/m3) 817(poured)


881(Vibrated)
Pellet Shape / Size Cubical(2.8mmX1.8mmX2.7 mm)
o
Melt Density at 285 C(g/cm3) 1.2 g/cc
Density (Amorphous) 1.33 g/cc
Density (SSP chips) 1.38 g/cc
Heat of Fusion 58 J/g
Thermal conductivity Melt 0.213 W/m.K
Thermal conductivity SSP chips 0.242 W/m K

Specific Heat of PET

2.20
Specific heat, J/g.K

2.00
1.80
1.60
1.40
1.20
1.00
0 50 100 150 200 250 280
J/g.K 1.13 1.26 1.51 1.70 1.88 1.99 2.05
Temperature, C
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7. Drying of PET
PET is very hygroscopic. PET granules can absorb as much as 3000ppm of moisture, under humid
conditions. Moisture adversely affects the I.V, during plasticization of polymer, due to hydrolytic degradation
of the molecular chain, with lower resultant IV of end product. Typically, the preform should have an I.V. of
approximately 0.69 dl/g or greater to prevent problems such as haze, thinning bottle sidewalls, or brittleness.
It is always better to have lowest possible IV drop, to have the full benefit of the resin paid for.

The critical factors, which play a vital role in drying of PET, are

Dew Point of Drying Air


Pellet Dwell Time
Airflow Rate
Inlet Air Temperature.

7.1: Dew point of hot air

Most advance de-humidifying dryers have the dew point meter, to measure dew point of hot air at hopper
inlet. A hand held dew point meter can be also used for dew point measurement. Engineers who are
conversant with the age-old practice of measurement of dew point with dry ice can do the same with the help
o
of thermometer and dry ice in a glass tube & stirrer. The recommended dew point for hot air is 40 C, and in
o
no condition the dew point should drop below 20 C, for effective drying and good product quality.

Following experimental graph gives the IV of the preform produced with various dew point values, from a
base resin IV of 0.74 dl/g, with a moisture content of 1500ppm.

These curves indicate that having a low dew point is important, but it is not as critical as it was once thought.
If the air temperature with flow rate, and pellet dwell time are optimum, a reasonably low I.V drop can be
obtained. Even so, the dew point should always be kept as low as possible, preferably 40C or lower.
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7.2: Pellet residence time in hopper

The pellet dwell time in the hopper can be calculated with the hopper full capacity, and resin consumption of
the injection molder.

3 3
Hopper full capacity (Kg) = Hopper full volume (M ) X 850 (Kg / M )

3,
Where, 850 Kg / M is the bulk density of the PET chips.

Hopper full capacity (Kg)


i.e. Pellet dwell time, hrs = --------------------------------------------
Consumption of Molder (Kg/hr)

This give the actual pellet dwell time in the hopper, but the effective dwell time for the calculation of drying
should be arrived at by reducing the time required for increasing the pellet temperature to the drying
temperature. This for practical purpose is approximated to hr.

Thus the effective pellet residence time in the hopper

7.3: Airflow rate

The amount of air required to dry pellets to less than 40 ppm of moisture content by weight, depends of
following factors,

o
Dew Point of hot air. C
Pellet Dwell Time, hrs.
o
Inlet Air Temperature, C
Moisture content of pellets. % wt.
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Devices such as the Pitot tube, anemometer can be used to estimate air velocity and thus airflow rate. But,
since the dryer hose has very short straight portions and bends, these tools may not be much suitable, due
to turbulence in the airflow.

The standard recommended air flow rate for drying is 0.062 cMm /Kg / hr (.ie. 0.062 Cubic meter of air per
minute for every Kg / hr of PET dryer output)

The other method for the estimation of the airflow rate in dryer, conventionally used by the processor is
estimation of the return air temperature of hopper. This has been effectively proved working. The following
graph provides effective tool for the estimation of airflow rate in a dryer.
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7.3.1: Procedure of airflow rate calculation:

Note: The dryer should have processed at least its full capacity for recording parameters for this calculation.
(.i.e. approx. 8 ~ 10 hrs from the start of the dryer, depends on the temperature used)

Steps for the calculation

1. Calculate the pellet residence time in the dryer.


2. Measure the actual air inlet temperature of the dryer.
3. Measure the air exit temperature at the exit hose of the dryer hopper. When fresh pellets are
dumped into the dryer, the return air temperature will typically drop 1525C. The
temperature will start to recover and peak will be reached at the just before the next dumping of
pellets. The peak temperature must be used in estimating airflow rate.

7.3.2: Deducing the airflow rate from the experimental curves

Once the pellet dwell time and the return and inlet air temperatures have been determined, the appropriate
graph for a given pellet dwell time is selected. The point at which the inlet and return air temperatures
intersect will indicate the approximate airflow rate. For example, assume the following values have been
determined:

Pellet dwell time = 4h


Dryer inlet air temperature = 155C
Dryer return air temperature = 95C

By referring to Figure A-1, it is seen that the point the temperature values intersect will indicate an airflow
rate of approximately 0.037cmm/kg/h. In such a case, an investigation should be conducted to determine
why the airflow rate is so low. Potential causes include:

Air filters needs cleaning.


Perforated screen in the bottom of the dryer needs cleaning.
Dryer blower is undersized for the PET throughput rate.
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7.4: Effect of Moisture in Pellet

The air flow rate change with the dwell time because the drier has constant flow rate of air and with increase
in resin throughput the specific air volume for Kg of resin processed / hour decreases and vice versa.

The second experimental graph has the entry moisture level of pellets increased from 0.15% wt to 0.35 % wt.
Higher moisture of chips has resulted in the narrowing of optimum processing region, and the dryer process
window gets reduced, and it requires close control for effective drying of pellets and thus the final preform IV.
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7.5: Effect of increase air flow rate in dryer process window

From the experimental graphs, we could infer following facts for effective drying.
Dew point of less than -20 C (-40 C recommended)
Optimum drying temperature is range bound for a particular drying time. Higher temperature always
does not ensure lower IV drop, though it may ensure better drying (.i.e. lower moisture content).
In a similar way residence time of pellets in the hopper at a particular temperature is range bound
beyond which the product IV will once again drop due to thermal degradation of pellets.

In case of increased moisture in the pellets, the dryer process window gets reduced. A considerable
improvement in the dryer process window can be effected by increasing specific airflow rate to the dryer
hopper. The following experimental graph provides the significance of increased airflow rate.

Considering all conditions, let us assume a process engineer encounters a wet bag, where the moisture
content may be as high as 1.0 % due to external moisture on the pellets, then how does he effectively
process the material. The best possible procedure for the lowest possible IV drop in product may be as
follows.

Opt for a mold with minimum throughput, so that the residence time can be kept more for the dryer. It
also does another added benefit, which is very crucial, the specific airflow for dryer throughput,
increases, as the blower capacity is constant.
In case the dryer residence time shots beyond 11 hours reduce the hopper fill height to control the
residence time to 10 ~ 11 hrs.
Select a dryer inlet air temperature of 130 C, and maintain the pellets hopper inlet temperature of not
less than 125 C.
Under these conditions, always maintain the lowest possible screw speed, as the resin has to pick
up additional 30 C from the extruder feed zone, as compared to normal optimum temperature of 150
~ 165 C at the feed throat of extruder. A lower speed will help to reduce resultant shear with lower
temperature of resin at hopper throat.
Under these conditions, ensure that the specific air flow rate in the hopper is about twice that of
normal (0.10cmm/kg/hr. min)
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Thus, a product with minimum IV drop could be achieved (0.03 ~ 0.04 dl/g). Which otherwise could have
been in the order of 0.10 dl/g, due to the combined effect of hydrolytic degradation at the hopper at high
temperature, residence time & moisture. Also, degradation during melting due to very high end groups, in the
dried resin initiating further chain breaking at extruder.

7.6: Dryer selection & design

Following are the key aspects to be considered during selection of a dryer.

The dryer must be a regenerative desiccant type capable of maintaining a dew point of 40C.
The hopper height to diameter (h/d) ratio is of utmost importance. As the h/d ratio increases, drying
becomes more uniform because the pellets start to approach "plug flow," meaning all pellets
experience about the same dwell time. The opposite is true of short hoppers with large diameters
where "channeling" will occur and proper drying is practically impossible. This is because pellets
near the hopper wall will have a very short dwell time. The h/d ratio should be at least 2:1, and
preferably 3:1.
The optimum dwell time for drying PET pellets is approximately 8.5 hours. With this dwell time,
relatively low process air temperatures should ensure proper drying. The lower temperature
translates into a very large savings in electrical energy. Therefore, in addition to providing more
effective drying, a dryer capable of an 8.5 hour dwell time should reduce the drying cost.
A good hopper dryer should have facility to control the level of the pellets in hopper, this will help us
in reducing the hopper capacity, when the throughput is very low. This can help to avoid over drying
and subsequent degradation in the dryer.
In cases, where a hopper of 8.5 hour dwell time is impractical because of space limitations, it is
strongly suggested that the dryer provide at least 6 hours dwell time. If this is also not
accommodated in the shop floor two small hoppers connected in series should be ideal choice, one
on the floor and one on the molding machine.
It is also important that the hopper be well insulated and the dryer blower large enough to provide at
least 0.062 cmm of air per kg for maximum intended processing capacity of the injection molder
(pellets processed per hour).
Having a built-in dew point alarm is also a desirable feature.

7.7: Dryer Maintenance

After selecting a good dryer, it is very important to maintain well, so as to achieve best performance.
Following checklist is suggested to observe optimum performance;

1) Air filters - Check daily. Fines or other contaminants will clog the filters and thus reduce the airflow. A
flow rate of at least 0.062 cmm of air per kg of pellets being processed per hour is essential.

2) Dew point - Check daily. Air having a low dew point (40C) is needed, so that the air can absorb the
moisture from the pellets. A high dew point is usually caused by

a) Air leak, in the dryer circuit.

b) Poor regeneration of the desiccant, or a bad desiccant. If the desiccant is believed to be bad, the
dryer manufacturer can provide assistance in testing it. Most manufacturers suggest changing the
desiccant every year or two.

3) Heaters - Check weekly. This includes process air heaters and desiccant regeneration heaters. Consult
your dryer manual for the proper regeneration temperature. Normally, it should be around 220C.

4) Hoses and connections - Check weekly. Air leaks can increase dew point and reduce airflow through the
dryer.
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8. PET Injection Molding
Injection molding is a process, where the polymer is melted under heat and shear to make a homogeneous
viscous fluid, which is injected under pressure into the mold, with the shape of the product and where it is
cooled to the final product shape and dimension.

A basic injection-molding machine has following parts,

Hopper: Where the plastic pellets are held ready for processing. In PET a de-humidified dryer hopper
replaces it, where the material is dried to moisture level of less than 40 PPM, to make it suitable for injection
molding.

Barrel: The barrel is a hollow tube, which houses the screw. Screw does the function of pumping and
plasticification of pellets into a homogeneous melt. The barrel is surrounded by heaters, which supply around
33 % of the heat required for plasticization of the polymer.

The barrel heater does the critical function of softening the pellets during start up, to enable the screw to start
rotation at a lesser torque, without any damage. The heater also maintains the surface melt temperature and
prevents from sticking to barrel.

Nozzle: The nozzle forms the front end of injection barrel, it injects hot melt into the cavity, either directly
through a sprue, or a Hot runner manifold as in case of a multi cavity mold.

Nozzle normally houses the Shut-Off valve, which closes the extruder during the plasticizing process and
avoids drooling of melt through the nozzle. Shut-off valve is present in all PET injection molders, as PET melt
has low viscosity, which causes it to drool during refilling.
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8.1: Injection Molding Preforms

The quality of the preform determines the quality of the final product the bottle. Thus the quality of the
preform is very significant stage in the making of the final bottle.

Following are the critical factors, which have effect on Final product (Preform):

1. Injection molding machine and equipments.


2. Resin characteristics, IV
3. Critical processing parameters;
a. Drying temperature & Time
b. Use of regrind
c. Process temperatures
d. Process Pressures
e. Process durations & Cycle time.

Injection molding equipment can be categorized as follows, based on the function.

1. Dryer
2. Plasticization & Injection system
3. Mold
4. Clamping unit
5. Preform Handling
6. De-humidifier
7. Chiller

8.1.1: Dryer:

The function of the dryer is to dry the material to less than 40 PPM of moisture, so that the material does not
undergo hydrolytic degradation / deterioration in properties. (Drying is discussed in Drying of PET)

8.1.2: Plasticization & Injection system:

The plasticization & Injection system may be same in case of normal machine, where extruder also functions
as injector for the melt into the mold cavity. There are machines having independent shooting pot to inject
the material into the mod cavity, where the extruder function is to only plasticize and supply the melt into the
shooting pot.

Some systems have packing ram in tandem with extruder, which takes over during hold phase, so extruder
can start plasticizing melt during hold phase and thus saves cycle time.

Extruder should have variable backpressure for optimum melt plasticization, depending on the IV and
product requirement. Backpressure should not be excess to cause shear degradation of melt or too low to
allow passage of air / bubbles into plasticized melt.

8.1.3: Hot runner:

The hot runner forms most vital part of the mold. Hot runner conveys the plasticized melt from the barrel to
cavities; this should be done with utmost care to avoid any melt separation, which can result in poor clarity,
degradation & separation of colors. To ensure the same, following aspects needs to be considered during
design and manufacturing;

1. Melt should not encounter sudden sharp corners.


2. Melt velocity should be constant from the moment it enters the sprue to the time it enters the cavity.
o
3. Melt temperature should not drop or increase more than 5 C, of melt temperature at metering Zone.
Any major change will lead to separation of melt layers, color, black specks and splay defects.
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8.1.4: Mold:

The essential feature of good mold is the polish and the air venting. Air venting in particular is very critical, as
melt enters the cavity at 10 ~ 12 g / sec, and the entrapped air has to be exhausted at the same speed, or
else, the leading edge of the polymer melt can burn due to high temperature & pressure and cause burn
marks. Typically a white mark found in the thread area of preform.

Inadequate, air venting can also considerably increase the injection pressure, and may also result in flash at
the neck ring opening due to use of high pressure used for packing the cavity.

8.1.5: Preform Handling:

Advance systems have robots for collecting the preforms from the core pins and dumping on the conveyor.
Most of these have cooling provision for preforms in the robot arms, so that the cooling time can be reduced
in the mold, this saving the cycle time.

When such cooling robots are available the preforms are ejected at surface temperature just below the Tg of
o o
PET, i.e. 78 C (the inner core may be of much higher temperature). Further cooling to < 45 C for packing
is done in the Robot cooling.

8.1.6: De-humidifier:
o
To maintain air around the mold at less than 8 C dew point.

Key requirements / Advantages:


1. Avoids dew formation & moisture ring defect at low chilled water temperature.
o
2. Lower cycle time possible due to cooling of mold with low temperature water 8 C.
3. Lower crystallinity of preforms & better blowing.
o o
The de-humidifier supplies air with dew point from 2 C to 2 C. This air forms an envelope around the
mold and prevents formation of dews on the cold mold surface.

