Texture

Crystallisation
Crystallisation of sugars is desirable in products such as fondant, dragees, fudge etc., but not in many other products like jam and jellies. Crystallisation occurs when the solubility limit of the sugar, typically sucrose or glucose, has been exceeded and a supersaturated environment has been created, as shown for sucrose in figure 1. The term ‘supersaturated’ refers to the situation where more sugar than theoretically possible from the solubility data is in solution. As indicated in figure 1, the supersaturated solution has been reached either by lowering the temperature or by increasing the sucrose concentration, or both. A metastable region exists where the solution is in fact supersaturated but in practice no crystallisation is likely to occur.

Sucrose, % (w/w) 90

Supersaturated region

Evaporation

80

Metastable limit

Cooling

70

Metastable region

Undersaturated region

Solubility limit

60 0 10 20 30 40 50 60 70 80 90

Temperature, °C

Figure 1. Phase diagram of the crystallisation of sucrose.

TExTURE 25
Nordic Sugar A/S

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which can occur when a jam is cooled in the refrigerator or the surface of a confectionery gel dries out. At very high viscosity. giving them a grainy look and a greyish colour. Sugars are used to control or prevent the formation of ice crystals in these products. kneading and pulling Insufficient mixing of ingredients added after cooking Recycling of products or intermediaries in the production line Not optimal storage conditions of finished products: high temperature and varying humidity Freezing-point depression Sugars are effective in lowering the freezing point of a solution. Frozen products containing sugars can be made softer and easier to scoop at a given temperature than the same products without sugars. as water is ’squeezed out’ when the sugar solids are concentrated in crystals. This is important in the manufacture of ice-cream products and frozen desserts. crystallisation in liquids is catalysed by the presence of small particles. the greater the depression of the freezing point. the more difficult for the ice crystals to form. above the metastable limit. texturisers and stabilisers influence crystallisation. and the texture of confectionery products can appear ’short’ and crispy. Typically high viscosity means slow crystallisation rates. Furthermore. Glucose syrups and invert sugar are typically used to avoid crystallisation of sucrose. The greater the number of solute molecules present.In the supersaturated state. Monosaccharides are more effective than sucrose at lowering the freezing point. Unwanted crystallisation of sugars in products like jams and confectionery jellies may affect the appearance of the products. The lower the freezing point. but also ingredients like proteins. To avoid unwanted crystallisation in jams and jellies the following issues should be considered: • • • • • • Sucrose/glucose syrup ratio in the recipe Crystallisation of glucose due to increasing invert sugar content Too heavy mechanical handling: mixing. TExTURE 26 . the onset of crystallisation requires a higher degree of supersaturation. the water activity of the product may increase. stirring or shaking. The freezing point is related to the number of molecules in solution. Increased water activity may affect the shelf life of the product. rough edges in the equipment. and in gels.

5 -4.5 -6.5 0 5 10 15 20 25 30 35 40 45 50 Concentration (%) 42 DE Glucose syrup Sucrose Glucose Figure 2: Freezing-point depression of 42 DE glucose syrup. sucrose and glucose TExTURE 27 .5 -1.5 -2.0 -5.0 -1.0 -2.5 -3.5 -7.0 -4.0 -3.5 -5.0 -7.°C 0 -0.0 -6.

