FLORIDA STATE HORTICULTURAL SOCIETY, 1952 226 presented in Tables 1 and 2. Degree Brix was determined by refractometer at 28 DC. and percent acid by titration with alkali, using the standard method of the citrus industry. Since previous work by Maurer et al. (5) showed a significant relationship between the naringin content of grapefruit and its maturity, some hope was held for finding a similar re lationship for Florida oranges and grapefruit. Unfortunately, this observation was not borne out by the grapefruit and orange varieties studied. Neither Brix, percent acid nor ratio could be correlated with the percent glucoside in the juice or its distribution in the fruit. The percent hesperidin in the juice of oranges was found to vary between 0.015 and 0.025 percent, while naringin in grapefruit juice va ried from 0.016 to 0.036 percent for most of the season. Distribution of Glucosides. — It is shown in Table 1 that almost 90 percent of the naringin in Duncan grapefruit is concentrated in the albedo, rag and pulp and this was also true for the other varieties of grapefruit stud ied. Also, it is shown in Table 2 that 75 to 80 percent of the hesperidin in Valencia oranges was concentrated in the albedo, rag and pulp. This also holds true for the other orange varieties. Thus, any attempt to ob tain higher juice yields by increased pressure or deeper burring by juice extractors would tend to increase the glucoside content of the juice (4). In this work, the fruit extracted to produce the largest juice yield contained the highest concentration of glucoside in the juice. 1. The glucoside content of four varieties of oranges and five varieties of grapefruit was found to be rather constant once the fruit had grown beyond an equatorial diameter of two inches. Thereafter, as the fruit grew larger, the glucoside content of all varieties studied decreased percentagewise with respect to weight of the fruit. 2. No correlation could be found between the change in glucoside content, distribution, percent in juice and the maturity of the fruit. The glucoside content of the orange juice samples varied between 0.015 and 0.025 per cent, while the grapefruit varieties ranged from 0.016 to 0.036 per cent. 3. The unusually high glucoside content of small fruit on a dry-weight basis suggested that it may have an important physiological role in citrus fruit metabolism. 4. From 75 to 80 per cent of the gluco side found in the four varieties of orange was concentrated in the albedo, rag and pulp, while in the grapefruit varieties 90 per cent was found in this same portion of the fruit. LITERATURE CITED 1. Armentano, L. The effect blood pressure. Feit. ges. zin 102: 219. 1938. 2. Davis, W. B. Determination of flavanones citrus fruits. Anal. Chem. 19: 476-8. 1947. in 3. Hall, J. A. Glucosides of the Navel orange. Amer. Chem. Soc. 47: 1191-1195. 1925. J. 4. Hendrickson, 5. Maurer, R. H., E. N. Burdick and C. W. Waibel. Distribution of naringin in Texas grapefruit. Lower Rio Grande Valley Citrus and Vegetable Inst. Fourth Annual Proceedings, Weslaco, Texas. 6. Rusznyak, I., and A. Szent-Gyorgyi. Flavanols as vitamins. Nature 138: 7. Szent-Gyorgyi, A. Methoden zur herstallung von citrin. Ztsch. f Physiol. Chem. 255: 126-131. 1938. Summary An investigation of the glucoside content of grapefruit and oranges led to the follow ing conclusions: of flavone dyes on Experimentelle Medi- R., and J. W. Kesterson. Orange concentrate evaporator scale identified as hespe ridin. Citrus 14: No. 14, 26-7. 1952. 1950. Vitamin P: 27. 1936. VISCOSITY OF CITRUS MOLASSES R. Hendrickson and J. W. Kesterson Florida Citrus Experiment Station Lake Alfred Citrus molasses often acquires such a viscous consistency that the familiar phrase "as slow as cold molasses" can be illustrated beyond all doubt. In fact, the viscosity at room tem perature sometimes increases to the point of solidification and, during this storage change, considerable insoluble (2). material precipitates Since high viscosity can lead to many difficulties in the handling and utilization of this product, a study was initiated to develop a better understanding of viscosity in citrus molasses. HENDRICKSON AND KESTERSON: To obtain representative material for the study, samples of citrus molasses were proeured monthly throughout the 1950-51 season from the evaporators of four processors. All samples were adjusted initially to a Brix of from 71° to 72°, and stored in one pint Mason jars in a constant-temperature room main tained at 80 °F. Viscosities were determined at 80 °F. with a Brookfield Synchro-lectric viscometer (multi-speed model LVF). The of ficial Lane-Eynon volumetric method was used to determine total sugars. The initial viscosity of each molasses sam ple, as shown in Table 1, was