8.1.7: Chiller:

To supply cold water for the mold and robot handling system for quenching the melt to preforms.
o
Operating temperature range 6 ~ 10 C.
8.2: Resin Characteristics

The key parameter, which affects the process and the product, is the IV (Intrinsic Viscosity) of the polymer.
Generally all bottle grade resins are made with IV ranging from 0.72 dl/g to 0.84 dl/g. An increasing IV has
following effects on the process ability of the PET.

1. Higher processing temperature.


2. Higher back pressure required to break the crystals.
3. Higher injection pressure to inject the melt into the mold.
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As IV shifts lower following are the effects on the bottle.

1. Lower IV resin or higher IV drop in processing will yield hazy preform. While increasing temperature
will usually reduce or eliminate the problem, it is not a suggested as this will further reduce the IV of
the preform. Lower preform IV will result in narrow blow molding process window. Such preforms
eventually yield defective bottles.
a. Uneven wall thickness distribution.
b. Thick shoulder and base, with thin sidewall thickness.
c. Brittleness in shoulder and gate area.
d. Bottles failing in drop test.
2. Lower burst strength of the bottle.
3. Inconsistent blowing, need to frequently change the blowing parameters.

Preform IV less than 0.68 dl/g is difficult to blow consistently.

Resin IV less than 0.70 dl/g, is difficult to process, in normal injection molding.

8.3: Use of Regrind:

Though use of hot runner molds in PET has greatly reduced the generation of regrind material, from
runners and sprue. There is need to consume small quantity of regrind generated from start up and
testing.

Critical aspects of using regrind.

1. The maximum allowed regrind is 10 %. Any higher dosage can reduce the mean IV of the mix
due to lower IV of the regrind. The mean IV should always be maintained above 0.76 dl/g.
2. Essential to maintain constant mixing ratio for uniform blow molding performance, as variation in
IV due to variation in level of regrind will affects the consistency of preform blowing.
3. Proper feeding screw should be used in the hopper for uniform feeding, incase of using bottle
flakes as these flakes tends to separate. Any separation of flakes in dryer or feed hopper will
result in inconsistent preforms.
4. The effect of IV drop in the molding system (Dryer + Molder) also plays a critical role in the
processing of regrind. If the system has very low IV drop, then higher dosage of regrind can be
safely done. In no case the IV of the preforms should be allowed to drop less than 0.68 dl /g.
5. Some studies suggest that the use of 2 ~ 3 % regrind can reduce the AA level in preforms. But
higher regrind dosage has always resulted in higher AA in preforms due to the higher AA content
in the regrind and also the higher end groups.
6. As regrind do not have smooth corner, they tend to generate more fines while transportation to
hopper and in the hopper. Thus process air filters need to be cleaned frequently. May be even
once a shift.
7. Precautions to be taken, while using regrind in following aspects.
a. Cleanliness of regrind.
b. Moisture content of the regrind. Flakes can have higher moisture content and thus a
cause for hydrolytic degradation during processing. Monsoon and high humid
environments needs special care to avoid haziness and low IV preforms.
c. The bottle and preform regrinds needs to be thoroughly sieved before loading into
hopper dryer, as higher fines content can
i. Choke the drier filters.
ii. Dust marks in the preforms, as fines are difficult to melt under normal
processing conditions.

Thus, use of regrind even though financially rewarding, can open up a big box of rejection, if not handled with
care.
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8.4: Injection Molding machine Cycle time Break up

Mold open Ejection


Mold Closing

Clamping Side

Cooling Injection side

Screw Idle time


Plasticization

Injection
Hold

Cycle time Break up for Direct Screw Injection Machine

8.4.1: Term Definitions:

Dry Cycle time: The dry cycle time basically comprises of mold closing, clamping, unclamping, opening of
mold and ejection stroke. Normally they are from fraction of second in advanced machines to 2 seconds in
slow systems.

Mold closing: The moving platen moves forward and closes with the fixed platen; on completion of closing
the clamping tonnage is applied.

Mold Opening: The clamping tonnage on the mold is released and the moving platen moves backward
separating the two halves of the mold so that the product can be ejected.

Ejection: During the process the components formed during the molding process is ejected from the core
side. Basically the components stick to the core side as the product shrinks on cooling. The product may be
ejected down or can be collected by a robot.

Plasticization: Plasticization is the process of melting the polymer and mixing the same into a homogeneous
melt.

Injection Phase: During this phase the hot plasticized melt is injected into the mold, at high pressure, for
PET the injection pressure range is 600 ~ 1400bars.

Hold Phase: This phase starts after the entire cavity is filled with the melt. During the hold phase a reduced
melt pressure is applied, about 30 % of the injection pressure. The additional material required for
compensate the product shrinkage is filled in hold.

Cooling: This time is given to cool the preforms, so that it could be handled without deformation in the
handling system. This may differ from machine to machine. In case of machine with ROBOT handling
o
system, the preform may be ejected at around 80 C, whereas in case of direct ejection system, the
o
preforms may be cooled to as low as 45 C.
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Ejection: The ejection of preforms to the conveyor or to the ROBOT handling system.

Mold open
Mold Closing Ejection

Mold Clamped Clamping Side

Cooling
Injection
Shooting Pot

Hold

Plasticization Extruder Side

Plasticization
Transfer
Screw Idle time

Cycle time Break Up for Shooting pot Injection Machines

Screw idle time: This is the time when the screw is idling without plasticizing or injecting / transfer. This
should as low as possible, may be 1 ~ 2 seconds.

Transfer: This phase is only in machine having a separate shooting pot for injecting the melt into the cavity.
During this phase the plasticized melt in the extruder is transferred to the shooting pot through the distributor.

