an. nr g 2 .3 t... I I f .T V ‘ . ire.» 3511.4 {Tel A I Uh LIBRARY Michigan State University This is to certify that the thesis entitled Interrupted Helical Screw Impeller To Characterize Fluid Foods With Large Particulates presented by Alison Paige Omura has been accepted towards fulfillment of the requirements for M.S. dcgfimin Biosystems Engineering jc: P414. or 51%.. fl/ Major professor Date y{/Z‘DI/Uuz 0-7639 MSU is an Affirmative Action/Equal Opportunity Institution PLACE IN RETURN BOX to remove this checkout from your record. TO AVOID FINES return on or before date due. MAY BE RECALLED with earlier due date if requested. DATE DUE DATE DUE DATE DUE 6/01 c1/CIRC/DateDuep65-p15 INTERRUPI'ED HELICAL SCREW IMPELLER TO CHARACTERIZE FLUID FOODS WITH LARGE PARTICULATES By Alison Paige Omura A THESIS Submitted to Michigan State University in partial fulfillment of the requirements for the degree of MASTER OF SCIENCE Department of Agricultural Engineering 2002 ABSTRACT INTERRUPTED HELICAL SCREW IMPELLER TO CHARACTERIZE FLUID FOODS WITH LARGE PARTICULATES By Alison Paige Omura Mixer viscometry is an effective means of characterizing fluids containing particulates. An interrupted helical screw impeller used to determine the flow behavior of fresh concrete was scaled-down to analyze fluid foods with large particulates. The mixer viscometer constant was determined to be 1.6 rad‘l by the matching viscosity method. Large particulate food materials successfully investigated in this study were cream corn, salsa, a smooth pasta sauce and a chunkier pasta sauce. Apparent viscosity curves were constructed for products with moderately sized particulates, or those not exhibiting significant particle-to-particle interaction based on the raw data: torque and angular velocity. Testing materials exhibited shear-thinning behavior and temperature dependence. Regression analysis revealed K and n values ranging from 10.1 Pa 3'1 to 40.3 Pa sn and 0.17 to 0.36, respectively. Regression control charts of In apparent viscosity versus ln average shear rate were constructed for each food product. A protocol was suggested for producing and utilizing these charts as a statistical quality control tool for industry. ACKNOWLEDGEMENTS With my deepest sincerity, I thank Dr. James Steffe for the opportunities he has opened to me. I greatly appreciate his invaluable guidance and support throughout the years. I thank my parents for their encouragement and unwavering faith in me. The friendships I have formed and kept during my years at Michigan State University I will treasure always for keeping my life balanced. I would also like to thank the Department of Agricultural Engineering and Food Science for acting as an extended family to me. A special thanks is given to Richard Wolthuis for his services in manufacturing the interrupted helical screw impeller. iii TABLE OF CONTENTS List of Tables List of Figures Nomenclature 1. Introduction 1.1. Overall Description 1.2. Objectives 2. Literature Review 2.1. Fluid Food Rheology 2.2. Mixer Viscometry 2.2.1. Mixer Viscometer Constant (k ') 2.2.2. Fluid Food Applications 2.3. Rheology of Suspensions 2.4. Rheology of Particulate Fluid Foods 2.5. Concrete Rheology 2.6. Statistical Quality Control 3. Theoretical Development 3.1. Mixer Viscometry 3.2. Evaluation of Mixer Viscometry Constant (k ') 3.2.1. Slope Method 3.2.2. Matching Viscosity Method 3.2.3. Torque Curve Method 3.3. Determination of Fluid Properties 4. Materials and Methods 4.1. Equipment 4.2. Experimental Materials 4.3. Data Collection 4.3.1. Phase Characterization 4.3.2. Determination of Mixer Viscometry Constants (k " and k ') 4.3.3. Particulate Food Flow Behavior ' 4.3.3.1. Room Temperature 4.3.3.2. Hot Testing 4.3.3.3. Cold Testing 4.4. Data Analysis 4.4.1. Phase Characterization 4.4.2. Determination of Mixer Viscometry Constants (k " and k ') iv Page vi viii Table of Contents (cont’d) 4.4.3. Particulate Food Flow Behavior 4.4.4. Regression Control Charts 5. Results and Discussion 5.1. Phase Characterization 5.2. Mixer Viscometry Constants (k " and k ') 5.3. Particulate Food Flow Behavior 5.4. Regression Control Charts 5.5. Statistical Quality Control Protocol 6. Summary and Conclusions 7. Future Research Appendix References 30 30 31 31 34 36 48 51 53 55 69 LIST OF TABLES Table 2.1. 4.1. 4.2. 5.1. 5.2. 5.3. 5.4. 5.5. 5.6. 5.7. 5.8. A.l. A2. A3. Mixer viscometer constants. Ingredient list of the fluid foods with large particulates selected for testing. Fluid food products with particulates that did and did not require a pre-shear phase. Measurements a, b, and c and the ranges of each dimension of foodstuffs in the fluid food products. Power law, rheological parameters of the fluid phase of foods with particulates at 23 °C determined by the helical ribbon system. Rheological parameters of the standard fluids at 23 °C used to evaluate k" and k '. Comparison of the interrupted helical screw impeller and concentric cylinder using ketchup at 23 °C. Rheological parameters for foods with particulates at cold, room, and hot temperatures using the interrupted helical screw impeller. Activation energy and A values for each fluid food with particulates using the interrupted helical screw impeller. Comparison of the rheological parameters of whole fluid food products with large particulates at room temperature (23 °C) using the interrupted helical screw impeller to the fluid phase at room temperature (23 °C) using a helical ribbon. Comparison of standard errors for each fluid food with large particulates at each temperature. Interrupted helical screw impeller data to determine k " using Newtonian fluids at 23 °C. Interrupted helical screw impeller data to determine k' using non- Newtonian fluids at 23 °C. Interrupted helical screw impeller data for cream corn. vi Page 24 27 33 33 34 36 41 42 45 48 56 58 61 List of Tables (cont’d) A.4. Interrupted helical screw impeller data for Prego. A.5. Interrupted helical screw impeller data for Ragu. A.6. Interrupted helical screw impeller data for salsa. vii 63 65 67 LIST OF FIGURES Figure 4.1. Interrupted helical screw impeller. 4.2. Interrupted helical screw impeller and container. 5.1. Percentage by weight of solid and fluid phases in foods with particulates. 5.2. Viscosity times angular velocity versus torque for the interrupted helical screw impeller with Newtonian standard fluids for the determination of the mixer coefficient constant, k " at 23 °C. 5.3. Mixer viscometer constant, k ' , versus angular velocity for the interrupted helical screw impeller using non-Newtonian standard fluids at 23 °C. 5.4. A typical raw data set from one trial using the interrupted helical screw impeller with Prego sauce at 8 °C. 5.5. 1n 11 versus ln 7“ for cream corn at cold (5 °C), room (23 °C) and hot (80 °C) temperatures using the interrupted helical screw impeller. 5.6. In 1] versus 1n 7,, for Prego at cold (8 °C), room (23 °C) and hot (80 °C) temperatures using the interrupted helical screw impeller. 5.7. In T] versus In 7'“ for Ragu at cold (7 °C), room (23 °C) and hot (80 °C) temperatures using the interrupted helical screw impeller. 5.8. 1n 1] versus In 7,, for salsa at cold (7 °C), room (23 °C) and hot (80 °C) temperatures using the interrupted helical screw impeller. 5.9. 1n 11 versus l/T at 18.88 Us for each fluid food with particulates using the interrupted helical screw impeller. 5.10. 1n 1] versus In 70 of fluid food products with large particulates at cold temperature (58 °C) using the interrupted helical screw impeller. 5.11. 1n 1] versus ln 7, of fluid food products with large particulates at room temperature (23 °C) using the interrupted helical screw impeller. 5.12. 1n 1] versus ln 7“ of fluid food products with large particulates at hot temperature (80 °C) using the interrupted helical screw impeller. viii Page 21 22 32 35 36 37 38 39 39 40 42 43 44 List of Figures (cont’d) 5.13. 1n 11 versus In 70 for Prego sauce at cold temperature (5 °C) using the interrupted helical screw impeller. ix 47 NONIENCLATURE A = constant (dimensionless) d = spindle diameter (m) D = container diamter (m) E, = energy of activation for flow (cal g'l mole") h = impeller height (m) k' = mixer viscometer constant (rad") k "= mixer coefficient constant (rad m") K = consistency coefficient (Pa 8") M = torque (N m) N = rotational speed (rev 3") n = flow behavior index (dimensionless) n = number of data points NPO= Power number (dimensionless) NR“ = impeller Reynolds number (dimensionless) P = power (N m s“) R = universal gas constant (1.987 cal/(g - mole K)) se = standard error of predicted y T = temperature (°C) T,= reference temperature (°C) x = independent variable y = dependent variable 7 = shear rate (5") Ya = average shear rate (5") 77 = apparent viscosity (Pa 3) 77, = reference apparent viscosity (Pa 8) y = Newtonian viscosity (Pa 3) pm: plastic viscosity of a Bingharn fluid (Pa 3) p = density (kg m3) 0' = shear stress (Pa) 0'II = average shear stress (Pa) 0'o = yield stress (Pa) 9 = rotational speed (rad s") CHAPTER 1 1. Introduction 1.1. Overall Description Rheology, or the study of the manner'in which materials respond to an applied stress or strain, is widely used for process engineering, product development, and quality control applications within the food industry. Flow behavior information is critical to efficiently design processing operations such as mixing, pumping and heating. Characterizing fluid foods is also needed to standardize and quantitatively evaluate product quality. Product quality is very important in most industries. Quality is a measure of a product’s acceptability to consumers. The food industry successfully utilizes statistical methods such as control charts and regression analysis to monitor and control quality variables. Fill-level, microbiological safety, and shelf life are examples of variables that can be monitored and controlled. Rheological information provides a quantitative measure of the physical material quality for food products. The utilization of mixer Viscometry to evaluate the rheological properties of fluids has been extensive. Mixer Viscometry involves the rotation of an impeller immersed in a sample material. Rheological properties are determined from information concerning the system geometry, rotational speed, and resulting torque. An advantage to using mixer Viscometry over traditional rotational Viscometry, such as concentric cylinders and cone and plate systems, is its ability to assess difficult fluids. Examples of difficult foods are those exhibiting slip, time-dependent behavior, particle settling problems, and those with large particles. Many prepared foods are essentially coarse solid-liquid mixtures. Examples include salsas, pasta sauces, cream corn and baked beans. Foods that contain large particulates pose problems with effective analysis and therefore, control. Presently, the individual solid and liquid phases that comprise the final product are tested separately, and/or an empirical quality control test is performed. However, the behavior of the separate phases will be different from the final product mixture. Also, empirical test results are very difficult to relate to fundamental rheological properties. No agreed upon means to test for objective, standard characteristics of a final fluid food product with large particulates exists. This research proposes a method to objectively test the rheological properties of these products. The success of using an interrupted helical screw impeller to determine rheological properties of fresh concrete inspired the experimental technology transfer described in this work. The name of the impeller describes the discontinuous helical pattern of the screw. A scaled down interrupted helical screw impeller has been designed to overcome some of the difficulties presented by complex foods. 