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FT4 Powder Rheometer Literature

1. (NEW) FT4 Powder Rheometer Brochure

By introducing a dynamic method of measuring powder flow properties, Freeman Technology has made possible the direct comparison of flowability data for different powders. A program of continuing development makes today’s FT4 Powder Rheometer a sophisticated universal powder testing system that is helping address a very broad range of powder processing challenges.

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Conference Papers

1. The Influence of Ambient Moisture on Powder Flow Characteristics

Presented at Partec 2013, 22-25 April 2013

Tim Freeman1,Brian Armstrong1, Katrina Brockbank1, Jamie Clayton1
1Freeman Technology, Tewkesbury

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2. Advanced Powder Characterisation Techniques for Process and Product Development

Presented at 8th International Materials Technology Conference and Exhibition, 9-12 July 2012

Tim Freeman1, Brian Armstrong1
1Freeman Technology, Tewkesbury

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3. Will a change in the weather shut my process down? – The evaluation of the effect of humidity on the flow properties of powders

Presented at 8th International Materials Technology Conference and Exhibition, 9-12 July 2012

Tim Freeman1, Brian Armstrong1
1Freeman Technology, Tewkesbury

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4. Consolidation of powders - how to evaluate the effect of vibration induced powder compaction through flow property measurement

Presented at PSA 2011 - September 5th to 7th 2011

Tim Freeman1, Brian Armstrong1
1Freeman Technology, Tewkesbury

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5. The Influence of Powder Flow Properties on the Filling of Dies and Capsules

Presented at PSA 2011 - September 5th to 7th 2011

Tim Freeman1, Jamie Clayton1, Xiaowei Fu1
1Freeman Technology, Tewkesbury

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6. The Development of a Compact Uniaxial Tester

Presented at PSA 2011 - September 5th to 7th 2011

Reg Freeman1, Xiaowei Fu1
1Freeman Technology, Tewkesbury

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7. Capsule Filling Performance of Powdered Formulations in Relation to Flow Characteristics

Presented at the UK-China Particle Technology Forum III - July 3rd to 6th 2011

Tim Freeman1, Xiaowei Fu1, V. Moolchandani1, S.W. Hoag2
1Freeman Technology, Welland
2School of Pharmacy, University of Maryland, Baltimore, MD21201, USA

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8. The Characterisation of Powders and Bulk Materials - a Multivariate Approach using Dynamic, Shear and Bulk Property Measurements

Presented at Bulk Solids India 2011 - April 6th to 8th 2011

Tim Freeman1, Reg Freeman1, Brian Armstrong1
1Freeman Technology, Welland

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9. The Characterisation of Powder Properties in the Pharmaceutical Industry - The Implications of QBD for Solids Dose Manufacture

Presented at Bulk Solids India 2011 - April 6th to 8th 2011

Tim Freeman1, Reg Freeman1, Brian Armstrong1
1Freeman Technology, Welland

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10. The characterisation of bulk material properties – the need for a multivariate approach

Presented at Bulk Solids Europe 2010 - September 9th to 10th 2010

Tim Freeman1, Reg Freeman1, Brian Armstrong1
Freeman Technology, Welland

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11. Getting to grips with Quality by Design

Presented at INTERPHEX 2010 - 20 to 22 April 2010

Tim Freeman
Freeman Technology, Welland

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12. The application of advanced powder characterisation techniques to pharmaceutical Quality by Design protocols

Presented at WCPT6 2010 - April 27th 2010, T1202: Food/Pharma/Life Science Applications

Jamie Clayton1, Tim Freeman1, Reg Freeman1, Brian Armstrong1
1Freeman Technology, Welland

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13. The influence of dry powder coating methods, including mechanofusion, on the flow properties of inhalable grades of lactose monohydrate

Presented at WCPT6 2010 - April 27th 2010, 11:50, T0311: Aerosols - Particle Production and Functionalization

David Morton1, Reg Freeman2, Tony Qi Zhou1, Peter Stewart1, Brian Armstrong2, Tim Freeman2, Ian Larson1
1Monash University, Melbourne,
2Freeman Technology, Welland

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14. Evaluation of dry powder blending using Positron Emission Tomography and the relationship between powder bulk properties and process parameters

Presented at WCPT6 2010 - April 29th 2010, T0933: Bulk Solids - Pneumatic- Conveying & Mixing

Brian Armstrong1, Jonathan Seville2, Mike Adams3, David Parker3, Xiangfeng Fan3, Trevor Page4, Reg Freeman1
1Freeman Technology, Welland,
2Uni of Warwick, Coventry,
3Uni of Birmingham, Birmingham,
4GEA Pharma Systems, Eastleigh

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15. Improving the flow and dispersion properties of several micronized drug powders using an innovative dry coating approach

Presented at WCPT6 2010 - April 29th 2010, T0312: Aerosols - Particle Production and Functionalization

Tony Qi Zhou1, David Morton1, Li Qu1, Brian Armstrong2, Peter Stewart1, Ian Larson1
1Monash University, Parkville,
2Freeman Technology, Welland

[Abstract not available]

16. Abstract: Combining modern powder characterisation techniques with real processing experience

PharmSciFair - June 8-12, 2009 - Nice - France

T. Freeman, Freeman Technology, Welland, UK (Presenting on June 9)

Powder processing represents a major part of pharmaceutical manufacturing and yet few predictive tools exist, relying instead on the skill of the individual operator. There is surprisingly little information regarding the factors that affect powder processing and what can be measured to predict potential problems and answer questions like "will this batch compress well?"

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17. Measuring powder characteristics relating to forced flow into confined spaces using a universal powder tester

Particulate Systems Analysis 2008 - Stratford-upon-Avon, UK

Tim Freeman and Xiaowei Fu

Very cohesive powders can behave like a fluid when pressurised or subjected to forced flow. Such powders may extrude like toothpaste, whereas normally free flowing powders will resist forced flow. This study focuses on understanding these characteristics and determining how they correlate with the known powder flowability parameters that describe dynamic flow behaviour, shear properties and bulk properties including permeability and compressibility.

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18. Characterisation of Powder Bulk, Dynamic Flow and Shear Properties in relation to Die Filling

2008 World Congress On Powder Metallurgy & Particulate Materials - Washington, DC

R E Freeman and X Fu

The bulk, dynamic flow and shear properties of tungsten, aluminium and two types of glass beads are investigated and correlated with the ability to fill a die. The results show how effectiveness of die filling correlates well with many powder properties and how entrained air is a critical factor.

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19. Volumetric dosing efficiency in relation to the bulk, flow and shear properties of powders

Presented at PARTEC 2007, Nuremberg, Germany - March 2007.

Reg Freeman & James Cooke

This study examines the efficiency of volumetric dosing for a number of different powders and shows how the results correlate with the powder properties measured using the FT4 Powder Rheometer.

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20. Measuring shear properties and normal stresses generated within a rotational shear cell for consolidated and non-consolidated powders

The French National Symposium on Powder Science & Technology - Ecole des Mines, d’Albi, May 2007

R E Freeman, J R Cooke and L C R Schneider

A study of 5 powders when consolidated and non-consolidated using conventional shear cell methodology and a new shear cell control methodology to investigate the stresses automatically generated normal to the shear plane as shearing proceeds.

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21. Flowability of Powders and the Effects of Flow Additives

World Congress on Particle Technology, Orlando - April 2006

R E Freeman and J R Cooke

A study of how the bulk and flow properties of potato starch and corn starch are affected by small amounts of fumed silica flow additive (AEROSIL® 200). A powder rheometer was used to measure dynamic flow properties as well as shear properties, including their yield loci when pre-consolidated and their shear strength (cohesion) at near zero consolidation stress.

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22. Measuring the flow properties of consolidated, conditioned and aerated powders - a comparative study using a powder rheometer and a rotational shear cell

Particulate Systems Analysis 2005 - Stratford-upon-Avon, UK

Reg Freeman

A comprehensive study of the flow properties of 6 powder types comparing the rheometer flow energy measurements with shear properties data.

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23. A Study of the Flow Properties of Toners in Relation to Physical & Environmental Factors

NIP19 International Conference on Digital Printing Technologies - September 2003

Reg Freeman

A study of the flow properties of a range of magnetic toners produced from a common base in relation to three physical variables - the milling method, the type and amount of flow additive and to a limited extent, particle size.

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24. The Importance of Air Content on the Rheology of Powders - an Empirical Study using the FT4 Powder Rheometer

Particulate Systems Analysis 2003, Harrogate, UK - August 2003

A study of how the rheological properties of powders are greatly influenced by the presence or absence of air.

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25. Powder Rheology as a Tool to Determine Optimum Blending Time

AAPS 2012

Overview of powder characterisation needs in pharmaceutical industry. Flow rate sensitivity of spray dried and hydrous lactose. How aeration and consolidation affects flow performance. How magnesium stearate affects the flowability of lactose. Characterising wet granulated blends of Avicel/lactose.

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26. Flowability of Powders - an Empirical Approach

International Conference on Powder and Bulk Solids Handling - IMechE - June 2000

Reviews flowability issues, describes the FT4 operating principle and includes case studies concerning flow rate, compaction, attrition and segregation of some powders.

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Conference Posters

Presented at DDL 2012

1. (NEW) The Use of Powder Rheology to Investigate the Effect of Carrier Properties and Lactose Fines on DPI Performance In-vitro

Presented atDDL 2012

1 Marina Maxwell1, 2 Mark Parry, 2 Mark Hammond , 1 Ben Forbes
1 1Department of Pharmacy, King’s College London, 2 2Melbourn Scientific Limited, Melbourn, UK

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Presented at Partec 2013

1. (NEW) Powder Rheology of Steel Powders for Additive Manufacturing

01/10/2013

O. Lyckfeldt1
1Swerea IVF AB, Sweden

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2. Quantifying the effect of caking through powder rheometry

Presented at Partec 2013, 22-25 April 2013

Tim Freeman1, Brian Armstrong1, Katrina Brockbank1
1Freeman Technology, Tewkesbury

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3. Investigation of the influence of atomic layer deposition coatings on powder rheology

Presented at Partec 2013, 22-25 April 2013

Tim Freeman1, Xiaowei Fu1, John Yin1, David M. King2, Dean S. Dinair3
1Freeman Technology, Tewkesbury, 2 PneumatiCoat Technologies, Westminster, CO, USA, 3 Lum Americas, Boulder, CO, USA

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Presented at AAPS 2012

1. Utility of Powder Rheology in Selection of Flow Aid and Lubricant in Dry Granulations

Presented at AAPS 2012 Annual Meeting and Exposition 14 - 18 October 2012

S. V. Kamath, A. Ekpe, P. Nayak, J. Meisel, E. First
Bayer HealthCare, Consumer Care Division, Morristown, New Jersey

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2. Powder Rheology as a Tool to Determine Optimum Blending Time

