PHYSIO CHEMICAL CHARACTERISTICS OF THREE TYPES OF CANE SYRUP

By Hashim Tag EL-Deen Hashim Abass B.Sc. Honours (Educ.) AL-Zaim AL-Azhari University ٢٠٠٢

Supervisor Dr. Hassan Ali Mudawi

A Thesis Submitted to the University of Khartoum in Partial Fulfillment for the Requirement of Master of Science (Agric)

Department of Food Science and Technology Faculty of Agriculture, University of Khartoum

٢٠٠٦-May ١

DEDICATION

I dedicated this research to my father soul,

Also, dedicated to my mother who gave me strength

Hashim

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ACKNOWLEDGEMENTS

I am grateful to Allah, my special praise and thanks for giving me the health, strength and patience to conduct this research. I would like to express my gratitude and sincere appreciation to my supervisor Dr. Hassan Ali Mudawi.for his excellent supervision, encouragement, and guidance throughout this work. Specially thank and respects are extended to En. Mahmmoud Mansor Osman, the researcher in industrial and consultancy research centre for his great aid and encouragement. Extra thank extended also to En. Abd-ELrahim Adam and staff of specialiaty products department of Kenana sugar factory for their helps. A lot of owed to laboratory technical staff of Shambat, El-Guneid factory, and Desertification Research Institute for their helps. Finally, great thank and obligation to every one contributed to this work and not mentioned.

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ABSTRACT

Comprehensive physio-chemical analyses were carried out for sugar cane syrup in an attempt to assess quality of locally edible cane syrup and to compare between Tate and Lyle syrup qualities. Within the study analysis were conducted on four locally cane syrups, which are Kenana amber and treacle syrup, Saeed golden syrup, and AL- Modhesh golden syrup, in addition to the British golden syrup (Tate and Lyle) which is used as a reference. The analysis included determination of total soluble solids (TSS), total sugars, reducing sugars, sucrose, gravity purity, ash, minerals, pH, acidity, moisture, nitrogen and protein content. Similarly physical properties were measured mainly: viscosity, color, and refractive index. The results obtained revealed that the average percentage of Kenana amber ,٪٨١ total soluble solids (TSS) of Tate and Lyle was Reducing .٪٧٩ and AL-Modhesh,٪٨١ Saeed ,٪٨١ Kenana treacle ,٪٨٢ Kenana ,٪٤٧٫٣ ,for Tate and Lyle, Kenana amber ٪٤٨٫٣ sugars were for AL-Modhesh. Sucrose was ٪٤٥٫٥ and ٪٤٦٫٣ treacle, Saeed ,for Tate and Lyle, Kenana amber ٪٣٧ ,٪٣٤٫٢ ,٪٣٣٫٦ ,٪٣٢٫٤ ,٪٣١٫٨ Kenana treacle, Saeed, and AL-Modhesh respectively. Three local samples results of sugars content were similar to the Tate and Lyle

٤ syrup and Sudanese Standards Metrology Organization (SSMO), while sugars content of AL-Modhesh syrup was different. ,for all the samples ٪٢١-١٨ Moisture content was between which is similar to the reference and SSMO. AL-Modhesh syrup was more acidic than other local syrups which were identical with the for Tate and ٪٣٩٫٢ reference and the standard. Gravity purity was for Kenana ٪٤٢ for Kenana amber, while it was ٪٣٩٫٦ Lyle and for ٪١٫٤ for AL-Modhesh. Ash content was ٪٤٦٫٨ ,treacle and Saeed ٪١٫٥ ,for Kenana amber and Saeed ٪١٫٢ Tate and Lyle, while it was for AL-Modhesh. All samples of syrup ١٫٠٥ for Kenana treacle, and were poor of nitrogen and protein content. Minerals were determined by atomic absorption spectrometer and it was found that, Tate and Lyle and AL-Modhesh has a higher percentage of sodium than other minerals, while Kenana sample amber and treacle) and Saeed has scored the highest percentage of calcium. All tested samples contained enough amounts of sodium, calcium, and magnesium, and these are the most important minerals from nutritional point of view. It was noticed that all samples contained less phosphate while they showed the same amounts of cobalt, iron, manganese, copper, chrome, nicle, lead and zinc. ,٤٫٠٨ ,٤٫٢٠ ٣٠ْc and found to be The viscosity was calculated at ,centistokes for Tate and Lyle, Kenana amber ٤٫٠٢ ,٤٫١٥ ,٤٫١١ Kenana treacle, Saeed, and AL-Modhesh respectively. The colour of ٢٠٠٠ the syrups was measured colour metrically and was found to be ICUMSA ,١٨٩٣ ,٢٢١٢ ,٩١٧٩ ,٢٤٠٠ ICUMSA for Tate and Lyle, and

٥ for Kenana amber, Kenana treacle, Saeed, and AL-Modhesh respectively. The colour of all local syrups matched with SSMO standard except AL-Modhesh syrup. ,for Tate and Lyle and Saeed ١٫٥٠٠٠ Refractive index was for ١٫٤٩٩٠ for Kenana amber and ١٫٤٩٦٠ ,for AL-Modhesh ١٫٤٩٣٠ the treacle.

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ﺑﺴﻢ اﷲ اﻟﺮﺣﻤﻦ اﻟﺮﺣﻴﻢ ﺧﻼﺻﺔ اﻷﻃﺮوﺣﺔ

ﺃﺠﺭﻴﺕ ﺘﺤﺎﻟﻴل ﻓﻴﺯﻴﺎﺌﻴﺔ ﻭﻜﻴﻤﻴﺎﺌﻴﺔ ﻋﻠﻰ ﻋﺴل ﻗﺼﺏ ﺍﻟﺴﻜﺭ ﻓﻲ ﻤﺤﺎﻭﻟﺔ ﻟﻠﺘﻌﺭﻑ

ﻋﻠﻰ ﺠﻭﺩﺓ ﺍﻟﻌﺴل ﺍﻟﻐﺫﺍﺌﻲ ﻭﺍﻟﻤﺼﻨﻊ ﻤ ﺤ ﻠ ﻴ ﺎﹰ ﻭﻤﻘﺎﺭﻨﺘﻪ ﺒﺎﻟﻤﻭﺍﺼﻔﺎﺕ ﺍﻟﺴﻭﺩﺍﻨﻴﺔ ﻭﻤﻭﺍﺼﻔﺎﺕ

ﺍﻟﻌﺴل ﺍﻹﻨﺠﻠﻴﺯﻱ ﺍﻟﻤﺴﺘﺨﺩﻡ ﻜﻤﺭﺠﻊ. ﺘﻡ ﺘﺤﻠﻴل ﺃﺭﺒﻌﺔ ﻋﻴﻨﺎﺕ ﻤﻥ ﺍﻟﻌﺴل ﺍﻟﻤﺼﻨﻊ ﻤﺤ ﻠ ﻴ ﺎﹰ

ﻭﻫﻲ ﻋﺴل ﻜﻨﺎﻨﺔ ﺍﻟﺫﻫﺒﻲ، ﻋﺴل ﻜﻨﺎﻨﺔ ﺍﻷﺴﻭﺩ، ﻋﺴل ﻤﺼﻨﻊ ﺴﻌﻴﺩ، ﻋﺴل ﻤﺼﻨﻊ ﺍﻟﻤﺩﻫﺵ

ﺒﺎﻹﻀﺎﻓﺔ ﺇﻟﻰ ﺍﻟﻌﺴل ﺍﻹﻨﺠﻠﻴﺯﻱ.

ﺘﻀﻤﻨﺕ ﺍﻟﺘﺤﺎﻟﻴل ﺘﻘﺩﻴﺭ ﺍﻟﻤﻭﺍﺩ ﺍﻟﺼﻠﺒﺔ ﺍﻟﺫﺍﺌﺒﺔ ﺍﻟﻜﻠﻴﺔ، ﺍﻟﺴﻜﺭﻴﺎﺕ ﺍﻟﻜﻠﻴﺔ، ﺍﻟﺴﻜﺭﻴﺎﺕ

ﺍﻟﻤﺨﺘﺯﻟﺔ ﻭﺍﻟﻤﺤﻭﻟﺔ، ﺍﻟﺴﻜﺭﻭﺯ، ﺍﻟﻨﻘﺎﻭﺓ ﺍﻟﻨﻭﻋﻴﺔ، ﺍﻟﺭﻤﺎﺩ، ﺍﻟﻤﻌﺎﺩﻥ، ﺍﻟﺤﻤﻭﻀﺔ، ﺍﻟﺭﻁﻭﺒﺔ،

ﻭﻤﺤﺘﻭﻯ ﺍﻟﻨﻴﺘﺭﻭﺠﻴﻥ ﻭﺍﻟﺒﺭﻭﺘﻴﻥ ﻭﻜﺫﻟﻙ ﻗﺩﺭﺕ ﺍﻟﺨﻭﺍﺹ ﺍﻟﻁﺒﻴﻌﻴﺔ ﻤﺜل ﺍﻟﻠﺯﻭﺠﺔ، ﺍﻟﻠﻭﻥ،

ﻤﻌﺎﻤل ﺍﻹﻨﻜﺴﺎﺭ.

ﺃﺸﺎﺭﺕ ﺍﻟﻨﺘﺎﺌﺞ ﺇﻟﻰ ﺃﻥ ﻨﺴﺒﺔ ﺍﻟﻤﻭﺍﺩ ﺍﻟﺼﻠﺒﺔ ﺍﻟﺫﺍﺌﺒﺔ ﺍﻟﻜﻠﻴﺔ ﺒﻠﻐﺕ ٨١% ﻓﻲ ﺍﻟﻌﺴل

ﺍﻹﻨﺠﻠﻴﺯﻱ ﺒﻴﻨﻤﺎ ﺒﻠﻐﺕ ٨٢% ﻓﻲ ﻋﺴل ﻜﻨﺎﻨﺔ ﺍﻟﺫﻫﺒﻲ ﻭ ٨١% ﻟﻌﺴل ﻜﻨﺎﻨﺔ ﺍﻷﺴﻭﺩ ﻭﻋﺴل

ﺴﻌﻴﺩ ﻭ٧٩% ﻟﻌﺴل ﺍﻟﻤﺩﻫﺵ. ﺍﻟﺴﻜﺭﻴﺎﺕ ﺍﻟﻤﺨﺘﺯﻟﺔ ﺒﻠﻐﺕ ٤٨,٣% ﻟﻠﻌﺴل ﺍﻹﻨﺠﻠﻴﺯﻱ

ﻭﻋﺴل ﻜﻨﺎﻨﺔ ﺍﻟﺫﻫﺒﻲ ﻭ٤٧,٣% ﻟﻌﺴل ﻜﻨﺎﻨﺔ ﺍﻷﺴﻭﺩ ﻭ ٤٦,٣% ﻟﻌﺴل ﺴﻌﻴﺩ ﻭ ٤٥,٥%

٧ ﻟﻌﺴل ﺍﻟﻤﺩﻫﺵ. ﺒﻠﻐﺕ ﻨﺴﺒﺔ ﺍﻟﺴﻜﺭﻭﺯ ٣١,٨% ، ٣٢,٤% ، ٣٣,٦% ، ٣٤,٢% ،٣٧%

ﻓﻲ ﻜل ﻤﻥ ﺍﻟﻌﺴل ﺍﻹﻨﺠﻠﻴﺯﻱ، ﻜﻨﺎﻨﺔ ﺍﻟﺫﻫﺒﻲ، ﻜﻨﺎﻨﺔ ﺍﻷﺴﻭﺩ، ﺴﻌﻴﺩ ﻭﺍﻟﻤﺩﻫﺵ ﻋﻠﻰ ﺍﻟﺘﻭﺍﻟﻲ.

ﻭﻗﺩ ﺃﺘﻀﺢ ﻤﻥ ﺍﻟﺩﺭﺍﺴﺔ ﺃﻥ ﻤﺤﺘﻭﻯ ﺍﻟﺴﻜﺭﻴﺎﺕ ﻓﻲ ﺜﻼﺜﺔ ﻋﻴﻨﺎﺕ ﻤﻥ ﺍﻟﻌﺴل ﺍﻟﻤﺤﻠﻲ

ﻤﺸﺎﺒﻪ ﻟﻤﺤﺘﻭﻯ ﺍﻟﺴﻜﺭﻴﺎﺕ ﻓﻲ ﺍﻟﻌﺴل ﺍﻹﻨﺠﻠﻴﺯﻱ ﻭﺍﻟﻤﻭﺍﺼﻔﺎﺕ ﺍﻟﺴﻭﺩﺍﻨﻴﺔ ﺒﻴﻨﻤﺎ ﻤﺤﺘﻭﻯ

ﺍﻟﺴﻜﺭﻴﺎﺕ ﻟﻌﺴل ﺍﻟﻤﺩﻫﺵ ﻜﺎﻥ ﻤ ﺨ ﺘ ﻠ ﻔ ﺎﹰ.

ﻤﺤﺘﻭﻯ ﺍﻟﺭﻁﻭﺒﺔ ﻟﻜل ﺍﻟﻌﻴﻨﺎﺕ ﺘﺭﺍﻭﺡ ﺒﻴﻥ ١٨% - ٢١% ﻭﻫﻭ ﺍﻟﻤﺩﻯ ﺍﻟﻤﺸﺎﺒﻪ

ﻟﻠﻌﺴل ﺍﻹﻨﺠﻠﻴﺯﻱ ﻭﺍﻟﻤﻭﺍﺼﻔﺔ ﺍﻟﺴﻭﺩﺍﻨﻴﺔ. ﻋﺴل ﺍﻟﻤﺩﻫﺵ ﻜﺎﻥ ﺃﻜﺜﺭ ﺤﻤﻭﻀﺔ ﻤﻥ ﻜل ﻋﻴﻨﺎﺕ

ﺍﻟﻌﺴل ﺍﻟﻤﺤﻠﻲ ﻭﺍﻟﺘﻲ ﺘﹸﻁﺎﺒﻕ ﺍﻟﻌﺴل ﺍﻹﻨﺠﻠﻴﺯﻱ ﻭﺍﻟﻤﻭﺍﺼﻔﺔ ﺍﻟﺴﻭﺩﺍﻨﻴﺔ ﻓﻲ ﺩﺭﺠﺔ ﺍﻟﺤﻤﻭﻀﺔ.

ﺒﻠﻐﺕ ﻨﺴﺒﺔ ﺍﻟﻨﻘﺎﻭﺓ ﺍﻟﻨﻭﻋﻴﺔ ﻓﻲ ﺍﻟﻌﺴل ﺍﻹﻨﺠﻠﻴﺯﻱ ٣٩,٢%، ﻜﻨﺎﻨﺔ ﺍﻟﺫﻫﺒﻲ ٣٩,٦%،

ﻜﻨﺎﻨﺔ ﺍﻷﺴﻭﺩ ﻭﺴﻌﻴﺩ ٤٢,٣% ﻭﺍﻟﻤﺩﻫﺵ ٤٦,٨% . ﻤﺤﺘﻭﻯ ﺍﻟﺭﻤﺎﺩ ١,٤% ﻟﻠﻌﺴل

ﺍﻹﻨﺠﻠﻴﺯﻱ ﺒﻴﻨﻤﺎ ﺒﻠﻎ ١,٢% ﻓﻲ ﻜﻨﺎﻨﺔ ﺍﻟﺫﻫﺒﻲ ﻭﺴﻌﻴﺩ، ١,٥% ﻓﻲ ﻜﻨﺎﻨﺔ ﺍﻷﺴﻭﺩ، ١,٠٥%

ﻓﻲ ﺍﻟﻤﺩﻫﺵ، ﻭﻗﺩ ﺘﻼﺤﻅ ﻓﻘﺭ ﻜل ﻋﻴﻨﺎﺕ ﺍﻟﻌﺴل ﻤﻥ ﺍﻟﻤﺤﺘﻭﻯ ﺍﻟﻨﻴﺘﺭﻭﺠﻴﻨﻲ ﻭﺒﺎﻟﺘﺎﻟﻲ

ﺍﻟﺒﺭﻭﺘﻴﻥ. ﻗﺩﺭﺕ ﺍﻟﻤﻌﺎﺩﻥ ﺒﺠﻬﺎﺯ ﺍﻹﻤﺘﺼﺎﺹ ﺍﻟﺫﺭﻱ ﻭﻗﺩ ﻭﺠﺩ ﺃﻥ ﺍﻟﺼﻭﺩﻴﻭﻡ ﻴﻤﺜل ﺃﻋﻠﻰ

ﻨﺴﺒﺔ ﻓﻲ ﺍﻟﻌﺴل ﺍﻹﻨﺠﻠﻴﺯﻱ ﻭﻋﺴل ﺍﻟﻤﺩﻫﺵ, ﺒﻴﻨﻤﺎ ﻴﻤﺜل ﺍﻟﻜﺎﻟﺴﻴﻭﻡ ﺃﻋﻠﻰ ﻨﺴﺒﺔ ﻓﻲ ﻋﺴل

ﻜﻨﺎﻨﺔ ﺍﻟﺫﻫﺒﻲ ﻭﺍﻷﺴﻭﺩ ﻭﻋﺴل ﺴﻌﻴﺩ. ﻜل ﺍﻟﻌﻴﻨﺎﺕ ﺒﻬﺎ ﻨﺴﺒﺔ ﺠﻴﺩﺓ ﻤﻥ ﺍﻟﺼﻭﺩﻴﻭﻡ ﻭﺍﻟﻜﺎﻟﺴﻴﻭﻡ

ﻭﺍﻟﻤﻐﻨﺴﻴﻭﻡ ﻭﻫﻲ ﺍﻟﻌﻨﺎﺼﺭ ﺍﻟﻬﺎﻤﺔ ﻏﺫﺍﺌﻴﺎﹰ. ﻭﻗﺩ ﺘﻼﺤﻅ ﻓﻘﺭ ﻜل ﺍﻟﻌﻴﻨﺎﺕ ﻤﻥ ﺍﻟﻔﻭﺴﻔﺎﺕ ﺒﻴﻨﻤﺎ

٨ ﻜﺎﻨﺕ ﻤﺘﺴﺎﻭﻴﺔ ﻓﻲ ﻨﺴﺏ ﺍﻟﻜﻭﺒﺎﻟﺕ، ﺍﻟﺤﺩﻴﺩ، ﺍﻟﻤﻨﺠﻨﻴﺯ، ﺍﻟﻨﺤﺎﺱ، ﺍﻟﻜﺭﻭﻡ، ﺍﻟﻨﻴﻜل، ﺍﻟﺭﺼﺎﺹ

ﻭﺍﻟﺨﺎﺭﺼﻴﻥ.

ﻗﺩﺭﺕ ﺍﻟﻠﺯﻭﺠﺔ ﻋﻨﺩ ٣٠ ﺩﺭﺠﺔ ﻤﺌﻭﻴﺔ ﻭﻗﺩ ﺒﻠﻐﺕ ٤,٢٠ ، ٤,٠٨ ، ٤,١١ ، ٤,١٥ ،

٤,٠٢ ﺴﻨﺘﻲ ﺍﺴﺘﻭﻙ ﻓﻲ ﺍﻟﻌﺴل ﺍﻟﺫﻫﺒﻲ ﺍﻹﻨﺠﻠﻴﺯﻱ، ﻜﻨﺎﻨﺔ ﺍﻟﺫﻫﺒﻲ، ﻜﻨﺎﻨﺔ ﺍﻷﺴﻭﺩ، ﺴﻌﻴﺩ،

ﺍﻟﻤﺩﻫﺵ ﻋﻠﻰ ﺍﻟﺘﻭﺍﻟﻲ . ﺘﻡ ﻗﻴﺎﺱ ﺍﻟﻠﻭﻥ ﺒﺠﻬﺎﺯ ﻗﻴﺎﺱ ﺍﻟﻠﻭﻥ ﻭﻗﺩ ﺒﻠﻎ ٢٠٠٠ ﺍﻴﻜﻭﻤﺴﺎ ﻓﻲ

ﺍﻟﻌﺴل ﺍﻹﻨﺠﻠﻴﺯﻱ ﺒﻴﻨﻤﺎ ﺒﻠﻎ ٢٤٠٠ ، ٩١٧٩ ، ٢٢١٢ ، ١٨٩٣ ﺍﻴﻜﻭﻤﺴﺎ ﻓﻲ ﻜﻨﺎﻨﺔ

ﺍﻟﺫﻫﺒﻲ، ﻜﻨﺎﻨﺔ ﺍﻷﺴﻭﺩ، ﺴﻌﻴﺩ، ﺍﻟﻤﺩﻫﺵ ﻋﻠﻰ ﺍﻟﺘﻭﺍﻟﻲ. ﻜل ﻋﻴﻨﺎﺕ ﺍﻟﻌﺴل ﺍﻟﻤﺤﻠﻲ ﻤﻁﺎﺒﻘﺔ ﻓﻲ

ﺍﻟﻠﻭﻥ ﻟﻠﻤﻭﺍﺼﻔﺎﺕ ﺍﻟﺴﻭﺩﺍﻨﻴﺔ ﻤﺎ ﻋﺩﺍ ﻋﺴل ﺍﻟﻤﺩﻫﺵ.

ﻤﻌﺎﻤل ﺍﻹﻨﻜﺴﺎﺭ ﺒﻠﻎ ١,٥٠٠٠ ﻓﻲ ﻜل ﻤﻥ ﺍﻟﻌﺴل ﺍﻹﻨﺤﻠﻴﺯﻱ ﻭﻋﺴل ﺴﻌﻴﺩ، ﺒﻴﻨﻤﺎ ﺒﻠﻎ

١,٤٩٣٠ ﻓﻲ ﻋﺴل ﺍﻟﻤﺩﻫﺵ ﻭ ١,٤٩٦٠ ﻓﻲ ﻜﻨﺎﻨﺔ ﺍﻟﺫﻫﺒﻲ ﻭ ١,٤٩٩٠ ﻓﻲ ﻋﺴل ﻜﻨﺎﻨﺔ

ﺍﻷﺴﻭﺩ.

٩

LIST OF CONTENTS

Page Dedication………………………………………………………… i Acknowledgements……………………………………………….. ii Abstract………………………………………………………….. iii Arabic Abstract………………………………………………….. vi List of Contents………………………………………………... ix List of Figures ……………………………………………….... xiii List of Tables ……………………………………………….. xv ١ ..……………………………………Chapter One: Introduction ١ .………………………………………………… Cane sugar .١٫١ ٢ .…………………………Production of cane sugar in Sudan .١٫٢ ٢ .……………………………………Liquid sugar and blends .١٫٣ ٣ .…………………………………… Sucrose liquid sugar .١٫٣٫١ ٣ .………………………………………Invert liquid sugar .١٫٣٫٢ ٣ ..………………………… Definition of edible cane syrups .١٫٤ ٤ ..…………………………………… Objectives of the study .١٫٥ ١٠ ٥ .………………………………Chapter Tow: Literature Review

٥ ………………………………………………………General ٢,١

٦ .....…………………………The raw cane sugar production ٢,٢

١٣ …………………………Composition of edible cane syrups .٢,٣

١٣ .……………… Production of cane syrups in local factories .٢,٤

١٣ ..…………………………………Kenana sugar company .٢,٤,١

Saeed food .٢,٤,٢ ١٥ ..………………………………………factory

Al- Modhesh .٢,٤,٣ ١٥ ……………………………………factory

١٥ ...... …………………………The types of edible syrups .٢,٥

١٥ ……………………………………………………Blends .٢,٥,١

١٦ ……………………………………Louisiana cane syrup .٢,٥,٢

١٦ …………………………………………Sulphited syrups .٢,٥,٣

١٧ …………………………………………Edible Molasses .٢,٥,٤

١٧ ..………………………………Sucrose and invert sugar .٢,٥,٥

١٨ ……………………………………………Simple syrup .٢,٥,٦

١٨ .……………………………………………Maple syrup .٢,٥,٧

١١ ١٩ ..………………………………Some physical properties ٢,٦

..……………………Freezing Points of Sugar Solutions ٢,٦,١ ١٩

…………………Boiling point of invert sugar solutions .٢,٦,٢

١٩

.…………………… Viscosity of invert sugar solutions .٢,٦,٣ ٢٠

٢٣ ……………Color development in invert sugar solutions .٢,٦,٤

٢٣ ..………………Color development in sucrose solutions .٢,٦,٥

٣٠ .………………………………Some chemical properties ٢,٧

.…………………………………Chemistry of inversion ٢,٧,١ ٣٠

.………………………………Acid inversion of sucrose ٢,٧,٢ ٣١

..………………………………………Rate of Inversion ٢,٧,٣ ٣٤

٣٤ ..…………………………Effect of acid concentration .٢,٧,٣,١

٣٤ ………………………………… Effect of temperature .٢,٧,٣,٢

٣٥ .…………………………………………Effect of time .٢,٧,٣,٣

١٢ ٣٩ .……Methods of preparing small volumes of invert syrups .٢,٨

٣٩ …………………Rapid, small batch, using tartaric acid .٢,٨,١

.…………………Slow, Large batch, using tartaric acid .٢,٨,٢

٣٩

٤٠ …………………Large batches, using hydrochloric acid .٢,٨,٣

٤٠ ……inverts syrup using tartaric acid ٪٥٠ Preparation of .٢,٨,٤

٤٢ …………………Methods for the clarification of the syrup .٢,٩

٤٢ ..…………………………………Turbidity of the syrup .٢,٩,١

٤٢ .………………………………Sulphitation of the syrup .٢,٩,٢

٤٣ .………………………………Clarification of the syrup .٢,٩,٣

The removal of suspended impurities by syrup .٢,٩,٤

٤٤...clarification

٥١ ………………………………………Cane syrup storage .٢,١٠

٥٢ .…………Preservation of the syrup during shut-down .٢,١٠,١ ٥٤ ………………………Chapter Three: Materials and Methods ٥٤ …………………………………………………Materials .٣٫١ ٥٤ .……………………………………Methods of Analysis .٣٫٢ ٥٥ .…………………(Total Soluble Solids (T.S.S) (BRIX .٣٫٢٫١ ٥٥ ………………………………………Moisture Content ٣٫٢٫٢ ١٣ ٥٦ ..…………………………Determination of pH Value .٣٫٢٫٣ ٥٦ ………………………………………Refractive Index .٣٫٢٫٤ ٥٦ .………………………………………………Acidity .٣٫٢٫٥ ٥٧ …………………………………………Gravity Purity .٣٫٢٫٦ ٥٧ ..…………………………………………Total Sugars .٣٫٢٫٧ ٥٨ ..……………………………………Reducing Sugars .٣٫٢٫٨ …………………………………………………Sucrose .٣٫٢٫٩ ٥٩ ٥٩ ……………………………………………Ash content .٣٫٢٫١٠ ٥٩ .……………………………………Carbonated ash .٣٫٢٫١٠٫١ ٦٠ ………………………………………Sulphated ash .٣٫٢٫١٠٫٢ ٦١ ………………………………Minerals determination .٣٫٢٫١١ ٦٢ .……………………………………Nitrogen content .٣٫٢٫١٢ ٦٣ .……………………………………………Viscosity .٣٫٢٫١٣ ٦٣ .………………………………………………Colour .٣٫٢٫١٤ ٦٥ ..……………………Chapter Four: Results and Discussion ٦٥ ...... Total soluble solids and sugars content .٤٫١ ٦٩ ……………Refractive index, pH, Acidity and Moisture .٤٫٢ ٧٢ …… Gravity purity, colour, nitrogen content and protein .٤٫٣ ٧٥ ………………………………Ash content and viscosity .٤٫٤ ٧٨ …………………………………Minerals determination .٤٫٥ ٨٠ ..………Chapter Five: Conclusion and Recommendations ٨٣ ……………………………………………REFERENCES ٩١ ……………………………………………APPENDICES .

