COMPARATIVE EVALUATION OF CLARIFYING REAGENTS OCTAPOL AND LEAD SUB ACETATE FOR USE WITH MASSECUITES AND MOLASSES. Niconor Reece and Sydney Roman

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1 COMPARATIVE EVALUATION OF CLARIFYING REAGENTS OCTAPOL AND LEAD SUB ACETATE FOR USE WITH MASSECUITES AND MOLASSES Niconor Reece and Sydney Roman

2 BACKGROUND OCTAPOL TM is a lead-free chemical reagent for the clarification of sucrose-containing materials prior to polarimetric analysis. Field-testing was carried out in cane sugar factories in several countries (USA, Guatemala, Brazil) during 1998(Baddley Chemical INC, 2007). OCTAPOLTM has been in use in the Jamaican Sugar Industry since 2002, as a replacement for lead subacetate use in juice clarification at the Core Laboratory.

3 RATIONAL Pressure to reduce the use of filter aids containing lead due to the adverse health concerns associated with the prolonged exposure to lead. Lead sub acetate difficult to source Variations to manufactures recommendations may be needed to get desired results.

4 OBJECTIVE Establish concentrations of octapol applicable to each substance, using manufacturer s recommendations as a guide, Recommend appropriate procedures based on manufacturers guide lines and research data.

5 EXPERIMENTAL PROCEDURES Samples of A, B, and C massecuites, syrup and final molasses collected from the sugar factories during the course of the 2007/2008 crop were used as sample material. General procedures followed throughout the determination were based on the manufacturer s guidelines for use of octapol, and methods accepted as standard in the local industry with the use of lead sub acetate.

6 EXPERIMENTAL PROCEDURES Initially, samples clarified with lead sub acetate were prepared according to the recommendations for Octapol. These samples were compared with samples analyzed by methods outlined by the manufacturer. Once a similarity was observed a procedure was drafted to find the best octapol concentration.

7 EXPERIMENTAL PROCEDURES The manufactures recommended quantities of reagent for each substance were as follows. Syrup 4-6g A-MASSECUITE 5-6g B-MASSECUITE 6-8g C-MASSECUITE 8-10g FINAL MOLASSES 10-15g

8 EXPERIMENTAL PROCEDURES Baddley Chemicals, Inc. recommendations for Octapol use were as follows: For syrup analyses, Weigh 26g of syrup into a 200ml flask, add water to the mark and mix well. Pipette 100ml of this solution into a 200ml bottle with stopper. Add about 5g of reagent, shake well and filter. Measure pol reading at 20 C. For massecuite and molasses analyses, Prepare a 1:1 dilution of massecuite (or molasses) and water. Weigh 26g of this diluted stock into a 200ml flask Add water to the mark and mix well. Pipette 100ml of this into a 200 ml bottle with stopper Add Octapol reagent, stopper and shake well. Filter and measure pol reading.

9 EXPERIMENTAL PROCEDURES Current Industry procedure for lead subacetate For syrup and massecuites, Weigh 26g of the sample into a counterpoised nickel dish Wash in a 100ml flask Clarify with 2g of basic dry lead acetate and filter Collect the filtrate and read on polarimeter For Final molasses, Weigh 13g of the sample in a counterpoised nickel dish, and transfer to a 200ml flask. Thoroughly dissolve the molasses by swirling, and fill up to the mark. Add 6-8g of Horne s dry lead. Mix and filter through #5 filter paper. Discard the first 20-25ml then pipette 100ml of the filtrate to a 110ml flask. Acidify with 5ml 20% acetic acid solution, and then make up to the mark with distilled water. Shake the entire flask and re-filter Read filtrate on polarimeter at 20 C.

10 RESULTS AND DISCUSSION higher levels of octapol use was needed to get favourable results. showed fluctuations in the difference in pol values. The differences were as low as a 0.03 in final molasses to 2.56 in C massecuite octapol use generally results in lower pol values than those obtained from lead subacetate

11 RESULTS AND DISCUSSION

12 RESULTS AND DISCUSSION Pol Differences Between A massecuite Samples Clarified by Lead Subacetate and OCTAPOL Pol Difference Lead (Pb) OCTAPOL SAMPLES Lead (Pb) OCTAPOL SAMPLES Difference

13 RESULTS AND DISCUSSION Pol Difference Between B Massecuites Samples Clarified with Lead subacetate and OCTAPOL Pol Difference Lead (Pb)65.66 OCTAPOL SAMPLES Lead (Pb)57.3 OCTAPOL SAMPLES Difference

14 RESULTS AND DISCUSSION Pol Difference in C Massecuites Clarified Lead sub acetate and OCAPOL Pol Difference Lead (Pb) OCTAPOL SAMPLES Lead (Pb) OCTAPOL SAMPLES Difference

15 RESULTS AND DISCUSSION Pol Difference Between Syrup Samples Clarified with Lead subacetate and OCTAPOL Pol Difference Lead (Pb) OCTAPOL SAMPLES Lead (Pb) OCTAPOL SAMPLES Difference

16 CONCLUSION The results showed Octapol to be a good substitute for lead subacetate. Octapol use resulted in good filtration rate and high filtrate clarity. However, Pol values estimated from Octapol use were generally lower than those obtained from use of lead subacetate. Therefore the recommendations are as follows Molasses and Massecuites.

17 CONCLUSION Therefore the recommendations are as follows Molasses and Massecuites 1) Weigh 13g of massecuite (or final molasses) in a counterpoised nickel dish. 2) Dissolved in about 40ml of hot water, and transfer to a 200ml volumetric flask. 3) Make up to the mark with distilled water and mix well. 4) Pipette 100ml of this sample and transfer to a 200ml bottle. 5) Clarify as follows SIRI Baddley A MASSECUITE: 6-8g 5-6g B MASSECUITE: 8-10g 6-8g C MASSECUITE: 11-13g 8-10g FINAL MOLASSES: 16-18g 10-15g 6) Shake well and allow standing for two minutes. 7) Filter and read filtrate on polarimeter for %pol. SYRUP 1) Weigh 26g of syrup in a counterpoised nickel dish. 2) Transfer to a 200ml volumetric flask using hot water. 3) Make up to the mark and mix well. 4) Pipette 100ml to a 200ml bottle. 5) Add 4-6g Octapol reagent, shake well and leave to stand for two minutes. 6) Filter, and read filtrate for % pol.

18 ACKNOWLEDGEMENT ACKNOWLEDGEMENT The Arthors which to extend thanks to the sugartech team and the UWI summer interns for work on this project. Special thanks to all fatory personel for there support on this project. REFERENCES Baddley Chemical INC. (2007, 2 22). FREQUENTLY ASKED QUESTIONS ABOUT OCTAPOL and OCTAPOL PLUS. Retrieved 10 13, 2008, from Baddley Chemicals: