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[1]
IN-PLANT TRAINING
REPORT
At

(1st
July to 28th
July)
Product Application and Research Centre,
(P.A.R.C.)
Chembur,Mumbai
Submitted by:
Suyash Trivedi
Central Institute of Plastics Engineering & Technology
(C.I.P.E.T.)
Lucknow
[2]
Preface
The main purpose of this project was to provide us the opportunity to
expand our theoretical concepts and lessons to a practical level of
working, thereby helping us to understand the application of those
principles in real situations.
Therefore our college “Central Institute of Plastics Engineering &
Technology” gives due importance to this aspect of education by
providing us this internship in a reputed business house “Reliance
Industries Ltd – Product Application and Research Centre
(PARC)”, to enhance our practical experience.
Our area of work during the internship was to work in the lab and
perform various tests relating to plastics and in the processing area to
learn different processingtechniques used for plastic.
This process has given us invaluable experience and enriched our skills
not only relating to polymer but also about raw materials, manufacturing
processes,testing etc.
We are thankful to PARC-RIL for providing us this good experience.
[3]
Acknowledgements
The training opportunity we had with Product Application and Research Center (PARC),
Reliance Industries Ltd (RIL) was a great chance for learning and professional
development. Therefore, we consider ourselvesas very lucky individuals as we were
provided with an opportunity to be a part of it. We are also grateful for having a chance
to meet so many wonderful people and professionals who led us though this internship
period.
We are deeply grateful to Mr. S.V.Raju, Head of the Department - Product Application
and Research Center (PARC), Reliance Industries Ltd (RIL) and Dr.Nitin V Joshi, Lab
in charge – PARC,RIL for extending its training facilities and giving us an opportunity
to gain an insight into the working of an industry.
We are using this opportunity to express our deepest gratitude and special thanks to
Mr.Nitin V. Joshi, our guide who in spite of being extraordinarily busy with his duties,
took time out to hear, guide and keep us on the correct path and allowing us to carry out
our training at their esteemed organization.
We would specially like to thank Mr. TusharDongre, Mr. Zubair Ahmed,Mr.Vinod
Kumar,Mr.Ajit Patel, Mr.Sundareshan,Mr.SunilMahajan,Mr. Surendra Gupta and
Mr. Kulkarni for their support and co-operation throughout the training period in spite of
their busy schedules.
Our sincere regards to Mr.Ravi Kumar, Mr. NileshBakare,Mr.RavindraKute,
Ms.RenukaSarode, Ms.SmithaKumbhare, Ms.NehaPawar, Ms.HimaPadhiar, Mr.
SoorajVadathala andMr.JigarPalecha for their continuous help during the training.
We are highly indebted to the executive & technical officers of PARC for their everyday
guidance and help and special thanks to Mr. AnantPawar, Mr.AjitGhate& Mr.
LalitPathaskar for their help in the processing centre.
Finally we would like to thank all the office and support staff for extending their
cooperation throughout the course of this training.
[4]
TABLE OF CONTENTS
Company Profile………………………………………………………..5
Manufacturing Facilities………………………………………………..7
Introduction to Polymers Testing at PARC………………………….…13
Introduction to PARC…………………………………………………24
Testing Division……………………………………………………….25
Processing Division……………………………………………………69
[5]
1. Company Profile
The Reliance Group , founded by Dhirubhai H. Ambani, is India's largest private sector enterprise,
with businesses in the energy and materials value chain. The flagship company, Reliance Industries
Limited, is a Fortune Global 500 company and is the largest private sector company in India.
Reliance Industries Limited (RIL) is an Indian conglomerate holding
companyheadquartered in Mumbai, Maharashtra, India. The company currently operates in
five major segments: exploration and production, refining and marketing,
petrochemicals,retail and telecommunications. The company is ranked114th on Fortune
Global 500 listof the world's biggest corporations for the year 2014. RIL is one of the
largest publiclytraded companies in India by market capitalization. It is the second
largest company inIndia by revenue after Indian Oil Corporation. RIL’s total turnover is
US$ 62.2 billionas of FY2014-15 making aa profit of US$ 3.8 billion. Reliance enjoys
global leadership in its businesses, being the largest polyesteryarn and fiber producer in the
world 2.5 million tons per annum and among the top five to ten producers in the world in
major petrochemical products.

RIL manufactures Polypropylene (PP), Polyethylene (PE) and Polyvinyl
Chloride(PVC) sold under the brand namesRepol, Relene&Reonrespectively.

Diverse applications across packaging, agriculture, automotive,
housing,healthcare, water and gas transportation and consumer durables.

Repol PP can turn any of your 'plastic' ideas into a reality.

Relene PE has completely transformed the concept of packaging.

Reon PVC is a versatile polymer with applications ranging from soft to rigid.
[6]

RIL has manufacturing sites atHazira, Nagothane, Jamnagar, Naroda and
Vadodara, Dahej, Allahabad, Dhenkanal, Barabanki, Kurkumbh, Nagpur,
Patalganga, Silvassa.

