Trends in Food Science & Technology 11 (2000) 451457

Review

Process viscometry for the food industry

P.J. Cullen,* A.P. Duy,* C.P. ODonnell*,y and D.J. OCallaghan{
*Department of Agricultural and Food Engineering, University College Dublin, Earlsfort Terrace, Dublin 2, Ireland (fax: +353-1-475-2119; e-mail: colm.odonnell@ucd.ie) { Food Ingredients Department, Dairy Products Research Centre, Teagasc, Moorepark, Fermoy, Co.Cork, Ireland
Real-time monitoring and control of food processing applications have grown signicantly over the past decade. Food processors are increasingly demanding automated and realtime techniques, which are capable of withstanding the process environment coupled with meeting sanitary requirements. As a result new process monitoring techniques are emerging and traditional techniques are being modied to meet these demands. Commercial instrument designs are reviewed specically for the food industry with a focus on their advantages and limitations combined with novel modications developed to overcome such limitations. Emerging technology, which has potential within the food industry, is also discussed. # 2001 Elsevier Science Ltd. All rights reserved.

Introduction
Viscosity measurement has emerged as an integral and necessary component of many quality control procedures in food processing. Monitoring viscosity online/in-line provides real-time analysis, enabling the

Corresponding author.

food technologist to control many unit operations in food processing with greater precision and condence. Applications include process monitoring, quality control and process control. A number of reviews are available on process viscometry in general [13] and the food industry in particular [4,5]. The food processing environment poses a number of challenges to obtaining rheological measurements. The complex rheological nature of typical uid foods (including: multiphase, elastic, shear thinning, brous, particulate and highly viscous) calls for robust and innovative sensor design. High temperature and pressure, such as those associated with UHT processing or spray drying, are also problematic demanding specic design. Exposure to hostile process conditions, such as plant vibrations, fouling, cleaning agents, dust, etc., pose additional challenges to instrument manufacturers. The ideal viscometer design should facilitate ease of cleaning-in-place with minimal possibility of fouling, a quick response time and good sample renewal to ensure that any measurement obtained is representative. Finally the sensor must meet sanitary requirements. Typical selection criteria are presented in Box 1. To date, no single universal viscometry technique has managed to encompass solutions to all the above problems; selection will, therefore, be specic for each case, requiring some degree of compromise. In a common trend with the general sensor market, food processors are showing a preference for instrumentation that contains few if any moving parts and are easy to use and install. Interest in the potential for nonevasive techniques, such as ultrasonic and optical methods, continues to grow. All instrument designs are taking advantage of microprocessor developments to overcome limitations, such a noise eects, by incorporating transient lters, and providing options such as temperature compensation allowing comparative measurements in a variable temperature environment. The object of this review is to present a description of the main viscometry instruments and techniques that are currently used or under development for process monitoring in the food industry. This review should be of particular use to those who are concerned with the engineering design of food production plants by discussing the merits and limitations associated with particular process viscometry instruments and techniques, and the benets of process viscometry to the food

0924-2244/00/$ - see front matter Copyright # 2001 Elsevier Science Ltd. All rights reserved. PII: S 0 92 4 - 2 24 4 ( 0 1 ) 0 0 03 4 - 6

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Box 1. Selection criteria for food process viscometers 1. 2. 3. 4. 5. 6. 7. 8. Conformity with grade standards Installation modeinline, side-stream or immersion; Output signal requiredintermittent or continuous, response time, etc.; Control parameterviscosity, or some secondary related parameter; yield point, G0 etc. Fluid characteristicsmultiphase, solid particulates suspension, brous, fouling characteristics, etc.; Rheological characteristics of uidi.e. Newtonian or non-Newtonian, viscosity level, plastic, thixotropic, dilatant, etc.; Process operating conditionsTemperature, pressure, and laminar/turbulent ow; Viscometer characteristicsrepeatability, reliability, precision required, construction materials, ease of cleaning, intrusiveness, moving parts, seals.

industry. Technologies that measure other rheological parameters such as viscoelastic moduli and instruments with potential future applications are also discussed.

Viscometer installation and selection

There are two basic types of installation for on-line viscometers: ow-through and immersion. Flowthrough devices can be either the in-line type, installed directly in the owing process stream, or in the sidestream type (also known as on-line), which requires a small bypass line in which the owrate and temperature can be controlled if required. Immersion or tankmounted models can be either top or side mounting, for use in either open or closed vessels. This installation is required for process monitoring in quiescent systems, such as milk coagulation during cheese manufacture.

Current process viscometer types and techniques

Viscosity of a uid can be measured by a number of approaches and methods (Table 1). Rotational, vibrational and tube viscometers are the more common types of traditional measuring techniques based upon controlled deformation of the sample. These instruments are evolving to meet current industry demands and are nding increased use in combination with other technology, such as velocity prole determination and potential techniques such as rheo-optics.

Rotational viscometers
On/in-line rotational viscometers were developed based upon the most sensitive and successful o-line viscometer/rheometer principle. A spindle (cylinder, cone or plate) is rotated continuously in a liquid and the torque required to rotate the spindle at this rate is measured. Therefore, only two parameters are measured, the torque and angular velocity on the rotating spindle. Shear stress is calculated from the torque and shear rate from the angular velocity. Viscosity is related to the shear stress on the surface of the turning cylinder, divided by shear rate. Shear rate is well dened and instruments can be adapted to inline, side stream or immersion installations. In on/in-line viscosity measurement, the sample is continuously replaced.

Gyrating elements have also been used in some designs of process viscometer, instead of rotating elements. Brabender Instruments (Kiekenbusch, Germany) have developed this design, particularly for the paper industry where it is used to control and measure the consistency of paper pulp slurries. This instrument has also been used in mayonnaise production. Rotational viscometers are very sensitive, can operate at low shear rates and can take precise measurements of viscosity [1]. However, they do have a number of serious limitations. Blockages can occur in the presence of particulates if the gap between the rotating and stationary surfaces is small. They cannot be used where violent agitation and bubbling conditions exist and are not suitable for highpressure processes such as spray drying applications. Food process engineers have a preference for process instruments with limited moving parts and absence of seals. The development of fouling in the measuring chamber was a problem with some initial designs of rotational viscometer. In an eort to overcome such limitations, rotational process viscometer manufacturers have eliminated the traditionally necessary seals and developed sanitary designs marketed directly at the food industry, such as the Brookeld STT100 (Brookeld, MA, USA). The natural extension of oline rheometer facilities to on-line techniques has been achieved with the manufacture of variable speed rotational process viscometers. These instruments can be used to give a rheological prole of a uid by performing a shear rate ramp allowing real-time multi-point measurements and subsequent modelling of the data.

Vibrating viscometers
Vibrational viscometers are popular as in-line instruments for process control systems [6] and trials have shown that vibrational techniques can deliver good repeatability over a wide range of uids and process conditions. Simplicity of probe design makes the technique attractive for process engineers, proving to be robust, easy to clean in place combined with the added advantage of no moving parts. Vibrational viscometers are considered surface loaded systems, responding to a thin layer of uid, which surrounds the oscillating

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probe. Measurement depends on the surrounding uid dampening probe vibration, in proportion to its viscosity and density. An advantage of vibration viscometry over rotational is that it may be employed in high-pressure applications, such as spray drying. Shear rate, however, is undened as it is not only a function of instrument parameters, i.e. probe geometry, frequency and amplitude of oscillation, but also uid parameters i.e. density and viscosity. Relationships between instruments may, however, be inferred, by comparing measurements of apparent viscosities [7]. Since the vibrational viscometer relies on surface loading, suspensions with coarse particles can be tested without the danger of plugging. They can be installed in-line, side-stream or immersed into tanks. Their response time to changes in viscosity is fast, in the order of a few seconds, for most systems. Torsional vibrational viscometers, such as the Nametre Viscoliner (Nametre, NJ, USA) and Hydramotion XL7 (Hydramotion, Malton, UK) can measure viscoelastic properties of the liquid. A disadvantage with this type of instrument is that some uids may be dependent upon ow rate. A traditional limitation of vibrational viscometers is their sensitivity to plant vibration/ noise. However, this can be overcome with instrument designs (e.g. Hydramotion XL7) operating at frequencies outside the usual plant vibration spectrum and making the transducer highly frequency selective. A prototype variable amplitude vibrational viscometer (Hydramotion) has proven useful in monitoring milk coagulation in cheese manufacture in a quiescent system. It had previously been reported by OCallaghan et al. [8] that vibrational instruments experienced problems caused by micro syneresis at the high amplitude of operation. However, reduction of amplitude using the prototype to 40% overcame this barrier. Such a technique has also shown potential in providing a viscosity prole of a uid from a controlled amplitude sweep, overcoming the limitation of single point measurements from such instruments. A newly designed torsional oscillating tube, through which a uid is passed, has been developed for blood viscosity measurements [9]. Such a design would prove ideal for hygiene and cleaning concerns within the food industry, and trials on foodstus using diameters of up to 60 mm have been carried out with some success.