١٤

LIST OF FIGURES Fig no Title Page

٥ ……………………Chemical structure of sucrose Molecule .١

٨ .………………………………Production of raw sugar .٢

The three Massecuite systems used in raw .٣

١١ .………………………………………Sugar production

Skip flow chart for the production of .٤

١٥ ١٢ ……………………………………refined white sugar Approximate freezing points of syrups (by method .٥ ٢١ .…………………………………(of isotonic solutions Approximate boiling points of syrups (by method .٦ ٢٢ .…………………………………(of isotonic solutions invert syrup at different concentrations ٪٩٠ Viscosity of .٧ ٢٥ ………………………(corrected refractive dry solids) Effect of concentration on viscosity for .٨ ٢٦ ..………………٢٠ْc varying proportions of invert syrups at invert syrup of٪٩٣ Color development in .٩ ٢٧ ..……………varying PH values approaching neutrality Effect of prolonged heating on color development in invert .١٠ ٢٨ ……syrups containing high percentage of invert sugars Color development in sucrose liquid .١١ ٢٩ ..…………………………sugar at elevated temperatures Effect of acid concentration of liquid sugar .١٢ ٣٦ ………………………(by hydrochloric acid (TEMP٩٠ْc Effect of acid concentration of inversion .١٣ ٣٧ .……………(of liquid sugar by tartaric acid (TEMP١٠٠ْc Effect of temperature on inversion of liquid .١٤ ٣٨ .………………………………sugar by hydrochloric acid LIST OF TABLES

Table no Title Page

٣٣ .……………………………Inverting power of acids .١ Colour and Turbidity Removal with Various .٢

١٦ ٤٧ ………Phosphatation Treatments on Raw Syrup Average Reduction of some Impurities .٣ ٤٨ .……in Raw Syrup with continuous Clarification Average Reduction in some Impurities of Raw sugar .٤ ٤٩ .……with Continuous Clarification of Raw Sugar ٦٧ ..……Total soluble solids and sugar contents of syrups .٥ ٧٠ .…Refractive index, PH, acidity and moisture of syrups .٦ Actual purity, colour, nitrogen content, and protein .٧ ٧٣ ..…………………………………………of syrups ٧٦ .……………………Ash content and viscosity of syrups .٨ ٧٩ ..……………………………(Minerals of syrups (Mg/L .٩

١٧

CHAPTER ONE

١٨ INTRODUCTION

Sugar cane (saccharum officinarum) is a tropical gramineous crop that grows well under hot dry conditions when sufficient water is available. The main growing sugar cane countries are India, Brazil, Cuba and Mexico. Sugar cane is a -٢٫٥ ,٦٠٠cm in height-١٥٠ tall perennial grass; the plants are ٧cm in diameter. They show no tape roots, but adventitious root system which originates from the lower nodes of the stem. The .٢٥cm long-٥ stem is solid and composed of a series of joint The length, diameter, shape and colour of the joints are very greatly different and these are used for classifying the plants. It and ١٩٩٨ ,grows well in tropical and sub-tropical areas (Ali .(١٩٩٩ ,Ahmed CANE SUGAR .١٫٤ The manufacturing of cane sugar consists of two different sets of operations. In the first of these, the sugar is extracted from the sugar cane stalks, partially purified, and then followed by crystallization to raw sugar. The second step consists in purifying the raw and ultimate crystallization to fully refined sugar. Some plants are equipped to manufacture sugar, starting with the sugar cane and ending with refined cane sugar. In other situations the raw sugar is extracted in plants located in cane- producing areas and the raw so produced are then shipped,

١٩ usually in bulk, to refining plants located in population centres .(١٩٨٠ ,where they are fully refined. (Harry and Junk PRODUCTION OF CANE SUGAR IN SUDAN .١٫٢ In the Sudan, sugar cane was first planted and produced on commercial scale in early sixties with the commissioning of El- as ١٩٦٥ followed by New Halfa in ١٩٦٢ Guneid factory in .(١٩٨٤) reported by El-Hassan With increase in domestic demand for sugar in the early seventies the government commenced the planning for a large expansion in sugar production, that included public sector which ,١٩٧٩ and Kenana ١٩٧٩ Assalya ,١٩٧٦ projects at Sennar .(١٩٩٢ ,is one of the largest factories in the world,. (Adam As well, edible cane syrups are produced by private and small factory, such as, Saeed food factory in the industrial area- Khartoum North and Al-Modhesh factory in Khartoum industrial area. The mentioned cane syrup factories are practicing different processes to produce cane syrup. As well they have different production capacities. LIQUID SUGAR AND BLENDS .١٫٣ Liquid sugar as originally proposed and new commonly accepted is simply a solution of sugar in water. The sugar can be sucrose or invert or mixture of the two. The more recently developed liquid sweetener blends are water solutions of

٢٠ sucrose and\ or invert sugar with dextrose and\ or various corn .(١٩٦٦ ,syrups. (Hoynak and Bollenback More important types of liquid sugars are: Sucrose liquid sugar .١٫٣٫١ In many food products the ash level in sucrose liquid sugars is of no importance to the quality of the finished product. Other ingredients used may contain much more ash and, as a consequence, the ash in the sugar becomes insignificant. Invert liquid sugar .١٫٣٫٢ Liquid sugar in varying percentages of inversion has become widely accepted because the higher density of the solutions makes them less susceptible to yeast and mould growth. In addition, the higher densities permit the storage of more sugar in any given tank size as compared with straight liquid sugar. Moreover, in many situations, the freight cost per unit volume is lower for the higher density syrups. Fifty percent contains only ٪٧٧ invert liquid sugar having a concentration of .water in sucrose liquid ٪٣٣٫٥ water as compared with ٪٢٣ (١٩٦١ ,Joslyn) DEFINITION OF EDIBLE CANE SYRUPS .١٫٤ Edible syrups are viscous sweet liquids containing un- crystallisable sucrose, reducing sugars, dextrins, organic acids, nitrogenous matter and inorganic constituents. Golden syrup, which contains the highest portion of sucrose and invert sugar, is prepared from residues obtained during the production of

٢١ refined sugar. After removing the crystallisable sugar, the residue is boiled with dilute sulphuric acid. After neutralizing with chalk, the syrup is filtered through charcoal and .(١٩٧٦ ,concentrated under reduced pressure. (Person OBJECTIVES OF THE STUDY .١٫٥ The objective of this research is to asess the production of cane syrup in the Sudan in general, to evaluate the quality of the produced syrup with special reference to the nutritional value. Moreover, draw attention to the significance of this work to improve and up-grade the quality of the indigenous cane syrups to reach the international standard level.

٢٢

٢٣

CHAPTER TWO LITERATURE REVIEW

General ٢,١ It is manifested that sugar cane and sugar beet are the main sources of commercial sugar. It is a sweet disaccharide widely distributed in higher plants. On hydrolysis, one molecule of sucrose yield a molecule of D-glucose and a molecule of D-

(١٩٧٠.fructose. (Metcalf et al

CHO12 22 11 + HO 2 → CHO 6 12 6 + CHO 6 12 6

Sucrose glucose fructose The structure of sucrose is given by the following formula

.(١.Fig) (١٩٩٠ ,as shown by (Knecht

٢٤

H٢COH

H HOCH٢ H H O O H OH H H OH OH O H٢COH H OH OH H

α - D- Glucopyranosyl - β -D Fructofuranoside

chemical structure of sucrose Molecule .١.Fig

In contrast to other mono-and- disaccharide’s is a non reducing sugars .The reducing groups, formyl or carbonyl of the mono saccharide constituents are consumed in the linkage between the two sugar units of glycoside formation. X-ray studies and work with enzymes, which were done by

showed that the configuration in the ,(١٩٧٢) Cann and Stumpt

fructose is β while that in the glucose is α . Sucrose is dextrorotary, glucose (dextrose) is also dextrorotary, while fructose (laevulose) is levorotatory when sucrose is broken down into two components of mono saccharides, and the resulting solution is levorotatory. This inversion from dextro- to levulo has given the name invert

.(١٩٩٠.sugar (Neil, and Charles

٢٥ Free glucose and fructose are also present in cane juice, raw sugar, molasses and treacle (black syrup). The presence of invert sugar in raw sugar interferes with polarimetric accurate

,١٠٠ْ + determination of sucrose. Pure sucrose polarizes

Lal) ٨ ,٩٨+ and ٩٦+ however, raw sugar values range between

.(١٩٩٠ ,Mathur

THE RAW CANE SUGAR PRODUCTION ٢,٣ The raw cane sugar production process at the factory is

and may be divided into the following unit (٢) .shown in Fig operations and chemical conversions: - The cane is first washed to remove mud and debris, then it is chopped and shredded by shredder as preparations for extracting the juice. - Pressing the crushed cane through series of mills each of which consists of three-roll mills that extends heavy pressure, squeezes the juice. - Hot water and diluted juice are added to help macerating the cane and aid in the extraction.

.of juice could be extracted from the cane ٪٩٣ about - - The remainder of the cane bagasse is either burned for fuel or used to manufacture paper and hard board. - The juice is limed to remove both the insoluble and soluble impurities and change the pH.

٢٦ - Phosphoric acid might be added to the juice that contain a small amount of phosphates to clarify well.

١٠٥ْc and and ١٠٣ The juice is heated to between -

is attained ٧,١ to ٥-٦ Lime is again added until a pH of -

.(١٩٩٦ ,MC. Adamand and Tait) - The settled mud with small particles of bagasse can be filtered through a vacuum filter. The filter cake obtained by

of cane, and % ٤,٠ to ٣,٠ vacuum filteration represents contains sugar not extracted during filtration as a loss of

(١٩٨١ ,sugar production process. (Lal Mathur

Production of raw sugar .٢.Fig

CANE

BAGASSE IMBIBITION WATER JUICE EXTRACTION

FILTER JUICE MIXED JUICE

LIME MUDS FILTERATION PURIFICATION HEAT

CLARIFIED JUICE FILTER CAKE HEAT EVAPORATION

SYRUP ٢٧

EVAPORATION WATER HEAT CRYSTALLIZATION

The filtrated and clarified juice of high lime content,

water. It is heated in vacuum evaporator to ٪٨٥ contains about remove approximately two-third of water. Antonio and Carlos

reported that the product of the evaporation stage is (٢٠٠١)

to ٥,٣ Brix and ٪٦٥ to ٦٠ ,purity ٪٨٦ to ٪٧٨ sugar syrup of

invert sugars. The sucrose concentration of syrup is ٪٤,٥ adequate to allow its crystallization at the next stage of the process. - The first step of crystallization process involves increasing

by ,١,٤٠ and ١,٢٥ supersaturating of the syrup to between

٢٨ boiling in vacuum pans in order to effect the spontaneous production of sugar crystals. - Sugar crystals then grow in size of massecuite crystals.

.(١٩٩٧ ,Bostok) - The massecuite is sent to the cooling crystallizers to allow sugar recovery. - Remaining sucrose is transferred from the mother liquor to the crystal.

-the A (٣.In a three massecuite system (A.B.C) (Fig - massecuite and B-massecuite are directed to commercial sugar, while C-massecuite is used as seeds for the production of A-and B-massecuite. - Molasses referred to as final molasses and is separated from the crystalline sugar by centrifugation. Losses at the crystallization stage of raw sugar production occur due to poor recovery of sucrose from the final molasses. A long time lapse between cutting and bringing of the cane results in an increase in both polysaccharide and oligosaccharide contents, thus increasing the viscosity of the molasses and decreasing diffusion of sucrose from the mother liquor to the

.(١٩٧٦.crystal. (Jeanne.C White sugar is produced by direct processing of sugar cane

with higher sucrose content and is less coloured than raw (٤.Fig)

٢٩ sugar, and can be used directly for both domestic and industrial consumption. White sugar is processed using either carbonation or sulphitation techniques.

The three Massecuite systems used in raw sugar .٣. Fig production.