1.2. Objectives The ultimate goal for this research was to develop an impeller for mixer Viscometry applications that is appropriate for fluid foods with large particulates, with the potential for use in statistical quality control programs. Specifically, the objectives were: 1) To design, construct and characterize an interrupted helical screw impeller; 2) To evaluate the potential of the interrupted helical screw impeller to characterize the flow behavior of fluid foods with large particulates; 3) To develop regression control charts for typical fluid foOds containing large particulates; 4) To develop a statistical quality control protocol for fluid foods with large particulates. CHAPTER 2 2. Literature Review 2.1. Fluid Food Rheology Mathematical models aid in the description of the flow behavior of fluid foods. A Newtonian model for fluids, 0' = M" [11} illustrates a simple, linear relationship between shear stress and shear rate. Typical food products that exhibit this behavior are water, corn oil, and corn syrup. The power law model, 0' = K 7" [2.2] represents fluids that are shear-thinning (n < l) or shear-thickening (n > 1). Common examples of power law fluids are applesauce, orange juice concentrate, and tomato ketchup. Another standard fluid model is the Bingham plastic, 0=#,.,(7)+0. [2.31 which incorporates a yield stress component, a finite stress required to initiate flow. Peanut butter, cream cheese, and toothpaste are often considered Bingham plastic fluids. Apparent viscosity is an important quantitative parameter for fluid foods. It is calculated by dividing the shear stress by the shear rate. For Newtonian fluids, the apparent viscosity is a constant value, independent of the shear rate. However, in the case of power law fluids, apparent viscosity changes with shear rate (Steffe, 1996): 77 = K ()"Y’"1 [2.4] The above models describe fluids that are considered time-independent. Other fluids will increase or decrease in shear stress over time at a constant shear rate: they are known as rheopectic and thixotropic materials, respectively. Viscosity can also be modeled as a function of temperature: Ed # - f (T) — ACXP[RT] [25] Using the above equation, apparent viscosities considered at a constant shear rate can be found at any temperature using reference values: melee—a ' This equation assumes that temperature has a negligible effect on the flow behavior index. Larger E, values indicate a faster change in viscosity with temperature. 2.2. Mixer Viscometry 2.2.1. Mixer Viscometer Constant (k ') The original investigators of non-Newtonian fluids using mixer Viscometry are Metzner and Otto (1957). They proposed a method based on a matching viscosity assumption (also known as the matching viscosity method), which asserts that the average shear rate for a non-Newtonian fluid is equal to shear rate for a Newtonian fluid when the Newtonian viscosity equals the apparent viscosity of the non-Newtonian fluid. They also assumed that the average shear rate is linearly related to the rotational speed of the impeller by a constant k ': 7.. = k'N [2.7] A constant value for k' was assumed, although the possibility of variation with the flow behavior index, n, was not dismissed. Table 2.1 contains a listing of k' values and details for studies mentioned in this section. man we was 8:22 >5. :52 3o no.“ SEE G8: 9&2 EN 222 a: 5-2 BESS uses ones 33 :3: 95 use sees: 86 :52 who 92 as was» as: man Ea: a a 5.82 com 222 Rd N: <>m 888 a a 3 2: m3 9: N 328 warm m3 a: $4 H 328 aeam Fe 36 e3 :25: Beam New 222 2: N2 8:22 68: a a museum 3: 34 8:63 3&3 min 222 e: w? Baas an 0 e5... 5? 835. «E 5N 3:63 3.72: :52 we 84 .883 ea c 2.3a 5? 0583 $3: a a 225 83 Boa and mi mam $3: a a 852328 $.33 aem 33.38 m 85.31;; 3.0-86 332 33-8.8 m 85.34.34 $.33 :52 32.88 m 03.31:; saga m 8%: seem as“ engage m3 85 52 O? 320... SB: age: 688 a a Bandeau a? 2: m3 Geese EEE 0:58 883 v a? a: a: 83:5 Eaaoa 858 883 m an 222 s: N .m emcee 2223 e023 N 83: $2582 ea xaeoeao N3 265 2a 84 $3 6%: seem Ea mmmem 9.25 a 15502 2; So 5:095 .853 95388 53:88? 652 AN 2an 8502 283.5 22032 u E? 23a oi. 22% 82. 8.2 8&8 m: 8:3 Dena >2 £3: Rom Ea deem 8.2” 222 $5 :2 .555. 62¢: a a 238m m3 3 8.2 :23: 28:0: 22 ad :2 55% new: BEE EN 256 3o :2 .565 $8: 282 as... 532 $2 0.22.0. who 82 one? 8 am :2 222 who 22 28a? 8 ea o3 aoa 3o :2 mac SN 22 8.0 23 $2 233: 3.80 Ba 82 3.2 222m 86 ”2 $2 $8: 82 a: 2>2 2 mm: 22.? 8 new $3: 82 2a 20 a: e: 2:. 8525 Base 683 .2 23502 2: so 5:282 eased. 8.288 .3 033. Rieger and Novak (1973) developed a test that served as an indicator of the suitability of the Metzner-Otto assumption (Eq. [2.7]). The Rieger-Novak method, also known as the slope method, provided an alternative means to determine k ' . The authors used several types of agitators to analyze the power consumption in mixing highly viscous, time-independent, inelastic non-Newtonian fluids with pseudoplastic behavior. The accuracy of the k' values for the anchor and pitched blade anchor agitators were best fit as functions of n, rather than constants. The authors compiled a table of k' values for comparison. Ducla et al (1983) showed that k' for varying turbine impellers was constant when mixing true pseudoplastic fluids over the entire shear rate range tested by using the Metzner-Otto method. The aim of this project was industrial mixing operations. Edwards et al (1976) established k' values of an anchor, helical ribbon, and two helical screw impellers using the matching viscosity method. This was one step in a process to calculate the power consumption with time when agitating a thixotropic liquid. Fluid properties were observed to influence k '; however, the authors chose not to elaborate on these relationships and instead accepted constant values as reasonable. Sestak et al (1986) developed k' as a function of n for anchor agitators. The function deduced was recommended as a first step of an iterative series to find a converging value for k'. This procedure was considered successful for both pseudoplastic and thixotropic fluids. The matching viscosity method and slope method were compared for the determination of an average shear rate by Rao and Cooley (1984). The flag impeller in the study done by Rao (1975) was used in this work along with a star impeller that has 8 vanes. k' values for both methods were in good agreement using each impeller. When k' is around 20 llrev or greater, the slope method must be used with caution because of a greater sensitivity to error. Overall, small errors are magnified because of the log-log relationship required in the slope method. The decided advantage of the slope method was its simplicity. Briggs and Steffe (1996) found k' for a Brookfield small sample adapter with a flag impeller using the slope and matching viscosity methods. While the slope method resulted in a constant value, the influence of the angular velocity was apparent when using the matching viscosity method. In this investigation, the flow behavior index produced inconsistent, but small, effects on k '. Nonetheless, both methods gave similar results and the use of a constant value was recommended. Castell-Perez and Steffe (1990) concluded that k' is dependent on n, as well as other variables for paddle impellers. Two versions of the matching viscosity method (power curve and torque curve) and the slope method were evaluated to determine the influence of fluid properties, system geometries and impeller rotational speeds on k'. The authors found that k' is directly related to n and inversely related to K. Above rotational speeds of 20 rpm, k.' can be assumed constant. Small gaps between the impeller and the cup were recommended to reduce the influence of fluid properties. Nagata (1975) produced an exhaustive investigation of mixing principles and applications. Nagata covered power consumption equations for different impellers and fluids and flow regimes, as well as flow models. A straightforward approach was outlined to develop a Power number/Reynolds number curve for pseudoplastic fluids based on work by Metzner and Otto (1957). 2.2.2. Fluid Food Applications Extensive work has been done with mixer Viscometry and fluid food materials. Castell-Perez and Steffe (1992) prepared a complete review of the development of mixer Viscometry as related to food applications. Rao (1975) measured the flow properties of food suspensions using a flag impeller as an alternative to narrow gap and tube viscometers. k' was found using the slope method. Tomato puree, applesauce, and apple pulp were determined to be pseudoplastic in nature. The flow properties for this investigation were valid over only limited ranges of shear rates however. k' was also determined via the slope method by Cantu-Lozano et a1 (2000) to study the rheological properties of apple suspensions using a helical ribbon screw agitator. Rao and Cooley’s (1984) star impeller along with a 6-vaned impeller was used in another study done by Qiu and Rao (1988). The goal was to evaluate the effectiveness of mixer Viscometry when analyzing applesauce for its yield stress and power law parameters. A constant k' was determined for the 6-vaned impeller using the matching viscosity method. The obtainable shear rate testing range was narrower than if using a concentric cylinder. The k' value of a Haake MV paddle impeller used for the analysis of strained apricots thickened with modified tapioca starch was investigated by Steffe and Ford (1985) using the slope method. Mixer Viscometry in this study was applied to thixotropic materials as well as time-independent (after mechanical degradation) materials. Castell-Perez et al (1987) used a flag impeller with a Brookfield small sample adaptor. k' was found using the slope method. In this study, as well as the work by 10 Briggs and Steffe (1996) on a flag impeller, the mixing systems were designed for the analysis of power law fluid foods. A flag impeller was also used by Mackey et a1 (1987) to analyze shear-thinning behavior of food with mixer Viscometry techniques. A matching viscosity method was used to define k' because the slope method indicated a dependency on rotational velocity and therefore an increased chance of error in calculations. It was also found that the influence of n on k' decreases with increasing angular velocity. This particular matching viscosity method, later coined the torque curve method by Castell-Perez and Steffe (1990), was also used in Lai et a1 (2000) to find the k’ value of a Rapid Visco Analyser (RVA) system impeller. At speeds of 60 rpm and greater the k' value was considered constant. Applications of the RVA system are primarily for analyzing the rheological behavior of starch slurries during heating and cooling. 