The distribution and orientation of the -OH groups appear to be the issue. If sucrose is substituted with glucose syrup. or from apple pomace. i. The interaction between carbohydrates and water is a secondary effect. In low ester pectin gels. contain so much pectin that they can form gels on their own. High ester pectins (high degree of esterification of the galacturonic acid chain) can form gels with the presence of sugar at low pH. while other fruits need supplementary gelling agents when used for jams and jellies. For making a high ester (HE) pectin gel certain conditions are needed. This behaviour might be of considerable importance in dietary gels. so by adding sugar in adequate quantities the water is kept away from the pectin molecules. typically berries. the conditions for gelation and the character of the gel differ. fructose. When dissolved in water the negatively charged pectin molecules first need a low pH to reduce the charge and hereby reduce one barrier for making the molecule bond to itself. polyols or bulking agents.4. or meshwork. pectin concentration of 0. TExTURE 28 . is formed. Furthermore. decreasing gel rigidity. lime. Commercial pectin for this purpose is derived from the peel of citrus fruits (lemon. not their effects on the colligative properties of water. Next. while low ester pectins (low degree of esterification) typically need calcium ions present for forming gels.4 glucosidic bonds. The mechanism behind low ester (LE) pectin gelling is as follows: When positively charged calcium ions are present. marmalades and jellies the long. the gel. Typical conditions for jam making are: pH of 2. Protopectin and cellulose form the structure of the plant cell walls.8-3. orange and grapefruit). they form bridges between the negatively charged points of the pectin molecules and a network. as the pectin molecule will otherwise tend to bond to water rather than to itself. allowing them to interact and form the network. therefore. the availability of water molecules must be reduced.000 and a degree of polymerisation of up to 800 units. This interaction can be unfavourable to the formation of pectin gel due to the decrease of calcium ions available to associate with pectin molecules and. different carbohydrate sweeteners have different abilities to form stable complexes with cations.5-1% and sugar content of 60-65%. Pectin is a polymeric carbohydrate of high molecular weight and is found in all plants. The galacturonic acid chain is partially esterified as methyl esters. Some fruits. Sugar’s great hydrophilic properties make it ideal for this application. Pectin consists primarily of a chain of galacturonic acid units linked by a-1. string-like pectin molecules convert liquid into a solid-like structure by bonding and forming a fine-meshed network that holds the liquid in its cavities. Pectin molecules have a molecular weight of up to 150.e. the rigidity essentially depends on the capacity of the carbohydrate sugar to compete with pectin for calcium ions.Effect of sugar and sweeteners on pectin gel formation In jams. but can work at low sugar contents or without any sugar at all.

Effect of sugar composition on pectin gel strength (relative to sucrose). HE-Pectin Glucose syrup DE40 Glucose syrup DE60 HFCS 42 HFCS 55 Fructose Invert sugar – – –   – LE-Pectin – –     Table 2. The large molecules tend to give a high deformation gel strength. The higher average molecular weight of the sweetener. TExTURE 29 . high levels of maltose and glucose and low levels of high molecular weight oligosaccharides are important. sucrose and maltose tend to give better true gel strengths than high molecular weight oligosaccharides found in glucose syrups. simple sugars like glucose. HE-Pectin Glucose syrup DE40 Glucose syrup DE60 HFCS 42 HFCS 55 Fructose Invert sugar  – –    LE-Pectin  –     Table 1. but with low elasticity and with syneresis. Effect of sugar composition on pectin gel setting temperature (relative to sucrose).In high ester pectin gels. Table 1 summarises the effect on pectin gel setting temperature when substituting sucrose with other sugars. When choosing glucose syrups for high ester pectin gels. The subsequent effect on gel strength is shown in table 2. the higher the tendency to increased setting temperature.

was substituted by a given alternative carbohydrate sweetener.67 0.65 0.6 3.6 3.7 81.1 78.6 °Bx 80. on a weight basis.1 DS% 81. see table 3.2 aw 0. and figure 2 shows the corresponding results for the glucose and fructose syrups listed in table 4.2 80. Case study : Gel strength from basic sugars Base : Formula X1 Force (N) Sucrose Resulting parameters pH Sucrose Fructose Glucose Sorbitol Xylitol 3.6 3.65 0.4 79.6 79. One third of the sucrose.63 Fructose Glucose Sorbitol Xylitol Distance (mm) Figure 1. Case study of gel strength – basic sugars. and the gel strength of the resulting pectin jellies was measured. TExTURE 30 .6 81.0 80. Figure 1 summarises the results for some of the basic sugars.66 0.The effect of various carbohydrate sweeteners on the gel strength of pectin jellies is illustrated in the following case study in which pectin jellies were made according to formula X1.9 80.6 3.

D.0 kg 24. Basic formula for case study of pectin jellies TExTURE 31 . C.0 kg 0.0 kg 46.74 kg Table 3.0 kg (as DS) Glucose syrup Starch moulded. Case study of gel strength – glucose / fructose syrups.Gel strenght of pectin jellies with various glucose/fructose syrups – Formula X1 Force (N) Glucose syrup DE40 Glucose syrup DE60 Isoglucose Glucose syrup DE45 High maltose Distance (mm) Figure 2. Pectin Sugar Sugar Water evaporated to 100 kg total 1.5 kg 5. 24-25 hours Citric acid 50% 0. Basic formula for case study with pectin jellies with various glucose/fructose syrups – Formula X1 Water 30.37 kg Grindsted XSS 100 A. Sodium Citric acid B.4 kg 0.

pH DE25 DE40 DE60 HM ISO-GL 3 . Reference: McGee.4 78 . Parameters for pectin jellies with glucose/fructose syrups.’On Food and Cooking’.67 Table 4.72 0 .9 78 .5 ˚Bx 78 .73 0 .3 3 . Parameters for pectin jellies with various glucose/fructose syrups.6 76 .70 0 .. H.0 78 .5 3 .4 3 .5 78 .9 aw 0 . TExTURE 32 .5 78 . Case study of formula X1.9 78 .72 0 .5 78 . Scribner. 2003.4 3 .5 DS% 78 .

