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

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1 EAST AFRICAN STANDARD Domestic mustard seed Specification and grading EAST AFRICAN COMMUNITY HS CD/K/471:2010 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/471:2010 In the preparation of this East African Standard, the following sources were consulted extensively: ISO 1237:1981, Mustard seed Specification Domestic mustard seed, Official Grain Grading Guide, August 1, 2009, Canadian Grain Commission CODEX STAN 193:1995 (Rev.5:2009), General Standard for Contaminants and Toxins in Foods CODEX STAN 228:2001 (Rev.1:2004), General methods of analysis for contaminants Codex Alimentarius website: USDA Foreign Agricultural Service website: USDA Agricultural Marketing Service website: USDA Plant Inspectorate Service website: Grain Inspection, Packers and Stockyards Administration: European Union: Assistance derived from these sources and others inadvertently not mentioned is hereby acknowledged. This standard has been developed to take into account: the needs of the market for the product; the need to facilitate fair domestic, regional and international trade and prevent technical barriers to trade by establishing a common trading language for buyers and sellers. the structure of the CODEX, UNECE, USA, ISO and other internationally significant standards; the needs of the producers in gaining knowledge of market standards, conformity assessment, commercial cultivars and crop production process; the need to transport the product in a manner that ensures keeping of quality until it reaches the consumer; the need for the plant protection authority to certify, through a simplified form, that the product is fit for crossborder and international trade without carrying plant disease vectors; the need to promote good agricultural practices that will enhance wider market access, involvement of small-scale traders and hence making farming a viable means of wealth creation; and the need to ensure a reliable production base of consistent and safe crops that meet customer requirements. Promotion of standardization and grading of agricultural commodities is an important aspect of agricultural marketing. The agricultural commodities are heterogeneous and hence it is very essential to grade these commodities as per standards to command better price either at domestic or international market. Sale of Mustard and Rapeseed is offered on the basis of variety, wholesomeness, appearance, colour, presence of foreign matter, damaged seeds, broken seeds, admixture of inferior variety, moisture, harmful contaminants, etc. A quality grain is that which meets the end user specifications with respect to range of pre-determined Quality and Safety standards. EAC 2010 All rights reserved iii

4 This standardl has been designed with the objectives to i. Create awareness about standards prescribed by various organizations for domestic and international markets so as to raise quality consciousness among the farmers, entrepreneurs and other market functionaries with the objective to equip them better to face the global competition in the post WTO era. ii. iii. provide details of various parameters responsible for quality; and describe the advantages of grading & standardization so that farmers may get prices commensurate with the quality produced by them. Following Parameters are important in determination of quality of mustard Foreign matter Dead,badly discoloured and damaged Unripe shriveled and slightly damaged Small atrophied seeds Admixture of other varieties of mustard Moisture content Following safety parameters are important: Pesticides residue Poisonous metals Parameters by which grades of mustard is differentiated Important parameters by which grades can be differentiated in case of mustard are Foreign matter Dead /badly discoloured and damaged seeds Unripe shriveled and slightly damaged seeds Small atrophied seeds Admixture of other varieties of mustard iv EAC 2010 All rights reserved

5 Contents CD/K/471: Scope Normative references Definitions and description Essential composition and quality factors Basis of determination Representative portion of domestic mustard for grading, grams General quality requirements Classification Unclassified mustard seeds Reject mustard seeds Contaminants Pesticide residues Heavy metals Mycotoxin and chemical limits Environment Hygiene Packaging Marking or labelling Sampling Annex A (normative) Determination of impurities, size, foreign odours, insects, and species and variety Annex B (normative) Determination of moisture content Annex C (informative) Determination of loss in mass at 103 C Annex D (informative) Determination of allyl isothiocyanate Annex E (informative) Determination of ρ-hydroxybenzyl isothiocyanate (Colorimetric method) Annex F (informative) Determination of ρ-hydroxybenzyl isothiocyanate (Argentimetric method) Annex G (informative) Recommendations relating to storage and transport Annex H (informative) Model certificate of conformity with standards for farm produce Annex I (normative) Mustard seed Fact sheet Annex J (informative) Mustard seed Codex, EU and USA pesticide residue limits Annex K (informative) Sieves for assessing dockage and grading factors EAC 2010 All rights reserved v

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7 EAST AFRICAN STANDARD CD/K/471:2010 Domestic mustard seed Specification and grading 1 Scope This East African Standard specifies the quality and grading requirements and methods of test for domestic mustard seed of cultivated varieties (cultivars) grown from: Sinapis alba Linnaeus White mustard, yellow mustard; Brassica nigra (Linnaeus) W.D.J Koch Black mustard; Brassica juncea (Linnaeus) Czernajew and Cosson in Czernajew Indian mustard. 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. ISO 605, Pulses Determination of impurities, size, foreign odours, insects, and species and variety Test methods ISO 711, Cereals and cereal products Determination of moisture content (Basic reference method) ISO 712, Cereals and cereal products Determination of moisture content Routine reference method ISO 5223, Test sieves for cereals ISO , Cereals and pulses Determination of hidden insect infestation Part 1: General principles ISO , Cereals and pulses Determination of hidden insect infestation Part 2: Sampling ISO , Cereals and pulses Determination of hidden insect infestation Part 3: Reference method ISO , Cereals and pulses Determination of hidden insect infestation Part 4: Rapid methods ISO 13690, Cereals, pulses and milled products Sampling of static batches ISO 16050, Foodstuffs Determination of aflatoxin B 1, and the total content of aflatoxin B 1, B 2, G 1 and G 2 in cereals, nuts and derived products High performance liquid chromatographic method CAC/RCP 1, Recommended international code of practice General principles of food hygiene EAS 38, Labelling of prepackaged foods Specification EAS 79, Cereals and pulses as grain Methods of sampling EAS 217, Methods for the microbiological examination of foods ISO 22000:2005, Food safety management systems Requirements for any organization in the food chain OIML R87:2004, Quantity of product in prepackages EAC 2010 All rights reserved 1

8 3 Definitions and description For the purpose of this East African Standard, the following definitions shall apply. 3.1 classes domestic mustard seed is classed as yellow, brown or oriental, or mixed. The class forms part of the grade name. Table 1 Identifying classes of domestic mustard seed Class Colour Approximate Shape Surface size Yellow Light creamy-yellow to yellow Occasional 2 to 3 mm in diameter Spherical or oval Textured, similar to an orange peel, hilum area small white spot on a seed is light or deep yellow to light tan circular area yellowish brown Brown Reddish-brown to 2 mm or less in Spherical or Predominant netting, ridges are dark-brown diameter oval thicker than oriental mustard, hilum area white on a black or darker brown circular area Oriental Predominantly 1.2 to 2.0 mm in Oval Predominant netting, not as yellow to darkyellow, width, 1.6 to 3.0 predominant as brown mustard, with some seeds ranging from light brown to brown in length ridges are fine, hilum area white on a darker yellow to lighter brown circular area Mixed Yellow and brown mustard seed containing less than 90.0% of one class See also Domestic mustard seed, oriental: Other classes 3.2 dockage all matter other than mustard seed that can be removed from the original sample by use of an approved device according to prescribed procedures. Dockage includes Material remaining on top of the round-hole hand sieve Material passing through the slotted hand sieve Material passing over the No. 000 riddle Material removed by aspiration Material removed by Cleaning for grade improvement 3.3 commercially clean primary samples commercially clean primary samples can have up to 0.5% for broken and reasonably sound mustard seed deducted from the gross weight of the dockage. Primary samples are considered commercially clean when the net dockage does not exceed 2.5% of the sample weight. 3.4 not commercially clean primary samples In not commercially clean primary samples, there is no allowance for broken and reasonably sound mustard seed. All the material removed by the slotted sieve is assessed as dockage. 3.5 net weight of sample the sample after cleaning and removal of dockage is referred to as the cleaned sample. Its weight is the net weight of the sample. Percentages by weight for grading refer to percentages of net weight. 3.6 kernel counts To do kernel counts you must have 500 grams of cleaned sample. All grading is done on representative portions divided down from the cleaned sample using a Boerner-type divider. 2 EAC 2010 All rights reserved

