Draft for comments only Not to be cited as East African Standard

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1 EAST AFRICAN STANDARD Beeswax Crude and refined Specification EAST AFRICAN COMMUNITY CD/K/650:2010 ICS ; EAC 2010 First Edition 2010

2 Foreword Development of the East African Standards has been necessitated by the need for harmonizing requirements governing quality of products and services in East Africa. It is envisaged that through harmonized standardization, trade barriers which are encountered when goods and services are exchanged within the Community will be removed. In order to meet the above objectives, the EAC Partner States have enacted an East African Standardization, Quality Assurance, Metrology and Test Act, 2006 (EAC SQMT Act, 2006) to make provisions for ensuring standardization, quality assurance, metrology and testing of products produced or originating in a third country and traded in the Community in order to facilitate industrial development and trade as well as helping to protect the health and safety of society and the environment in the Community. East African Standards are formulated in accordance with the procedures established by the East African Standards Committee. The East African Standards Committee is established under the provisions of Article 4 of the EAC SQMT Act, 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. Article 15(1) of the EAC SQMT Act, 2006 provides that Within six months of the declaration of an East African Standard, the Partner States shall adopt, without deviation from the approved text of the standard, the East African Standard as a national standard and withdraw any existing national standard with similar scope and purpose. 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. East African Community 2010 All rights reserved * East African Community P O Box 1096 Arusha Tanzania Tel: /8 Fax: / eac@eachq.org Web: * 2010 EAC All rights of exploitation in any form and by any means reserved worldwide for EAC Partner States NSBs. ii EAC 2010 All rights reserved

3 Introduction CD/K/650:2010 Beeswax is a wax secreted in form of scales by the worker bees through their wax glands. It is extracted from honeycombs of either wild or domesticated bees after the removal of honey. The beeswax as obtained from the comb is called raw beeswax and is progressively modified by physical treatment to yield crude and refined beeswax and by chemical treatment to yield bleached beeswax. Beeswax has many uses in industry, pharmacy and medicine. Some of the documented uses include making of adhesives, candles, cosmetics, electrical insulation, explosives, floor polishes, lubricants, pencils, pharmaceuticals, printing inks, shoe creams, varnishes in leather, moulding, paper and rubber industries. In the preparation of this East African Standard, the following sources were consulted extensively: KS :1997, Specification for natural beeswax IS 1504:1996(R2004), Beeswax, Crude and Refined Specification IS 4028:1992(R2006), Beeswax, Bleached for Cosmetic Industry Specification Codex Alimentarius website: USDA Foreign Agricultural Service website: USDA Agricultural Marketing Service website: USDA Plant Inspectorate Service website: European Union: Assistance derived from these sources is hereby acknowledged. EAC 2010 All rights reserved iii

4 Contents 1 Scope Normative references Definitions Types and grades Presentation Requirements Sampling Packaging and labelling... 3 Annex A (normative) Determination of meting point... 8 Annex B (normative) Determination of specific gravity... 9 Annex C (normative) Determination of refractive index Annex D (normative) Determination of matter insoluble in benzene Annex E (normative) Determination of acid value Annex F (normative) Determination of ester value Annex G (normative) Determination of matter soluble in water Annex H (normative) Determination of saponification value Annex J (normative Determination of iodine vale (Wijs method) Annex K (normative) Determination of ash Annex L (normative) Test for fats, fatty acids, Japan wax and rosin Annex M (normative) Sampling of beeswax, crude and refined iv EAC 2010 All rights reserved