Presented at AAPS 2012 Annual Meeting and Exposition 14 - 18 October 2012

S. V. Kamath, A. Ekpe, P. Nayak, J. Meisel, E. First
Bayer HealthCare, Consumer Care Division, Morristown, New Jersey

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3. Quantifying the effect of ambient moisture on powder flow properties

Presented at AAPS 2012 Annual Meeting and Exposition 14 - 18 October 2012

Tim Freeman, B Armstrong, K Brockbank, J Yin
Freeman Technology, Tewkesbury

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Presented at Drug Delivery to the Lungs (DDL) 2011

1. Powder rheology analysis as tool for the characterisation of interactive powder mixtures

Presented at Drug Delivery to the Lungs (DDL) 22 - 7 - 9 December 2011

E Cordts & H Steckel
Department of Pharmaceutics and Biopharmaceutics, Christian Albrecht University Kiel Grasweg 9a, 24118 Kiel, Germany

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Presented at Powder Flow 2011

1. The impact of loaded drug dose and the surface roughness of the coarse lactose carrier to the fluidisation characteristics of dry powder inhaler formulations

Presented at Powder Flow 2011 - 6 December 2011

Hanne Kinnunen1, Jag Shur1, Gerald Hebbink2 and Robert Price1
1Pharmaceutical Surface Science Research Group, Department of Pharmacy and Pharmacology, University of Bath, Bath, BA2 7AY, UK 2DFE Pharma, Borculo, Netherlands

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Presented at AAPS 2011

1. Powder Rheology as a Tool to Predict Impact of Different Sources of Excipient on Tablet Compression

Presented at AAPS 2011 - 24 to 27 October 2011

F. Opawale, K. Landgren, L. Wagner, S. Suralik, P. Nayak, J. Miesel and E. First
Bayer HealthCare, Consumer Care Division, Morristown, New Jersey

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2. Measuring more meaningful powder flow properties – the limitations of ‘Compressibility Index’ data

Presented at AAPS 2011 - 24 to 27 October 2011

Tim Freeman1, Brian Armstrong1
1Freeman Technology, Welland

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Presented at 5th International Granulation Conference

1. The characterisation of the physical properties of wet masses

Presented at 5th International Granulation Conference - 20 to 22 June 2011

Reg Freeman1, Tim Freeman1, Brian Armstrong1
1Freeman Technology, Welland

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Presented at AAPS 2010

1. The Relationship Between Powder Flow Properties and Dosing Machine Geometry for Pharmaceutical Die Filling Applications

Presented at AAPS 2010 - 14 to 18 November 2010

Xiaowei Fu1, Tim Freeman1, Graham Shirley2, Brian Armstrong1, Jeremy Baker2
1Freeman Technology, Welland
2Molins ITCM, Coventry

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2. Novel Applications of Traditional Lubricants Using a Dry Particle Coating Technique to Improve the Functionality of Cohesive Drug or Excipient Powders

Presented at AAPS 2010 - 14 to 18 November 2010

Qi Tony Zhou1, Li Qu1, Ian Larson1 , Brian Armstrong2, Peter J Stewart1, and David A V Morton1
1Drug Delivery, Disposition and Dynamics, Monash Institute of Pharmaceutical Sciences, Monash University, Australia
2Freeman Technology, Worcestershire, UK

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3. To develop and evaluate new methodology for excipients compatibility together with api’s using rheological and thermal tools

Presented at AAPS 2010 - 14 to 18 November 2010

Maitri R. Trivedi, Rutesh H. Dave, Ph.D.
Division of Pharmaceutical Sciences, Arnold & Marie Schwartz College of Pharmacy, Long Island University,Brooklyn, NY

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Presented at UK PharmSci 2010

1. The Application of QbD to Pharmaceutical Powder Processing

Presented at UK PharmSci 2010 - 1 to 3 September 2010

Tim Freeman1
1Freeman Technology, Welland

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Presented at WCPT6 2010

1. The characterisation of the physical properties of wet masses

Presented at WCPT6 2010 - Poster #165 - 26 to 29 April 2010

Jamie Clayton, Tim Freeman, Reg Freeman, Xiaowei Fu, Brian Armstrong
Freeman Technology, Welland

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2. The quantification of particle shape and size using image analysis and its effect on the flow properties of various forms of lactose

Presented at WCPT6 2010 - Poster #166 - 26 to 29 April 2010

Xiaowei Fu1, Deborah Huck2, Ulf Willen2, Lisa Makein2, Reg Freeman1, Tim Freeman1, Jamie Clayton1
1Freeman Technology, Welland,
2Malvern Instruments, Malvern

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Presented at AAPS 2009

1. An Investigation into the Wall Friction Angle of a Range of Low Friction Materials Used in the Manufacture of Pharmaceutical Processing Equipment

Presented at AAPS 2009

Tim Freeman1, Xiaowei Fu1, Brian Armstrong1 and Karlheinz Seyfang2
1Freeman Technology, Welland
2Harro Höfliger Verpackungsmaschinen GmbH

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2. The Effect of Fluid-Bed Granulation Process on the Physical and Mechanical Properties of Powders and Granules

Presented at AAPS 2009

Kevin H. Yoo, Zafar Ali, Chimanlall Goolcharran, Krishnendu Ghosh, Ruchi Shah, Jovita Tauro and Arwinder Nagi
Pfizer Pharmaceutical Development Centre, Pfizer, Pearl River, NY 10965 (USA)

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3. Determining Endpoint for Wet Granulation Using Rheological and Effusivity Measurement