Vacuum

MCA MCB MCC

٣٠

SKIP FLOW CHART FOR THE PRODUCTION OF REFINED .٤.Fig WHITE SUGAR

CONCENTRATED LIQUOR

A A A A A-SKIP

A- SUGAR

٣١ A- SUGAR

COMPOSITION OF EDIBLE CANE SYRUPS .٢,٣

reported about the composition of the (١٩٧٠,Person)

total sugars , ٪٨٣ following products- golden syrups; total solids

-٤٧ ,reducing sugars as invert sugar ,٪٣٣-٣١ sucrose ,٪٨٣-٧٩

total sugars ,٪٨٣ Treacle, total solids :٪١,٧ sulphated ash ,٪٥٠

-٣٧ reducing sugars as invert sugar ,٪٣٣-٢٣ sucrose ,٪٨٠-٧٢

.٪٤,٠ sulphated ash ,٪٥٠

٣٢ reported that a good quality treacle must (١٩٩٩) .Amin, et al have the following figures for the suggested five calculated

%total sugar ,(٢-١,٥) parameters: sucrose / reducing sugars ratio

% sucrose% / total sugar ,٩٥ total soluble solid % not less than /

and reducing ,(٣٥-٣٠) reducing sugars% / total sugar ,(٦٥-٦٠)

.٪١٦ sugar / ash ratio

PRODUCTION OF CANE SYRUPS IN LOCAL .٢,٤ FACTORIES Cane syrup can be produced by local factories such as, EL- Guneid factory, New Halfa factory, Sennar factory, Assalya factory, Kenana Sugar Company, Saeed food factory and Al- Modhesh factory. These factories are using the same procedures for cane syrup production, but differ in the capacity, recipes and types of cane syrup.

Kenana sugar company .٢,٤,١ Kenana Sugar Company produces two types of edible syrups: Amber (golden) syrup produced by taking silver cane sugar liquor or A, B runoff silver, inverted and concentrated to form syrup. Treacle syrup produced by taking a runoff of refinery sugar, inverted and concentrated to form syrup. The Manufacturing steps are as follows:-

.٦٥Bْx Dilution of liquor or run-off to - ٣٣ .٨٥cْ Heating of liquor or run-off to - - Inversion of liquor or runoff by addition of HCL (food

.(١٥- to ١٠-) grade) to melt in inversion tank to get pol - Quantity of HCL depend on liquor or run-off pH,

(kg / Ton syrup ٢,٧ ≈ ) Quantity of HCL

.(kg / Ton syrup ١,١ ≈ ) Quantity of NaOH - Neutralization of inverted sugar by addition of caustic soda

.٦ food grade) to get pH) - Addition of liquor or run-off to the inverted sugar to get pol

.٦ and pH ,٥٨ inversion ,١٨ - Inversion was calculated by the following formula: inversion = BX – POL = X

٠,٠١٣ ¯ BX

Assume that inversion of final product required =

٥٨ = Y X – Y = Z

٠,٥ = inversion of fresh liquor

٥٧,٥ = ٠,٥ – ٥٨

Added quantity = 57.5 = H % z

٣٤ Added quantity = S = N H Where: S = quantity of melt before inversion. - Concentration of final syrup in evaporator under vacuum to

.BْX ٨٠,٥ reach

Saeed food factory .٢,٥,٢ Saeed food factory produce golden syrup by using the

٪١٢ ,sugar ٪٦٠ kg of syrup contained ١٠٠ formula: Each

٨٠ml HCL acid. It gm and ١٣٥ water, carbonate ٪٢٨ ,glucose applies the same procedure of cane syrup production, but with small quantities and one type of cane syrup which is “golden”. Al- Modhesh factory .٢,٥,٣ This factory produces edible syrup by using the following

,glucose ٪٢٠ ,sugars ٪٥٠ kg syrup contained ١٠٠ recipe: Each

,٧٠ml HCL acid, in addition gm carbonate and ١٢٠ ,water ٪٣٠ small amount of natural flavors and preservative material. THE TYPES OF EDIBLE SYRUPS .٢,٥ Blends .٢,٥,١ Most edible cane syrups in the market are blends of various types. Many are blended with maple syrup for flavoring, others contain added invert sugar and corn syrup. Refinery syrup are partly inverted char-filtered material, the most widely

٣٥ known of which is Tate and Lyles “golden syrup” (Kooreman,

(١٩٧١

Louisiana cane syrup .٢,٥,٢ These syrups are concentrated cane juice with no sugar removed. The simplest process has direct fired “open kettle” evaporators, but steam heat is common in larger plants, three- roller milling yields a juice from which syrup of superior flavor is obtained. Heat is the only clarifying agent, with constant skimming and brushing during evaporation to remove

reported that a second method uses a (١٩٧٢) ,impurities. Kool small amounts of lime, heat to boiling and settle. Brushing and skimming during evaporation remove further impurities. This product is darker and inferior in flavor to that of the simple

(٧٥ – ٧٣) ٣٥ْBe skim method. Both syrups are about ـand ـboil Brix. Sulphited syrups .٢,٥,٣ ton or more per day ٢٠٠ The larger syrup plants grinding employ sulphitation. Six – roller mills with little imbibitions are

and then , preferred. The strained juice is saturated with SO٢

pH. Boiling and setting follow, and ٦,٠ lime is added to about the clear juice is decanted, evaporated either in open kettles or

BX, and again allowed to settle, after ٥٠ multiple effect to about

٣٦ ٧٢ – ٧٠ which evaporation is continued in open evaporators to Brix. Fancy grades are stored in large tanks for further settling before canning. Much of this sulphited syrup is sold in bulk for blending with corn syrup or Molasses. A still fancier modification known as “cuite” is evaporated to heavy viscous

(١٩٧٧ ,confection for table use only. (Timbie and Keeny

Edible Molasses .٢,٥,٤ Many Louisiana Sugar houses which make cane syrup on large scale by the sulphitation process produce direct- consumption sugar by sulphitation from part of either cane crop ٨٠ and sell the molasses from this sugar. This Molasses is about apparent purity, clear, and light brown in color. It is ٥٠-٤٥ ,Brix known to the trade as boil- back molasses, and generally sold in .(١٩٧٦ ,bulk for blending. (LaL mathur The old- fashioned New Orleans molasses, which is no, longer on the market, was made by the open kettles, allowed to stand in cooling tanks, and then purged in centrifugals. The molasses was quite dark but had characteristic flavor which was (١٩٤٤.highly prized for many purposes. (Dahlberg and penczek

Sucrose and invert sugar .٢,٥,٥ By far the largest volume of syrup for human consumption consists of the “liquid sugars” of the refinery trade. These range Brix to white, yellow and light ٦٧ from water – white sucrose of

٣٧ Brix of sucrose and invert sugar in (٧٧ – ٧٦) brown solution .(١٩٨٠ ,varying percentages. (Culp Inverted sugar syrup is sucrose – based syrup treated with the enzyme invertase, and/or an acid which splits each sucrose molecule into one glucose and one fructose molecule, giving more rounded sweetness and preventing crystallization. Inversion can be partial as in products like golden syrup or conversion to glucose and fructose) depending ٪١٠٠) complete on the functional properties required. It is marketed under various names, including golden syrup (Tate and Lyle). (Marov, .(١٩٦٧

Simple syrup .٢,٥,٦ This is a mixture of sugar and water, that’s brought to boil and simmered for about five minutes, so that the sugar dissolves and the mixture becomes syrup. When it cools, it is used to make mixed drinks, liqueurs, baked goods, sorbets, sauces, and many other things. The thickness of the syrup depends upon the ratio of sugar to water used. Many simple syrup recipes call for equal parts sugar and water. For thinner syrup, combine two (١٩٦٠ ,parts water with one part sugar. (Charles

Maple syrup .٢,٥,٧ Maple syrup is made from the boiled sap of sugar maple trees. The taste and color are depending on the temperature at which the sap was boiled, and how long the sap was cooked.

٣٨ Grade (A) maple syrup is the most popular grade for every day use as a topping or pancakes, desserts, and other foods. It is usually made throughout most of the short syrup production season. Grade (B) syrup is generally made toward the end of the season; Grade (B) is much darker and has a stronger flavor, which makes it more suitable for flavoring and cooking purposes. It is thought that this late season syrup contains more minerals. Grade (C) syrup is no longer an official syrup grade. .(١٩٧٠ ,Gillett) SOME PHYSICAL PROPERTIES .٢٫٦ Freezing Points of Sugar Solutions ٢,٦,١ The approximate freezing points for solutions of sucrose, invert sugar, dextrose, and levulose (fructose) are shown in ٪٥٠ invert and ٪٥٠ invert syrup consists of ٪٥٠ The .٥.Fig invert syrup consists of ٪١٠٠ sucrose in the concentrations. The an equimolecular concentration of dextrose and fructose. The solubility of dextrose (glucose) at the temperatures indicated is lower than fructose, sucrose, or invert syrup, thus the reason for the shape of the solubility curve. The smaller graph in the figure illustrates the composition of the sugar at its eutectic point. This graph will be helpful in the selection of suitable sugar mixtures in the frozen food production. Of course any other soluble non- sugar substance in the solution may materially alter the freezing (١٩٥٨.point of the mixture. (Swindells, et al

Boiling point of invert sugar solutions .٢,٦,٢ ٣٩ Boiling point data are given in terms of the temperature of the solution or in terms of the boiling point elevation. The boiling point of a solution of invert sugar will depend upon the total concentration of the solids, the ratio of sucrose to invert Illustrates the variation of .٦.sugar, and to the pressure, Figure boiling points among invert syrup, sucrose, and dextrose or .(١٩٦٨ ,levulose. (Nicol

Viscosity of invert sugar solutions .٢,٦,٣ Three factors affect the viscosity of invert sugar solutions . These are temperature, concentration of total solids, and the percentage of invert sugar. The effects of both temperature and concentration of total invert sugar solutions of differing concentrations ٪٩٠ solids on corr.RDS” refers to“ .٧.of invert sugar. The expression in Fig Refractive Dry Substance with a correction for difference between sucrose and invert sugar readings. The effect of the degree of inversion on viscosity is (solids (corrected RDS ٪٧٢ Fore example, at .٨.illustrated in Fig ٪٩٠ ,٥٠٠ invert ٪٥٠ ,٨٥٠ the viscosity in centipoises is: sucrose .(١٩٦٧ ,Norrish) .٣١٠ invert ٪١٠٠ and ,٣٣٥ invert

٤٠ APPROXIMATE FREEZING POINTS OF SYRUPS (BY.٥.Fig METHOD OF ISOTONIC SOLUTIONS)

٤١ APPROXIMATE BOILING POINTS OF SYRUPS (BY METHOD.٦.Fig OF ISOTONIC SOLUTIONS)

Color development in invert sugar solutions .٢,٦,٤

٤٢ Invert sugar solutions have less color stability than sucrose solutions of the same concentration when stored under the same conditions. This is due to chemically active reducing sugar in the invert sugar solution. The pH of the solution is highly important in lowering the rate of color formation. This In addition, the temperature of .٩.relationship is depicted in Fig the solution and the length of time it is heated markedly affects Illustrates the .١٠.the color development in invert syrups. Fig rate of color formation as a function of time. (Mynott, et .(١٩٧٥.al

Color development in sucrose solutions .٢,٦,٥ described the two factors that make up (١٩٧١) ,McGinnis the concept of color which may be optically determined in sucrose solutions. The first was the absorption of radiant energy in the presence of colorants. The second was the scattering of radiant energy due to any turbidity in the solution. Color development in sucrose solution is dependent upon several factors. Among these are the temperatures of the solution, time of storage, pH, presence of traces of reducing reported ,(١٩٥٣) ,sugars, and colored non – sugars. Gillett extensively on color development in sucrose syrups during and ٢٠ْc the rate of color development is extremely after refining. At slow but at higher temperatures, over a period of time, color Illustrates the results of .١١.begins to appear in the solution. Fig Brix sucrose ٦٦٫٥ْ gal) of ٨٠٠٠) liters ٣٠،٣٠٠ a study in which ٤٣ ٧٢ْc solution were held several days. The initial temperature of f) in the days. During this storage ٩٨٫٦ْ) ٣٧ْc ١٦٢ْf) decreased to) period the pH of the solution remained essentially constant. A lower rate of color development as the temperature became progressively lower was noticed. The factor of pH is apparently related to the presence of colorants which are pH sensitive, a common phenomenon of many naturally occurring organic substances. The presence of very low concentrations of reducing sugar, and possibly of traces of amino acids, can accelerate color development in sucrose solution.

٤٤ INVERT SYRUPS AT DIFFERENT ٪٩٠ VISCOSITY OF .٧.Fig CONCENTRATIONS (CORRECTED REFRACTIVE DRY

SOLIDS)

٤٥

EFFECT OF CONCENTRATION ON VISCOSITY FOR .٨.Fig VARYING .٢٠ْc PROPORTIONS OF INVERT SYRUPS AT

٤٦

٪٩٣ TYPICAL CURVE SHOWING COLOR DEVELOPMENT IN.٩.Fig INVERT SYRUP OF VARYING PH VALUES APPROACHING NEUTRALITY.

٤٧

٤٨

٤٩ TYPICAL CURVE SHOWING EFFECT OF PROLONGED.١٠.Fig HEATING ON COLOR DEVELOPMENT IN INVERT SYRUPS CONTAINING HIGH PERCENTAGE OF INVERT SUGARS.

٥٠ COLOR DEVELOPMENT IN SUCROSE LIQUID SUGAR AT.١١.Fig ELEVATED TEMPERATURES.

(١٩٧٠) From Gillett

SOME CHEMICAL PROPERTIES .٢٫٧

٥١ chemistry of inversion .٢٫٧٫١

Sucrose is α -D glucopyranosyl– β -D fructofuranoside. It

is a disaccharide with one molecule of α -D- glucose in the membered ring and is condensed with one-٦ pyranose or

member ring -٥ molecule of β -D- fructose in the furanose or form. It is quite stable both in the dry form and in solution but is subject to hydrolysis in acid solution or when acted upon by the

enzyme invertase. Upon hydrolysis α -D glucose (α -D-

glucopyranose) and β -D fructose ( β –D fructopyranose) are formed. This reaction is also termed inversion because of the net

α (١٩٦٦) Reed .(١٩٧٣ ,change in optical rotation( )D . (Hashkell states this change may be represented as follows:- Sucrose + water D (+) – glucose + D (-) – fructose

α α α ٩٢ْ - = D( ) ٥٢٫٥ْ + = D( ) ٦٦٫٥ْ+ = D()

α ٢٠ْ - = D( )

α -D- glucose is generally referred to as dextrose in its food

applications. β -D- fructose is also known as levulose but more commonly as fructose.

The inversion reaction may be empirically represented by the following equation:-

٥٢ ٥٢٫٦٣ ٥٢٫٦٣ ٥٫٢٦ ١٠٠

CHO12 22 11 + HO 2→ CHO 6 12 6 + CHO 6 12 6

Sucrose water dextrose fructose

Invert sugar

,in solids ٪٥ Thus there is a gain of approximately depending upon the degree of inversion, which is of economic importance to the food processor. This reaction is frequently used in food preparation in order to alter the properties of sucrose. For example, equal amounts of sucrose and dextrose – fructose in solution offer near maximum solubility of the sugar. This is especially important in those products of high sugar solids.

reported that there are three methods (١٩٧٣) Moroz et al that are used to produce invert syrups. The oldest procedure is probably the use of invertase which is still used to some extent. Acid inversion, using hydrochloric acid, is widely used in both batch and continuous systems. The third method is to use an ion-exchange resin. Acid inversion of sucrose .٢,٧,٢ The sucrose inverting capacity of acids will vary according to their degree of ionization or a dissociation

٥٣ has been prepared in which HCL has been ,١.constant, Table

.١٠٠ assigned an arbitrary value of Commercially, HCL is usually used because of its high inverting power. When the hydrolysis of sucrose is brought to the desired degree of inversion, the acid is neutralized with a suitable alkaline material such as sodium or calcium hydroxide.

.(١٩٦٥ ,Flavell) Large batches of invert are made in tanks which may be

٦٠ْ heated. The sucrose solution is prepared to a concentration of

٧٠ْc and acidified to a pH of a Brix. It is heated to about ٧٠ْ to

Adequate mixing of the acid is essential. It is held for .٢,٠ bout two to four hours, depending upon the desired extent of hydrolysis. At the end of the inversion, the solution is

and cooled in order to prevent color ٤,٥ neutralized to about pH

.(١٩٦٦ ,development. (Flavell

٥٤

.Inverting power of acids .١ Table

Acid Inverting power

١٠٠,٠ HCL

٥٣,٦ H٢SO٤

٦,٢١ H٣PO٤

٣,٠٠ Tartaric

١,٧٢ Citric

١,٠٧ Lactic

٥٥

Rate of Inversion .٢,٧,٣ The rate of inversion of sucrose by acidic catalysts has been extensively studied by many investigators. The information in the following paragraphs will provide some data on the influence of acid concentration, temperature, and time.

Effect of acid concentration .٢,٧,٣,١ The effect of acid concentration on the rate of inversion

For hydrochloric acid and in .١٢.of sucrose is shown in Fig

For tartaric acid. The percentage shown on each of the .١٣.Fig curves denotes acid content on sugar solids basis. A comparison of the curves between the two figures shows the greater hydrolyzing value of HCL as compared with tartaric acid.

.(١٩٢٤ ,Jackson and Silsbee)

Effect of temperature .٢,٧,٣,٢ The effect of temperature on the rate of inversion of

.١٤.sucrose is shown in Fig

٩٠ْc and ٨٠ْ Note: In commercial practice, temperature between

HCL are used. This provides for a rapid rate of ٪٠,٠٠٨٧٥ and

٥٦ hydrolysis but it is not too fast for proper control of the process.

.(١٩٤٧ ,Junk, et al)

Effect of time .٢,٧,٣,٣

٤٦ state, Tests showed that ,(١٩٧٣) Bonney and Thomas

invert syrup by partial ٪٥٠ hours were required to produce

.٣,٣min inversion of the sucrose syrup at room temperature and

٩٠ْc. The great difference in time needed to produce the At

and ١٢.required amount of inversion is also emphasized in Fig

.١٤

٥٧

TYPICAL CURVES SHOWING EFFECT OF ACID.١٢.Fig CONCENTRATION OF LIQUID SUGAR BY HYDROCHLORIC (٩٠ْc ACID (TEMP

٥٨

٥٩ TYPICAL CURVES SHOWING EFFECT OF ACID.١٣.Fig CONCENTRATION OF INVERSION OF LIQUID SUGAR BY .(١٠٠ْC TARTARIC ACID (TEMP

٦٠ TYPICAL CURVES SHOWING EFFECT OF TEMPERATURE.١٤.Fig

ON INVERSION OF LIQUID SUGAR BY HYDROCHLORIC ACID.

٦١ METHODS OF PREPARING SMALL VOLUMES OF .٢,٨ INVERT SYRUPS In some situations it may be desirable to prepare small batches of invert syrups in a food plant rather than obtaining them from outside sucrose. The following information should be helpful in such instances.

Rapid, small batch, using tartaric acid .٢,٨,١

٠,٣٥) gm ١٠ Ib) of granulated sugar and ٢٢,٠٥) Ten gm

gal) water and ١,١) ٤,٢١ oz) of tartaric acid are to be added to

١٠٠ْc. Temperature is maintained for heated, while stirring, to

min. In order to neutralize the added acid, with rapid ٣٠

oz) of sodium bicarbonate which has ٠,٤٠) gm ١١,٣٤ ,stirring been dissolved in small quantity of water are to be adedd. Use

١٠,٤٥ hot, or cool, as desired. The quantity produced should be

.solids ٪٧٤,١٥ gal) containing ٢,٧٦) liters In this procedure, and the one that follows, the sucrose

(١٩٧٤ ,complete. (Eitenmiller, et al ٪٩٠ inversion is about

Slow, Large batch, using tartaric acid .٢,٨,٢ When preparing larger batches of invert syrup the following procedure may be used by multiplying the specified

٦٢ quantities of ingredients by the number of hundred weight of sugar that is used.

٢٢٠,٥١b) of granulated sugar were) Hundred kg

١٠٠ْc with constant gal) water. Heat to ١١,٠)٤١,٦١ dissolved in

oz) of tartaric acid ٣,٥٣) gm ١٠٠ stirring and thoroughly mix dissolved in a small quantity of water. Turn off heat and allow

١٠٠ْf) in an insulated container or in a) ٣٨ْc to cool gradually to location essentially free of cooling air circulation. The desired

hours. Slowly ١٦ inversion and cooling is usually obtained with

oz) of sodium ٣,٩٧) gm ١١٢,٥ mix in with constant stirring bicarbonate which has been dissolved in a small quantity of

١٠٣,٣١ water. The quantity of invert syrup produced is about

,solids, (Van der linden ٪٧٤,١٥ gal) containing ٢٧,٣)

.(١٩٧٩

Large batches, using hydrochloric acid .٢,٨,٣

liters ٢٠٠ reported that, to invert (١٩٧٣) ,Ramanaushkas

floz) USP ٣,٩) ml ١١٥ Brix syrup, add ٦٦,٥ْ gal) of ٥٢,٨)

Heat to .٪٣٧ HCL approximately ١,١٩ hydrochloric acid, sp gr

hours. Cool and ١,٥ ١٥٨ْf) and hold at this temperature for) ٧٠ْc

٦٣ oz) of sodium bicarbonate which has ٣,٩) gm ١١١ slowly mix in been dissolved in a small quantity of water with constant

gal) of invert ٥٢,٢) liters ١٩٧,٦ stirring. This method produces

.solid ٪٦٩,٨ syrup containing about

inverts syrup using tartaric acid ٪٥٠ Preparation of .٢,٨,٤

lb) of granulated sugar were ٢٢٠,٥) Hundred kg

١٠٠ْc with constant gal) water. Heat to ٨,٨) ٣٣,٣١ dissolved in

١٠٠ stirring and, while maintaining temperature, thoroughly mix

oz) of tartaric acid dissolved in a small quantity of ٣,٥٣) gm water. Turn off the heat and allow the solution to cool gradually

f) in an insulated container or in a location ١٠٠ْ) ٣٨ْc to essentially free of cooling air circulation. The desired inversion

hours. Slowly add, with constant ١٦ is usually obtained in

oz) of sodium bicarbonate dissolved in ٣,٩٧) ١١٢,٥gm ,stirring

(lb ٢٢٠,٥) kg ١٠٠ a small quantity of water. Finally, add

gal) of hot water, and stir until ٩,٩) ٣٧,٥١ ,granulated sugar completely dissolved.

٥٢,٣) liters ١٩٨,٠ This procedure makes approximately

solids. (Chen and ٪٧٥,٤ invert syrup containing ٪٥٠ gal) of ٦٤ states, in the event either density (١٩٦٣) ,Meade .(١٩٧٧ ,Meade

gal) of hot water instead ٨,٨) liters ٣٣,٣ of syrup is desired use

gal) in the last step. This will make ٩,٩) liter ٣٧,٥ of

gal) of invert syrup containing ٥١,٢) liters ١٩٣,٨ approximately

solids. However, since this solution is approximately ٪٧٦,٧

١٠٠ْf), the dissolving of the granulated sugar in) ٣٨ْc saturated at the last step may be time consuming. An additional amount of water may be necessary to compensate for possible loss of water by evaporation during inversion. This would also apply to evaporation losses in preparing the other solution.

METHODS FOR THE CLARIFICATION OF THE SYRUP .٢,٩

Turbidity of the syrup .٢,٩,١ The syrup as it leaves the evaporator assumes again some turbidity due to suspended or floating particles which were soluble in thin juice and insoluble in syrup, and dark coloration as a consequence of the over heating and caramelization of some of its constituents at the higher temperature. Most of the impurities deposit on the heating tubes of the evaporator, but a good part remains in the syrup, making it turbid. This syrup is ٦٥ unfit to be worked up for white sugar manufacture. Therefore, the first requirement for a syrup intended to yield white sugar is that it should be clear and free from suspended particles which might form a nucleus for the crystals or might crystallize with

.(١٩٥٢ ,the sugar giving it a dark tinge. (Deitz, et al

Sulphitation of the syrup .٢,٩,٢ In the normal practice, the sulphitation and carbonation syrups are bleached by the action of sulphur dioxide, and no efforts are made to remove the floating particles. The sulphur dioxide reduces the ferric salts in the syrup to ferrous salts; which are colorless and do not crystallize together with the sugar in an acid syrup. The syrup sulphitation is done in modern practice in a continuous manner either in quarez installation or

The .٥,٦-٥,٤ in sulphitation vessels to a distinct acidity of pH sulphited syrup is then pumped to storage tank, from where it is used to boil massecuite. It has been observed that during storage a part of the suspended particles settle down but much remain in the syrup which is decanted off. The impurities settled at the bottom must be removed at regular intervals and the tanks

.(١٩٦٥ ,thoroughly cleaned and washed. (Carruthers, et al

Clarification of the syrup .٢,٩,٣ To deprive of its floating particles as in the case of defecated syrup to manufacture white sugar, different methods

٦٦ are used in practice. One important method is that the syrup be

Beaume and ١٥ْ milk of lime at ٪٢,٥ to ٢ treated with neutralized with sulphur dioxide and heated to the boiling point. The copious precipitate formed is filtered through cloth in filter presses or over animal charcoal. The clear filtrate is then cooled and boiled to ٥٫٨-٥٫٤ ٦٠ْc and sulphited to pH to about massecuite. The dose of lime should be sufficient as otherwise the same dose not filter well. While sulphuring the syrup it is prudent to keep the temperature of the sulphited syrup low, near ٦٠ْc, as absorption of gas improve at a lower-٥٥ about temperature. The cooling may be done by heat exchangers, through which cold water flows and carries off the surplus heat. Practical: The degree of sulphuring is regulated by the operator in the following ways: (a) By visual appearance of the sulphited syrup which should appear like honey colour. (b) By comparing with prepared sample test tube at definite pH and density. The sample tube should be prepared in the laboratory and be changed every alternate day. (c) By Hellige’s comparator using C.P.R. indicator. Precautions The temperature of the acid syrup should never goes above .١ ;٦٠ْc-٥٠ ٣٧ْc: preferably, it should be maintained between

٦٧ so that there may be very little risk of “inversion” losses, and the absorption of the gas improves. To determine daily the glucose ratio of the unsulphited .٢ syrup and the first massecuite, provided there has not been any return of molasses between these two stages. If the glucose ratio is found to have risen, this indicates that the syrup has been too acidic and steps should be taken to remedy this possible error. The syrup storage tanks in which the impurities have .٣ settled down should be cleaned and washed regularly which would otherwise foul the heating tubes of the .(١٩٧١,pan.(Arabie and Moskowitz