50 0 . For crystalline.. During the crystallisation process a specific crystal size and crystal size distribution are obtained by strict control of the nucleation and growth parameters of the sucrose crystals. Sugar particle size is normally determined by way of a sieve analysis in which the particles are sorted by size.35 80%<0. The mean particle size and the particle distribution determine the physical behaviour of the sugar.1-0 . Various commercial grades of crystallised sugar with different particle sizes are obtained by screening or milling of the crystalline sugar.75 0 .Particle size Sugar particle size An important stage in sugar production is the crystallisation of sucrose. non-screened sugar it is assumed that the size distribution follows a normal distribution. bulk density. A narrow particle size distribution – i.g. see table 1. Particle size for 90% of the sugar mm 1 . e. resulting in higher bulk density. the voids between the large particles can be filled by smaller particles.5-1 . Bulk density primarily depends on the particle size and increases with decreasing particle size. which is the standard deviation related to the mean particle size. flow properties and abrasion.20 0 . the particles are relatively uniform in size – means a lower bulk density than for a wide particle size distribution. Influence of particle size on bulk density (van der Poel et al. 1998).25 0 . and the relations between the amounts of the different ‘fractions’ are calculated.1 mm Bulk density g/l 822 864 887 894 902 565 Table 1. the crystals are separated into different size fractions. Size reduction can be obtained by grinding the sugar crystals. Based on this assumption the mean particle size is calculated as the hypothetical mesh aperture of a sieve that allows 50% of the sugar to pass. Chemical properties such as purity and dissolution rate are also influenced by the crystal size. In the latter case. The standard deviation is used as a measure for the particle size distribution and is normally stated as the coefficient of variance. By passing sugar through vibrating multi-deck screens. TExTURE 33 .0-2 .e.2-0 .2-0 .

when particles become very small they are difficult to moisten and disperse and tend to lump.9% with the major non-sugar present being water. Instant Sugar is made from finely milled sugar spray-dried onto water droplets. The average particle size of Instant Sugar is 200-400 micron. respectively. non-sucrose substances are mainly found in the syrup film covering the crystal surface. see figures 1-2. The dissolution rate of sugar depends on the size of the particles (other conditions remaining constant). sugar with a coarse crystal size is purer than sugar with a fine crystal size. However. and it affects volumetric dosing. the purity of commercial sugars is above 99. granulated 250-400 micron 500-850 micron Figure 1: Dissolution time of different sugars at 5°C. Dissolution time of different types of sugar at 5°C % dissolved 120 100 80 60 40 20 0 0 10 20 30 40 50 60 70 80 90 Seconds Icing sugar Instant sugar < 250 micron Std. Since the specific surface area decreases markedly with increasing crystal sizes. since increasing temperature increases dissolution rates. In most cases. vacuum or compressed air. As regards purity. This process produces agglomerates with a porous structure that makes the product rapid dissolving. In combination with the moisture content. as fine particles dissolve more rapidly than coarse particles. Temperature also affects the dissolution rate.The bulk density determines the space required for bulk storage of sugar in silos. the particle size distribution determines the flow properties of the sugar. In practice this is observed when more than 5% of the particles are less than 200 micron. The purity of icing sugar and other milled products of course depends on the purity of the starting material. The average particle size of Icing Sugar and Standard Granulated Sugar is 20 micron and 500-600 micron. TExTURE 34 . If crystalline sugar is stored correctly (above 10°C and at 40-65% RH) it will remain free-flowing and can easily be conveyed by means of gravity.

Fine particles give a smooth texture and. granulated 250-400 micron 500-850 micron Figure 2. however. Dissolution time of different sugars at 80°C. recrystallises during the conching process. In cookies and sweet biscuits. The finer the sugar.Dissolution time at 80°C % dissolved 120 100 80 60 40 20 0 0 10 20 30 40 50 60 70 80 90 Seconds Icing sugar Instant sugar < 250 micron Std. as a rule-of-thumb. The main purpose of the refining process is to reduce the particle size to avoid a sandy-gritty mouthfeel in the final product. the particle size affects the dough spread during baking and as such the diameter and height of the final product. Sugar particle size also affects the texture of the cookie or sweet biscuit and thus the mouthfeel. Particle size also influences the flow and solid formation of chocolate. where most of the sugar is dispersed in the fat phase. the more spread. although some amorphous sugar is formed during the preceding sugar milling and chocolate mass refining. A coarser sugar produces a crisper cookie. TExTURE 35 . the mouthfeel is smooth and no particles are sensed when less than 5% of the particles are bigger than 30 micron. In moulded chocolate. sugar is found mainly in the crystalline state. Most of the amorphous sucrose. Sugar particle size and applications The crystal size distribution affects the quality of the foods in which sugar is only partially dissolved and it is the main contributor to the structure or consistency of the product.

toffee/fudge and marzipan are other examples of how sugar particle size influences the functional properties of food. Reiser (1995): Sucrose. where the porous structure of the agglomerates ensures good binding of other ingredients. where sucrose is used as a carrier for other ingredients. Schwartz (1998): Sugar Technology. Schiweck. TExTURE 36 .W. H. T. The fondant colour is also influenced by the sugar particle size. frostings and fondants. as smal particles give a whiter icing or fondant due to a different reflection of light. The risk of segregation of ingredients can be minimised by using screened sugar with a particle size close to that of the other ingredients or by using Instant Sugar. Some of the factors affecting the grain size are the presence or introduction of undissolved sugar crystals.The texture and mouthfeel of fat/sugar-based biscuit fillings. P. van der Poel. including colours and flavours. In dry blends. Beet and Cane Sugar Manufacture (Bartens). Sugar particle size is also essential for the texture and mouthfeel of icings. References: P. the temperature at which the agitation starts during cooling. M. In classical fondant manufacture the size of the crystals precipitated from the supersaturated solution affects the mouthfeel. Mathlouthi. properties and applications (Blackie Academic & Professional). A high quality fondant has a particle size of about 10 micron. crystal size is an important property. and the presence of invert sugar.

meaning that the viscosity is independent of the shear rate. The results are presented in tables 1-2 and illustrated in figures 1-2. The viscosity has been measured. °C 65 72 76 78 79 80 81 82 83 84 Viscosity mPas 31 16 20 17 56 26 32 27 97 46 56 48 176 87 105 92 110 69 55 50 200 125 110 90 415 269 220 190 1020 664 500 490 1600 2300 4800 7000 11900 19000 580 2840 2588 1000 7000 5000 1500 7400 2100 3240 5000 10300 15000 21200 10400 21000 42800 59000 72600 240 1040 904 390 2300 1700 510 3220 2100 700 4800 2880 1050 6660 4000 5650 9500 15400 1700 120 454 372 180 900 500 220 1220 780 290 1700 998 446 2270 1500 1780 2800 4230 580 243 171 500 270 702 330 850 411 1040 560 709 1100 1480 Sucrose Invert Glucose Fructose Sucrose Invert Glucose Fructose Sucrose Invert Glucose Fructose Sucrose Invert Glucose Fructose 50 50 50 50 40 40 40 40 30 30 30 30 20 20 20 20 Table 1. glucose and fructose at different Rt and temperatures.Viscosity The viscosity of sucrose solutions and other bulk sweeteners is highly dependent on the dry substance and temperature. and mixes of them. at different concentrations and temperatures for selected sugars. However. TExTURE 37 . Pure sucrose. sugar mixes and glucose syrups. the viscosity decreases when the shear rate increases. Viscosity of sucrose. invert sugar. fructose and glucose solutions. 1 mPas = 1 cP. using flow curves on a Bohlin VOR Rheometer. are all Newtonian. Rt temp. i. highly concentrated glucose syrups can be slightly pseudoplastic.e.