Packing: This phase is also applicable for the shooting pot type machine. During this phase, the shooting
pot is packed with polymer under pressure. This follows the transfer phase, to adequately pack the polymer
into the Pot.
8.5: Preform Molding Process Setting
Parameter Significance Typical Values
Process Temperature
1 Hopper Throat First zone in the feed section of the The temperature set should not induce the
screw. The function of temperature in softening of pellets, leading to
this zone is to increase the heat agglomeration, hence the temperature,
o
content of the material, aiding the should be lowest, about 15 C less than
melting in the transition zone plasticizing temperature, 270 ~ 275 deg C.
2 Barrel The barrel heaters provide around ASPET 19C: 275 +/- 5 deg C
temperature 33% of heat required for ASPET 20 C: 280 +/- 5 deg C
plasticization. Balance is provided by ASPET 21 C/CF: 285 +/- 5 deg C
screw shear. ASPET22 CJ: 270 +/- 10 degC
3 Distributor The melt flow through distributor 2 ~ 5 deg C more than the Last zone in
temperature without any change. Hence, maintain the extruder.
temperature equal to melt
temperature, to avoid melt separation
4 Shooting Pot The melt is stored here for next shot. 2 ~ 5 deg C more than the extruder
temperature Temperature set should maintain the temperature.
melt without separation, as cross-
sectional diameter is high.
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5 Injection unit The narrowest cross-section melt Normally 5 deg C more than the Extruder
Nozzle channel in injection unit. Any ambient temperature.
temperature variation will have
remarkable effect on the melt
temperature.
Mold temperature
6 Sprue Sprue transfers the melt from Injection 5 deg C more than the extruder
Temperature Nozzle to Hot Runners. temperature.
7 Manifold Runner Manifold transfers melt to 5 deg C more than the Extruder.
temperature individual cavities.
8 Nozzle NT Nozzle NT, is normally a Time Depends on mold / Preform weight /
Proportional Heater. Keeps the melt Cycle time / incoming melt temperature.
from crystallizing & settling. Setting (%)
depends on volume of melt flow,
temperature and condition of incoming
melt.
Plasticizing Parameters
9 Screw Speed The screw rotation feeds, melts, and For 100mm screw speed is typically in
plasticize the pellets. Screw speed the range of 50 RPM.
depends on diameter of screw, it should
be maintained minimum, for target cycle
time.
10 Back pressure The backpressure aids in uniform Low IV & AA grades: 20~150 bar.
plasticizing of melt, and uniform mixing High IV: 50 ~ 300 bar.
of colorants. Backpressure may be higher by 50 bar,
when colorants are used, for uniform
dispersion of color.
11 Screw Idle time The waiting time of the screw before The screw Idle time should be as
start of Injection / Transfer. Low idle minimum as possible, in the order of 1 ~
time, reduces separation of colorant 2 seconds.
and melt. Ensure homogeneous melt.
12 Extruder Extruder cushion is the length of melt in 10 ~ 20 mm
Cushion front of the screw at end of Injection /
Transfer. Extruder cushion avoids of
variation in shot weight due difference
in melt conditions & feed. Protects
screw tip from damage.
Transfer Parameters
13 Transfer Pressure applied to transfer melts Typically 800 Bar or less than or equal to
pressure from extruder to shooting pot. maximum injection pressure.
Recommended to maintain the
pressure equal to Injection pressure
or lower.
13 Packing The pressure used for packing the Normally, 65 ~ 85 % of the transfer
pressure melt into shooting pot. pressure.
14 Packing time. The duration of packing pressure. 0.5 sec
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Injection Parameters
15 Injection The maximum pressure for injecting 600 ~ 1400 bar, depending on the mold.
Pressure the melt into cavity, in a laminar flow.
16 Injection The injection velocity profile is set to Preferred: Three stage.
velocity Profile give a constant flow in the cavity, so Stage 1: Size / Volume equal to the end
that the molecules are arranged in a cap Preform.
linear fashion. Speed 1: 30 ~ 35 m/s
Stage 2: Size / Volume equal to body of
the preform.
Speed 2: 50 ~ 70 m/s (To match injection
time)
Stage 3: Size / Volume equal to Neck
Finish of Preform.
Speed 3: 30 ~ 35 m/s
17 Injection time The time required for filling the cavity The rate of Injection for PET is 10 g/s ~ 12
with melt. g/s
18 Hold pressure Pressure required for packing the 30 ~ 40 % of Injection Pressure.
melt into the cavity, to compensate Recommended: Three stages.
shrinkage during solidification. Stage 1: 40% Injection Pressure.
Stage 2: 35% Injection Pressure.
Stage 3: 30% Injection Pressure.
19 Hold Time The time required for packing the 1.5 times the wall thickness of preform.
melt, to compensate shrinkage during Divided into three equal portions, for each
solidification. hold pressure.
2
20 Cooling time Time required to cool preforms to For 3 Stage Robot machines: t /4.
2
packing temperature or handling For machines without Robot: t
temperature in case of robot m/c.
t = Wall thickness of preform.
21 Transition The position of the Screw / Ram at Typically:
position which cavity is filled. Any additional (Cushion + 10% of shot weight)
melt injected further goes for
compensating the shrinkage of 80 ~ 100% of the value represents the
Preform on solidification. transition position.
Melt density is 1.2gms/cc, and
Preform density is 1.33gms/cc. Low wall thickness preform ~80%
High wall thickness preform ~100%
22 Shot Size The shot size is equal to weight of the Shot Weight: Preform weight X no. of
product produced in each shot + cavities.
Cushion Shot Volume: Shot weight / 1.2
Shot size: (Shot volume / Projected Area
of screw or Injection Ram) + Cushion.
23 Cushion The material in the front of the screw / 5 ~ 10 mm.
Injection Ram

Process parameter setting for injection molding is critical, as the machines gets faster and faster and their
throughput ever increasing any time consumed in setting a process right will increase the waste generated.
To start the machine and run it with least start up waste, it is very important to have the basic right. Following
are the basic parameters in injection molding, for which the values can be even set before starting the
machine, with the experience the PET industry accumulated.
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9. Stretch Blow Molding of PET
Stretch Blow Molding process involves the production of hollow objects, such as bottles, having biaxial
molecular orientation. Biaxial orientation enhanced physical properties, clarity, and gas barrier properties.

There are two distinct stretch blow-molding techniques.

Single stage.
Two stage.

In the one-stage process, preforms are injection molded, conditioned to the proper temperature, and blown
into containersall in one continuous process. This technique is most effective in specialty applications,
such as wide mouthed jars, cosmetics, where production rates are low.

In the two-stage process, preforms are injection molded, stored and blown into containers using a reheat-
blow (RHB) machine. This technique is best suited for producing high volume items.

9.1: Benefits of Stretching PET

There are two major reasons for stretching PET. The first is purely economic. Stretching allows thinner, more
uniform sidewalls and thus less expensive containers. Second, with the stretching orients the polymer matrix,
and hence dramatically improving the physical and barrier properties. Orientation is a physical alignment of
the polymer chains in a regular configuration.

Figure 1: Polymer Matrix

9.1.1: Typical Properties of Oriented & Un-Oriented PET


ASTM
Property Method Unoriented Oriented
Thickness, mm (mil) 0.25 (10) 0.36 (14)
Water Vapor Transmission Rate,
F372 6 (0.4) 2.3 (0.15)
g/m224h (g/100 in.224h)
Oxygen Permeability,
D3985 5.1 (13) 2.2 (5.5)
cm3mm/m224hatm (cm3mil/100 in.224hatm)
Carbon Dioxide Permeability,
D1434 28 (70) 14 (35)
cm3mm/m224hatm (cm3mil/100 in.224hatm)
Tensile Modulus of Elasticity, MPa (psi) D882 2,200 (320,000) 4,960 (720,000)
Tensile Stress @ Yield, MPa (psi) D882 57 (8,300) 172 (25,000)
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9.2: General Stretching Behavior of Polyesters

Most materials fall into three basic categories of stretching behavior: elastic stretching, viscous stretching,
and plastic stretching.

Figure 2: (A) Stress vs. Strain

Elastic materials, like rubbers have memory effect, they return to the original shape after the force is relieved.
In the contrary the Viscous materials, like the tar, does not have any memory it retains the newly formed
shape, readily.

PET falls into Plastics. A typical stretching sequence for PET is shown in Figure 3. As force is applied to the
material, there is a region where very little stretching occurs (A). Here PET behaves somewhat like an elastic
material: if it is stretched only a small amount and released, it will shrink back to its original size. If stretching
continues past the yield point (B), however, the material will start to stretch and become thinner, causing
permanent deformation. In this region the stretching continues at almost constant force. Once the material
has been stretched past its natural stretch ratio (NSR) (D), a dramatic increase in force is required for
additional stretching to occur. This is known as the strain-hardening region (E). It is here that the highly
desired increases in physical properties are maximized. Therefore, it is critical that the natural stretch ratio be
surpassed slightly during the stretching process.

Figure 3: Typical Plastic Behavior

9.3: Factors affecting the Stretching Behavior of PET Preforms

A number of factors can affect the stress/strain curve. Four major factors are

Intrinsic viscosity (I.V.)


Copolymer level.
Temperature of blowing
Moisture level of PET preforms.
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Figure 4: Effect of Intrinsic Viscosity (I.V.)

Figure 5: Effect of Copolymer Level (CL)

Figure 6: Effect of Temperature (T)

Figure 7: Effect of Moisture Level (ML)

Since, all four factors have effect on the Stress Strain Curve, a fundamental of stretch blow molding
process, a thorough understanding and control of these parameters is necessary to have a good bottle.
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Intrinsic Viscosity: Slight variations in I.V. can be compensated, by adjusting the preform temperature. As
I.V. goes down, the reheat temperature should be reduced. If the preform I.V. is too low, however, it will
become impossible to blow high-quality bottles.

