A seminar on

        Industrial Aspect
           of Rheology


                 Presented by
                 Modh Sudipkumar c.
                 PA /2010 /11
Introduction


Rheology is Responsible for any formulation, production, appearance, usage, and
finally affect stability

Affects final cost of product

Class I recalls of Fentanyl Reservoir patches from Innovator and generic
manufacturers

In short………
If a material is pumped, sprayed, extended, extruded, molded, coated, mixed,
chewed, swallowed, rubbed, transported, stored, heated, cooled, aged …
RHEOLOGY is important ….!!


                                    sudip kumar modh                           2
contents
Viscometer vs. Rheometer

Types of the viscometer used in industry

Characteristics

Application of viscometer in stability and evaluation

Rheology: A Rapid Screening Method for Testing Stability

Latest types of viscometers and Rheometers




                                 sudip kumar modh          3
Viscometer vs. Rheometer


• Viscometer: instrument that measures:
viscosity over a limited shear rate range

• Rheometer: instrument that measures:

• Viscosity over a wide range of shear rates, and…
• Viscoelasticity of fluids, semi-solids and solids




http://pioneer.netserv.chula.ac.th/~sanongn1/course.html

                                                           sudip kumar modh   4
Types of the viscometer used in industry:
Capillary viscometer
Falling sphere viscometer
Cup and bob viscometer
cone and plate viscometer

How will you choose appropriate viscometer?
•Newtonian types of fluids shear rate directly proportional to shear stress
•Instrument are operated at single shear rate can be used
   -Capillary viscometer
   -Falling sphere viscometer
 but these give erroneous result

•Non Newtonian types of fluids shear rate not directly proportional to shear stress
•Instrument are operated at variety of shear rate can be used
   -Cup and bob viscometer
   -cone and plate viscometer


                                        sudip kumar modh                              5
Characteristics:
Capillary viscometer
Exp Ostwald viscometer
Based on poiseuille’s equation
According to US pharmacopeia capillary apparatus used for high viscous
methyl cellulose type of solution

Falling sphere viscometer
Exp hoeppler viscometer

Cup and bob viscometer
Exp Couette type
    McMichael searle type
    Roto viscometer
    Brookfield viscometer(rotational type of viscometer)

cone and plate viscometer
Exp ferranti-shirley


                                sudip kumar modh                         6
Application of viscometer in stability and evaluation:

1) Polaxomer vehicles
Used in tear solution for treating “dry eye syndrome “
For evaluation computer controlled couette viscometer is used

2) Suppositories
Release and absorption is depend on rectal temperature,
Brookfield viscometer is used study characteristic of triglycerides base at various
temperature

3) Emulsion
Stabilized with triethanolamine stearate at various temperature
Brookfield viscometer is used

4) cosmetic sticks
Ferranti-shirley cone plate viscometer used




   Physical pharmacy by martin page 581-582
                                              sudip kumar modh                        7
5) Tablet Excipient

  Microcrystalline cellulose is used as granulating agent
  Mixture torque rheometer is used to measure torque changes as water is added

  6)Lamination *

  process of lamination various stages
  a) softening point of the resin -resin starts to soften and flow as elastic material
  drops of viscosity (~107 poise down to 100 to 5000 poise)

  b) material is most fluid, and reaction rates start to increase as viscosity starts to build
  as the resin starts to gel.
  at gel point tan delta is one
  parallel plate Rheometer+ is used




*Focus on Rheology By Arlon, Materials for Electronics, Inc   .
                                                                  sudip kumar modh               8
+parallel plate Rheometer:

upper plate is attached to transducer to measure torque resulting from
strain upon the sample

system computer compares material stress to input strain and
determines tan delta

or phase angle along with the storage and loss modulus components




                               sudip kumar modh                          9
7)Suspensions

     Settling of particles by Brookfield viscometer fitted with helipath attachment
     Consists of rotating T bar spindle
     Dial reads resistance at various levels of suspension

     8)Ointment

     Consistency measured by Burrell severs Rheometer with helipath attachment
     Ointment is loaded into a cylinder and extruded with measured force
     Amount extruded is measurement of consistency

     9)Aerosol

     Viscosity is measured by Brookfield viscometer

     10)Paste

     capillary extrusion viscometer for the viscosity measurement of fish protein paste

Journal compilation © 2008 Wiley Periodicals, Inc.

                                                     sudip kumar modh                      10
capillary extrusion viscometer




                                 sudip kumar modh   11
Rheology: A Rapid Screening Method for Testing Stability



•   To understand rheology of viscoelastic fluids, frequency dependence of their G'
    and G" material functions to be measured




     shear storage modulus G'

      shear loss modulus G“




                                    sudip kumar modh                                  12
http://pioneer.netserv.chula.ac.th/~sanongn1/course.html


sudip kumar modh                                               13
An oscillatory (sinusoidal)
                                                                                                G’
   deformation (stress or strain)
   is applied to a sample.


   the material response
                                                                                                G”
   (strain or stress) is measured.


   The phase angle δ, or phase
   shift, between the deformation
   and response is measured.

                                                           shear storage modulus G'
                                                             shear loss modulus G“

ideal solid, elastic       Tan delta= 0º            high viscosity
Newtonian fluid           Tan delta= 90º            low viscosity



                                     http://pioneer.netserv.chula.ac.th/~sanongn1/course.html

                                      sudip kumar modh                                               14
• The ratio of G"/G', known as tandelta is predictive parameter for studying
  the storage stability of suspensions



• single rheological test can rapidly predict the stability of a drug suspension
  by monitoring the value of a well-defined parameter tan delta#




               Tan delta= G"/G'
                                                                   Tan delta




•   *http://www.pharmaceutical-int.com/article/rapid-screening-methods.html
•   # http://ciks.cbt.nist.gov/~garbocz/SP946/node11.htm

                                                      sudip kumar modh         15
Latest types of viscometers and Rheometers

1)HAAKE RheoStress 6000 (2007)1
Universal Rheometer
variety of temperature control units
temperatures ranging from -80 up to 500°C

2) Brookfield viscometes2




                                               2 Achieving the Basics in Viscosity Measurement to Comply with 21CFR Part 11   16
1© 2007/10 Thermo Fisher Scientific Inc.   ·   By Len Thibodeau Rheometer
Significance of Helipath Stand


  substances with yield values unsuitable for viscosity or consistency            measurements
  with rotational viscometers
  rotating spindle, be it cylinder, disc, or paddle, will create channel
  Produce negligible and meaningless torque


  The Brookfield Helipath™ Stand is designed to slowly lower or raise rotating T-bar spindle
   By always cutting into fresh material, the problem of channelling or separating is
  eliminated




                                                                sudip kumar modh                  17
http://www.brookfieldengineering.com/products/accessories/helipath-stand.asp
3) Interfacial Shear Rheometer




                                                    KSV NIMA
                                 sudip kumar modh              18
Interfacial Shear Rheometer

Viscoelastic films relationships are nonlinear
intermediate between purely viscous and purely elastic responses in industry and in
biologicals
To define product stability in different industries such as food, petrochemical, cosmetics,
and pharmaceuticals

Application:

Prediction of emulsion, froth and foam stability
Determination of thin film structure
Examination of phase transitions
Real time monitoring of surface reactions
Continuous monitoring of molecule adsorption into interfaces
                                        sudip kumar modh                                 19
4) STRESSTECH




           Where flow characteristic of a material determines its processibility, performance,
           and/or consumer acceptance.


Rheological instrumentation for the characterization of polymers-BY STEVEN M. COLO,

                                                                  sudip kumar modh               20
I never did anything worth doing by accident, nor did any of
my inventions come by accident; they came by work
                                 - Thomas Alva Edison

I'm a great believer in luck, and I find, the harder I work, the
more I have of it.
                                    -Thomas Jefferson




                                   Thank u………
                            sudip kumar modh                       21

Rheology pdf

  • 1.
    A seminar on Industrial Aspect of Rheology Presented by Modh Sudipkumar c. PA /2010 /11
  • 2.
    Introduction Rheology is Responsiblefor any formulation, production, appearance, usage, and finally affect stability Affects final cost of product Class I recalls of Fentanyl Reservoir patches from Innovator and generic manufacturers In short……… If a material is pumped, sprayed, extended, extruded, molded, coated, mixed, chewed, swallowed, rubbed, transported, stored, heated, cooled, aged … RHEOLOGY is important ….!! sudip kumar modh 2
  • 3.
    contents Viscometer vs. Rheometer Typesof the viscometer used in industry Characteristics Application of viscometer in stability and evaluation Rheology: A Rapid Screening Method for Testing Stability Latest types of viscometers and Rheometers sudip kumar modh 3
  • 4.
    Viscometer vs. Rheometer •Viscometer: instrument that measures: viscosity over a limited shear rate range • Rheometer: instrument that measures: • Viscosity over a wide range of shear rates, and… • Viscoelasticity of fluids, semi-solids and solids http://pioneer.netserv.chula.ac.th/~sanongn1/course.html sudip kumar modh 4
  • 5.
    Types of theviscometer used in industry: Capillary viscometer Falling sphere viscometer Cup and bob viscometer cone and plate viscometer How will you choose appropriate viscometer? •Newtonian types of fluids shear rate directly proportional to shear stress •Instrument are operated at single shear rate can be used -Capillary viscometer -Falling sphere viscometer but these give erroneous result •Non Newtonian types of fluids shear rate not directly proportional to shear stress •Instrument are operated at variety of shear rate can be used -Cup and bob viscometer -cone and plate viscometer sudip kumar modh 5
  • 6.
    Characteristics: Capillary viscometer Exp Ostwaldviscometer Based on poiseuille’s equation According to US pharmacopeia capillary apparatus used for high viscous methyl cellulose type of solution Falling sphere viscometer Exp hoeppler viscometer Cup and bob viscometer Exp Couette type McMichael searle type Roto viscometer Brookfield viscometer(rotational type of viscometer) cone and plate viscometer Exp ferranti-shirley sudip kumar modh 6
  • 7.
    Application of viscometerin stability and evaluation: 1) Polaxomer vehicles Used in tear solution for treating “dry eye syndrome “ For evaluation computer controlled couette viscometer is used 2) Suppositories Release and absorption is depend on rectal temperature, Brookfield viscometer is used study characteristic of triglycerides base at various temperature 3) Emulsion Stabilized with triethanolamine stearate at various temperature Brookfield viscometer is used 4) cosmetic sticks Ferranti-shirley cone plate viscometer used Physical pharmacy by martin page 581-582 sudip kumar modh 7
  • 8.
    5) Tablet Excipient Microcrystalline cellulose is used as granulating agent Mixture torque rheometer is used to measure torque changes as water is added 6)Lamination * process of lamination various stages a) softening point of the resin -resin starts to soften and flow as elastic material drops of viscosity (~107 poise down to 100 to 5000 poise) b) material is most fluid, and reaction rates start to increase as viscosity starts to build as the resin starts to gel. at gel point tan delta is one parallel plate Rheometer+ is used *Focus on Rheology By Arlon, Materials for Electronics, Inc . sudip kumar modh 8
  • 9.
    +parallel plate Rheometer: upperplate is attached to transducer to measure torque resulting from strain upon the sample system computer compares material stress to input strain and determines tan delta or phase angle along with the storage and loss modulus components sudip kumar modh 9
  • 10.
    7)Suspensions Settling of particles by Brookfield viscometer fitted with helipath attachment Consists of rotating T bar spindle Dial reads resistance at various levels of suspension 8)Ointment Consistency measured by Burrell severs Rheometer with helipath attachment Ointment is loaded into a cylinder and extruded with measured force Amount extruded is measurement of consistency 9)Aerosol Viscosity is measured by Brookfield viscometer 10)Paste capillary extrusion viscometer for the viscosity measurement of fish protein paste Journal compilation © 2008 Wiley Periodicals, Inc. sudip kumar modh 10
  • 11.
  • 12.
    Rheology: A RapidScreening Method for Testing Stability • To understand rheology of viscoelastic fluids, frequency dependence of their G' and G" material functions to be measured shear storage modulus G' shear loss modulus G“ sudip kumar modh 12
  • 13.
  • 14.
    An oscillatory (sinusoidal) G’ deformation (stress or strain) is applied to a sample. the material response G” (strain or stress) is measured. The phase angle δ, or phase shift, between the deformation and response is measured. shear storage modulus G' shear loss modulus G“ ideal solid, elastic Tan delta= 0º high viscosity Newtonian fluid Tan delta= 90º low viscosity http://pioneer.netserv.chula.ac.th/~sanongn1/course.html sudip kumar modh 14
  • 15.
    • The ratioof G"/G', known as tandelta is predictive parameter for studying the storage stability of suspensions • single rheological test can rapidly predict the stability of a drug suspension by monitoring the value of a well-defined parameter tan delta# Tan delta= G"/G' Tan delta • *http://www.pharmaceutical-int.com/article/rapid-screening-methods.html • # http://ciks.cbt.nist.gov/~garbocz/SP946/node11.htm sudip kumar modh 15
  • 16.
    Latest types ofviscometers and Rheometers 1)HAAKE RheoStress 6000 (2007)1 Universal Rheometer variety of temperature control units temperatures ranging from -80 up to 500°C 2) Brookfield viscometes2 2 Achieving the Basics in Viscosity Measurement to Comply with 21CFR Part 11 16 1© 2007/10 Thermo Fisher Scientific Inc. · By Len Thibodeau Rheometer
  • 17.
    Significance of HelipathStand substances with yield values unsuitable for viscosity or consistency measurements with rotational viscometers rotating spindle, be it cylinder, disc, or paddle, will create channel Produce negligible and meaningless torque The Brookfield Helipath™ Stand is designed to slowly lower or raise rotating T-bar spindle  By always cutting into fresh material, the problem of channelling or separating is eliminated sudip kumar modh 17 http://www.brookfieldengineering.com/products/accessories/helipath-stand.asp
  • 18.
    3) Interfacial ShearRheometer KSV NIMA sudip kumar modh 18
  • 19.
    Interfacial Shear Rheometer Viscoelasticfilms relationships are nonlinear intermediate between purely viscous and purely elastic responses in industry and in biologicals To define product stability in different industries such as food, petrochemical, cosmetics, and pharmaceuticals Application: Prediction of emulsion, froth and foam stability Determination of thin film structure Examination of phase transitions Real time monitoring of surface reactions Continuous monitoring of molecule adsorption into interfaces sudip kumar modh 19
  • 20.
    4) STRESSTECH Where flow characteristic of a material determines its processibility, performance, and/or consumer acceptance. Rheological instrumentation for the characterization of polymers-BY STEVEN M. COLO, sudip kumar modh 20
  • 21.
    I never didanything worth doing by accident, nor did any of my inventions come by accident; they came by work - Thomas Alva Edison I'm a great believer in luck, and I find, the harder I work, the more I have of it. -Thomas Jefferson Thank u……… sudip kumar modh 21