errors associated with this viscometer type. End eects can have a noticeable inuence on results, because of pinching of the food product stream at the entry and exit of the tube if length-to-diameter ratio is less than 50. Wall slip may also be a problem with uids containing particulates (i.e. food suspensions like fruit and vegetable purees, pizza sauces). Larger-diameter tubes must be used for particulate foods. If the owrate is constant, then simple raw pressure drop data may be used as an in-line monitoring technique and has been found to correlate well with conventional o-line techniques for such products as milk concentrates [10] and sauces [11] (Fig. 1). Dierential pressure transmitters with remote sanitary process isolators (Rosemount, Bognor Regis, UK) are suitable for food applications, since they can cope with particulates and harsh process environment conditions, with the non-intrusive pressure transducer membranes ush with the pipeline wall. Slit rheometers can provide sidestream monitoring of the elastic properties of uids. These dier from tube rheometers in that the pressure drop is measured directly in the slit die. An advantage of this geometry over the tube is that two pressure transducers can be mounted directly in the wall of the slit to determine the pressure drop in a region of fully developed ow and thus the true wall stress (i.e. no entrance correction is necessary) [2].

Other/potential techniques
A novel translational piston viscometer (Cambridge Applied Systems, Cambridge, MA, USA) has recently been adopted for food applications. This viscometer, based upon the cyclic speed of a piston between two magnetic coils along a small measuring chamber, uses the piston stroke to refresh the sample [3]. This translational technology has been demonstrated at pilot scale level in a milk powder spray drying plant to some success [10]. However, further research is required to determine inuence of fouling, CIP, and plant vibrations on instrument performance. Problems of sample renewal may arise for high yield stress uids, such as ketchup, due to the small diameter-measuring chamber, while response time can be quite poor [10]. The hot wire technique of viscosity measurement, which measures the intensity of natural convection around a hot wire, has traditionally been limited to stagnant systems. However by using a stainless steel shielded hot wire sensor, to eliminate the eect of ow outside the shield, this method has been extended to owing systems. Miyawaki et al. [12] reported that this modied sensor responded well to changes in viscosity in a Newtonian uid and to changes in the apparent viscosity in a non-Newtonian uid over a wide dynamic range. The sensor was able to monitor viscosity at a very low shear rate during xanthan production and to withstand high-pressure steam sterilization.

Tube viscometers
Tube viscometers are based on uid ow (created by pressure dierence) through a cylinder. The length to diameter ratio may range from 2 to 400, but is typically of the order of 100. Raw data for tube or capillary viscometers are pressure drop and volumetric ow rate. Their construction is simple, ow is continuous and sample-holding time can be very short. Tube viscometry proves particularly suitable for uid -foods containing particulates. However, there are a number of potential

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Fig. 1. O-line measurements of pizza sauce viscosity (Bookeld viscometer) and consistency (Bostwick Consistometer) versus measured pressure drop during tube ow.

The principle of mixer viscometry, where high precision measurements of torque and impeller rotational speed for a given geometry can determine apparent viscosity in the mixing vessel, is well documented. However, these trials are based upon scale down mixing geometries, relying on traditional rheometer/viscometer measurement of torque and speed [13]. The development of a sensitive low-cost torque transducer based upon acoustics (Sensor Technology Ltd, Oxon, UK) will facilitate the uptake of the technique to full-scale mixing systems, allowing monitoring of process development at the mixing stage and of complex food suspensions.