Copolymer Level: the resin manufacturer maintains Co-Polymer levels constant and they do not change
during the processing, hence the customer need not worry on the effect of the same, if he is not changing to
a different resin.

Temperature: By adjusting the lamp settings, preform temperature can be optimized. Typically, temperature
changes should be made in small increments; allow at least 5 minutes for the machine to equilibrate before
assessing the effect of the change.

The temperature of the preform should be maintained, not more than 2 degC above the temperature at which
the preform yields the pearlescent bottles (this is the lower processing temperature of the preform, can be
called as (P+2)). Ideally (P+2) temperature will result in better strain hardening for the particular preform /
bottle combination, and will be different for different Preform / Bottle combination.

It is also important that the temperature of the preforms being fed into the reheat blow machine is constant.
Preforms that are colder than set; will tend to yield bottles that are pearlescent. Preforms that is hotter than
set will tend to yield bottles that are hazy. To eliminate the need to adjust the temperature of the machine to
compensate for varying preform temperatures, maintain a constant preform storage temperature.

In cases where preforms have been stored in unusually cold or hot conditions, allow the temperature of the
preforms to reach the normal preform temperature before feeding them into the machine. This process is
known as conditioning of the preforms. Normally the preforms are conditioned for 6 hrs in the blow molding
room, for a tropical environment, were the temperature changes are not more than 5 deg C.

Moisture Level: PET preforms start to absorb moisture almost immediately after they are molded. Within a
few days, the amount of moisture absorbed can start to have a rather dramatic effect on the natural stretch
ratio (NSR) of PET preforms. Reducing the reheat-blow temperature will help compensate for higher NSR
due to moisture. However, if the preforms get too "wet" because of long exposures to high humidity, it may
become impossible to make high-quality bottles from them.

Therefore, the best results can be obtained when storage time and conditions are consistent after molding
preferably no more than 2 days at 24C with low humidity. This condition does not exist in Indian
environment, were the preforms are blown at the filler location, depending on the production need.

To have a uniform blown properties of the bottle, preforms of not more than 2 days of production interval
should be mixed during the continuous loading in the hopper. If different age of preform is to be blown, the
earlier preforms should be emptied from hopper before next batch is loaded. The process parameter shall be
retuned to suit the preform with different age (moisture level).

9.4: Re-Heat Blow Molding

The critical stage of the Re-heat blow molding process is the design of the preform to match the bottle
design. For all the discussion under this topic, we assume that the preform is suitably designed for the blow
shell.

In the stretch blow molding process, the preform is placed inside the blow mold and preblow (low pressure)
air is introduced. As pressure starts to build within the preform, there is very little initial expansion. The
stretch rod pulls the preform down till the base. An aneurysm (bulb) starts to form in the middle of the
preform. At this point, high-pressure blow air is used to finish blowing the prebottle out against the inside wall
of the mold.
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When blown correctly, the bottle should have a wall thickness that is relatively uniform starting at about the
middle of the shoulder and going down the entire sidewall to a point about midway around the base. If the
prebottle is not formed, the center section of the sidewall will be much thinner than areas toward the base
and shoulder region of the bottle.

Number of variables can prevent the formation of the proper prebottle. These include:

Preform I.V. too low due to improper drying.


Preform I.V. too low due to the use of too much regrind.
Preform temperature too high.
Preform moisture level too high.
Preform designed for a different NSR resin.

In SBM, prebottle condition defines the NSR position of the preform. The pre blow pressure and the
stretching of the rod will be able to take the preform to the pre bottle condition (NSR), beyond which
additional force required would be delivered by the high blow pressure.

The surface area of the mold should be more the Pre bottle (NSR, at the particular blown condition for the
preform) by 5 ~ 10 %, to get a final bottle with best performance, in tensile & barrier properties. If prebottle is
larger than the mold cavity, when preform is blown, the surface of the mold stops expansion of the preform
before the NSR. This results in bottles having thin sidewalls and thick shoulders / bases.
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9.5: Re-Heat Blow Molding Start Up Anomaly & its Significance

Pearlescence and haze are both aesthetic defects that reduce the clarity of a bottle. While both have the
same general hazy appearance, the cause for each is entirely different.

When a clear preform becomes hazy in the RHB process, it is because the preform was too hot and started
to crystallize. In the vast majority of cases, crystalline haze is due to low I.V. This is because the
crystallization rate of PET increases as the I.V. decreases. Since a preform is heated from the outside, haze
occurs on the outside surface.

Pearlescence, on the other hand, occurs on the inside surface. It is due to two factors. First, the inside
surface of the preform must stretch approximately 35% more than the outside surface for a 2-liter bottle.
Second, the inside surface is the coolest part of the preform and therefore does not stretch as easily as the
warmer areas toward the outside. The combination of both factors causes the PET to stretch much too far
into the strain-hardening region, producing thousands of very tiny cracks. These micro fractures affect the
passage of light and cause a somewhat hazy appearance. Pearlescence can be distinguished from
crystalline haze by its luminous sheen that is similar to an oyster pearl.

When the preform I.V. is correct, it is relatively easy to find an RHB temperature setting that will heat the
inside surface enough to avoid pearlescence but not so hot that the outside becomes hazy. If the preform
I.V. gets too low, however, it may become impossible to make clear bottles. In these cases, increasing the
temperature to eliminate pearlescence will make the haze worse, whereas decreasing it to eliminate haze
will make the pearlescence worse

9.6: Establishing Optimum Reheat-Blow Conditions

To produce a uniform bottle sidewall thickness, RHB conditions must be properly adjusted.

1. The stretch rod should be used only to center the gate of the preform in the bottom of the bottle; do
not use it to obtain orientation. If the speed of the rod can be adjusted, reduce it to the point where
the gate moves off center. Then increase the speed in very small increments until the gate is again
centered. Hold that speed setting.

2. Increase the line speed until a slight pearlescence appears. Then adjust individual heater
temperatures to make the pearlescence uniform. Clear areas indicate the preform is hotter in that
location; temperature in these areas should be reduced. Once the pearlescence is uniform, decrease
the line speed to its normal setting.

3. If the machine is normally run at its maximum speed, a different approach will be required. Reduce
the temperatures of the heaters until a slight pearlescence appears; then adjust the individual
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heaters to make the pearlescence uniform. Once it is uniform, record the settings. Then increase the
temperature of each by the same relative amount. For instance, if one heater is set at 80 and
another at 40, and an increase of 5% is desired, increase them to 84 and 42 respectively. By doing
this in small increments, the pearlescence should disappear in a uniform manner.

4. If the bottle sidewall thickness is not uniform, increase the preblow pressure and check the uniformity
again. If this makes the sidewall less uniform, decrease the preblow pressure.

5. Once optimum preblow pressure is established, further improvements can sometimes be made by
adjusting the timing of the preblow relative to the timing of the stretch rod. Therefore, change the
preblow timing so that it starts sooner, as well as later, in the sequence and assess the results to
determine which timing is best.

NOTE: The preblow pressure and the time can have a great effect on the thickness of the shoulder
and base of the bottle. An increase in both will usually increase base thickness, while a decrease in
both will typically increase shoulder thickness.

6. If there is no noticeable change in wall thickness, by changing the preblow pressure and its timing,
increase the high-pressure blow delay time. As high pressure may be coming on too soon, thus not
giving preblow chance to do its job.

7. If changes in the high-pressure delay do not give the desired thickness uniformity, try increasing the
stretch rod speed in small increments.

8. As a last resort, change the heater profile. Normal practice of tuning the heater profile, practiced by
many engineers as quick measure, reduces the performance of the bottles, even though it may not
be visually found. A drop in properties, like GV, & top load is very much imminent.

When adjusting the machine, never change more than one variable at a time.

9.7: Bottle Shrinkage and Creep

After a bottle is blown, it will shrink as the internal stresses relax. While most of the shrinkage occurs
immediately after blowing, the bottle will continue to get smaller for several days. The reverse of this occurs
when the bottle is filled with carbonated soft drink; the high pressure [typically 0.41 MPa] will cause the bottle
to "creep" or expand. It is important that the degree of shrinkage and creep be controlled since most bottlers
have strict specifications on the maximum limits.

Reheat-blow conditions have a great effect on shrinkage and creep. Bottles blown from preforms that were
heated to a temperature just slightly above the pearlescent point [approximately 95C] will shrink the most
but will have the best resistance to creep. The opposite is true of bottles made from preforms that were
heated to a higher temperature, just slightly below the haze point [approximately 105C]; these bottles will
shrink less but creep more.

While preform temperature generally has the greatest effect on the level of bottle shrinkage, it is important to
note that the temperature of the blow mold will also have an effect.

Warmer mold Higher post mold shrinkage.

Cold mold Lower post mold shrinkage.

This is because a warm mold tends to promote relaxation of internal stress. For the same reason, bottles
stored in a warehouse will shrink more during the hotter months.
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10. Injection Stretch Blow Molding

Single stage machine process resin and provide bottle as output. Single stage machines are basically of two
types four station versions and three station versions. These machines mold the preforms in first station and
blow them to bottles in their 2 / 3 stations.

The main advantage of these machines is that they do not require additional energy to heat the cold
preforms for blowing, as in two stage machines. As here the preforms are ejected from the mold at
temperature close to blowing temperature and conditioned at the next station, so that the temperature is
more or less uniform across the cross section of the preform, as required for blowing.

In these machines the preforms are held in position, without any rotary motion imparted to them. Hence it is
possible to heat the particular sector of the preform and control the blow-ability of the preform sector wise,
which is extremely helpful in blowing, unsymmetrical cross section containers, such as Kidney shape used in
liquor, oblong shapes used in cosmetic industry, with uniform wall thickness along circumference.

In single stage machines the preforms are held by means of neck rings as it is molded, and hence there is no
tilting or variation in positions as they are moved between stations. The accurate position of preforms help
them blow uniformly without any gate offset and variation in wall thickness for bottles with volumes less than
60 ml, which becomes extremely difficult in case of two stage machines due to small size of preforms and
inability to hold tight at exact position.

The containers made out of single stage machines always have less scratches and blemishes, since the
preforms do not come in contact with each other. In two stage process preforms are packed together in
cartons, rubbing of surfaces of preforms and hard gates of preforms, causes, considerable scratches. Which
when blown spoils the surface appearance of the bottle.

Functional units of Single stage machine:

Extruder: Plasticize the pellets into uniform melt. The L/d ratio of the screw used in these extruders are 21:1
to 25:1, to aid uniform gentle plasticization.

Conditioning Station Injection Station


Condition the make preform
preform for blowing
Extruder:
Plasticize
the pellets

Blow Station
Blow into
bottle

Ejection Station
Eject the bottle

4 Station Stretch Blow Molding Machine


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Injection Station: The injection station consists of injection mold mounted over a hot runner, which
distributes the melt from the extruder to individual cavities, at uniform rate & pressure.
The injection mold consists of three functional parts the Cavity, which is mounted over the hot runner; Core,
which is fixed to the top moving platen; and the Lip / Neck rings, which forms the threaded portion of the
preform, mounted to the indexing table. The number of sets of lip plates is equal to number of stations in the
machine. The neck rings in the lip plate carries the preforms, to other stations, till ejection.

Conditioning station: The objective of the conditioning station is to increase the temperature of the preform
skin, and to maintain uniform along the cross section of the preform. The conditioning station is present in
four station machines. In case of three station machines the conditioning process is accomplished by
preform design and cooling channel balancing in the injection mold.

Injection Stage:
Blow Stage: make preform
Blow into
bottle Extruder:
Plasticize
the pellets

Ejection Stage:
Eject the bottle

3 Station Stretch Blow Molding Machine

The conditioning station consists of two features; the provision for heating the outer wall of the preform is
called a POT, this normally provides additional heat to the external surface, which is cooled faster in the
injection mold, due to higher cross sectional area of cooling water channels.

The feature to heat or cool the inner surface of the preform is called the CORE. Cooling cores are normally
used in unsymmetrical cross section bottles. They basically cool the preform interior for the particular sector,
for which the thickness needs to be increased, or which forms the farthest surface of the bottle from the
center. The conditioning core temperature is maintained by circulating water / oil from thermo-regulator.

The schematic diagram shows the operation of a conditioning core, with elliptical cross section bottle. Here,
you can see the major diameter of the ellipse is more than 2.5times the minor diameter. Hence the sector,
which forms the minor surface needs to be stretched faster, before it comes in contact with the blow shell
wall, vice versa, the sector which form the major surface of the ellipse, to be stretched slower, so that it does
not thins, thus achieving uniform wall thickness along the entire circumference. To achieve lower
temperature at sector which needs to be stretched slower, the conditioning core is brought in contact, to cool
the sector. The sector which needs to be kept warm is relieved so as to maintain higher temperatures.
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Preform
Bottle

Conditioning core:
Cool the sector, and
increase wall thickness.
Conditioning core operation Cross sectional view

Heating cores are normally deployed in conical preforms, which have thick shoulder area, which needs to be
heated more to distribute the wall thickness evenly. They are heated by electrical systems.

Schematic view: Heating Core


Heating core in operation UP:
Not in use

Heating core
Down:
In operation

Conical preform

Heating pot consists of heating elements, heated electrically; there may be 2 to 5 horizontal zones
depending on the length of the preform.
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Heating Pot Bottle Cap


Zone 1, 2, 3
Preform

Bottle

Schematic diagram: Heating pot operation

Blow Station: Blow station, blows the conditioned preforms into blown final bottle. The blowing is
accomplished by means of primary blow, which is a low pressure blowing operation, in the order of 4 ~ 10
bars, which helps in forming the pre-bottle, during the stretching operation.

The secondary blow or the high pressure blow is in the order of 25 bars to 35 bars depending the bottle
stretch ratio and intricacies.

Once the bottle is blown it is cooled by the blow mold surfaces to solidify the polymer matrix. Normally the
blow mold is maintained at temperature of 20 ~ 25 degC.

Ejection Station: At ejection station the bottles are ejected.


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11. Product testing Preform / Bottle

Bottle forms the final product and preforms is the intermediate product, we need to check the quality at these
two stages to ensure proper performance of the product at the final destination. Preform testing is more
critical as the PET resin undergone transformation from a highly crystalline stage to an amorphous stage at
higher temperatures and pressures, and hence the chances of occurring defects are more at this stage and
identifying a defect at this stage will avoid subsequent wastage of material and energy at the next stage
(Blowing).

Preform quality check need to be conducted at various levels to ascertain the quality of the product;

Level 1: Visual inspection (with normal light)


Level 2: Visual inspection (With polarized light)
Level 3: Dimensional inspection
Level 4: Chemical inspection

Level1: Visual inspection (Normal Light)

Level 1 inspection is carried out with the naked eye with or without the aid of following tools;
1. White light table, with magnification glass, 5 X
2. Preform cutter.

Most of the start up defects come under this category, during a regular run, few of the these defects may
reappear due to faulty process conditions, which needs periodical check, as per the process machinery
consistency, hence frequency of such check to be decided by internal Quality control.