9 3.7 gross weight sample the sample as it arrives is referred to as the uncleaned sample. Its weight is the gross weight of the sample. 3.8 hazardous substances in samples any pesticide, herbicide or desiccant 3.9 cleaning for grade improvement if the grade of a delivery can be improved by additional cleaning, perform the cleaning and add the additional material to dockage. Cleaning for grade improvement can be done at any time. See Table 2. Table 2 Cleaning for grade improvement domestic mustard seed Material to be removed Equipment Effect on composition of dockage Excessive inseparable weed seeds or damaged mustard Spiral cleaner on request, for yellow mustard seed only Carter dockage tester set as follows: Not more than about 5.0% of domestic mustard seed may be seeds for all classes of Feed control #3 removed for each grade mustard seed Air control #7 improvement achieved. NOTE The material Riddle No. 000 originally removed by aspiration is to be Top sieve No. 4.5 or No. 5 reconstituted back into the round-hole sample prior to cleaning for Centre sieve blank tray improvement. Bottom sieve none Sieve cleaner control off Canola or wild Carter dockage tester set as follows: The material passing mustard in yellow Feed control #3 through the sieve is mustard seed Air control off included in the dockage. Riddle No. 000 Not more than 5.0% of Top sieve none sound domestic mustard Centre sieve No. 4.5 or No. 5 seed may be removed round-hole for each grade Bottom sieve blank tray improvement achieved. Sieve cleaner control off 3.10 contaminated grain grain containing any substance in sufficient quantity that the grain is unfit for consumption by persons or animals or is adulterated within the meaning of the regulations on food safety 3.11 crush one pass of the roller under firm pressure over a 100-seed stick on masking tape 3.12 blotched seeds Blotched seeds are oriental mustard seeds with black or brown discolourations on the seed coat. Seeds only partly discoloured but otherwise sound are considered sound, but the discolouration is taken into account in the evaluation of colour. See Colour. Seeds completely discoloured by blotch are considered damaged. See Damage canola in brown and oriental mustard, canola is classed as inconspicuous admixture. In yellow mustard seed, EAC 2010 All rights reserved 3

10 canola is classed as Distinctly detrimental cockle cockle, or cow cockle, is a hard roundish seed with a dull surface covered with numerous small bumps giving the seed a rough spiky appearance. Colour can be deep black, bluish-black or orangish-brown. In oriental mustard, cockle is part of Conspicuous admixture colour In analysing colour, consider The general degree of maturity The amount and degree of discolouration, such as from weathering The proportion of damaged seeds, which are distinctly green or otherwise colour-damaged. See Damage and Distinctly green. The amount of rime light rime is considered in the overall appearance of the sample. See Damage conspicuous admixture Conspicuous admixture is called Conspicuous inseparable seeds in the grade determinants tables. In brown and oriental mustard, conspicuous admixture includes Small seeds or broken seeds of other grains Weed seeds such as cow cockle, lamb s-quarters, ball mustard, pigweed, cleavers, smartweed and lady s-thumb. Any conspicuous foreign material except stones and soft earth pellets In yellow mustard seed, conspicuous admixture includes Seeds and foreign material designated as distinctly detrimental. See Distinctly detrimental Small seeds and broken kernels of other grains Weed seeds such as pigweed, lady s-thumb, lamb s-quarters and smartweed Any conspicuous foreign material except stones and soft earth pellets 3.17 damaged seeds Damaged seeds include those that are Distinctly shrunken or shrivelled Badly discoloured from mould Completely and densely covered with rime or dried white mucilage. See Colour. Excessively weathered, sprouted, distinctly green, heated or otherwise damaged 3.18 distinctly detrimental Admixtures considered distinctly detrimental include Cow cockle Sclerotinia Admixtures considered distinctly detrimental in yellow mustard seed include Cow cockle Sclerotinia Wild mustard, canola/rapeseed Other distinctly detrimental seeds (see Other distinctly detrimental seeds) o Ball mustard Stinkweed or pennycress o Cleavers Tansy mustard o Cockle Tumbling mustard o Dog mustard Wild buckwheat o Hare s ear mustard Wormseed mustard o There are separate distinctly detrimental tolerances for cow cockle, sclerotinia and wild mustard in combination with canola or rapeseed and other distinctly detrimental seeds. All 4 EAC 2010 All rights reserved

11 listed are included in the total of distinctly detrimental and total of conspicuous inseparable seeds distinctly green distinctly green tolerances are applied to crushed seeds which are a distinct green throughout. Pale green or immature seeds are taken into account in the evaluation of colour. See Colour earth pellets Hard earth pellets are pellets that do not crumble under light pressure. See Stones. Soft earth pellets are pellets that crumble under light pressure. See Soft earth pellets ergot sclerotia (sclerotium, in singular) of the fungus, Claviceps species, which are associated with some seeds other than canola where the fungal organism has replaced the seed. A plant disease producing elongated fungal bodies that have a purplish-black exterior, a purplish-white to off white interior, and a relatively smooth surface texture fertilizer pellets fertilizer pellets are typically either small, round and white or irregular shaped and pink or red. Fertilizer pellets are not considered a hazardous substance however there is no visible means of assuring that material resembling fertilizer pellets is not some other contaminant. Fertilizer pellets are considered as a separate grading factor in all grades of domestic mustard seed fireburnt Samples that show any evidence of being charred or scorched by fire are considered fireburnt. Evidence includes odour, pieces of charred wood, and so on. Fireburnt seeds pop when crushed foreign matter foreign material in flaxseed includes anything that is not mustard seed, such as stones, ergot, sclerotinia, etc 3.25 heated-damaged kernels Heated refers only to seeds that are distinctly heated or badly binburnt. Heated seeds have a heated odour. Crushed seeds may be Black badly binburnt Dark chocloate brown distinctly heated Light tan slightly damaged from oxidation. If they have an odour or are present with brown or black crushed seeds, they are considered heated. Otherwise, they are included in Total damage, not heated inconspicuous admixture In brown mustard seed and oriental mustard only, inconspicuous admixture includes Canola Common wild mustard seed Any other seeds that blend with brown or oriental mustard seed and are not readily identified 3.27 mixed classes samples are designated mixed classes when they contain sufficient quantities of other classes of mustard seed. See Other classes inert material mineral matter such as stones, coal shale and hard and soft earth pellets EAC 2010 All rights reserved 5

12 3.29 moisture water content in mustard seed as determined by an approved device and procedures 3.30 odour there is no numeric tolerance for odour. Consider The basic quality of the sample The type and degree of the odour The presence of visible residue causing the odour 3.31 other classes If a sample contains more than 10.0% other classes, it is designated Mixed. Mixed mustard seed is graded according to all specifications except other classes. In brown mustard seed, other classes are yellow and oriental mustard seed. Other classes of domestic mustard seed in oriental mustard seed are yellow or brown. Other classes of domestic mustard seed in yellow mustard seed are brown and oriental mustard seed other distinctly detrimental seeds In yellow domestic mustard seed, the seeds listed below are considered Other distinctly detrimental seeds. Ball mustard Cleavers Cockle Dog mustard Hare s ear mustard Stinkweed or pennycress Tansy mustard Tumbling mustard Wild buckwheat Wormseed mustard IMPORTANT! Grain inspectors are authorized to withhold grades on samples with unidentifiable admixtures until results of analysis are confirmed by seed analysts poisonous, toxic and/or harmful seeds any seed which if present in quantities above permissible limit may have damaging or dangerous effect on health, organoleptic properties or technological performance such as Jimson weed dhatura (D. fastuosa Linn and D. stramonium Linn.) corn cokle (Agrostemma githago L., Machai Lallium remulenum Linn.) Akra (Vicia species), Argemone mexicana, Khesari and other seeds that are commonly recognized as harmful to health 3.34 rime Rime is the lining of the pod adhered to the seed. Seeds that are completely and densely covered with white rime are classed as damaged in any grade. Seeds with light rime sparsely covering the seed coat are Classed as sound if not otherwise damaged Considered in the evaluation of colour. See Colour Sclerotia (sclerotium, singular) dark colored or black resting bodies of the fungi Sclerotinia and Claviceps 6 EAC 2010 All rights reserved