2.3. Rheology of Suspensions The rheological properties of particulate suspensions have been investigated for many purposes such as particle removal from surfaces, fines mobilization in porous media, transport of proppants in fractured reservoirs, and cleaning of drill holes (Patankar and Hu, 2000). Wildemuth and Williams (1984) focused on packing fraction when evaluating the apparent viscosity of concentrated suspensions. These concepts were intended for examining the rheology of dense coal suspensions. Using a helical ribbon stirrer, the rheological changes of mixing an emulsion with a suspension were studied by Hugelshofer et al (2000). These mixtures are relevant for calorie-reduced food products. Using a model suspension, the slope method and 11 matching viscosity method were both employed to calculate apparent viscosities and shear rates. These results were similar to concentric cylinder data. 2.4. Rheology of Particulate Fluid Foods There has been much research on the rheological behavior of fine food particles. Schubert (1987) discusses the branch of process engineering associated with particles known as particle technology. Specifically, Schubert’s article addresses fine solid particles on the order of micrometers (the largest sector of particle technology) and reviews the properties and characterization of these systems. Examples from food technology were used to illustrate key aspects. Rao (1987) clarified the relationship between composition and rheological behavior of food suspensions of plant origin, such as applesauce and concentrated orange juice. The flow properties of plant food suspensions were put in terms of temperature, concentration, suspending medium and suspended solids. Flow behavior studies pertaining to fluids with larger particulates are less abundant. Currently, there is no agreement on a methodology or instrumentation to investigate these solid-liquid food mixtures. Particulate food mixtures differ from food suspensions based on the size of the individual solids. Large particulates are generally measured on a centimeter scale, come in a variety of shapes and have only a small difference in density with the carrier fluid. The carrier fluids are most often non-Newtonian, specifically pseudoplastic, and are highly viscous (Lareo et al, 1997). Some studies on the heat transfer of fluid foods with large particulates have been conducted. Sannervik et al (1996), for example, found that the inner heat transfer coefficient increased with increasing food particulate concentration in a tubular heat exchanger. 12 Bhamadipati and Singh (1990) investigated the flow behavior of frozen thawed peas and dry soybeans in tomato sauce, using tube Viscometry. These particulates were used as model foods rather than being an actual, commercial food product. Pressure gradients and volumetric flow rates were used to determine the flow properties. Based on their results, the power-law model best represents the flow behavior of solid-liquid mixtures. Solids and particulate presence increases the consistency coefficient and decreases the flow behavior index. The disadvantage of this technique is the large amount of testing material required. Rotational Viscometry was utilized by Pordesimo et al (1994) to evaluate solid- liquid food mixtures at low shear rates. A very-large-gap parallel plate system was used to determine rheological properties of edible compounds made to imitate liquid food products with large particulates in the range of 0.32 cm to 0.95 cm. Effects of carrier viscosity, particle size, particle concentration, and particle shape were investigated. Pordesimo (1991) reviewed several proposed instruments and procedures to evaluate coarse mixtures. Still, however, not enough is known about large-gap rotational viscometers. Martinez-Padilla et a1 (1999) used mixer Viscometry to evaluate the physical properties of coarse food suspensions; specifically Mexican sauces. A shear-thinning fluid with pepper and tomato seeds was analyzed using a helical ribbon, a tube viscometer and a wide gap spindle. The helical ribbon best characterized the flow behavior. The ribbon was better able to maintain a pseudo-homogenous flow and required the smallest sample. The disc-shaped seeds were the largest (albeit still on the 13 small side of large particulate systems) particles used in combination with mixer Viscometry. A 2.5. Concrete Rheology In the concrete industry, many empirical tests exist to determine the flow properties of fresh concrete (Bartos, 1992). Rheological information about concrete is important because many aspects such as case of placement, durability and strength depend on the flow characteristics. An obstacle for the analysis of fresh concrete is the complexity of the composition. Particles found in concrete range from 1pm cement grains to 10 mm coarse aggregates to even 100 mm particulates found in dams (Ferraris, 1999). Tattersall (197 3).argues that since it has been accepted that. fresh concrete behaves as a Bingharn plastic fluid, at least two shear rates are necessary for an accurate characterization of its flow curve. Tattersall and Bloomer (1979), discussed the trials and tribulations of developing an apparatus to test fresh concrete. The authors diverged from historical usage and approached the problem using mixer Viscometry. The device developed became the first and most widely known instrument to measure the flow properties of concrete (Ferraris, 1999). A mixer (of interrupted helix form) that alloWed concrete to fall back through the gaps and create localized mixing was fabricated. Mathematical relationships were formed translating the raw data to rheological values. Wallevik and Gjorv (1990) modified the apparatus and testing procedure of Tattersall and Bloomer (1979) to produce more reliable results. The main drawbacks to this apparatus were the required calibration, the large size of the apparatus making it not test-site friendly, and the computations required to find results (Bartos, 1992). Versions 14 of this instrument are now commercially available as the BML Viscometer or the [BB Concrete Rheometer (Ferraris, 1999). 2.6. Statistical Quality Control Statistical quality control is used in many areas of the food industry, such as product research and development, material control, production quality control and product performance (Hubbard, 1990). When a process is in statistical control, the distribution of data is attributed to stable and repeatable variation inherent in the process (Bafna, 1995). Dr. Walter A. Shewhart first developed control charts in 1924 as a graphical device for the detection of unusual variation of data resulting from a repetitive process. Control charts can be categorized by the type of application: for variables, attributes, or individual points. Variables encompass any quality characteristic that can be measured, while attributes are classified as either defective or nondefective. Rather than plotting characteristics against time, as in variable and attribute charts; individual charts plot against each specific observation (Puri et al, 1979). Upper and lower control limits are put in place as the boundaries of acceptability. A common method is to use control charts in pairs: one chart for the value of the variable, and one chart for the range or spread of the values. Bafna (1995) discussed the importance of rheological instruments in statistical control. The variability of the instrument should less than or equal to one tenth of the variability of the process it is monitoring. When monitoring viscosity, Bafna recommended taking values from the highest and lowest shear rates and plotting them on 15 individual charts. The author also outlined six rules when using individual charts to 0 determine whether a process is out of control. Mandel (1969) combined linear regression and control chart theory to construct regression control charts as a means to analyze postal efficiency. Regression control charts are applicable when controlling a variable that is linearly dependent upon the magnitude of an independent variable. The chart is a linear plot of a variable with upper and lower control limits running parallel with the control line. In the case of several nonlinear relationships, a suitable transformation can make them linear (Chatterjee and Price, 1977). The control limits can be set at any distance from the control line, but are usually kept at 2 or 3 times the standard error of estimate. This decision is based upon economics and experience of the management (Mandel, 1969). The Mandel (1969) method was used in the current research. 16 CHAPTER 3 3. Theoretical Development 3.1. Mixer Viscometry Applying dimensional analysis to mixer Viscometry with Newtonian fluids yields the following empirical relationship: Npo = —- [3.1] This relationship is Widely accepted when applied in the laminar flow regime, and can be used for non-Newtonian fluids. The Power number and impeller Reynolds number are defined as P NPo = p523d5 [3.2] and 2 . NM = ‘ [3.3] ju Substituting Equations [3.2] and [3.3] into Equation [3.1] yields 5”, = ’2‘” [3.4] d £2 ,0 d 52p Using the definition of power, P = M $2 [3.5] Equation [3.4] simplifies to M = A 3.6 (139 ll [ ] By replacing the Newtonian viscosity with an apparent viscosity (Equation [24]), that is evaluated at an average shear rate given by 17 7.. = k '9 13-7] Equation [3.6] becomes . M (13:2 = AK (k '52)"1 [3.8] The mixer viscometer constant, k ', is exclusive to each mixer system. 