Presented at AAPS 2009

H.H. Patel, S. Wu, R.Pugh, T. Freeman, B.Armstrong and R.H. Dave
Long Island University; Covidien/Mallinckrodt; C-THERM Technologies; Freeman Technology

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4. Flow and Compaction Characteristics of A Direct Compression Formulation (1)

Presented at AAPS 2009

Dong Yang, Jennifer Q. Liang, Kevin Yoo, Iqbal Bhuiyan, Narendra R. Desai, Syed M. Shah
Pfizer Pharmaceutical Development; Pfizer Product Development, Pfizer, Pearl River, NY 10965 (USA)

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5. Flow and Compaction Characteristics of A Direct Compression Formulation (2)

Presented at AAPS 2009

Dong Yang, John Yin, Iqbal Bhuiyan, Narendra R. Desai, Syed M. Shah
Pfizer Formulation Development; Freeman Technology

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6. To Measure the Additive Effect of Magnesium Stearate and Stear-O-Wet on Wet Granulation

Presented at AAPS 2009

P. C. Okoye, S.H. Wu, R.Pugh, J. Yin, T. Freeman, R.H. Dave
Long Island University; Covidien; C-THERM Technologies; Freeman Technology; Kolmar Labs Group

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Presented at ISAM 2009

1. Characterisation of the Flow Properties of a Novel Spray Dried Tobramycin Powder For Dry Powder Inhalation (DPI)

Presented at ISAM 2009

Francesca Buttini, Brian Armstrong, Tim Freeman, Mark Saunders, Paolo Colombo
Department of Pharmacy, University of Parma; Freeman Technology; Synectix Pharmaceutical Solutions

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Presented at AAPS 2008

1. A Critical Evaluation of Two Commercial Shear Cell Instruments for Determining the Flow Properties of Powders

Presented at AAPS 2008

Paul D. Jager and Frank M. Etzler
Boehringer-Ingelheim Pharmaceuticals, Inc., Pharmaceutical R&D, 900 Ridgebury Road, P.O. Box 368, Ridgefield, CT 06877 (USA)

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2. Development of a Material Sparing Method to Determine Powder Permeability to Air

Presented at AAPS 2008

Glenn Carlson, Bruno Hancock
Pfizer Global Research & Development, Groton Laboratories, Pfizer Inc, Groton, CT 06340

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3. Discrete Element Simulations of a Powder Rheometer: A Study of Particle Property Effects

Presented at AAPS 2008

Rahul Bharadwaj, William Ketterhagen and Bruno C Hancock
Pfizer Global Research & Development, Groton Laboratories, Pfizer Inc, Groton, CT 06340

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4. Evaluating the Impact of Particle Size Reduction Techniques on the Powder Properties of Pharmaceutical Solids

Presented at AAPS 2008

Yang Guo, Neera Jain, Jimin Xiong, Ada Eluwa and Suresh Babu
Synta Pharmaceuticals Corporation, Lexington, MA 02421

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5. Evaluation of Stear-O-WetTM as a Lubricant for Making Tablets

Presented at AAPS 2008

Stephen H. Wu, Brian Cheng, Dan Ramlose and Gary Nichols
Covidien / Mallinckrodt Pharmaceuticals, 385 Webster Groves, MO 63119

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6. Effects of Lubricants at Different Operating Speeds in the Tableting Process on Quality of Tablets Containing High-loading of Acetaminophen

Presented at AAPS 2008

Brian Cheng, Dan Ramlose, Gary Nichols and Stephen Wu
Covidien / Mallinckrodt Pharmaceuticals, 385 Webster Groves, MO 63119

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7. Evaluation of Lubricants for Making Tablets Containing High-loading of Acetaminophen

Presented at AAPS 2008

Brian Cheng and Stephen Wu
Covidien / Mallinckrodt Pharmaceuticals, 385 Webster Groves, MO 63119

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Presented at DDL 2008

1. Characterisation and Functionality of Anhydrous Inhalation Lactose

Presented at DDL19 Edinburgh 2008

C Pitchayajittipong1, J Shur1, J S Kaerger2, S Edge3 & R Price1
1Pharmaceutical Surface Science Research Group, University of Bath, Bath, UK
1Aeropharm GmbH, Rudolstadt, Germany
1Novartis Pharma AG, Basel, Switzerland

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White Papers

1. Using powder characterisation methods to assess blending behaviour

Tim Freeman and Brian Armstrong, Freeman Technology, June 2012

Blending a mixture of powders to homogeneity is a critical step in many manufacturing processes. Making uniform tablets, for example, relies on the homogeneous dispersion of active ingredients, often in small quantities, with excipients such as binders and disintegrants to form a suitable feed blend for the press. Similarly, in industries as diverse as food production and metal powder processing, homogeneity is crucial to defining product characteristics: flavour or colour in foods for instance, or the mechanical properties of a sintered metal component.

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2. Quantifying the impact of humidity on powder properties

Brian Armstrong and Jamie Clayton, Freeman Technology, April 2012

Of the many factors that influence powder behaviour, moisture, or humidity, is perhaps one of the most instantly recognised. Adding even small amounts of water to a powder can transform its properties.

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3. Powder characterisation for inhaled drug delivery

Tim Freeman, Director of Operations, Freeman Technology, May 2011

Manipulating and controlling powder behaviour is a demanding but essential element of pharmaceutical manufacturing. The development and production of dry powder inhalers (DPIs) exemplifies and highlights the difficulties faced, arguably presenting the industry with its toughest powder engineering challenge. Fine by necessity, to ensure deposition in the lung, dry powder formulations tend to be highly cohesive and difficult to handle. The need to understand the aerosolisation processes that ensure successful drug delivery adds an additional and substantial layer of complexity.