13 3.36 Sclerotinia genus name which includes the fungus Sclerotinia sclerotiorum which produces sclerotia. The sclerotia vary in size and shape, have a course surface texture, vary in exterior color from dark black to grey to white and have a pure white interior soft earth pellets Soft earth pellets are pellets that crumble under light pressure if they do not crumble, they are considered stones. These pellets can be Earth and fertilizer pellets Any non-toxic material of similar consistency IMPORTANT! In domestic mustard seed, fertilizer pellets are not considered soft earth pellets. See Fertilizer pellets stones hard shale, coal, hard earth pellets, and any other non toxic materials of similar consistency. Fertilizer pellets are assessed as stones when constituting 1.0% or less of the net sample weight. NOTE Fertilizer pellets are not assessed as stones in samples of Domestic Mustard Seed. See Fertilizer pellets treated seed and other chemical substances (a) Treated seed is grain that has been coated with an agricultural chemical for agronomic purposes. These seed dressings contain a dye to render the treated seed visually conspicuous. The colour of the dye varies depending upon the type of treatment and the type of grain. The coatings or stains may appear greasy or powdery and surface area distribution ranges from tiny flecks to complete coverage. (b) Other chemical substances refers to any chemical residues either adhering to the kernel or remaining in the sample and to samples having a chemical odour of any kind variety domestic mustard seed is graded without reference to variety 3.41 wild mustard In brown and oriental mustards, wild mustard seeds are classed as Inconspicuous admixture. In yellow mustard, wild mustard seeds are classed as Distinctly detrimental. IMPORTANT! Grain inspectors are authorized to withhold grades on samples with unidentifiable admixtures until results of analyses are confirmed by seed analysts. 4 Essential composition and quality factors 4.1 Basis of determination Other determinations not specifically provided for under the general provisions are made on the basis of the grain when free from dockage, except the determination of odour is made on either the basis of the grain as a whole or the grain when free from dockage. 4.2 Representative portion of domestic mustard for grading, grams All grading is done on representative portions divided down from the cleaned sample, using a Boerner-type divider. EAC 2010 All rights reserved 7

14 Table 3 Representative portion of domestic mustard, brown for grading, grams Grading factor Minimum Optimum Export Canola Cockle Colour working sample working sample working sample Conspicuous admixtures Damage Distinctly detrimental Distinctly green 5 crushes 10 crushes 10 crushes Ergot Excreta working sample working sample working sample Fertilizer pellets Fireburnt working sample working sample working sample Heated 5 crushes 10 crushes 10 crushes Inconspicuous admixture Odour working sample working sample working sample Other classes Rime Sclerotinia sclerotiorum Soft earth pellets 100 working sample working sample Stones 100 working sample working sample Wild mustard seed Table 4 Representative portion of domestic mustard, oriental for grading, grams Grading factor Minimum Optimum Export Blotched seeds Canola Cockle Colour working sample working sample working sample Conspicuous admixture Damage Distinctly detrimental Distinctly green 5 crushes 10 crushes 10 crushes Ergot Excreta working sample working sample working sample Fertilizer pellets Fireburnt working sample working sample working sample Heated 5 crushes 10 crushes 10 crushes Inconspicuous admixture Odour working sample working sample working sample Other classes Rime Sclerotinia sclerotiorum Soft earth pellets 100 working sample working sample Stones 100 working sample working sample Wild mustard seed Table 5 Representative portion of domestic mustard, yellow for grading, grams Grading factor Minimum Optimum Export Canola Cockle Colour working sample working sample working sample Conspicuous admixture Damage Distinctly detrimental Distinctly green 5 crushes 10 crushes 10 crushes Ergot Excreta working sample working sample working sample Fertilizer pellets Fireburnt working sample working sample working sample Heated 5 crushes 10 crushes 10 crushes Odour working sample working sample working sample Other classes Other distinctly detrimental seeds Rime Sclerotinia sclerotiorum Soft earth pellets 100 working sample working sample Stones 100 working sample working sample Wild mustard seed EAC 2010 All rights reserved

15 4.3 General quality requirements CD/K/471: Mustard shall meet the following general requirements/limits as determined using the relevant standards listed in Clause 2. Mustard seeds a) shall consist of dry grains of: Sinapis alba Linnaeus White mustard, yellow mustard; Brassica nigra (Linnaeus) W.D.J Koch Black mustard; Brassica juncea (Linnaeus) Czernajew and Cosson in Czernajew Indian mustard. b) be sweet, hard, clean, wholesome, uniform in size, shape, colour and in sound merchantable condition; c) shall be free from a substance which renders it unfit for human or animal consumption or processing into or utilisation thereof as food or feed; d) shall be free of pests, live animals, animal carcasses, animal droppings, fungus infestation, added colouring matter, moulds, weevils, obnoxious substances, glass, metal, coal, dung, discoloration and all other impurities except to the extent indicated in this standard and must meet any other phytosanitary requirements specified by the importing country authority; e) shall be free from filth (impurities of plant and animal origin including insects, rodent hair and excreta) in amounts that represent a hazard to human health; f) shall be free from toxic or noxious seeds that are commonly recognized as harmful to health; g) shall be free from abnormal flavours, musty, sour or other undesireable odour, obnoxious smell and discolouration; h) shall be free from micro-organisms and substances originating from micro-organisms or other poisonous or deleterious substances in amounts that may constitute a hazard to human health. i) shall contain no chemical residues which exceed the prescribed maximum residue limit: Provided that: (i) (ii) if the prescribed maximum residue limit of an importing country is lower than is permissible, the prescribed maximum residue limit of the importing country shall be complied with; and the Food Safety Authority may grant permission for mustard seed with a higher maximum residue limit, to be exported to countries where this higher residue limit is permissible: Provided that the export documents are accordingly endorsed with the name of the importing country; j) shall contain not more than 10 microgram per kilogram aflatoxin of which not more than 5 microgram per kilogram may be aflatoxin B1: Provided that: (i) (ii) (iii) if the prescribed maximum aflatoxin limit of an importing country is lower than is permissible, the prescribed maximum aflatoxin limit of the importing country shall be complied with; the Food Safety Authority may grant permission for mustard seed with a higher maximum aflatoxin content to be exported to countries where this higher aflatoxin limit is permissible: Provided that the export documents are accordingly endorsed with the name of the importing country; and an inspector shall verify compliance to the levels of aflatoxin by sampling and submitting samples for analysis of only certain consignments according to a risk-based plan. EAC 2010 All rights reserved 9

16 k) shall comply with the requirements for declared plant injurious organisms of phytosanitary importance as determined by the plant health protection agency Mustard seeds shall be in form of well-filled seeds of uniform colour If mustard seeds are presented in bags, the bags shall also be free of pests and contaminants. In addition the mustard seeds shall comply with any conditions set by the importing country authority If mustard seeds are rejected because pests or contaminants are found in inspected samples, the mustard seeds are not to be re-presented for inspection unless they have been treated or cleaned Blending of rejected mustard seeds is not permitted as a treatment for insect infestation or as a method of cleaning for contaminants for which there is a nil tolerance Brushing the outside of bags is not permitted as a remedy to remove pests or contaminants. 4.4 Classification Mustard seeds shall be classified into four grades on the basis of the tolerable limits established in Table 6, Table 7 and Table 8 which shall be additional to the general requirements set out in this standard. 4.5 Unclassified mustard seeds Shall be mustard seeds which do not fall within the requirements of Grades 1, 2, 3 or 4 of this standard but are not rejected mustard seeds. 4.6 Reject mustard seeds Reject mustard seeds are those that: (a) (b) (c) (d) Does not meet the requirements for the Grades Nos. 1, 2, 3 or 4; or Contains 8 or more stones which have an aggregate weight in excess of 0.2 percent of the sample weight, 2 or more pieces of glass, 3 or more crotalaria seeds (Crotalaria spp.), 2 or more castor beans (Ricinus communis L.), 4 or more particles of an unknown foreign substance(s) or a commonly recognized harmful or toxic substance(s), 10 or more rodent pellets, bird dropping, or equivalent quantity of other animal filth per 1065 ml to 1183 ml of mustard seed; or Has a musty, sour, or commercially objectionable foreign odor (except smut or garlic odor), or Is heating or otherwise of distinctly low quality. 10 EAC 2010 All rights reserved