The removal of suspended impurities by syrup clarification .٢,٩,٤ The impurities that increase syrup viscosity and hinder subsequent massecuite curing are the high molecular weight polysaccharides and the wide range of insoluble impurities which account for the turbidity of the syrup. Removal of some of these materials was considered possible using a phosphate defection process and initial results obtained using different reagents showed some promise, as can be seen in the results in .٢ table Removal of the calcium phosphate precipitate was difficult, as had been experienced by other workers attempting The problem was finally .(١٩٧٢ ,syrup clarification (Saranin

٦٨ resolved using a new flotation /clarification technique in .(١٩٧٥ ,association with a specific flocculent (Bennett The next step was to perfect continue operation of such a treatment on a plant scale. Using an old Jacobs’s clarifier, the feasibility of continuous operation was confirmed in a Venezuelan factory, but unfortunately, many new problems were identified. Considerable further work was therefore carried out on the plant layout and clarifier design. A second attempt in South Africa with the new layout and purpose-designed clarifier produced more consistent results. resulted in an ١٩٧٥ and ١٩٧٤ Further improvements in .٣.installation that gave consistently good clarification. Table shows the average removal of some of important impurities present in raw syrup. The flocculation / flotation technique and clarifier design are now the subject of granted patents (International society. J, and the process has been named the “TALODURA ,(١٩٧٧ Process”. The process involves the addition of lime and phosphoric acid, or sodium phosphate, in a reaction- aeration vessel. TALODURA flocculent is then added, and clarification takes place in a circular clarifier which incorporates a special retention flocculation chamber. The entire process is completed .min ٢٠ in

٦٩ As expected, the raw sugar boiled from clarified syrup showed a substantial improvement in quality. This shown in .٤.table

Colour and Turbidity Removal with Various .٢.Table Phosphatation Treatments on Raw Syrup

Sample treatment Turbidity Removal of Colour Removal of (%) ٥٦٠nm colour@) nm Turbidity ٩٠٠@) in mau.. ) (%) in After

٧٠ µm ٠٫٤٥ filtration

- ٢٫٧٦٠ - ١٫٠٧٠ Untreated

١١ ٢٫٤٥٠ ٨٠ ٢١٠ sodium phosphate +

ppm po2 5 ٣٠٠ ≡

١٥ ٢٫٣٥٠ ٨٧ ١٤٠ Phosphoric acid+

٣٠٠ppm p2o5 ≡ +NaOH to neutral

١٥ ٢٫٣٥٠ ٩٢ ٩٠ phosphoric acid +

٣٠٠ppm p2o5 ≡

+ ca() OH 2 to neutral

Average Reduction of some Impurities in Raw Syrup .٣.Table with continuous Clarification

Impurity Removal From Syrup Average Quantity Removed (% During Clarification of that Originally Present)

٧١

٦٣٫٥ nm ٤٢٠ Turbidity (mau.. At (µm filtration ٠٫٤٥

١١٫٥ nm ٤٢٠ Colour (mau.. At (µm filtration ٠٫٤٥

١٠٫٢ Starch

١٤٫٩ Gum

was obtained ٪٠٫٣٨ NOTE: An average increase in syrup purity of across the clarification process.

Average Reduction in some Impurities of Raw sugar .٤.Table with Continuous Clarification of Raw Sugar

٧٢

Raw sugar Analysis Change Due to syrup clarification (%)

٠٫١٧ Pol Increased

٣٢٫٣ nm Decreased ٤٢٠ Turbidity (mau.. at (µm filtration ٠٫٤٥

٢٧٫٥ ٤٢٠nm Decreased Colour(mau.. at (µm filtration ٠٫٤٥

٣٦٫٠ Ash (sulphated) Decreased

٢٢٫٠ Filterability Increased

However, the largest improvement in sugar quality occurs when mill white sugar clarified syrup prepared using juice sulphitation. reported that it is expected that the (١٩٧٦ ),Smith increasing interest in the production of both plantation white

٧٣ sugar and raw sugar of high quality will focus attention on raw syrup quality in the factory. Having identified undesirable impurities of raw syrup, steps can be taken in the factory to reduce the levels of these impurities in the pan feed syrup. In the case of process generated colorants, preventative measures such as inhibition of colour formation by juice sulphitation are likely to prove increasingly attractive. Levels of other impurities such as insoluble gums which, although present in relatively small quantities, affect sugar quality significantly and factory recovery can be reduced at reasonable cost by clarification of the raw syrup. The removal of such impurities has proved attractive to factories producing plantation white sugar. Improvements in recovery indicated from the viscosity reducing effect of syrup clarification is also likely to generate interest in the industry. Raw syrup impurities, such as insoluble matter, gums and process-generated colorants, have a detrimental effect on factory sugar quality and boiling house recovery. Anew process involving the clarification of raw syrup to remove some of these impurities is described together with the process improvements achieved from full scale operation. These improvements are most marked when a mill-white sugar is .(١٩٦٢ ,being made. (Anon

CANE SYRUP STORAGE .٢,١٠ ٧٤ Syrup has been kept in storage in appreciable volumes for ٨ months and experimentally in small volumes up to ٣ up to .weeks ٦ to ٤ months. In general syrup keeps well for about After that time some foaming may be observed and a drop in pH This .٤٫٠ which is the pH of fresh syrup, to around ,٦٫٥ from takes place in a few days. Then foaming disappears and a slow inversion of sucrose occurs as a result of the low pH. The rate of per week at an average ٪٠٫٥ sucrose loss is approximately ٢٧ْc. During the short period of foaming ambient temperature of days) a drop in the content of reducing sugars has been ٧ to ٥) determined. Afterwards the content of total sugars remains constant. Looking at diluted samples of syrup under a microscope during the foaming period, the presence of some type of osmophylic yeast that grows in the form of chains has been detected. All this leads us to speculate that the cause of foaming, with loss of reducing sugars and a drop in pH, are result of the activity of this micro-organism that probably converts sugar into acids and that ceases to multiply at the lower pH where inversion of sucrose occurs. The possibility that the destruction of reducing sugars and foaming of the syrup, which is due to carbon dioxide formation, are caused by a purely chemical reaction, such as Maillard reaction, has also been .(١٩٧١ ,considered.( McGinnis Another important feature of stored syrup is the formation of sludge in the bottom of the tanks. This sludge consists of the

٧٥ suspended matter present in the original syrup and very fine crystals of calcium sulphate that slowly precipitate during the period of storage. The best way to deal with sludge when the processing mill is still grinding cane is to mix it with the limed juice going to clarification. If cane crushing has stopped the sludge must be processed with the rest of the syrup at a reduced .(١٩٧٣ ,rate of operation. (McGinnis

Preservation of the syrup during shut-down .٢,١٠,١ Some times, it becomes necessary to store syrup for several hours or even days; this is possible with the use of some ٦٠ْc) preservatives. Ordinarily, if the Brix of the syrup is high then syrup can be kept ,٦٫٨ and ٦٫٠ Brix) and the pH between hours or even more ٣٦ under tropical conditions for a bout without any preservative. But when the syrup is highly acidic brix) it should be evaporated to higher ٥٥ْ-٥٠) and the Brix low brix). Alternatively, during shut-down the use ٨٠ْ-٧٠) densities of preservatives, such as formaldehyde is generally recommended. Beaume syrup during a ٣٠ْ preserved ,(١٩٤٥) Spencer per cent ٤٠ ml of ٦ period of seven days by the addition of .(١:٥٠٠٠) formaldehyde solution per cubic food Precautions The temperature of the syrup should be lowered down as .١ much as possible.

٧٦ The syrup need not be sulphured at all or is slightly sulphured .٢ .(٦٫٨-٦٫٥ pH) .Profuse use of preservatives .٣ -٦٠) The concentration of the syrup be increased to high brix .٤ .(brix ٧٠ْ Cleanliness of the storage tanks is necessary at regular .٥ intervals of time to check growth of micro-organisms.

٧٧

CHAPTER THREE MATERIALS AND METHODS

٧٨ Materials .٣٫١ Samples of cane syrup were collected during the seasons at Kenana sugar factory, Saeed food factory and ٢٠٠٥/٢٠٠٤ AL-Modhesh food factory. Methods of Analysis .٣٫٢ Laboratory analyses according to ICUMSA were carried out to determine chemical and physical characteristics. The analysis included:- a. Total Soluble Solids (Brix) using table Refractometer. b. Moisture Content. c. PH determination. d. Refractive Index. e. Acidity as “citric acid”. f. Gravity Purity. g. Total Sugars. h. Reducing Sugars. i. Sucrose. j. Ash content. k. Minerals. l. Nitrogen content. m. Viscosity. n. Colour. (Total Soluble Solids (T.S.S) (BRIX .٣٫٢٫١ The Brix was determined according to the method of the International Commission of Uniform) (١٩٩٤) ICUMSA

٧٩ Methods for Sugar Analysis) using refractometer ranged A portion of sample was placed in the .٩٠-٤٠ between refractometer. The reading was recorded as Brix directly. Moisture Content ٣٫٢٫٢ Moisture Content was determined according to the .(١٩٧٤) method of ICUMSA ٣٠ An empty dish with lid opened was heated for ١٠٥ْc. Then removed from the oven, the minutes in an oven at lid was replaced and placed in a desicator at room temperature

then weighed ()M 1 Twenty grams of the sample were placed in the dish and

weighed with the lid on it()M 2 . Then returned to the oven, with the opened state for exactly three hours. The lid was replaced and removed to the desicator and weighed at room

temperature ()M 3 . Calculation 100(M −M ) Moisture percent = 21 MM23−

Where

M 1 = Mass of dish (g).

M 2 = Mass of dish + sample before drying (g).

M 3 = Mass of dish + sample after drying (g). Determination of pH Value .٣٫٢٫٣

٨٠ was used. It was standardized with ٣٣٨ A pH- meter type ,٢٠ْc at ٤٫٠٠ a buffer solution, potassium hydrogen oxalate pH at ٩٫٠٠ and disodium tetraborate pH ٧٫٠٠ distilled water pH .١٠٠g distilled water was used/٥٠g ٢٠ْc. A sample solution of .degree ٠٫٠١ The result was expressed as pH to the nearest Refractive Index .٣٫٢٫٤ Using table refractometer HILGER. M 46.315 . A portion 56304 of sample was placed in table refractometer. The reading was recorded as refractive index directly. Acidity .٣٫٢٫٥ Two grams of sodium hydroxide pellets (NaOH) were N ٠٫١ ٥٠٠ml distilled water for preparation of dissolved in NaOH solution. Ten grams of sample were weighed in beaker ١٠ml of sample after .١٠٠ml distilled water and diluted by drops of ٣ ,١٠٠ml volumetric flask dilution was taken in phenolphthalein indicator were added and the titration was followed till the pink colour appeared. Calculation Acidity as “Citric acid” was Calculated from the formula:-

Titration ×0.07× 10×100 Weight of Sample

Where .citric acid factor = ٠٫٠٧

٨١ .(sample volume (ml = ١٠ Gravity Purity .٣٫٢٫٦ Gravity purity was calculated from the formula:- Sucrose ×100 Brix Total Sugars .٣٫٢٫٧ Total sugars were determined by the Lane and Eynon .(١٩٧٠ ;method (ICUMSA ١٫٥gram of sample were Empty beaker was weighed and gram potassium oxalate ٠٫٥ gram lead acetate and ٠٫٥ .put in it ml by ٢٥٠ were added, and then the volume was completed to distilled water. The sample was transferred to the burette. gram ٥ gram of Fehling’s solution (A) and ٥ ,In a beaker drops of Methylene ٣ .of Fehling’s solution (B) were weighed ml of the burette were added, then ١٥ .blue indicator were added ٧ْc) and the colour was) the beaker was put in water bath ml of Fehling’s ١٢٫٥ .noticed. The colour was changed to red drops of Methylene blue and ٣ .solutions (A) and (B) were used minutes and more ٣ ١٥ml of sample were added, then heated for of sample was added till the red colour appeared. Calculation The total sugar was calculated from the formula:-

250×mg of reducing sugar × 100 weight of sample ×100 stock solution = ٢٥٠

٨٢ Mg reducing sugars obtained from standard table (ICUMSA, .according to the volume of titration (١٩٧٠ Reducing Sugars .٣٫٢٫٨ ٥٠ml of sample was taken from stock solution which was ٦٫٥ml of .prepared to total sugar and put in conical flask concentrated hydrochloric acid were added, and then transferred ٥ miniutes; the sample was cooled for ٥ ٧٢ْc for to water bath till ٪٤٠ minutes. Neutralized with drops of sodium hydroxide the colour was changed to pink; the volume was completed to .١٠٠ml with distilled water (grams of Fehlling’s solution (A) and (B ٥ ,In the beaker .drops of Methylene blue indicator were added ٣ .were weighed ١٥ml of the sample in the burette were added, then the beaker ٧ْc) and the colour was noticed, when the) was put in water bath ١٢٫٥ml of Fehling’s solution (A) and ,colour was changed to red drops of Methylene blue ٣ .B) were added in another beaker) minutes and ٣ ١٥ml of sample were added, then heated for and more of sample was added till the red colour appeared. Calculation The reducing sugar calculated from the formula:-

