2004 SPRI CONFERENCE

ABSTRACTS OF PRESENTATIONS

April 4 - 7, 2004

Abstracts are presented in alphabetical order according to first author. Abstracts of posters follow this section according to first author.

Measuring Sugar Losses in Brazilian Mills. Henrique V. Amorim, Fermentec, Piracicaba SP, Brazil

Brazilian mills produce 14 x 10⁹ liters of ethanol and 23 x 10⁶ tons of sugar per year. Many factors affect industrial efficiency, but the losses of sugar are very significant. Without measuring the losses, it is impossible to control and to manage the factory with high efficiency. The main losses measured in Brazilian mills are the amounts of sugar in sugarcane wash-outs, filter cake, barometric column and residual waters. During the last harvest season, the losses varied from 0.06 to 1.05% of sugar in sugarcane wash-outs, 0.19 to 2.60% in filter cake, 0.01 to 1.49% in barometric columns, 0.025 to 1.78% in residual waters and 2.5 to 8.0% in bagasse (extraction). Data will be presented on sugar destruction at evaporators (pre-evaporation to final syrup), where there are losses up to 3.5% of the sugar in cane.

Composition and Structure of Cell Wall Polysaccharides From Sugar Beet Grown Under Mediterranean Climate and Relation with Beet Processing. Maria El Amrani¹, Khalid Fares ¹, Qamar R'Zina¹, Marie-Jeanne Crepeau² and Jean-François Thibault², ¹Université Cadi Ayyad, Faculté des Sciences Semlalia, Département de Biologie, Marrakech. Maroc, ²INRA, Unité de Recherches sur les Polysaccharides, Nantes, France

Cell wall polysaccharides were isolated as alcohol-insoluble solids from Moroccan sugar beet, wet pulps, pressed pulps and diffusion juice at two stages of the harvest season (Early and Late samples). Pectins and hemicelluloses were extracted from beet slices and pulp by a sequential treatment with water, EDTA, hot dilute hydrochloric acid, cold dilute sodium hydroxide, cold 1 M and 4 M sodium hydroxide and finally water at pH 7. Composition of the pectin and hemicellulose extracts was determined and the purification carried out by ion exchange chromatography. The hemicellulose extracts were further precipitated by aqueous ethanol at 50% and 75 %, and fractioned on DEAE Sepharose, giving arabinan, xylan, xyloglucan and glucomannan fractions. The polysaccharides precipitated with alcohol from factory diffusion juice were mostly pectic in nature. Phenolic acids associated to the cell wall polysaccharides were also extracted and analysed by HPLC. Percentages of methylation and acetylation of pectins were determined.

Marked differences in yield and composition of beet polysaccharides can be obtained in relation to the variety and the site of the crop. The behaviour of the polysaccharides and phenolic acids during beet processing and their contribution to color formation is discussed.

The Effect of Ozone and Air on Off-Odors in Beet Sugar. Emmanuel Duffaut¹, Mary An Godshall², and Casey Grimm³, ¹Azucarera Ebro (Grupo Ebro Puleva), Valladolid, Spain; ²Sugar Processing Research Institute, Inc., New Orleans, Louisiana, USA; ³Southern Regional Research Center, Agriculture Research Service, U. S. Department of Agriculture, New Orleans, Louisiana, USA

This study investigated ozone and air as potential polishing agents for the elimination of off-odors sometimes present in beet sugars. Ozone and air were directly circulated through a bed of crystalline sugar to oxidize and/or remove volatile compounds responsible for off-odors. Various experimental parameters including treatment time, temperature, pressure and ozone concentration were tested to determine optimum conditions for best ozone and air action. Volatile off-odor compounds were extracted and analyzed using solid phase micro extraction-gas chromatography-mass spectrometry (SPME-GC-MS). The effect of ozone and air on the volatile fatty acids (VFA) profile was monitored, since these compounds are the major source of off-odors in beet sugar.

Air was more efficient than ozone in removing odoriferous compound from crystalline beet sugar. Under optimal conditions, air removed most volatile compounds. Under the most optimum conditions, ozone removed most compounds and rendered the sugar odorless, but ozone created new oxidation products if not properly applied. Air did not cause new compounds to form, and is also a better treatment from an economical point of view.

Ethanol Production by the ZeaChem Process: An Element of a Sugarcane Biorefinery. Les A. Edye, Sugar Research Institute, Mackay, Australia

In the near future the biorefinery concept of complete utilization of cane field biomass will become a pivotal element for a sustainable sugarcane industry. An industry that produces liquid fuels, electricity and commodity chemicals from a renewable source in regional communities will contribute to all elements of the triple bottom line and should be considered a compelling vision. In Australia, the Cooperative Research Centre for Sugar Industry Innovation through Biotechnology commenced in August 2003 and will embark on a significant program of research and development to underpin sugar cane biorefining. Fermentation to ethanol and other renewable commodities and biomass treatment processes such as pulping are technical elements of the biorefinery concept. The Sugar Research Institute has undertaken to assess the ZeaChem process – a novel fermentation route to bio-ethanol. This presentation covers the capacity of the sugar industry to produce ethanol and our preliminary assessment of the ZeaChem process.

New Insights on Sucrose Losses Across Factory Juice and Syrup Clarifiers and Evaporators. Gillian Eggleston¹, Michael Damms², Adrian Monge³, and Trevor Endres⁴, ¹SRRC-USDA-ARS, New Orleans, Louisiana, USA, ² Formerly U.S. Sugars Inc., Clewiston, Florida, USA, ³ Cora Texas Manufacturing Co., White Castle, Louisiana, USA, ⁴Formerly Raceland Factory, Raceland, Louisiana, USA

Major aims of an Agricultural Research Service project of the United States Department of Agriculture have been to improve the measurement of industrial sucrose losses, and to reduce sucrose losses. This paper discusses new insights gained on sucrose losses in sugarcane juices and syrups at high temperatures (55-115^oC) during different clarification and evaporation processes. The accurate method of gas chromatography was used to determine glucose, fructose, and sucrose concentrations on a Brix or chloride basis. Sucrose losses to acid inversion across one factory’s juice and syrup clarification processes were investigated. In the juice clarifier, chloride trended with Brix and, therefore, either could be used as a sucrose loss reference. In comparison, in the syrup clarifier Brix was more preferentially destroyed than chloride. Kestoses were shown not to be viable markers of sucrose losses across both clarifiers. High operational pHs for juice hot (~200^oF) lime clarification (pH range=8.38-9.55 measured at room temperature) minimized sucrose losses to ~0.00-0.58% even with an estimated R_t of 3h, but excessive lime addition can accelerate scaling and color formation. Higher acidic conditions (pH range=6.28-7.35) across syrup clarification (phosphatation) caused considerable sucrose losses of ~0.57-1.26% even at a lower R_t and temperature of ~1h and 165^oF, respectively. Comprehensive studies were also conducted at two other U.S. factories to determine the effects of time between cleanings of Robert’s-type calandria and plate evaporators on sucrose losses and overall evaporator performance. In general for both factories, most sucrose inversion losses occurred in the pre-evaporators, and only occurred in later evaporator bodies when scale had built up after a clean-out and, usually, became worse until the next clean. Less inversion occurred across the low retention time plate evaporator; the plate was also susceptible to scaling although to a lesser extent than the Robert’s type evaporators. Increasing the factory target pH of the clarified juice (CJ) or final evaporator syrup (FES) systematically reduced losses of sucrose and a target FES pH of ~6.3-6.5 (equivalent to a target CJ pH of ~ 7.0-7.3) is recommended; however, scaling effects can override pH effects. There was a consistent increase in pH in the last evaporator bodies because of the evaporation of volatile acids into the condensates. Economic implications of sucrose losses are also described.

The Harmonized Sucrose Standards for Beverage Manufacturers. Michael Finnerty and Marie Tanner, Pepsi Cola International, Valhalla, New York, USA

A technical manual on granulated sucrose will be published through the International Society of Beverage Technologists. ISBT’s objective is to enhance the promotion, development and dissemination of knowledge relating to the Art and Science of Beverage Technology. This work is accomplished through twelve individual committees that have been established to cover various phases of the industry. The granulated sucrose manual was created in a subcommittee of the sweetener technical committee. The manual is a collaborative effort between the beverage industry, sugar vendors and sugar experts. The manual contains global quality guidelines, rationale definitions, paragraphs that explain the importance of certain quality parameters, storage conditions and analytical methods (or references). This paper will focus on the global quality guidelines set forth by the sucrose subcommittee.

The Effect of Ozone, Hydrogen Peroxide and Sulfite on Cane and Beet Macromolecules. Mary An Godshall and Marianne McKee, Sugar Processing Research Institute, New Orleans, Louisiana, USA

Ozone, hydrogen peroxide and sulfite are powerful agents with activity against sugar colorant. All have been used at one time or another in sugar processing, with sulfite by far the most commonly used. Sulfitation, as in the production of plantation white sugar and in the production of white beet sugar, results in less color transfer into the crystal than a normal raw sugar process (no sulfitation). Thus, the effect of sulfite on colorants and on color transfer is of great interest. If other decolorizing agents, such as ozone and hydrogen peroxide, are used as alternatives to sulfite, will they have the same beneficial effect on color transfer? Preliminary studies have shown that ozone and hydrogen peroxide have little effect on the polysaccharide content of cane juice, but sulfite (in the form of ammonium bisulfite) removed some 12 percent. Gel permeation chromatography of the high molecular weight (HMW) fraction >12,000 Daltons showed that sulfitation removed a large portion of the HMW during plantation sugar production. GPC has also shown that both peroxide and ozone treatment of clarified juice resulted in a shift of macromolecules toward a slightly lower MW after treatment.

Dextran in Refined Sugar. Lynn Haynes, Kraft Foods, East Hanover, New Jersey, USA

Dextran content in sugar is a major concern for end users such as candy manufacturers. Contamination of the sugar with dextran, above a certain ppm level, will affect hard candy processing. The impact is measured in changes in candy thickness/weight and is related to dextran content in sugar. We report on the monitoring of dextran in refined sugar, over the course of

several months, using the Midland Sucrotest monoclonal antibody method. We correlate dextran content in refined sugar with changes in hard candy weight and geometry. Data suggests that dextran content in refined sugar is related to the amount in raw sugar used in refining. Estimates of dextran removal during the refining process are given.

Process and Energy Optimized Beet Sugar Factories. Reinhold Hempelmann, Dr. Andreas Lehnberger, and Burkhard Bartels, BMA AG, Braunschweig, Germany

The technological processes of a modern beet factory require continuous reconsideration and development, priority being given to saving of primary energy, improvement of quality and consideration of more stringent environmental regulations. More optimization means correlations become increasingly complex and can only be looked at in all their details. Examples of modern beet factory models will be presented considering especially optimized parameters for the main process steps, major developments like steam drying and/or continuous crystallization and their impact on the overall factory concept.

Possibilities for Ion Exchange Softening of Cane Clarified Juice. Vadim Kochergin¹, Jose F. Alvarez², William Jacob¹ and Larry Velasquez¹, ¹Amalgamated Research, Inc., Twin Falls, Idaho, USA, ² Florida Sugar Cane Growers Cooperative, Belle Glade, Florida, USA

Softening of sugar juices and molasses has become an established unit operation in the beet sugar industry. Being a necessary prerequisite for molasses chromatographic separation technology, thin juice ion exchange softening positively affects on downstream operations. It eliminates the need for descaling evaporators and improves heat transfer efficiency. The softening process also improves boiling characteristics of juice and has a positive effect on sugar quality. Cane juice typically has higher hardness then beet thin juice, which means that larger softening systems could be required and more regenerant will be generated. Also the presence of higher suspended solids in cane juice makes it difficult to use fine ion exchange resins. It has been proven that softening of membrane filtered clarified juice was quite efficient. However, the cost of membrane filtration remains relatively high. A fractal softener with a short bed has been tested for unfiltered clarified juice. Test results and the benefits of clarified juice softening will be discussed.