17 Table 6 Specific requirements for domestic mustard seed, brown CD/K/471:2010 Parameter Specification Method of Grade 1 Grade 2 Grade 3 Grade 4 test Physical and Chemical Parameters Description Brown mustard seed tended for delivery shall be free from any uncharacteristic odours, live stored product insect infestation and any nominated commercially unacceptable contaminant Oil 42% base level 42% base level 42% base level 42% base level 1.5% premium or deduction for each 1% above or below 42% Moisture, max (%) ISO 711/ % max for immediate processing -if accepted over the maximum, 2% deduction for each 1% over maximum. For storage -if accepted over the maximum, 1.5% deduction for each 1% over maximum plus a drying charge Free fatty acid 2% deduction for each 1% over base level, rejectable over 2.5% 1.0% base level 1.5% base level 1.5% base level 1.5% base level Standard of quality Minimum test weight kg/hl n/a n/a n/a n/a Rejectable if under this limit Degree of soundness Reasonably well matured, sweet, good natural colour Fairly well matured, sweet, reasonably good colour May have the natural colour associated with lowquality seed not any odour that would indicate serious deterioration May have the natural colour associated with lowquality seed not any odour that would indicate serious deterioration Other classes, % by mass, max Protein n/a n/a n/a n/a Seed Retention n/a n/a n/a n/a Germination n/a n/a n/a n/a Inconspicuous admixture, % by mass, max Defective mustard seed (Max % Distinctly green wt/wt based on cleaned 0.5L sample Heated retained above 1.0mm round hole sieve) Total Conspicuous Distinctly Cow cockle inseparable seeds, detrimental Sclerotinia % by mass, max Total Total Broken or split, % by mass, max Unripe, shriveled & slightly damaged, % by mass, max Small atrophied seeds, % by mass, max Foreign matter, % Ergot by mass, max. Excreta 1K 1K 1K 1K Soft earth pellets Stones Total Inconspicuous admixture, % by mass, max Seed Type 1 (Alligator Weed, Giant Sensitive Nil Nil Nil Nil Contaminants (maximum tolerance per half litre to Plant, Parthenium Weed, Saffron Thistle, Star Burr, Stinkwort, St. Johns Wort, Jute, Mexican Poppy) Type 2 (Castor oil plant, coriander, darling Nil Nil Nil Nil apply to individual seeds, pea, ragweed, rattlepod, opium poppy, crow garlic) Type 3 (a) (Cape Tulips, Dodder, Burrs rejectable over) (Xanthium spp.) all except where otherwise stated, Wild Mignonette, Thornapple) Type 3 (c) (Common Heliotrope,) Type 4(a) (Skeleton Weed, Darnel, Hexham Scent, Mintweed, Nightshade) Type 5 (Sesbania pea) Contaminants Chemicals not approved for mustard seed Nil Nil Nil Nil (Maximum per Total aflatoxin (AFB1+AFB2+AFG half litre unless otherwise +AFG2), ppb Aflatoxin B1 only, ppb stated, Fumonison, Total ppb(fb1 + FB2 + FB3) rejectable over Field Insects unless 10 large per ½ 10 large per ½ Includes Rutherglen bugs, ladybirds, 10 large per ½ litre 10 large per ½ litre deductions are litre litre grasshoppers and wood bugs stated as Field insects 100 small per ½ 100 small per 100 small per ½ litre 100 small per ½ litre applying) All species of aphid and of mites litre ½ litre Snails Nil above screen Nil above Nil above screen Nil above screen Nil tolerance per 2.5L sample for any snails remaining above a 3.0 mm round hole screen. If one snail is found above the screen in the 0.5L sample, then a further four 0.5L samples should be taken. If a snail is found in any one of the subsequent samples, the load is to be rejected. screen Tolerance of 1 snail per 0.5L sample, passing through a 3.0 mm round hole screen. 1 snail per 0.5L below screen 1 snail per 0.5L below screen 1 snail per 0.5L below screen 1 snail per 0.5L below screen Objectionable material (entire load) Nil Nil Nil Nil ISO 605 Other non-objectionable material,% by wt K Number of kernel-sized pieces in 500 g. NOTE The class, whether yellow, oriental, brown or mixed, is added to the grade name. EAC 2010 All rights reserved 11

18 Table 7 Specific requirements for domestic mustard seed, oriental Parameter Specification Method of Grade 1 Grade 2 Grade 3 Grade 4 test Physical and Chemical Parameters Description Oriental mustard seed tended for delivery shall be free from any uncharacteristic odours, live stored product insect infestation and any nominated commercially unacceptable contaminant Oil 42% base level 42% base level 42% base level 42% base level 1.5% premium or deduction for each 1% above or below 42% Moisture, max (%) ISO 711/ % max for immediate processing -if accepted over the maximum, 2% deduction for each 1% over maximum. For storage -if accepted over the maximum, 1.5% deduction for each 1% over maximum plus a drying charge Free fatty acid 2% deduction for each 1% over base level, rejectable over 2.5% 1.0% base level 1.5% base level 1.5% base level 1.5% base level Standard of quality Minimum test weight kg/hl n/a n/a n/a n/a Rejectable if under this limit Degree of soundness Reasonably well matured, sweet, good natural colour Fairly well matured, sweet, reasonably good colour May have the natural colour associated with lowquality seed not any odour that would indicate serious deterioration May have the natural colour associated with lowquality seed not any odour that would indicate serious deterioration Other classes (*), % by mass, max Protein n/a n/a n/a n/a Seed Retention n/a n/a n/a n/a Germination n/a n/a n/a n/a Inconspicuous admixture, % by mass, max Defective mustard seed (Max % Distinctly green wt/wt based on cleaned 0.5L sample Heated retained above 1.0mm round hole sieve) Total Conspicuous Distinctly Cow cockle inseparable seeds, detrimental Sclerotinia % by mass, max Total Total Broken or split, % by mass, max Unripe, shriveled & slightly damaged, % by mass, max Small atrophied seeds, % by mass, max Foreign matter, % Ergot, % by mass, max by mass, max. Excreta, % by mass, max. 1K 1K 1K Soft earth pellets, % by mass, max Stones, % by mass, max Total Inconspicuous admixture, % by mass, max Seed Type 1 (Alligator Weed, Giant Sensitive Nil Nil Nil Nil Contaminants (maximum tolerance per half litre to Plant, Parthenium Weed, Saffron Thistle, Star Burr, Stinkwort, St. Johns Wort, Jute, Mexican Poppy) Type 2 (Castor oil plant, coriander, darling Nil Nil Nil Nil apply to individual seeds, pea, ragweed, rattlepod, opium poppy, crow garlic) Type 3 (a) (Cape Tulips, Dodder, Burrs rejectable over) (Xanthium spp.) all except where otherwise stated, Wild Mignonette, Thornapple) Type 3 (c) (Common Heliotrope,) Type 4(a) (Skeleton Weed, Darnel, Hexham Scent, Mintweed, Nightshade) Type 5 (Sesbania pea) Contaminants Chemicals not approved for mustard seed Nil Nil Nil Nil (Maximum per Total aflatoxin (AFB1+AFB2+AFG half litre unless otherwise +AFG2), ppb Aflatoxin B1 only, ppb stated, Fumonison, Total ppb(fb1 + FB2 + FB3) rejectable over Field Insects unless 10 large per ½ 10 large per ½ Includes Rutherglen bugs, ladybirds, 10 large per ½ litre 10 large per ½ litre deductions are litre litre grasshoppers and wood bugs stated as Field insects 100 small per ½ 100 small per 100 small per ½ litre 100 small per ½ litre applying) All species of aphid and of mites litre ½ litre Snails Nil above screen Nil above Nil above screen Nil above screen Nil tolerance per 2.5L sample for any snails remaining above a 3.0 mm round hole screen. If one snail is found above the screen in the 0.5L sample, then a further four 0.5L samples should be taken. If a snail is found in any one of the subsequent samples, the load is to be rejected. screen Tolerance of 1 snail per 0.5L sample, passing through a 3.0 mm round hole screen. 1 snail per 0.5L below screen 1 snail per 0.5L below screen 1 snail per 0.5L below screen 1 snail per 0.5L below screen Objectionable material (entire load) Nil Nil Nil Nil ISO 605 Other non-objectionable material,% by wt K Number of kernel-sized pieces in 500 g. NOTE The class, whether yellow, oriental, brown or mixed, is added to the grade name. (*) See working tolerance for Other Classes 12 EAC 2010 All rights reserved