250×mg T × 100 weight of sample ×100 Where (١٩٧٠ ,Mg T = obtained from standard table (ICUMSA according to the volume of titration. .stock solution = ٢٥٠ ٨٣ Sucrose .٣٫٢٫٩ After total invert sugars and reducing sugars were determined, the sucrose was calculated from the formula:- Sucrose = Total invert sugars – Reducing sugars Ash content .٣٫٢٫١٠ Carbonated ash .٣٫٢٫١٠٫١ Reagents ١٠gm :Ammonium nitrate solution containing ammonia ١٠ml of ammonium ammonium nitrate were dissolved in ١٠٠ml with distilled ١٠٠ml) and made up to/ ٢٥g) hydroxide ١٠gm of ammonium :water. Ammonium carbonate solution .١٠٠ml carbonate were dissolved in water and made up to Procedure .١٠٠ml Five grams of sample were heated carefully in a ٦٠٠ْc until the mass carbonized. It Platinum dish in a furnace at was left to cool down, and just moistened with hot water. Then ground in a mortar. The mass was then filtered through ash less filter paper. The residue plus filter paper were returned to the platinum dish, dried, carbonized, evaporated to dryness and .٤٥٠ْc incinerated in furnace at The ash was moistened with ammonia containing nitrate solution, dried on a water-bath and heated again in muffle ٤٥٠ْc. The residue was then moistened with furnace at ammonia carbonate solution. After drying on water-bath, it

٨٤ ٤٥٠ْc.The last step was repeated twice, till a was heated at constant weight was attained. The remainder was weighed and expressed as percentage carbonated ash. Calculation 100× (ww − ) Carbonated = 31 ww21− Where

w 1 = weight of empty dish.

w 2 = weight of dish + the sample before ashing

w 3 = weight of the dish + ash. Sulphated ash .٣٫٢٫١٠٫٢ Reagents g/cm 3 ١٫٨٤ Concentrated sulphuric acid g/cm 3 ١٫١٨ Concentrated hydrochloric acid Procedure A dish was cleaned with boiling hydrochloric acid solution. It was rinsed thoroughly with water, and then heated in mg after it ٠٫٢ ± ٥٥٠ْc; the dish was weighed to the furnace at was left to cool down. Ten grams of sample were weighed in platinum. Two ml of sulphuric acid were added, and then the dish was heated in a Bunzen burner until the mass carbonized. The dish with hours. It ٢ ٥٥٠ْc for carbonized mass was heated in furnace at .٢ml of sulphuric acid were added again was left to cool and

٨٥ ,mg (ICUMSA ٠٫٢ ± The dish was evaporated and weighed to .(١٩٩٤ Calculation M − M 0 ١oo × 2 = % Sulphated ash M 1 − M 0 Where M 0 = weight of empty dish.

M 1 = weight of dish + sample before ashing.

M 2 = weight of dish + ash. Minerals determination .٣٫٢٫١١ The minerals were determined by the method of (Perkin- .Using (A.A.S) (Atomic Absorption spectrometer .(١٩٩٤ ,Elmer (.٣١١٠ :Model Procedure grams of the sample were taken in crucible, then ٢ ٣-٢ ,٦٠٠ْc-٥٥٠ sample was ashed to white colour in the furnace drops of concentrated hydrochloric acid were added to the sample which was ashed. The crucible was transferred with ١٠٠ml volumetric flask with funnel. The some distilled water to crucible washed to avoid losses. The volume was completed to ١٠٠ml. Then the solution was filtered by ash less filter paper to separate the silica. The paper was ashed in weighed ٦٠٠ْc.The silica weight was founded. The clear-٥٥٠ْc crucible at solution (filtered) was kept in clean container and was

٨٦ transferred to atomic absorption spectrometer. The readings were recorded as value of mineral directly. Nitrogen content .٣٫٢٫١٢ The nitrogen content was determined by micro – kjeldahl In semi-micro .(١٩٦٤) method as described by Whalley gram of the sample, one gram of a catalyst ٠٫٢ ,digestion flask ml of sulphuric acid ٣٫٥ potassium sulphate + cupric acid) and) were mixed together. The mixture was digested for two hours. The solution was NaOH ٪٤٠ then transferred to the distillation unit. Ten ml of solution were added to the solution, the mixture was heated and boric ٪٢ ml ١٠ ,the nitrogen was collected in flask containing acid and few drops of mixed indicator Methyl red, the solution ٠٫٠٢N. The following formula was then titrated against HCL .(١٠٠/was used to determine nitrogen percentage (g ١٠٠ ×١٤ × Nitrogen% = V× N ١٠٠٠ × W Where .٠٫٠٢N) used for titration) V = volume of hydrochloric acid .(٠٫٠٢N) N = normality of Hcl W = weight of original sample (g). The nitrogen percentage was then multiplied by the factor .to determine the percentage of protein in the sample ٦٫٢٥ Viscosity .٣٫٢٫١٣

٨٧ The viscosity is generally given in centipoises (cps) or centistock (cm2 / s ), or as a relative viscosity. The kinematic Bx), was determined according ٥٠ْ) viscosity of diluted syrup using a U–shaped viscometer and (١٩٨٤) to the AOAC method .٣٠ْc using a water- bath measured at Calculation = (kinematic viscosity (centistock .١ ١٫٠٠٣٨ ×٣٠ْc Flow time of sample at ٣٠ْc Flow time of water at Where cْ ٢٠ viscosity of water at = ١٫٠٠٣٨

− Relative viscosity = TTo .٢ To Where T = flow time of the sample. To = flow time of distilled water at the same temperature. Colour .٣٫٢٫١٤ Colour measurement was done according to ICUMSA using automatic digital sucroscan ٩-٣/Method No.Gs٢ ,(١٩٩٤) MAARC LABS.PVT.LTD), capable of light) ٠٦٠٥/٣١٢٢ .٤٢٠nm transmission measurements at wavelength of The absorbency of the samples was measured after the membrane filteration (using kieselguhr (acid washed) and at .(٧٫٠ neutral pH of ٧gm of brix was prepared by dissolving ٥ْ.The solution ca . ١٠٠cm 3 syrup in water to a total volume of ٨٨ ٤gm ,The filter pad was prepared in the Buchner flask cm 3 of the prepared ٥٠.kieselguhrs were used, and the ca sample was filtered under vaccum and the first cloudy runnings were discarded. The filtrate was collected in a clean dry flask, ١٠٠cm 3 beaker and covered with a watch and transferred to .٠٫٢ ±٧٫٠ glass. Using hydrochloric acid, the pH was adjusted to The refractometer brix was measured and the measured temperature was recorded. The optical density was measured in .nm against water as reference ٤٢٠ mm cell at ٥ Calculation oD × 10 Attenuation Index ()α ∗ c = 420 bc Where OD = an absorbance. B = cell length in mm. C = concentration of solids in g percm 3 .

٨٩

٩٠ CHAPTER FOUR RESULTS AND DISCUSSION

Total soluble solids and sugars content .٤٫١ shows results of T.S.S and sugars content of (٥) Table Tate and Lyle syrup as reference and syrup samples which are produced by local factories. The Total soluble solids were the highest in amber syrup which is produced by Kenana Sugar Company, where it was produced by taking silver cane sugar liquor or A, B run-off silver, inverted and concentrated to form syrup. But the T.S.S was the lowest in Al-Modhesh golden syrup, where it is produced by dissolving the white sugar, inverted and concentrated to form syrup. Other types of syrup which are treacle from Kenana Sugar Company and golden syrup from Saeed food factory were found to be similar with the reference (Tate and Lyle). Comparable results for total soluble who reported that (١٩٧٠)solids were demonstrated by Person for golden syrup and treacle while the ٪٨٣ total soluble solids is Sudanese Standards and Metrology Organization (SSMO), stated that, the total soluble solids for golden syrup is between (١٩٨٢) ICUMSA .٨٢-٨٠ while for treacle between ,٨٤-٨٢ for golden syrup ٨٣٫٥-٨٢٫٥ reported that total soluble solids are stated that, T.S.S of (١٩٧١) for treacle. Oliver ٨٢٫٥-٨١ and The golden syrup of Al-Modhesh .٪٨٣ golden syrup is about food factory was the lowest, if compared with the standard and

٩١ reference, that applies the type of concentration of syrup, which is carried out by open Kettles, which lead to incomplete concentration. Total sugars were the highest in Al-Modhesh syrup sample comparing with the reference (Tate and Lyle), Kenana syrups samples and Saeed syrup samples matched the reference, in which the raw sugar is used in syrup manufacturing. Person ,٪٨٣-٧٩ reported that total sugars of golden syrup lie ,(١٩٧٠) The total .٪٨٠-٧٢ while the treacle found in the range between ,(١٩٨٢) ICUMSA ٪٨٢-٧٧ sugars of golden syrup were between ,SSMO), reported that) .٪٨١-٧٥ while the treacle was between while the ,٪٧٨-٧٤ total sugars of golden syrup was between Samples total sugars values for .٪٧٨-٧٣ treacle was between local factories were almost identical with reference and ICUMSA standards, but differ with (SSMO). Reducing sugars scored the highest value for Kenana syrup samples, compared to reference (Tate and Lyle), and were found to be the lowest for Saeed and AL-Modhesh, in which the rate of inversion depends completely on time and temperature, where, in AL-Modhesh factory the inversion was practiced on reported that, in commercial (١٩٤٧ ,٧٥ْc. (Junk, et al-٧٠ ٩٠ْc. In-٨٠ practice, temperature of inversion must be between hours are used for inversion. Bonney and ٤٠ Saeed food factory stated that, tests (١٩٧٣) Thom’s

٩٢

Total soluble solids and sugar contents of syrups .٥.Table

ANALYSIS Tate and Kenana Kenana Saeed AL- Lyle (amber) (treacle) Modhesh ٧٩ ٨١ ٨١ ٨٢ ٨١ % Brix

٨٢٫٦ ٨٠٫٦ ٨١ ٨٠٫٨٣ ٨٠٫١٣ Total sugars % ٤٥٫٥٥ ٤٦٫٣٨ ٤٧٫٣٥ ٤٨٫٣٥ ٤٨٫٣٣ Reducing sugars % ٣٧٫٠٥ ٣٤٫٢٢ ٣٣٫٦٥ ٣٢٫٤٨ ٣١٫٨ % Sucrose

٩٣ invert syrup ٪٥٠ hours were required to produce ٤٦ showed that by partial inversion of the sucrose. Comparable results for who (١٩٧٠) reducing sugars were demonstrated by Person -٤٧ reported that reducing sugars of golden syrup were between (١٩٨٢) ICUMSA .٪٥٠-٣٧ and that of treacle were between ,٪٥٠ -٤٨ stated that, reducing sugars of golden syrup were between Sudanese .٪٤٨-٣٥ and that of treacle were between ٪٥٠ Standards and Metrology Organization (SSMO), reported that and ,٪٦٠-٥٨ the reducing sugars of golden syrup were between Results of reducing sugars .٪٥٨-٥٥ that of treacle were between but ,(١٩٨٢) were in agreement with that reported by ICUMSA differ with (SSMO) which reported high degree for reducing sugars. The sucrose % was the highest in Saeed and AL- Modhesh syrup samples, and the lowest in the reference sample (Tate and Lyle). Kenana amber and treacle were within the standards range. The increase of sucrose % degree in Saeed and AL-Modhesh samples were attributed to the rate of inversion and utilization of during raw sugar syrup manufacturing, as well glucose was used in the syrup ٪٢٠ ,as, in AL-Modhesh factory formula, that add more of total sugars for this sample. Comparable results for sucrose were demonstrated by Person who reported that sucrose in golden syrup was between (١٩٧٠) (١٩٨٢) ICUMSA .٪٣٣-٢٣ and treacle was between ,٪٣٣-٣١ ,in golden syrup ٪٣٣-٣٢ stated that, the sucrose percent must be

٩٤ in the treacle. Sudanese Standards and Metrology ٪٣٤-٢٣ and sucrose in ٪١٨-١٦ Organization (SSMO), reported that about sucrose in the treacle. Ruslts of ٪٢٠-١٨ golden syrup, and sucrose shown were identical with most of references, but differ greatly with results obtained by (SSMO). Refractive index, pH, Acidity and Moisture .٤٫٢ shows results of Refractive index, pH, acidity (٦) Table and moisture % of Tate and Lyle reference sample and syrups of local factories. Refractive index was the highest for Saeed syrup sample which complied with the reference; AL-Modhesh syrup sample scored the lowest value, which has high percentage of total sugars than other samples. Kenana amber and treacle reported, that the ,(١٩٧١) samples showed similar results. Oliver .٢٠ْc at ١٫٤٩٧٠ refractive index of golden syrup is The pH of Kenana treacle syrup was the highest sample, where it was the lowest in AL-Modhesh syrup sample, Kenana amber and Saeed syrup samples matched with the reference (Tate and Lyle). Sudanese Standards and Metrology Organization (SSMO), reported, that pH of golden syrup is The .٦٫٥-٥٫٨ and for treacle lies between ,٥٫٨-٥٫٦ between golden syrup samples were almost identical with the reference, except AL-Modhesh syrup sample, while the treacle sample was found in the range of Sudanese Standards and Metrology ,(١٩٧٥) ,Organization in inversion percentage. Mynott, et al stated, that the pH of the invert

٩٥

Refractive index, pH, acidity and moisture of syrups .٦.Table

ANALYSIS Tate and Kenana Kenana Saeed AL- Lyle (amber) (treacle) Modhesh ١٫٤٩٣٠ ١٫٥٠٠٠ ١٫٤٩٩٠ ١٫٤٩٦٠ ١٫٥٠٠٠ Refractive index ٤٫٧ ٥٫٥ ٥٫٩ ٥٫٥ ٥٫٥ pH