3.2. Evaluation of Mixer Viscometry Constant (k ') 3.2.1. Slope Method The slope method asSurnes a constant value for k'. Simplifying Equation [3.8] and! taking the logarithm of each side yields log", [5%) = logm(A) — (1 — n) logw(ki') [3.9] k' is determined from the slope of the line, loglo (£375) vs. (1 — n) . Rieger and Novak (1973) argued that if Equation [3.9] was not linear, then the average shear rate assumption expressed by Equation [3.7] is not valid. 3.2.2. Matching Viscosity Method This technique is a valuable alternative to the slope method for determining the mixer viscometer constant. A power curve is first constructed using Newtonian fluids to determine A. Then, a standard non-Newtonian fluid, in which the K and n values are known, is mixed at a constant rate using the chosen impeller system and the resulting Power Number is measured. Using the matching viscosity assumption (1] = p.) and Equation [3.1], the apparent viscosity is defined by ,7 = (4252mm...) A [3.10] 18 Considering Equation [2.4], the average shear rate can be calculated: 1 . = 17:1 7. [K] [3.11] When several iterations of the process have been conducted at different speeds, using standard non-Newtonian fluids with well defined flow behavior indices, k'can be calculated from Equation [3.7] as . 7 k =—"— 3.12 9 [ ] Using this method allows for k' to be evaluated as a function of angular velocity and the flow behavior index. 3.2.3. Torque Curve Method To determine k', Mackey et a] (1987) developed a method which was later coined the torque curve method by Castell-Perez and Steffe (1990). Rearranging Equation [3.6] yields _ M _k"M M352 :2 g [3.13] where k", the mixer coefficient constant, is dependent solely on the system geometry. Making the matching viscosity assumption and substituting Equation [2.4] into Equation [3.13], yields an equation for k ': were): 3.3. Determination of Fluid Properties In laminar mixing, the relationship between torque and angular velocity is found from Equation [3.8] 19 log,o(M) = log,o(d3AK(k )"")+nrog,o(rz) [3.15] where n is the slope of the line. K can be determined by either of two methods. If the values of d, A, k’, and n are known, then K can be calculated using the constant term (loglo (d3AK (k ')"") of Equation [3.15]. The alternative method is to solve for K using the following equation: r2"! k "y M,)( ,( D K =K( ’ My Q:’(k')"’ x ) [3.16] where x denotes the fluid with unknown properties and y designates the reference fluid with known properties. This method eliminates the need for determining the value of A. If the value of k' is known, then rheological parameters may also be determined by assembling a plot of apparent viscosity versus average shear rate. The average shear rate is calculated using Equation [3.7]. Apparent viscosity is found by applying the matching viscosity assumption and substituting the apparent viscosity for Newtonian viscosity in Equation [3.13]: k"M =— 3.17 77 Q l l Curve fitting programs can then easily characterize the fluid using an appropriate rheological model. 20 CHAPTER 4 4. Materials and Methods 4.1. Equipment The interrupted helical screw impeller was fabricated from stainless steel and consists of 4 triangular blades (0.08 cm thick) joined to the shaft, pointing toward the shaft, in a helical pattern (Figure 4.1 and 4.2). The initial impeller and cup system was a 1/3-scale replica of the design by Wallevik and Gjorv (1990), intended for testing fresh concrete. Through preliminary trials, the cup diameter was increased to improve movement of the particulate foods and reduce slip of particulates against container. fir.— 0.4 +1594— 12.18 C 788 y” ’ 75° 2.71 V v |1.88| Figure 4.1. Interrupted helical screw impeller (all dimensions in cm). 21 1 3.2.01» 1 9.3 D TV 27 t/ i Figure 4.2. Interrupted helical screw impeller and container (all dimensions in cm). Using an adaptor, the impeller was attached to a Haake VT550 Viscometer (Haake, Paramus, NJ). The torque range of the instrument is 0.1 m Nm to 30 m Nm. A rheological software program, RheoWinZ, controlled the VT550 and collected the raw data: angular velocity and torque. The testing material was loaded into an 800ml capacity glass beaker. A foam jacket was used to insulate the beaker and prevent slippage on the test stand. The container was raised into testing position by a scissor jack. Samples for cold temperature testing were cooled in a kitchen refrigerator (Kenmore, Hoffman Estates, IL) with temperatures varying by i1 °C. Heating of the samples for hot temperature testing took place in a drying oven (Isotemp Oven, Fisher 22 Scientific, Itasca, IL) with a variation of :1 °C. Thermometers provided temperature verification. Using the Haake VT550, the W1 concentric cylinder system with a gap of 1mm was chosen for evaluating non-particulate fluids. Properties were determined using standard rheological methods (Steffe, 1996). The temperature was controlled using a water bath (Haake F6, Paramus, NJ) to within :tO.1 °C. Densities of the Newtonian fluids were determined with a 100 ml specific gravity cup. A ‘11 inch square gap sieving pan was used to separate large particulates from the testing foods. An electronic scale was employed to weigh both solid and liquid phases. Particulate sizes were manually measured using a caliper (10.02 mm). The liquid phase contained M: inch particulates able to pass through the sieve; therefore, a concentric cylinder system was not appropriate to assess the rheological properties because of the small gap size. A helical ribbon and W1 cup attached to the Haake VT550 was able to successfully evaluate the fluids. The helical ribbon was 3.4 cm in height and 3.3 cm in diameter. Agrawal (2001) determined the k" and k' values as 12566 rad m'3 and 1.38 rad", respectively, for this mixer viscometer system. 4.2. Experimental Materials Home Harvest Pure Honey (United Wholesale Grocery Company, Grand Rapids, MI) and Karo Light Corn Syrup (Bestfoods, Englewood Cliffs, NJ) were the Newtonian fluids used to determine k " for the interrupted helical screw impeller system. All food samples were purchased at a local grocery store. Three standard power law fluids were used to determine k ': 2.5% and 2.0% (by weight) hydroxypropyl methylcellulose (Dow Chemical Company, Midland, MI) and 23 1.0% guar gum (Sigma Chemical, St. Louis, MO). The hydroxypropyl methylcellulose solutions were prepared by the hot/cold technique for aqueous media as directed by the manufacturer. The guar gum solution was prepared by directly adding the powder to room temperature deionized water. The food products with particulates chosen for this investigation were Ragu Old World Style Traditional pasta sauce (Lipton, Englewood Cliffs, NJ), Prego with Fresh Mushrooms pasta sauce (Campbell, Camden, NJ), Chi-Chi’s Restaurante Fiesta Thick and Chunky salsa (Hormel Foods, Austin, MN), and Del Monte Sweet Corn Cream Style (Del Monte, San Fransisco, CA). Table 4.1 lists all the ingredients in each food product. Dinty Moore Beef Stew (Hormel Foods, Austin, MN) and Bush’s Original Baked Beans (Bush’s, Knoxville, TN) were initially explored but rejected as test subjects for reasons to be discussed later. Table 4.1. Ingredient list of the fluid foods with large particulates selected for testing. Food Ingredients Cream Corn Corn, water, modified food starch, sugar, salt (for flavor) Prego Tomato puree (water, tomato paste), diced tomatoes, corn syrup, vegetable oil (corn cottonseed, and/or canola), mushrooms, salt, spices (Basil, Oregano and other spices), onion powder, dehydrated garlic, citric acid, dehydrated parsley, spice extract. Ragu Tomato puree (water, tomato paste), soybean oil, high fructose corn syrup, salt, dried onions, extra virgin olive oil, Romano cheese (cow's milk, cheese cultures, salt, enzymes), spices, natural flavor Salsa Tomatoes, Jalapeno peppers, water, tomato paste, onions, vinegar, salt, sugar, garlic powder, onion powder, spices, sodium benzoate (to retard spoinlage after opening), citric acid, natural flavor 24 4.3. Data Collection Method 4.3.1. Phase Characterization The particulate foods were emptied onto the Ms inch sieve in an even layer, enough to cover the entire screen. A collection pan underneath the sieve caught the draining fluid. Gravity and slight manual agitation of the sieve facilitated the separation of solid and liquid components. When the drainage had abated, the two phases were ready for analysis. Each phase was weighed separately. Three sieving trials were run using fresh samples. The solids portion was divided into the different groups of food present, such as tomatoes, onions, and corn kernels. Ten of each type of food were randomly chosen and measured in three directions: a, b, and c. a is the longest dimension, b is the longest dimension perpendicular to a, and c is the longest dimension perpendicular to both a and b. This method of characterizing the shapes was recommended by Mohsenin (1986). Rheological pr0perties of the fluid portion were determined at room temperature (23 °C) with the helical ribbon system. A steady-state shear rate ramp up from 1 s'1 to 27 s" and then back down from 27 s'1 to 1 s'1 was conducted for each sample. Two-second equilibrating times were assigned to each data point. Three repetitions of each fluid food were conducted. 4.3.2. Determination of Mixer Viscometry Constants (k " and k ') The reference fluids included Newtonian fluids (corn syrup and honey) and non- Newtonian fluids (methylcellulose and guar gum solutions). The flow properties of the reference fluids were evaluated at room temperature (23 °C) using the MVl concentric cylinder. Shear rates ranged from 10 s'1 to 100 s'1 for the corn syrup and 3 s'1 to 23 s‘1 for 25 the honey. The differing maximum shear rates were based on the torque capacity of the instrument. The steady state test consisted of increasing and decreasing through the shear rate ranges twice. Each ramp was divided into 10 steps with a 30 second equilibrium time taken before a viscosity reading was recorded. Two repetitions of corn syrup and honey were completed. Apart from the different shear rate ranges, the Newtonian data collection method was repeated for non-Newtonian fluids. For 1.0% guar gum, the range was 20 s'1 - 150 s' ‘; for 2.0% Methylcellulose, 30 s‘1 — 250 s"; and 2.5% Methylcellulose, 10 s" — 70 s“. The different shear rate ranges represent the obtainable torque ranges for each fluid. Each fluid trial was duplicated with fresh samples. The constant, k ", of the interrupted helical screw system was determined using the Newtonian fluids at room temperature (23 °C). Approximately 500 ml of a reference fluid was loaded into the glass beaker. The container was raised into position until the top of the highest blade was just below the fluid surface (Figure 4.2). The impeller was centered in the beaker using a ruler. A bubble balance was used to assure a level testing surface. A steady state ramp up test ran from 1 rad s’1 to 30 rad s'1 and from 0.5 rad s'1 to 12 rad s'1 for the corn syrup and honey, respectively. The torque capacity of the Haake VT550 was reached at the respective maximum angular velocity for each fluid. Each test consisted of thirty steps with an acquisition time of thirty seconds for each torque measurement. Two trials were conducted for each fluid. The procedure to determine k ' of the interrupted helical screw system was carried out at room temperature (23 °C). Samples were loaded in the same manner as for the k " trials. The steady-state test for guar gum and 2.0% Methylcellulose consisted of 25 steps, 26 ramping up from 1 rad s'I to 30 rad s", in thirty second increments. While the protocol was identical to the former two fluids, the maximum angular velocity for the 2.5% . Methylcellulose was 20 rad 5". Two tests were executed for each fluid. 