CD/K/2:2013 ICS FDEAS 819 : 2013 FINAL DRAFT EAST AFRICAN STANDARD. Molasses for Industrial use Specification EAST AFRICAN COMMUNITY

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1 CD/K/2:2013 ICS FDEAS 819 : 2013 FINAL DRAFT EAST AFRICAN STANDARD Molasses for Industrial use Specification EAST AFRICAN COMMUNITY EAS 2013 First Edition 2013

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3 CD/K/2:2013 Copyright notice This EAC document is copyright-protected by EAC. While the reproduction of this document by participants in the EAC standards development process is permitted without prior permission from EAC, neither this document nor any extract from it may be reproduced, stored or transmitted in any form for any other purpose without prior written permission from EAC. Requests for permission to reproduce this document for the purpose of selling it should be addressed as shown below or to EAC s member body in the country of the requester: East African Community 2013 All rights reserved East African Community P.O.Box 1096 Arusha Tanzania Tel: /8 Fax: / eac@eachq.org Web: Reproduction for sales purposes may be subject to royalty payments or a licensing agreement. Violators may be persecuted ii EAC 2013 All rights reserved

4 CD/K/2:2013 Contents Page 1. Scope Normative references Compositional Requirements Hygiene Packaging Labelling/Marking... Error! Bookmark not defined. Annex A Brix Determination (Normative) Annex B Determination of total invert sugars (Normative) Annex C Ash determination (Normative) Annex D Density determination (Normative) Annex... E Calcium determination (Normative) 17 ANNEX...F Determination of Phosphorus (Normative) 18 Annex... G Loose Sludge determination (Normative) 19 Annex... H Determination of ph (Normative) 20 Annex J Sulphur dioxide determination (Normative) Annex... K Determination of Nitrogen (Normative) 22 Annex L (informative) Bibliography EAC 2013 All rights reserved iii

5 CD/K/2:2013 Foreword Development of the East African Standards has been necessitated by the need for harmonizing requirements governing quality of products and services in the East African Community. It is envisaged that through harmonized standardization, trade barriers that are encountered when goods and services are exchanged within the Community will be removed. In order to achieve this objective, the Community established an East African Standards Committee mandated to develop and issue East African Standards. The Committee is composed of representatives of the National Standards Bodies in Partner States, together with the representatives from the private sectors and consumer organizations. Draft East African Standards are circulated to stakeholders through the National Standards Bodies in the Partner States. The comments received are discussed and incorporated before finalization of standards, in accordance with the procedures of the Community. East African Standards are subject to review, to keep pace with technological advances. Users of the East African Standards are therefore expected to ensure that they always have the latest versions of the standards they are implementing. CD/K/2 was prepared by Technical Committee EASC/ TC/015, Sugar and Sugar Products. iv EAC 2013 All rights reserved

6 CD/K/2:2013 Introduction EAC 2013 All rights reserved v

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8 DRAFT EAST AFRICAN STANDARD CD/K/2:2013 Molasses for Industrial use Specification 1. Scope This Draft East African Standard specifies quality requirements and methods of sampling and test for molasses for industrial use. The standard does not cover molasses as a direct feed for livestock. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies AOAC : Determination of Sulfadiazine and Sulfamerazine Spectrophotometric Method ISO 5809 : Starches and derived products -- Determination of sulphated ash AOAC : Ash of Sugars and Syrups: Sulfated Ash ISO 5379: Starches and derived product, Determination of sulfur dioxide content 3. Terms and Definition For purposes of this standard the following definitions shall apply. 3.1 Sugar sucrose obtained from processing of physiologically mature sugar cane or other sources EAC 2013 All rights reserved 1

9 3.2 Molasses dark, sweet, syrupy by-product made during the extraction of sugars from sugarcane and other sources to which no other material has been added Extraneous matter Organic matter originating from sugar cane plants and/or their products other than molasses Foreign matter Organic and inorganic materials ( such as sand, soil, glass) and other extraneous matter in molasses 4. Requirements 4.1 General Requirements Molasses shall a) have characteristic brown/dark brown colour. b) Be viscous with a characteristic flavour and smell. c) Be free from any extraneous matter, adulterants, and other harmful constituents. d) Be free from insects, rodents and their parts e) Be free from foreign matter 4.1 Specific Requirements Molasses shall comply with the quality requirements/limits stipulated in Table 1.below; 2 EAC 2013 All rights reserved

10 Table 1: quality Requirements/Limits for molasses S.NO. Parameters i Standard Brix degree at 20 0 C min ii Total Invert sugars, % m/m, min. iii Sulphated ash, % m/m max iv Total ash,%, m/m, max Requirements/Limits Test Methods 75 AOAC ICMSA GS 1/3/71994 Annex Annex A Annex B 25 ISO 5809 Annex C 15 AOAC Annex C v Density, g/cm 3 min vi Calcium as Ca, %, m/m, max, viii Phosphorous as P, %,m/m, max. ix Loose Sludge,%,v/v, max x PH of 10% solution, M/V xi Sulphur dioxide as SO 2 ppm max 1.30 Annex D 2.1 Annex E 0.5 Annex F 40 Annex G ICUMSA GS 1/2/3/4/7/8-23 Annex H 400 ISO 5379 Annex J xii Cobalt (Co), ppm, max Contaminants 5.1 Pesticide residues Molasses shall comply with those maximum pesticide residues established by the codex alimentarius commission for this commodity EAC 2013 All rights reserved 3

11 5.2 Heavy metal Molasses shall be free from heavy metals in amounts which may represent a hazard to human health. 6 Hygiene 6.1 molasses shall be prepared and handled in accordance to the EAS 39 Code of Practice for Food and Drink Manufacturing Industry. 6.2 molasses shall comply with microbiological limits stipulated in Table 3 Table 3: Microbiological Limits for molasses S.No. Parameter Limits Test Method i ii iii iv v Yeast and Mould per gram, CFU max 10 3 ISO EAC 2013 All rights reserved

12 7. Packaging / Storage 7.1 molasses shall be stored and packaged in material which guarantees the safety and integrity of the product. 7.2 The fill of each package shall comply with weights and measures legislation and legal metrology of the importing Partner State. 8 Labelling/Marking 8.1 Molasses in bulk packages shall be accompanied with document bearing information as indicated below : Name of the product as Molasses Name, physical location and address of the manufacturer/distributor/importer Net contents by mass in metric units (Kg/Tonnes) Country of origin.storage instruction 8.2 Molasses in non-bulk packages shall be labelled in accordance with EAS In addition to 9.1 tankers (bulk packages) used for transporting molasses shall be conspicuously labelled/marked with the word MOLASSES ) 9 Sampling EAC 2013 All rights reserved 5

13 9.1 Sampling of cane molasses In drawing, preparing, storing and handling test samples, the following precautions and directions shall be taken The sampling instrument shall be clean and dry when used The samples, the material being sampled the sampling instrument and the containers for samples shall be protected from adventitious contamination To draw a representative sample, the contents of each container selected for sampling shall be mixed as thoroughly possible by shaking or stilling or both, or by rolling so as to bring all portions into uniform distribution The sample shall be placed in suitable clean, dry and air-tight metal or glass containers, on which the material has no action The sample containers shall be of such a size that they are almost, but not completely, filled by the sample Each sample container shall be sealed airtight and market with full details of sampling and the date of sampling Sampling can: Consists of a weighted metal cylinder with removable top, to which a rod is attached (see Fig.1). The cylinder is fasted to suitable rod. For tacking a sample, it is lowered in the tank to the required depth, and the top is removed with the help of the rod and the can then filled. For other containers, the sampling device of the design shown in figure 2 may be used. 6 EAC 2013 All rights reserved