RIL is the largest producer of PE & PP in India.
Reliance's polymer business is integrated with its cracker facility at Hazira, as well as its
refinery at Jamnagar, ensuring feedstock availability at all times. The company operates
world-scale plants for Polyolefins and PVC with state-of-art technologies from global
licensors like Novacor, Geon and Union Carbide. Along with IPCL, Reliance is among the
world's top 10 plastic producers.
Reliance Industries Limited is Asia's largest manufacturer of Polypropylene (PP). Reliance
figures the fifth largest Polypropylene producers in the world. The four production sites
offer a wide range of Homopolymer, Random and Impact copolymer grades. These can
cater to the entire spectrum of Extrusion, Injection & Blow molding processes.
“Relene” HDPE is available in densities ranging from 0.941g/cc to 0.965g/cc & melt flow
index from as low as fractional to 20. Relene HDPE is widely used for numerous extrusion
& molding applications. Specially formulated HDPE Raffia grade has placed "Relene"
way above the competing materials for this application. The grade has excellent
processability on high output raffia lines & exhibits superior balance of tenacity /
elongation.
Reliance LLDPE grades are marketed under trade name "Reclair" & is available in density
range of 0.916 to 0.935 g/cc & MFI range from fractional to as high as 50.
[7]
2. Manufacturing Facilities
1.Hazira
Hazira Manufacturing Division is located near Surat, Gujarat. It comprises of a Naptha
cracker feeding downstream fibre intermediates, plastics and polyester plants.
The first phase of the complex was commissioned in 1991-92 to generate power/utility and
to manufacture Ethylene Oxide (EO), Mono Ethylene Glycol (MEG), Vinyl Chloride
Monomer(VCM), Poly Vinyl Chloride (PVC) and High Density Polyethylene (HDPE). A
jetty was built for loading and unloading operation of raw material and final products.
The second phase of the project, started in 1995, involved commissioning of the Polyester
Complex (POY & PSF) and continued in full backward integration with commissioning of
the new Polypropylene (PP), Naphtha Cracker, Purified Terephthalic Acid (PTA) plants
and also involved expansion of existing phase 1 plants.
2.Jamnagar
Jamnagar Manufacturing Division is located near Jamnagar, Gujarat. It comprises of a
petroleum refinery and associated petrochemical plants. The refinery is equipped to refine
various types of crude oil (sour crude, sweet crude or a mixture of both) and manufactures
various grades of fuel from motor gasoline to Aviation Turbine Fuel (ATF). The
petrochemicals plants produces plastics and fibre intermediates.
The Polypropylene plant at Jamnagar has a huge capacity of 1030 KTA of Polypropylene
producing a wide range of grades that cater to an equally diverse range of sectors which
include Raffia, Films (BOPP/IPP), Injection Molding, Extrusion, Fibre etc.
The new PP line in the SEZ facility resulted in additional capacity of 900 KTA.
[8]
3.Allahabad
Allahabad Manufacturing Division located in Allahabad, Uttar Pradesh, is spread over 105
acres.It is equipped with batch polymerization and continuous polymerization facilities.
The batch plant produces wider range of specialty polymers and continuous plant produces
both commodity and differentiated products. Both the plants are equipped with pilot
positions to produce customer specific products and for development activities. The plant
also has integrated facilities of draw twisting, draw texturizing, Yarn Dyeing and Twisting.
The first phase of the plant was commissioned with a batch plant
in 1991 with technology from Toray Industries Inc. , Japan. In the second phase, the plant
was further expanded in 1997 with technology from Toray
Engineering Company, Japan. Since then, the plant has developed indigenous technologies
with its development activities to produce a large range of
Specialty polymers, for different downstream processes like draw twisting, draw warping,
draw texturizing, air texturizing etc.
4. Nagothane
Nagothane Manufacturing Divisionlocated in Raigad, Maharashtra, is spread over 1,860
acres.It comprises of an ethane and propane gas cracker and five downstream plants for the
manufacture of polymers, fibre intermediates and chemicals.
5.Patalganga
Patalganga Manufacturing Division located near Mumbai, Maharashtra, is spread over 200
acres. It comprises of polyester, fibre intermediates and linear alklyl benzene
manufacturing plants.
[9]
Products Manufactured:
Product Manufactured from
Para - Xylene (Px) Naphtha
Purified Terephthalic Acid (PTA) Para - Xylene
Polyester Filament Yarn (PFY) PTA & MEG
Polyester Staple Fibre (PSF) PTA & MEG
Linear Alkyl Benzene (LAB) Kerosene - n paraffin
6. Naroda
Naroda Manufacturing Division located near Ahmedabad, Gujarat, is RIL’s first
manufacturing facility. This synthetic textiles and fabrics manufacturing facility
manufactures and markets woven and knitted fabrics for home textiles, synthetic and
worsted suiting and shirting, ready to wear garments and automotive fabrics.
7.Dahej
Dahej Manufacturing Division is located near Bharuch, Gujarat. It comprises of an
ethane/propane recovery unit, a gas cracker, a caustic chlorine plant and 4 downstream
plants, which manufacture polymers and fibre intermediates.
The plant has its own facility for separating ethane/propane. The ethane / propane mixture
is used as a feedstock for the gas cracker plant.
The division was commissioned in two phases. The Caustic Chlorine, VCM and PVC
pants in phase one was commissioned in 1997. After this, in phase two, HDPE plant, MEG
plant, ethane / propane recovery plant and gas cracker unit were commissioned in 2000.
[10]
8. Hoshiarpur
RIL- Hoshiarpur Division is located in Hoshiarpur, Punjab. It manufactures a wide range
of PSF, PFF, POY and polyester chips.
The Plants at Hoshiarpur Manufacturing Divisional
The plants of PSF-I, PSF-II, POY, PFF are commissioned in 1989, 1995, 1995, 2004.
In addition to the regular products, Hoshiarpur Manufacturing Division has added the
following differentiated value added products:
1. Dope Dyed Olive Green & Khaki Fibre
2. Recron 3s for Construction & Paper Industry
3. Polyester Fibre Fill
4. Cluster Fibre
5. Conjugate Fibre
9. Nagpur
Nagpur Manufacturing Division is located in Nagpur, Maharashtra. It manufactures
polyester filament yarn, dope-dyed specialty products of different ranges, fully drawn yarn
and polyester chips.
The plant has facilities like housing for its employees, school, guest house and a Ganesha
temple.
RIL - Nagpur Manufacturing Division is an ISO: 9001:2000 certified unit accredited by
BVQI, along with certification for ISO14001: 2004 and OHSAS 18001:1999 as well.
Products Manufactured:
1. Polyester Filament Yarn (PFY) from PTA & MEG
2. DD Specialty product of different range
3. Fully Drawn Yarn
[11]
10. Barabanki
Barabanki Manufacturing Division is located near Lucknow, Uttar Pradesh. It
manufactures Black Fiber.
Barabanki Manufacturing Division was commissioned in January, 1987, with technical
collaboration from M/s. Du Pont, USA to manufacture 15,000 MT per annum of
Commodity Polyester Staple Fibre. The capacity was gradually increased to 30,000 MT
per annum by de-bottlenecking. The Commodity Polyester Staple Fibre produced was sold
in national and international markets.
In 2004, further capacity of 10,000 MT per annum was added by installing an extrusion
based Spinning Plant. With this addition the present installed capacity of Barabanki
Manufacturing Division is 40,000 MT per annum.
11. Silvassa
Reliance Silvassa Manufacturing Division is located in the Union Territory of Dadra and
Nagar Haveli. It manufactures a wide range of specialty products such as Recron Stretch,
Linen Like, Melange, Thick-n-thin and Bi-shrinkage yarns.
This division is the largest unit of it's kind in the world engaged in the field of texturizing
of polyester partially oriented yarn (POY) to produce a wide range of polyester textured
yarns (PTY) such as crimp, tex, intermingle in various deniers ranging from 30 D to 1200
D. The Denier per Filament (DPF) ranges from 0.5 to 4.8. It produces a wide variety of
specialty products such as Recron Stretch, Linen Like, Melange, Thick-n-thin and Bi-
shrinkage yarns. This division is the largest supplier of Recron stretch products to Denim
industry in India. Moreover, it also offers various tailor-made products to suit the specific
end use requirements. The textured yarn produced is used in suitings, shirtings, dress
materials, home furnishings and automotive fabrics.
This division has 158 state-of-the-art false twist texturising machines of Barmag, Murata,
TMT, ICBT, Himson and Alidhra makes. The installed capacity of division is 150 KTA
[12]
and it exports 25 % of its production to various high quality demanding advanced markets
of Europe, USA, North America, Far East and African markets to about 45+ countries.
This division enjoys various international certifications and accreditations such as ISO
9001, ISO 14001, OHSAS 18001 and Oekotex certificate for exports. To achieve continual
improvements and growth, the Division has also deployed Six Sigma & Quality Circle
activities in various functional areas.
This division offers the best quality products with a three tier quality assurance system. All
the machines are equipped with on line tension monitoring (OLT) system wherein every
meter of yarn is continuously monitored by computers for product quality during
texturising, itself.
The products deliver competitive edge to the customers by virtue of :
Equal length packages that minimize waste,
Uniform package density for consistent package unwinding at high speed,
Continuity of batch nos. to enhance productivity and reliability,
100 % transfer tail end to improve the machine efficiencies
12. Vadodara
Vadodara Manufacturing Division located in Vadodara, Gujarat. It comprises of a Naphtha
cracker and 15 downstream plants for the manufacture of polymers, fibers, fiber
intermediates and chemicals.
[13]
Introduction to Polymers Testing at PARC
Polypropylene
Polypropylene (PP), also known as polypropene, is a thermoplastic polymer used in a wide
variety of applications including packaging and labeling, textiles (e.g., ropes, thermal
underwear and carpets), stationery, plastic parts and reusable containers of various types,
laboratory equipment, loudspeakers, automotive components, and polymer banknotes. An
addition polymer made from the monomer propylene, it is rugged and unusually resistant
to many chemical solvents, bases and acids.
There are three general types of polypropylene: homopolymer, random copolymer, and
block copolymer. The comonomer is typically used with ethylene. Ethylene-propylene
rubber or EPDM added to polypropylene homopolymer increases its low temperature
impact strength. Randomly polymerized ethylene monomer added to polypropylene
homopolymer decreases the polymer crystallinity, lowers the melting point and makes the
polymer more transparent.
Polymerization of propylene can yield any of the three polymer forms, isotactic,
syndiotactic or atactic. Polypropylene has three basic polymeric forms: isotactic,
syndiotactic and atactic. These different polymeric forms arise because, compared to the
starting substance for polyethylene CH2=CH2 (ethene), the starting substance propylene
CH3•CH=CH2 (propene), has a methyl (CH3) group in place of a hydrogen. In the
isotactic form of polypropylene the methyl group has the same configuration at each
tertiary carbon atom along the polymer chain. In the syndiotactic form, the methyl group
alters position on alternative tertiary carbon atoms. In the atactic form, the methyl group
takes up random positions on the tertiary carbon atoms.
[14]
Reliance Brand Name:Repol
[15]
Industrial Process:
Traditionally, three manufacturing processes are the most representative ways to produce
polypropylene.
Hydrocarbon slurry or suspension: Uses a liquid inert hydrocarbon diluent in the reactor
to facilitate transfer of propylene to the catalyst, the removal of heat from the system, the
deactivation/removal of the catalyst as well as dissolving the atactic polymer. The range of
grades that could be produced was very limited. (The technology has fallen into disuse).
Bulk (or bulk slurry): Uses liquid propylene instead of liquid inert hydrocarbon diluent.
The polymer does not dissolve into a diluent, but rather rides on the liquid propylene. The
formed polymer is withdrawn and any unreacted monomer is flashed off.
Gas phase: Uses gaseous propylene in contact with the solid catalyst, resulting in a
fluidized-bed medium.
Manufacturing:
Melt processing of polypropylene can be achieved via extrusion and molding. The most
common shaping technique is injection molding, which is used for parts such as cups,
cutlery, vials, caps, containers, housewares, and automotive parts such as batteries. The
related techniques of blow molding and injection-stretch blow molding are also used,
which involve both extrusion and molding.
Application:
Product Classification Features Uses
REPOL H110MA Homopolymer
Antistatic, Food
contact Acceptable
Blending;
Compounding,
Containers,
Furniture,
Houseware
REPOLSRM100NC Random copolymer
Antistatic; Food
Contact Acceptable;
High Clarity
Blow Molding
Applications;
Containers;
Household Goods
REPOL H030SG Homopolymer
Food Contact
Acceptable; Good
Processability
Industrial
Applications; Carpet
Backing;
Monofilament
[16]
REPOL H200MA Homopolymer
Antistatic; Food
Contact Acceptable
Thin-walled
Containers
REPOL B120MA Impact Copolymer
Food Contact
Acceptable; General
Purpose; Medium
Automotive
Applications;
Furniture; General
Purpose
REPOL H100EY Homopolymer
Antiblocking; Food
Contact Acceptable;
General Purpose
Slip Bags; Film;
Food Packaging;
General Purpose;
Packaging
REPOL SR20NC Random Copolymer
Food Contact
Acceptable
Blow Molding
Applications;
Bottles; Containers
REPOL H034SG Homopolymer
Food Contact
Acceptable
Pacific Bi-axially
Oriented Film; Film;
Food Packaging
Polyethylene
Polyethylene (abbreviated PE) or polythene (IUPAC name polyethylene or
poly(methylene)) is the most common plastic. Its primary use is in packaging (plastic bag,
plastic films, geomembranes, containers including bottles, etc.).
Polyethylene is classified into several different categories based mostly on its density and
branching. Its mechanical properties depend significantly on variables such as the extent
[17]
and type of branching, the crystal structure and the molecular weight. With regard to sold
volumes, the most important polyethylene grades are HDPE, LLDPE and LDPE.
 Ultra-high-molecular-weight polyethylene (UHMWPE)
 Ultra-low-molecular-weight polyethylene (ULMWPE or PE-WAX)
 High-molecular-weight polyethylene (HMWPE)
 High-density polyethylene (HDPE)
 High-density cross-linked polyethylene (HDXLPE)
 Cross-linked polyethylene (PEX or XLPE)
 Medium-density polyethylene (MDPE)
 Linear low-density polyethylene (LLDPE)
 Low-density polyethylene (LDPE)
 Very-low-density polyethylene (VLDPE)
 Chlorinated polyethylene (CPE)
Reliance Brand Name:Relene
[18]
Application:
HDPE
Raschel bags for fruits and vegetables , containers for packaging edible oil, processed
food, carrier bags, pipes for water supply, irrigation.
LDPE
LDPE is widely used for manufacturing various containers, dispensing bottles, wash
bottles, tubing, plastic bags for computer components, and various molded laboratory
equipment. Its most common use is in plastic bags.Trays and general purpose containers
Corrosion-resistant work surfaces Parts that need to be weldable and machinable Parts that
require flexibility, for which it serves very well Very soft and pliable parts such as snap-on
lids, six pack rings
LLDPE
Filmsfor packaging milk, edible oil, salt, roto-molded containers for storage of water,
protective films and pipes for agriculture.
There are different grades that are produced by reliance. Some of the grades along with
their applicationsare given below.
Product Classification Features Uses
RELENE1005FY20 LDPE
FoodContact Acceptable;
Good Heat Seal; Good
Impact strength
Film; Packaging
RELENE1070LA17 LDPE
Contact Acceptable; Good
Adhesion; Good
Drawdown
Coating
Applications; Film;
Laminates
RELENE
1003FA20
LDPE
Food Contact Acceptable;
Good Impact Resistance
Agricultural
Applications; Film;
Shrink Wrap; Wire
RELENE54GB012 HDPE
Bimodal Molecular Weight
Distribution;
Containers;Blow
Molding;Foodcontact
RELENE LDPE Food Contact Acceptable Flow Masterbatch;
[19]
16MA400 Thin-walled Parts
RELENE M60075 HDPE
Food Contact Acceptable;
Good Dimensional
Stability
Containers; Crates;
Industrial
applications;
Luggage
RELENE
1020FA20
LDPE Food Contact AcceptableFilm;
Laminates
RELENE 24FS040 LDPE
Contact Acceptable;
General Purpose
Food; High Slip
Bags; General
Purpose; Packaging
RELENE E52009 HDPE Food Contact Acceptable
Low Gel; Low Water
Carryover
Monofilaments; Tape
RELENE F19010 LLDPE
Antiblocking; Antioxidant;
ButeneComonomer
Food and film
Packaging
Polyvinyl Chloride
PVC comes in two basic forms: rigid (sometimes abbreviated as RPVC) and flexible. The
rigid form of PVC is used in construction for pipe and in profile applications such as doors
and windows. It is also used for bottles, other non-food packaging, and cards (such as bank
or membership cards). It can be made softer and more flexible by the addition of
plasticizers, the most widely used being phthalates. In this form, it is also used in
plumbing, electrical cable insulation, imitation leather, signage, inflatable products, and
many applications where it replaces rubber. Pure poly(vinyl chloride) is a white, brittle
solid. It is insoluble in alcohol but slightly soluble in tetrahydrofuran.
[20]
Polyvinyl chloride is produced by polymerization of the vinyl chloride monomer (VCM),
as shown.
About 80% of production involves suspension polymerization. Emulsion polymerization
accounts for about 12% and bulk polymerization accounts for 8%. Suspension
polymerizationsaffords particles with average diameters of 100–180 μm, whereas
emulsion polymerization gives much smaller particles of average size around 0.2 μm.
Chlorinated Polyvinyl Chloride (CPVC) is PVC (polyvinyl chloride) that has been
chlorinated via a free radical chlorination reaction. This reaction is typically initiated by
application of thermal or UV energy utilizing various approaches. In the process, chlorine
gas is decomposed into free radical chlorine which is then reacted with PVC in a post-
production step, essentially replacing a portion of the hydrogen in the PVC with
chlorine.CPVC shares most of the features and properties of PVC. It is also readily
workable, including machining, welding, and forming. Because of its excellent corrosion
resistance at elevated temperatures, CPVC is ideally suited for self-supporting
constructions where temperatures up to 200 °F (90 °C) are present.
Reliance Brand Name:Reon
[21]
Application:
Pipes and fittings, Door and window profile, rigid bottles and containers for packaging
applications, footwear, flooring & blood bags. The uses of different grades of REON are
Product Classification Features Use
Reon 67-01 PVC Homopolymer
Good Processability;
Homopolymer;
Medium Molecular
Weight
Film; Piping;
Profiles; Sheet
Reon 57GMR01 PVC Homopolymer
Low Molecular
Weight; High Flow;
Homopolymer
Foam; Handles;
Piping; Sheet
Reon 57-11 PVC Homopolymer
Good Processability;
High Flow;
Homopolymer; Low
Molecular weight
Bottles; Cosmetics;
Film; Handles;
Packaging; Piping;
Sheet
Reon 60-11 PVC Homopolymer
Good Processability;
Homopolymer; Low
Molecular weight
WeightBottles;
Containers;
Cosmetic
Packaging;
Cosmetics
Reon 57-01 PVC Homopolymer
Food Contact
Acceptable; High
Flow; Low molecular
weight
Containers; Foam;
Foamed Insulation
Board
Reon 57GER01 PVC Homopolymer
Good Processability;
High Flow;
Homopolymer; Low
Molecular weight
Bottles; Containers;
Cosmetics; Film;
Foam; Handle
Reon 67GER01 PVC Homopolymer
Good Processability;
HighFlow;
Homopolymer;Medium
molecular weight
Film; Piping;
Profiles; Sheet
[22]
Reon 60GER01 PVC Homopolymer
Good Processability;
High Flow;
Homopolymer; Low
Molecular weight
Bottles; Cosmetic
Packaging;
Cosmetics; Film;
Packaging
Reon 67GEF01 PVC Homopolymer
Food Contact
Acceptable;
Homopolymer;
Medium Molecular
weight
Cable Jacketing;
Footwear; Hose;
Insulation; Medical
application
Reon 67-11 PVC
Homopolymer
Food Contact
Acceptable;
Homopolymer;
Medium Molecular
Cable Jacketing;
Film; Footwear;
Hose;
Insulation;...View
entire Reon product
line.
 Plants of Reliance where Polymers aremanufactured
 Polypropylene
Type of Polymer
manufactured
Plant Sites
HP,ICP Hazira
HP Jamnagar DTA
HP Jamnagar SEZ
HP,RCP,ICP Naroda
HP,RCP Nagothane
[23]
 Polyethylene
Type of Polymer
manufactured
Plant Sites
LDPE Baroda
Nagothane
HDPE Gandhar
EVA
LLDPE/HDPE Swing Nagothane
Hazira
 Polyvinyl chloride
Type of Polymer
manufactured
Plant Sites
PVC Hazira, Baroda &Gandhar
[24]
4. INTRODUCTION TO PRODUCT APPLICATION &
RESEARCH CENTRE
The product application & research centre (PARC), Reliance Industries Limited
petrochemical division was established in 1990 at Chembur, Mumbai as a technical wing
of the polymer marketing division. It is deeply involved in the development of new grades
& the optimization of the existing grades in terms of cost & properties. It also carries out
continuous valuation of various lots produced at Jamnagar &Hazira plants. PARC is
committed to deliver value addition to polymer business of Reliance Industries Limited by
providing technical service, constant product up gradation and initiating market
development with the sole objective of total customer satisfaction. It also carries out
testing and trials of various modified and developmental grades.
PARC is a conduit between business enterprises and their vendors, converting basic needs
into commercially viable technology and helping to produce useful products. To fulfill
these objectives, sophisticated analytical & processing facilities have been established at
PARC.
PARC is recognized by the department of science and industrial research as an in-house
research & development wing of reliance-plastic & petrochemical division.
Functions of PARC:
Product development
Process development
Customer Support / Technical service
Co-ordination with plant & marketing department for benchmarking exercises
Training & manpower development
The Activities of PARC can be divided into:
Testing
Processing
[25]
5. TESTING DIVISION
Testing of raw material is absolutely necessary for quality control &
characterization. The analytical laboratory is involved in the analysis & testing of resin and
product samples received from the customers as well as from the PARC division.
Testing for resin:
 Melt Flow Index
 Ash Content
 Bulk Density
 FTIR Spectroscopy
 Measurement of Color
 Differential Scanning Calorimeter
 Thermo Gravimetric Analysis
 Density
Testing for plastic films:
 Shrinkage Test for films
 Tear Strength
 Coefficient of Friction (COF)
 Haze
 Dart Impact Strength
 Tensile Properties
 Haze test
Testing for Molded samples:
 Tensile properties
 Scanning Electron Microscope(SEM)
 Izod-Impact strength
 Shrinkage Test
 Heat Deflection Temperature &Vicat Softening point
[26]
 Environmental Stress Cracking Resistance (ESCR)
 Specular Gloss Testing
 Indentation Hardness Testing
 Flexural Properties of Plastics
 Gardener Impact Resistance
[27]
TESTING FOR RESIN
Melt Flow Index Determination
Reference: ASTM D1238
Machine Make:Davenport Flow Indexer.
Summary: For this, molten polymer is extruded through a die and flow of polymer
ismeasured under a specified load and at particular temperature per 10 min
Scope: This procedure is used to determine melt flow properties of resins with the help
ofDavenport Flow Indexer. Melt Index is an inverse measure of molecular weight.
Sinceflow characteristics are inversely proportional to the molecular weight, a low
molecular polymer weight polymer will have a high melt index value and vice versa.
Principle: MFI indicates the rate of extrusion of molten resin through a die of specified
length and diameter under prescribed conditions of temperature,load and piston position in
barrel.
[28]
Apparatus: (I) Melt Flow Indexer (Davenport make) with accessories:
Temperature: PE: 1900C
PP: 2300C
Preheating time :
o PP: 6 min
o PE:5 min
Barrel diameter= 9.5504 ±0.0016 mm
Die diameter= 2.0955 ± 0.0016 mm
Die Length= 8 ± 0.025 mm
Weight= 2.16 kg, 6.48 kg (± 0.5% of the total weight)
Procedure:
1. Manual
 A small amount of the polymer sample (around 4 to 5 grams) is taken as per the
expected MFI of material in the specially designed MFI apparatus. The apparatus
consists of a small die inserted into the apparatus, with the diameter of the die being
around 2 mm.
 The material is packed properly with the help of suitable piston inside the barrel to
avoid formation of air pockets.
 A piston is introduced which acts as the medium that causes extrusion of the molten
polymer.
 The sample is preheated for a specified amount of time: 5 min at 190°C for
polyethylene and 6 min at 230°C for polypropylene.
 Push the piston a little above the mark to ensure good packing (known as purging).
 After the preheating a specified weight is introduced onto the piston. Examples of
standard weights are 2.16 kg, 5 kg, etc.
 The weight exerts a force on the molten polymer and it immediately starts flowing
through the die.
[29]
 A sample of the melt is cut in regular intervals of time and is weighed accurately.
 MFI is expressed as grams of polymer/10 minutes of flow time.
2. Automatic
 Weigh the specimen and put it in the apparatus as per the expected MFI.
 Select remote control on apparatus and start the computer.
 In the computer start console software.
 Feed polymer type, melt density, cut-off length and file name.
 Start the test.
 Purge after 3 minutes just before the mark on piston.
 Put the arrester of 71mm or 81mm height depending on whether the material is Hi-
Flow or Low-Flow.
 Put the weight on plate above the apparatus.
 Record the output.
ASH CONTENT
Reference: ASTM D2584, D5630
[30]
Machine Make:Mettler Balance, Bunsen burner
Scope: This test is used to find out the inorganic residues in a polymer sample by ashing it
in a muffle furnace.
Summary: A weighed amount of sample is heated to 850±10⁰C and residue after treating
is expressed in terms of % ash content.
Principle: The organic matter in a polymer sample is burnt at 850±10⁰C until constant
mass of inorganic matter is obtained.
Apparatus: 1. Weighing balance
2. Silica crucible
3. Bunsen burner
4. Silica triangle & tripod
5. Holder
Sample specification: 3-5 g of sample
Procedure
 The sample weight and the weight of the empty crucible are noted.
 Sample is put in the crucible and allowed to burn till it becomes completely black
and the organic materials have vanished.
 In case of PVC sample (self-extinguishing in nature) the sample is now wetted
completely with 98% sulphuric acid and it is again heated to give out CaSO4.
 After heating, the PVC sample is now put in the oven for 1 hour at 850°C.
 For other samples, after burning is completed they are put in an oven maintained at
550°C
 Now the sample is kept in a desiccant (containing silica gel) for ½ hour to absorb
all the moisture.
 It is then weighed and the ash content is found.
Calculation
% ash content = Weight of ash × 100
Weight of sample
[31]
NOTE: WITH THE HELP OF STOICHIOMETRY WE CAN EASILYCALCULATE
THE WEIGHT OF FILLER CONTENT. FILLER CONTENT MEANS MIXTURE OF
CALCIUM CARBONATE AND MAGNESIUM SULPHATE(TALC).HEATING AT
850°CWILL HAVE NO EFFECT ON MAGNESIUM SULPHATE WHEREAS
CALCIUM CARBONATE DECOMPOSES INTOCALCIUM OXIDE AND GAS IS
RELEASED. WITH THE HELP OF CALCIUM OXIDE CONTENT LEFT WE CAN
EASILY CALCULATE THE AMOUNT OF CALCIUM CARBONATE PRESENT
INITIALLY.
FourierTransformInfrared Spectroscopy(FTIR)
Reference: ASTM E1252
Machine make-Perkin Elmer, spectrum 100 series
[32]
Principle:
FTIR utilize an ingenious device called Michelson interferometer, which was developed
many years ago by A. A. Michelson for making precise measurement of the wavelengths
of electromagnetic radiations.
FTIR instruments contain no dispersing elements and all wavelengths are detected and
measured simultaneously. Instead of a monochromator an interferometer is used to
produce interference patterns that contain the infrared spectral information.
In FTIR when an infrared spectrum is introduced to a sample stretching and bending of
various bonds takes place and due to different bond energies, each molecule absorbs
energy at a different frequency.
One of the components of an electromagnetic wave is a rapidly reversing electric field
(E). This field alternately stretches and compresses a polar bond. When the electric field is in the
same direction as the dipole moment, the bond is compressed and its dipole moment decreases.
When the field is opposite the dipole moment, the bond stretches and its dipole moment increases.
If this alternate stretching and compressing of the bond occurs at the frequency of the molecule's
natural rate of vibration, energy may be absorbed. The energy is absorbed by a molecule only
when there is a change in dipole moment.
[33]
The Source: Infrared energy is emitted from a glowing black-body source. This
beampasses through an aperture which controls the amount of energy presented to the
sample (and, ultimately, to the detector).
The Interferometer: The beam enters the interferometer where the “spectral encoding”
takes place. The resulting interferogram signal then exits the interferometer
[34]
The Sample: The beam enters the sample compartment where it is transmitted throughor
reflected off of the surface of the sample, depending on the type of analysis being
accomplished. This is where specific frequencies of energy, which are uniquely
characteristic of the sample, are absorbed.
The Detector: The beam finally passes to the detector for final measurement.
Thedetectors used are specially designed to measure the special interferogram signal.
The Computer: The measured signal is digitized and sent to the computer where
theFourier transformation takes place. The final infrared spectrum is then presented to the
user for interpretation and any further manipulation.
Procedure:
 Take small amount of material on a glass slide and place it on a hot plate. Ensure
the material melts and press it into a uniform film by applying steady pressure by
means of another glass plate. If material is already in film form it can be used
directly.
 Once the background scan has been completed the spectroscopy of the material is
carried out.
 Place the film sample on the Universal Attenuated Total Reflectance Cell and scan
it for background radiation.
 The interference pattern of the material is obtained which is converted by the
Fourier analyzer into a spectrum.
 The graph obtained is of % transmittance v/s wave number.
[35]
(A typical FTIR spectrum)
NOTE: WE NEED TO DO BLANK FTIR FOR THE DETECTON OF NOISE
PRODUCED DUE TOAIR (BACKGROUND DISTURBANCES) BEFORE
PERFORMING FTIR FOR THE CHEMICAL COMPOUND. LATER, AREA OF
THE PEAKS DUE TO NOISE IS SUBSTRACTED WITH THE RESULT TO FIND
OUT THE DISTURBANCES DUE TO SAMPLEONLY.
[36]
DIFFERENTIALMECHANICAL ANALYSIS
REFERENCE: ASTM D-5279/D-4065
SCOPE: Studying viscoelastic behavior of polymers , glass transition temperature.
SUMMARY: a sinusoidal stress is applied and the strain in the material is measured
allowingone to determine the complex modulus.The temperature of the sample or the
frequency of the stress are often varied , leading to variations in the complex modulus.
NOTE: IT IS 10 TO 100 TIMES MORE SENSITIVE THAN DSC FOR THE
MEASUREMENT OF GLASS TRANSITION TEMPERATURE. IT ALSO
MEASURES STIFFNESS AND DAMPING REPORTED AS MODULUS AND TAN
DELTA RESPECTIVELY.
THEORY:
Polymers composed of long molecular chains have unique viscoelastic properties, which
combine the characteristics of elastic solids and Newtonian fluids. The classical theory of
elasticity describes the mechanical properties of elastic solid where stress is proportional to
strain in small deformations. Such response of stress is independent of strain rate. The
classical theory of hydrodynamics describes the properties of viscous fluid, for which the
response of stress is dependent on strain rate. This solidlike and liquidlike behavior of
polymer can be modeled mechanically with combinations of springs and dashpots
[37]
INSTRUMENTATION:
The instrumentation of a DMA consists of a displacement sensor such as a linear variable
differential transformer, which measures a change in voltage as a result of the instrument
probe moving through a magnetic core, a temperature control system or furnace, a drive
motor (a linear motor for probe loading which provides load for the applied force), a drive
shaft support and guidance system to act as a guide for the force from the motor to the
sample, and sample clamps in order to hold the sample being tested. Depending on what is
being measured, samples will be prepared and handled differently.
Temp range : -190 to 400 °C
Sample size maximum: 52.5(mm)* 12.8(mm)* 8 (mm)
APPLICATION:
One important application of DMA is measurement of the glass transition temperature of
polymers. Amorphous polymers have different glass transition temperatures, above which
the material will have rubbery properties instead of glassy behavior and the stiffness of the
material will drop dramatically with an increase in viscosity. At the glass transition, the
storage modulus decreases dramatically and the loss modulus reaches a maximum.
[38]
Temperature sweep:
A common test method involves measuring the complex modulus at low constant
frequency while varying the sample temperature. A prominent peak in appears at the glass
transition temperature of the polymer. Secondary transitions can also be observed, which
can be attributed to the temperature-dependent activation of a wide variety of chain
motions. In semi-crystalline polymers, separate transitions can be observed for the
crystalline and amorphous sections. Similarly, multiple transitions are often found in
polymer blends.
For instance, blends of polycarbonate and poly(acrylonitrile-butadiene-styrene) were
studied with the intention of developing a polycarbonate-based material without
polycarbonate’s tendency towards brittle failure. Temperature-sweeping DMA of the
blends showed two strong transitions coincident with the glass transition temperatures of
PC and PABS, consistent with the finding that the two polymers were immiscible.
Figure shows Storage modulus and loss modulus against Temperature were
plotted.
[39]
Determination of Density
Reference: ASTM D792
Scope: This test is used to measure the density of solid samples.
Principle: Archimedes Principle
Apparatus:
Weighing Balance (METTLER )
Density meter assembly: Beaker stand, Beaker (500mL), a frame attached to the
weighing pan and a sample holder which facilitates weight in air and in liquid.
Chemicals Used: 1. n-butyl acetate
2.DM Water
[40]
NOTE: BUTYL ACETATE IS USED IN PLACE OF WATER BECAUSE IT HAS
DENSITY OF 0.88 g/L AT ROOM TEMPERATURE. SINCE IT IS NECESSARY
FOR POLYMER TO SINK IN IT FOR DENSITY DETERMINATION AND ALL
POLYMERS HAVE DENSITY GREATER THAN 0.88 g/L, BUTYL ACETATE IS
IDEAL FOR THIS USE.
Sample Specification:1 cm x 1 cm smoothly cut sample is used for densitydetermination.
The sample shouldnot have any sharp edges.
Procedure:
The weight of the sample was measured in air and then in a liquid (n-butyl acetate) of
known density. The density of the liquid used was less than the expected density of the
sample. The ratio of weight in air to loss of weight in liquid was used to calculate the
density of the sample.
Calculation:
Density of sample at Tm =
Wa
ρs
Wa̵ Ws
Where:
Tm = Temperature of measurement
Wa = Weight in air
Ws = Weight in the liquid
ρs = Density of the liquid at Tm
[41]
Determination of Tear Strength of films
Reference: ASTM D1938
Machine Make: CEAST Italy
Scope: Used to measure the tear strength of plastic films.
Summary: To force to propagate a tear across a film or sheeting specimen is
measured using a constant rate of grip separation machine.The force necessary to
propagate the tear is interpreted from the load time chart.
Principle:
The force to propagate a tear across a film or sheeting specimen is measured. The force
necessary to propagate the tear is measured.
Apparatus: CEAST ED 30 machine, Digital micrometer
Sample Specification:
The specimens shall be of the single tear type and shall consist of strips 76 mm long by 64
mm wide. The thickness of the specimen is noted along the path where tear will occur. The
samples are cut in the machine direction (MD) and the transverse direction (TD).
Procedure: Different weights available are 4000mN, 8000mN, 16000mN,
32000mN,64000mN, 50N, 100N. The weight is selected such that the film reading lies
between 20-90% of the weight. The blank reading is taken and the machine is calibrated.
The sample is inserted in the pneumatic sample holder. The cover is shut and the film
tears. The reading is noted from the display.
Calculation: Tear Strength (in g/µm) = Force in cN / thickness (µm)
[42]
NOTE: TEAR STRENGTH IN MACHINE DIRECTION IS ALWAYS LESS THAN
TRANSVERSE DIRECTION BECAUSE MOLECULES ARE ALIGNED IN
MACHINE DIRECTION. SO IT IS EASIER TO SEPARATE DIFFERENT
CHAINS (M.D) THAN TO BREAK BONDS OF CHAINS (T.D).
Determination of Coefficient of friction of Plastic
Films
Reference: ASTM D1894
Machine Make: Davenport
Scope: Used to find coefficient of friction between a plastic film with respect to
otherfilms and metal surfaces.
Summary: Two surfaces are made to slide against each other and the force required for
this is measured.
Principle:
Frictional force f is related to the normal force acting on a body at rest as follows: f=µN,
where µ is the coefficient of friction. The COF associated with the force required to start a
body from rest is known as coefficient of static friction and that associated with a moving
body is known as the coefficient of kinetic friction.
Apparatus: Davenport friction measuring apparatus, template, vacuum pump
Sample Specification: 675 mm x 255 mm should be attached to the testing plane and
6.5mm x 6.5 mm minimum for sliding.
[43]
Analytical Procedure:
The vacuum is switched on and the film is placed on the plane, without wrinkles. The film
is attached to the 200g sled with cellophane tape taking care to avoid wrinkles. The cord is
attached to the sled and placed gently on the plane at two fixed points parallel to the
machine direction. The speed is selected to be 15 cm/min. There should be no tension in
the cord and both the force meter displays are zero. The first reading as soon as the cord
pulls the slab is the static friction. The reset button is then pressed to get the value of the
kinetic friction.
Calculation:
COSF = Static force/ weight of the sled=SF/20
COKF = Kinetic force/ weight of the sled=KF/20
NOTE: IT IS EASIER TO BREAK IN MACHINE DIRECTION THAN IN
TRANSVERSE DIRECTION.
Determination of Dart Impact Strength for Plastic Films
[44]
Reference: ASTM D1709
Apparatus: Dart Impact Testing apparatus (International Engineering Industries), Weights
Scope: Used to measure the dart impact strength of plastic films
Summary: Darts of various weights are made to fall on a clamped film and the weight at
which 50% of the samples fail is measured.
Sample Specification: Greater than the diameter of the specimen holder
Principle:
Dart Impact strength values are very important for plastics packaging. They theoretically
give the impact strength of the plastic film. In the test, falling weights from a specified
height are made to fall on the film until fracture occurs. The weight at which 50% of the
samples fail is the dart impact weight value. This value divided by thickness in microns
gives dart impact strength.
Analytical Procedure:
The two different types of dart used are:
A.38.1 ± 0.13 mm of 55g weight
B.50.8 ± 0.13 mm of 283g weight Vacuum applied is 700 mm of Hg
A. Dropped from 66 cm and is used for films requiring masses of about 50g to 2 kg to
fracture
B. Dropped from 152 cm and used for films requiring masses of 0.3 to 2 kg to fracture
10 samples are tested on each weight level and the weight at which 50% failure occurs is
reported.
[45]
Calculation:
Dart Impact Strength (g/µm) = Weight to cause 50% fracture (g)/ thickness (µm)
Determination of Tensile Properties of Plastic Films
Reference: ASTM D882
Machine make:Lloyd, LRX plus
Scope:This test method covers the determination of tensile properties of plastics in the
form of thin sheeting, including film (less than 1.0 mm (0.04 in.) in thickness).
Sample specifications: The width of the sample should be 15 mm - 25 mm and the
gaugelength should be 5 cm.
SPEED OF CROSSHEAD : 500mm/min
Principle:
Plastic products when subjected to tensile force initially resist deformation, get elongated
and finally break. Tensile elongation and tensile modulus measurements are amongst the
most important indications of strength in a material and are the most widely specified
[46]
properties of the plastic materials. Tensile test, in a broad sense, is a measurement of the
ability of the material to withstand forces that tend to pull it apart and to determine to what
extent the material stretches before breaking. Tensile modulus, an indication of the relative
stiffness of a material can be determined from a stress-strain diagram.
Procedure:
The film is cut in exact dimensions making sure that the sides are uniform. The sample is
clamped carefully and the thickness of the film is measured using a digital micrometer.
The dimensions and batch references are entered in the software. The initial load is tare
and the speed of testing is set to 500 mm/min and the machine is started. The stress vs.
extension curve of the specimen is recorded and the required values are taken.
NOTE: TENSILE STRENGTH IN MACHINE DIRECTION IS ALWAYS MORE
THAN IN TRANSVERSE DIRECTION BECAUSE MOLECULES ARE ALIGNED
IN MACHINE DIRECTION. SO IT IS DIFFICULT TO BREAK BONDS OF
CHAINS (IN M.D) THAN TO SEPARATE DIFFERENT CHAINS (IN T.D)
Haze Test
Reference: ASTM D 1003
[47]
Scope: This test is used to measure the haze (% Transmittance) of plastic films and sheets
Principle: The haze is determined by percentage of light scattered from the product.
The haze of the specimen is the percentage of transmitted light which is passing through
the specimen deviates from the incident beam by forward scattering.For the purpose of this
method only light flux deviating more than 2.5’ on the average is considered to be haze
The haze can be inherent in the material,a result of the moldingprocess,or a result of
surface texture.
Haze can also be a result of environmental factors such as weathering or surface abrasion.
Sample: Size suitable to cover the port.
Procedure:
 The instrument is calibrated before haze measurement in the Total Transmittance
Mode
 The mode “large area view “ and “UV filter out” are selected
 The blank reflectance trap is placed against the receptor lens and the machine is
allowed to read.
 The white tile is placed in the reflectance port and the transmittance compartment
is kept away.
 The sample holder is placed against the sphere and the machine is allowed to read.
Instrument is now ready for haze measurement.
[48]
TESTING FOR MOLDED SAMPLES
Determination of Tensile Properties of Molded Plastics
Reference: ASTM D638
Scope: This test is used to determine the tensile properties of molded polymer samples.
Summary: Standard molded specimens were exposed to tension and force required to
elongate and break the specimen of elongation were observed.
Principle:
Plastic products when subjected to tensile force initially resist deformation, get elongated
and then finally break. Tensile elongation and tensile modulus measurements are among
the most important indications of strength in a material and are most widely specified
properties of plastic materials. Tensile test in a broad sense is a measurement of the ability
of a material to withstand forces that tend to pull it apart and to determine to what extent
the material stretches before breaking. Tensile modulus, an indication of the relative
stiffness of a material can be determined from a stress-strain diagram.
[49]
Apparatus:
(i) Universal Testing Machine
(ii) Grips for mounting the specimen
(iii) VernierCalipers
Sample Specification: Five specimens are tested as per the following specifications:
Sample PE PP
Sample Type ASTM D638 Type IV Type I
Grip separation rate 50mm/min 50 mm/min
Distance between the grips 64 ± 5 mm 114 ± 1 mm
Procedure:
The testing machine is switched on and the program for determining the tensile properties
is selected. Test samples, previously conditioned are used for testing. Two marks, 1.0,0.1
inches apart are on all the test samples at the center of the narrow portion of the sample.
The width and thickness of the sample is measured to the nearest 0.001 mm and entered as
data. The specimen is placed in the grips of the testing machine and the grips are tightened.
The extensometer is then attached on the marks made on the sample. The initial load is
tare. The speed of the testing machine is set and the machine is started. The load vs.
extension curve of the specimen is recorded and the load and extension at the yield point
and the point of rupture are noted. Tensile strength at yield (TYS), UTS, % elongation at
break and % elongation at yield were directly displayed on the screen.
[50]
Calculations:
Tensile modulus was calculated from the points on the stress-strain curve
Tensile Modulus = Difference in stress/difference in corresponding
Strain Tensile strength= force/ area
Determination of Izod-Impact Strength of
Plastics
[51]
Reference: ASTM D256
Machine Make: ResilImpactor
Scope: This procedure is used to determine the impact strength of molded
polymersamples.
Summary: Notched specimens were subjected to impact with the help of a
strikingpendulum hammer. Energy required for the sample to break was noted.
Principle:
Impact test indicates the energy required to break standard test specimens of a specified
size. Energy lost by the pendulum during the breaking of the specimen was noted.
The objective of the Izod Impact test is to measure the relative susceptibility of a standard
test specimen to the pendulum-type impact load. The results are expressed in terms of
energy consumed by the pendulum in order to break the specimen. The energy required to
break a standard specimen is actually the sum of the energies needed to deform it, to
initiate its fracture and to propagate the fracture across it, and the energy needed to throw
the broken ends of the specimen.
Apparatus:
 Izod Impact Tester- CEAST (Resil-25)
 Notch cutter with micrometer-screw gauge
 Vernier Calipers- Accuracy 0.01 mm
[52]
Notchcutter
Sample specification: Molded specimens have width between 3.17 and 12.7 mm.
Thedepth of the plastic material remaining in the bar under the notch was 10.16 ± 0.05 mm
and the distance of the notch from the end was between 31.5 to 32 mm.
Analytical Procedure:
1. Hammer was selected along with the relevant range and installed by means of
the range selector and the range switch.
2. The hammer was manually checked so as to ensure that it could be swung freely
between the anvils.
[53]
3. The hammer was initially released without the specimen and the value
displayed indicated the amount of energy lost due to friction, wind age, and
other factors.
4. This value was subtracted from each of the final sample readings.
5. The hammer was positioned on the anvil and the test samples (conditioned for 40
hours at 23±2 °C) were positioned and tightened with the torque wrench.
6. The hammer was then released and the breaking energy value on the digital
display was noted down.
7. If the display exceeded 70% of the 2.75 J, then the hammer was replaced by a
higher energy hammer and the above steps were repeated again.
Calculation:
Izod Impact Energy required to break the specimen – Air resistance
Energy = Thickness
Shrinkage Test
Reference: ASTM D6289
Scope: This test method is intended to measure shrinkage from mold cavity to
moldeddimensions of thermosetting plastics when molded by compression, injection, or
transfer under specified conditions
Principle:
Plastic products have a tendency of shrinking when they once they are cooled down in the
mold. This happens as the polymer coming from extruder is highly stressed and upon
cooling the polymeric chains relieve their stress by orienting themselves randomly. This
random orientation leads to shrinkage of polymer. The shrinkage is more in case of
crystalline polymers as compared to amorphous polymers due to closer packing of chains.
[54]
Apparatus:
(i) VernierCalipers
Sample Specification: Standard mold dimension
Procedure:
 We take a standard circular molded specimen.
 The diameter of the specimen is measured.
 The diameter of the mold is measured.
 The % change is reported as shrinkage
Determination of Heat Deflection Temperature and
Vicat SofteningPoint
Reference:
HDT: ASTM D 648
Vicat Softening: ASTM D1525
[55]
Scope: This procedure is used to determine the heat deflection temperature and
Vicatsoftening point of the polymer.
Summary:
HDT of a polymer is the temperature at which a specimen deflects by 0.25 mm at a
specified stress of 455kPa or 1820kPa.
VICAT softening point is the temperature at which a flat ended needle of 1 mm2 surface
area penetrates into the sample to a depth of 1 mm under 1 kg or 5 kg load.
Principle:
A molded, rectangular sample is placed in a temperature-controlled bath. The temperature
of the bath is increased at a constant rate. Mechanical properties of polymers are
temperature dependent.
Both HDT and VST have their own purposes i.e. when the softening temperature of a
polymer under stress is to be found the HDT test is used.
However, when the softening temperature of a plastic without any stress (say when it is
held by a support) is to be found VSP is used.
Apparatus:
 Specimen supports: 100 mm apart
 Immersion bath: 6-station HDT-Vicat testing machine capable of providing a
heating rate of 2±.0.2⁰C/ min. (make: CEAST)
 Deflection measurement device: Accuracy = 0.01 mm
 Weights: Set of weights to provide maximum fiber stress of 1820 kPa (264 psi) ±
2.5% or 455 kPa (66 psi) ± 2.5%
 Working thermometer
[56]
Calibration:
Working thermometer is calibrated as per standard method.
Sample: Injection molded samples of the following dimensions are employed:
Dimension Heat Distortion Temperature Vicat Softening Point
Length 110 – 130 mm 1cm
Depth 13 ± 0.13 mm 3 – 13 mm
Width 3.2 mm 10mm
(I) Heat Distortion Temperature (HDT)
The test assembly was taken out from the bath and supported with a moving support. The
test heads were fitted below the rods using the keys and the gauge block provided.
According to the specimen dimensions the weight to be applied was calculated using the
following formula:
P=2bh2σ
3L
P = weight to be applied in KN
σ = Maximum fiber stress in the specimen
b = width of the specimen in mm
h = depth of the specimen in mm
L = Support span in mm
134.2g (the combined weight of the testing head, loading rod assembly, dial gauge and
cylindrical support fixed by the grub screw) were subtracted from the calculated weight
and then this weight was made up with the auxiliary weights provided. The Bakelite nut
[57]
was loosened and the indicator was moved sideways. The weights were placed on the load
rod and the indicator was returned to its original position and the Bakelite nut was
tightened. Test samples, previously conditioned at 23±2 ⁰C for 48 hours were placed on
the round supports. The loading unit was lowered by rotating the lever so that the HDT
head rested on the specimen. Springs were inserted to avoid the specimen from dropping
into the tank. The test assembly was then lowered by removing the moving support.
The test start preset was subsequently adjusted to 23-25⁰C and the test end preset to a
temperature 10-15⁰C higher than the expected HDT of the sample. The main switch was
switched in and the heater switched on about 30 seconds later. The zero was adjusted on
the indicator by loosening the block ring, after the heater switch started blinking (allowing
5 minutes as thermo station time) and the regulator screw was rotated such that the LED of
the corresponding station was switched off. The heating was then started. When the
required deflection was reached the instrument read the recorded value.
Sample orientation in HDT
[58]
(ii) VICAT softening Point (VSP)
The procedure was same as that of HDT except for the following:
The Vicat test heads were fitted instead of the HDT heads. The weight was place on the
Vicat head assembly totally amounting to 1000g (including the weight of the assembly i.e.
134.3g). The preset was testing started, set at least 50± 2 °C lower than the expected VSP
of the sample. The deflection on the gauge is adjusted to 1 mm. The tester was then
started. When the deflection on the gauge reached 1 mm, the instrument recorded that
temperature as the VSP of the sample.
Sample orientation in VST
[59]
Determination of Flexural Properties of Plastics
Reference: ASTM D790
Scope: This procedure is used to determine the flexural properties of plastic materials
Summary: A sample was placed on a support span and subjected to flexural stress by a
loading nose and from the deflection data, flexural properties were determined.
Principle: Plastic Products when subjected to flexural strain resist deformation.
Flexuralstrength is the ability of the material to withstand bending forces applied
perpendicular to its longitudinal axis. The stresses induced due to the flexural load are a
combination of compressive and tensile stresses. Flexural properties are reported and
calculated in terms of the maximum stress and strain that occur at the outside surface of
the test bar. Many polymers do not break under flexure even after a large deflection that
makes determination of the ultimate flexural strength impractical for many polymers.
Apparatus:
(i) Universal Testing Machine (Lloyd)
(ii) Loading noses and supports
(iii) VernierCalipers (Mitotoyo make)
[60]
Sample specification:
Five samples of the following dimensions are tested:
Length = 127 ± 5mm
Width = 12.7 ± 1mm
Thickness = 3.2 ± 0.4 m
Support span length is 16 times the specimen thickness (Tolerance +4 or –2 mm)
Analytical Procedure:
An appropriate load cell (depending upon the type of material) is mounted on the machine.
The loading nose is attached to the load cell and the supports to the stationary crosshead.
The parallel alignment of the loading nose and supports is critical here. The machine is
switched on and the following instrumental parameters are set:
Speed of testing for the PP samples = 1.3 mm/min
The appropriate program for flexural properties is selected. Previously conditioned
(Maintained at 23 ± 2°C for 40 hours) test specimens are used. The width and thickness of
the samples being tested are entered as data and the support span is set at 50 ± 2mm for
PP. The specimen is entered on the supports. The experiment was performed and the load
deflection curve was displayed and the program gave the flexural yield strength, modulus
of elasticity, and 1% secant modulus directly.
Calculation:
Eb=L3F/ (4bh3Y)
σf =3FL/ (2bh2)
F: Force @ midpoint
L: Span
b: Width
h: Thickness
[61]
Measurementof Colour of Plastics
Reference: ASTM E313
Machine make: Color quest II, Hunterlab
Scope: This test is used to measure the L*, a*, b* values of the given sample and also
theYellowness Index, Whiteness Index, and color differences between the standard and
sample.
Sample specifications: Typically a 50 mm (2") or 100 mm (4") disk, although any
flatsample that the specimen holder will grasp can be tested.
Procedure:
 The instrument is first standardized for color measurements and the instructions in
the computer are followed to get the required values.
 L* indicates brightness,
 a* indicated greenness or redness,
 b* indicates blueness or yellowness.
 ΔE= ((∆L* )2 + (∆b* )2 + (∆a* )2 )
 Standardization includes selection of specular reflectance mode with large area of
view and UV filter out.
[62]
 The standard light trap is then inserted followed by the standard white and the
standard gray tiles.
 The test sample is inserted into the specimen holder, and the spectrophotometer
takes the reading
 The result obtained is in the form of L, a, b values, whiteness index (WI) and
yellowness index (YI).
Color analysis can be used to match adjacent parts molded from different materials, or to
evaluate color change due to outdoor exposure. Visual color and Spectrophotometer
readings can also be affected by surface texture, molding parameters, processing method,
and viewing light sources.
Gardener Impact Test
Reference: ASTM D5420
[63]
Scope: This method covers the determination of the relative ranking of materialsaccording
to the energy required to crack or break flat, rigid plastic specimens under various
specified conditions of impact of a striker impacted by a falling weight.
Summary: The procedure determine the energy (mass*gravity*height) that will cause50%
of the specimens tested to fail called as mean failure energy (MFE). For low temperature
cryo-test air chamber, condition the specimen for minimum 3 hours, once the required sub-
zero temperature is reached, carry out the test accordingly.
Principle: Energy of the falling weight at the instant of impact is kinetic energy which
isequal to the energy used to raise the weight to the height of the drop. It is the potential
energy possessed by the weight the instant it is released. Since the potential energy is (m x
g x h), the guide tube can be marked with a liner scale showing the impact range of the
instrument. Purpose of the impact testing is to find the amount of energy necessary to
cause failure of specimen and to establish a standard for impact resistance, and test
samples of the product against the established standard. Nature and extent of impact
damage that constitutes failure must be established, variables such as material thickness,
specimen shape, end use of the product are factors for evaluation. Once the failure point
has defined, the actual test program can be developed (i.e. number of specimens to be
impacted and what energy to use with each impact.
Apparatus: Gardner impact tester consist of a Cast Al base, a slotted vertical guide
tube,round nosed punch(up) and punch holder, 8 – lb. weight (3.6kgs), die and die support
(anvil) and a cryo-test air chamber (low temperature) a separate attachment.
Nose of the punch: - 0.600” (1.37cm) dia.;
Inside diameterof the die: - 0.640” (1.64cm);
Height of the guide tube: - 40” (101.6cm);
Scale graduation: - 0 to 320inch-pound
Specimen size: - Diameter = 100mm, Thickness = 3.2mm
[64]
Procedure:
 Determine the number of specimens for each sample to be tested.
 Place the test specimen on the tester anvil, after raising the weight and striker foot.
 Be sure the specimen is flat against the specimen support plate before the striker
foot is brought in contact with the top surface of the specimen.
 Raise the weight in the tube to the desired impact value as shown on the scale, and
release it so that the weight drops on the striker.
 Remove the specimen and examine it to determine whether or not it has failed.
 Permanent deformations alone are not considered failure, but note the extent of
deformation (depth, area).
In the first specimen fails, decrease the drop height while keeping the mass constant. If the
first specimen does not fail, increase the drop height one increment and then testthe second
specimen.
In this manner, select the impact height for each test from the results observed with the
specimen just previously tested. Test each specimen only once.
[65]
Environmental Stress Cracking Resistance (ESCR)
Reference: ASTM D 1693
Scope: This procedure is used to determine the resistance of materials to cracking , when
in contact with certain reagents and under mechanical stress.
Summary: A set of specimens with controlled imperfections is immersed in a reactive
liquid maintained at specified temperature . Time required for 50% of the specimens to fail
is noted.
Principle: Polymers when exposed to certain chemicals show physical failure at
mechanical stresses that are much less than expected . ESCR quantifies resistance to such
type of failure.
Apparatus:
1. A jig for making a controlled imperfection in specimen of the dimensions,parallel to
long edges of specimen and centered on one of the broad faces.
2. Specimen Holders
3. Test Tubes
4. Corks wrapped withaluminium foil.
5. Constant temperature bath maintained at 50±0.5⁰C
6. Bending clamp and transfer tool.
7. Thermometer.
[66]
Sample: Ten samples of following dimensions shall be cut from an Injection Molded or
Compression Molded sheet; 38±2.5mm×13±0.08mm×3.15±0.15mm
Procedure:
 Give each specimen a controlled imperfection (notch) of 0.575±0.075mm depth on
one surface after conditioning the test samples for 24 hours at 23⁰C before testing.
 Bend the specimen using bending tool.Make sure that the notch is on the outer side.
Transfer them to the specimen holder.
 Insert holder in the test tube. Fill the tube with fresh reagent. Stopper the tube with
foil wrapped cork and immediately place it in the constant temperature bath.
 Temperature of water bath checked and set to 50⁰C with thermometer before
starting the test.
 Note the time required for 50% of the samples fail.
Specular Gloss of Plastic Products
Reference: ASTM D 523
Scope: This procedure is used to measure the specular gloss of plastics
[67]
Summary: The gloss meter is placed on the sample and the program for gloss
measurement is run.
Principle: Gloss value is determined from the ratio of incident light reflected from the
surface of the sample.
Apparatus: 3 Angle Hunter labsProgloss
Sample:PE , PP & PVC
Procedure:
1. The mode switch is first set for set up mode to prepare instrument for operation.
Select all three angles for measurements (20⁰,60⁰&85⁰).
2. Place the film samples on a vacuum activated surface with a perfectly white
background.
3. Then place the instrument on the sample.
4. Press the red key.
5. The gloss values are displayed on the instrument.
Indentation Hardness of Plastics
Reference:ASTM D 2240
[68]
Scope: This procedure is used to determine the Indentation Hardness of plastic
materials.
Summary:Needle tip of specified dimensions and geometry is made to penetrate into
the polymer and the depth of penetration gives the level of the hardness of the material.
Principle:Resistance to Indentation of the material is found with the help of a hard
needle tip.
Apparatus:Shore D Hardness tester – Blue steel make.
Sample:The specimen shall be at least 6 mm thick. Two or more samples of lesser
thickness can be plied up to achieve the desired thickness.
Procedure:
1. Place the specimen on hard, even and horizontal surface.
2. Hold the tester vertically on the specimen. While holding, the pressure foot should
be parallel to the surface of the specimen.
3. Apply the pressure with hand without shock so that the casing is fully pressed
against the specimen.
4. The readings are to be taken after about 3seconds after the contact between the
surface of the specimen and the pressure foot is made.
5. Three tests should be carried out on each specimen and the mean value of these 3
readings should be rounded off to a shore number.
[69]
6. PROCESSING DIVISION
Various Processing Facilities at PARC
MOLDING
 Injection Molding Machines
 Blow Molding Machine
 Compression Molding Machine
 Rotational Molding Machine
EXTRUSION
 Blown Film Extrusion Plant
 Tubular Quenched PP Plant
 PVC Pipe Extrusion Plant
COMPOUNDING
 Single screw compounding extruder
 Twin screw compounding extruder
 Tumbler Mixer
 High speed mixer
 Granulator
 Pulverizing Unit
[70]
Brief Descriptionof Processing Machines:
1.InjectionMolding
Principle:
 In the process the material is plasticized and melted by the heat added through
barrel heaters and friction due to shearing.
 Then the material is injected through nozzle into a relatively cold mold to get the
desired shape.
 After the shape is formed, the ejector pins push the specimen out of the mold.
 The process is used to make solid articles like caps, plugs, bobbins, furniture&
house ware products, industrial & automobile parts etc.
[71]
Machines available:
Klockner Windsor FR 110
Klockner Windsor SP 180 (Family mold machine)
Arburg 320C All-rounder (ASTM standards)
Parts of a molded specimen:
[72]
Injection molding machine detailed specification
Specifications Units DGP Klockner Arburg
Windsor Windsor All rounder
SP180 FR110 320 C 500-100
Screw diameter mm 50 45 30
Injection pressure Bar 1800 1900 1550
L/D - 18:1 19:1 20:1
Clamping force KN 1800 1100 500
Min mold height mm 350 250 200
Max mold height mm 900 700 200
The theory of injection molding can be reduced to four simple individual steps:
Plasticizing, Injection, Cooling, and Ejection. Each of those steps is distinct from
theothers and correct control of each is essential to success of the total process.
The steps are as follows:
 Plasticizing - describes the conversion of the polymer material from its
normal hard granular form at room temperatures, to the melt necessary for
injection at its correct melt temperature.
 Injection - is the stage during which this melt is introduced into a mold to
completely fill a cavity or cavities.
 Cooling - is the action of removing heat from the melt to convert it from
melt back to its original rigid state. As the material cools, it also shrinks.
 Ejection - is the removal of the cooled, molded part from the mold cavity
and from any cores or inserts.
[73]
Advantages of Injection Molding
 High Production rates
 Design flexibility
 Repeatability within tolerances
 Can process a wide range of materials
 Relatively low labor
 Very good finishing of parts
 Minimum scrap losses
Limitations of Injection Molding
 High initial equipment investment
 High start-up and running costs possible
 Part must be designed for effective molding
 Accurate cost prediction for molding job is difficult
Application: PARC uses injection molding machine for manufacturing of spiral flow
testsample, tensile testing sample, flexural testing sample, Izod testing sample, disc shape
sample and color testing sample
[74]
2.Blown Film Plant
Blown film extrusion process and salient features:
The majority of polymer films are manufactured by film blowing.Plastic melt is
extruded through an annular slit die, usually vertically, to form a thin walled tube.
Air is introduced via a hole in the centre of the die to blow up the tube like a
balloon. Mounted on top of the die, a high-speed air ring blows onto the hot film to
cool it. The tube of film then continues upwards, continually cooling, until it passes
through nip rolls where the tube is flattened to create what is known as a ' lay-flat'
tube of film. This lay-flat or collapsed tube is then taken back down the extrusion '
tower' via more rollers. On higher output lines, the air inside the bubble is also
exchanged. This is known as IBS (Internal Bubble Cooling).
The lay-flat film is then either kept as such or the edges of the lay-flat are slit off to
produce two flat film sheets and wound up onto reels. If kept as lay-flat, the tube of
film is made into bags by sealing across the width of film and cutting or perforating
to make each bag. This is done either in line with the blown film process or at a
later stage.
Typically, the expansion ratio between die and blown tube of film would be 1.5 to
4 times the die diameter. The drawdown between the melt wall thickness and the
cooled film thickness occurs in both radial and longitudinal directions and is easily
controlled by changing the volume of air inside the bubble and by altering the haul
off speed. This gives blown film a better balance of properties than traditional cast
or extruded film which is drawn down along the extrusion direction only
Tubular films show excellent toughness as they are a mild form of biaxial
orientation. Tubular lines produce products which can be easily made in to bags,
edge-trimming can be frequently avoided and a film width is easily changed simply
by blowing a bigger tube.
[75]
Machine Specifications:
LDPE/LLDPE plant HM/HDPE plant
Make Rajoo Engineers Limited Rajoo Engineers Limited
Model No RELL-4040 LAB REHD-4040 LAB
Screw diameter 40mm 40mm
Screw length 1200mm 1200mm
L/D ratio 30:1 30:1
Screw speed range 10-100rpm 10-100rpm
Die diameter 110mm spiral type 75mm spiral type
Die gap 1.2, 1.5,1.8mm 0.8,1.2mm
Parts of a tubular blown film plant:
 Extruder
Extruder comprisesof hopper, barrel/screw and dies. Fig shows the component of a
modernextruder.
[76]
 Hopper:
All the extruder has an opening in the barrel at the driven end, through which the plastic
graduals enter the extruder. The hopper, a simple sheet –metal enclosure, is mounted
above the opening and holds about a hopper’s capacity material. Hopper is provided with
heating system, if the material has to be preheated before entering the extruder.
 Screw:
This is the heart of the extruder. Screw conveys the molten polymer to the opening of the
die after properly homogenizing the molten polymer.
There is considerable variation in the design of the screw for various materials, the most
important variable being the depth of the channels. Despite much desire for universal
screw, it is advisable to use a different design for each material to achieve the best results.
PE screw is designed to have shallow channels, sudden compression and long metering
join.
Screw diameter: 20-250mm,CR: 2.5-3: 1,L/D: 24-33: 1
 Mixing Heads
The metering section of a standard is not a good mixer. Smooth laminar flow patterns are
established in the channel, which do not mix dissimilar elements in the melt. Mixing
devices are frequently installed in screw to disrupt these flow patterns and improve melt
homogenization.
 Breaker plate/screen pack:
[77]
Breaker plate with screen packs inserted is kept in the adapter, which connect the dies and
extruder barrel. This assembly has several functions.
1. Arrest the rotational flow of the melt and convert into axial flow.
2. Improves melt homogeneity by splitting and recombining the flow.
3. Improves mixing by increasing backpressure.
4. Remove any contamination and unmelt.
Screen packs are made up of series of screen of differing mesh. With the coarse screen
placed against the breaker plate to support the finer screens.
 Die:
The dies used for tubular extrusion are centre-fed or side-fed. Centre fed dies are better as
all the points on the lip are equidistant from the feed-entry point. This gives uniform flow
and uniform thickness. The spider arms of the centre-fed die always divide the flow into
separate paths which must come together and weld completely before leaving the die or
else weld lines are formed, which are lines of weakness.
Die gap is also a very important parameter as too small die gap may cause increase in die
resistance and cause overheating in extruder and reduce output rate. And if the gap is too
large resistance becomes so less that weld lines may appear.
For the processing of PE, a die with spiral is used as shown in the figure. As the plastic
flows from the entry point it spirals around the mandrel section of the die. The land depth
between the spiral section and wall increases as the wall increases as the material progress
through the die, .as a result, the distribution around the die periphery made uniform in
order to control the gauge of extruded tube.
[78]
 Corona treatment:
Many plastics, such as polyethylene and polypropylene, have chemically inert and
nonporous surfaces with low surface tensions causing them to be non-receptive to bonding
with printing inks, coatings, and adhesives. Although results are invisible to the naked eye,
surface treating modifies surfaces to improve adhesion.
Corona treatment (sometimes referred to as air plasma) is a surface modification technique
that uses a low temperature corona discharge plasma to impart changes in the properties of
a surface. The corona plasma is generated by the application of high voltage to sharp
electrode tips which forms plasma at the ends of the sharp tips. A linear array of electrodes
is often used to create a curtain of corona plasma.
Parameterof blown film extrusion:
 Temperature:
A lower temperature is needed for tubular film (e.g., 170oC for PE of 2.0 MFI) since the
cooling capacity often limits the output as a higher temperature may mean lower output.
The other possible disadvantages of higher temperature are:
Increased blocking
Reduced bubble stability
Promotion of decomposition in the die with resultant impaired appearance
Possible bubble breaks.
 Blow up Ratio:
The blow-up ratio is defined as the ratio of the bubble diameter to the die diameter and is
one of the important factors to determine the final film size and properties. A high blow
ratio means that a smaller and less expensive die is needed for any given film size, but a
high blow-up ratio yields the strongest film as the increased stretching has an orientation
effect. However, high blow-up ratio also encourages bubble instability, requires more
drawdown and magnifies all the imperfections in the die, thus a compromise blow-up ratio
is needed. Bubble instability is a major problem in tubular film extrusion as it produces
wrinkles, thickness variation, and “walking” of the film along the windup roll.
[79]
The blow-up ratio is determined in advance, when a die is selected to do a given job. Die
gap also has significant effect on the film properties. Increasing die gap will increase
machine direction orientation which then results in lower machine direction tear strength,
lower machine elongation, improved transverse direction tear strength, & improved
machine direction tensile strength.
 Frost-Line Height:
The area of change, where the viscous fluid is changed to solid film, is called the "frost-
line" because here the hardening film first appears "frosty" in some films. An irregularity
here indicates that something is wrong with the filmmaking process, and this may result in
poor film.
Increasing FLH will decrease machine direction orientation with slower quenching rates
resulting in higher film crystallanity. Optical properties will reach an optimum & then start
to decrease.
The frost line can be raised or lowered by means of extruder output, take-off speed, and
the volume of cooling air blown against the bubble. When the screw speed goes up the
distance between the die and the frost line is increased; when more cooling air is blown
against the bubble, the frost line drops. The frost line can be change by adjusting the
cooling-air volume. The frost line in the bubble can effectively be raised by means of a so-
called annealing chamber (or "chimney") placed between the die and the air ring.
[80]
Start-up & shutdown of the process:
The first minutes of the production always yield scrap material as the system much yield
equilibrium. The die bolts may have to adjust to get the uniform thickness, and the
extrusion speed and the winder speeds must be balanced to get the desired overall
thickness. The process is started quite cool in order to minimize formation of decomposed
material in the system, which could subsequently contaminate the film and cause streaks.
Once the screw is turning and plastic is running through the die, the temperatures are raise
to normal values. As the tube is being formed, air is introduced through the die in small
amounts to keep the tube slightly blown. After the threading is complete, more air is blown
in to bring the bubble to the desired size. Care must be taken to keep the die faces clear of
the molten resin as this may later be decomposed and cause die lines.
Shut down is one of the most vital steps in blown film extrusion in order to avoid damageto
the head and the die. Such decomposition can be caused by the degradation, oxidation of hot
plastic in contact with air, or by both. For all materials degradation and decomposition may
produce hardened bits of material which can break off and lodge in the die lips. Such bits form
weld lines which are not only unsightly but are also lines of weakness.
When the film line is shut down, material is kept moving as the zones cool to about 130oC
(LDPE) then the extruder is stopped and the die and head are cooled with air as fast as
possible to inhibit decomposition. Polyethylene is often left in the extruder barrel as well
as inside the die to prevent air from entering the system and oxidizing any bits of plastic
left. Likewise, before start-up the die is not left hot any longer than absolutely necessary.
 Winding:
Winding is the final operation in the film manufacturing process. In blown film, because
there are two sides of the tube, two winders are requires. Film is wound on a spiral wound
paper core which is supported by the winding shaft. This shaft is attached to the winder at
the ends. The core is secured to the shaft using either a cable lock mechanisms or lugs
which are pneumatically protruded from the shaft surface.
Two basics techniques used for winding films are: driving the winding roll from
thecentre using a driven wind up shaft, or applying a driven roll directly to the
surface of the winding roll of the film.
[81]
Centre winders: Centre winders have the advantage in that the tension in the film can
becontrolled as the diameter of the film increases. This is done by sensing the diameter of
the film & decreasing the tension of the film as the diameter of the film increases. Tension
is controlled by controlling the differences in speed between the nip rolls & the winding
rolls Tension can also be controlled by a pneumatically activated idler roll that applies
pressure on the film web. This roll is called the dancer since it pivots up& down as it
maintains the constant pressure in the web. With the higher force required to move the
dancer roll, more tension will be applied to the film. Decreasing the tension as the roll
diameter grows up, helps to keep the film roll form winding too tight. Tight winding will
cause the film to block & make it sensitive to shrink as it cools on the toll. If winding is
too tight, the shrinking film will become distorted & difficult to print or laminate.
Surface winders: Surface windersare easy to operate since they don’t have the
complexmethods of tension control. In case of surface winders, tension is applied to the
film by winding the film faster than the nip rolls. However, this does not allow for the
finer adjustments in tension as in a dancer-bar arrangement. Surface winders rely on the
pressure of the drive roll to control the roll hardness. Therefore, because some pressure is
required to drive the roll, they tend to wind harder rolls than centre winders. However,
because there is not the variation in tension & because there is no dancer rolls, some
processors believe that surface winders can wind flatter rolls than centre winders. It is
difficult, however, to change the direction of the wind on a surface winder compared to the
centre winder.
[82]
3.CompressionMolding Machine
Machine Specifications: Compression cylinder: 6 inch diameter
Make: Carver Inc. LMV 50H-15-C (50T)
Process: The process of compression molding may be simply described by reference
toFig. Two-piece mold provides a cavity in the shape of the desired molded article. The
mold is heated, and an appropriate amount of molding material is loaded into the lower
half of the mold. The two parts of the mold are brought together under pressure. The
compound, softened by heat, is thereby molded into a continuous mass having the shape of
the cavity. The mass then must be hardened, so that it can be removed without distortion
when the mold is opened.
Advantages
Advantages ofCompression Molding
 Mold costs tend to be lower because the molds are simpler.
 Low volume jobs are better suited to compression molding because start up is
usually quicker, easier and generates less scrap.
 Cycle times for compression molded is more than injection molding
[83]
Disadvantages of Compression Molding

Compression molded parts usually are more labor intensive. Preforms must be
made, heated and loaded into the mold by an operator or a robot.

Across parting line dimensions can be more difficult to control.

It can be more difficult to mold metal inserts into the parts without flashing them.
Application: PARC uses compression molding for manufacturing of
thermoplasticsheet (testing sample are punch from sheet)
NOTE: FOR PVC FOR FIRST 1 MIN IT IS OPERATED UNDER 0 BAR
PRESSURE, FOR NEXT 1 MIN IT IS 15 BAR PRESSURE AND FOR NEXT 2
MINUTES IT IS 30 BAR PRESSURE.
FOR PE, PP FOR THE FIRST 1 MINUTES IT IS 0 BAR PRESSURE, FOR NEXT 2
MINUTES IT IS 15 BAR PRESSURE AND FOR THE NEXT 3 MINUTES IT IS 30
BAR PRESSURE.
COOLING IS DONE AT 70 °C FOR PVC AND 50°C FOR PP,PE.
[84]
4.RotationalMolding
Make: Fixotron 50K2
Rotational molding (often referred to as Rotomolding or Rotomolding) is a process used
for producing hollow plastic products. By using additional post-molding operations,
complex components can be produced enabling the process to compete effectively with
other molding and extrusion practices.
Rotational molding differs from other processing methods in that the heating, melting,
shaping, and cooling stages all occur after the polymer is placed in the mold, therefore no
external pressure is applied during forming.
Advantages of RotationalMolding
 Economically produced large products
 Minimum design constraints
 Stress-free products
 No polymer weld lines
 Comparatively low mold costs
[85]
Disadvantages of Rotational Molding
 The manufacturing times are long
 The choice of molding materials is limited
 The material costs are relatively high due to the need for special additive packages
and the fact that the material must be ground to a fine powder
 Some geometrical features (such as ribs) are difficult to mold
Process:The Rotational Molding process is essentially split into four operations:
Charging Mold:A pre-determined amount of polymer powder is placed in the mold. With
the powder loaded, the mold is closed, locked and loaded into the oven. The powder can
be pre-compounded to the desired color.
Heating & Fusion:Once inside the oven, the mold is rotated around two axes, tumbling
the powder – the process is not a centrifugal one. The speed of rotation is relatively slow,
less than 20 rev/min. The ovens are heated by convection, conduction and, in some cases,
radiation. As the mold becomes hotter the powder begins to melt and stick to the inner
walls of the mold. As the powder melts, it gradually builds up an even coating over the
entire surface.
Cooling: When the melt has been consolidated to the desired level, the mold is cooled
either by air, water or a combination of both. The polymer solidifies to the desired shape.
Unloading/Demolding: When the polymer has cooled sufficiently to retain its shape and
be easily handled, the mold is opened and the product removed. At this point powder can
once again be placed in the mold and the cycle repeated.
[86]
Typical Materials Used
LDPE, LLDPE,PP,PVC
Rotation Molded Kyak
[87]
6.ExtrusionBlow Molding
Make: Klockner Windsor India Ltd, Model : KBM-5
Blow molding is a manufacturing process by which hollow plastic parts are formed.
Principle: The blow molding process begins with melting down the plastic and forming it
into a parison or in the case of injection and injection stretch blow molding (ISB) a
preform. The parison is a tube-like piece of plastic with a hole in one end through which
compressed air can pass.The parison is then clamped into a mold and air is blown into it.
The air pressure then pushes the plastic out to match the mold. Once the plastic has cooled
and hardened the mold opens up and the part is ejected.
Process: In Extrusion Blow Molding (EBM), plastic is melted and extruded into a hollow
tube (a parison). This parison is then captured by closing it into a cooled metal mold. Air is
then blown into the parison, inflating it into the shape of the hollow bottle, container, or
part. After the plastic has cooled sufficiently, the mold is opened and the part is
ejected.Continuous and Intermittent are two variations of Extrusion Blow Molding. In
Continuous Extrusion Blow Molding the parison is extruded continuously and the
individual parts are cut off by a suitable knife. In Intermittent blow molding there are two
processes: straight intermittent is similar to injection molding whereby the screw turns,
then stops and pushes the melt out. With the accumulator method, an accumulator gathers
melted plastic and when the previous mold has cooled and enough plastic has
accumulated, a rod pushes the melted plastic and forms the parison. In this case the screw
may turn continuously or intermittently.[3] with continuous extrusion the weight of the
[88]
parison drags the parison and makes calibrating the wall thickness difficult. The
accumulator head or reciprocating screw methods use hydraulic systems to push the
parison out quickly reducing the effect of the weight and allowing precise control over the
wall thickness by adjusting the die gap with a parison programming device
Advantages of extrusion blow molding
 High rate of production
 Low tooling cost
Disadvantages of extrusion blow molding
 High scrap rate
 A limited control over wall thickness
 Difficulty of trimming away excess plastic.
[89]
COMPOUNDING
1. Single screw compounding extruder:
Make: Thermo Electron Corporation
Machine Specifications:

Screw diameter: 19mm

L/D ratio: 25:1

Compression ratio- 3:1

Maximum screw speed: 200rpm
Overview: Single-screw laboratory extruder deliver reliable data captured during the extrusion
process to verify process parameters (speed, energy, temperature) for unknown materials or to
manufacture smaller quantities of a new polymer (as strands, sheets, pellets, blown films) during
research and development. The extruder is equipped with measuring ports for melt pressure and melts
temperature to study the process parameters along the extruder barrels. A die can be connected to the
end of the extruder barrel to form the polymer melt as strand or film. Special rheological dies allow
the determination of shear- and elongational viscosity at defined shear rates.. Standard feeders for
pellets and special feeding systems for powders, pastes,liquids are there.
Application: Single screw compounding extruder is use for checking the decrease
inproperties of material after no. of passes.
2.Twinscrew compounding extruder:
Type: Co-rotating twin screw extruder
Make: Omega 30 STEER
[90]
Process:In the extrusion of plastics, raw compound material in the form of nurdles (small
beads, often called resin) is gravity fed from a top mounted hopper into the barrel of the
extruder. Additives such as colorants and UV inhibitors (in either liquid or pellet form) are
often used and can be mixed into the resin prior to arriving at the hopper.
The material enters through the feed throat (an opening near the rear of the barrel) and comes
into contact with the screw. The rotating screw (normally turning at up to 120 rpm) forces
the plastic beads forward into the heated barrel. The desired extrusion temperature is rarely
equal to the set temperature of the barrel due to viscous heating and other effects. In most
processes, a heating profile is set for the barrel in which three or more independent PID-
controlled heater zones gradually increase the temperature of the barrel from the rear (where
the plastic enters) to the front. This allows the plastic beads to melt gradually as they are
pushed through the barrel and lowers the risk of overheating which may cause degradation in
the polymer.
Extra heat is contributed by the intense pressure and friction taking place inside the barrel. In
fact, if an extrusion line is running certain materials fast enough, the heaters can be shut off
and the melt temperature maintained by pressure and friction alone inside the barrel. In most
extruders, cooling fans are present to keep the temperature below a set value if too much heat
is generated. If forced air cooling proves insufficient then cast-in cooling jackets are
employed.
At the front of the barrel, the molten plastic leaves the screw and travels through a screen
pack to remove any contaminants in the melt. The screens are reinforced by a breaker plate
(a thick metal puck with many holes drilled through it) since the pressure at this point can
[91]
exceed 5,000 psi (34 MPa). The screen pack/breaker plate assembly also serves to create
back pressure in the barrel. Back pressure is required for uniform melting and proper mixing
of the polymer, and how much pressure is generated can be "tweaked" by varying screen
pack composition (the number of screens, their wire weave size, and other parameters). This
breaker plate and screen pack combination also does the function of converting "rotational
memory" of the molten plastic into "longitudinal memory".
After passing through the breaker plate molten plastic enters the die. The die is what gives
the final product its profile and must be designed so that the molten plastic evenly flows
from a cylindrical profile, to the product's profile shape. Uneven flow at this stage can
produce a product with unwanted residual stresses at certain points in the profile which can
cause warping upon cooling. Almost any shape imaginable can be created so long as it is a
continuous profile.
The product must now be cooled and this is usually achieved by pulling the extrudate
through a water bath.
Machine Specifications:

Screw diameter: 30mm

L/D ratio- 40:1

Screw speed range: 0-1200 rpm

Throughput : 50-100 kg/hour
Application :Twin screw extruder is use mainly for PP compounding and PVC
3.Pulverizing Unit:
The pulveriser unit is capable of pulverizing polymer granules 500μm to 1.75mm.
Make: Fixopan Machines Pvt Ltd.
Model no: FP14-SGL
Capacity: 40-60 kg per hour
Grinding teeth: Multiple (Over 250)
[92]
4.Tumbler Mixer:
Capacity –40kg of pellets
Application : It is use for the physical mixing of granules
5.High Speed Mixer:
Make: KOLSITE
Specifications:
Capacity: 40kg
Speed: 1440rpm
Application :Used for PVC compounding.
6. Granulator:
Make: PIMCO
Specifications: 5hp, 3.7kW induction motor.
Application: Use for making granules
[93]
References
 ASTM Standards Handbook volume 08.01, 08.02, 08.03 , 08.04
 Polymer Science and Technology- V. Gowarikar
 http://ulprospector.com
 BRYDSON, J. A. (1999) Plastics Materials (7th edition)

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Report on PARC

  • 1. [1] IN-PLANT TRAINING REPORT At (1st July to 28th July) Product Application and Research Centre, (P.A.R.C.) Chembur,Mumbai Submitted by: Suyash Trivedi Central Institute of Plastics Engineering & Technology (C.I.P.E.T.) Lucknow
  • 2. [2] Preface The main purpose of this project was to provide us the opportunity to expand our theoretical concepts and lessons to a practical level of working, thereby helping us to understand the application of those principles in real situations. Therefore our college “Central Institute of Plastics Engineering & Technology” gives due importance to this aspect of education by providing us this internship in a reputed business house “Reliance Industries Ltd – Product Application and Research Centre (PARC)”, to enhance our practical experience. Our area of work during the internship was to work in the lab and perform various tests relating to plastics and in the processing area to learn different processingtechniques used for plastic. This process has given us invaluable experience and enriched our skills not only relating to polymer but also about raw materials, manufacturing processes,testing etc. We are thankful to PARC-RIL for providing us this good experience.
  • 3. [3] Acknowledgements The training opportunity we had with Product Application and Research Center (PARC), Reliance Industries Ltd (RIL) was a great chance for learning and professional development. Therefore, we consider ourselvesas very lucky individuals as we were provided with an opportunity to be a part of it. We are also grateful for having a chance to meet so many wonderful people and professionals who led us though this internship period. We are deeply grateful to Mr. S.V.Raju, Head of the Department - Product Application and Research Center (PARC), Reliance Industries Ltd (RIL) and Dr.Nitin V Joshi, Lab in charge – PARC,RIL for extending its training facilities and giving us an opportunity to gain an insight into the working of an industry. We are using this opportunity to express our deepest gratitude and special thanks to Mr.Nitin V. Joshi, our guide who in spite of being extraordinarily busy with his duties, took time out to hear, guide and keep us on the correct path and allowing us to carry out our training at their esteemed organization. We would specially like to thank Mr. TusharDongre, Mr. Zubair Ahmed,Mr.Vinod Kumar,Mr.Ajit Patel, Mr.Sundareshan,Mr.SunilMahajan,Mr. Surendra Gupta and Mr. Kulkarni for their support and co-operation throughout the training period in spite of their busy schedules. Our sincere regards to Mr.Ravi Kumar, Mr. NileshBakare,Mr.RavindraKute, Ms.RenukaSarode, Ms.SmithaKumbhare, Ms.NehaPawar, Ms.HimaPadhiar, Mr. SoorajVadathala andMr.JigarPalecha for their continuous help during the training. We are highly indebted to the executive & technical officers of PARC for their everyday guidance and help and special thanks to Mr. AnantPawar, Mr.AjitGhate& Mr. LalitPathaskar for their help in the processing centre. Finally we would like to thank all the office and support staff for extending their cooperation throughout the course of this training.
  • 4. [4] TABLE OF CONTENTS Company Profile………………………………………………………..5 Manufacturing Facilities………………………………………………..7 Introduction to Polymers Testing at PARC………………………….…13 Introduction to PARC…………………………………………………24 Testing Division……………………………………………………….25 Processing Division……………………………………………………69
  • 5. [5] 1. Company Profile The Reliance Group , founded by Dhirubhai H. Ambani, is India's largest private sector enterprise, with businesses in the energy and materials value chain. The flagship company, Reliance Industries Limited, is a Fortune Global 500 company and is the largest private sector company in India. Reliance Industries Limited (RIL) is an Indian conglomerate holding companyheadquartered in Mumbai, Maharashtra, India. The company currently operates in five major segments: exploration and production, refining and marketing, petrochemicals,retail and telecommunications. The company is ranked114th on Fortune Global 500 listof the world's biggest corporations for the year 2014. RIL is one of the largest publiclytraded companies in India by market capitalization. It is the second largest company inIndia by revenue after Indian Oil Corporation. RIL’s total turnover is US$ 62.2 billionas of FY2014-15 making aa profit of US$ 3.8 billion. Reliance enjoys global leadership in its businesses, being the largest polyesteryarn and fiber producer in the world 2.5 million tons per annum and among the top five to ten producers in the world in major petrochemical products.  RIL manufactures Polypropylene (PP), Polyethylene (PE) and Polyvinyl Chloride(PVC) sold under the brand namesRepol, Relene&Reonrespectively.  Diverse applications across packaging, agriculture, automotive, housing,healthcare, water and gas transportation and consumer durables.  Repol PP can turn any of your 'plastic' ideas into a reality.  Relene PE has completely transformed the concept of packaging.  Reon PVC is a versatile polymer with applications ranging from soft to rigid.
  • 6. [6]  RIL has manufacturing sites atHazira, Nagothane, Jamnagar, Naroda and Vadodara, Dahej, Allahabad, Dhenkanal, Barabanki, Kurkumbh, Nagpur, Patalganga, Silvassa.  RIL is the largest producer of PE & PP in India. Reliance's polymer business is integrated with its cracker facility at Hazira, as well as its refinery at Jamnagar, ensuring feedstock availability at all times. The company operates world-scale plants for Polyolefins and PVC with state-of-art technologies from global licensors like Novacor, Geon and Union Carbide. Along with IPCL, Reliance is among the world's top 10 plastic producers. Reliance Industries Limited is Asia's largest manufacturer of Polypropylene (PP). Reliance figures the fifth largest Polypropylene producers in the world. The four production sites offer a wide range of Homopolymer, Random and Impact copolymer grades. These can cater to the entire spectrum of Extrusion, Injection & Blow molding processes. “Relene” HDPE is available in densities ranging from 0.941g/cc to 0.965g/cc & melt flow index from as low as fractional to 20. Relene HDPE is widely used for numerous extrusion & molding applications. Specially formulated HDPE Raffia grade has placed "Relene" way above the competing materials for this application. The grade has excellent processability on high output raffia lines & exhibits superior balance of tenacity / elongation. Reliance LLDPE grades are marketed under trade name "Reclair" & is available in density range of 0.916 to 0.935 g/cc & MFI range from fractional to as high as 50.
  • 7. [7] 2. Manufacturing Facilities 1.Hazira Hazira Manufacturing Division is located near Surat, Gujarat. It comprises of a Naptha cracker feeding downstream fibre intermediates, plastics and polyester plants. The first phase of the complex was commissioned in 1991-92 to generate power/utility and to manufacture Ethylene Oxide (EO), Mono Ethylene Glycol (MEG), Vinyl Chloride Monomer(VCM), Poly Vinyl Chloride (PVC) and High Density Polyethylene (HDPE). A jetty was built for loading and unloading operation of raw material and final products. The second phase of the project, started in 1995, involved commissioning of the Polyester Complex (POY & PSF) and continued in full backward integration with commissioning of the new Polypropylene (PP), Naphtha Cracker, Purified Terephthalic Acid (PTA) plants and also involved expansion of existing phase 1 plants. 2.Jamnagar Jamnagar Manufacturing Division is located near Jamnagar, Gujarat. It comprises of a petroleum refinery and associated petrochemical plants. The refinery is equipped to refine various types of crude oil (sour crude, sweet crude or a mixture of both) and manufactures various grades of fuel from motor gasoline to Aviation Turbine Fuel (ATF). The petrochemicals plants produces plastics and fibre intermediates. The Polypropylene plant at Jamnagar has a huge capacity of 1030 KTA of Polypropylene producing a wide range of grades that cater to an equally diverse range of sectors which include Raffia, Films (BOPP/IPP), Injection Molding, Extrusion, Fibre etc. The new PP line in the SEZ facility resulted in additional capacity of 900 KTA.
  • 8. [8] 3.Allahabad Allahabad Manufacturing Division located in Allahabad, Uttar Pradesh, is spread over 105 acres.It is equipped with batch polymerization and continuous polymerization facilities. The batch plant produces wider range of specialty polymers and continuous plant produces both commodity and differentiated products. Both the plants are equipped with pilot positions to produce customer specific products and for development activities. The plant also has integrated facilities of draw twisting, draw texturizing, Yarn Dyeing and Twisting. The first phase of the plant was commissioned with a batch plant in 1991 with technology from Toray Industries Inc. , Japan. In the second phase, the plant was further expanded in 1997 with technology from Toray Engineering Company, Japan. Since then, the plant has developed indigenous technologies with its development activities to produce a large range of Specialty polymers, for different downstream processes like draw twisting, draw warping, draw texturizing, air texturizing etc. 4. Nagothane Nagothane Manufacturing Divisionlocated in Raigad, Maharashtra, is spread over 1,860 acres.It comprises of an ethane and propane gas cracker and five downstream plants for the manufacture of polymers, fibre intermediates and chemicals. 5.Patalganga Patalganga Manufacturing Division located near Mumbai, Maharashtra, is spread over 200 acres. It comprises of polyester, fibre intermediates and linear alklyl benzene manufacturing plants.
  • 9. [9] Products Manufactured: Product Manufactured from Para - Xylene (Px) Naphtha Purified Terephthalic Acid (PTA) Para - Xylene Polyester Filament Yarn (PFY) PTA & MEG Polyester Staple Fibre (PSF) PTA & MEG Linear Alkyl Benzene (LAB) Kerosene - n paraffin 6. Naroda Naroda Manufacturing Division located near Ahmedabad, Gujarat, is RIL’s first manufacturing facility. This synthetic textiles and fabrics manufacturing facility manufactures and markets woven and knitted fabrics for home textiles, synthetic and worsted suiting and shirting, ready to wear garments and automotive fabrics. 7.Dahej Dahej Manufacturing Division is located near Bharuch, Gujarat. It comprises of an ethane/propane recovery unit, a gas cracker, a caustic chlorine plant and 4 downstream plants, which manufacture polymers and fibre intermediates. The plant has its own facility for separating ethane/propane. The ethane / propane mixture is used as a feedstock for the gas cracker plant. The division was commissioned in two phases. The Caustic Chlorine, VCM and PVC pants in phase one was commissioned in 1997. After this, in phase two, HDPE plant, MEG plant, ethane / propane recovery plant and gas cracker unit were commissioned in 2000.
  • 10. [10] 8. Hoshiarpur RIL- Hoshiarpur Division is located in Hoshiarpur, Punjab. It manufactures a wide range of PSF, PFF, POY and polyester chips. The Plants at Hoshiarpur Manufacturing Divisional The plants of PSF-I, PSF-II, POY, PFF are commissioned in 1989, 1995, 1995, 2004. In addition to the regular products, Hoshiarpur Manufacturing Division has added the following differentiated value added products: 1. Dope Dyed Olive Green & Khaki Fibre 2. Recron 3s for Construction & Paper Industry 3. Polyester Fibre Fill 4. Cluster Fibre 5. Conjugate Fibre 9. Nagpur Nagpur Manufacturing Division is located in Nagpur, Maharashtra. It manufactures polyester filament yarn, dope-dyed specialty products of different ranges, fully drawn yarn and polyester chips. The plant has facilities like housing for its employees, school, guest house and a Ganesha temple. RIL - Nagpur Manufacturing Division is an ISO: 9001:2000 certified unit accredited by BVQI, along with certification for ISO14001: 2004 and OHSAS 18001:1999 as well. Products Manufactured: 1. Polyester Filament Yarn (PFY) from PTA & MEG 2. DD Specialty product of different range 3. Fully Drawn Yarn
  • 11. [11] 10. Barabanki Barabanki Manufacturing Division is located near Lucknow, Uttar Pradesh. It manufactures Black Fiber. Barabanki Manufacturing Division was commissioned in January, 1987, with technical collaboration from M/s. Du Pont, USA to manufacture 15,000 MT per annum of Commodity Polyester Staple Fibre. The capacity was gradually increased to 30,000 MT per annum by de-bottlenecking. The Commodity Polyester Staple Fibre produced was sold in national and international markets. In 2004, further capacity of 10,000 MT per annum was added by installing an extrusion based Spinning Plant. With this addition the present installed capacity of Barabanki Manufacturing Division is 40,000 MT per annum. 11. Silvassa Reliance Silvassa Manufacturing Division is located in the Union Territory of Dadra and Nagar Haveli. It manufactures a wide range of specialty products such as Recron Stretch, Linen Like, Melange, Thick-n-thin and Bi-shrinkage yarns. This division is the largest unit of it's kind in the world engaged in the field of texturizing of polyester partially oriented yarn (POY) to produce a wide range of polyester textured yarns (PTY) such as crimp, tex, intermingle in various deniers ranging from 30 D to 1200 D. The Denier per Filament (DPF) ranges from 0.5 to 4.8. It produces a wide variety of specialty products such as Recron Stretch, Linen Like, Melange, Thick-n-thin and Bi- shrinkage yarns. This division is the largest supplier of Recron stretch products to Denim industry in India. Moreover, it also offers various tailor-made products to suit the specific end use requirements. The textured yarn produced is used in suitings, shirtings, dress materials, home furnishings and automotive fabrics. This division has 158 state-of-the-art false twist texturising machines of Barmag, Murata, TMT, ICBT, Himson and Alidhra makes. The installed capacity of division is 150 KTA
  • 12. [12] and it exports 25 % of its production to various high quality demanding advanced markets of Europe, USA, North America, Far East and African markets to about 45+ countries. This division enjoys various international certifications and accreditations such as ISO 9001, ISO 14001, OHSAS 18001 and Oekotex certificate for exports. To achieve continual improvements and growth, the Division has also deployed Six Sigma & Quality Circle activities in various functional areas. This division offers the best quality products with a three tier quality assurance system. All the machines are equipped with on line tension monitoring (OLT) system wherein every meter of yarn is continuously monitored by computers for product quality during texturising, itself. The products deliver competitive edge to the customers by virtue of : Equal length packages that minimize waste, Uniform package density for consistent package unwinding at high speed, Continuity of batch nos. to enhance productivity and reliability, 100 % transfer tail end to improve the machine efficiencies 12. Vadodara Vadodara Manufacturing Division located in Vadodara, Gujarat. It comprises of a Naphtha cracker and 15 downstream plants for the manufacture of polymers, fibers, fiber intermediates and chemicals.
  • 13. [13] Introduction to Polymers Testing at PARC Polypropylene Polypropylene (PP), also known as polypropene, is a thermoplastic polymer used in a wide variety of applications including packaging and labeling, textiles (e.g., ropes, thermal underwear and carpets), stationery, plastic parts and reusable containers of various types, laboratory equipment, loudspeakers, automotive components, and polymer banknotes. An addition polymer made from the monomer propylene, it is rugged and unusually resistant to many chemical solvents, bases and acids. There are three general types of polypropylene: homopolymer, random copolymer, and block copolymer. The comonomer is typically used with ethylene. Ethylene-propylene rubber or EPDM added to polypropylene homopolymer increases its low temperature impact strength. Randomly polymerized ethylene monomer added to polypropylene homopolymer decreases the polymer crystallinity, lowers the melting point and makes the polymer more transparent. Polymerization of propylene can yield any of the three polymer forms, isotactic, syndiotactic or atactic. Polypropylene has three basic polymeric forms: isotactic, syndiotactic and atactic. These different polymeric forms arise because, compared to the starting substance for polyethylene CH2=CH2 (ethene), the starting substance propylene CH3•CH=CH2 (propene), has a methyl (CH3) group in place of a hydrogen. In the isotactic form of polypropylene the methyl group has the same configuration at each tertiary carbon atom along the polymer chain. In the syndiotactic form, the methyl group alters position on alternative tertiary carbon atoms. In the atactic form, the methyl group takes up random positions on the tertiary carbon atoms.
  • 15. [15] Industrial Process: Traditionally, three manufacturing processes are the most representative ways to produce polypropylene. Hydrocarbon slurry or suspension: Uses a liquid inert hydrocarbon diluent in the reactor to facilitate transfer of propylene to the catalyst, the removal of heat from the system, the deactivation/removal of the catalyst as well as dissolving the atactic polymer. The range of grades that could be produced was very limited. (The technology has fallen into disuse). Bulk (or bulk slurry): Uses liquid propylene instead of liquid inert hydrocarbon diluent. The polymer does not dissolve into a diluent, but rather rides on the liquid propylene. The formed polymer is withdrawn and any unreacted monomer is flashed off. Gas phase: Uses gaseous propylene in contact with the solid catalyst, resulting in a fluidized-bed medium. Manufacturing: Melt processing of polypropylene can be achieved via extrusion and molding. The most common shaping technique is injection molding, which is used for parts such as cups, cutlery, vials, caps, containers, housewares, and automotive parts such as batteries. The related techniques of blow molding and injection-stretch blow molding are also used, which involve both extrusion and molding. Application: Product Classification Features Uses REPOL H110MA Homopolymer Antistatic, Food contact Acceptable Blending; Compounding, Containers, Furniture, Houseware REPOLSRM100NC Random copolymer Antistatic; Food Contact Acceptable; High Clarity Blow Molding Applications; Containers; Household Goods REPOL H030SG Homopolymer Food Contact Acceptable; Good Processability Industrial Applications; Carpet Backing; Monofilament
  • 16. [16] REPOL H200MA Homopolymer Antistatic; Food Contact Acceptable Thin-walled Containers REPOL B120MA Impact Copolymer Food Contact Acceptable; General Purpose; Medium Automotive Applications; Furniture; General Purpose REPOL H100EY Homopolymer Antiblocking; Food Contact Acceptable; General Purpose Slip Bags; Film; Food Packaging; General Purpose; Packaging REPOL SR20NC Random Copolymer Food Contact Acceptable Blow Molding Applications; Bottles; Containers REPOL H034SG Homopolymer Food Contact Acceptable Pacific Bi-axially Oriented Film; Film; Food Packaging Polyethylene Polyethylene (abbreviated PE) or polythene (IUPAC name polyethylene or poly(methylene)) is the most common plastic. Its primary use is in packaging (plastic bag, plastic films, geomembranes, containers including bottles, etc.). Polyethylene is classified into several different categories based mostly on its density and branching. Its mechanical properties depend significantly on variables such as the extent
  • 17. [17] and type of branching, the crystal structure and the molecular weight. With regard to sold volumes, the most important polyethylene grades are HDPE, LLDPE and LDPE.  Ultra-high-molecular-weight polyethylene (UHMWPE)  Ultra-low-molecular-weight polyethylene (ULMWPE or PE-WAX)  High-molecular-weight polyethylene (HMWPE)  High-density polyethylene (HDPE)  High-density cross-linked polyethylene (HDXLPE)  Cross-linked polyethylene (PEX or XLPE)  Medium-density polyethylene (MDPE)  Linear low-density polyethylene (LLDPE)  Low-density polyethylene (LDPE)  Very-low-density polyethylene (VLDPE)  Chlorinated polyethylene (CPE) Reliance Brand Name:Relene
  • 18. [18] Application: HDPE Raschel bags for fruits and vegetables , containers for packaging edible oil, processed food, carrier bags, pipes for water supply, irrigation. LDPE LDPE is widely used for manufacturing various containers, dispensing bottles, wash bottles, tubing, plastic bags for computer components, and various molded laboratory equipment. Its most common use is in plastic bags.Trays and general purpose containers Corrosion-resistant work surfaces Parts that need to be weldable and machinable Parts that require flexibility, for which it serves very well Very soft and pliable parts such as snap-on lids, six pack rings LLDPE Filmsfor packaging milk, edible oil, salt, roto-molded containers for storage of water, protective films and pipes for agriculture. There are different grades that are produced by reliance. Some of the grades along with their applicationsare given below. Product Classification Features Uses RELENE1005FY20 LDPE FoodContact Acceptable; Good Heat Seal; Good Impact strength Film; Packaging RELENE1070LA17 LDPE Contact Acceptable; Good Adhesion; Good Drawdown Coating Applications; Film; Laminates RELENE 1003FA20 LDPE Food Contact Acceptable; Good Impact Resistance Agricultural Applications; Film; Shrink Wrap; Wire RELENE54GB012 HDPE Bimodal Molecular Weight Distribution; Containers;Blow Molding;Foodcontact RELENE LDPE Food Contact Acceptable Flow Masterbatch;
  • 19. [19] 16MA400 Thin-walled Parts RELENE M60075 HDPE Food Contact Acceptable; Good Dimensional Stability Containers; Crates; Industrial applications; Luggage RELENE 1020FA20 LDPE Food Contact AcceptableFilm; Laminates RELENE 24FS040 LDPE Contact Acceptable; General Purpose Food; High Slip Bags; General Purpose; Packaging RELENE E52009 HDPE Food Contact Acceptable Low Gel; Low Water Carryover Monofilaments; Tape RELENE F19010 LLDPE Antiblocking; Antioxidant; ButeneComonomer Food and film Packaging Polyvinyl Chloride PVC comes in two basic forms: rigid (sometimes abbreviated as RPVC) and flexible. The rigid form of PVC is used in construction for pipe and in profile applications such as doors and windows. It is also used for bottles, other non-food packaging, and cards (such as bank or membership cards). It can be made softer and more flexible by the addition of plasticizers, the most widely used being phthalates. In this form, it is also used in plumbing, electrical cable insulation, imitation leather, signage, inflatable products, and many applications where it replaces rubber. Pure poly(vinyl chloride) is a white, brittle solid. It is insoluble in alcohol but slightly soluble in tetrahydrofuran.
  • 20. [20] Polyvinyl chloride is produced by polymerization of the vinyl chloride monomer (VCM), as shown. About 80% of production involves suspension polymerization. Emulsion polymerization accounts for about 12% and bulk polymerization accounts for 8%. Suspension polymerizationsaffords particles with average diameters of 100–180 μm, whereas emulsion polymerization gives much smaller particles of average size around 0.2 μm. Chlorinated Polyvinyl Chloride (CPVC) is PVC (polyvinyl chloride) that has been chlorinated via a free radical chlorination reaction. This reaction is typically initiated by application of thermal or UV energy utilizing various approaches. In the process, chlorine gas is decomposed into free radical chlorine which is then reacted with PVC in a post- production step, essentially replacing a portion of the hydrogen in the PVC with chlorine.CPVC shares most of the features and properties of PVC. It is also readily workable, including machining, welding, and forming. Because of its excellent corrosion resistance at elevated temperatures, CPVC is ideally suited for self-supporting constructions where temperatures up to 200 °F (90 °C) are present. Reliance Brand Name:Reon
  • 21. [21] Application: Pipes and fittings, Door and window profile, rigid bottles and containers for packaging applications, footwear, flooring & blood bags. The uses of different grades of REON are Product Classification Features Use Reon 67-01 PVC Homopolymer Good Processability; Homopolymer; Medium Molecular Weight Film; Piping; Profiles; Sheet Reon 57GMR01 PVC Homopolymer Low Molecular Weight; High Flow; Homopolymer Foam; Handles; Piping; Sheet Reon 57-11 PVC Homopolymer Good Processability; High Flow; Homopolymer; Low Molecular weight Bottles; Cosmetics; Film; Handles; Packaging; Piping; Sheet Reon 60-11 PVC Homopolymer Good Processability; Homopolymer; Low Molecular weight WeightBottles; Containers; Cosmetic Packaging; Cosmetics Reon 57-01 PVC Homopolymer Food Contact Acceptable; High Flow; Low molecular weight Containers; Foam; Foamed Insulation Board Reon 57GER01 PVC Homopolymer Good Processability; High Flow; Homopolymer; Low Molecular weight Bottles; Containers; Cosmetics; Film; Foam; Handle Reon 67GER01 PVC Homopolymer Good Processability; HighFlow; Homopolymer;Medium molecular weight Film; Piping; Profiles; Sheet
  • 22. [22] Reon 60GER01 PVC Homopolymer Good Processability; High Flow; Homopolymer; Low Molecular weight Bottles; Cosmetic Packaging; Cosmetics; Film; Packaging Reon 67GEF01 PVC Homopolymer Food Contact Acceptable; Homopolymer; Medium Molecular weight Cable Jacketing; Footwear; Hose; Insulation; Medical application Reon 67-11 PVC Homopolymer Food Contact Acceptable; Homopolymer; Medium Molecular Cable Jacketing; Film; Footwear; Hose; Insulation;...View entire Reon product line.  Plants of Reliance where Polymers aremanufactured  Polypropylene Type of Polymer manufactured Plant Sites HP,ICP Hazira HP Jamnagar DTA HP Jamnagar SEZ HP,RCP,ICP Naroda HP,RCP Nagothane
  • 23. [23]  Polyethylene Type of Polymer manufactured Plant Sites LDPE Baroda Nagothane HDPE Gandhar EVA LLDPE/HDPE Swing Nagothane Hazira  Polyvinyl chloride Type of Polymer manufactured Plant Sites PVC Hazira, Baroda &Gandhar
  • 24. [24] 4. INTRODUCTION TO PRODUCT APPLICATION & RESEARCH CENTRE The product application & research centre (PARC), Reliance Industries Limited petrochemical division was established in 1990 at Chembur, Mumbai as a technical wing of the polymer marketing division. It is deeply involved in the development of new grades & the optimization of the existing grades in terms of cost & properties. It also carries out continuous valuation of various lots produced at Jamnagar &Hazira plants. PARC is committed to deliver value addition to polymer business of Reliance Industries Limited by providing technical service, constant product up gradation and initiating market development with the sole objective of total customer satisfaction. It also carries out testing and trials of various modified and developmental grades. PARC is a conduit between business enterprises and their vendors, converting basic needs into commercially viable technology and helping to produce useful products. To fulfill these objectives, sophisticated analytical & processing facilities have been established at PARC. PARC is recognized by the department of science and industrial research as an in-house research & development wing of reliance-plastic & petrochemical division. Functions of PARC: Product development Process development Customer Support / Technical service Co-ordination with plant & marketing department for benchmarking exercises Training & manpower development The Activities of PARC can be divided into: Testing Processing
  • 25. [25] 5. TESTING DIVISION Testing of raw material is absolutely necessary for quality control & characterization. The analytical laboratory is involved in the analysis & testing of resin and product samples received from the customers as well as from the PARC division. Testing for resin:  Melt Flow Index  Ash Content  Bulk Density  FTIR Spectroscopy  Measurement of Color  Differential Scanning Calorimeter  Thermo Gravimetric Analysis  Density Testing for plastic films:  Shrinkage Test for films  Tear Strength  Coefficient of Friction (COF)  Haze  Dart Impact Strength  Tensile Properties  Haze test Testing for Molded samples:  Tensile properties  Scanning Electron Microscope(SEM)  Izod-Impact strength  Shrinkage Test  Heat Deflection Temperature &Vicat Softening point
  • 26. [26]  Environmental Stress Cracking Resistance (ESCR)  Specular Gloss Testing  Indentation Hardness Testing  Flexural Properties of Plastics  Gardener Impact Resistance
  • 27. [27] TESTING FOR RESIN Melt Flow Index Determination Reference: ASTM D1238 Machine Make:Davenport Flow Indexer. Summary: For this, molten polymer is extruded through a die and flow of polymer ismeasured under a specified load and at particular temperature per 10 min Scope: This procedure is used to determine melt flow properties of resins with the help ofDavenport Flow Indexer. Melt Index is an inverse measure of molecular weight. Sinceflow characteristics are inversely proportional to the molecular weight, a low molecular polymer weight polymer will have a high melt index value and vice versa. Principle: MFI indicates the rate of extrusion of molten resin through a die of specified length and diameter under prescribed conditions of temperature,load and piston position in barrel.
  • 28. [28] Apparatus: (I) Melt Flow Indexer (Davenport make) with accessories: Temperature: PE: 1900C PP: 2300C Preheating time : o PP: 6 min o PE:5 min Barrel diameter= 9.5504 ±0.0016 mm Die diameter= 2.0955 ± 0.0016 mm Die Length= 8 ± 0.025 mm Weight= 2.16 kg, 6.48 kg (± 0.5% of the total weight) Procedure: 1. Manual  A small amount of the polymer sample (around 4 to 5 grams) is taken as per the expected MFI of material in the specially designed MFI apparatus. The apparatus consists of a small die inserted into the apparatus, with the diameter of the die being around 2 mm.  The material is packed properly with the help of suitable piston inside the barrel to avoid formation of air pockets.  A piston is introduced which acts as the medium that causes extrusion of the molten polymer.  The sample is preheated for a specified amount of time: 5 min at 190°C for polyethylene and 6 min at 230°C for polypropylene.  Push the piston a little above the mark to ensure good packing (known as purging).  After the preheating a specified weight is introduced onto the piston. Examples of standard weights are 2.16 kg, 5 kg, etc.  The weight exerts a force on the molten polymer and it immediately starts flowing through the die.
  • 29. [29]  A sample of the melt is cut in regular intervals of time and is weighed accurately.  MFI is expressed as grams of polymer/10 minutes of flow time. 2. Automatic  Weigh the specimen and put it in the apparatus as per the expected MFI.  Select remote control on apparatus and start the computer.  In the computer start console software.  Feed polymer type, melt density, cut-off length and file name.  Start the test.  Purge after 3 minutes just before the mark on piston.  Put the arrester of 71mm or 81mm height depending on whether the material is Hi- Flow or Low-Flow.  Put the weight on plate above the apparatus.  Record the output. ASH CONTENT Reference: ASTM D2584, D5630
  • 30. [30] Machine Make:Mettler Balance, Bunsen burner Scope: This test is used to find out the inorganic residues in a polymer sample by ashing it in a muffle furnace. Summary: A weighed amount of sample is heated to 850±10⁰C and residue after treating is expressed in terms of % ash content. Principle: The organic matter in a polymer sample is burnt at 850±10⁰C until constant mass of inorganic matter is obtained. Apparatus: 1. Weighing balance 2. Silica crucible 3. Bunsen burner 4. Silica triangle & tripod 5. Holder Sample specification: 3-5 g of sample Procedure  The sample weight and the weight of the empty crucible are noted.  Sample is put in the crucible and allowed to burn till it becomes completely black and the organic materials have vanished.  In case of PVC sample (self-extinguishing in nature) the sample is now wetted completely with 98% sulphuric acid and it is again heated to give out CaSO4.  After heating, the PVC sample is now put in the oven for 1 hour at 850°C.  For other samples, after burning is completed they are put in an oven maintained at 550°C  Now the sample is kept in a desiccant (containing silica gel) for ½ hour to absorb all the moisture.  It is then weighed and the ash content is found. Calculation % ash content = Weight of ash × 100 Weight of sample
  • 31. [31] NOTE: WITH THE HELP OF STOICHIOMETRY WE CAN EASILYCALCULATE THE WEIGHT OF FILLER CONTENT. FILLER CONTENT MEANS MIXTURE OF CALCIUM CARBONATE AND MAGNESIUM SULPHATE(TALC).HEATING AT 850°CWILL HAVE NO EFFECT ON MAGNESIUM SULPHATE WHEREAS CALCIUM CARBONATE DECOMPOSES INTOCALCIUM OXIDE AND GAS IS RELEASED. WITH THE HELP OF CALCIUM OXIDE CONTENT LEFT WE CAN EASILY CALCULATE THE AMOUNT OF CALCIUM CARBONATE PRESENT INITIALLY. FourierTransformInfrared Spectroscopy(FTIR) Reference: ASTM E1252 Machine make-Perkin Elmer, spectrum 100 series
  • 32. [32] Principle: FTIR utilize an ingenious device called Michelson interferometer, which was developed many years ago by A. A. Michelson for making precise measurement of the wavelengths of electromagnetic radiations. FTIR instruments contain no dispersing elements and all wavelengths are detected and measured simultaneously. Instead of a monochromator an interferometer is used to produce interference patterns that contain the infrared spectral information. In FTIR when an infrared spectrum is introduced to a sample stretching and bending of various bonds takes place and due to different bond energies, each molecule absorbs energy at a different frequency. One of the components of an electromagnetic wave is a rapidly reversing electric field (E). This field alternately stretches and compresses a polar bond. When the electric field is in the same direction as the dipole moment, the bond is compressed and its dipole moment decreases. When the field is opposite the dipole moment, the bond stretches and its dipole moment increases. If this alternate stretching and compressing of the bond occurs at the frequency of the molecule's natural rate of vibration, energy may be absorbed. The energy is absorbed by a molecule only when there is a change in dipole moment.
  • 33. [33] The Source: Infrared energy is emitted from a glowing black-body source. This beampasses through an aperture which controls the amount of energy presented to the sample (and, ultimately, to the detector). The Interferometer: The beam enters the interferometer where the “spectral encoding” takes place. The resulting interferogram signal then exits the interferometer
  • 34. [34] The Sample: The beam enters the sample compartment where it is transmitted throughor reflected off of the surface of the sample, depending on the type of analysis being accomplished. This is where specific frequencies of energy, which are uniquely characteristic of the sample, are absorbed. The Detector: The beam finally passes to the detector for final measurement. Thedetectors used are specially designed to measure the special interferogram signal. The Computer: The measured signal is digitized and sent to the computer where theFourier transformation takes place. The final infrared spectrum is then presented to the user for interpretation and any further manipulation. Procedure:  Take small amount of material on a glass slide and place it on a hot plate. Ensure the material melts and press it into a uniform film by applying steady pressure by means of another glass plate. If material is already in film form it can be used directly.  Once the background scan has been completed the spectroscopy of the material is carried out.  Place the film sample on the Universal Attenuated Total Reflectance Cell and scan it for background radiation.  The interference pattern of the material is obtained which is converted by the Fourier analyzer into a spectrum.  The graph obtained is of % transmittance v/s wave number.
  • 35. [35] (A typical FTIR spectrum) NOTE: WE NEED TO DO BLANK FTIR FOR THE DETECTON OF NOISE PRODUCED DUE TOAIR (BACKGROUND DISTURBANCES) BEFORE PERFORMING FTIR FOR THE CHEMICAL COMPOUND. LATER, AREA OF THE PEAKS DUE TO NOISE IS SUBSTRACTED WITH THE RESULT TO FIND OUT THE DISTURBANCES DUE TO SAMPLEONLY.
  • 36. [36] DIFFERENTIALMECHANICAL ANALYSIS REFERENCE: ASTM D-5279/D-4065 SCOPE: Studying viscoelastic behavior of polymers , glass transition temperature. SUMMARY: a sinusoidal stress is applied and the strain in the material is measured allowingone to determine the complex modulus.The temperature of the sample or the frequency of the stress are often varied , leading to variations in the complex modulus. NOTE: IT IS 10 TO 100 TIMES MORE SENSITIVE THAN DSC FOR THE MEASUREMENT OF GLASS TRANSITION TEMPERATURE. IT ALSO MEASURES STIFFNESS AND DAMPING REPORTED AS MODULUS AND TAN DELTA RESPECTIVELY. THEORY: Polymers composed of long molecular chains have unique viscoelastic properties, which combine the characteristics of elastic solids and Newtonian fluids. The classical theory of elasticity describes the mechanical properties of elastic solid where stress is proportional to strain in small deformations. Such response of stress is independent of strain rate. The classical theory of hydrodynamics describes the properties of viscous fluid, for which the response of stress is dependent on strain rate. This solidlike and liquidlike behavior of polymer can be modeled mechanically with combinations of springs and dashpots
  • 37. [37] INSTRUMENTATION: The instrumentation of a DMA consists of a displacement sensor such as a linear variable differential transformer, which measures a change in voltage as a result of the instrument probe moving through a magnetic core, a temperature control system or furnace, a drive motor (a linear motor for probe loading which provides load for the applied force), a drive shaft support and guidance system to act as a guide for the force from the motor to the sample, and sample clamps in order to hold the sample being tested. Depending on what is being measured, samples will be prepared and handled differently. Temp range : -190 to 400 °C Sample size maximum: 52.5(mm)* 12.8(mm)* 8 (mm) APPLICATION: One important application of DMA is measurement of the glass transition temperature of polymers. Amorphous polymers have different glass transition temperatures, above which the material will have rubbery properties instead of glassy behavior and the stiffness of the material will drop dramatically with an increase in viscosity. At the glass transition, the storage modulus decreases dramatically and the loss modulus reaches a maximum.
  • 38. [38] Temperature sweep: A common test method involves measuring the complex modulus at low constant frequency while varying the sample temperature. A prominent peak in appears at the glass transition temperature of the polymer. Secondary transitions can also be observed, which can be attributed to the temperature-dependent activation of a wide variety of chain motions. In semi-crystalline polymers, separate transitions can be observed for the crystalline and amorphous sections. Similarly, multiple transitions are often found in polymer blends. For instance, blends of polycarbonate and poly(acrylonitrile-butadiene-styrene) were studied with the intention of developing a polycarbonate-based material without polycarbonate’s tendency towards brittle failure. Temperature-sweeping DMA of the blends showed two strong transitions coincident with the glass transition temperatures of PC and PABS, consistent with the finding that the two polymers were immiscible. Figure shows Storage modulus and loss modulus against Temperature were plotted.
  • 39. [39] Determination of Density Reference: ASTM D792 Scope: This test is used to measure the density of solid samples. Principle: Archimedes Principle Apparatus: Weighing Balance (METTLER ) Density meter assembly: Beaker stand, Beaker (500mL), a frame attached to the weighing pan and a sample holder which facilitates weight in air and in liquid. Chemicals Used: 1. n-butyl acetate 2.DM Water
  • 40. [40] NOTE: BUTYL ACETATE IS USED IN PLACE OF WATER BECAUSE IT HAS DENSITY OF 0.88 g/L AT ROOM TEMPERATURE. SINCE IT IS NECESSARY FOR POLYMER TO SINK IN IT FOR DENSITY DETERMINATION AND ALL POLYMERS HAVE DENSITY GREATER THAN 0.88 g/L, BUTYL ACETATE IS IDEAL FOR THIS USE. Sample Specification:1 cm x 1 cm smoothly cut sample is used for densitydetermination. The sample shouldnot have any sharp edges. Procedure: The weight of the sample was measured in air and then in a liquid (n-butyl acetate) of known density. The density of the liquid used was less than the expected density of the sample. The ratio of weight in air to loss of weight in liquid was used to calculate the density of the sample. Calculation: Density of sample at Tm = Wa ρs Wa̵ Ws Where: Tm = Temperature of measurement Wa = Weight in air Ws = Weight in the liquid ρs = Density of the liquid at Tm
  • 41. [41] Determination of Tear Strength of films Reference: ASTM D1938 Machine Make: CEAST Italy Scope: Used to measure the tear strength of plastic films. Summary: To force to propagate a tear across a film or sheeting specimen is measured using a constant rate of grip separation machine.The force necessary to propagate the tear is interpreted from the load time chart. Principle: The force to propagate a tear across a film or sheeting specimen is measured. The force necessary to propagate the tear is measured. Apparatus: CEAST ED 30 machine, Digital micrometer Sample Specification: The specimens shall be of the single tear type and shall consist of strips 76 mm long by 64 mm wide. The thickness of the specimen is noted along the path where tear will occur. The samples are cut in the machine direction (MD) and the transverse direction (TD). Procedure: Different weights available are 4000mN, 8000mN, 16000mN, 32000mN,64000mN, 50N, 100N. The weight is selected such that the film reading lies between 20-90% of the weight. The blank reading is taken and the machine is calibrated. The sample is inserted in the pneumatic sample holder. The cover is shut and the film tears. The reading is noted from the display. Calculation: Tear Strength (in g/µm) = Force in cN / thickness (µm)
  • 42. [42] NOTE: TEAR STRENGTH IN MACHINE DIRECTION IS ALWAYS LESS THAN TRANSVERSE DIRECTION BECAUSE MOLECULES ARE ALIGNED IN MACHINE DIRECTION. SO IT IS EASIER TO SEPARATE DIFFERENT CHAINS (M.D) THAN TO BREAK BONDS OF CHAINS (T.D). Determination of Coefficient of friction of Plastic Films Reference: ASTM D1894 Machine Make: Davenport Scope: Used to find coefficient of friction between a plastic film with respect to otherfilms and metal surfaces. Summary: Two surfaces are made to slide against each other and the force required for this is measured. Principle: Frictional force f is related to the normal force acting on a body at rest as follows: f=µN, where µ is the coefficient of friction. The COF associated with the force required to start a body from rest is known as coefficient of static friction and that associated with a moving body is known as the coefficient of kinetic friction. Apparatus: Davenport friction measuring apparatus, template, vacuum pump Sample Specification: 675 mm x 255 mm should be attached to the testing plane and 6.5mm x 6.5 mm minimum for sliding.
  • 43. [43] Analytical Procedure: The vacuum is switched on and the film is placed on the plane, without wrinkles. The film is attached to the 200g sled with cellophane tape taking care to avoid wrinkles. The cord is attached to the sled and placed gently on the plane at two fixed points parallel to the machine direction. The speed is selected to be 15 cm/min. There should be no tension in the cord and both the force meter displays are zero. The first reading as soon as the cord pulls the slab is the static friction. The reset button is then pressed to get the value of the kinetic friction. Calculation: COSF = Static force/ weight of the sled=SF/20 COKF = Kinetic force/ weight of the sled=KF/20 NOTE: IT IS EASIER TO BREAK IN MACHINE DIRECTION THAN IN TRANSVERSE DIRECTION. Determination of Dart Impact Strength for Plastic Films
  • 44. [44] Reference: ASTM D1709 Apparatus: Dart Impact Testing apparatus (International Engineering Industries), Weights Scope: Used to measure the dart impact strength of plastic films Summary: Darts of various weights are made to fall on a clamped film and the weight at which 50% of the samples fail is measured. Sample Specification: Greater than the diameter of the specimen holder Principle: Dart Impact strength values are very important for plastics packaging. They theoretically give the impact strength of the plastic film. In the test, falling weights from a specified height are made to fall on the film until fracture occurs. The weight at which 50% of the samples fail is the dart impact weight value. This value divided by thickness in microns gives dart impact strength. Analytical Procedure: The two different types of dart used are: A.38.1 ± 0.13 mm of 55g weight B.50.8 ± 0.13 mm of 283g weight Vacuum applied is 700 mm of Hg A. Dropped from 66 cm and is used for films requiring masses of about 50g to 2 kg to fracture B. Dropped from 152 cm and used for films requiring masses of 0.3 to 2 kg to fracture 10 samples are tested on each weight level and the weight at which 50% failure occurs is reported.
  • 45. [45] Calculation: Dart Impact Strength (g/µm) = Weight to cause 50% fracture (g)/ thickness (µm) Determination of Tensile Properties of Plastic Films Reference: ASTM D882 Machine make:Lloyd, LRX plus Scope:This test method covers the determination of tensile properties of plastics in the form of thin sheeting, including film (less than 1.0 mm (0.04 in.) in thickness). Sample specifications: The width of the sample should be 15 mm - 25 mm and the gaugelength should be 5 cm. SPEED OF CROSSHEAD : 500mm/min Principle: Plastic products when subjected to tensile force initially resist deformation, get elongated and finally break. Tensile elongation and tensile modulus measurements are amongst the most important indications of strength in a material and are the most widely specified
  • 46. [46] properties of the plastic materials. Tensile test, in a broad sense, is a measurement of the ability of the material to withstand forces that tend to pull it apart and to determine to what extent the material stretches before breaking. Tensile modulus, an indication of the relative stiffness of a material can be determined from a stress-strain diagram. Procedure: The film is cut in exact dimensions making sure that the sides are uniform. The sample is clamped carefully and the thickness of the film is measured using a digital micrometer. The dimensions and batch references are entered in the software. The initial load is tare and the speed of testing is set to 500 mm/min and the machine is started. The stress vs. extension curve of the specimen is recorded and the required values are taken. NOTE: TENSILE STRENGTH IN MACHINE DIRECTION IS ALWAYS MORE THAN IN TRANSVERSE DIRECTION BECAUSE MOLECULES ARE ALIGNED IN MACHINE DIRECTION. SO IT IS DIFFICULT TO BREAK BONDS OF CHAINS (IN M.D) THAN TO SEPARATE DIFFERENT CHAINS (IN T.D) Haze Test Reference: ASTM D 1003
  • 47. [47] Scope: This test is used to measure the haze (% Transmittance) of plastic films and sheets Principle: The haze is determined by percentage of light scattered from the product. The haze of the specimen is the percentage of transmitted light which is passing through the specimen deviates from the incident beam by forward scattering.For the purpose of this method only light flux deviating more than 2.5’ on the average is considered to be haze The haze can be inherent in the material,a result of the moldingprocess,or a result of surface texture. Haze can also be a result of environmental factors such as weathering or surface abrasion. Sample: Size suitable to cover the port. Procedure:  The instrument is calibrated before haze measurement in the Total Transmittance Mode  The mode “large area view “ and “UV filter out” are selected  The blank reflectance trap is placed against the receptor lens and the machine is allowed to read.  The white tile is placed in the reflectance port and the transmittance compartment is kept away.  The sample holder is placed against the sphere and the machine is allowed to read. Instrument is now ready for haze measurement.
  • 48. [48] TESTING FOR MOLDED SAMPLES Determination of Tensile Properties of Molded Plastics Reference: ASTM D638 Scope: This test is used to determine the tensile properties of molded polymer samples. Summary: Standard molded specimens were exposed to tension and force required to elongate and break the specimen of elongation were observed. Principle: Plastic products when subjected to tensile force initially resist deformation, get elongated and then finally break. Tensile elongation and tensile modulus measurements are among the most important indications of strength in a material and are most widely specified properties of plastic materials. Tensile test in a broad sense is a measurement of the ability of a material to withstand forces that tend to pull it apart and to determine to what extent the material stretches before breaking. Tensile modulus, an indication of the relative stiffness of a material can be determined from a stress-strain diagram.
  • 49. [49] Apparatus: (i) Universal Testing Machine (ii) Grips for mounting the specimen (iii) VernierCalipers Sample Specification: Five specimens are tested as per the following specifications: Sample PE PP Sample Type ASTM D638 Type IV Type I Grip separation rate 50mm/min 50 mm/min Distance between the grips 64 ± 5 mm 114 ± 1 mm Procedure: The testing machine is switched on and the program for determining the tensile properties is selected. Test samples, previously conditioned are used for testing. Two marks, 1.0,0.1 inches apart are on all the test samples at the center of the narrow portion of the sample. The width and thickness of the sample is measured to the nearest 0.001 mm and entered as data. The specimen is placed in the grips of the testing machine and the grips are tightened. The extensometer is then attached on the marks made on the sample. The initial load is tare. The speed of the testing machine is set and the machine is started. The load vs. extension curve of the specimen is recorded and the load and extension at the yield point and the point of rupture are noted. Tensile strength at yield (TYS), UTS, % elongation at break and % elongation at yield were directly displayed on the screen.
  • 50. [50] Calculations: Tensile modulus was calculated from the points on the stress-strain curve Tensile Modulus = Difference in stress/difference in corresponding Strain Tensile strength= force/ area Determination of Izod-Impact Strength of Plastics
  • 51. [51] Reference: ASTM D256 Machine Make: ResilImpactor Scope: This procedure is used to determine the impact strength of molded polymersamples. Summary: Notched specimens were subjected to impact with the help of a strikingpendulum hammer. Energy required for the sample to break was noted. Principle: Impact test indicates the energy required to break standard test specimens of a specified size. Energy lost by the pendulum during the breaking of the specimen was noted. The objective of the Izod Impact test is to measure the relative susceptibility of a standard test specimen to the pendulum-type impact load. The results are expressed in terms of energy consumed by the pendulum in order to break the specimen. The energy required to break a standard specimen is actually the sum of the energies needed to deform it, to initiate its fracture and to propagate the fracture across it, and the energy needed to throw the broken ends of the specimen. Apparatus:  Izod Impact Tester- CEAST (Resil-25)  Notch cutter with micrometer-screw gauge  Vernier Calipers- Accuracy 0.01 mm
  • 52. [52] Notchcutter Sample specification: Molded specimens have width between 3.17 and 12.7 mm. Thedepth of the plastic material remaining in the bar under the notch was 10.16 ± 0.05 mm and the distance of the notch from the end was between 31.5 to 32 mm. Analytical Procedure: 1. Hammer was selected along with the relevant range and installed by means of the range selector and the range switch. 2. The hammer was manually checked so as to ensure that it could be swung freely between the anvils.
  • 53. [53] 3. The hammer was initially released without the specimen and the value displayed indicated the amount of energy lost due to friction, wind age, and other factors. 4. This value was subtracted from each of the final sample readings. 5. The hammer was positioned on the anvil and the test samples (conditioned for 40 hours at 23±2 °C) were positioned and tightened with the torque wrench. 6. The hammer was then released and the breaking energy value on the digital display was noted down. 7. If the display exceeded 70% of the 2.75 J, then the hammer was replaced by a higher energy hammer and the above steps were repeated again. Calculation: Izod Impact Energy required to break the specimen – Air resistance Energy = Thickness Shrinkage Test Reference: ASTM D6289 Scope: This test method is intended to measure shrinkage from mold cavity to moldeddimensions of thermosetting plastics when molded by compression, injection, or transfer under specified conditions Principle: Plastic products have a tendency of shrinking when they once they are cooled down in the mold. This happens as the polymer coming from extruder is highly stressed and upon cooling the polymeric chains relieve their stress by orienting themselves randomly. This random orientation leads to shrinkage of polymer. The shrinkage is more in case of crystalline polymers as compared to amorphous polymers due to closer packing of chains.
  • 54. [54] Apparatus: (i) VernierCalipers Sample Specification: Standard mold dimension Procedure:  We take a standard circular molded specimen.  The diameter of the specimen is measured.  The diameter of the mold is measured.  The % change is reported as shrinkage Determination of Heat Deflection Temperature and Vicat SofteningPoint Reference: HDT: ASTM D 648 Vicat Softening: ASTM D1525
  • 55. [55] Scope: This procedure is used to determine the heat deflection temperature and Vicatsoftening point of the polymer. Summary: HDT of a polymer is the temperature at which a specimen deflects by 0.25 mm at a specified stress of 455kPa or 1820kPa. VICAT softening point is the temperature at which a flat ended needle of 1 mm2 surface area penetrates into the sample to a depth of 1 mm under 1 kg or 5 kg load. Principle: A molded, rectangular sample is placed in a temperature-controlled bath. The temperature of the bath is increased at a constant rate. Mechanical properties of polymers are temperature dependent. Both HDT and VST have their own purposes i.e. when the softening temperature of a polymer under stress is to be found the HDT test is used. However, when the softening temperature of a plastic without any stress (say when it is held by a support) is to be found VSP is used. Apparatus:  Specimen supports: 100 mm apart  Immersion bath: 6-station HDT-Vicat testing machine capable of providing a heating rate of 2±.0.2⁰C/ min. (make: CEAST)  Deflection measurement device: Accuracy = 0.01 mm  Weights: Set of weights to provide maximum fiber stress of 1820 kPa (264 psi) ± 2.5% or 455 kPa (66 psi) ± 2.5%  Working thermometer
  • 56. [56] Calibration: Working thermometer is calibrated as per standard method. Sample: Injection molded samples of the following dimensions are employed: Dimension Heat Distortion Temperature Vicat Softening Point Length 110 – 130 mm 1cm Depth 13 ± 0.13 mm 3 – 13 mm Width 3.2 mm 10mm (I) Heat Distortion Temperature (HDT) The test assembly was taken out from the bath and supported with a moving support. The test heads were fitted below the rods using the keys and the gauge block provided. According to the specimen dimensions the weight to be applied was calculated using the following formula: P=2bh2σ 3L P = weight to be applied in KN σ = Maximum fiber stress in the specimen b = width of the specimen in mm h = depth of the specimen in mm L = Support span in mm 134.2g (the combined weight of the testing head, loading rod assembly, dial gauge and cylindrical support fixed by the grub screw) were subtracted from the calculated weight and then this weight was made up with the auxiliary weights provided. The Bakelite nut
  • 57. [57] was loosened and the indicator was moved sideways. The weights were placed on the load rod and the indicator was returned to its original position and the Bakelite nut was tightened. Test samples, previously conditioned at 23±2 ⁰C for 48 hours were placed on the round supports. The loading unit was lowered by rotating the lever so that the HDT head rested on the specimen. Springs were inserted to avoid the specimen from dropping into the tank. The test assembly was then lowered by removing the moving support. The test start preset was subsequently adjusted to 23-25⁰C and the test end preset to a temperature 10-15⁰C higher than the expected HDT of the sample. The main switch was switched in and the heater switched on about 30 seconds later. The zero was adjusted on the indicator by loosening the block ring, after the heater switch started blinking (allowing 5 minutes as thermo station time) and the regulator screw was rotated such that the LED of the corresponding station was switched off. The heating was then started. When the required deflection was reached the instrument read the recorded value. Sample orientation in HDT
  • 58. [58] (ii) VICAT softening Point (VSP) The procedure was same as that of HDT except for the following: The Vicat test heads were fitted instead of the HDT heads. The weight was place on the Vicat head assembly totally amounting to 1000g (including the weight of the assembly i.e. 134.3g). The preset was testing started, set at least 50± 2 °C lower than the expected VSP of the sample. The deflection on the gauge is adjusted to 1 mm. The tester was then started. When the deflection on the gauge reached 1 mm, the instrument recorded that temperature as the VSP of the sample. Sample orientation in VST
  • 59. [59] Determination of Flexural Properties of Plastics Reference: ASTM D790 Scope: This procedure is used to determine the flexural properties of plastic materials Summary: A sample was placed on a support span and subjected to flexural stress by a loading nose and from the deflection data, flexural properties were determined. Principle: Plastic Products when subjected to flexural strain resist deformation. Flexuralstrength is the ability of the material to withstand bending forces applied perpendicular to its longitudinal axis. The stresses induced due to the flexural load are a combination of compressive and tensile stresses. Flexural properties are reported and calculated in terms of the maximum stress and strain that occur at the outside surface of the test bar. Many polymers do not break under flexure even after a large deflection that makes determination of the ultimate flexural strength impractical for many polymers. Apparatus: (i) Universal Testing Machine (Lloyd) (ii) Loading noses and supports (iii) VernierCalipers (Mitotoyo make)
  • 60. [60] Sample specification: Five samples of the following dimensions are tested: Length = 127 ± 5mm Width = 12.7 ± 1mm Thickness = 3.2 ± 0.4 m Support span length is 16 times the specimen thickness (Tolerance +4 or –2 mm) Analytical Procedure: An appropriate load cell (depending upon the type of material) is mounted on the machine. The loading nose is attached to the load cell and the supports to the stationary crosshead. The parallel alignment of the loading nose and supports is critical here. The machine is switched on and the following instrumental parameters are set: Speed of testing for the PP samples = 1.3 mm/min The appropriate program for flexural properties is selected. Previously conditioned (Maintained at 23 ± 2°C for 40 hours) test specimens are used. The width and thickness of the samples being tested are entered as data and the support span is set at 50 ± 2mm for PP. The specimen is entered on the supports. The experiment was performed and the load deflection curve was displayed and the program gave the flexural yield strength, modulus of elasticity, and 1% secant modulus directly. Calculation: Eb=L3F/ (4bh3Y) σf =3FL/ (2bh2) F: Force @ midpoint L: Span b: Width h: Thickness
  • 61. [61] Measurementof Colour of Plastics Reference: ASTM E313 Machine make: Color quest II, Hunterlab Scope: This test is used to measure the L*, a*, b* values of the given sample and also theYellowness Index, Whiteness Index, and color differences between the standard and sample. Sample specifications: Typically a 50 mm (2") or 100 mm (4") disk, although any flatsample that the specimen holder will grasp can be tested. Procedure:  The instrument is first standardized for color measurements and the instructions in the computer are followed to get the required values.  L* indicates brightness,  a* indicated greenness or redness,  b* indicates blueness or yellowness.  ΔE= ((∆L* )2 + (∆b* )2 + (∆a* )2 )  Standardization includes selection of specular reflectance mode with large area of view and UV filter out.
  • 62. [62]  The standard light trap is then inserted followed by the standard white and the standard gray tiles.  The test sample is inserted into the specimen holder, and the spectrophotometer takes the reading  The result obtained is in the form of L, a, b values, whiteness index (WI) and yellowness index (YI). Color analysis can be used to match adjacent parts molded from different materials, or to evaluate color change due to outdoor exposure. Visual color and Spectrophotometer readings can also be affected by surface texture, molding parameters, processing method, and viewing light sources. Gardener Impact Test Reference: ASTM D5420
  • 63. [63] Scope: This method covers the determination of the relative ranking of materialsaccording to the energy required to crack or break flat, rigid plastic specimens under various specified conditions of impact of a striker impacted by a falling weight. Summary: The procedure determine the energy (mass*gravity*height) that will cause50% of the specimens tested to fail called as mean failure energy (MFE). For low temperature cryo-test air chamber, condition the specimen for minimum 3 hours, once the required sub- zero temperature is reached, carry out the test accordingly. Principle: Energy of the falling weight at the instant of impact is kinetic energy which isequal to the energy used to raise the weight to the height of the drop. It is the potential energy possessed by the weight the instant it is released. Since the potential energy is (m x g x h), the guide tube can be marked with a liner scale showing the impact range of the instrument. Purpose of the impact testing is to find the amount of energy necessary to cause failure of specimen and to establish a standard for impact resistance, and test samples of the product against the established standard. Nature and extent of impact damage that constitutes failure must be established, variables such as material thickness, specimen shape, end use of the product are factors for evaluation. Once the failure point has defined, the actual test program can be developed (i.e. number of specimens to be impacted and what energy to use with each impact. Apparatus: Gardner impact tester consist of a Cast Al base, a slotted vertical guide tube,round nosed punch(up) and punch holder, 8 – lb. weight (3.6kgs), die and die support (anvil) and a cryo-test air chamber (low temperature) a separate attachment. Nose of the punch: - 0.600” (1.37cm) dia.; Inside diameterof the die: - 0.640” (1.64cm); Height of the guide tube: - 40” (101.6cm); Scale graduation: - 0 to 320inch-pound Specimen size: - Diameter = 100mm, Thickness = 3.2mm
  • 64. [64] Procedure:  Determine the number of specimens for each sample to be tested.  Place the test specimen on the tester anvil, after raising the weight and striker foot.  Be sure the specimen is flat against the specimen support plate before the striker foot is brought in contact with the top surface of the specimen.  Raise the weight in the tube to the desired impact value as shown on the scale, and release it so that the weight drops on the striker.  Remove the specimen and examine it to determine whether or not it has failed.  Permanent deformations alone are not considered failure, but note the extent of deformation (depth, area). In the first specimen fails, decrease the drop height while keeping the mass constant. If the first specimen does not fail, increase the drop height one increment and then testthe second specimen. In this manner, select the impact height for each test from the results observed with the specimen just previously tested. Test each specimen only once.
  • 65. [65] Environmental Stress Cracking Resistance (ESCR) Reference: ASTM D 1693 Scope: This procedure is used to determine the resistance of materials to cracking , when in contact with certain reagents and under mechanical stress. Summary: A set of specimens with controlled imperfections is immersed in a reactive liquid maintained at specified temperature . Time required for 50% of the specimens to fail is noted. Principle: Polymers when exposed to certain chemicals show physical failure at mechanical stresses that are much less than expected . ESCR quantifies resistance to such type of failure. Apparatus: 1. A jig for making a controlled imperfection in specimen of the dimensions,parallel to long edges of specimen and centered on one of the broad faces. 2. Specimen Holders 3. Test Tubes 4. Corks wrapped withaluminium foil. 5. Constant temperature bath maintained at 50±0.5⁰C 6. Bending clamp and transfer tool. 7. Thermometer.
  • 66. [66] Sample: Ten samples of following dimensions shall be cut from an Injection Molded or Compression Molded sheet; 38±2.5mm×13±0.08mm×3.15±0.15mm Procedure:  Give each specimen a controlled imperfection (notch) of 0.575±0.075mm depth on one surface after conditioning the test samples for 24 hours at 23⁰C before testing.  Bend the specimen using bending tool.Make sure that the notch is on the outer side. Transfer them to the specimen holder.  Insert holder in the test tube. Fill the tube with fresh reagent. Stopper the tube with foil wrapped cork and immediately place it in the constant temperature bath.  Temperature of water bath checked and set to 50⁰C with thermometer before starting the test.  Note the time required for 50% of the samples fail. Specular Gloss of Plastic Products Reference: ASTM D 523 Scope: This procedure is used to measure the specular gloss of plastics
  • 67. [67] Summary: The gloss meter is placed on the sample and the program for gloss measurement is run. Principle: Gloss value is determined from the ratio of incident light reflected from the surface of the sample. Apparatus: 3 Angle Hunter labsProgloss Sample:PE , PP & PVC Procedure: 1. The mode switch is first set for set up mode to prepare instrument for operation. Select all three angles for measurements (20⁰,60⁰&85⁰). 2. Place the film samples on a vacuum activated surface with a perfectly white background. 3. Then place the instrument on the sample. 4. Press the red key. 5. The gloss values are displayed on the instrument. Indentation Hardness of Plastics Reference:ASTM D 2240
  • 68. [68] Scope: This procedure is used to determine the Indentation Hardness of plastic materials. Summary:Needle tip of specified dimensions and geometry is made to penetrate into the polymer and the depth of penetration gives the level of the hardness of the material. Principle:Resistance to Indentation of the material is found with the help of a hard needle tip. Apparatus:Shore D Hardness tester – Blue steel make. Sample:The specimen shall be at least 6 mm thick. Two or more samples of lesser thickness can be plied up to achieve the desired thickness. Procedure: 1. Place the specimen on hard, even and horizontal surface. 2. Hold the tester vertically on the specimen. While holding, the pressure foot should be parallel to the surface of the specimen. 3. Apply the pressure with hand without shock so that the casing is fully pressed against the specimen. 4. The readings are to be taken after about 3seconds after the contact between the surface of the specimen and the pressure foot is made. 5. Three tests should be carried out on each specimen and the mean value of these 3 readings should be rounded off to a shore number.
  • 69. [69] 6. PROCESSING DIVISION Various Processing Facilities at PARC MOLDING  Injection Molding Machines  Blow Molding Machine  Compression Molding Machine  Rotational Molding Machine EXTRUSION  Blown Film Extrusion Plant  Tubular Quenched PP Plant  PVC Pipe Extrusion Plant COMPOUNDING  Single screw compounding extruder  Twin screw compounding extruder  Tumbler Mixer  High speed mixer  Granulator  Pulverizing Unit
  • 70. [70] Brief Descriptionof Processing Machines: 1.InjectionMolding Principle:  In the process the material is plasticized and melted by the heat added through barrel heaters and friction due to shearing.  Then the material is injected through nozzle into a relatively cold mold to get the desired shape.  After the shape is formed, the ejector pins push the specimen out of the mold.  The process is used to make solid articles like caps, plugs, bobbins, furniture& house ware products, industrial & automobile parts etc.
  • 71. [71] Machines available: Klockner Windsor FR 110 Klockner Windsor SP 180 (Family mold machine) Arburg 320C All-rounder (ASTM standards) Parts of a molded specimen:
  • 72. [72] Injection molding machine detailed specification Specifications Units DGP Klockner Arburg Windsor Windsor All rounder SP180 FR110 320 C 500-100 Screw diameter mm 50 45 30 Injection pressure Bar 1800 1900 1550 L/D - 18:1 19:1 20:1 Clamping force KN 1800 1100 500 Min mold height mm 350 250 200 Max mold height mm 900 700 200 The theory of injection molding can be reduced to four simple individual steps: Plasticizing, Injection, Cooling, and Ejection. Each of those steps is distinct from theothers and correct control of each is essential to success of the total process. The steps are as follows:  Plasticizing - describes the conversion of the polymer material from its normal hard granular form at room temperatures, to the melt necessary for injection at its correct melt temperature.  Injection - is the stage during which this melt is introduced into a mold to completely fill a cavity or cavities.  Cooling - is the action of removing heat from the melt to convert it from melt back to its original rigid state. As the material cools, it also shrinks.  Ejection - is the removal of the cooled, molded part from the mold cavity and from any cores or inserts.
  • 73. [73] Advantages of Injection Molding  High Production rates  Design flexibility  Repeatability within tolerances  Can process a wide range of materials  Relatively low labor  Very good finishing of parts  Minimum scrap losses Limitations of Injection Molding  High initial equipment investment  High start-up and running costs possible  Part must be designed for effective molding  Accurate cost prediction for molding job is difficult Application: PARC uses injection molding machine for manufacturing of spiral flow testsample, tensile testing sample, flexural testing sample, Izod testing sample, disc shape sample and color testing sample
  • 74. [74] 2.Blown Film Plant Blown film extrusion process and salient features: The majority of polymer films are manufactured by film blowing.Plastic melt is extruded through an annular slit die, usually vertically, to form a thin walled tube. Air is introduced via a hole in the centre of the die to blow up the tube like a balloon. Mounted on top of the die, a high-speed air ring blows onto the hot film to cool it. The tube of film then continues upwards, continually cooling, until it passes through nip rolls where the tube is flattened to create what is known as a ' lay-flat' tube of film. This lay-flat or collapsed tube is then taken back down the extrusion ' tower' via more rollers. On higher output lines, the air inside the bubble is also exchanged. This is known as IBS (Internal Bubble Cooling). The lay-flat film is then either kept as such or the edges of the lay-flat are slit off to produce two flat film sheets and wound up onto reels. If kept as lay-flat, the tube of film is made into bags by sealing across the width of film and cutting or perforating to make each bag. This is done either in line with the blown film process or at a later stage. Typically, the expansion ratio between die and blown tube of film would be 1.5 to 4 times the die diameter. The drawdown between the melt wall thickness and the cooled film thickness occurs in both radial and longitudinal directions and is easily controlled by changing the volume of air inside the bubble and by altering the haul off speed. This gives blown film a better balance of properties than traditional cast or extruded film which is drawn down along the extrusion direction only Tubular films show excellent toughness as they are a mild form of biaxial orientation. Tubular lines produce products which can be easily made in to bags, edge-trimming can be frequently avoided and a film width is easily changed simply by blowing a bigger tube.
  • 75. [75] Machine Specifications: LDPE/LLDPE plant HM/HDPE plant Make Rajoo Engineers Limited Rajoo Engineers Limited Model No RELL-4040 LAB REHD-4040 LAB Screw diameter 40mm 40mm Screw length 1200mm 1200mm L/D ratio 30:1 30:1 Screw speed range 10-100rpm 10-100rpm Die diameter 110mm spiral type 75mm spiral type Die gap 1.2, 1.5,1.8mm 0.8,1.2mm Parts of a tubular blown film plant:  Extruder Extruder comprisesof hopper, barrel/screw and dies. Fig shows the component of a modernextruder.
  • 76. [76]  Hopper: All the extruder has an opening in the barrel at the driven end, through which the plastic graduals enter the extruder. The hopper, a simple sheet –metal enclosure, is mounted above the opening and holds about a hopper’s capacity material. Hopper is provided with heating system, if the material has to be preheated before entering the extruder.  Screw: This is the heart of the extruder. Screw conveys the molten polymer to the opening of the die after properly homogenizing the molten polymer. There is considerable variation in the design of the screw for various materials, the most important variable being the depth of the channels. Despite much desire for universal screw, it is advisable to use a different design for each material to achieve the best results. PE screw is designed to have shallow channels, sudden compression and long metering join. Screw diameter: 20-250mm,CR: 2.5-3: 1,L/D: 24-33: 1  Mixing Heads The metering section of a standard is not a good mixer. Smooth laminar flow patterns are established in the channel, which do not mix dissimilar elements in the melt. Mixing devices are frequently installed in screw to disrupt these flow patterns and improve melt homogenization.  Breaker plate/screen pack:
  • 77. [77] Breaker plate with screen packs inserted is kept in the adapter, which connect the dies and extruder barrel. This assembly has several functions. 1. Arrest the rotational flow of the melt and convert into axial flow. 2. Improves melt homogeneity by splitting and recombining the flow. 3. Improves mixing by increasing backpressure. 4. Remove any contamination and unmelt. Screen packs are made up of series of screen of differing mesh. With the coarse screen placed against the breaker plate to support the finer screens.  Die: The dies used for tubular extrusion are centre-fed or side-fed. Centre fed dies are better as all the points on the lip are equidistant from the feed-entry point. This gives uniform flow and uniform thickness. The spider arms of the centre-fed die always divide the flow into separate paths which must come together and weld completely before leaving the die or else weld lines are formed, which are lines of weakness. Die gap is also a very important parameter as too small die gap may cause increase in die resistance and cause overheating in extruder and reduce output rate. And if the gap is too large resistance becomes so less that weld lines may appear. For the processing of PE, a die with spiral is used as shown in the figure. As the plastic flows from the entry point it spirals around the mandrel section of the die. The land depth between the spiral section and wall increases as the wall increases as the material progress through the die, .as a result, the distribution around the die periphery made uniform in order to control the gauge of extruded tube.
  • 78. [78]  Corona treatment: Many plastics, such as polyethylene and polypropylene, have chemically inert and nonporous surfaces with low surface tensions causing them to be non-receptive to bonding with printing inks, coatings, and adhesives. Although results are invisible to the naked eye, surface treating modifies surfaces to improve adhesion. Corona treatment (sometimes referred to as air plasma) is a surface modification technique that uses a low temperature corona discharge plasma to impart changes in the properties of a surface. The corona plasma is generated by the application of high voltage to sharp electrode tips which forms plasma at the ends of the sharp tips. A linear array of electrodes is often used to create a curtain of corona plasma. Parameterof blown film extrusion:  Temperature: A lower temperature is needed for tubular film (e.g., 170oC for PE of 2.0 MFI) since the cooling capacity often limits the output as a higher temperature may mean lower output. The other possible disadvantages of higher temperature are: Increased blocking Reduced bubble stability Promotion of decomposition in the die with resultant impaired appearance Possible bubble breaks.  Blow up Ratio: The blow-up ratio is defined as the ratio of the bubble diameter to the die diameter and is one of the important factors to determine the final film size and properties. A high blow ratio means that a smaller and less expensive die is needed for any given film size, but a high blow-up ratio yields the strongest film as the increased stretching has an orientation effect. However, high blow-up ratio also encourages bubble instability, requires more drawdown and magnifies all the imperfections in the die, thus a compromise blow-up ratio is needed. Bubble instability is a major problem in tubular film extrusion as it produces wrinkles, thickness variation, and “walking” of the film along the windup roll.
  • 79. [79] The blow-up ratio is determined in advance, when a die is selected to do a given job. Die gap also has significant effect on the film properties. Increasing die gap will increase machine direction orientation which then results in lower machine direction tear strength, lower machine elongation, improved transverse direction tear strength, & improved machine direction tensile strength.  Frost-Line Height: The area of change, where the viscous fluid is changed to solid film, is called the "frost- line" because here the hardening film first appears "frosty" in some films. An irregularity here indicates that something is wrong with the filmmaking process, and this may result in poor film. Increasing FLH will decrease machine direction orientation with slower quenching rates resulting in higher film crystallanity. Optical properties will reach an optimum & then start to decrease. The frost line can be raised or lowered by means of extruder output, take-off speed, and the volume of cooling air blown against the bubble. When the screw speed goes up the distance between the die and the frost line is increased; when more cooling air is blown against the bubble, the frost line drops. The frost line can be change by adjusting the cooling-air volume. The frost line in the bubble can effectively be raised by means of a so- called annealing chamber (or "chimney") placed between the die and the air ring.
  • 80. [80] Start-up & shutdown of the process: The first minutes of the production always yield scrap material as the system much yield equilibrium. The die bolts may have to adjust to get the uniform thickness, and the extrusion speed and the winder speeds must be balanced to get the desired overall thickness. The process is started quite cool in order to minimize formation of decomposed material in the system, which could subsequently contaminate the film and cause streaks. Once the screw is turning and plastic is running through the die, the temperatures are raise to normal values. As the tube is being formed, air is introduced through the die in small amounts to keep the tube slightly blown. After the threading is complete, more air is blown in to bring the bubble to the desired size. Care must be taken to keep the die faces clear of the molten resin as this may later be decomposed and cause die lines. Shut down is one of the most vital steps in blown film extrusion in order to avoid damageto the head and the die. Such decomposition can be caused by the degradation, oxidation of hot plastic in contact with air, or by both. For all materials degradation and decomposition may produce hardened bits of material which can break off and lodge in the die lips. Such bits form weld lines which are not only unsightly but are also lines of weakness. When the film line is shut down, material is kept moving as the zones cool to about 130oC (LDPE) then the extruder is stopped and the die and head are cooled with air as fast as possible to inhibit decomposition. Polyethylene is often left in the extruder barrel as well as inside the die to prevent air from entering the system and oxidizing any bits of plastic left. Likewise, before start-up the die is not left hot any longer than absolutely necessary.  Winding: Winding is the final operation in the film manufacturing process. In blown film, because there are two sides of the tube, two winders are requires. Film is wound on a spiral wound paper core which is supported by the winding shaft. This shaft is attached to the winder at the ends. The core is secured to the shaft using either a cable lock mechanisms or lugs which are pneumatically protruded from the shaft surface. Two basics techniques used for winding films are: driving the winding roll from thecentre using a driven wind up shaft, or applying a driven roll directly to the surface of the winding roll of the film.
  • 81. [81] Centre winders: Centre winders have the advantage in that the tension in the film can becontrolled as the diameter of the film increases. This is done by sensing the diameter of the film & decreasing the tension of the film as the diameter of the film increases. Tension is controlled by controlling the differences in speed between the nip rolls & the winding rolls Tension can also be controlled by a pneumatically activated idler roll that applies pressure on the film web. This roll is called the dancer since it pivots up& down as it maintains the constant pressure in the web. With the higher force required to move the dancer roll, more tension will be applied to the film. Decreasing the tension as the roll diameter grows up, helps to keep the film roll form winding too tight. Tight winding will cause the film to block & make it sensitive to shrink as it cools on the toll. If winding is too tight, the shrinking film will become distorted & difficult to print or laminate. Surface winders: Surface windersare easy to operate since they don’t have the complexmethods of tension control. In case of surface winders, tension is applied to the film by winding the film faster than the nip rolls. However, this does not allow for the finer adjustments in tension as in a dancer-bar arrangement. Surface winders rely on the pressure of the drive roll to control the roll hardness. Therefore, because some pressure is required to drive the roll, they tend to wind harder rolls than centre winders. However, because there is not the variation in tension & because there is no dancer rolls, some processors believe that surface winders can wind flatter rolls than centre winders. It is difficult, however, to change the direction of the wind on a surface winder compared to the centre winder.
  • 82. [82] 3.CompressionMolding Machine Machine Specifications: Compression cylinder: 6 inch diameter Make: Carver Inc. LMV 50H-15-C (50T) Process: The process of compression molding may be simply described by reference toFig. Two-piece mold provides a cavity in the shape of the desired molded article. The mold is heated, and an appropriate amount of molding material is loaded into the lower half of the mold. The two parts of the mold are brought together under pressure. The compound, softened by heat, is thereby molded into a continuous mass having the shape of the cavity. The mass then must be hardened, so that it can be removed without distortion when the mold is opened. Advantages Advantages ofCompression Molding  Mold costs tend to be lower because the molds are simpler.  Low volume jobs are better suited to compression molding because start up is usually quicker, easier and generates less scrap.  Cycle times for compression molded is more than injection molding
  • 83. [83] Disadvantages of Compression Molding  Compression molded parts usually are more labor intensive. Preforms must be made, heated and loaded into the mold by an operator or a robot.  Across parting line dimensions can be more difficult to control.  It can be more difficult to mold metal inserts into the parts without flashing them. Application: PARC uses compression molding for manufacturing of thermoplasticsheet (testing sample are punch from sheet) NOTE: FOR PVC FOR FIRST 1 MIN IT IS OPERATED UNDER 0 BAR PRESSURE, FOR NEXT 1 MIN IT IS 15 BAR PRESSURE AND FOR NEXT 2 MINUTES IT IS 30 BAR PRESSURE. FOR PE, PP FOR THE FIRST 1 MINUTES IT IS 0 BAR PRESSURE, FOR NEXT 2 MINUTES IT IS 15 BAR PRESSURE AND FOR THE NEXT 3 MINUTES IT IS 30 BAR PRESSURE. COOLING IS DONE AT 70 °C FOR PVC AND 50°C FOR PP,PE.
  • 84. [84] 4.RotationalMolding Make: Fixotron 50K2 Rotational molding (often referred to as Rotomolding or Rotomolding) is a process used for producing hollow plastic products. By using additional post-molding operations, complex components can be produced enabling the process to compete effectively with other molding and extrusion practices. Rotational molding differs from other processing methods in that the heating, melting, shaping, and cooling stages all occur after the polymer is placed in the mold, therefore no external pressure is applied during forming. Advantages of RotationalMolding  Economically produced large products  Minimum design constraints  Stress-free products  No polymer weld lines  Comparatively low mold costs
  • 85. [85] Disadvantages of Rotational Molding  The manufacturing times are long  The choice of molding materials is limited  The material costs are relatively high due to the need for special additive packages and the fact that the material must be ground to a fine powder  Some geometrical features (such as ribs) are difficult to mold Process:The Rotational Molding process is essentially split into four operations: Charging Mold:A pre-determined amount of polymer powder is placed in the mold. With the powder loaded, the mold is closed, locked and loaded into the oven. The powder can be pre-compounded to the desired color. Heating & Fusion:Once inside the oven, the mold is rotated around two axes, tumbling the powder – the process is not a centrifugal one. The speed of rotation is relatively slow, less than 20 rev/min. The ovens are heated by convection, conduction and, in some cases, radiation. As the mold becomes hotter the powder begins to melt and stick to the inner walls of the mold. As the powder melts, it gradually builds up an even coating over the entire surface. Cooling: When the melt has been consolidated to the desired level, the mold is cooled either by air, water or a combination of both. The polymer solidifies to the desired shape. Unloading/Demolding: When the polymer has cooled sufficiently to retain its shape and be easily handled, the mold is opened and the product removed. At this point powder can once again be placed in the mold and the cycle repeated.
  • 86. [86] Typical Materials Used LDPE, LLDPE,PP,PVC Rotation Molded Kyak
  • 87. [87] 6.ExtrusionBlow Molding Make: Klockner Windsor India Ltd, Model : KBM-5 Blow molding is a manufacturing process by which hollow plastic parts are formed. Principle: The blow molding process begins with melting down the plastic and forming it into a parison or in the case of injection and injection stretch blow molding (ISB) a preform. The parison is a tube-like piece of plastic with a hole in one end through which compressed air can pass.The parison is then clamped into a mold and air is blown into it. The air pressure then pushes the plastic out to match the mold. Once the plastic has cooled and hardened the mold opens up and the part is ejected. Process: In Extrusion Blow Molding (EBM), plastic is melted and extruded into a hollow tube (a parison). This parison is then captured by closing it into a cooled metal mold. Air is then blown into the parison, inflating it into the shape of the hollow bottle, container, or part. After the plastic has cooled sufficiently, the mold is opened and the part is ejected.Continuous and Intermittent are two variations of Extrusion Blow Molding. In Continuous Extrusion Blow Molding the parison is extruded continuously and the individual parts are cut off by a suitable knife. In Intermittent blow molding there are two processes: straight intermittent is similar to injection molding whereby the screw turns, then stops and pushes the melt out. With the accumulator method, an accumulator gathers melted plastic and when the previous mold has cooled and enough plastic has accumulated, a rod pushes the melted plastic and forms the parison. In this case the screw may turn continuously or intermittently.[3] with continuous extrusion the weight of the
  • 88. [88] parison drags the parison and makes calibrating the wall thickness difficult. The accumulator head or reciprocating screw methods use hydraulic systems to push the parison out quickly reducing the effect of the weight and allowing precise control over the wall thickness by adjusting the die gap with a parison programming device Advantages of extrusion blow molding  High rate of production  Low tooling cost Disadvantages of extrusion blow molding  High scrap rate  A limited control over wall thickness  Difficulty of trimming away excess plastic.
  • 89. [89] COMPOUNDING 1. Single screw compounding extruder: Make: Thermo Electron Corporation Machine Specifications:  Screw diameter: 19mm  L/D ratio: 25:1  Compression ratio- 3:1  Maximum screw speed: 200rpm Overview: Single-screw laboratory extruder deliver reliable data captured during the extrusion process to verify process parameters (speed, energy, temperature) for unknown materials or to manufacture smaller quantities of a new polymer (as strands, sheets, pellets, blown films) during research and development. The extruder is equipped with measuring ports for melt pressure and melts temperature to study the process parameters along the extruder barrels. A die can be connected to the end of the extruder barrel to form the polymer melt as strand or film. Special rheological dies allow the determination of shear- and elongational viscosity at defined shear rates.. Standard feeders for pellets and special feeding systems for powders, pastes,liquids are there. Application: Single screw compounding extruder is use for checking the decrease inproperties of material after no. of passes. 2.Twinscrew compounding extruder: Type: Co-rotating twin screw extruder Make: Omega 30 STEER
  • 90. [90] Process:In the extrusion of plastics, raw compound material in the form of nurdles (small beads, often called resin) is gravity fed from a top mounted hopper into the barrel of the extruder. Additives such as colorants and UV inhibitors (in either liquid or pellet form) are often used and can be mixed into the resin prior to arriving at the hopper. The material enters through the feed throat (an opening near the rear of the barrel) and comes into contact with the screw. The rotating screw (normally turning at up to 120 rpm) forces the plastic beads forward into the heated barrel. The desired extrusion temperature is rarely equal to the set temperature of the barrel due to viscous heating and other effects. In most processes, a heating profile is set for the barrel in which three or more independent PID- controlled heater zones gradually increase the temperature of the barrel from the rear (where the plastic enters) to the front. This allows the plastic beads to melt gradually as they are pushed through the barrel and lowers the risk of overheating which may cause degradation in the polymer. Extra heat is contributed by the intense pressure and friction taking place inside the barrel. In fact, if an extrusion line is running certain materials fast enough, the heaters can be shut off and the melt temperature maintained by pressure and friction alone inside the barrel. In most extruders, cooling fans are present to keep the temperature below a set value if too much heat is generated. If forced air cooling proves insufficient then cast-in cooling jackets are employed. At the front of the barrel, the molten plastic leaves the screw and travels through a screen pack to remove any contaminants in the melt. The screens are reinforced by a breaker plate (a thick metal puck with many holes drilled through it) since the pressure at this point can
  • 91. [91] exceed 5,000 psi (34 MPa). The screen pack/breaker plate assembly also serves to create back pressure in the barrel. Back pressure is required for uniform melting and proper mixing of the polymer, and how much pressure is generated can be "tweaked" by varying screen pack composition (the number of screens, their wire weave size, and other parameters). This breaker plate and screen pack combination also does the function of converting "rotational memory" of the molten plastic into "longitudinal memory". After passing through the breaker plate molten plastic enters the die. The die is what gives the final product its profile and must be designed so that the molten plastic evenly flows from a cylindrical profile, to the product's profile shape. Uneven flow at this stage can produce a product with unwanted residual stresses at certain points in the profile which can cause warping upon cooling. Almost any shape imaginable can be created so long as it is a continuous profile. The product must now be cooled and this is usually achieved by pulling the extrudate through a water bath. Machine Specifications:  Screw diameter: 30mm  L/D ratio- 40:1  Screw speed range: 0-1200 rpm  Throughput : 50-100 kg/hour Application :Twin screw extruder is use mainly for PP compounding and PVC 3.Pulverizing Unit: The pulveriser unit is capable of pulverizing polymer granules 500μm to 1.75mm. Make: Fixopan Machines Pvt Ltd. Model no: FP14-SGL Capacity: 40-60 kg per hour Grinding teeth: Multiple (Over 250)
  • 92. [92] 4.Tumbler Mixer: Capacity –40kg of pellets Application : It is use for the physical mixing of granules 5.High Speed Mixer: Make: KOLSITE Specifications: Capacity: 40kg Speed: 1440rpm Application :Used for PVC compounding. 6. Granulator: Make: PIMCO Specifications: 5hp, 3.7kW induction motor. Application: Use for making granules
  • 93. [93] References  ASTM Standards Handbook volume 08.01, 08.02, 08.03 , 08.04  Polymer Science and Technology- V. Gowarikar  http://ulprospector.com  BRYDSON, J. A. (1999) Plastics Materials (7th edition)