4.3.3. Particulate Food Flow Behavior 4.3.3.1. Room Temperature The food products were tested at three different application temperatures: a cold refrigerated temperature, ambient temperature, and a hot serving temperature. The particulate foods were emptied from their original containers into a large, separate beaker. Since large particulates may settle during storage and shipping, slow and gentle manual mixing with a spoon for approximately 15 seconds was done to create a homogenous mixture. Loading of the samples into the testing apparatus was completed as outlined for k". Preliminary tests revealed that a pre-shearing phase to eliminate slight time-dependent behavior was necessary for some foods. This pre-shear session consisted of rotating the interrupted helical screw impeller for 100 seconds at 5 rad 8". Table 4.2 notes which products and temperature settings required the pre-shear test. Table 4.2. Fluid food products with particulates that did and did not require a pre-shear phase. Food Product Cold Room Hot Cream Corn X X - Prego X X - Ragu - - - Salsa X X X X pre-shear; - no pre-shear 27 After the pre-shear, the particulate foods were all subjected to a steady state test: 3 rad 5" through 20 rad s"; and 20 rad 3'1 through 3 rad s". 30 torque measurements were recorded in each direction with a 2 second equilibrating time for every point. The presence of slip and particulate interaction were carefully monitored. Ten repetitions, the minimum number to calculate a standard deviation (Bafna, 1995), were completed for each brand of food using fresh samples each time. 4.3.3.2. Hot Testing Samples were loaded in the glass beaker containers as done for the room temperature trials and covered. The containers were placed into the oven, set at a temperature of 90 °C. When the samples had reached a temperature comfortably over 80 °C, they were quickly transported to the Haake VT550. The temperature at the time of testing was approximately 80 °C with a temperature drop of 3 to 4 °C throughout the duration of the test. The setup and testing protocol was the same as that described for the room temperature tests. A pre-shearing section was not conducted for cream corn, Prego, or Ragu because no time-dependent behavior was evident from preliminary trials. Ten trials of each food product were completed. 4.3.3.3. Cold Testing Samples, already loaded into the testing containers, were placed in a kitchen refrigerator. The samples were allowed to equilibrate to approximately 6 °C before being tested. Temperature differences between the beginning and the end of the test were maintained at less than 2 °C. The setup and testing protocol followed the room temperature testing procedure. A pre-shear section was incorporated into the test for 28 cream corn, Prego and the salsa to eliminate time dependency. Ten replicates were made of each product. 4.4. Data Analysis 4.4.1. Phase Characterization To characterize the solid phase, averages of the measurements in each direction were taken of each food type (onions, peppers, mushrooms, etc.). Torque and angular velocity data from the helical ribbon system were used to evaluate the fluid phase. Apparent viscosity was calculated using Equation [3.17] and Equation [3.7] was used to calculate the average shear rate. The rheological parameters were determined by regression analysis of apparent viscosity versus average shear rate plots using the power law model (Equation [2.4]). 4.4.2. Determination of Mixer Viscometry Constants (k " and k ') The RheoWin2 software automatically converted the data to viscosity and shear rate readings for the concentric cylinder tests. Averages were taken of the Newtonian viscosity readings for a representative value for each Newtonian fluid. Rheograms of apparent viscOsity versus shear rate were made and regression analysis was performed to determine the K and n values of the non-Newtonian fluids. The raw data used from the interrupted helical screw impeller trials were torque and angular velocity. Based on Equation [3.13], a plot of Newtonian viscosity times angular velocity versus torque was constructed from the Newtonian fluid data. The slope of the line was equal to k". k' was determined using Equation [3.14] for each of the non-Newtonian standards. A plot of k' versus angular velocity was produced to show any dependency on n and mixing speeds. 29 4.4.3. Particulate Food Flow Behavior Using the newly determined mixer viscometer constants, apparent viscosities and average shear rates were calculated with Equations [3.17] and [3.7], respectively. The flow behavior of the particulate foods was characterized by a rheograrn of ln 1] versus ln 7,. Results were compared for temperature dependence and to the properties of the fluid phase determined using the helical ribbon system. 4.4.4. Regression Control Charts The general procedure to set up regression control charts is outlined by Mandel (1969). In the current study, a linear plot of ln 77 versus 1n 7, was chosen as the quality control condition. Ten trials of each food type at a certain temperature were averaged to produce one characterizing control line. The standard error based on the predicted y is se = "I -n(nl_—2)] "Z yz “ (Z Y)2 - [nznx§;(2?(2:(§):zy)]z [41] Three times the standard error above and below the control line were drawn as the limits of the regression chart. 3O CHAPTER 5 5. Results and Discussion 5.1. Phase Characterization The result of separating the fluid and solid phases of the particulate foods is illustrated in Figure 5.1. Ragu pasta sauce contained the highest liquid portion by weight, while salsa had the highest amount of solids. Table 5.1 lists the average measurements of a (maximum dimension), b (maximum dimension perpendicular to a), and c (maximum dimension perpendicular to a and b) for each food type in all the particulate food products. Also included in Table 5.1 is the range of measurements taken for each dimension. The tomato pieces in the salsa were the largest at nearly 2 cm. The largest particulate in each product was close to 1 cm and above. Some of the dimensions of the spices and small onion and garlic flakes were not measured because they were considered insignificant. Power law models best fit the flow behavior of the particulate food fluid phase. The rheological parameters for each fluid phase measured using the helical ribbon are listed in Table 5.2. The fluids of the cream corn and salsa had similar, low consistency coefficient values. Prego and Ragu fluids had similar flow behavior indices; while the cream corn fluid was the least shear-thinning. 31 100% 80% 60% 40% 20% 0% F Liquids D Solids Cream Corn Prego Ragu Salsa Figure 5.1. Percentage by weight of solid and fluid phases in foods with particulates. 32 Table 5.1. Measurements a, b, and c and the ranges of each dimension of foodstuffs in the fluid food products. Food Product Average 3 Range* Average b Range* Average c Range* (cm) (cm) (cm) (cm) (cm) (cm) Cream Corn -Kernel 1.00 0.33 0.81 0.32 0.44 0.20 Prego -Tomato 1.48 0.65 1.23 0.93 0.68 0.77 ~Mushroom 0.81 0.34 0.74 0.25 0.61 0.49 -Onion/Garlic 0.64 0.54 0.29 0.30 —Spice 0.90 1.04 Ragu -Onion 1.24 1.20 0.35 0.22 0.19 0.14 Salsa -Tomato 1.94 1.46 1.27 0.61 1.00 0.91 -Pepper 1.09 0.44 0.79 0.60 0.47 0.35 -Onion 0.99 0.36 0.83 0.45 0.36 0.26 -Seed 0.36 0.19 0.14 0.06 ' *Highest value - lowest value Table 5.2. Power law, rheological parameters of the fluid phase of foods with particulates at 23 °C determined by the helical ribbon system. Food K n R2 (Pa 8“) (-) Cream Corn 3.2 0.43 0.981 Prego 23.8 0.17 0.997 Ragu 18.8 0.19 0.993 Salsa 3.4 0.29 0.987 33 5.2. Mixer Viscometry Constants (k " and k ') The pr0perty values of the standard fluids are listed in Table 5.3. A graphical representation of Equation [3.13] as Newtonian viscosity times angular velocity versus torque was constructed (Figure 5.2) utilizing the Newtonian standards. The mixer coefficient constant (k"), equal to the slope, was found to be 3047.4 rad rn’3 with a R2 >0.99. This value is unique to the specific geometry of the interrupted helical screw/cup system used in this study. Table 5.3. Rheological parameters of the standard fluids at 23 oC used to evaluate k" and k'. Standard Fluid p. K n (Pa 8) (Pa 8") 0 Honey 7.5 1.00 Corn Syrup 2.3 1.00 1.0% Guar Gum 7.6 0.29 2.0% Methylcellulose 9.9 0.54 2.5% Methylcellulose 16.8 0.59 34 100 *3 0 Corn Syrup X Honey , I 53. 80 ~ ' .é‘ . .8. , .3 5' § 60 - .5 .9? g Q . " ' Slope = 3047.4 * (i " .4.) r b x ‘ 8 20 ,_ . o O 8 . ' s , O 1 1 1 1 1 1 0.000 0.005 0.010 0.015 0.020 0.025 0.030 0.035 Torque , uNm Figure 5.2. Viscosity times angular velocity versus torque for the interrupted helical screw impeller with Newtonian standard fluids for the determination of the mixer coefficient constant, k" at 23 °C. k' was determined using Equation [3.14] for each non-Newtonian standard fluid. The data show that k' varies with angular velocity and n (Figure 5.3). However, when focusing on data from 3 to 30 rad s", the k' values become relatively independent of angular velocity. A value of 1.6 rad" was determined for k' by plotting the average shear rate versus the angular velocity for each material. The slope of the regressed line for all the data was taken as the mixer viscometer constant. This finding is comparable to other studies (Qiu and Rao (1988), Rao and Cooley (1984), and Lai et al (2000)). An approximate value of k' is acceptable because it is used to estimate the average shear rate. The actual shear rate varies widely during mixing. The suitability of this value was verified against a conventional rheometer using ketchup. Table 5.4 compares the 35 regression curves of the ketchup data for each instrument. The match is not exact but adequately close because the k' value is an estimate. 