19 Table 8 Specific requirements for domestic mustard seed, yellow CD/K/471:2010 Parameter Specification Method of Grade 1 Grade 2 Grade 3 Grade 4 test Physical and Chemical Parameters Description Yellow mustard seed tended for delivery shall be free from any uncharacteristic odours, live stored product insect infestation and any nominated commercially unacceptable contaminant Oil 42% base level 42% base level 42% base level 42% base level 1.5% premium or deduction for each 1% above or below 42% Moisture, max (%) ISO 711/ % max for immediate processing -if accepted over the maximum, 2% deduction for each 1% over maximum. For storage -if accepted over the maximum, 1.5% deduction for each 1% over maximum plus a drying charge Free fatty acid 2% deduction for each 1% over base level, rejectable over 2.5% 1.0% base level 1.5% base level 1.5% base level 1.5% base level Standard of quality Minimum test weight kg/hl n/a n/a n/a n/a Rejectable if under this limit Degree of soundness Reasonably well matured, sweet, good natural colour Fairly well matured, sweet, reasonably good colour May have the natural colour associated with lowquality seed not any odour that would indicate serious deterioration May have the natural colour associated with lowquality seed not any odour that would indicate serious deterioration Other classes, % by mass, max Protein n/a n/a n/a n/a Seed Retention n/a n/a n/a n/a Germination n/a n/a n/a n/a Inconspicuous admixture, % by mass, max Defective mustard seed (Max % Distinctly green wt/wt based on cleaned 0.5L sample Heated retained above 1.0mm round hole sieve) Total Conspicuous Distinctly Cow cockle inseparable detrimental Sclerotinia seeds, % by Wild mustard, mass, max canola/rapeseed Other distinctly detrimental Total Total Broken or split, % by mass, max Unripe, shriveled & slightly damaged, % by mass, max Small atrophied seeds, % by mass, max Foreign matter, % Ergot, % by mass, max by mass, max. Excreta, % by mass, max. 1K 1K 1K Soft earth pellets, % by mass, max Stones, % by mass, max Total Inconspicuous admixture, % by mass, max Seed Type 1 (Alligator Weed, Giant Sensitive Nil Nil Nil Nil Contaminants (maximum tolerance per half litre to Plant, Parthenium Weed, Saffron Thistle, Star Burr, Stinkwort, St. Johns Wort, Jute, Mexican Poppy) Type 2 (Castor oil plant, coriander, darling Nil Nil Nil Nil apply to individual seeds, pea, ragweed, rattlepod, opium poppy, crow garlic) Type 3 (a) (Cape Tulips, Dodder, Burrs rejectable over) (Xanthium spp.) all except where otherwise stated, Wild Mignonette, Thornapple) Type 3 (c) (Common Heliotrope,) Type 4(a) (Skeleton Weed, Darnel, Hexham Scent, Mintweed, Nightshade) Type 5 (Sesbania pea) Contaminants Chemicals not approved for mustard seed Nil Nil Nil Nil (Maximum per Total aflatoxin (AFB1+AFB2+AFG half litre unless otherwise +AFG2), ppb Aflatoxin B1 only, ppb stated, Fumonison, Total ppb(fb1 + FB2 + FB3) rejectable over Field Insects unless 10 large per ½ 10 large per ½ Includes Rutherglen bugs, ladybirds, 10 large per ½ litre 10 large per ½ litre deductions are litre litre grasshoppers and wood bugs stated as Field insects 100 small per ½ 100 small per 100 small per ½ litre 100 small per ½ litre applying) All species of aphid and of mites litre ½ litre Snails Nil above screen Nil above Nil above screen Nil above screen Nil tolerance per 2.5L sample for any snails remaining above a 3.0 mm round hole screen. If one snail is found above the screen in the 0.5L sample, then a further four 0.5L samples should be taken. If a snail is found in any one of the subsequent samples, the load is to be rejected. screen Tolerance of 1 snail per 0.5L sample, passing through a 3.0 mm round hole screen. 1 snail per 0.5L below screen 1 snail per 0.5L below screen 1 snail per 0.5L below screen 1 snail per 0.5L below screen Objectionable material (entire load) Nil Nil Nil Nil ISO 605 Other non-objectionable material,% by wt K Number of kernel-sized pieces in 500 g. NOTE The class, whether yellow, oriental, brown or mixed, is added to the grade name. EAC 2010 All rights reserved 13

20 5 Contaminants 5.1 Pesticide residues Mustard seeds shall comply with those maximum pesticide residue limits established by the Codex Alimentarius Commission for this commodity. 5.2 Heavy metals Mustard seeds shall be free from heavy metals in amounts which may represent a hazard to health. If present, they shall not exceed the limits established in Table 9. Table 9 Metal contaminant limits Parameter Limit Test method i) Arsenic (As), ppm max EAS 101 or EAS 100 ii) Copper (Cu), ppm max EAS 100 iii) Lead (Pb), ppm max EAS 100 iv) Cadmium (Cd), ppm max EAS 100 v) Tin, Sn vi) Zinc, Zn 50.0 vi) Mercury (Hg), ppm max. 1.0 EAS 100 vii) Methyl mercury, calculated as Hg Mycotoxin and chemical limits Mustard seeds shall comply with those maximum mycotoxin limits established by the Codex Alimentarius Commission for this commodity Uric acid shall not exceed 100 milligrams per kilogram Total aflatoxin levels in mustard seeds for human consumption shall not exceed 10 ppb with B 1 not exceeding 5 ppb when tested according to ISO The mustard seed shall comply with the chemical requirements in Table 10. Table 10 Chemical requirements for mustard seed Parameter Limit Test method Loss in mass at 103 C, % (m/m) max Annex C Total ash, % (m/m) on dry basis, max. 6.5 ISO 928 Acid-insoluble ash, % (m/m) on dry basis, max 1.0 ISO 930 Non-volatile ether extract, % (m/m) on dry basis, min ISO 1108 Allyl isothiocyanate, % (m/m) on dry basis a) in Brassica nigra, min. b) in Brassica juncea, min. p-hydroxybenzyl isothiocyanate, % (m/m) on dry basis in Sin&is alba, min. 5.4 Environment 14 EAC 2010 All rights reserved Annex D 2.3 Annex E or Annex F Mustard seeds shall be produced, processed and handled under conditions complying with the stipulations of relevant environmental regulations and therefore conform to cleaner production technological practices.