Emerging technologies Tomographicvelocity proling

Numerous tomographic techniques are available or emerging, based upon determining the velocity prole at a specied cross section of a pipe and corresponding pressure drop over a known length. Shear rate information may be determined by dierentiating velocity values as a function of position, ranging from zero at the tube centre to a maximum at the tube wall (Fig. 2). Shear stress data is determined from auxiliary pressure drop and conservation of linear momentum (tube viscometry). In contrast to conventional tube viscometry, which depends on volumetric formulas to determine one viscosity data point from a single pressure drop and owrate measurement, tomographic viscometry provides multiple shear viscosity/shear rate data points from one combined viscosity prole/pressure drop measurement [14]. Advantages of these techniques include their non-invasive and non-destructive mode of operation along with determination of rheological model parameters (shear viscosity, yield stress, slip velocity) on-line or in-line. Techniques for determination of velocity proles include electromagnetic, acoustic and electrical property measurement. Accuracy of

rheological property determination is dependent upon the spatial resolution of the instrument. Electromagnetic (optical and nuclear magnetic resonance) techniques pose the best spatial resolution; about 1% with acoustic based devices around 5% [14]. Ultrasonic Doppler Velocimetry (UDV) has proven an eective tool for on-line viscosity determination of Newtonian, non-Newtonian and multiphase opaque foods [15]. Real-time rheological analysis of ow processes at industrial scale have been evaluated for crystallization processesconcentrated chocolate [16] and fat suspensions [17]. This technique, teamed with a slit rheometer, was reported by Ouriev [18] to be employed in an industrial dough extrusion process. The technique may also be extended to determine ow behaviour, which aects rheological measurements (slip velocity) and more complex rheological behaviour such as viscoelasticity, extensional viscosity [19] and yield stress [18]. Reported results, particularly from industrial scale plant trials, demonstrate the potential of this technology. The response time for UDV is fast, in the order one second or less. Optical techniques such as laser Doppler anemometry and light scattering are limited by requirements of optically transparent uids and a transparent pipe or window for light access [20]. Nuclear Magnetic Resonance Imaging (NMRI/MRI) may, however, be used for opaque or transparent uids and therefore has a range of potential applications within the food industry. The technique potential to determine shear viscosity data for non-Newtonian uids has been evaluated and compared against traditional viscometers [14,21,22]. More complex rheological analysis may also be carried out-characterization of uid/ particulate mixtures by McCarthy and Kerr [23], apparent wall slip by Rofe et al. [24], particle migration by Hampton et al. [25] and modelling suspensions by determining relationships between relative viscosity, shear rate and particle loading [23]. MRI

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Fig. 2. A MR spatial-velocity (Axial velocity as a function of radial position, density distribution image and velocity prole for a pure suspending uid [23].

has proven extremely sensitive to rheological property variations as evidenced by recent work by Sun et al. [26] and Arola et al. [14,27], the latter determining dynamic yield values of a cellulose solutions to within 2% of a conventional rheometer. In general, the limit of MRI spatial resolution is not approached in MRI viscosity measurement. Commercial NMR/MRI systems are available for process control. The response time for MRI is in the order of 15 s or less.

Ultrasonic reectance sensor

Ultrasonic sensors, based upon reectance at the liquid interface rather than transmittance through the liquid, have been evaluated for real time process monitoring. A density and viscosity sensor employing longitudinal and shear ultrasonic reectance was applied to measure the viscosity of water-based solutions and slurries displaying potential for many food products [28]. Reported advantages of the technique include robustness and non-sensitivity to owrate, entrained air or vibrations. Using a similar in-line technique, Saggin [29] found shear reectance as a sensitive measurement of oil viscosity and both shear and longitudinal reectance a measure of solid content of lipids.

Fig. 3. Comparison of viscoelastic moduli of an F-actin, as measured by DWS (circles, G0 and squares G00 ) and strain-controlled mechanical rheometry (losangles) [32].

Diusing wave spectroscopy (DWS)

A non-evasive dynamic light-scattering technique known as diusing wave spectroscopy (DWS) has

recently been employed to measure rheological properties of macromolecular solutions, networks and gels in quiescent systems. Horne and McKinnon [30] compared DWS measurements and rheological measurements over a sol-gel transition for a gelatin suspension and found the technique could be used to track the process. ten Grotenhuis et al. [31] subsequently applied the techni-

