FT4 Powder Rheometer Literature
1. 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. (NEW) Getting to grips with Quality by Design
Presented at INTERPHEX 2010 - 20 to 22 April 2010
Tim Freeman
Freeman Technology, Welland
2. (NEW) 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
3. (NEW) 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
4. (NEW) 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
5. (NEW) 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]
6. 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?"
7. 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.
8. 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.
9. 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.
10. 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
Published in Powder Technology 190 (2009), pp. 65-69 DOI information
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.
Download via [Powder Technology Website]
11. 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.
12. 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
Published online by Powder Technology
Reg Freeman
A comprehensive study of the flow properties of 6 powder types comparing the rheometer flow energy measurements with shear properties data.
Download via [Powder Technology Website]
13. 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.
14. 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.
15. The Flowability of Wet & Dry Powders
20th Pharmaceutical Technology Conference - April 2001
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.
16. 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.
Conference Posters
Presented at WCPT6 2010
1. (NEW) The characterisation of the physical properties of wet masses
Presented at WCPT6 2010 - Poster #165 - 26 to 29 April 2010
Jamie Clayton1, Tim Freeman1, Reg Freeman1, Xiaowei Fu1, Brian Armstrong1
1Freeman Technology, Welland
2. (NEW) 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
Presented at INTERPHEX 2010
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 Freeman, Xiaowei Fu, Brian Armstrong and Karlheinz Seyfang
Freeman Technology; Harro Höfliger Verpackungsmaschinen GmbH
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)
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
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)
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
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
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)
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
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
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
5. Evaluation of Stear-O-Wet™ 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
Presented at DDL 2008
1. Characterisation and Functionality of Anhydrous Inhalation Lactose
Presented at DDL19 Edinburgh 2008
C Pitchayajittipong(1), J Shur(1), J S Kaerger(2), S Edge(3) & R Price(1)
(1) Pharmaceutical Surface Science Research Group, University of Bath, Bath, UK
(2) Aeropharm GmbH, Rudolstadt, Germany
(3) Novartis Pharma AG, Basel, Switzerland
White Papers
1. (NEW) 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.
2. 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.
3. 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.
4. 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.
5. 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.
6. 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.
7. 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..
8. 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.
9. 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.
10. 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.
11. 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.
12. 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.
13. 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.
The article can be downloaded by clicking on the icon on the right.
To go to the Powder Coating magazine's website click here.
Articles
1. (NEW) 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
2. (NEW) 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.
3. (NEW) 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.
4. (NEW) 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.
5. (NEW) 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.
6. (NEW) 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.
7. (NEW) 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.
8. 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.
9. 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.
10. 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.
11. 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.
12. 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.
13. 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.
14. Understanding Powder behaviour by measuring Bulk, Flow and Shear Properties
Publiched 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.
15. 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.
16. 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.
17. 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.
Application Studies
1. Titanium Dioxide
October 2002
Flow properties study of untreated and two types of treated titamium dioxide powders.
2. Gypsum
March 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.