21 6 Hygiene CD/K/471: It is recommended that the produce covered by the provisions of this Standard be prepared and handled in accordance with the appropriate sections of CAC/RCP 1, ISO 22000, and other relevant Codex texts such as Codes of Hygienic Practice and Codes of Practice. 6.2 The produce should comply with any microbiological criteria established in accordance with CAC/GL To the extent possible in good agricultural practice, the products shall be free from objectionable mater. 6.4 When tested by appropriate standards of sampling and examination listed in Clause 2, the products: shall be free from microorganisms in amounts which may represent a hazard to health and shall not exceed the limits stipulated in Table 11; shall be free from parasites which may represent a hazard to health; and shall not contain any substance originating from microorganisms in amounts which may represent a hazard to health. Table 11 Microbiological limits for mustard seed Type of micro-organism Limits Test method i) Yeasts and moulds, max. per g 10 2 ii) S.aureus per 25 g Nil iii) E. Coli, max. per g Nil iv) Salmonella, max. per 25 g Nil 7 Packaging EAS Mustard seeds shall be packed suitable packages which shall be clean, sound, free from insects, fungal infestation and the packing material shall be of food grade quality. 7.2 Mustard seeds shall be packed in containers which will safeguard the hygienic, nutritional, technological and organoleptic qualities of the products. 7.3 The containers, including packaging material, shall be made of substances which are safe and suitable for their intended use. They shall not impart any toxic substance or undesirable odour or flavour to the product. 7.4 The net weight of the mustard seeds in a package shall comply with OIML R Each package shall contain mustard seeds of the same type and of the same grade designation. 7.6 Each package shall be securely closed and sealed. 8 Marking or labelling 8.1 In addition to the requirements in EAS 38, each package shall be legibly and indelibly marked with the following: i) product name as Mustard seeds ; ii) Botanical name and variety; EAC 2010 All rights reserved 15

22 iii) iv) grade; name, address and physical location of the manufacturer/ packer/importer; v) lot/batch/code number; vi) vii) viii) ix) net weight, in g/kg; the declaration Food for Human Consumption ; storage instruction as Store in a cool dry place away from any contaminants ; crop year; x) packing date; xi) xii) xiii) xiv) xv) expiry date or best before month year; a declaration of the product lifespan; instructions on disposal of used package; country of origin; a declaration on whether the mustard seed was genetically modified or not. 8.2 A declaration of any inaccurate information in marking/labelling is prohibited and shall be punishable by law under the statutes of the Partner States. 8.3 The authorized packer shall observe all instructions regarding testing, grading, packing, marking, sealing and maintenance of records applicable to the product. 9 Sampling 9.1 Sampling shall be done in accordance with the EAS 79/ISO For the determination of total ash, use the method specified in ISO 928, with the following modifications to 8.3.2: Leach the ash with hot water, filter through a medium-fine, ashless filter paper and wash thoroughly. Transfer the filter paper and contents to the dish (6.1), dry and heat again in the muffle furnace (6.2) for 1 h. Cool and add 5 to 10 drops of analytical quality nitric acid, evaporate to dryness on the steam bath (6.4) and heat in the muffle furnace for 30 min. Repeat the addition of 5 to 10 drops of the nitric acid, again evaporate to dryness and heat in the muffle furnace for 1 h. Cool the dish, add the filtrate, and evaporate to dryness on the steam bath. Heat again in the muffle furnace for 1 h, cool and weigh. Repeat these operations until the difference between two successive weighings is less than g. Record the lower mass. The total ash may be retained for the determinations of water-insoluble ash and acid-insoluble ash. 16 EAC 2010 All rights reserved

23 Annex A (normative) CD/K/471:2010 Determination of impurities, size, foreign odours, insects, and species and variety These shall be determined in accordance with ISO 605, Pulses Determination of impurities, size, foreign odours, insects, and species and variety Test methods EAC 2010 All rights reserved 17

24 Annex B (normative) Determination of moisture content Moisture content shall be determined in accordance with the following standards: ISO 711, Cereals and cereal products Determination of moisture content (Basic reference method) ISO 712, Cereals and cereal products Determination of moisture content Routine reference method 18 EAC 2010 All rights reserved

25 C.1 Apparatus C.1.1 C.1.2 C.1.3 C.1.4 Annex C (informative) Determination of loss in mass at 103 C Dish, of corrosion-resistant metal, with a suitable tight-fitting lid. Constant temperature oven, controlled at 103 ± 2 C. Desiccator, provided with an efficient desiccant. Analytical balance C.2 Procedure C.2.1 Test portion Weigh, to the nearest g, about 2 g of the sample in the tared dish (C.1.1). C.2.2 Determination CD/K/471:2010 Heat the dish and contents, with the lid alongside the dish, in the oven (C.1.2) at 103 ± 2 C for 3 h. Fit the lid, cool in the desiccator (C.1.3) and weigh. Heat in the oven for 1 h, cool in the desiccator and weigh again. Repeat the operations of heating for 1 h in the oven, cooling and weighing, until the difference between two successive weighings does not exceed 0,001 g. C.2.3 Number of determinations Carry out two determinations on the same sample. C.3 Expression or results C.3.1 Method of calculation and formula The loss in mass at 103 C, H, expressed as a percentage by mass of the sample, is equal to: where m 0 m ( m 0 m1) m 0 is the initial mass, in grams, of the test portion; is the mass, in grams, of the test portion after heating in the oven. Take as the result the arithmetic mean of the two determinations (C.2.3), provided that the requirement for repeatability (see C.3.2) is satisfied. C.3.2 Repeatability The difference between the results of the two determinations (C.2.3), carried out simultaneously or in rapid succession by the same analyst, shall not exceed 1 % of the mean value. EAC 2010 All rights reserved 19

26 Annex D (informative) Determination of allyl isothiocyanate D.1 Principle After two successive soakings of the sample, the first in water at a temperature of 70 C and the second in alcoholic medium, distillation of the allyl isothiocyanate liberated into an alcoholic ammonium hydroxide solution, addition to the distillate of a standard volumetric silver nitrate solution, and titration of the excess silver nitrate with standard volumetric potassium, or ammonium, thiocyanate solution in the presence of ammonium iron(lll) sulphate. D.2 Reagents All reagents shall be of recognized analytical quality. The water used shall be distilled water or water of at least equivalent purity. D.2.1 D.2.2 D.2.3 D.2.4 Ethanol, 95 % (V/V). Ammonium hydroxide solution, ρ 20 = g/ml. Nitric acid, ρ 20 = 1.40 g/ml. Silver nitrate, standard volumetric solution, c(agno 3 ) = 0.1 mol/l. D.2.5 Potassium thiocyanate or ammonium thiocyanate, standard volumetric solution, c(kcns) or c(nh 4 CNS) = 0.1 mol/l. D.2.6 Ammonium iron(lll) sulphate solution, saturated when cold. D.3 Apparatus Usual laboratory apparatus, and in particular D.3.1 D.3.2 D.3.3 A. D.3.4 Grinding mill. Entrainment distillation apparatus (see Figure D.1 for a suitable example). Burette, graduated at 0.05 ml intervals, complying with the requirements of ISO 385, class Analytical balance. D.4 Procedure D.4.1 Preparation of the sample After very careful mixing of the sample, take 15 to 20 g and grind it (see ISO 2825). D.4.2 Test portion Take about 2 g of the ground sample and weigh it to the nearest g. D.4.3 Determination Transfer the test portion to the pear-shaped flask of the distillation apparatus, add 80 ml of water previously heated to 70 ± 2 C, close the flask with its ground glass stopper and leave to stand for 15 min. Then add 20 ml of the ethanol (D.2.1) and allow to soak for 45 min. 20 EAC 2010 All rights reserved

27 After the soaking, connect the flask quickly to the distillation apparatus. Distil, and collect the distillate in a conical flask containing a mixture of 5 ml of the ammonium hydroxide solution (D.2.2) and 10 ml of the ethanol (D.2.1). (Entrainment distillation lasts, on average, for 5 min.) The quantity of the distillate should be at least 100 ml. Add to the distillate 10 ml of the standard volumetric silver nitrate solution (D.2.4) and leave for 12 h at ambient temperature (the operation will be faster if the conical flask is placed for 1 h in a water bath heated to 70 to 80 C). Filter through a fine filter paper, rinse the flask and residue several times with hot water (approximately 90 C). To the bulked filtrate and washings add 10 ml of the nitric acid (D.2.3) and then titrate with the standard volumetric potassium, or ammonium, thiocyanate solution (D.2.5) using the ammonium iron(lll) sulphate solution (D.2.6) as indicator, until a persistent pink colour is obtained. B.4.4 Number of determinations Carry out two determinations on the same prepared sample. D.5 Expression of results D.5.1 Method of calculation and formula The allyl isothiocyanate content, expressed as a percentage by mass on the dry basis, is equal to where m V H 10 V ( ) 3 m 100 H 10 is the mass, in grams, of the test portion; is the volume, in millilitres, of the standard volumetric potassium, or ammonium, thiocyanate solution used in the titration; is the moisture content of the sample, expressed as a percentage by mass, determined by the method specified in Annex C. NOTE If the standard volumetric solutions used are not of the exact concentrations indicated in D.2, a suitable correction factor should be used in calculating the result. Take as the result the arithmetic mean of the two determinations (D.4.4), provided that the requirement for repeatability (see D.5.2) is satisfied. D.5.2 Repeatability The difference between the results of the two determinations (D.4.4), carried out simultaneously or in rapid succession by the same analyst, shall not exceed 1 % of the mean value. D.6 Notes on procedure D.6.1 During the analysis, all contact with copper or rubber shall be avoided, especially in the distillation apparatus. Use cork or, preferably, ground glass stoppers. D.6.2 The enzymic activity of the mustard seed diminishes with age; thus, it may be necessary to modify the analytical method in the case of old seed. After a preliminary determination giving particularly low figures for allyl isothiocyanate, add to the distillation residue 5 g of Sinapis alba (take care to check that sulphur-containing volatile substances are not present in it) and then proceed to a second determination. The addition of the two results will give the real figure of allyl isothiocyanate that may be formed in the sample. However, the actual quality of the sample should be considered as very reduced and it is recommended that the two figures, found before and after the addition of Sinapis alba, should be given in the test report. EAC 2010 All rights reserved 21