10 A 1.0% Guar Gum (n = 0.29) 8 _ B D 2.0% Methylcellulose (n = 0.54) 0 2.5% Methylcellulose (n = 0.59) '7 6 'o -o 8 o a .34 _ fl 4 g B o B a 2 30 38330403550“. 5°05 u u a ” u u a a A 5 585 0200555055.} 0 l l I l l 0 5 10 15 20 25 30 Angular Velocity, rad s’1 Figure 5.3. Mixer viscometer constant, k', versus angular velocity for the interrupted helical screw impeller using non-Newtonian standard fluids at 23 °C. Table 5.4. Comparison of the interrupted helical screw impeller and concentric cylinder using ketchup at 23 °C. Instrument K n R2 (Pa 8“) (-) Interrupted Helical Screw Impeller 27.1 0.23 0.979 Concentric Cylinder 23.8 0.22 0.993 5.3. Particulate Food Flow Behavior Figure 5.4 shows a typical plot of the raw data scatter for one run using the interrupted helical screw impeller and Prego sauce at the cold temperature (8 °C). The resulting trend showing torque to be linearly related to angular velocity was found for all 36 the products with particulates. Each product exhibited a high level of variation in torque response most probably due to the impeller blades coming in contact with different particulates. Variation between tests was attributed to the slightly different composition of particulates in each test batch. Cold Prego 6 Torquex10,Nm moofia’a‘o o 8 8 § § § § l l l i 0 5 10 15 20 25 Angular Velocity, rad s’l Figure 5.4. A typical raw data set from one trial using the interrupted helical screw impeller with Prego sauce at 8 °C. Using the value of k' and Equation [3.7], the average shear rate range for testing the fluid foods with particulates was 4.8 s‘1 to 32 s". By taking the logarithm of each side of Equation [2.4], a linear relationship between apparent viscosity and average shear rate is formed: ln 77=ln K+(n—l)ln 70 [5.1] 1n 7] versus In 70 was plotted for cream corn, Prego, Ragu, and salsa (Figures 5.5 — 5.8). The regressed lines for all three temperatures appear on each figure. The upper range of 37 the angular velocity (17.1 rad s'l - 20 rad s") for the salsa trials at hot temperature was eliminated from analysis because excessive slip (a violation of a basic assumption) was observed at the wall of the container. Data results were no longer linear for those conditions. 2.5 . 0 Cold U Room A Hot w o 5?. 2 ' o 0 Cream Corn . E o 5‘ 9 ° 0 '5 2 R O 0 O .E A D D O 0 o > A A D D 0 ‘E AAEDDDD °°°°°o g l P Abbagnnunng 0% Q. A AA 0 2‘ AAAAZZDQE' 5 0 5 ‘ “MM 0 l l l 1.5 2 2.5 3 3.5 In Average Shear Rate, 5’1 Figure 5.5. 1n 11 versus 1n ya for cream corn at cold (5 °C), room (23 °C) and hot (80 °C) temperatures using the interrupted helical screw impeller. 38 P Ln o D o 0 Cold 0 Room A Hot 0 o 5: 2 ‘ a 0 >2 A D 3 ° .0 Prego 3.: A D D o m 0 o 1 5 .. A '3 :1 ° 0 8 A °n°° > A no °o¢ 0.5 A an O t: A CH3 00° 1 _ A DD 00 g A A A ”DDCGWO & A A A < “AAA 5 0.5 ' A AAA 0 L 1 4 1.5 2 2.5 3 3.5 In Average Shear Rate, 5'1 Figure 5.6. ln 7] versus ln 7, for Prego at cold (8 °C), room (23 °C) and hot (80 °C) temperatures using the interrupted helical screw impeller. 1.8 o 0 Cold 0 Room A Hot 8 0 ° N D o o 9" l 2 r U o Rag“ 5: A U D O 0 '8 A D o o 8 A D 0 ° 0 o > 0.6 ‘ A D a 0 o G A A Dan °°o :a A A an 000° < 0 * A A A .5 AAAA AAA -06 . . 4 1.5 2 2.5 3 3.5 In Average Shear Rate, s'1 Figure 5.7. 1n 1] versus ln ya for Ragu at cold (7 °C), room (23 °C) and hot (80 °C) temperatures using the interrupted helical screw impeller. 39 E" U! 0 Cold 0 Room A Hot 0 23 2 - ° . 9* 0 ° 0 Salsa >1 n .5 a a g 1.5 - o o E A D :1 ° ° 0 c: a o 1 _ A D u °o° g A A ”a 0°00 D. A Dunn °°OQ 2‘ A A A an 00 5 0.5 - A A A A A A A A AAAAA 0 1 1 1 AL 1.5 2 2.5 3 3.5 In Average Shear Rate, 3‘1 Figure 5.8. 1n 11 versus 1n ya for salsa at cold (7 °C), room (23 °C) and hot (80 °C) temperatures using the interrupted helical screw impeller. All products exhibited similar slopes over the temperatures studied, and the lowest temperature trial always produced the highest apparent viscosity readings. Table 5.5 lists the regressed K and n values at each temperature for all four products. The temperatures listed are average values. The n values do not appear to be a strong function of temperature. As the temperature increases, the consistency coefficient decreases for all food products except for cream com. 40 Table 5.5. Rheological parameters for foods with particulates at cold, room, and hot temperatures using the interrupted helical screw impeller. Fluid Food K n R2 Temperature (Pa 8“) (-) (°C) Cream Corn ~Cold 23.8 0.35 0.854 5 -Room 17.9 0.36 0.871 23 -Hot 20.4 0.26 0.979 80 Prego -Cold 40.3 0.19 0.978 8 -Room 38.3 0.17 0.959 23 -Hot 21.8 0.18 0.984 80 Ragu -Cold 15 .9 0.26 0.969 7 -Room 13.7 0.24 0.959 23 -Hot 10.1 0.20 0.988 80 Salsa -Cold 30.8 0.20 0.957 7 -Room 22.6 0.23 0.932 23 -Hot 10.9 0.28 0.877 80 Figure 5.9 is a graphical representation of the logarithm of Equation [2.5]. An intermediate average shear rate of 18.88 s’1 was chosen to compare apparent viscosities at each temperature. Apparent viscosity is clearly dependent on temperature. The slope (activation energy) and y-intercept (constant A) were determined by regression analysis of these plots and compared in Table 5.6. Looking at the energy activation terms, salsa’s apparent viscosity changes the most with temperature. 41 1.4 1.2 I 1.0 - 0.8 + 0.6 - 0.4 - 0.2 - 1n Apparent Viscosity, Pa 8 0.0 F -0.2 ‘ X Cream Corn El Prego 0 Ragu A Salsa 0.0025 0.003 Figure 5.9. 1n 1] versus 1/T at 18.88 s'1 for each fluid food with particulates using the interrupted helical screw impeller. Table 5.6. Activation energy and A values for each fluid food with particulates using the interrupted helical screw impeller. . 0.0035 l/T, 1/K Product Eo/R A R2 Cream Corn 561 0.45 0.879 Prego 898 0.15 0.995 Ragu 840 0.09 0.999 Salsa 1057 0.07 0.997 Figure 5.10-12 depicts regression lines of each product at cold, room and hot temperatures respectively on a 1n 1] versus ln 7“ plot for comparison. Ragu pasta sauce was consistently the least viscous. Prego, Ragu, and salsa had similar slopes; while 42 0.004 cream corn intercepted the salsa and Prego lines at cold temperature and only the salsa line at room temperature. At the cold and room temperatures, Prego was the most viscous of the food products. For the hot temperature, the cream corn was more viscous thanPrego. 2.5 t 2 E] XCream Corn UPrego ORagu ASalsa m E] a“: 2 ” X z; U C] a? K 5 £30 9 .53 0 X §15_ ° 0 “Aggggg S 0 0 A R’v E: 000 5 05 P °°°°°W 0 1 l 1 1.5 2 2.5 3 3.5 In Average Shear Rate, 3’1 Figure 5.10. 1n 1] versus ln 70 of fluid food products with large particulates at cold temperature (5-8 °C) using the interrupted helical screw impeller. 43 E" m El [XCreamCorn DPrego ORagu ASalsaJ _ El 195 N C] 1n Apparent Vrscosrty, Pa s c O Ur t— <> 0 0 0 0 0 OX 0 DX DX DX DX DX X ' DX 395 if 3 6 u u m D< I .O U! p—0 U1 N 2.5 3 3.5 In Average Shear Rate, 3'1 Figure 5.11. 1n 7] versus 1n 7a of fluid food products with large particulates at room temperature (23 °C) using the interrupted helical screw impeller. 2 fi XCream Corn DPrego ORagu ASalsa m a 6 53 1.5 - E 6 >2 A 6 x x g 1 . A A '3 :1 x xx .E 0 A DC] XXX > . <> 0 A A UUUDXX a 0 AAA 23 A 8 ° 0 o o AAAAA . < O -05 . . , 00M 1.5 2 2.5 3 3.5 In Average Shear Rate, 5'1 Figure 5.12. 1n 11 versus 1n 70 of fluid food products with large particulates at hot temperature (80 °C) using the interrupted helical screw impeller. Table 5.7 contrasts the power law parameters for the whole fluid food and the fluid phase analyzed by the helical ribbon at room temperature (23 °C). Similar shear rates were selected for each instrument (4 s'1 to 27 s“) for a fair comparison. Relatively speaking, there is a large increase in the consistency coefficient that corresponds with the loading of particulates for all products except Ragu. The similarity of the results reflects the small amount of particulates in the fluid initially, and therefore, small effect in the fluid. Based on the flow behavior indices, the fluid phase appears to be less shear- thinning than the complete product with the particulates included. These findings are in agreement with past investigations (Bhamadipati and Singh, 1990). Table 5.7. Comparison of the rheological parameters of whole fluid food products with large particulates at room temperature (23 °C) using the interrupted helical screw impeller to the fluid phase at room temperature (23 °C) using a helical ribbon. Fluid Food K n R2 (Pa 8“) (-) Cream Corn 18.5 0.34 0.854 Cream Corn Fluid 2.8 0.47 0.955 Prego 38.9 0.16 0.952 Prego Fluid 22.3 0.19 0.993 Ragu 14.2 0.22 0.953 Ragu Fluid 17.7 0.21 0.980 Salsa 23.8 0.21 0.936 Salsa Fluid 3.09 0.33 0.965 45 Preliminary trials of Bush’s Baked Beans and Dinty Moore Beef Stew were unsuccessful. The baked beans exhibited high particle—to-particle interaction and appeared to move as a whole entity rather than moving as discrete particles, which indicates excessive slip. Another issue of concern with the beans was the observation of particle degradation during testing. Also, the beef stew particulates (the largest tested in this investigation) became jammed between the impeller and side of the beaker. 5.4. Regression Control Charts 1n n were plotted against In in for each food product with large particulates at each temperature. Figure 5.13, a plot for Prego pasta sauce at cold temperature, is an example of typical results. All ten repetitions are represented in the figure. Linear regression produced an average control line and the upper and lower control limits for each figure. Due to the wide spread of the data, the control limits are based on three times the standard error rather than two. This allows for a lower risk of false alarms. Table 5.8 compares the standard errors for each food product at each temperature. The lower average standard error values correspond to the food products with lower percentages of solids by weight. Temperature did not affect the standard errors in a consistent manner. One trial from cream corn and Ragu at room temperature appear separated from the rest of the data pool. When reviewing the circumstances of the tests, no extraordinary conditions were recorded; therefore, these outlying test trials were included in the analysis. 46 ColdPrego ‘0 2.5 - «3 a. 3;; 2 - o .8 > 1.5 ~ 7% ‘3. 1 . o. < E 0.5 - O r r r 1.5 2 2.5 3 3.5 In Average Shear Rate, 3'1 Figure 5.13. 1n 11 versus ln 7“ for Prego sauce at cold temperature (5 °C) using the interrupted helical screw impeller. 47 Table 5.8. Comparison of standard errors for each fluid food with large particulates at each temperature. Fluid Food Standard Error of 1n 1] Data Cream Corn -Cold 0.142 -Room 0.131 -Hot 0.057 Average 0.1 10 Prego Hot -Cold 0.064 ~Room 0.091 -Hot 0.056 Average 0.070 Ragu -Cold 0.071 -Room 0.083 -Hot 0.048 Average 0.067 Salsa -Cold 0.090 -Room 0.1 10 -Hot 0.130 Average 0.1 10 5.5. Statistical Quality Control Protocol Using the interrupted helical screw impeller, a quality control program can be established for fluid food products with large particulates. Based on steady-state shear ramp tests similar to this study, regression control charts can be produced. The number of trials on acceptable product samples to establish the control line and control limits is a 48 management decision based on the variance of the product. Recommended values differ between authors (Bafna, 1995; Hubbard, 1990). Personnel can run a test on the product and compare results to the established control chart. The management would decide the frequency of the testing. The most thorough assessment would be to run the same steady state ramp up—and—down test and compare the regressed curve to the control chart. Occasional outlying points, caused by random particulates colliding with the'impeller blade may be eliminated from the data p00] using residual analysis. If the result lies within the limits, then the product is in accordance with accepted values. A test result that intersects a control line indicates a problem with the flow behavior index; whereas, a test line that runs parallel to the control line but outside the control limits, indicates an unacceptable value of K. The protocol for actions to be taken when a product is found to be out of specification is a management decision, that may involve reformulation or disposal. Another quality control test option using the regression control chart is to determine the apparent viscosity at two different shear rates and see if the points are located within the control limits. This test would only give a general indication of how the product behaves because it is based on only two points. Adding more apparent viscosity point tests would make the quality control procedure more laborious, but may be necessary with some products. Single point testing is generally unacceptable with shear-thinnin g products. This type of test and regression control chart for quality control purposes is aimed at batch processes rather than continuous. This type of chart is not as suitable to follow the progress of a process with time because the chart represents only one test result. 49 Separate tests could be run at different points in the processing of the product. Another use for regression control charts is in product development of fluid foods with large particulates. The results can be compared with acceptable rheological parameters of competing products. 50 CHAPTER 6 6. Summary and Conclusions A mixer viscometer impeller modeled after an impeller used to evaluate the rheological properties of fresh concrete was successfully designed and constructed. Using Newtonian fluids, it was characterized by a mixer coefficient constant (k") value of 3047.4 rad m’3. The mixer viscometer constant (k') was determined with non- Newtonian fluids to be 1.6 rad'l over the angular velocity range of 3 — 30 rad s'l. The interrupted helical screw impeller was effectively used to evaluate the rheological behavior of fluid foods with large particulates. Apparent viscosity measurements were obtained and power law parameters were found using regression analysis for cream corn, salsa, a smooth pasta sauce and a chunky pasta sauce at typical application temperatures: cold (6 °C), room (23 °C), and hot (80 °C). The largest particulates in each food ranged from approximately 1 cm to 2 cm in the longest direction. There was variation within a single test and between tests due to the positioning and quantity of particulates in the samples. However, a definite trendcould be determined: higher particulate loading resulted in higher standard error values. Apparent viscosity was found to decrease with increasing temperature. For cream corn, Prego, and salsa, K was larger for the whole product versus only the fluid phase. The chunky pasta sauce was the most viscous, followed by cream corn, salsa, and then the smooth pasta sauce at room temperature. Regression control charts of 1n 7] versus ln ya were made for all the food products investigated at each temperature. The control line and control limits represent the 51 acceptable range of flow behavior for each product. Such charts can be established in food manufacturing facilities for quality control purposes. Fluid foods with large particulates can be tested using the interrupted helical screw impeller and compared to a regression control chart. This is a valuable discovery to the food industry because currently no standardized test exists to assess objective parameters of such foods. The ability to quantitatively test rheological properties of fluid foods containing large particulates is also important for process design calculations involving pipeline design, mixing and pumping. 52 CHAPTER 7 7. Future Research The following topics are recommended for future study: 1. Expanding the pool of large particulate fluid foods analyzed to include items such as fruit preserves and chunky soups. 2. One specific brand was chosen to represent each type of food considered in the current study. Evaluating different brands, of similar large particulate products for comparison of rheological parameters is suggested. 3. In this study, the amount of solids in the fluid foods affected the rheological parameters. Future study correlating particulate loading (size, shape and volume) with changes in flow behavior is recommended. 4. Determining the range of sizes and loading of particulates appropriate for the interrupted helical screw impeller in this study. 5. Studying the effect of different gap sizes. 6. Constructing a permanent temperature control device for the testing container. 53 7. 10. Beef stew contained particulates that were of a size inappropriate for this study. A scaling investigation is suggested to address extraordinarily sized particulates. First, a basis for sealing must be determined. The author suggests scaling on a geometrical basis. Next, a relationship must be developed between the particulates in question and the impeller system for sealing. lrnportant factors must be established, such as blade size and gap size, so if distortion is necessary, those design factors will not be sacrificed. Torque capacity of the instrument may become an important issue with large impellers. The quality control plan for this study was aimed at batch processes, and therefore did not lend itself to monitoring historical trends in results. A method is needed to measure the progress with time of the rheological parameters of fluid foods using statistical quality control applications. Multivariate quality control was investigated for monitoring K and n values; however, the process involved complex statistical analysis inappropriate for typical food plant environment. Designing a software program to easily carry out multivariate quality control calculations would greatly simplify the process. This technique may be useful in some applications. Using rheological data found by the interrupted helical screw impeller system to model pipeflow problems found in aseptic processing systems. 54 APPENDIX: Typical experimental data for the interrupted helical screw impeller 55 Table A.1. Interrupted helical screw impeller data to determine k" using Newtonian fluids at 23 °C. Fluid Angular Velocity Torque x 1045 Viscosity (rad/s) (Nm) (Pa 5) Corn Syrup 1.04 722 2.3 2.07 1454 3.10 2188 4.14 2930 5.17 3660 6.21 4400 7.24 5146 8.26 5860 9.30 6568 10.40 7310 1 1.40 8030 12.40 8802 13.40 9510 14.50 10260 15.50 1 1000 16.60 1 1760 17.60 12510 18.60 13270 19.70 14060 20.70 14840 21.70 15640 22.80 16390 23.80 17220 24.80 18000 25.90 18870 26.90 19660 27.90 20490 29.00 21250 30.00 22040 56 Table A.1. (cont’d) Fluid Angular Velocity Torque x 1043 Viscosity (rad/s) (Nm) (Pa 3) Honey 0.42 1068 7.5 0.83 2082 1.25 3180 1.65 4236 2.07 5300 2.48 6314 2.90 7390 3.31 8410 3.73 9466 4.14 10480 4.55 1 15 10 4.96 12560 5.38 13600 5.79 14580 6.21 15650 6.62 16640 7.04 17650 7 .43 18620 7.86 19660 8.26 20630 8.70 21720 9.09 22650 9.51 23670 9.94 24680 10.40 25680 10.80 26690 1 1.20 27580 1 1.60 28660 12.00 29520 57 Table A2. Interrupted helical screw impeller data to determine k' using non-Newtonian fluids at 23 °C. Fluid . Angular Velocity Torque x 10'6 (rad/S) (N m) 1% Guar Gum 0.03 74 1.28 1300 2.53 1900 3.78 2310 5.03 2630 6.27 2880 7.53 3090 8.77 3290 10.00 3470 l 1.30 3650 12.50 3820 13.80 4010 15.00 4180 16.30 4370 17.50 4550 18.80 4740 20.00 4930 21.20 5120 22.50 5320 23.80 5530 25.00 5750 26.30 5960 27.50 6190 28.70 6430 30.00 6670 58 Table A2. (cont’d) Fluid Angular Velocity Torque x 106 (rad/s)- (N m) 2.0% Methylcellulose 0.03 24 1.28 1370 2.53 2470 3.78 3440 5.03 4340 6.27 5160 7 .53 5920 8.77 6640 10.00 7320 l 1.30 7970 12.50 8590 13.80 9200 15.00 9770 16.30 10300 17.50 10900 18.80 1 1500 20.00 12000 21.20 12500 22.50 13100 23.80 13600 25.00 14100 26.30 14600 27.50 15100 28.70 15600 30.00 16100 59 Table A2. (cont’d) Fluid Angular Velocity Torque x 1045 (rad/S) (N m) 2.5% Methycellulose 0.03 90 0.87 2480 1.70 4320 2.53 5990 3.36 7450 4.19 8800 5.03 10100 5.85 1 1200 6.69 12300 7 .53 13400 8.35 14400 9.19 15300 10.00 16200 10.80 17100 11.70 17900 12.50 18800 13.30 19500 14.20 20300 15.00 21000 15.80 21700 16.70 22400 17.50 23000 18.30 23700 19.20 24300 20.00 24900 60 Table A3. Interrupted helical screw impeller data for cream corn. Angular Velocity Torque x 10'6 (rad/S) (Nm) 5 °C 23 °C 80 °C 3.0 8530 6860 65 80 3.6 9430 6860 6730 4.2 10400 7050 6320 4.8 10700 7120 6600 5.3 1 1200 7660 6890 5.9 11500 8520 7170 6.5 11600 8120 6830 7.1 12700 8430 7740 7 .7 12300 8850 7980 8.3 12600 8920 7950 8.9 13200 9150 7750 9.4 13300 9260 8200 10.0 13500 9100 8280 10.6 14200 9990 8040 1 1.2 13900 9590 8370 l 1.8 13900 9760 8500 12.4 14300 9660 8780 13.0 13700 10300 8950 . 13.6 14500 10800 9140 14.1 14800 11100 8810 14.7 14900 10300 9140 15.3 15400 10300 9140 15.9 15500 11400 9210 16.5 16000 11400 8820 17.1 15700 11600 9010 17.7 16300 11700 9310 18.3 16100 11900 9060 18.8 16600 12300 9600 19.4 16100 11800 9630 20.0 16500 12500 10200 61 Table A3. (cont’d) Angular Velocity Torque x 10'6 (rad/s) (Nm) 5 °C 23 °C 80 °C 20.0 16100 12000 10200 19.4 15600 12200 10500 18.8 15900 11300 10000 18.3 15600 11800 9660 17.7 15100 11500 10200 17.1 15100 11100 9140 16.5 15000 10600 9130 15.9 14700 10900 9460 15.3 14600 9860 8660 14.7 14500 9820 8600, 14.1 13700 9830 8960 13.6 13200 9630 8390 13.0 13300 10500 8400 12.4 12900 8870 7580 11.8 13000 9140 7950 1 1.2 12900 8570 8620 10.6 13000 8970 8800 10.0 12200 8680 8060 9.4 12100 8570 7970 8.9 11900 7870 7310 8.3 11100 8010 7170 7.7 10500 7830 7170 7 .1 10600 7780 7380 6.5 9880 7250 7250 5.9 9620 6800 7200 5.3 9470 6860 6710 4.8 8890 6680 6770 4.2 8860 6410 6470 3.6 8420 6620 6420 3.0 7990 61 10 6010 62 Table A.4. Interrupted helical screw impeller data for Prego. Angular Velocity Torque x 104‘ (rad/s) (Nm) 8 °C 23 °C 80 °C 3.0 10900 11200 5420 3.6 11500 10900 5620 4.2 11400 11600 5870 4.8 11700 11600 6020 5.3 12000 1 1800 6180 5 .9 12200 12200 6290 6.5 12500 12100 6290 7.1 12400 12500 6620 7 .7 12900 12500 6920 8.3 13100 12600 7170 8.9 13500 12500 7290 9.4 13700 13000 7400 10.0 13500 13100 7590 10.6 13500 13100 7520 11.2 13700 13300 7610 11.8 13800 13600 8080 12.4 14300 13200 7720 13.0 13900 13400 7900 13.6 14200 13700 7890 14.1 14500 13800 8040 14.7 14900 14200 8030 15.3 15200 14200 8160 15.9 15500 14100 8170 16.5 15500 14100 8290 17 . 1 15600 14300 8350 17.7 15500 14200 8550 18.3 16000 14600 8440 18.8 15900 14400 8580 19.4 16300 14500 8790 20.0 16000 14600 8940 63 Table A.4. (cont’d) Angular Velocity Torque x 104 (rad/S) (Nm) 8 °C 23 °C 80 °C 20.0 16100 14700 8850 19.4 16000 14800 8180 18.8 15700 14600 8550 18.3 15900 14300 8450 17.7 15500 14200 8320 17.1 15800 14200 8220 16.5 15200 14000 8050 15.9 15000 14000 7980 15.3 14700 13900 8010 14.7 14900 13700 7890 14.1 14300 13600 8050 13.6 14200 13800 7890 13.0 14200 13500 8110 12.4 14600 13200 8110 11.8 13800 13400 7830 11.2 14300 12900 7570 10.6 13600 13000 7680 10.0 13600 12900 7660 9.4 13600 12900 7480 8.9 13500 12600 7420 8.3 13400 12600 7360 7 .7 13400 12500 7360 7.1 13400 12300 7430 6.5 12900 12300 7180 5.9 12600 12000 7020 5.3 12600 12100 6860 4.8 l 1800 l 1600 6910 4.2 1 1900 11600 6720 3.6 12000 11000 6630 3.0 11400 11400 6320 Table A5. Interrupted helical screw impeller data for Ragu. 65 Angular Velocity Torque x 104‘ (rad/s) (Nm) 7 °C 23 °C 80 °C 3.0 5490 4110 3080 3.6 5610 4220 3120 ' 4.2 5790 4380 3170 4.8 5900 4510 3170 5.3 6040 4550 3240 5.9 6160 4640 3270 6.5 6270 4750 3320 7.1 6450 4810 3410 7.7 6610 4860 3460 8.3 6630 4950 3510 8.9 6800 5020 3620 9.4 6820 51 10 3620 10.0 6980 5170 3720 10.6 7110 5180 3800 11.2 7210 5330 3830 1 1.8 7330 5450 3800 12.4 7380 5500 3860 13.0 7510 5600 3930 13.6 7570 5690 4010 14.1 7750 5710 4050 14.7 7830 5800 4060 15.3 7890 6030 4170 15.9 8030 6050 4220 16.5 8040 6030 4260 17.1 8160 6250 4230 17.7 8310 6410 4320 18.3 8400 6550 4360 18.8 8460 6720 4430 19.4 8530 6660 4430 20.0 8590 6620 4520 Table A5. (cont’d) Angular Velocity Torque x 10'6 (rad/s) (Nm) 7 °C 23 °c 80 °C 20.0 8660 6540 4530 19.4 8520 6580 4460 18.8 8490 6440 4380 18.3 8450 6320 4320 17.7 8290 6370 4320 17.1 8260 6310 4250 16.5 8210 6350 4160 15.9 8140 6200 4180 15.3 8060 6110 4090 14.7 7890 5950 4080 14.1 7820 6220 4000 13.6 7700 5980 3980 13.0 7700 5750 3920 12.4 7510 5630 3890 1 1.8 7450 5550 3920 11.2 7330 5500 3850 10.6 7260 5500 3780 10.0 7190 5400 3760 9.4 7010 5370 3710 8.9 6970 5300 3730 8.3 6920 5230 3640 7.7 6840 5140 3590 7.1 6680 5090 3590 6.5 6480 5080 3470 5.9 6380 4960 3450 5.3 6270 4900 3470 4.8 6140 4660 3360 4.2 5960 4670 3340 3.6 5730 4470 3220 3.0 5610 4270 3170 66 Table A6. Interrupted helical screw impeller data for salsa. Angular Velocity Torque x 104‘ (rad/s) (Nm) 8 °C 23 °C 80 °C 3.0 8540 7920 3380 3.6 8050 7910 3860 4.2 8370 7090 4290 4.8 8510 8000 4670 5.3 8910 .8340 3940 5.9 85 80 7960 4130 6.5 9380 8380 4130 7.1 9620 8680 4200 7.7 8840 8590 4550 8.3 8530 8880 4460 8.9 9480 8580 4560 9.4 10000 9340 4580 10.0 9590 9100 4520 10.6 10100 9940 4430 1 1.2 9860 9020 4710 11.8 10200 9320 5570 12.4 10700 9170 5100 13.0 10500 9850 5350 13.6 10300 9620 5020 14.1 10800 11200 5040 14.7 11200 10100 5710 15.3 10500 9860 5740 15.9 10800 10100 5280 16.5 10800 11300 5980 17.1 11100 10400 5750 17.7 12000 10800 6210 18.3 1 1600 1 1600 6420 18.8 11000 12100 6640 19.4 11200 11900 7220 20.0 11200 1 1700 7520 67 Table A6. (cont’d) Angular Velocity Torque x 1045 (rad/s) (Nm) 8 °C 23 °C 80 °C 20.0 11600 11700 7490 19.4 11000 11700 6960 18.8 1 1200 11000 7040 18.3 11100 11400 6770 17.7 10500 10300 6590 17.1 10400 10500 6360 16.5 10200 10800 6080 15.9 10500 9990 5990 15.3 9930 9850 5650 14.7 10100 10200 5590 14.1 10100 10300 5390 13.6 10100 9730 5590 13.0 10100 9980 5300 12.4 10300 9490 5330 11.8 10100 9130 5150 1 1.2 9490 9690 5290 10.6 9530 9030 4870 10.0 8900 8790 4860 9.4 9010 8860 4530 8.9 8850 9390 4380 8.3 8530 8800 4280 7.7 8440 8720 4390 7.1 9120 8300 4.110 6.5 8260 8210 4020 5.9 8170 8170 4020 5.3 7880 8440 3930 4.8 7490 7620 4290 4.2 7470 7730 4000 3.6 7500 7750 3380 3.0 6950 7610 3690 68 LIST OF REFERENCES AGRAWAL, Eva. 2001. Evaluation of fluid foods using a helical ribbon viscometer. MS. Thesis. Department of Food Science and Human Nutrition, Michigan State University, East Lansing, MI, USA. BAFNA, S. S. 1995. The application of statistical process control to rheological measurements. Journal of Applied Polymer Science. 57, 1233-1244. BARTOS, P. 1992. Fresh concrete: properties and tests. El Sevier, Amsterdam. BRIGGS, J.L. and STEFFE, J.F. 1996. Mixer viscometer constant (k’) for the Brookfield small sample adapter and flag impeller. Journal of Texture Studies 27, 671-677. BHAMADIPATI S. and SINGH R.K. 1990. Flow behavior of tomato sauce with or without particulates in tube flow. J. Food Proc. Eng. 12, 275-293. CASTELL-PEREZ, ME. and STEFFE, J .F. 1990. Evaluating shear rates for power law fluids in mixer Viscometry. Journal of Texture Studies 21 , 439-453. CASTELL-PEREZ, ME. and STEFFE, J .F. 1992. Using Mixing to evaluate rheological properties. In: Rao, M.A. (editor). Viscoelastic Properties. Elsevier Applied Science Publishers Ltd., Barking, England. CASTELL-PEREZ, M.E., STEFFE, J .F. and MORGAN, R.G. 1987. Adaptation of a Brookfield (I-IBTD) viscometer for mixer Viscometry studies. Journal of Texture Studies 18, 359-365. CANTU-LOZANO, D., RAO, MA. and GASPARE'ITO, GA. 2000. Rheological properties of noncohesive apple dispersion with helical and vane impellers: effect of concentration and particle size. Journal of Food Process Engineering 23, 373-385. CHATTERJEE, S. and PRICE, B. 1977. Regression Analysis by Example. John Wiley & Sons, New York. DUCLA, J.M., DESPLANCHES, H. and CHEVALIER, J .L. 1983. Effective viscosity of non-Newtonian fluids in a mechanically stirred tank. Chem. Eng. Commun. 21, 29-36. EDWARDS, M.F., GODFREY, J .C. and KASHANI, M.M. 1976. Power requirement for the mixing of thixotropic liquids. Journal of Non-Newtonian Fluid Mechanics. I , 309-322. 69 FERRARIS, CF. 1999. Measurement of the Rheological Properties of high Performance Concrete: State of the art Report. Journal of Research of the National Institute of Standards and Technology. 104, 461-477. HUBBARD, MR. 1990. Statistical Quality Control for the Food Industry. Van Nostrand Reinhold, New York. HUGELSHOFER, D., WINDHAB, E]. and WANG, J. 2000. Rheological and structural changes during the mixing of suspensions and emulsions. Applied Rheology. 10, 22-30. LAI, K.P., STEFFE, J .F. and NG, P.K.W. 2000. Average shear rates in the rapid Visco analyser (RVA) mixing system. LAREO C., FRYER P.J., BARIGOU M. 1997. The fluid mechanics of two-phase solid- liquid food flows: A review. Trans. Institution of Chemical Engineers. 75( C), 73- 105. MACKEY, K.L., MORGAN, R.G. and STEFFE, J.F. 1987. Effects of shear-thinning behavior on mixer Viscometry techniques. Journal of Texture Studies 18, 231-240. MANDEL, B]. 1969. The regression control chart. Joumal of Quality Technology I, 1- 9. MARTINEZ-PADILLA L.P., CORNEJO-ROMERO L., CRUZ-CRUZ C.M., JAQUEZ- HUACUJA C.C., BARBOSA-CANOVAS G.V. 1999. Rheological characterization of a model food suspension containing discs using three different geometries. J. Food Proc. Eng. 22, 55-79. METZNER, AB. and OTTO, RE. 1957. Agitation of non-Newtonian fluids. A.I.Ch.E. Journal 3, 3-10. MOHSENIN, N. N. 1986. Physical properties of plant and animal materials, 2nd Ed. Gordon and Breach, Science Publisher, Inc. New York. NAGATA, S. 1975. Mixing: Principles and Applications. John Wiley and Sons, New . York. PATANKAR, NA. and HU, H.H. 2001. Rheology of a suspension of particles in Viscoelastic fluids. J. Non-Newtonian Fluid Mech. 96, 427—443. PORDESIMO, L0. 1991. Flow behavior of coarse solid-liquid food mixtures. Ph.D. Thesis. The Pennsylvania State University, University Park, PA, USA. PORDESIMO L.O., ZURITZ C.A., SHARMA MG. 1994. Flow behavior of coarse solid-liquid food mixtures. J. Food Eng. 21, 495-511. 70 PURI, S.C., ENNIS, D., MULLEN, K. 1979. Statistical Quality Control for Food and Agricultural Scientists, G. K. Hall & Co., Boston, MA. QIU, CG. and RAO, M.A. 1988. Role of pulp content and particle size in yield stress of apple sauce. Journal of Food Science 53, 1165-1170. RAO, M.A. 1975. Measurement of flow properties of food suspensions with a mixer. Journal of Texture Studies 6, 533-539. RAO M.A. 1987. Predicting the flow of properties of food suspensions of plant origin. Food Technology 41, 85-88. RAO, M.A. and COOLEY, H]. 1984. Determination of effective shear rates in rotational viscometers with complex geometries. Journal of Texture Studies 15, 327- 335. REGER, F. and NOVAK, V. 1973. Power consumption of agitators in highly viscous non—Newtonian liquids. Trans. Instn. Chem. Engrs. 51 , 105-111. SANNERVIK J., BOLMSTEDT U., TRAGARDH C. 1996. Heat transfer in tubular heat exchangers for particulate containing liquid foods. J. of Food Eng. 29, 63-74. SCHUBERT H. 1987. Food particle technology. Part 1: Properties of particles and particulate food systems. J. of Food Eng. 6, 1-32. SESTAK, 1., ZIT NY, R. and HOUSKA, M. 1986. Anchor-agitated systems: power input correlation for pseudoplastic and thixotropic fluids in equilibrium. AIChE Journal. 32,155-158. STEFFE, J .F. 1996. Rheological Methods in Food Process Engineering, 2nd Ed. Freeman Press. East Lansing, MI. STEFFE, J .F. and FORD, W. 1985. Rheological techniques to evaluate the shelf- stability of starch-thickened, strained apricots. Journal of Texture Studies 16, 179- 192. TA'ITERSALL, OH. 1973. The rationale of a two-point workability test. Magazine of Concrete Research 25, 169-172. TATTERSALL CH. and BLOOMER SJ. 1979. Further development of the two-point test for workability and extension of its range. Magazine of Concrete Research 31, 202-210. WALLEVIK OH. and GJORV DE. 1990. Modification of the two-point workability apparatus. Magazine of Concrete Research 42, 135-142. 71 WILDEMUTH, CR. and WILLIAMS, MC. 1984. Viscosity of suspensions modeled with a shear-dependent maximum packing fraction. Rheologica Acta 23, 627-635. 72 iWill/[Ill(11121111111111! ‘ 0