5 EAST AFRICAN STANDARD CD/K/650:2010 Beeswax Crude and refined Specification 1 Scope This East African Standard specifies the minimum requirements and methods of test for beeswax. This standard applies to all beeswax produced from honey combs (after removal of honey) and cappings that cover cells of honey combs derived from honey bee species Apis spp. It includes the various forms offered for direct use whether in crude, refined or bleached forms. 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. CAC/GL 21, Principles for the establishment and application of microbiological criteria for foods CAC/RCP 1, Recommended international code of practice General principles of food hygiene CAC/GL 30, Principles and guidelines for the conduct of microbiological risk assessment EAS 38, Labelling of prepackaged foods Specification EAS 123, Distilled water Specification 3 Definitions For the purposes of this standard, the following definitions shall apply: 3.1 beeswax a natural animal wax produced by Apis spp. species of the honey bee. The wax is secreted by four pairs of glands located on the ventral side of the abdomen of worker bees. Bees use it to make cells and cappings for the purpose of storing honey pollen and rearing brood. 3.2 crude beeswax The wax obtained from the honey combs after the removal of honey and after being subjected to a preliminary treatment, such as melting, scumming decantation and moulding. 3.3 refined beeswax The wax obtained after subjecting crude beeswax to further purification by melting (usually in hot water or steam) and finer filtration. 3.4 bleached beeswax Refined beeswax which has been naturally bleached (solar) and finally filtered. 4 Types and grades 4.1 The beeswax shall be of the following two types: a) Crude beeswax The material obtained from the honeycombs after the removal of honey and after subjecting the material to a preliminary treatment, such as melting, scumming, EAC 2010 All rights reserved 1

6 decantation and moulding. It shall not contain any other added material, such as paraffin wax and starch. b) Refined wax The material obtained after subjecting crude beeswax to further purification by melting and finer filtration. 4.2 The refined beeswax shall be of two grades, namely, Grade A and Grade B. Grade A beeswax shall be derived from Apis cerana indica, A mellifera bees, whereas Grade B may be derived from other species of Apis or a mixture thereof. 5 Presentation The material shall be in the form as agreed between the purchaser and the supplier. In the absence of such an agreement, it shall be in the form of slabs. 6 Requirements 6.1 Colour and aroma The colour of crude and refined beeswax shall be whitish yellow to yellowish brown and it shall have a characteristic aroma. The aqueous extract of Grade A refined beeswax shall not be acidic. 6.2 Freedom from foreign matter Beeswax shall be free from inorganic or organic matter such as bees, brood, debris, sand or any other extraneous matter. 6.3 Purity Beeswax shall be pure and unadulterated. It shall not be blended or contain any other waxes such as paraffin, microcrystalline or synthetic waxes nor shall it be mixed with any oil, fat or any other contaminant. 6.4 Composition of natural beeswax Generally, beeswax consists of hydrocarbons (14 per cent), mono-esters (35 per cent), diesters (14 per cent), triesters (3 per cent), hydroxymonoester (4 per cent), hydroxy polyesters (8 per cent), free acids (12 per cent), acid esters (1 per cent) acid polyesters (2 per cent), free alcohols (1 per cent) and unidentified substances including pigments and proprolis (6 per cent). 6.5 Specific requirements Beeswax shall also comply with the requirements given in Table 1. 2 EAC 2010 All rights reserved

7 Table 1 Requirements for beeswax, crude and refined CD/K/650:2010 Characteristic Crude Refined Method of test Grade A Grade B Specific gravity to to to Refractive index an 75 C to to Melting point, C 58 to to to 63 Acid value, Max 5 to 24 5 to 24 5 to 24 Saponification value Not less than to to 105 Iodine value, Max to to 10.0 Ash, % by mass, max ) Sulphated ash, % by mass, max Total volatile matter, % by mass, max Matter insoluble in benzene, % by mass, max Matter soluble in water, % by mass, max ) Shall not contain any particles of gritty nature which are retained on a 425 µm sieve 7 Sampling The method of preparing representative test samples of the material and the criteria for conformity shall be as prescribed in Annex M. 8 Packaging and labelling 8.1 Packaging Beeswax shall be packed in greaseproof paper or any suitable material like polythene, jute or sisal bags. 8.2 Labelling Each container of beeswax shall be suitably labelled to give the following information: (i) (ii) (iii) (iv) name and address of manufacturer (or dealer); name or type of wax; net contents in appropriate SI units; country of origin. EAC 2010 All rights reserved 3

8 Crude beeswax Yellow Beeswax pastiles 4 EAC 2010 All rights reserved

9 Refined white beeswax Beeswax presentations Hexagonal CD/K/650:2010 EAC 2010 All rights reserved 5

10 Beeswax presentations Hexagonal chunk 6 EAC 2010 All rights reserved

11 Beeswax presentations Beeswax presentations CD/K/650:2010 EAC 2010 All rights reserved 7

12 Annex A (normative) Determination of meting point A.1 Quality of reagents Unless specified otherwise, pure chemicals and distilled water shall be used in tests. A.2 Apparatus A.2.1 Thermometer With an accuracy of 0.1 ºC and graduated at every 0.1 ºC. A.2.2 Test tube With centrally bored cork to take thermometer and with a slit to permit air circulation. A.2.3 Water bath With a thermometer. A.3 Procedure A.3.1 A.3.2 Melt the wax by warming it in water bath at a temperature just sufficient to melt it. Dip the thermometer and withdraw, so as to get the bulb thinly coated with wax. A.3.3 Insert the thermometer into the test tube through the bored cork and then place the test tube in the water bath. A.3.4 Rise the temperature gradually, at the rate of 1 ºC in 3 minutes. Note the temperature, accurately to 0.1 ºC, at which a transparent drop forms on the end of the thermometer bulb. A.3.5 Record this temperature as the melting point of the wax. 8 EAC 2010 All rights reserved

13 B.1 Apparatus B.1.1 B.1.2 Water bath Maintained at 25 ºC ± 1 ºC. Specific gravity bottle 25 ml capacity. B.2 Reagents B.2.1 Rectified spirit B.3 Procedure B.3.1 B.3.2 B.3.3 B.3.4 B.3.5 Annex B (normative) Determination of specific gravity CD/K/650:2010 Melt approximately 2 g of the wax in a porcelain crucible at a temperature of about 100 ºC. Allow to cool at room temperature. Remove the solidified beeswax from the crucible, warming slightly if necessary. Attach a tared silk thread that will suspend the beeswax during weighing. Store the sample for 2 hours at a temperature of 25 ± 1 ºC. B.3.6 Determine the mass of the sample, first in air and then in rectified spirit maintained at 25 ± 1 ºC. B.3.7 Determine the specific gravity at 25 ºC/25 ºC of the rectified spirit by means of the specific gravity bottle. B.3.8 Calculation M1d Specific gravity at 25 ºC/25 ºC = M M where, 1-2 M 1 = Mass in g of the material in air, d = Specific gravity of rectified spirit, and M 2 = Mass in g of the material in rectified spirit. EAC 2010 All rights reserved 9

14 Annex C (normative) Determination of refractive index C.1 Apparatus C.1.1 Abbe Refractometer with a thermostatically controlled water bath at 75 ± 0.1 C and an arrangement to circulate water through the instrument. The instrument should be standardized, following the manufacturer s instructions, with a liquid of known purity and refractive index, or with a glass prism of known refractive index. Distilled water which has a refractive index of at 20.0 C is a satisfactory liquid for standardization. C.1.2 Light source If the refractometer is equipped with a compensator, a tungsten lamp or a daylight bulb may be used. Otherwise, monochromatic light, such as an electric sodium vapour lamp, should be used. A.2.2 Procedure Melt the material and filter it through a filter paper to remove any impurities and the last traces of moisture. Make sure that the sample is completely dry. Adjust the temperature of the refractometer to 75.0 ± C by circulating water from the water-bath. Ensure that the prisms are clean and completely dry, and then place a few drops of the sample on the lower prism. Close the prisms, tighten firmly with the screw-head and allow to stand for one or two minutes. Adjust the instrument and the light to obtain the most distinct reading possible and determine the refractive index. 10 EAC 2010 All rights reserved

15 Procedure Annex D (normative) Determination of matter insoluble in benzene CD/K/650:2010 Agitate 5 g of beeswax with 100 ml of pure benzene until no more will dissolve. Heat to 60 C to promote further dissolution and coagulate the insoluble matter. Allow to cool without further disturbance for three hours. Filter the insoluble matter on a sintered glass crucible and wash with benzene. Dry on a boiling water bath for two hours and express the result in percent by mass. EAC 2010 All rights reserved 11

16 Annex E (normative) Determination of acid value E.1 Procedure E.1.1 E.1.2 E.1.3 Accurately weigh 3 g of wax and place in a 200 ml flask. Add 25 ml of neutralized dehydrated alcohol and warm until melted. Shake the mixture and add 1 ml of phenolphthalein indicator solution. E.1.4 Tiltrate the warm liquid with 0.5 N alcoholic potassium hydroxide solution until a permanent, faint pink colour is obtained. E.2 Calculation Acid value = where, V = N = M = 56.1 V N M volume in ml of standard potassium hydroxide solution used, normality of standard potassium hydroxide solution, mass in g of the wax taken for the test. 12 EAC 2010 All rights reserved

17 F.1 Procedure Annex F (normative) Determination of ester value CD/K/650:2010 F.1.1 To the solution resulting from the determination of acid value add ml of 0.5 N alcoholic potassium hydroxide and 50 ml of aldehyde-free alcohol. F.1.2 F.1.3 F.1.4 Reflux the mixture for 4 hours. Tiltrate the excess alkali with 0.5 N hydrochloric acid. Perform a blank determination. F.1.5 The difference between the volumes, in ml, of 0.5N hydrochloric acid consumed in the actual test and in the blank test, multiplied by and divided by the weight in g of the specimen taken, is the ester value. EAC 2010 All rights reserved 13

18 Annex G (normative) Determination of matter soluble in water G.1 Apparatus G.1.1 C.1.2 G.1.3 G.1.4 Evaporating dish, 10 cm diameter and 5 cm deep. Measuring flask, 250 ml Boiling water-bath Oven, at 100 ± 2 C. G.2 Procedure G.2.1 Take 5 g of the material in 500 ml beaker and add to it 100 ml of distilled water (see IS 1070:1992), boil and stir thoroughly. Cover the beaker with a watch-glass and allow it to stand for 4 hours at room temperature with occasional stirring. Filter into a 250 ml measuring flask. Wash the residual sample and the filter paper with distilled water (see IS 1070:1992) and make up the volume. Transfer a measured volume of the filtrate into a weighed evaporating dish and evaporate to dryness over a boiling water bath. Dry the residue to constant mass in an oven maintained at 100 ± 2 C. G.3 Calculation G.3.1 Matter soluble in water, percent by mass = where M 1 = mass, in g, of the residue; V = volume in ml ofthe filtrate taken; and M 2 = mass, in g, of the sample taken. M , V M 14 EAC 2010 All rights reserved 2

19 H.1 Outline of the method Annex H (normative) Determination of saponification value CD/K/650:2010 The wax is saponified by refluxing with a known excess of alcoholic potassium hydroxide solution. The alkali consumed for saponification is determined by tiltrating the excess alkali with standard acid. H.2 Apparatus H.2.1 H.2.2 Conical Flasks 250 ml to 300 ml made of alkali resistant glass. Reflux Air Condenser At least 65 cm long. H.3 Reagent H.3.1 H.3.2 Methyl ethyl ketone Stored in a dark place. Rectified spirit Neutral to phenolphthalein indicator. H.3.3 Alcoholic potassium hydroxide solution Dissolve 30 g of potassium hydroxide in rectified spirit and make up to 1 litre. Allow to settle overnight in a dark place, decant the clear liquid and keep in a bottle closed tight with a cork or rubber stopper. H.3.4 Phenolphthalein indicator solution Same as E.1.4 H.3.5 Standard hydrochloric acid 0.5 N. H.4 Procedure H.4.1 H.4.2 H.4.3 H.4.4 H.4.5 Weigh accurately about 2 g of the wax in a tarred conical flask. Add 25 ml of methyl ketone, followed by 25 ml of alcoholic potassium hydroxide solution. Add a few pieces of pumice stone and connect the reflux air condensed to the flask. Heat the flask on a water-bath or electric hot-plate for about 2 hours. Boil steadily but gently. H.4.6 After the flask and condenser have cooled, wash down the inside of the condenser with about 10 ml of rectified spirit. H.4.7 acid. H.4.8 H5 where, Add about 1 ml of phenolphthalein indicator solution and tiltrate with standard hydrochloric Carry out a blank determination at the same time. Calculation 56.1( B - S) N Saponification value = M B = S = N = M = volume in ml of the standard hydrochloric acid. Required for the blank, volume in ml of standard hydrochloric acid required for the wax, normality of standard hydrochloric acid, and mass in g of the wax taken for the test. EAC 2010 All rights reserved 15

20 Annex J (normative Determination of iodine vale (Wijs method) J.1. Procedure J.1.1 To a 500 ml iodine flask transfer an accurately weighed quantity, in g, of the substance to be tested about equal to that calculated by the formula 25/I, in which I is the Iodine Value, except that, for substances having iodine values not greater than 2.5, take about 10 g accurately weighed, for the test. J.1.2 Dissolve the test sample in 20 ml of carbon tetrachloride then add 25 ml of iodochloride. Insert the stopper securely in the vessel, and allow to stand at 25 ºC ± 5 ºC for 30 minutes, protected from light, with occasional shaking. J.1.3 Add, in the order named, 20 ml of potassium iodide (150 g/l) tiltrate the liberated iodide with 0.1 N sodium thiosulfate, shaking thoroughly after each addition of thiosulfate. J.1.4 When iodide colour becomes quite pale, add 3 ml of starch and continue the tiltration with 0.1N sodium thiosulfate until the blue colour is discharged. J.1.5 Perform a blank test at the same time with the same quantities of the same reagents and in the same manner. J.1.6 The difference between the volume in ml, of 0.1 N sodium thiosulfate consumed by the blank test and the actual test, multiplied by and divided by the weight in g of the sample taken, is the iodine value. 16 EAC 2010 All rights reserved

21 K.1 Apparatus K.1.1 Annex K (normative) Determination of ash Platinum dish Having a capacity of 100 ml. K.2 Procedure K.2.1 K.2.2 CD/K/650:2010 Heat the platinum dish to redness, cool to room temperature in a dessicator and weigh. Take about 5 g of the material in a watch-glass and weigh accurately. K.2.3 Transfer about three-quarters of this quantity to the platinum dish and heat on a Bunsen burner so that the material burns gently at the surface. When about half of the material is burnt away, stop heating, cool and add the remainder of the material. K.2.4 Weigh the watch-glass again an find, by difference, the exact mass of the sample transferred to the platinum dish. K.2.5 K.2.6 K.2.7 Heat again as before till the material is completely charred. Incinerate in a muffle furnace at 55 ºC to 65 ºC for 1 hour. Cool to room temperature in a dessicator and weigh. K.2.8 Repeat incineration, cooling and weighing until the difference between two successive weighing is less than one milligram. K.3 Calculation of results 100 M Ash, per cent by mass = M where, M 2 = M 1 = 1 2 mass on g of the ash, and mass in g of the material taken for the test. EAC 2010 All rights reserved 17

22 Annex L (normative) Test for fats, fatty acids, Japan wax and rosin L.1 Reagent L.1.1 Sodium hydroxide solution 3.5 N. L.1.2 Dilute hydrochloric acid 1 N. L.2 Procedure L.2.1 Boil 1 g of the wax for 30 minutes with 35 ml of 3.5 N sodium hydroxide contained in a 100 ml beaker maintaining the volume by the occasional addition of water. L.2.2 Allow the mixture to cool at room temperature for about 2 hours. The wax separates, leaving the liquid clear, turbid, or translucent but not opaque. L.2.3 Filter the cool mixture, and acidify the clear filtrate with dilute hydrochloric acid. L.2.4 The wax will have passed the test if the liquid remains clear or shows not more than a slight amount of turbidity or precipitate. 18 EAC 2010 All rights reserved

23 M.1 General requirements of sampling Annex M (normative) Sampling of beeswax, crude and refined CD/K/650:2010 In drawing, preparing, storing and handling samples, the following precautions and directions shall be observed. M.1.1 M.1.2 Samples shall be taken in a protected place not exposed to damp air, dust or soot. The sampling instrument shall be clean and dry when used. M.1.3 Precautions shall be taken to protect the samples, the material being sampled, the sampling instrument and the containers for the sample from adventitious contamination. M.1.4 The samples shall be placed in clean and dry glass containers. M.1.5 Each container shall be sealed air-tight after filling and marked with full details of sampling, batch or code number, name of the manufacturer, and other important particulars of the consignment. M.1.6 Samples shall be stored in such a manner that the temperature of the material does not vary unduly from the normal temperature. M.2 Scale of sampling M.2.1 Lot All the containers in a single consignment of the same material drawn from a single batch of manufacture shall constitute a lot. If the consignment is declared to consist of different batches of manufacture, the batches shall be marked separately and the groups of containers in each batch shall constitute a separate lot. M Samples shall be tested for each lot for ascertaining the conformity of the material to the requirement of this specification. M.2.2 The number of containers to be selected from the lot shall depend on the size of the lot and shall be in accordance with col. 1 and 2 of Table 2. M.2.3 The containers shall be selected at random from the lot and for this purpose a random number table as agreed to between the purchaser and the supplier shall be used. If such a table is not available, the following procedure shall be adopted: Starting from any container in the lot, count them as 1, 2, 3 up to r in a systematic manner, where r is equal to the integral part of N/n, N being the total number of containers in the lot and n the number of containers to be chosen (see Table 2). Every rth container thus counted shall be separated until the requisite number of containers is obtained from the lot to give samples for test. M.3 Test samples and referee samples M.3.1 Preparation of individual samples Draw with suitable sampling instrument equal quantities of the material from different parts of the container till 500 g of the material is drawn and divide it into three equal parts. Each part so obtained shall constitute an individual sample representing the container and shall be transferred immediately to thoroughly cleaned and dry containers, sealed air-tight and marked with particulars given under EAC 2010 All rights reserved 19

24 M.1.5. The individual sample so obtained shall be divided into three sets in such a way that each set has a sample representing each selected container. One of these shall be marked for the purchaser, another for the vendor and the third for the referee. M.3.2 Preparation of Composite Sample From the material from each of the selected container, remaining after the individual sample has been taken, approximately equal quantities of the material shall be taken and mixed together so as to form a composite sample weighing 150 g. This composite sample shall be divided into three equal parts and transferred to clean and dry containers, sealed air-tight and labelled with particulars as given in M.1.5. One of these composite samples shall be for the purchaser, another for the vendor and the third for the referee. M.3.3 Referee samples Referee samples shall consist of a set of individual samples (M.3.1) and a composite sample (M.3.2) marked for this purpose and shall bear the seals of the purchaser and the vendor. These shall be kept at a place as agreed to between the two. M.4 Number of tests M.4.1 Test for melting point, total volatile matter, ash and sulphated ash shall be conducted on each of the samples constituting a set of individual samples. M.4.2 Test for specific gravity, refractive index at 75 C, acid value, saponification value and iodine value, matter insoluble in benzene and matter soluble in water shall be conducted on the composite sample. M.5 Criteria for conformity M.5.1 A lot shall be declared to have satisfied all the requirements of this specification when conditions given in M to M are satisfied. M The test results on each of the individual samples for melting point, total volatile matter, ash and sulphated ash shall satisfy the corresponding requirements as specified in Table 1. M The test results on the composite sample for the characteristics as mentioned in M.4.2 shall satisfy the corresponding requirements as given in Table 1. Table 2 Number of containers to be selected for sampling Lot size N No. of containers to be selected n Up to to to to and above 9 20 EAC 2010 All rights reserved

25 EAC 2010 All rights reserved