determined immediately after adjusting the Brix to 71° 72° and the temperature to 80 °F. Samples from plants C and D, which partially clarify their citrus press liquor, were more uniform and of lower viscosity than molasses from plants A and B. None of these exhibited the low viscosities (300 to 375 cps. at 80 °F.) typical of fully clarified citrus molasses of the same Brix (1). The centipoise is a viscosity unit that scientifically described how thick or thin a liquid is. It is more readily under standable by thinking of 0-500 centipoises as indicating a viscosity somewhere between wa ter and table syrup, while honey would read about 5,000 centipoises. Between 5,000 and 50,000 centipoises molasses pours with increas ing difficulty and pyramids when it falls be^lorida Agricultural ries, No. 38. Experiment Station TABLE Journal 1. — Se fore leveling out. 11-18-50 12-21-50 1-19-51 2-20-51 4-12-51 5-17-51 6-27-51 Somewhere between 50,000 and 100,000 centipoises molasses is so thick that a pint Mason jar of it can be inverted without losing the contents and for all prac tical purposes it is a solid. Color can be used to a limited extent as an indication of initial viscosity. In general, the lighter the color, the more insolubles present and the higher the viscosity. The samples under study were analyzed for total sugars to establish any relationship that might exist between sugar content and vis cosity. It seemed possible that a molasses of low sugar content would reflect a higher viscosity, since loss of sugars through fermen tation of the press liquor would require great er concentration to reach the same Brix. This greater concentration would increase the in solubles content which is a contributing fac tor to high viscosities. No significant relation ship between total sugar content, shown in Table 2, and the initial viscosity was found due to the overshadowing effect of other vari ables. An interesting note is that less than 30 per cent of the samples studied would pass the state minimum requirements of 45 per cent total sugars if concentrated only to the minimum Brix (71°) required by the state standards. Improper peel and press liquor storage is indicated by the low sugar con tent. A typical plot showing how the viscosity of citrus molasses changes while in storage Initial viscosity of freshly produced citrus molasses procured from four plants throughout the 1950-51 season. (71°72° Brix, 80°F.) Viscosity Date Processed 227 MOLASSES VISCOSITY Plant A 4140 2000 2000 2300 4200 47,500 19,500 Plant in Centipoises B Plant C Plant D 8500 16,000 4800 1500 1960 2840 2000 1900 2500 2500 750 3100 10,600 2900 1700 2300 11,600 8,000 1800 1200 1550 TABLE 2. — Total sugar content of citrus molasses samples procured for viscosity study. Percent Dale Processed 11-18-50 12-21-50 1-19-51 2-20-51 4-12-51 5-17-51 6-27-51 Plant A 44.4 45.6 48.0 47.4 44.2 44.0 43.0 Total Plant 42.7 35.8 37.0 40.4 45.8 44.2 43.7 B Sugars as Invert Plant C Plant D 35.8 36.9 46.4 43.8 38.5 41.8 34.6 35.9 46.4 45.5 44.1 37.5 44.8 34.7 FLORIDA STATE HORTICULTURAL SOCIETY, 1952 228 is given in Fig. 1. The particular samples depicted were obtained early in the 1950-51 season and since other later samples produced similar curves they were omitted for the sake of brevity. The viscosity of most samples was found to increase linearly in relation to the time of storage. The increase in viscosity fur ther was found attributable to the formation of a gelatinous structure easily broken by stir ring or heating. Although viscosity measure ments made at the beginning of this study indicated a non-changing viscosity on account of excessive stirring, subsequent readings es tablished -the linearly increasing viscosity. However, the insolubles of the molasses tend ed to settle, thus causing the top portion of the sample to exhibit too low a viscosity. This occurred only in samples of sufficiently low viscosity to allow settling of insolubles. Formation and evolution of gas which in creased the volume of the sample and broke the fragile built-up structure also caused false ly low viscosity readings. When the molasses samples were stirred violently to disperse the gelatinous structure 30 formed during 160 days of storage, the ac cumulated viscosity increase practically dis appeared. Further static storage, however, brought about viscosity increases at corre spondingly similar rates. The citrus molasses processor can therefore lower the viscosity of his molasses considerably by merely pumping it from his storage tank. On the other hand, if it is stored for any considerable period by the purchaser there is always the possibility that a highly viscous condition will return. Since the viscosity of citrus molasses can in crease rapidly while in storage, the processor must