28 D.6.3 The enzymic activity of the seeds increases during certain periods of the year (particularly in spring); thus, identical results are not always found with a given lot of seed, according to the season in which the analysis is carried out. Figure D.1 Entrainment distillation apparatus 22 EAC 2010 All rights reserved

29 Annex E (informative) CD/K/471:2010 Determination of ρ-hydroxybenzyl isothiocyanate (Colorimetric method) E.1 Principle Decomposition, by enzymatic hydrolysis, of the sinalbin (glucoside of Sinapis alba) into glucose, the hydrogen sulphate of sinapin and p-hydroxybenzyl isothiocyanate, the last-mentioned giving p- hydroxybenzyl and thiocyanate. Colorimetric determination of the thiocyanate so formed. E.2 Reagents All reagents shall be of recognized analytical quality. The water used shall be distilled water or water of at least equivalent purity. E.2.1 E.2.2 E.2.3 E.2.4 Calcium carbonate, pulverized. Mercury(ll) chloride, 50 g/l solution. Potassium hexacyanoferrate(ll), 106 g/l solution. Zinc acetate solution. Dissolve 21.9 g of zinc acetate [(CH 3 COO) 2 Zn] in water, add 3 ml of glacial acetic acid (CH 3 COOH) and dilute to 100 ml with water. E.2.5 E.2.6 Nitric acid, approximately 1 mol/l solution. Sodium hydroxide, approximately 1 mol/l solution. E.2.7 Ammonium iron(lll) sulphate, 200 g/l solution in approximately 0.5 mol/l sulphuric acid solution. E.2.8 Potassium thiocyanate or ammonium thiocyanate, standard volumetric solution, c(kcns) or c(nh 4 CNS) = 0.1 mol/l, i.e. containing g of CNS - per litre. E.3 Apparatus Usual laboratory apparatus, and in particular E.3.1 Grinding mill. E.3.2 One-mark volumetric flasks, of capacities 50, 250 and 1000 ml, complying with the requirements of ISO 1042, class A. E.3.3 Pipettes, delivering 2 ml and 5 ml, complying with the requirements of ISO 648, class A, or ISO 835. E.3.4 E.3.5 Colorimeter, suitable for measurements at a wavelength of 450 nm. Analytical balance. E.4 Procedure E.4.1 Preparation of test sample Carefully render the sample homogeneous, then take a portion of 20 to 25 g of the mustard seed and grind it (see ISO 2825). EAC 2010 All rights reserved 23

30 E.4.2 Test portion Take approximately 5 g of the ground sample and weigh it to the nearest g. E.4.3 Hydrolysis Transfer the test portion to a 250 ml beaker. Add 100 ml of water at 70 ± 2 C and at least 100 mg of the calcium carbonate (E.2.1). Cover the beaker with a watch glass. Leave to soak for 15 min at 70 C, cool, add 20 ml of the sodium hydroxide solution (E.2.6), and leave in contact for 15 min. E.4.4 Clarification Add a sufficient quantity of the nitric acid solution (E.2.5), to bring the contents of the beaker to a ph of about 6.0 to 6.5. Pour the contents of the beaker into a 250 ml volumetric flask and, shaking the flask, add 2 ml of the potassium hexacyanoferrate(ll) solution (E.2.3) and then 2 ml of the zinc acetate solution (E.2.4). Dilute to 250 ml with water and add 2 ml of water by pipette (E.3.3) (to take into account the volume of the precipitate). Shake, and filter through a rapid filter shaded from bright light. The filtrate (F) should} clear and colourless. E.4.5 Determine Add to a 50 ml volume flask: 5 ml of the filtrate (F), 5 ml of ammonium iron(lll) sulphate solution (E.2.7). Dilute to 50 ml with water, shake, and measure the absorbance at a wavelength of 450 nm by means of the colorimeter (E.3.4). E.4.6 Calibration curve Transfer, by means of a pipette (E.3.3), 5 ml of the standard volumetric potassium, or ammonium, thiocyanate solution (E.2.8) to a 1000 ml volumetric flask and dilute to the mark with water. Into a series of five 50 ml volumetric flasks, transfer the volumes of this diluted potassium, or ammonium, thiocyanate solution indicated in the following table: Volume of diluted potassium, or ammonium, thiocyanate solution Corresponding mass of thiocyanate ion ml μg Add to each flask, 5 ml of the ammonium iron(lll) sulphate solution (E.2.7), dilute to the mark with water, shake, and measure the absorbance as indicated in E.4.5. Plot a calibration curve, giving the absorbance as a function of the number of micrograms of thiocyanate. E.4.7 Matching test Carry out a matching test in the same conditions as the actual test, but adding 2 drops of the mercury(ll) chloride solution (E.2.2) to correct for errors due to the reaction of phenols with the iron(lll) salts. 24 EAC 2010 All rights reserved

31 Note on the calibration curve the difference in absorbance between the test solution, containing the thiocyanate and phenols, and the matching test solution. E.4.8 Number of determinations Carry out two determinations on the same prepared sample. E.5 Expression of results E.5.1 Method of calculation and formula The p-hydroxybenzyl isothiocyanate content, expressed as a percentage by mass on the dry basis, is equal to where m 0 m 1 H m m 100 H 0 is the mass, in grams, of the test portion; is the mass, in micrograms, of thiocyanate read from the calibration curve; is the moisture content of the sample, expressed as a percentage by mass, determined by the method specified in Annex C; 2.84 is the conversion factor from thiocyanate ion (CNS - ) to p-hydroxybenzyl isothiocyanate. Take as the result the arithmetic mean of the two determinations (E.4.8), provided that the requirement for repeatability (see E.5.2) is satisfied. E.5.2 Repeatability The difference between the results of the two determinations (E.4.8), carried out simultaneously or in rapid succession by the same analyst, shall not exceed 2 % of the mean value. E.6 Note on procedure The enzymic activity of the seeds increases during certain periods of the year (particularly in spring); thus, identical results are not always found with a given lot of seed, according to the season in which the analysis is carried out. EAC 2010 All rights reserved 25

32 Annex F (informative) Determination of ρ-hydroxybenzyl isothiocyanate (Argentimetric method) F.0 Introduction Laboratories not in possession of a calorimeter may determine thiocyanate by argentimetry. In this case it is necessary either a) to carry out a preliminary check for the absence of Cl - ions in the seed (no reaction with silver nitrate on the ash of the mustard seed); or b) to provide for correction by carrying out the determination of Cl - ions on an aliquot portion of the filtrate. This method may be substituted for the calorimetric method by agreement between the parties concerned. F.1 Principle Decomposition, by enzymic hydrolysis, of sinalbin (glucoside of Sinapis alba) into glucose, the hydrogen sulphate of sinapin and p-hydroxybenzyl isothiocyanate, the last-mentioned giving p- hydroxybenzyl alcohol and thiocyanate. Determination of the thiocyanate thus formed, by argentimetry in nitric acid medium; back titration of the excess of silver nitrate using standard volumetric potassium thiocyanate solution in the presence of ammonium iron(lll) sulphate. F.2 Reagents All reagents shall be of recognized analytical quality. The water used shall be distilled water or water of at least equivalent purity. The reagents necessary for hydrolysis and clarification (see Annex E), together with F.2.1 F.2.2 F.2.3 F.2.4 Nitric acid, ρ 20 = 1.40 g/ml. Silver nitrate, standard volumetric solution, c(agno 3 ) = 0.1 mol/l. Potassium thiocyanate, standard volumetric solution, c(kcns) = 0.1 mol/l. Ammonium iron(iii) sulphate solution, saturated when cold. F.3 Apparatus The apparatus necessary for the preparation of the sample, hydrolysis and clarification (see Annex E), together with F.3.1 One-mark pipettes, of capacities 5 and 100 ml, complying with the requirements of ISO 648, class A. F.3.2 Burette, graduated at every 0.05 ml, complying with the requirements of ISO 385, class A. F.4 Procedure F.4.1 Preparation of test sample, test portion, hydrolysis and clarification Proceed as specified in E.4.1 to E.4.4 of Annex E. 26 EAC 2010 All rights reserved