٢٫٨ ٢٫١ ١٫٤ ١٫٤ ١٫٤ % Acidity

٢١ ١٩ ١٩ ١٨ ١٩ % Moisture

٩٦ sugar solution is highly important in lowering the rate of color formation, and the parameter of pH is apparently related to the presence of colorants which are pH sensitive. The acid which is used in practicing inversion makes varying pH values to be used as an indicator for inversion. Acidity was the highest in AL-Modhesh and Saeed syrup samples respectively, while the Kenana syrup samples (amber and treacle) were confirmed well with the reference (Tate and Lyle). The variations in results are due to amount of acid used for inversion, and alkali which is used for neutralization of acid. In Kenana factory, the quantities of HCL acid and caustic soda ١٫١kg / Ton syrup respectively by quality ,٢٫٧kg are calculated control department, while in AL-Modhesh and Saeed factories -١٠٠kg syrup. In AL ٨٠ml HCL for every ,٩٠ml they use Modhesh factory a preservative material was added which increase the acidity ratio. Moisture % was the highest in AL-Modhesh syrup sample, and was the lowest in Kenana amber syrup. Kenana treacle and Saeed syrup samples matched with the reference Tate and Lyle sample. In AL-Modhesh factory, the concentration operation of syrup occurs in an open kettle, which leads to lower concentration of solution, so that the moisture percent was the highest in AL-Modhesh sample than all other samples. The Kenana syrup is prepared by a suitable procedure for concentration. The moisture content has a significant effect

٩٧ on shelf life of the syrup, because, the moisture controls the microorganisms growth. Gravity purity, colour, nitrogen content and protein .٤٫٣ shows results of actual purity, color, nitrogen (٧) Table content and protein of Tate and Lyle syrup as reference and all other samples which are produced by local factories. Gravity purity was the highest in AL-Modhesh syrup sample, and the lowest for the Kenana amber syrup, which lied within the range of reference Tate and Lyle sample. The increase of gravity purity was due to high percentage of sucrose; while the decrease of gravity purity was due to crystallization of sucrose. Gravity purity may be used in inversion evaluation. When in practice complete inversion of sucrose to monosaccharide occurred, sucrose properities will change to uncrystallized sucrose which plays an important role in purity and quality of syrup. Kenana treacle syrup got the highest color value, while AL-Modhesh syrup scored the lowest one. Kenana amber and ٢١٢-٤٠٠ Saeed syrups were higher than the reference sample by units. Comparable results for colour were demonstrated by which reported that; colour of golden syrup (١٩٨٢) ICUMSA ICUMSA units. Sudanese Standards ٢٥٠٠-٢٠٠٠ was between and Metrology Organization (SSMO) stated that, colour of while the treacle was between ,٢٠٠٠ golden syrup was about .ICUMSA units ١٠٠٠٠-٦٠٠٠

٩٨

Gravity purity, colour, nitrogen content, and protein of .٧.Table syrups

ANALYSIS Tate and Kenana Kenana Saeed AL- Lyle (amber) (treacle) Modhesh ٤٦٫٨٩ ٤٢٫٢٢ ٤٢٫٠٦ ٣٩٫٦٠ ٣٩٫٢٥ Gravity purity % ١٨٩٣ ٢٢١٢ ٩١٧٩ ٢٤٠٠ ٢٠٠٠ Colour ICUMSA ٠٫٠٩٨ ٠٫١٧٢ ٠٫١٦٥ ٠٫١٦٥ ٠٫١٧٦ Nitrogen content % ٠٫٦١٢ ١٫٠٧٥ ١٫٠٣١ ١٫٠٣١ ١٫١ % Protein

٩٩ Kenana treacle color conformed with (SSMO), while Kenana amber and Saeed syrups were higher than that of (SSMO) by units; however, the colour depends upon colour of raw ٢١٢-٤٠٠ material which has been used in the syrup manufacture. Mynott, reported that, invert sugar solution have less color ,(١٩٧٥) ,et al stability than sucrose solution of the same concentration when stored under the same conditions. This is due to chemically active reducing sugars in the invert sugar solution. The pH of the solution is highly important in lowering the rate of color In addition, the .٩.formation. This relationship is depicted in Fig temperature of the solution and the length of time it is heated markedly affect the color development in invert syrups, Mc described the two factors that make up the (١٩٧١) ,Ginnis concept of color which may be optically determined in sucrose solution. The first of these is the absorption of radiant energy in the presence of colorants. The second is the scattering of radiant energy due to any turbidity in the solution. Color development in sucrose solution is dependent upon several factors. Among these are the temperature of the solution, time of storage, pH, presence of trace of reducing sugars, and reported extensively on ,(١٩٥٣) ,colored non-sugars. Gillett color development in sucrose syrups during and after refining.

٢٠ْc the rate of color development is extremely slow but at At higher temperatures, over a period of time, color begins to appear in the solution.

١٠٠ Nitrogen content was the highest in Saeed syrup sample, and it was the lowest in AL-Modhesh syrup sample, while the Kenana samples (amber and treacle) had the same results. All the samples results were found to be lower than the reference sample (Tate and Lyle)in nitrogen content ratio, however, low nitrogen value was due to low nitrogen content in the raw sugar. Protein was determined via nitrogen content, so that protein has lower results. Comparable results for nitrogen and who (١٩٧٤) protein content were demonstrated by Braner reported that, the sugars were found to be very poor in nitrogen and consequently in protein content, this is due to the process and refining techniques employed for sugar extraction and crystallization. Ash content and viscosity .٤٫٤ shows results of ash content and viscosity of (٨) Table Tate and Lyle syrup as reference and other Sudanese local samples. Carbonated ash was the highest for Kenana treacle sample and it was the lowest for AL-Modhesh syrup sample. Kenana amber and Saeed syrups had the same result. All samples of golden syrup have lower carbonated ash ratio than the reference (Tate and Lyle).

١٠١ Ash content and viscosity of syrups .٨.Table

ANALYSIS Tate and Kenana Kenana Saeed AL- Lyle (amber) (treacle) Modhesh Ash content C S C S C S C S C S % ٣٫٩٢ ١٫٠ ٤٫٤ ١٫٢ ٤٫٣ ١٫٥ ٤٫٣٩ ١٫٢ ٤٫١٧ ١٫٤ ٥ ٧ ٠ Viscosity R Cs R Cs R Cs R Cs R Cs % ٤٫٠٢ ٢٫٥ ٤٫١ ٣٫٤٢ ٤٫١ ٣٫٤١ ٤٫٠٨ ٣٫٤٠ ٤٫٢٠ ٣٫٤٣ ٦ ٥ ١

Where C = carbonated ash S = sulphated ash R = relative viscosity Cs = centistock viscosity

١٠٢ Analysis of sulphated ash value for Saeed syrup sample showed the highest result, and it was the lowest in AL-Modhesh syrup sample, while Kenana samples (amber and treacle) had the same result. Samples of golden syrups except AL- Modhesh sample were almost greater in sulphated ash than the reference points, while AL-Modhesh sample ٣٠-١٣ Tate and Lyle) by) points. Comparable ٠٫٢٥ was lower than that of reference by who (١٩٧٠) results for ash content were demonstrated by Person ٪٤ for golden syrups, and ٪١٫٧ reported that, sulphated ash is for the treacle. Sudanese Standards and Metrology Organization for both golden syrup ٪٥-٢ SSMO) stated that, the ash ratio is) and treacle. The entire samples were identical with (SSMO). Some important factors affect the ash content ratio, of these, is ٪٣٦ syrup clarification, which decreases the sulphated of ash by .(٣ when it is practiced well (see table Relative viscosity was the highest in Saeed syrup sample, and it was the lowest in AL-Modhesh syrup sample, if compared with the reference (Tate and Lyle), while centistokes viscosity was the highest in Kenana (treacle) sample, and it was the lowest in AL-Modhesh syrup sample. Approximately all the samples were identical with the reference. Comparable results for viscosity were demonstrated who reported that, three factors affect the (١٩٦٧) by Norrish viscosity of invert sugar solutions. These are temperature,

١٠٣ concentration of total soluble solids, and the percentage of invert sugars. Minerals determination .٤٫٥ shows results of minerals for the reference (٩) Table sample and other local syrup samples. Sodium ratio was the highest in the reference (Tate and Lyle) sample, and the phosphor ratio was the lowest among other metals. Kenana (amber and treacle) and Saeed samples included high ratio of calcium, while AL-Modhesh syrup sample scored a high ratio of sodium which is similar to the reference. The entire samples showed lower ratios of phosphate that refers to the purification and clarification processes which are practiced in sugar and syrup manufacturing. All the samples included high ratio of calcium, sodium, and magnesium which are an important minerals. Saeed and AL- Modhesh sample had the same ratio of potassium which is lower than Kenana samples, that refers to the quality of raw materials used in syrups manufacture. Approximately all the samples have similar ratio of copper, manganese, iron, cobalt, chrome, nicle, lead, and zinc.

١٠٤

(Minerals of syrups (Mg/L .٩.Table

Type of Ca Mg Na K Cu Mn Fe Co Cr Ni Pb Zn P sample

٠٫٠٠١٢٠ ٠٫١١٠ ٠٫٠٢٣ ٠٫٠٣٤ ٠٫٠١٣ ٠٫١٥٧ ٠٫٠٦٥ ٠٫٠٤١ ٠٫٠٥٨ ٠٫٩١ ٩٫٣٠ ٠٫١٣ ٠٫٦٤ Tate and

Lyle

٠٫٠٠١٦١ ٠٫٠٣٩ ٠٫٠٢١ ٠٫٠٤٧ ٠٫٠٢٤ ٠٫٢٤٢ ٠٫٠٦٣ ٠٫٠١٣ ٠٫٠٢١ ٠٫١٩ ٠٫٥٨ ٠٫١٨ ٠٫٧٢ Kenana

(amber)

٠٫٠٠١٧٧ ٠٫٠٧٩ ٠٫٠٤٧ ٠٫٢٢ ٠٫٠٢٢ ٠٫٠٥٦ ٠٫١٥٦ ٠٫٠٤١ ٠٫٠٢٢ ٠٫٥١ ٠٫٦٧ ٠٫٤٣ ٠٫٩٨ Kenana

(treacle)

٠٫٠٠١٥٦ ٠٫٠٩٠ ٠٫٠٥٩ ٠٫٠٢٥ ٠٫٠١٤ ٠٫٠٦٥ ٠٫١٧٦ ٠٫٠٢٦ ٠٫٠٤٤ ٠٫٠٥ ٠٫٣٦ ٠٫١١ ٠٫٦٢ Saeed

٠٫٠٠١٤٦ ٠٫٠٦٩ ٠٫٠٤٥ ٠٫٠٤٠ ٠٫٠٤١ ٠٫١٦٢ ٠٫١٢٥ ٠٫٠٢٩ ٠٫٠٤١ ٠٫٠٥ ٠٫٥٦ ٠٫١٠ ٠٫٣٧ -AL

Modhesh

١٠٥

١٠٦ CHAPTER FIVE CONCLUSION AND RECOMMENDATIONS The work embodied in thesis was carried out on four local types of edible syrups (Kenana amber and treacle, Saeed, and AL-Modhesh), and compared with a reference syrup which is produced by Tate and Lyle company. ♦ The analytical studies involved physical and chemical analysis. These investigations were carried out for studying the quality of local edible syrups. They involved determination of total soluble solids (TSS), total sugars, reducing sugars, sucrose percent, refractive index, gravity purity, colour and acidity, in addition to viscosity, pH value, ash, minerals, moisture, nitrogen and protein content. ♦ The analytical data obtained for syrups revealed that AL- Modhesh syrup contained the lowest values in total soluble solids and reducing sugars, while Kenana amber syrup contained the highest values. Similar values were found for Kenana treacle and Saeed syrups. ♦ AL-Modhesh syrup had the highest value in sucrose percent than other local syrups. ♦ Indigenous edible syrups were slightly acidic. ♦ All the local syrups were found to be very poor in nitrogen and consequently in protein content. ♦ The treacle of Kenana had the highest colour value.

١٠٧ ♦ Indigenous edible syrup contained the highest portions of the calcium, sodium and magnesium, while it contained the lowest portions of phosphorous. ♦ The comparison between the four indigenous edible syrups and the reference Tate and Lyle revealed that AL-Modhesh syrup had the lowest quality, while the Kenana amber and Saeed golden syrups had a good quality compared with the reference. Kenana treacle had high quality compared with standards. ♦ Indigenous edible cane syrups had a high percent of sugars and minerals, and low percent of the protein. ♦ Most of the locally made golden syrups are made from white sugar, mostly locally manufactured. The practice showed that, the quality of the golden syrup wholly depends on two factors, which are the quality of the raw material, and the process conditions such as temperature. The improvements of the above factors lead to a high quality of golden syrups which were able to compete with the standard. ♦ It is recommended to manufacture the golden syrups from high quality sugars. Moreover, the ideal process conditions of golden and treacle syrup should be implemented, so as to avoid any undesirable malfunction caused by fluctuation of the process conditions, and to achieve this, modern controllable equipment are to be used for processing of

١٠٨ golden syrups and treacle. As well the packing materials must be attractive to the consumer. All the above factors enhance the quality and marketing effectively.

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