use pumps and motors of higher capacity and horsepower to pump molasses from a stor age tank. This necessity is aggravated by the settling of suspended insolubles which significantly adds to the viscosity of molasses near the storage tank outlet and is further amplified by reason of pipe friction increasing in proportion with viscosity. When the molasses samples were diluted to 65° Brix and held in 80 °F. storage, the ma jority of samples acted much like the 71° -72° Plant A Pldnt B Plant C Plant D Citrus Molasses 7l-72°Brix Procured n/18/50 .4 V) Samples ,/Vigorously Vi r Stirred Samples before reading Viscosity Stirre o o o J0- ,€) i i Insolubles Settling Out o u I 20 40 60 80 100 120 Days of 80°F Storage 140 Fig. 1. — Rate of viscosity change of citrus molasses samples while in storage. 160 180 200 HENDRICKSON AND KESTERSON: Conclusions Brix samples but maintained a correspondingly lower viscosity. Although previous laboratory experiments established that more insolubles precipitated from high pH press liquors with the possible consequence of a higher viscosity, no corre lation was found between pH and viscosity. An attempt to relate the quality and quantity of pectin in citrus molasses to viscosity was also to no avail. The procedure for determin ing pectin measured the quantity of alkali re quired to de-esterify a known weight of al cohol precipitate from 150 grams of molasses. No attempt was made to relate viscosity to percent pectin since the data of Iranzo and Veldhuis (3) showed it to be futile. When the rate of viscosity increase in centipoises per day was determined and tabulated as shown in Table 3, no relation was found between this factor and sugar content, pH, insoluble solids, quality and quantity of pec tin. The rate was calculated to represent the average change during the first month of stor age. No seasonal trends were noted either in the initial viscosity or rate of viscosity in crease. Initial viscosity, however, is prob ably a rough index of the rate of future vis cosity change and therefore an aid in antici pating high viscosity troubles. Sub-surface gas formation was clearly visi ble in approximately 50 per cent of the sam ples, while swelling from more profuse gas formations occurred only in 25 percent of the samples. Three samples were found to be very noticeably unstable, so much so that even mild stirring released such quantities of gas from solution that the molasses foamed up and overflowed from the container in a mat ter of minutes. This phenomenon is much like charged soda water which also foams and boils with only mild agitation. The high viscosity of molasses as compared to water prevents the quick escape of the released carbon dioxide and thereby causes swelling. TABLE 3. 1. Partial clarification of press liquor in the manufacture of citrus molasses has the beneficial effect of providing a lower and more uniform viscosity in the final molasses. 2. Total sugar content, pH, quality and quantity of pectin in citrus molasses were not significantly related to the initial viscosity or to the rate of viscosity increase while in storage. 3. The viscosity of most molasses samples appeared to increase linearly with time and was considerably influenced by agitation, set tling of insoluble solids and sub-surface gas formation. 4. The viscosity increase of citrus molasses during storage was in a large part due to the formation of a gelatinous structure. When the gelatinous structure was broken, it would immediately start to reform. 5. The viscosity of most molasses samples continued to increase even after 160 days of storage. This increase in viscosity can be practically eliminated by thorough agitation or heat. 6. Molasses samples of 65° Brix exhibited changes similar to 71°-72° Brix samples, but at a lower level. 7. No seasonal trends were noted either in initial viscosity or the rate of viscosity in crease. 8. A viscosity increase of more than 500 centipoises per day is cause for serious con cern since the molasses will probably solidify within three months. LITERATURE CITED 1. Hendrickson, R. Florida citrus molasses — Clari fication of citrus press liquor. Fla. Agr. Exp. Sta. Tech. Bui. 469: 5-24. 1950. 2. Hendrickson, R., and J. W. Kesterson. Storage changes in citrus molasses. Proc. F'la. Hort. Soc. 63: 154-162. 1950. 3. Iranzo, J. R., and M. K. Veldhuis. The composi tion of Florida citrus molasses. Proc. Fla. Hort. Soc. 11-18-50 12-21-50 1-19-51 2-20-51 4-12-51 5-17-51 6-27-51 61: 205-211. 1948. Rate of viscosity increase for citrus molasses samples in undisturbed storage. Centipoise Date Processed 229 MOLASSES VISCOSITY Plant A 220 580 240 450 430 1300 2200 Plant B 310 200 730 190 490 370 700 Increase per Day Plant C Plant D 70 120 130 120 130 80 60 70 250 130 70 70 220 90