14 9.2 Scale of Sampling Supply in Tank/Tankers Samples shall be drawn from each cane/tanker as follows. Equal portions of the material shall be taken from different la yers of the tank/tanker with the help of the sampling can to obtain a composite sample not less than 2.5 liters and mixed thoroughly in a suitable container. Divide this composite sample into three equal portions of not less than 750 ml in dried bottles or other containers, seal airtight and label with all the particulars of the sample Supply in containers All the containers in a single consignment shall constitute one lot Gross sample. For the purpose of drawing samples for test a number of containers shall be selected at random from a lot. The number of containers in relation to the size of the lot or scale of sampling shall be as in the following table. Table II: Showing the minimum number of containers to be selected for sampling from various sizes of lots. Lot size Sample size 2 to to 27 3 EAC 2013 All rights reserved 7

15 28 to to to to to to to to Sampling from containers Mix thoroughly the contents of all the containers in the gross sample whether they are drams or cans of other, by shaking or stirring or both, or by rolling so as to bring all portions into uniform distribution Drawing Samples: Samples shall be drawn by inserting the sampling device thorough the bung hole any other convenient opening equal portions of the well-mixed material from each container in the gross sample shall be taken so as to obtain a quantity not less than 2.5 liters. The composite sample thus obtained shall be divided into three equal portions of not less than 750 ml in dried bottles or other containers, sealed airtight and labeled with all the particulars of the sample Reference sample: The third sample bearing the seals of sampler and the producer shall be kept in appropriate place to be used in the case of dispute Time limit for analysis: All samples shall be tested with in two months from the date of sampling Criterion for acceptance: If on testing, the sample is found to conform to the requirements specified in the standard, the consignment shall be accepted. 8 EAC 2013 All rights reserved

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17 Annex A Brix Determination (Normative) (a) Brix Determination by Spindle Method Determine the Brix by using an appropriate spindle 30 0 C Baume-60 0 C Baum. Note the reading and the temperature from the thermometer attached to the base of the spindle. Apply the temperature correction and record the Brix at 20 0 C. (b) Brix Determination by Refractometer Method Using a 50 % sample solution pipette a few ml through the clarity filter rubber teat pipette and pour onto the glass prism cover. Press the read function to take the reading.multiply the reading by two to get the result. 10 EAC 2013 All rights reserved

18 Annex B Determination of total invert sugars (Normative) (i) Weigh approximately 5.0 g of raw molasses and dissolve in distilled water. (ii) Transfer to a 250 ml volumetric flask, rinse the beaker and add the rinse to the flask. (iii) Add 10 ml of neutralized lead acetate solution and shake vigorously. Add 5 ml of potassium oxalate solution and shake again. (iv) Fill the flask to volume with distilled water, mix well and allow it to precipitate. (v) Filter using clean filter paper No. 1 and collect the filtrate for analysis. Determination of Reducing Sugar and Invert Sugars (Lane & Eynon Method) i) Scope and field of application The Lane & Eynon method is used for determination of invert sugar, dextrose, fructose, maltose and lactose. ii) PRINCIPLE The reducing sugar solution is titrated against a strongly alkaline cupricomplex salt solution (Fehlings solution mixture), which is then boiled. This estimates sugars by the measurement of reduction of Cull and Cul. Fehlings solution consists of alkaline cupric tartarate and is converted to insoluble cuprous oxide when boiled with a solution of reducing sugar. iii) APPARATUS Conical flasks 250 ml Burette 50 ml graduated in 0.1 ml Pipette, 5, 10 ml. Volumetric flask 200 ml and 250 ml. Measuring cylinder 100 ml Water bath Stop watch Balance hot plate Glass rod. EAC 2013 All rights reserved 11