The Impact of Using Rapid Action Biocides for Mill and Cane Sanitation on Quality of Sugar and Molasses. V.M. Kulkarni, VM Biotech, Pune, India

Sugarcane juice is very nutritive and can inhibit the action of many biocides. The time required to kill microbes is also an important factor for achieving optimum economic benefits. During milling, only 15 to 20 minutes are available for biocide to kill microbes. The fiberizer used for better cane preparation acts as a source of further microbial infection of the cane, and it is not usually treated in mill sanitation programs. For treatment of the fiberizer, the biocide must act within a few minutes. When biocides capable of killing a significant portion of mesophilic as well as microbes capable of growing at higher temperature (about 90°C) in 1 minute for cane sanitation and 10 minutes for mill sanitation are used, there should be a minimal rise in reducing sugar as well as acidity during the entire process. The improved quality will be reflected in final molasses and sugar.

Quaternary ammonium compounds (Quats) and dithiocarbamates (DTC) are currently used for mill sanitation according to US FDA guidelines. Quats are inhibited by calcium, organic matter and bagasse, and may not kill microbes effectively in cane juice; DTCs require more than 25 minutes in cane juice at 10 ppm dose to kill about 90% microbes. Formulations of synergistically acting dithiocarbamates with permitted activators and penetrating agents can be made to achieve about 90% killing of microbes in 1 minute and in 10 minutes (Indian Patents application no. 306 / BOM / 99).

These biocide formulations are thus ideal for cane sanitation (Biocide 01) or for diffuser sanitation and mill sanitation (Biocide 10). Experiments were conducted in a sugar factory to evaluate various biocides for one week each. A minimum of 4 two-hourly composite samples of primary juice, mixed juice, clear juice, syrup and final molasses were collected (mercuric chloride used as preservative). Reducing sugars and acidity by titration were determined. Data was collected for a week using 10 ppm Quats, 10 ppm DTC mixture, 10 ppm Biocide 10 and 5 ppm Biocide 01 prior to the fiberizer with 10 ppm Biocide 10 for mill sanitation. Samples of sugar per shift were also collected. Sugar samples and final molasses samples were analyzed by HPLC for polysaccharide, glucose, fructose and sucrose. Results showed that Biocide 10 was effective in reducing microbial sugar losses to molasses and reduced polysaccharide in molasses and sugar. Cane sanitation using Biocide 01 reduced microbial losses to minimal levels and significantly reduced polysaccharides in sugar.

Laboratory Clarification Tests Using Natural Flocculants: Potential Application for Organic Sugar Production. J.E. Larrahondo¹, C.F. Sánchez¹, C.O. Briceño¹, J.I. Victoria¹, and M.A. Godshall^{2, 1}CENICAÑA (Sugar Research Center of Colombia), Cali, Colombia; ² Sugar Processing Research Institute, Inc., New Orleans, Louisiana, USA

The primary objective of the clarification process in sugar production is to obtain a juice with good colour and low turbidity by removing the maximum amount of the impurities (dissolved and/or in suspension). Clarification is done by adding synthetic anionic polyelectrolytes, which are not acceptable for producing organic sugar. For this reason, this research evaluated aqueous or mucilaginous extracts from the fruits of the plant Cordia lutea (fam. Boraginaceae) and chitosan as possible flocculating agents to clarify cane juice. Two polysaccharides, which are responsible for the flocculant properties that contribute to the removal of impurities in the cane juices, were found in the aqueous fraction of C. lutea, bound to an insoluble lignocellulosic portion. The general sedimentation trials on a lab scale and the conditions for using both the extract of C. lutea and chitosan as flocculating agents in cane juices are discussed in this paper.

Water-Sucrose Interactions, the Quality of Crystals and the Storage Stability of White Sugar. Mohamed Mathlouthi, Laboratoire de Chimie Physique Industrielle, Faculté des Sciences, Université de Reims Champagne-Ardenne, B.P. 1039 -51687 Reims Cedex 2, France

Caking of white sugar can be considered as a spontaneous agglomertation phenomenon which occurs under certain conditions of quality of crystals (especially large C.V., broken crystals, presence of amorphous and fine particles) and characteristics of surrounding air (Temperature, Relative Humidity).

To account for the interactions between water and sucrose in the thin layer of syrup surrounding the sugar crytsal, water vapour sorption isotherms are obtained at different temperatures and the water content at the surface and inside the crystals determined using Karl Fischer titration method.

To characterize the quality of crystals and the defects engendered during the manipulation of dry sugar in dryers, coolers, elevators and sieves, image analysis was used applying LUCIA software to the images of crystals obtained with Nikon binocular and camera.

A relation exists between the quality of sugar crystals and their flowability in silo determined with a Jenike shear cell. To thorooughly understand the mechanism of caking, there is a need of approaching both the macroscopic visual image of the crystals and the microscopic molecular interactions between water and sucrose.

The Sugar Industry in Between Tradition and the Future. Giorgio Mantovani, Department of Chemistry, University of Ferrara, Ferrara, Italy

Sugar manufacture follows a traditional flow sheet: raw material (beet or cane), diffusion/extraction, raw juice purification, juice concentration, crystallization, sugar. Such a scheme, even after moving to completely continuous processing, has remained unchanged in the course of the last more than 100 years. Important and fundamental the modernization which has taken place, and in particular as far as management, control and automation are concerned, but all involving single steps or procedures whilst the basic scheme remained unchanged. This fact permitted, and still permits, to limit the relevant investments not only going on with utilizing at the best already tested facilities and amortized plants but also even considerably enlarging factories by moving expensive machines from others the closure of which has been planned. Bearing in mind this type of policy, which occurs in the presence of an unfavourable sugar market, it is understandable that the sugar industry is not open to proposals which, in one way or another, may upset the traditional trend of sugar manufacture. Some of these proposals, made in recent years, are considered and discussed and, in particular, the one, which is, more than a proposal, a reality, that is to bring new HIS, High Intensity Sweeteners, onto the market.

Technological and Economical Process Integration of VTIR (Technological and Industrial Value of Beet): Harvesting, Washing and Processing. Fernando Martin-Dominguez, Marta Garcia-Quevedo and Manuel Ruiz-Holst, Azucarera Ebro (Grupo Ebro Puleva), Valladolid, Spain

During the 2003-04 campaign (fall and spring sowing) several pilot scale experiments that reproduced the factory process from harvested beets to thick juice were conducted with variable beet post-harvest treatment and washing conditions. The data obtained showed an influence of these two factors upon the results of the process.

This study presents and quantifies the effects of some of the parameters of post-harvest treatment and washing on industrial yields for both south and north of Spain beet culture conditions. More precisely, it presents the fluctuation in ranges of parameters such as sucrose losses, juice filterability, color and purity of thick juice that is induced by post harvest factors including storage time, temperature, mechanical damage, providing the ability to calculate the technolgical and economical repercussions of these factors.

This paper also shows and quantifies the potenical increase in the industrial value of beet (VTIR) that can reasonably be attained through the optimization of both beet post-harvest treatment and beet washing conditions.

A New Technology for Regenerating Sugar Decolorizing Activated Carbon, Hugh McLaughlin. Groton, Massachusetts, USA

Activated carbon is widely used l for decolorizing in-process solutions during the production of refined sugar. Activated carbon "adsorbs" the organic compounds from the liquid streams, which means it acts like a sponge – in that the color bodies removed from solution are accumulated within the activated carbon. Once the carbon has reached its capacity for adsorbing material, the carbon becomes "spent" and must be treated to recover the adsorption capacity or disposed of.

The current practice in the sugar refining industries is to regenerate the spent decolorizing carbon by a high temperature process called Thermal Reactivation. That process returns the spent material to the same conditions used to make the original activated carbon, over 800°C (1500°F) under a blanket of steam. The harsh reaction conditions and scale of the sugar refining operations typically utilize multiple hearth kilns, involving significant capital investment and ongoing operational costs. Between heating the carbon to such high temperatures, providing supplemental steam and treating the off gases with an afterburner, the total energy requirement is 3000 to 8000 Btu’s per pound of reactivated carbon. In addition, the aggressive conditions typically destroy 5% of the activated carbon present, which must be replaced with virgin activated carbon.

A new lower temperature process, called CarbOxLT (which stands for Carbon Oxidation at Low Temperatures and pronounced Car-Box-Lite), has been developed that can cut the energy requirement for regenerating activated carbon to less than 1000 Btu’s per pound. In addition, the make up requirements for virgin activated carbon are expected to be less than the current thermal reactivation process and the capital equipment costs will be significantly less than the multiple hearth technology due to the lower operating temperatures and lack of refractory-lined equipment. The CarbOxLT regeneration process has been demonstrated on samples of actual spent decolorizing carbons and the regenerated material appears to be equivalent or superior to the reactivated carbon produced by on-site multiple hearth kilns. The new low temperature regeneration process will be compared to the traditional multiple hearth reactivation process and the current state of commercialization of the CarbOxLT process will be reviewed.

Direct Consumption White Sugar Production At a Cane Diffusion Sugar Plant. M. Narendranath and R. Nanda Kumar, Andrha Sugars Limited, Tanuku, A.P., India

Most sugar plants in India are plantation white sugar producing plants that use milling and double sulfitation, producing sugar of 100 ICUMSA color, 30 ppm SO₂ and 45 turbidity. The Andrha Sugars Limited is an exception to this norm in the Indian sugar industry. We use cane diffusers in place of mills and have modified/improved the process to the extent that we are able to produce sugar that meets the Indian Pharmacopoeia requirements, and is of 40 ICUMSA color, 9 ppm SO₂ level and 25 turbidity. We continue to work on various aspects of our process to produce sugar at a plantation white sugar plant that will be closer to refined sugar quality. This paper will discuss the steps that were taken to achieve this level of quality.

Real-time Solution Colour of Crystalline Sugar. Bjarne Chr. Nielsen, Neltec, Bevtoft, Denmark

The ColourQ instrument for real-time automatic measurement of sugar colour in solution is now in use in many sugar factories and refineries. The system measures white, yellow, and brown sugars. The measurements are taken on wet or dry crystalline sugar directly in the conveyor - without any sample preparation. Nevertheless, the results are presented in ICUMSA units for Solution Colour, with excellent correlation between the instrument and control samples taken to the laboratory to monitor the instrument's performance. The presentation will cover main aspects of the principle of measurement, the calibration, the accuracy, and some typical applications. The robustness and stability of the instrument will be discussed.

The Concept of Different Natural Antibacterials for the Sugar Industry. Guenter Pollach¹, Walter Hein¹ and Daivd Beddie², ¹Zuckerforschung Tulln Gesellschaft GmbH, Tulln, Austria, ²Botanix Ltd, Worcestershire, UK

During the last decade hop beta-acids have been used in the sugar industry as a natural biocide with specific inhibitory effects on thermophilic and other Gram-positive micro-organisms. As a consequence of their very specific bacterial action, these natural products are considered harmless to humans as they are regularly consumed in food, and additionally they are degradable in the environment. However, micro-organisms may become insensitive to natural products after repeated application. In comparison to human health and the use of antibiotics, it is necessary to have different natural biocides in the sugar industry in order to meet with most of the constraints, caused by micro-organisms in beet sugar factories. In 2002, rosin acids were presented as a natural alternative to hop beta-acids, and this was the start of a natural biocide range concept. This concept could be adopted by sugar factories, which have environmental problems with chemicals in their particular situation and thus are in favor of harmless natural products. Now a further group of natural acids and a main representative will be shown, which could be effective in the case of insensitivity. Laboratory trials and full-scale factory trials from the 2002 beet campaign and the coming 2003 campaign will be shown. In factory trials during the first campaign, a rosin-insensitive strain occurred, by chance, in the extraction tower and could be eliminated by shock dosing of a new product. This result already shows the importance of a natural product range to meet with various situations.