1 mPas = 1 cP. Viscosity of glucose syrup DE40 and DE60 at different Rt and temperatures. Rt Temp. invert sugar. TExTURE 38 . Viscosity of sucrose. °C DE40 DE60 DE40 DE60 DE40 DE60 DE40 DE60 50 50 40 40 30 30 20 20 65 72 76 78 79 80 81 82 83 84 Viscosity mPas 48 32 102 51 207 91 400 176 238 99 460 184 987 378 2370 894 600 230 1120 370 2900 1120 8000 2800 992 401 1860 836 5080 2710 15300 6180 1130 516 2800 1140 7500 2880 24000 8870 1320 686 3540 1540 9590 4100 30700 12800 2500 945 6500 2150 20000 6180 70000 21100 3900 1300 11100 3020 32000 8720 32800 5460 1860 15000 4660 49800 14900 57900 21800 93800 6840 2420 114000 219000 Table 2. glucose and fructose at different Rt and temperatures.Viscosity at different Rt and temperatures Viscosity mPas 100000 10000 1000 100 10 64 66 68 70 72 74 Rt % Sucrose 50°C Sucrose 40°C Sucrose 30°C Sucrose 20°C Invert 50°C Invert 40°C Invert 30°C Invert 20°C Glucose 50°C Glucose 40°C Glucose 30°C Glucose 20°C Fructose 50°C Fructose 40°C Fructose 30°C Fructose 20°C 76 78 80 82 84 Figure 1.

glucose syrup DE40 and glucose syrup DE60 at different Rt and temperatures. TExTURE 39 .Viscosity at different Rt and temperatures Viscosity mPas 100000 10000 1000 100 10 64 66 68 70 72 74 Rt % DE40 50°C DE40 40°C DE40 30°C DE40 20°C DE60 50°C DE60 40°C DE60 30°C DE60 20°C Sucrose 50°C Sucrose 40°C Sucrose 30°C Sucrose 20°C 76 78 80 82 84 Figure 2. Viscosity of sucrose.

9 82 .7 65 .3 1 .5 84 .5 66 .6 Table 3.4 Difference 1 .0 0 .8 80 .0 Difference -1 .8 Ds 63 .9 72 .1 2 . Table 3 shows the difference between Rt and Ds values of selected sugars.4 Glucose Rt 62 .2 2 .0 0 . glucose.5 82 .4 Ds 66 .4 -1 .5 -1 .7 Difference 1 .1 86 .4 75 .5 1 .0 Ds 76 .6 78 .4 Difference 0 . Rt is the same as real dry substance (Ds) for sucrose.9 77 .4 70 .3 77 .9 2 .4 64 . Differences between refractometric dry substance (Rt) and true dry substance (Ds).9 67 .7 82 .9 2 . whereas there is a difference between Rt and Ds for fructose. TExTURE 40 .Rt stands for refractometric dry substance.0 84 .3 1 .3 82 .3 Difference 1 .0 76 .4 1 .3 DE40 DE60 Rt 65 76 80 84 Rt 78 80 84 Ds 65 .7 Invert Rt 65 76 80 84 Ds 66 . Fructose Rt 65 .0 80 .5 1 . invert sugar and some types of glucose syrups.0 0 .

028 1. The viscosity of sucrose.817 5.134 1.140 119.055 1.021 1.188 6.028 1. sugars are mostly used in low concentrations.052 1.054 1. the viscosity provided by the sugar is quite important for the overall mouthfeel of the beverage.904 2.432 58.837 2.592 1.891 37. In jams and marmalades. % weight Sucrose 1 2 5 10 15 20 30 40 50 60 64 68 70 1.479 120.573 58. In food.330 1.Figures 1-2 cover highly concentrated sugar solutions and can be used by the food industry to choose the right pump for sugar solutions.045 10. Viscosity of sucrose.190 Viscosity mPas Glucose 1. Source of data: Leatherhead Food RA Scientific & Technical Surveys.480 285.336 1. which usually contain high amounts of sugar.453 Fructose 1.309 1. Although the viscosity of beverages is quite low (usually around 10%).491 11.048 178.710 476.566 1.998 5. the viscosity of the sugar has a big impact on the mouthfeel of the product. glucose and fructose at 20°C and at concentrations between 1% and 70% appears from table 4 and figure 3.161 15.145 1.146 1.533 1.571 Table 4.945 3. TExTURE 41 . glucose and fructose at 20°C.823 32.

Viscosity of sucrose. Viscosity of sucrose. TExTURE 42 . glucose and fructose at 20°C. glucose and fructose at 20°C Viscosity mPas 1000 100 10 1 0 10 20 30 40 Weight % Sucrose Glucose Fructose 50 60 70 80 Figure 3.

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