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4. Introducing a new solution for uniaxial powder testing

Tim Freeman, Director of Operations, Freeman Technology, October 2010

For many years the routine use of uniaxial testing for powder characterization has been compromised by the practical difficulties associated with its application. Steps taken to tackle these issues have resulted in the development of a new solution that makes it easier to obtain high quality data with this simple technique. Correlations with rotational shear cell data are excellent.

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5. Understanding powder caking

Tim Freeman, Director of Operations, Freeman Technology, July 2010

Caking, or unwanted agglomeration, presents major problems in powder processing, capable of making even those powders that are normally free-flowing and easily processable, challenging. Its control depends on understanding the influence of, and closely managing, environmental conditions. Modern powder testers help make the link between different variables and the tendency towards caking, providing useful information for the determination of an optimal environment.

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6. Analytical techniques for successful cosmetic compact manufacture

Tim Freeman, Freeman Technology, Welland, Worcs, UK. April 2010

Formulating and manufacturing cosmetic compacts to deliver market-leading performance characteristics requires a high degree of powder processing expertise. This paper considers the measurement of some of the most appropriate properties of both the formulation and the finished product.

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7. Choosing the best construction material for powder processing equipment

Tim Freeman, Freeman Technology, Welland, Worcs, UK. November 2009

Selecting the best material of construction is a crucial part of the plant design process, the aim being to balance performance and cost to best advantage. For powder processors, choosing a material that eases flow can pay dividends throughout the lifetime of the plant, but there is limited data on which to base this decision. A recent study by Freeman Technology highlights the role of the FT4 universal powder tester for such studies and provides some valuable comparative data for a wide range of commercially available materials and finishes.

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8. Implementing QbD: Powder characterization for design space definition

Tim Freeman, Freeman Technology, Welland, Worcs, UK. September 2009

For those seeking to adopt a Quality by Design approach to pharmaceutical development and manufacture, effective definition of the ‘design space’ is a key activity. This paper considers the role of modern powder testers such as the FT4 from Freeman Technology, within this context.

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9. Better wet granulation: development, scale-up and manufacture

Tim Freeman, Freeman Technology, Welland, Worcs, UK. July 2009

Wet granulation is a common unit operation in the pharmaceutical industry yet accurate endpoint detection remains a challenge. Here we examine the contribution that dynamic powder rheometry can make, highlighting its ability to detect the transition from wet mass to granulate with the required sensitivity. Quantification of this transition point, with a measure that is independent of process scale, accelerates development and scale-up and improves manufacture.

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10. Assessing powder stability

Reg Freeman, Freeman Technology, Welland, Worcs, UK

Some powders appear inherently variable, sensitive to the slightest change in conditions, while others are much more forgiving. Stability testing assesses this critical aspect of powder behavior.

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11. Developing powder processing expertise for the implementation of Quality by Design

Reg Freeman, Freeman Technology, Welland, Worcs, UK

Powder characterization techniques have improved significantly in recent decades, developing well beyond the simplistic methods traditionally used. This paper examines the changes in approach encouraged by QbD and the contribution modern powder testers can make.

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12. Intelligent powder processing

Reg Freeman, Freeman Technology, Welland, Worcs, UK

Do you completely understand all aspects of your powder process, formulating, specifying and manufacturing product in an optimal manner on the basis of underlying knowledge? Or do you, like many other pharmaceutical producers, rely heavily on the experience of formulators, supervisors and operators running sub-optimally but well enough to get by? Here we discuss how your experience can be fully exploited by correlating process observations with measurable powder parameters. This approach brings improved understanding, which in turn leads to cost reductions and a lowering of the risks associated with change.

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13. Modern Tools for Hopper design

Tim Freeman, Freeman Technology, Welland, Worcs, UK

Describes the application of the recently launched Hopper Design Software package for the FT4 Powder Rheometer. Drawing on the characterization capabilities of this universal powder tester, the new software improves access to well-established hopper design methodologies, speeding up and simplifying compilation and interpretation of the required data.

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14. Predicting the in-process behaviour of powders

Tim Freeman, Freeman Technology, Welland, Worcs, UK

A knowledge of which existing formulations do or do not process well, in conjunction with comprehensive powder characterization, enables the processing behavior of new powders to be predicted before they are introduced into a plant.

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15. Investigating the confined and unconfined flow behavior of powders

Reg Freeman, Freeman Technology, Welland, Worcs, UK

This paper examines the mechanisms associated with powder flow, contrasting the way in which materials behave when confined and unconfined. The different extrusion behaviour of cohesive and non-cohesive powders and their ability to switch from ‘good’ to ‘bad’ flowability is described.

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16. Characterizing powders for optimized pharmaceutical processing

Tim Freeman, Freeman Technology, Welland, Worcs, UK

A review of powder characterisation and some of the ways in which manufacturers can use the data produced to cost effectively increase the efficiency of production processes and more closely control product quality.

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17. Validation of shear testing using the FT4 Powder Rheometer and limestone powder CRM 116

James Cooke and Tim Freeman, Freeman Technology, Welland, Worcs, UK. May 2005

This study validates shear tests carried out using an FT4 Powder Rheometer fitted with a shear cell using a standard CRM 116 limestone powder. Yield loci at the four pre-shear normal stresses as laid down in the standard were derived and shown to be within 5% of the standard and well within it's uncertainty tolerance.