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Table 1. Reported applications of process viscometry in food processing Technique Tube Vibrational Rotational CAS Hot wire (Flow) Mixer viscometry MRI UDV Ultrasonic reectance DWS @ @ @ @ @ @ @ @ Pilot scale Industry scale @ @ @ Selected applications General uid foodsspray drying skim milk, Sauces [11], soups, gravies, starch solutions General uid foodsmilk coagulation [8], ketchup [7], pizza sauces [7], yoghurt, fruit juices, sauces General uid foodsspray drying skim milk [34], mayonnaise, sauces Milk concentrates [10] xanthan production [12] (Industrial use in quiescent systemscheese milk coagulation) Food suspensions/foods with large particulates CMC [21], tomato concentrates [35] (tube viscometry products) Crystallization processeschocolate [16] and fat suspensions [17], dough [18] Slurries [28], lipids [29] Milk coagulation for cheese production [31], gels [33]

que to milk coagulation monitoring in a 200 l cheesemaking vat and showed the curd-rming process could be followed up to the point of curd cutting. Rufener et al. [32] used this technique to extract frequency-dependent viscoelastic moduli and time-dependent compliance from protein networks over an extended frequency range in a single measurement (Fig. 3), Arikainan et al. [33], in a similar study, estimated the viscoelastic modulus of an acidied milk gel. Both were found to correspond with mechanical rheometer measurements.

References
1 Kawatra, S.K. and Bakshi, A.K. (1995) On-line Viscometry in Particulate Processing in Mineral Proc. and Extrac. Metall. Rev. 14, 249273 2 Dealy, J.M. and Broadhead, T.O. (1998) Rheometry for Process Control in Rheological Measurements (Collyer, A.A., Cleg, D.W., eds), pp. 666722, Chapman and Hall, London 3 Barnes, H.A. (1999) On-line Or Process ViscometryA Review in Applied Rheology 9, 102107 4 OConnor, W., McEntee, S. and OCallaghan, D. (1995) In-line Viscometry in the Dairy Processing Industry in J. Society of Dairy Technology 48, 4449 5 Cheng, D-C.H. (1990) A Review of On-line Rheological Measurement in Food Science and Technology Today 4, 242249 6 Stee, J.F. (1996) Rheological Methods in Food Process Engineering, Freeman Press, East Lansing, USA 7 Cullen, P.J., Duy, A., ODonnell, C.P. and OCallaghan, D. (2000) In-line Prediction of Bostwick Consistency of Tomato Ketchup Using a Vibrational Viscometer in Irish Journal of Agricultural and Food Research 39, 151 8 OCallaghan, D.J., ODonnell, C.P. and Payne, F.A. (2000) Online Sensing Techniques for Coagulum Setting in Renneted Milks in Journal of Food Engineering 43, 155165 9 Ha usler, K., Reinhart, W.H., Schaller, P., Dual, J., Goodbread, J. and Sayir, M. (1996) A Newly Designed Oscillating Viscometer for Blood Viscosity Measurement in Biorheology 33, 397404 10 Hade, J., ODonnell, C.P. and OCallaghan, D. (2000) Application of In-line Viscometry to Milk Powder Manufacture in Irish Journal of Agricultural and Food Research 39, 172 11 Cullen, P.J., Duy, A., ODonnell, C.P. and OCallaghan, D.J. (2000) In-line viscosity measurement of pizza sauces using tube and vibrational viscometry in Proceedings of the 8th International Congress on Engineering and Food, 913 April 2000, Puebla, Mexico (Welti-Chanes, J. and Wesche-Ebeling, P. eds), p. 259 12 Miyawaki, O., Yoshikawa, M., Kuwaharada, H., Nakamura, K., Yamakawa, T., Kodama, T., Ito, K. and Nakajima, I. (1996) Application of Shielded Hot-wire Viscosity Sensor to Monitor Cultivations of Xanthomonos Campestris and Nicotiana Tabacum BY2 in Journal of Fermentation and Bioengineering 82, 6872 13 Brito-de La Fuente, E., Nava, J.A., Lopez, L.M., Medina, L., Ascanio, G. and Tanguy, P.A. (1998) Process Viscometry of

Future trends and conclusions

Problems associated with real-time rheological characterization of uid foods are numerous and complex. However, solutions based upon a number of approaches are rapidly developing. Some degree of compromise is required when choosing a real-time process instrument with selection application specic. Both traditional and novel designs are now targeted specically at the food industry, rather than marketing instruments designed for other industries. In the future, instruments combining a number of sensor technologies to futher characterize the rheology of complex foods are likely to be developed. Rheooptical techniques have proven benecial for determination of ow eects on crystallisation or phase behaviour of multiphase polymers and foods, using modied traditional o-line rheometers. Such collaboration with on-line rheometers is rare. However in-situ light scattering measurements does represent a potential future on-line technique. The benets of on/in line monitoring or control are, at last, being recognized by the food sector to which instrument manufacturers and scientists alike are responding with novel and imaginative designs.

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