33 F.4.2 Titration Add to the beaker, shaking after each addition: CD/K/471: ml, by means of a pipette (F.3.1), of the filtrate (F) (see E.4.4), and approximately equivalent to 2 g of mustard seed; 1 ml of the nitric acid (F.2.1); 5 ml, by means of a pipette (F.3.1), of the standard volumetric silver nitrate solution (F.2.2); 2 ml of the ammonium iron(lll) sulphate solution (F.2.4). Shake the flask to coagulate the precipitate, and titrate with the potassium thiocyanate solution (F.2.3) until a persistent faint red colour is obtained. F.4.3 Number of determinations Carry out two determinations on the same prepared sample. F.5 Expression of results F.5.1 Method of calculation and formula The p-hydroxybenzyl isothiocyanate content, expressed as a percentage by mass on the dry basis, is equal to where m V H ( 5 V) m 100 H is the mass, in grams, of the test portion (see Annex E, E.4.2); is the volume, in millilitres, of the standard volumetric potassium thiocyanate solution (F.2.3) used in the titration; is the moisture content of the sample, expressed as a percentage by mass, determined by the method specified in Annex C. NOTE If the standard volumetric solutions used are not of the exact concentrations specified in clause F.2, a suitable correction factor should be used in calculating the result. Take as the result the arithmetic mean of the two determinations (F.4.3), provided that the requirement for repeatability (see F.5.2) is satisfied. F.5.2 Repeatability The difference between the results of the two determinations (F.4.3), carried out simultaneously or in rapid succession by the same analyst, shall not exceed 0.1 g of p-hydroxybenzyl isothiocyanate per 100 g of dry matter in the sample. EAC 2010 All rights reserved 27

34 Annex G (informative) Recommendations relating to storage and transport G.1 The packs of mustard seed should be stored in covered premises well protected from the sun, rain and excessive heat. G.2 The store room should be dry, free from objectionable odours and proofed against entry of insects and vermin. The ventilation should be controlled so as to give good ventilation under dry conditions and no ventilation under damp conditions. In a storage warehouse, suitable facilities should be available for fumigation. G.3 The packs should be so handled and transported that they are protected from the rain, from the sun or other sources of excessive heat, from objectionable odours and from cross-infestation, especially in the holds of ships. 28 EAC 2010 All rights reserved

35 Annex H (informative) CD/K/471:2010 Model certificate of conformity with standards for farm produce 1. Trader: Certificate of conformity with the Community marketing standards applicable to fresh fruits and vegetables 2. Packer identified on packaging (if other than trader) No... (This certificate is exclusively for the use of inspection bodies) 3. Inspection body 4. Place of inspection/country of origin ( 1 ) 6. Identifier of means of transport Packages (number and type) 9. Type of product (variety if the standards specifies) Internal Import Export 5. Region or country of destination 10. Quality Class 11. Total net weight in kg 12. The consignment referred to above conforms, at the time of issue, with the Community standards in force, vide: CD/K/471:2010, Domestic mustard seed Specification and grading Customs office foreseen. Place and date of issue. Valid until (date): Signatory (name in block letters): Observations: Signature ( 1 ) Where the goods are being re-exported, indicate the origin in box 9. Seal of competent authority EAC 2010 All rights reserved 29

36 Annex I (normative) Mustard seed Fact sheet I.1 Brassica campestris Description Authority L. Family Magnoliopsida:Dilleniidae:Capparales:Cruciferae Synonyms Common Bird rape, Field mustard, Summer turnip rape, Polish rape, names Toria, Sarson, Navette d'hiver, Navette d'ete, wild turnip Editor Ecocrop 3844 code A herbaceous plant with a slender, erect, branched stem and a taproot reaching cm in height. It has broad-based, stem-clasping leaves and the flowers yellow to cream. Uses An edible oil used in cooking is extracted from the seeds. Killing temperature Bird rape is resistant to frost at all stages of growth. Growing period Annual, growing days. Further information Scientific synonyms: B. campestris var. olifera subvar. biennis (winter turnip rape), B. campestris var. olifera subvar. annua (summer turnip rape). Seed yields of t/ha are considered good, while yields about t/ha are more usual. I.2 Brassica juncea Authority (L.)Czern. Family Magnoliopsida:Dilleniidae:Capparales:Cruciferae Synonyms Sinapis juncea L. Common Leaf mustard, Brown mustard, Indian mustard, Leaf names mustard cabbage, Mustard greens, Chinese mustard, White mustard, Moutarde de Chine, Mostaza de la Rierra, Kai Choy, Kaai Ts`oi, Sesawi, Sarson kaag, Brown mustard, Rai. Editor Ecocrop 548 code 30 EAC 2010 All rights reserved

37 Description CD/K/471:2010 A herbaceous plant with an erect, branched stem up to 1 m tall, with a taproot reaching cm in depth. Flowers yellow to cream. Uses The seeds contain 25-35% of an edible oil used in cooking. The basal leaves are stalked, up to 20 cm long. The pungent leaves are used as aromatic potherbs, in mixed salads, and as cooking vegetables. Growing period Annual. Leaves may be harvested days from transplanting or days from sowing, the plant mature in days. Further information Scientific synonyms: B. lanceolata, B. cernua, Synapis juncea, S. ramosa. Leaf mustard is possibly of Chinese origin. In tropical areas optimum growing conditions can be found in the lowland at elevations up to 2000 m. A dry season after the emergence of fruit will hamper the development of seeds, thus causing severe loss of yield. Leaf yields may be t/ha and average seed yield t/ha. I.3 Brassica napus Description Authority L. Family Magnoliopsida:Dilleniidae:Capparales:Cruciferae Synonyms B. napus L. ssp. oleifera (Moench) Metzg., B. napus L. var. oleifera (Moench) Delile (ssp. napus), B. napus L. ssp. napobrassica (L.) O. Schwarz, B. napus L. ssp. napus sensu Hämet-Ahti et al. Common Rape, olraps, colza, raapzaad, rypsi, raps, rapsi, oil-seed names rape, canola, rutabaga, fodder rape, hungry gap kale, winter oil seed rape, swede rape, Siberian kale, rape seed, swede; Argentine rape, Colza d'hiver, Colza d'ete. Editor Ecocrop 549 code A herb, m tall with a strongly branched stem. Basal leaves of flowering plant stalked, highest leaves sessile and clasping stem. Flowers with mm long, pale to bright yellow petals. Uses The seeds are extracted for an oil used especially in margarine and for cooking. Newly bred cultivars with a high content of erucic acid are used for extraction of industrial oil. It is also used as a fodder crop. Killing temperature Rape is resistant to frost at all stages of growth. Unhardened plants can survive -4 C, while fully-hardened spring type rapeseed can survive -10 to -12 C, and hardened winter rapeseed can survive short periods of exposure to -15 to -20 C. Growing period Annual or biennial herb. Spring cultivars growing days, and winter cultivars days. Further information Swede rape is native of Europe. It is a temperate crop but it can be grown in the tropics at elevations between m. Yields of 2-4 t/ha are considered good, while yields of t/ha are more usual. EAC 2010 All rights reserved 31

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