Level 2: Visual inspection (Polarized light)

Level 2, inspection is carried out with aid of polarized light inspection table, and inference charts.

The polarized light inspection indicates the nature of filling of the preforms and packing, by stress pattern
made visible by the polarized light. Another critical defect identified by this method is the surface moisture,
called the moisture ring due to the unique appearance.

Level 3: Dimensional check

Dimensional checks are one to confirm whether the preforms meet the nominal sizes and tolerances laid
down during design. Dimensional checks are done by measuring devices during initial run of the mold /
product qualification and during production normally a Go -No Go gauge is used to speed up the process.

The inspection aids for Level 3 process:


1. Vernier caliper
2. Screw gauge
3. Profile projector
4. Preform cutter
5. Go No Go gauge
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Level 4: Chemical test

Chemical test are done to ascertain transition undergone by the polymer during drying, plasticization, and
molding has not had any detrimental effect on the polymer, to affect the performance of the final product. The
two properties which are monitored at this stage are;
1. Intrinsic Viscosity (IV)
2. Acetaldehyde (AA)

The equipments used for this purpose and test methods are similar to the procedure done for PET resin, for
details refer Quality Parameter section 6.

Defects could be further classified as


1. Indicative defects
2. Major defects
3. Critical defects

Indicative defects: These defects are indicative of variation in quality of preforms due to variation
processing conditions and raw material. These defects may not create problems in final product quality, but if
they are not attended on time, may lead to more serious defects.

Major defects: These defects can create problems in blowing and have appearance problem in final product
(Bottle). These defects need immediate correction.

Critical defects: These defects will create problem in blowing as well as functional problems in the final
bottle quality. These defects need to be attended by stopping the machine in most cases as any delay in
correction will lead to wastage of material.

Classification of preform defects & effects

No. Defect Status Test Level Effect of defect


1 Bubbles Major Level 1 Bursting.
Double layer in bottle wall.
Poor bottle appearance.
2 Un-melt Major Level 1 Bursting.
Poor bottle appearance
3 Long gate Major Level 1 Probability to hit upper row of IR lamps.
Bottle gate deformation.
4 Stringing Indicative Level 1 Sticking to hot preform wall.
Surface lines on the bottle wall.
5 Moisture marks Critical Level 1 / 2 Bursting during blowing.
White patch or pearlescence like bottle wall
appearance.
Bottle wall weakness.
6 Gate crystallinity Critical Level 1 Stress cracking.
Bursting during blowing.
Weak gate / failure in drop test.
7 Hazy preform Major Level 1 Dirty bottle appearance.
Unstable blowing operation.
8 Knit line / crack Critical Level 1 Bursting of neck finish during blowing.
in neck finish Poor seal integrity.
9 Black specks Critical Level 1 Bursting during blowing.
Poor appearance.
10 Flash at neck Critical Level 1 Higher capping force.
finish Improper capping / seal integrity.
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11 Flash below NSR Major Level 1 Poor parting line appearance in bottle.
Preform holding and transfer problem in high
speed blow molders.
12 Gate dimpling Indicative Level 1 Poor gate appearance.
13 Gate peel off Indicative Level 1 Poor gate appearance
14 Internal gate Major Level 1 Weak gate.
deformation Drop test failure.
15 Burn marks Critical Level 1 Bursting during blowing.
Poor appearance
Higher AA
Lower IV / weak bottle
16 Heat splay Major Level 1 Weak bottle.
Poor surface marks.
17 Preforms Critical Level 1 Preform cannot be blown
buckling
18 Gate pin hole Critical Level 1 Bursting during blowing.
19 Color variation Major Level 1 Appearance problem.
20 Spider web Indicative Level 1 Poor appearance around gate.
21 Void in gate Critical Level 1 Bursting during blowing
22 Wall thickness Critical Level 3 Can cause dancing of preform in oven.
variation, > 0.2 Gate offset in bottle.
mm Uneven bottle wall thickness and weakness.
23 IV drop > 0.03 Critical, Level 4 Weak bottle.
dl/g CSD Higher stress cracking probability.
Higher gas loss in CSD bottles.
24 Higher AA, > 4 Critical, Level 4 Flavor change in water packed.
ppm Water
25 Neck finish Go Critical Level 3 Capping problem may arise
No Go failure
26 Neck finish ID Critical Level 3 Preform may not be held properly in blowing
Go No Go mandrel.
failure Capping may be a problem in case of inner
sleeve caps.

All the defects can be present in various degrees of intensity, which may call for difference in opinion than
the ones discussed above, which require expert opinion or the final end user comments.

Shelf life:

Normally the shelf life of the preform can be safely taken as 6 months, beyond which it may require further
testing to ascertain the suitability for the particular application. The storage ambient conditions of
temperature and humidity play a vital role in the shelf life of the preform. High moisture absorption of
preforms can lead to increase in Natural stretch ratio of the preform, which may lead to not optimally strain
hardened bottles, with lower strength, barrier properties etc,.
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Preform inspection sheet
Machine Date
Mold Operator
Cavities Time
Weight Box no.
Sample
No. Parameter AQL Defective
0.65% 1.5% 4.0%
1 Damaged neck finish 0.65%
2 Gate problems, Pin hole, void 0.65%
3 Full crystallinity, > 10mm diameter 0.65%
4 Spider web 4.0%
5 Contamination, dirt, oil 1.5%
6 Drag marks, sink marks 4.0%
7 Wall thickness variation, > 0.2mm 0.65%
8 Weight variation, > 0.5gms 0.65%
9 Neck finish, Go No Go failure 0.65%
Total defects
Sample size, Pcs. Status
32 Acceptance 0 1 3
Rejection 1 2 4
50 Acceptance 1 2 5
Rejection 2 3 6
500 Acceptance 7 14 21
Rejection 8 15 22
Inspected by Approved by

Typical preform inspection sheet

Bottle testing;

Bottle forms the final product of the PET chain, and it is used in direct contact with the food material, which is
stored, transported and protected by the inherent strength of the bottle. Hence the bottle testing should
consider the product packed and the conditions it is subjected during the shelf life for design of a specific test
method. The bottle test method and specifications will vary from product to product.

All PET bottle testing methods are in-process in nature, to help aid the blow molding engineer to tune the
machine to produce bottle to meet specifications.

1. Bottle sectional weight.


2. Bottle wall thickness.
3. Bottle volume.
4. Bottle top load
5. Bottle drop test
6. Bottle burst test.
7. Bottle stress crack test.
8. Bottle head space AA
9. Bottle shelf life.
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Bottle sectional weight:

Bottle sectional weight measurement is an easy method to control the distribution of wall thickness in the
bottle, as it can be done much quicker compared to actually measuring the wall thickness at all locations.

Here the bottle is cut into three pieces horizontally;

Section 1: Base section: Along the base mold parting line.


Section 2: Panel section: Along the top limit of the panel.
Section 3: Shoulder section: The remaining top portion.

The sectioning is done by hot wire cutter, with wires positioned along the exact position. The weights of each
section is calculated during the bottle design stage and adequate tolerance imparted based on the process,
so as to enable the blowing engineer to take a quick decision on the process changes.

Base Section Label Section Shoulder Section

Cutting Location

Typical CSD bottle with sectioning lines

Bottle wall thickness:

Bottle wall thickness is measured to ensure that there is no variation in the wall thickness along the
circumference of the bottle in a particular plane / section, due to gate offset or any other blowing variations. It
is also helpful to ensure proper wall thickness at intricate sections, which are critical for the strength of the
bottle like the petaloid legs. Bottle wall thickness is measured using a magnetic wall thickness tester, or by
means of CCD scanning. As the scanners are quite expensive in normal circumstances a magnetic probe is
used.
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Bottle volume:

Bottle volume test is done in order to ensure that the bottle is blow properly and also to control the volume of
the content, as filling machines fill quantities by means of fill height and not by measurement, hence and
variation in bottle volume will affect the product content.

Normally bottle volume is measured at two conditions; filled to brim, which is called the brimful volume, and
filled up the fill height, called the fill volume.

Brimful Volume: In brimful volume the weight of the empty bottle is measured, and followed by weight of
bottle with water filled to the brim level. The difference in weight give the weight of water, this value divided
by the density at the measuring temperature, gives the volume of the bottle.
Brimful volume is measured at time zero (immediately after blowing), and after 24 hrs, allowing for the bottle
to shrink and set, the volume at T + 24 hrs is always lower than the volume measured at T. Volume at
T+24 is considered as the final volume.

Fill Volume: Fill volume is the volume of the bottle, when filled up to the fill height. The fill level is measured
from the lip surface / top of the bottle, and specified in mm. The fill height is as low as 25 mm in case of
water bottle, as there is no need for a head space, to as high as 50 mm in case of carbonated soft drink
bottle, to allow for adequate head space for carbon dioxide. The procedure for measurement of fill volume is
also same as that of brimful volume, except here the water is filled up to the fill point.

Bottle top load:

Top load test is done to understand the stack ability of PET bottle crate, over another crate during storage.
Top load strength or the nominal top load depend on the storage requirements, and differ for different bottle
capacities and products. Top load test is conducted on a top load tester, with capacity up to 100Kgs.

Typical top load values:


Top load (Kgs)
No. Bottle volume Water CSD
1 500 ml 7.5 35
2 1000ml 10 35
3 1500ml 12 35
4 2000ml 16 35

Bottle drop test:

Bottle drop test is done to understand failure of bottle in drop fall during handling of bottles. Drop test are
conducted under three conditions;
1. Vertical drop
2. Horizontal drop
o
3. Oblique drop (45 )
All the drop tests are conducted for 1.5 meter fall of filled bottle up to the fill point.

Vertical drop test: The bottle is filled up to the fill point and capped. The bottle is held by the neck and
allowed to fall from 1.5 M on a flat concrete surface. The drop is done for 3 times for the same bottle
continuously and the failure if present is recorded.

Horizontal drop test: The bottle is filled up to the fill point and capped. Then it is held by the body
horizontally and allowed to fall horizontally on the concrete surface for three times continuously and the
failure if any is recorded.

Oblique drop test: The bottle is filled up to the fill point and capped. Then it is held vertically above a
o
concrete slab inclined at 45 to the horizontal plane at distance of 1.5 M, the drop is repeated for 3 times and
failure if any is recorded.
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Bottle stress crack test:

Stress cracking is the crazing or cracking that can occur when plastic is under tensile stress. PET material is
strongest in a highly oriented state, such as in the sidewall of the container. It is most susceptible to stress
cracking when it is in an amorphous state, such as in the area surrounding the center of the base (gate
area), and under tensile stress.

The following are the factors which can accelerate the stress cracking of bottle and eventually lead to
bursting of bottle abruptly, with high force, which is dangerous. Hence it is important to understand the stress
cracking strength of the bottle, through accelerated method.

High alkalinity of environment


Poor material distribution
Excessive IV degradation
Over carbonation
Contact with incompatible chemicals
High temperature exposure

Objective: To determine the level of resistance to sodium hydroxide induced stress cracking, on a
carbonated soft drink bottle.

Principle: One known mode of stress crack attack on PET bottles is by hydroxide ion. A bottle that has more
resistance to Sodium Hydroxide attack should be more resistant to stress crack initiators that a bottle may be
exposed to during its lifetime.

Apparatus:

1. Beaker / containers.
2. stop watch or timer
3. Compressed air regulated to 5.31 bars
4. distilled water
5. bottle closures
6. 0.2% NaOH solution prepared with distilled water and solid NaOH.

Sample quantity: 2 set for each cavity of blow mold.

Procedure:
1. Bottles should be less than 2 weeks old, then aged at 50C +/ -1 C and 50% RH for 24 hours. After
aging, the bottles should be stored at 22C +/ -1C for a minimum of 16 hours. Label the bottles.
2. Prepare the solution of 0.2% NaOH solution. (Alkalinity 2.4 -2.6 g/l CaCO3).
3. Fill each bottle with the target net contents of water. (2L bottle would contain 2000ml of water) The
water should be equilibrated to 22C +/- 1 C.
4. Pressurize each bottle with compressed air to internal pressure of 5.31 bars.
5. 5 minutes after pressurizing the bottles mark the liquid level on each bottle and then gently place
each bottle into beaker of 0.2% NaOH solution at 22C +/-1C. The solution must cover the base. Start
the timer and check at following frequency.
Time Frequency of check
0 ~ 30 Continual check
30 ~ 60 Every 2 minutes
60 ~ 90 Every 5 minutes
6. Record the time to failure in minutes for each bottle. Failure is defined as a burst or a slow leak. A
slow leak is evidenced by a visual fill point drop.
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Report:
1. Complete fill out report form including Alkalinity of the NaOH solution, Room Temperature, Bottle
Temperature, and Caustic Temperature.
2. Preform numbers and blow cavity numbers.
3. Time to failure in minutes
4. Location of failure, choosing one of five categories:
a. Gate through or tangent to it.
b. Amorphous region (around gate and stretch rod area)
c. Oriented region (base of foot)
d. Strap area
e. Stretch rod impression
5. Type of failure, i.e. catastrophic (burst) or slow leak.
6. Manufacturing defects, if present.
Bottle head space AA

Bottle head space AA method check the amount of AA that has migrated into the empty space of the bottle
over a period of 24hrs or higher depending on the requirement of the customer, under standard temperature
(25 degC). This value is used to extrapolate the amount of AA that will migrate to the content after packing in
storage. This helps the designers and quality controllers to design and control the impact of AA on the
packed contents.

Equipments used:
Gas chromatograph with capillary column to sense AA in 1 ~ 10 PPB, head space sampler.
Nitrogen gas for purging
Temperature cabinet to maintain 25 deg C.
Septum for sealing nitrogen purged bottles.

Procedure: Freshly blown bottles collected from the machine are purged with nitrogen, so that the
atmospheric air does not interfere with the analysis. The bottles are closed with septum and kept in
controlled environment for 24 hrs. After 24hrs the bottle internal space air is collected by means of a head
space sampler with a needle, and injected into the gas chromatograph, which gives the results in PPM (parts
per billion).

Shelf life:

Bottle shelf life: Blown bottles do not normally have a fixed shelf life, and can be used after any duration,
excluding the case of Hear set bottles. But the users may be aware of the fact that bottles undergo
continuous secondary shrinkage after the primary post mold shrinkage. Hence brimful volume of the bottles
could have considerable variation depending on the period of storage and the ambient conditions.

Product shelf life: Product shelf life with the bottle is a complex analysis which depends on the product
packed and the requirements of the product manufacturer, which may differ from case to case. In basic term,
a shelf life study for product and package combination is to study the period till which the product can be
safely stored in the package in a shelf without any degradation in its preset qualities for consumption.

In case of a carbonated drink, a loss 15% of gas volume of carbon dioxide is considered as the end of the
shelf life. i.e. directly proportional to the outward migration of carbon dioxide from the product.

In case of beer packaging, apart from carbon dioxide outward migration, the inwards migration of oxygen is
also critical, which causes stalling and settling of beer.

Whereas in case of a crisp product the migration of moisture into the package which cause the loss of
crispness of the product is considered for estimating the shelf life.

Hence the equipment and procedure used for estimating and analyzing the shelf life will also differ from
product to product.

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