19 iv) PROCEDURE i) Weigh 5.0 g of raw molasses, add 50 ml of distilled water and stir thoroughly to dissolve the molasses. ii) Transfer the solution into a 250 ml volumetric flask. iii) Add 10 ml of20 % Neutralized Lead Acetate and shake well. iv) Add 5 ml of 10 % Potassium Oxalate solution and mix thoroughly. (v) fill the flask to volume with distilled water and mix well. (vi) Filter then transfer 50 ml of the filtrate into 250 ml volumetric flask. (vii) Add 5 ml concentrated hydrochloric acid and place in water bath set at 65 C for w0 minutes. (viii) Cool the solution and neutralise with20 % NaOH using phenolphthalein indicator to pink colour end-point. (ix) Make up to volume with distilled water to 250 ml. (x) Titrate 5 ml each of Fehlings A and B solution with the sugar solution using methylene blue solution as indictor and take the titre value and from the provided sugars conversion table record the corresponding invert sugars level. (xi) Calculate percentage total reducing sugar thus:- % Reducing Sugars = Mg Invert Sugar x 250 x 250 x 250 x x Titrate value x 50 xwt of sample * 50 = M/s of filtrate hydrolysed. Note 1 Mg Invert Sugar is calculated with reference to Lane and Eynon tables of particular sugar in relation to titre value vis-à-vis volume of reaction mixtures. 12 EAC 2013 All rights reserved

20 Annex C Ash determination (Normative) C.1 Scope and Field of Application Ash may be determined by two distinct procedures; Gravimetrically and Conductimetrically. (a) Gravimetric To give the sum of water-soluble and water-insoluble ash. Gravimetric ash may be determined in two forms carbonated ash or sulphated ash. In the case of products containing magnesium salts, the sulphated ash procedure is slightly modified. (b) Conductimetric To give a measure of the concentration of ionised soluble salts present. The ash determined conductimetrically, known as conductivity ash cannot be directly compared with the gravimetric ash determined by incineration and weighing of ash. Conductivity ash has its own individual significance and can be determined with a minimum of time and effort. The factors for converting conductivity to conductivity ash are chosen in such a way that the conductivity ash values correspond approximately to values for sulphated ash. The methods are applicable not only to commercial sugars but also to intermediate products in the sugar manufacturing process. C.2 Sulphated Ash C.2.1 Principle of Method Double sulphitation is necessary to ensure conversion of ash to the sulphate form. C.2.2 Apparatus Platinum silica, stainless steel dish or porcelain dish (100 ml) Dessicator, muffle furnace and analytical balance. C.2.3 Reagents Sulphuric Acid (concentrated, AR) C.2.4 Procedure (a) Weigh about 5 g of molasses into a pre-dried and weighed platinum dish or silica crucible. (b) Moisten the sample with 0.5 ml of concentrated sulphuric acid. (c) Heat gently in a fume chamber avoiding overflow of froth by heating both from below and above the dish until the sample is carbonised. (d) Place the carbonised sample in a muffle furnace at 550 o C for two hours. (e) Remove the sample, cool and moisten again with one or two drops of sulphuric acid (conc) and put in the furnace at 800 o C for one hour or until the carbon disappears. Cool in a dessicator to room temperature. EAC 2013 All rights reserved 13

21 Weigh the ash. The weight of the residue shall be expressed as a percentage of the weight of sample taken. Wt. of Ash x 100 Sulphated Ash = Per cent Wt. of sugar Sample NOTE: (a) Silica crucibles are recommended as porcelain crucible tends to crack at high temperatures. The crucible capacity should be 25 ml. (b) The muffle furnace used should be able to attain a temperature of 900 o C. C.3 Conductivity Ash (i) Principle of Method The specific conductivity of a molasses solution of known concentration is determined. It is assumed that the conductivity has its own significance and the equivalent ash is calculated by the application of a constant factor. A concentration of 28 g/100 g is used. The factors used for transforming measured conductivity into ash are purely conventional and applicable only to sugar solutions. (ii) Apparatus (a) Fume chamber (b) Conductivity meter (c) Balance (d) Thermometer (e) Waterbath (f) Volumetric flasks (100 ml, 500 ml, 1000 ml) (e) Pipettes (10 ml) (iii) Reagents Deionised water 14 EAC 2013 All rights reserved

22 (iv) Procedure For the preparation of all solutions of molasses and potassium chloride distilled or de-ionized water with conductivity of less than 2 s /cm must be used. All vessels and all pipettes shall be rinsed with water of this quality before use. (a) Determination of specific conductivity of water The same quantity of water as used for dissolving the molasses is shaken in a 1000 ml; volume flask it is then made to the mark and a reading made at about 20 o C. For this measurement, precise temperature control is not needed since the temperature correction involved is distinctly less than the limits of error. (b) Standardization of conductivity measuring instruments This is effected with a N solution of potassium chloride. For this purpose, mg of potassium chloride (analar),. At exactly 20 o C or room temperature this N Potassium Chloride Solution shall have a specific conductivity of s/cm after deduction of the specific conductivity of the water used. According to the method of operation of this instrument and the method used for measuring conductivity, the instrument shall be set up in such a way that it indicates the above value, increased by the specific conductivity of the water used. Alternatively, the above value, increased by the specific conductivity of the water used, shall be used for calculating the cell-constant. The potassium chloride solutions shall be freshly prepared before each calibration. (c) Measurement of conductivity A molasses solution of 28 g/100 g is prepared either by dissolving g of sugar at o C in a 100 ml graduated flask, or by dissolving 28 g of sugar in water and making up to 100 g. Mix thoroughly. Transfer the solution into the measuring cell and measure its conductivity at 20 o C (C read). From the reading is deducted 20 per cent of the value for the distilled water. The following result shall thus be obtained: C 28 = C read 0.2 C water where, C = specific conductivity in s/cm Ash in percentage = x 1.8 x C 28 = 6 x C 28, x 10-4 NOTE: If conductivity cannot be determined at the standard temperature of 20 C, use the following temperature corrections. a) For each o C, below 20 o C add 2.6 per cent. b) For each o C, above 20 o C substract 2.6 per cent. EAC 2013 All rights reserved 15

23 Annex D Density determination (Normative) i) Accurately transfer the above-diluted molasses into a 100 ml volumetric flask to the level mark. ii) Take the weight and calculate the density thus:- Density = 2X Weight of 100ml gml 1 16 EAC 2013 All rights reserved

24 Annex E Calcium determination (Normative) D1 Take g of ash from test a above into a 100 ml volumetric flask, add drops of cone. HCl and allow to stand to hydrolyse D2 Add distilled water, shake thoroughly and make to volume with distilled water. Pipette out 25 ml of the homogenised sample into a conical flask, add 5 ml of ammonium buffer solution and 0.1g of ferrochrome black indicator. Titrate against 0.02 N EDTA or blur colour development. Calculation % Calcium; T. V x x100 x100 x % Ash % Ca2* = wt. sample x 25 x100 EAC 2013 All rights reserved 17

25 ANNEX F Determination of Phosphorus (Normative) i. Take 10 ml of the digested solution in 100 ml volumetric flask and neutralise the solution with 20 % NaOH till distinctly alkaline. ii) Add about 25 ml of distilled water, 2 ml of metabisulphite solution 4 ml each of ammonium molybdate reagent and metal solution. iii) Prepare likewise blank using distilled water in place of the sample. iv) Leave the flasks in the dark for 30 minutes for colour development. v) Remove the flasks and make to volume with distilled water. vi) Determine the concentration of the samples at 620 mm in spectro-colorimeter using standard solution for calibration. Calculation % P2O5 = Titrateval uexf a x0.0014x100x100 25xwtofsampletakenxDMS f a = normality correction factor for H 2SO 4 18 EAC 2013 All rights reserved

26 Annex G Loose Sludge determination (Normative) Weigh 270 g of raw molasses and add the following quantity of distilled water Xg, Where X = 6 x (Brix 45) g of distilled 20 0 C. Adjust the ph to 4.5 using 10 % H 2 s0 4. Boil for 3 minutes and allow settling in graduated cones. Note the settled volume after 30 minutes and express as % (v/v) loose sludge. EAC 2013 All rights reserved 19

27 Annex H Determination of ph (Normative) A1. Apparatus A1.1 ph Meter An electrometric ph meter of the glass electrode type capable of measuring ph values to 0.1 ph value. Before each series of measurement, the ph meter shall be standardized against two standard buffer solutions, one having a ph value of 4 and the other a ph value of 9. A1.2 Procedure Weigh, to the nearest 0.001g, 10 g of the prepared sample and completely dissolve it in 100 ml of water in a beaker at room temperature. Measure the ph of the solution with the ph meter. Take the average of two measurements and report the mean of two ph values. 20 EAC 2013 All rights reserved

28 Annex J Sulphur dioxide determination (Normative) 1. Iodine solution: Dissolve 12 gms of Potassium Iodide (KI) in 9 mls of water, add 8 gms of Iodine crystals, stir until completely in solution and dilute to 200 ml. Store the solution in glass stoppered amber reagent bottle. Dilute 12.8 ml of the above iodine solution with water to 200 mls to make 0.02 N Iodine solution N H 2 S0 4 Add 50 mls of conc. Sulphuric acid (96-98 % w/w) to 150 ml of water cooled in an ice bath. Mix well % NaOH Dissolve slightly more than 20 gms of NaOH in recently boiled and cooled water and dilute to 200 ml. in a plastic bottle. Store PROCEDURE Weigh 25 gms of molasses into each of two 250 mls conical flasks. Add about 50 mls of hot water and stir until homogenous solution is obtained. Add two ice cubes and place the conical flasks and contents in a water bath near 0 0 C, when the solution reaches 5 0 C, add 10 mls of NaOH AND allow the conical flasks to remain in water bath for additional 10 minutes. The add 10 ml of 9NH 2 SO 4 and 2 ml of starch indicator to both beakers and mix. Immediately titrate one of t he conical flasks with 0.02 N Iodine solution until the blue colour purists for 1 minute. A blank is obtained by adding 10 ml of 3 % H to the other conical flask before titrating. Calculation ( SampleTitreValue BlankTitreValue ) x 0.02 x0.032 x SO2( PPM ) Sampleweight EAC 2013 All rights reserved 21

29 Annex K Determination of Nitrogen (Normative) (i) Weigh accurately about 0.6 g of the yeast cake, transfer into the Kjeldahl digestion flask and add a few ml of distilled water. (ii) Begin the wet digestion at low temperature and gradually increase the heat until a completely clear solution is obtained. (iii) Begin the wet digestion at low temperature and gradually increase the heat until a completely clear solution is obtained. (iv) Set aside to cool and dilute with distilled water to 100 ml volume. (v) Take 25 ml. of this solution for distillation in another Kjeldahl flask, add to it 20 ml of 20 % NaOH and proceed with steam distillation. Collect the ammonia distillate in 10 ml of 2 % Boric acid solution to which a few drops of mixed indicator has been added. Continue distillation for 2½ minutes from the time the indictor turns to green. (vi) At the end of the distillation process, titrate the solution against 0.1 N H 2 SO 4 to a purple red end-point. Calculate the % Nitrogen thus:- % Nitrogen (N2) = Titrateval ue x f x x100x100 a 23 x wt of sampletaken x DMS f a= normality correction factor for H 2SO 4 22 EAC 2013 All rights reserved

30 Annex L (informative) Bibliography Canadian Standard: Specification for molasses: M. Pakistan Standard 139: Specification for cane molasses EAC 2013 All rights reserved 23

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32 DEAS 304:2013 EAC 2013 All rights reserved