Sustainable Technologies and Valuable New Polysaccharide-Based Products from Sugar Beet Pulp. Brett J. Savary, Marshall L. Fishman, Arland T. Hotchkiss, LinShuLiu, and Kevin B. Hicks, Eastern Regional Research Center, USDA-ARS, Wyndmoor, Pennsylvania, USA

Efficient utilization of sugar beet pulp generated from beet sugar processing is critical for the economic viability of beet sugar production. Dried pulp pellet and shreds are a nutritious and valuable animal feed co-product for both local and export markets. However, the future of such markets is threatened by increased availability of distillers’ dried grain solids from corn-based bioethanol production and customer concern for beet pulp derived from genetically modified plants that are being developed and pending commercial release.

Beet pulp represents a largely untapped source of cell wall polysaccharides that can be converted into higher-value biobased products. Such biorenewable products may replace imported and/or petroleum-based products and generate more revenue for growers and processors. Research in the Crop Conversion Science and Engineering Research Unit is being conducted toward developing fundamental knowledge of the enzyme and polysaccharide components of the sugar beet cell wall; creating innovative new functional food, feed, and non-food biomedical and industrial bioproducts; and establishing efficient and sustainable conversion processes for their isolation and production. Details of our specific objectives, capabilities, and accomplishments will be presented.

Development of an On-line NIRS Procedure for the Analysis of Quality Parameters in Individual Consignments of Shredded Cane. Kevin J. Schäffler, Sugar Milling Research Institute, University of Natal, Durban, South Africa

In South Africa (SA), individual consignments of shredded cane are analysed by the direct analysis of cane method (DAC). Although this procedure is capable of producing excellent sampling and accurate analysis of consignments, it is labour intensive. NIRS (Near Infra Red Spectroscopy) has been used by several sugar industries for determining cane quality for cane payment purposes. Earlier work in SA indicated that AT-LINE NIRS could produce excellent estimates of cane quality and could possibly replace the current DAC analysis for payment. To be economically viable and to gain the best advantages, NIRS has to be used ON-LINE for automated analysis. This paper describes the progress made from 2000 to 2003.

Observations on Sucrose ERH-Moisture Relationships. Charles L. Schmalz & Michael L. Stroebel, Amalgamated Sugar Company, Ogden, Utah, USA

The sugar-water relationship on the surface of refined sucrose crystals is a complex and only partially understood phenomenon. The mechanism appears to be related to the film of amorphous sugar formed on the crystal surface during drying. This film slowly gives up moisture on standing, a condition sometimes referred to as curing. Using Equilibrium Relative Humidity (ERH) measurements the authors present a model for the curing step and its relationship to frequently observed caking and lumping problems. They also explore the behavior of sugar in storage and some of the apparent anomalies in the measurement of moisture in freshly produced sugar.

The Application of Network NIR Calibration Equations at the Maryborough Sugar Factory. S. Staunton¹, D. Mackintosh¹, G. Peatey² , ¹BSES Ltd., ²Maryborough Sugar Factory, Indooroopilly, QLD, Australia

The work described in this paper includes the installation, commissioning and validation to successful performance of a FOSS Cane Analysis System (CAS) at the Maryborough Sugar Factory in 2003. It is noted that the system equations loaded contained no data from the Maryborough region or the NIR spectrophotometer used in the CAS. The results demonstrate that the transfer of FOSS based calibrations can be achieved with no loss in analytical performance.

The system was implemented at the Maryborough Sugar Factory to address cane quality issues, high processing costs, provide outputs for improved factory control and determine the effects to Millers and Growers of using the CAS for direct determination of CCS for payment purposes.

The system library required the addition of 350 valid spectra collected over roughly one week to adequately represent the new instrument and cane supply. Constituent bias was calculated and applied after the first week of operation and were the only adjustments made to the system. The precision of the CAS results were found to be within expected limits for all constituents except brix in cane and fibre, the reasons for the higher than expected error for these constituents are still under investigation.

The bias for all constituents was demonstrated to have a diurnal cycle and long-term drift. This effect was found to be due to variation in cane temperature and adjustment based on this parameter resolved the problem for all constituents.

Comparison of the seasonal averages for the current laboratory method for CCS (15.1286) using class fibre, and the CCS directly determined by NIR (15.0713) and given that the reported errors were within expected system limits, there is no equity barrier to the implementation of direct NIR CCS in cane payment for the 2004-crushing season.

All stakeholders in the Maryborough cane-growing district agree in principle with this philosophy. The hurdle remaining is the technical considerations in changing the cane payment formula to achieve a win-win scenario for all parties.

POSTER ABSTRACTS

Successful Application Points to Control Bacterial Infections Throughout Sugar Factories Using Beta Acids/Beta Stab® 10A. David Bebbie¹, Natalie Isles¹,Tobias Wirth², Guenter Pollach³ and W. Hein^{3 , 1}Botanix Ltd, Worcestershire, UK, ²Beta Tec HopFenproducts GmbH, Nuernberg, Germany, ³Zuckerforschung Tulln Gesellschaft m.b.H, Tulln, Austria

Over the past 5 years BetaStab®10A has emerged as an exceptional natural biocide being applied to the extraction stage of sugar processing to successfully control bacterial infections. More recently studies have shown that the efficacy of BetaStab®10A is evident over a wide range of conditions and variables including temperature and pH. Furthermore due to its natural properties can be added at later stages of sugar processing without any risks of toxic residues remaining in the final product. As a result BetaStab®10A is successful at combating infection in many additional stages and diverse environments that are found in sugar factories examples of which are discussed within this presentation.

Molecular Probes for Assessing Boiling Difficulties. Emmanuel Duffaut¹ and Mary An Godshall², ¹Azucarera Ebro (Grupo Ebro Puleva), Valladolid, Spain; ²Sugar Processing Research Institute, Inc., New Orleans, Louisiana, USA

Mills in Louisiana periodically experience a phenomenon known as "hard to boil massecuite" (HTB). During the 2002 grinding season, a combination of tropical storms and unrelenting rains caused a difficult harvest season, and episodes of difficult-to-boil and slow-to-boil episodes were experienced. Examples of HTB massecuites were compared to normal boiling massecuites.

Trends observed included higher levels of polysaccharides, dextran and calcium and lower phosphate and invert in the HTB samples. Polysaccharides, starch and dextran did not seem to be the main cause of the problem. Indications are that excess calcium may play an important part in the over-all control of HTB. The need to use extra lime for clarification due to high mud and polysaccharide levels along with a low natural phosphate in the juice led to high levels of calcium carrying through the process, with a deleterious effect on crystallization.

Treatment of HTB molasses with compounds chosen for their various properties was undertaken with the idea that these compounds would act as "molecular probes" providing information about the mechanisms involved in HTB. The most effective of these treatments were hydrochloric acid and hydrogen peroxide. Soda ash had variable effects.

Optimization of Factory Applications of Dextranases in The U.S. Gillian Eggleston¹ and Adrian Monge², ¹ Southern Regional Research Center-USDA-ARS, New Orleans, Louisiana, USA; ² Cora Texas Manufacturing Co., White Castle, Louisiana, USA

Although the use of commercial dextranases to break down dextran in sugar manufacture was pioneered by Australian researchers in the 1970s, applications in the U.S. sugar industry are still not optimized. This is partly because of misinformation about where to add the enzyme and which enzyme to use. Furthermore, there is no national or international method to measure the activity of dextranases, which has meant that direct comparison of activities is not possible. In this dextranase optimization study, a simple method to determine the relative activity of dextranases was identified, which is based on titration and could be easily undertaken at factories. All the relative activities were further confirmed with ion chromatography with integrated pulsed amperometry detection (IC-IPAD) using a sodium hydroxide/sodium acetate gradient method.

The Shape of Sucrose (Molecules, That Is). Alfred D. French¹, Anne-Marie Keltere², Christopher J. Cramer³, and Glenn P. Johnson¹. ¹Southern Regional Research Center, USDA, ARS, New Orleans, Louisiana, USA; ²Institut für Physikalische und Theoretische Chemie, Technische Universität Graz, Graz, Austria; ³Department of Chemistry and Supercomputer Institute, Minneapolis, MN, USA.

The shape properties of sucrose have many important ramifications. They are responsible for its sweet taste, for its crystallization behavior and for many of the intermolecular interactions that are unique to sucrose. The shapes of sucrose are conveniently described in terms of the extent of rotation of the glucose and fructose monomers about their bonds to the mutually held oxygen atom. The most definitive method for studying shape is diffraction crystallography. It precisely locates each of the atoms but it requires a crystal and in most cases gives only a single structure when the desired result is probabilities for the range of plausible structures. The problem of a limited number of structures has been overcome by finding crystals of very similar molecules and complexes, giving a wide range of observed structures.

Another precise method is to calculate the energy of the different shapes to learn the shape with lowest energy. In principle, that structure is the most likely one, and structures with progressively higher energy are progressively less probable. Although this method can give a very precise answer, it may not be accurate. There are many ways to calculate the energy and they give different answers.

Our poster presents a method that shows all of the crystallographically observed structures to have fairly low energy. This suggests that other shapes are unlikely to be observed in future experiments. The lowest energy occurs when hydrogen bonds connect the glucose and fructose rings, but may of the observed structures do not have such hydrogen bonds. This suggests that hydrogen bonds do not determine the structure but that they can form if the molecule otherwise has the correct shape. Other workers have proposed that water plays a special role in determining the shape of the molecule in solution, but that is not indicated by our modeling method.

Composition of Indian Plantation White Sugar: Comparison to International Standards. Mary An Godshall, Sugar Processing Research Institute, Inc., New Orleans, Louisiana, USA

India produces 18-20 million tons of sugar per year, making it the largest sugar producer in the world. The majority of this sugar is direct-consumption sugar, or plantation white sugar, most of which is consumed domestically, with only 1.2 million tons exported in 2002. In view of growing sugar stocks, India is seeking to diversify its production and to export sugar. There are two avenues for India to export sugar: Begin producing raw sugar for export or improve the quality of the plantation white sugar to make it a more desirable export. Until recently, raw sugar production was not allowed by law, and it will take some time to build the raw sugar producing and exporting infrastructure. In the meantime, Indian producers have undertaken to improve the quality of plantation sugar by adopting ICUMSA methods and setting quality criteria that conform to the revised Codex Standard for Sugars 212-1999. This paper shows the compositional range of quality parameters in plantation white sugar compared to refined sugar and show areas where improvement has occurred in the last decade and highlights areas where further improvements can be made.

Dextran in White Sugar, a Comparison of Three Methods. Mary An Godshall, Marianne McKee, Ron Triche and Sara Moore, Sugar Processing Research Institute, Inc., New Orleans, Louisiana, USA

The analysis of dextran is of great importance to the sugar industry at all stages. It is obvious that dextran is deleterious to the process when present in cane (or beet) juice and high dextran raw sugars cause many problems in the processing of refined sugar. It is less obvious that dextran can be a problem in refined sugar. However, dextran in refined sugars is implicated in crystal distortion in hard candies, leading to packaging problems and misshaped candies, such as lifesavers. In this study three methods for dextran were compared -- the ICUMSA haze method for dextran in raw sugar, the Roberts copper method, and the Midland monoclonal antibody (MCA). It was necessary to modify the ICUMSA haze method for the lower levels of dextran found in white sugar. All three methods gave comparable results, with the MCA method tending to give lower and more variable results. The study showed the range of dextran found in cane, beet and plantation white sugars. It is felt that the closeness of the results is due to the presence of mainly high molecular weight dextran (>50,000 Da) in white sugar, which is detected by all three methods.

A Rapid Starch Test for Use in Cane Mills. Mary An Godshall, Ron Triche and Sara Moore, Sugar Processing Research Institute, Inc., New Orleans, Louisiana, USA

Starch is an important quality factor in raw sugar production, as well as in sugar refining. Starch is higher in immature cane plants, as sometimes harvested in Louisiana, and in green (not burned) cane, which is being harvested more frequently in all parts of the world. There is a need for a rapid and simple method that can be used in cane mills. Although an accurate and precise method for starch, based on the blue starch-iodine complex, was developed in the 1970s in South Africa, the method consists of many steps and is lengthy. A rapid and simple method was developed for use in cane mills by modifying the existing method. It uses equipment already available in a core lab. Results showed good correlation (>95%) of results between the standard method and the rapid method. The method was successfully tested on site in a Louisiana cane mill and can be applied to raw juice, clarified juice and raw sugar. This poster will also review the behavior of starch in the mill during the grinding season.

Determination of the Saponins Content in Sugar Products. Boguslaw Król, Joanna Milala, Maciej Wojtczak, Technical University of Lodz, Institute of Chemical Technology of Food, Poland

Determination of saponins by HPLC based on separation by SPE from white sugar solutions, followed by determination of saponins before the hydrolysis and oleanolic acid after the hydrolysis of saponins is presented. The saponins content in white sugar and other sugar products from selected Polish sugar factories was determined by the method. The average saponins content in the analylzed population of sugars was 0.25 mg of oleonolic acid monoglucuronide in 1kg of white sugar.

Extraneous Matter and Its Relationship to Different Harvesting Systems in the Colombian Sugar Agro-Industry. Jesús E. Larrahondo, Carlos A. Viveros, Carlos O. Briceño, MSc, and Aybi Patiño, CENICAÑA (Sugar Research Center of Colombia), Cali, Colombia

Extraneous matter content is one of the factors of great importance associated with the cutting, loading and transport of sugarcane from the field to the mill. Extensive research conducted in different regions has shown that extraneous matter affects the production and quality of the end product (sugar); therefore, the need for evaluation systems that guarantee the rapid and reliable determination of extraneous matter that enters a mill has been one of the objectives proposed by the Colombian agro-industry to identify the best harvesting options, especially for green (i.e., nonburnt) cane and to reduce the content of extraneous matter in the cane delivered in the field or at the mill. The implementation of sampling systems and control of extraneous matter by means of a mechanised core sampling or the manual cleaning of samples obtained at a station for the postharvest evaluation of cane were evaluated for different harvesting methods. Similarly, three harvesting systems for green cane were evaluated under the conditions of the Colombian sugar sector, and their impact on the incorporation of extraneous matter during the harvest as well as on factory yield and sugar quality were determined. Based on the results obtained, it was concluded that harvesting sugarcane with manually cut, clean green cane contributed to reducing the levels of extraneous matter in the cane for milling and to increasing the sugar yields. The possibility of using NIR methodology (near infrared spectroscopy) and the characteristics of extraneous matter, such as levels of phenols, polysaccharides, minerals, etc., are being explored in conjunction with a pilot mill in the Cauca Valley to quantify extraneous matter incorporated in the cane during its cutting, loading, transporting and delivery to the mill.

Investigation on the Efficiency of Carbonatation Sludge Addition Into Turkish Fuels for Desulfurization of Flue Gases. Jale Leblebici¹ and Ferit Leblebici², ¹Turkish Sugar Authority, Ankara, Turkey, ²Turkish Sugar Factories, Ankara, Turkey

Nowadays, SO₂ emission is more strictly controlled due to the sensitivity of environmental protection. As a result of this, use of either fuel containing low sulfur or reduction of SO₂ emission has gained importance. Reduction of SO₂ emission in flue gases by physical and chemical treatments is preferred by the industries in which huge amount of fuel is used, since fuels containing low sulfur are expensive.

There are many methods for desulfurization of flue gases in the world. One of the most popular methods is the treatment of SO₂ with alkaline earth oxides producing alkaline earth sulfates. The addition of carbonatation sludge into fuel provides not only the reduction of SO₂ emission, but also utilization of a sugar factory’s by-product.

In this study, a laboratory method was proposed to determine the efficiency of carbonatation sludge addition into high sulfur containing fuel oil or coal used in Turkish sugar factories in order to determine the parameters needed for industrial applications.

Studies on Bagasse Fly Ash as an Adsorbent for Waste Materials. Marianne McKee and Mary An Godshall, Sugar Processing Research Institute, Inc., New Orleans, Louisiana, USA

Bagasse fly ash, the material remaining after bagasse has been burned in the boilers during sugarcane processing, is considered a waste product. The only possible commercial use for this material is as an amendment for potting soils. Recent literature has shown that fly ash may have the potential for use as an adsorbent trap for different organic and inorganic materials such as pesticides, dyes, and metals. This makes way for a new value-added product for the sugar industry. In this study, we examined the usefulness of the bagasse fly ash as an adsorbent for textile waste dyes and heavy metals. We have seen promising results with the bagasse fly ash removing 99.8 % of textile waste dyes upon treatment of the waste dye solution at 55°C and pH 3. The heavy metals tested include arsenic, cadmium, chromium, mercury, and lead. The effectiveness of the bagasse fly ash at removing the metals varied from 7.5% removal of arsenic to 99.9% removal of chromium, mercury, and lead.

Changes in Number 1 Liquor on Storage. Sara Moore, Marianne McKee, and Mary An Godshall, Sugar Processing Research Institute, Inc., New Orleans, LA, USA

Sugar degradation is not only a problem during processing, but is also a frequent concern on storage. The storage of high brix sugar solutions is of potential interest to the cane sugar industry. In this study, we illustrate changes that occurred in liquor samples under storage conditions. In addition to the liquors, a model system consisting of a white refined cane sugar was subjected to the same conditions as the liquor samples. The changes observed in the liquors were fairly rapid and of a significant order for all parameters analyzed. For the model system, pH and invert showed significant changes, but color remained unchanged.

Comparison of Two Methods of Volatile Analysis for Determining the Causes of Off-odors in White Beet Sugars -- SPME and Headspace. Sara Moore¹, Mary An Godshall¹ and Casey Grimm², ¹Sugar Processing Research Institute, Inc., New Orleans, LA, USA; ²USDA, SRRC, ARS, New Orleans, LA, USA

White beet sugars periodically exhibit off-odors, causing them to be rejected by customers. An understanding of the nature and source of the compounds responsible will help in eventually eradicating the problems that cause them. However, determining volatile substances in white sugar is challenging because the amounts present are very small, often in the parts-per-million or even parts-per-billion range. In this study, we describe a set of white beet sugar samples that were received from several locations. Each sugar was given an over-all sensory rating of: 1 = acceptable; 2 = borderline; or 3 = reject, by a sensory panel. The samples were analyzed by two methods of volatile analysis: Solid-Phase Micro Extraction (SPME) and Headspace. Sample chromatograms were evaluated for compounds at mass to charge ratio (m/z) 60, where volatile fatty acids are found, with the exception of propionic acid. Representative chromatograms illustrating acceptable, borderline, and reject sugars are shown. Samples in the acceptable and borderline categories appeared to have lower levels of the more volatile fatty acids than did the reject sugars. This was true for both SPME and Headspace. However, it was apparent that SPME was a better technique for volatile analysis.

Critical Influence of pH and Invertase Addition on Polyols Production by Hansenula anomala in Sucrose Based Medium. S. V. Patil¹, R. V. Burase¹, V. K. Jayaraman² and B. D. Kulkarni^{2 1}Vasantdada Sugar Institute, Department of Alcohol Technology, Pune 412 307, India ²National Chemical Laboratory, Pune, India

Sugar cane and sugar beet processing products viz. molasses, cane/beet juice or crystalline sucrose are renewable raw materials that can be used to develop new fermentation products. Production of glycerol and related polyols viz. arabitol, erythritol, mannitol by fermentation of renewable sugary raw materials by osmophilic yeast is assuming an increasing importance. Glucose based fermentation media for polyols production using osmophilic yeast has been reported by various researchers. Commercial glucose is much costlier than sucrose and not a desirable raw material for industrial fermentation process from the viewpoint of overall cost economics. There are very few reports on use of molasses or juice or even synthetic sucrose media for production of polyols employing osmophilic yeast. In the present study, Hansenula anomala was cultivated on complex medium consisting of sucrose as carbon source and yeast extract, urea, casein hydrolysate and MgSO₄.7H₂O as source of nitrogen and other essential nutrients. H. anomala used in the study was able to produce two polyols from sucrose viz. glycerol and arabitol under controlled aerobic conditions. The effect of pH in the range of 4.0 to 8.5 and external invertase addition on combined polyols yield and productivity by H. anomala has been investigated. pH 8.0 was found to be optimum but substantial amount of sucrose remained unutilized. Though H. anomala is known to possess invertase activity, under the conditions of fermentation it has been found to be not strong enough to invert all sucrose to reducing sugars. External invertase addition resulted in maximum sugar utilization rate of 2.17 g/l.h at pH 8.0 and a polyols yield of 41.1 % based on total initial sugars. Chromatographic analysis of fermentation broth samples showed that glycerol and arabitol are the only polyols produced in an approximate ratio of 4:1. Studies for further improvement of yield and productivity by optimizing oxygen transfer rate in the sucrose-based medium are in progress.

Application of a New GC-MS Method for Determining Ester Contents Following Base- and Enzyme-Hydrolysis of Sugar Beet Pulp and Pectin. Brett J. Savary, Brett R. Newswanger, and Alberto Nuñez, Eastern Regional Research Center, USDA-ARS, Wyndmoor, Pennsylvnia, USA

Sugar beet pulp is composed largely of the cell wall polysaccharides pectin and associated arabinan-galactan, hemicelluloses, and cellulose. Beet pulp is a rich source of pectin, which is a valuable bioproduct that is used as a food gum and in pharmaceutical and nutraceutical applications. Pectin’s functional properties are influenced by structural decorations such as methyl- and acetylesters. There is a critical need for specific and sensitive analytical methods capable of determining the content of these decorations, especially in research on new uses for U.S. agricultural processing residues such as sugar beet pulp. Current standard methodologies for these determinations need replacement since they are labor-intensive, time-consuming, and require large sample sizes.

We have developed a simple, fast, and direct GC procedure for the simultaneous and sensitive determination of methanol and acetic acid present as esters in pectin and other cell wall polysaccharides. This method takes advantage of readily available deuterated isotopomers for use as internal standards, a suitable solid-phase microextraction fiber for headspace sampling, and the selectivity of a mass spectrometry detector. The method can also be applied for detecting and quantifying corresponding esterase activities upon treatment of pectin and sugar beet pulp. Details of the method and its application to enzyme analysis will be presented.

Determination of Components of Insoluble Matter in White Sugar by Means of X-ray Micro-Analyzer EDX. Maciej Wojtczak¹, Krzysztof Polanski², ¹Technical University of Lodz, Institute of Chemical Technology of Food, ²University of Lodz, Department of Solid State Physics, Poland

The paper presents possibilities of using X-ray micro-analyzer (EDX) to determine the components of insoluble matter in white sugar. The X-ray micro-analysis (EDX) is a non destructive analytical technique which enables to determine the elements and their content on microscopic surface of analyte. The scanning microscopy and X-ray spectroscopy are connected by this technique and we can observe objects and analyze the chemical content of surface of objects at the same time. Electronic scanning microscopy VEGA 5135 MM TESCAN and X-ray micro analyzer EDX ISIS system LINK 3000 made by Oxford Instruments were used in this work for study components of water-insoluble matter in white sugar.

Solutions of different white sugars from Polish sugar-factories were filtered through membrane filters of pore size 8.0 um (according to GS2/3-19 ICUMSA Method). These membranes and retained insoluble matter were analyzed by means of X-ray micro-analyzer EDX. In result many different substances were found in water-insoluble matter in white sugar, such as: cellulose fiber, carbon, silica, small parts of iron (rust), calcium carbonate (lime), and others.

The paper states that the type of the main component of insoluble matter in sugar is determined by local conditions of technological process in concrete sugar-factory. The proposed technique seems very useful for further study of insoluble matter content in white sugar leading to a decrease of the content of different types of insoluble matter in white sugar.

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