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18. Developing multicolored powder primers at PSA Peugeot Citroën

Claire Pichon and Nicolas Guillot - PSA Peugeot Citroën
Cyril Conesa - PSA Peugeot Citroën and Compiègne University of Technology
Pierre Guigon and Khashayar Saleh - Compiègne University of Technology. March 2005

This article discusses how France-based PSA Peugeot Citroën developed multi-coloured polyester-epoxy powder primers for use on cars produced at it's newly renovated Mulhouse paint shop, one of the first lines in Europe to use coloured powder primer coats. The article explains how two key measuring devices including the FT4 Powder Rheometer helped the automaker overcome powder flowability problems.

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Articles

1. Solid Dosage Form Manufacturing

Published in European Pharmaceutical Review - October 2012

Erik Skibsted, Principal Scientist -Novo Nordisk

The Quality by Design (QbD) paradigm is being introduced to more and more R&D and manufacturing units in the pharmaceutical industry.

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2. The Attraction And Challenge Of Continuous Manufacturing

Published in Pharmaceutical Online Magazine - Spring 2012

Jamie Clayton, Operations Manager - Freeman Technology

Moves toward greater processing efficiency and continuous manufacturing are intertwined. The practices associated with quality by design (QbD) and defining the design space are being applied to bring knowledge-led practice to batch process development.

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3. Controlling the impact of humidity

Published in Process Industry Informer - September 2012

Tim Freeman, Managing Director, Brian Armstrong, Powder Technologist, Jamie Clayton, Operations Manager - Freeman Technology

The properties of dry and damp powders can be as dissimilar as those of chalk and cheese. The uptake of even small amounts of moisture can transform powder properties, making humidity and its impact a critical issue for powder processors.

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4. The Next Wave of PAT: Advancing Process Understanding to Process Control

Published in AAPS News Magazine - September 2012

Tim Freeman, Freeman Technology, Zhenqi Shi Lilly and David E Reed, Research Laboratory, George L Read Pfizer, Worldwide Research & Development

The Food and Drug Administration (FDA) issued the Process Analytical Technology (PAT) guidance in September 2004,1 which stated, “PAT is defined as a system for designing, analyzing, and controlling manufacturing through timely measurements (i.e., during processing) of critical quality and performance attributes of raw and in-process materials and processes with the goal of ensuring final product quality.” Per FDA’s definition, PAT is composed of three components: designing, analyzing, and controlling.

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5. Optimising Tabletting Processes with Quality by Design

Published in Pharmaceutical Technology Europe Digital - May 2012

Tim Freeman, Managing Director Freeman Technology & Carl Levoguer, Product Marketing Manager (Laser, Particle Sizing and Imaging), Malvern Instruments

We all know the importance of particle size distribution when it comes to processing the perfect tablet, but there are also many other factors that must be considered. Authors from Freeman Technology and Malvern Instruments step forward to give you their insight on enhancing tabletting with quality by design and analytical techniques.

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6. Dynamic Testing Methods Pinpoint Parameters Suitable for Further Insight into In-process Powder Behavior

Published in Processing Magazine - April 2012

Jamie Clayton, Freeman Technology & Michael Mayer, AZO GmbH + Co. KG.

Use of a Powder Rheometer has enhanced powder-testing capabilities at the research center of AZO GmbH + Co. KG, Osterburken, Germany. Gains include not only dynamic powder testing, but also fully automated shear- and bulk-property measurement.

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7. The Attraction and Challenge of Continuous Manufacture

Published in Pharmaceutical Online - May 2012

Jamie Clayton, Freeman Technology.

Across the pharmaceutical industry, continuous manufacturing is seen to have valuable benefits. Global efforts are transforming the efficiency of the pharmaceutical industry, with continuous manufacturing viewed as a strategy for success.

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8. Effective Powder Processing Across The Pharma Life Cycle

Published in Pharmaceutical Online - Spring 2011

Tim Freeman, Freeman Technology.

The key to success in any market is finding the right balance between performance and cost. When dealing with commodity products, brand differentiation tends to be low, with cost arguments dominating and forcing lean, highly efficient manufacturing. In more specialized areas, including pharmaceuticals, profit is often derived from unique patented performance that commands a premium price, well above the cost of production. Historically, this position has shielded pharmaceutical manufacturers from many of the rigors faced by, for example, bulk chemical producers, where the legacy is relatively inefficient production. In the prevailing economic and regulatory climate this is rapidly becoming unsustainable and significant pharmaceutical industry resources are being pushed towards process understanding and establishing better manufacturing practices.

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9. Powder Characterisation for Efficient Processing: Moving to a New Manufacturing Model

Published in Innovations in Pharmaceutical Technology - June 2011

Tim Freeman, Freeman Technology.

The pharmaceutical industry is currently focusing significant resources into the area of process development and design. An aspiration is to emulate, at least to some extent, the manufacturing gains already achieved in other sectors where efficiencies as high as 99 per cent are already a daily reality. For manufacturers the cost base is a key driver, but the regulatory perspective brings other benefits into focus. Fully defined, well-understood products, manufactured in efficiently monitored, closely controlled processes present a relatively low risk. For those who can demonstrate such practice there is the potential for a lighter regulatory touch, to complement financial gains.

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10. Modern Pharmaceuticals interview: Tim Freeman discusses the importance of efficient powder processing, and how the FT4 can help solve challenges in formulation and product development

Published in Modern Pharmaceuticals - April 2011

Chandreyee Bhaumik & Tim Freeman, Freeman Technology.

Efficient powder processing is essential for the production of many different materials including foodstuffs, cosmetics, metal powders, minerals and, of course, pharmaceutical formulations. However, when compared with handling liquids and gases, the less predictable nature of powder behaviour complicates formulation, plant design and day-to-day operation alike. This makes the development and production of quality products challenging. During the past 10 years Freeman Technology has worked with powder processors from all areas of industry and academia in order to understand the difficulties that they face. In this interview, Tim Freeman discusses Freeman Technology’s approach to characterising powders, and the unique benefits the FT4 Powder Rheometer provides in measuring process-relevant powder behaviour.

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11. 10 years in powders. Making powders and processes fit

Published in Processing Magazine - March 2011

Tim Freeman, Director of Operations at Freeman Technology

The last decade has been a pivotal one for powder testing. Leaving behind the simplistic idea of trying to define the complexities of powders with just a single number, developers of powder testing instrumentation have combined powerful complementary techniques to bring to industry the toolkit it needs to tackle the considerable challenges of solids processing. Key to the development of new methodologies has been the recognition that they must reflect the environment to which a powder is subject within manufacturing processes.

Significant efforts have been made to understand how the powder properties measured by modern universal powder testers relate to in-process behavior. This ‘work in progress’ holds the key to a better powder processing future across all industry sectors.With reproducible, relevant powder characterization now a reality, there is an opportunity to understand how to formulate and tailor powder blends, and select and design process equipment, that have the compatibility necessary for long-term, efficient manufacturing.

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12. Powder testing techniques for QbD

Published in International Labmate - September 2010

Quality by Design, the new way of working enshrined in guidance from the FDA, raises the profile of pharmaceutical manufacturing and process development. More specifically it demands the detailed consideration of processing issues during the earlier stages of development. This poses the question of how best to inject the necessary expertise from the outset. Analytical tools that ease communication across the traditional formulation/process development/production boundaries can help.

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13. Powder Testing for Better Formulation

Published in Innovations in Pharmaceutical Technology - Issue Number 34 - October 2010

Almost all pharma products exist in powder form at some point on their way to finished product, so an understanding of powder behaviour is critical to the development of an optimal formulation.

The prevailing commercial and regulatory environment exerts apparently conflicting demands on the pharmaceutical formulator. Cutting time to market in order to realise a return more rapidly demands the acceleration of product development. However, there is an increasing emphasis on getting the manufacturing process right from the outset. As the seeds of reliable and successful manufacture are sown during formulation - the concept of Quality by Design - this broadens the scope of information gathering at the earlier stages of a project. Formulators need to understand how their decisions affect ease of manufacture in order to develop products that are not only clinically efficacious but can also be routinely and reliably manufactured to the necessary standard.

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14. Pharmaceutical Technology Europe - Analytical techniques today and tomorrow

Published in Pharmaceutical Technology Europe - May 2010

The pharmaceutical industry relies on analytical technologies for many testing and monitoring purposes, including formulation analysis, quality control and the identification of counterfeit products. The use of analytical instrumentation has also increased with the FDA’s PAT initiative and a growing emphasis on Quality by Design.

Given the wide range of applications for analytical instruments in the pharmaceutical industry, Pharmaceutical Technology Europe has dedicated both this month’s special feature and the May issue of PTE Digital to analytical technologies. We spoke with experts to identify the main challenges facing analytical scientists and what future advances are waiting on the horizon. Experts discuss the innovations and hurdles in bioanalysis, powder testing and NIR chemical imaging, as well as dissolution testing and the opportunities for improving sample preparation techniques.

Topics covered:

Bioanalysis: hurdles and hopes

Patrick Bennett, Strategic Marketing Director, Pharma, Thermo Fisher Scientific

Innovations in dissolution testing

Tony Copley, Managing Director, Copley Scientific

When and why should the pharmaceutical industry use NIR chemical imaging?

Janie Dubois, PhD, Product Manager Analytical Imaging in the Americas at Malvern Instruments

Understanding powder behaviour

Tim Freeman, Director of Operations at Freeman Technology

Industry must improve sample preparation techniques

Rob Darrington, Marketing & Business Development Manager at Genevac

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15. Ask the Expert: Why is effective powder characterisation so important for the pharmaceutical industry?

Published in Pharmaceutical Technology Europe - June 2010 - Title: The importance of powder characterisation

Effective powder characterisation can lead to better powder understanding and control, which is crucial in the pharma industry where the majority of APIs are delivered as powders. Tim Freeman explains why powder characterisation is not always an easy task and offers advice on how best to obtain rich data sets that can be used to predict powder behaviour in different situations.

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16. Measuring powder properties

Published in Inhalation Magazine - June 2010

Achieving consistent behavior of powders for inhalation, especially during dosing and aerosolization, presents a unique engineering challenge for the pharmaceutical industry, in part because the industry lacks a thorough understanding of the mechanisms that underpin successful drug delivery. Methods such as angle of repose, Hausner ratio, and Carr’s Index all provide some insight into the behavior of micronized pharmaceutical powders but have limitations in their reproducibility, sensitivity, and ability to capture diverse aspects of behavior, especially with respect to characterizing the response of a formulation to air.

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17. Characterising Powders for Better Solids Processing

Published in Pharma Magazine - May 2010

The pharmaceutical industry is moving towards greater emphasis on efficient manufacture. In simple terms, the regulators aim to reduce risk by encouraging developers to design product quality into the manufacturing process from the outset (ICH Q8, Q9 and Q10 - Quality by Design). For producers, this approach also addresses tough industry challenges, such as waste, time-to-market and capital utilization. It is clear, however, that the foundations for successful manufacture must be laid during the early stages of product development

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18. Enhancing dose consistency

Published in Manufacturing Chemist - March 2010

The right material and surface finish on filling equipment can be key to consistent capsule filling. Tim Freeman, Freeman Technology, and Dr Karlheinz Seyfang, Harro Höfliger, look at technology helping to get it right.

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19. Optimizing Ceramic Powder Specification

Published in Ceramic Industry magazine - December 2009

Powder characterization that is both reliable and relevant to the process makes it easier to develop a blend or granulate suitable for ceramic powder processing applications.

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20. Measuring powder behaviour in relation to QbD

Published in European Process Engineer - November 2009

Characterising and understanding a powder’s flowability is critical, particularly in relation to the pharmaceutical industry’s Quality by Design (QbD) and PAT initiatives.

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21. Dynamic powder characterization for DPI formulation

Published in Drug Delivery Technology - May 2009

Tim Freeman, Director of Operations, Freeman Technology Limited & Dr Robert Price, Pharmaceutical Surface Science Group

Formulating pharmaceutical blends for dry powder inhalers (DPI) is challenging, even for an industry with well-established powder processing skills. For a DPI, the active pharmaceutical ingredient (API) is usually a fine cohesive powder, which is then blended with a coarser carrier excipient to improve flow properties. During inhalation, the API is stripped from the surface of the carrier and delivered to the lungs, leaving the excipient to be ingested. With a passive DPI, the motive force for this aerosolization/elutriation process is provided by the patient, with inhalation activating the device.

The inclusion of excipient fines in the blend has been shown to improve drug delivery, a finding that has been explained by a number of hypotheses. In this discussion, we consider the way powders behave in DPIs and examine the dynamic and bulk powder properties that help to explain the mechanisms that dominate performance. Experimental studies illustrate the impact of blending on the in situ formation of fines and the effect this has on powder properties and aerosolization characteristics.

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22. Quantifying experience in powder processing

Published in Pharmaceutical Technology Europe - March 2009

Enshrined in the concept of Quality by Design is the premise that optimized pharmaceutical manufacturing requires detailed understanding of products and processes. With this in mind, many benefits can be achieved by combining modern powder characterization techniques with real processing experience.

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23. Process relevant powder characterization - a powerful tool for development and troubleshooting

Published in Pharmaceutical Online Magazine - Spring 2009

This article examines modern strategies for powder characterization in the pharmaceutical industry, with reference to commonly used technologies. It explores the value of systems that offer multiple methodologies in a single instrument, examining the way they provide a cost- and time- effective route to generating data that support product development and process operation.

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24. Fine tuning DPI formulas

Published in Manufacturing Chemist - June 2008

Various researchers have found that the inclusion of excipient fines in a formulation enhances Dry Powder Inhaler drug delivery. Jagdeep Shur and Robert Price from the University of Bath and Tim Freeman of Freeman Technology believe they can explain the reasons why.

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25. Formulation Optimization For Tableting Applications

Published in Pharmaceutical Solutions Update - November 2007

Tablet production is an essential operation for the pharmaceutical industry, considering the majority of drugs are being delivered in this form. Tablet presses operating on the principle of direct compression have been developed over several decades and it is now possible to make in excess of one million tablets per hour. Developing formulations that process well in these units to consistently deliver uniform tablets with the required properties, remains an ongoing challenge.

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26. Powder Testing for QC Applications

Published in Powder Handling & Processing - Vol.19,01 2007

QC is a vital part of any manufacturing process. Verifying the properties and consistency of both feed materials and products is critical in ensuring efficient process operation and customer satisfaction.

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27. Going with the Flow

Published in Polymers Paint Colour Journal (PPCJ) - October 2006

Powder Coatings - the importance of specifying, monitoring and controlling powder flow properties.

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28. Understanding Powder behaviour by measuring Bulk, Flow and Shear Properties

Published in Pharmaceutical Technology Europe - September 2006

A review of pharmaceutical processing and the relevance of powder properties in relation to four types of lactose varying from finely milled to spray dried.

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29. Testing Powders in Process Relevant Ways

Published in Powder Handling & Processing - Vol. 18, No 1, March/April 2006

A review of some everyday processing issues and how knowledge of key powder properties can be correlated with processing experience to improve productivity and product quality.

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30. The Importance of Air Content on the Rheology of Powders: An Empirical Study

Published in American Laboratory News - November 2004

Powders are sometimes considered to be relatively stable entities like the individual solid particles that make up their mass. This is not the case however, since their rheological properties can change by factors of between 100 and 1,000 in the presence of air. This paper describes how a powder can be characterized in relation to air content using methods that provide reproducible data from which databases on powder flow properties can be created.

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31. Measuring the Rheology of Difficult Materials

Published in Applied Rheology - November 2000

'Difficult materials', FT4 principle and data analysis and the comparison of different types of materials including Newtonian, pseudo plastic, dilitant and many types of powders.

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Application Studies

1. Titanium Dioxide

01/10/2002

Flow properties study of untreated and two types of treated titamium dioxide powders.

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2. Gypsum

01/03/2001

Evaluation of 5 types of gypsum powders showing how flow properties depend upon flow rate, compaction, aeration and moisture as well as basic flowability measurements.

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3. Talcum

01/03/2001

Evaluation of standard and micronised talcum powders showing how flow properties depend upon flow rate, compaction, aeration and de-aeration as well as basic flowability measurements.

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4. Lactose / Magnesium Stearate

01/10/2000

How magnesium stearate affects the flow properties of Lactose.

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