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IS 6793 (1996): Fumaric Acid, Food Grade [FAD 8: FoodAdditives]

IS 6793 : 1996

(m*@u Indian Standard /

FY;MARIC ACID, FOOD GRADF - SPECIFICATION

( First Revision )

KS 664.099.62 : 547.462.3

0 BIS 1996

BUREAU OF INDIAN STANDARDS ’ MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

August 1996 Price Group 2

Food Additives Sectional Committee, FAD 8

FOREWORD

This Indian Standard (First Revision) was adopted by the Bureau of Indian Standards, after the draft finalized by the Food Additives Sectional Committee had been approved by the Food and Agriculture Division Council.

With the increased production of processed foods, manufacturers have started adding a large number of substances, generally in small quantities, to improve the appearance, flavour, texture, storage properties, etc, of the processed foods. As certain impurities in these substances have been found to be harmful, it is necessary to have strict quality control of these food additives. A series of standards was, therefore, prepared by this Institution to cover purity and identification of these substances. These standards would help in checking purity which requires to be checked at~the stage of manufacture, for it is difficult to detect the impurity once these substances have been added to the processed foods. Besides, these standards are intended to guide the indigenous manufacturers in making their product conform to specifications that are accepted by scientists, health authorities and international bodies.

Use of fumaric acid as a food additive is permitted in the Prevention ofFoodA&lterution Rufes, 1955.

Chemical Description - Its chemical names are trans-butenedioic acid and trans-1,2 ethylenedicarboxylic acid. Its empirical formula is CtH404. Its molecular weight is 116.07. Its structural formula is given below (see Fig. 1):

HOOC - C - H II

H-C - COOH

FIG. 1 STRUCTURAL FORMULA

This standard was first published in 1972, it has been revised totake into consideration the requirements given in the Food Chemical Codex, 1981 Pub. National Academy of Sciences and National Research Council and the practices being followed in trade.

In this revision, the following changes have been made:

i) Description clause covering the solubility of the product is removed from requirement clause and provided separately to keep in line with Food Chemical Codex Standard, and

ii) Requirement of lead has been replaced by heavy metals with its corresponding test method.

For the purpose of deciding whether a particular requirement of this standard is complied with, the final value, observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance with IS 2 : 1960 ‘Rules for rounding off numerical values (revised)‘. The number of significant places retained in the rounded off value should be the same as that of the specified value in this standard.

.

IS 6793 : 1996

Indian Standard

FUMARIC ACID, FOOD GRADE - SPECIFICATION

( First Revision ) 1 SCOPE

This standard prescribes the requirements and methods of sampling and test for fumaric acid, food grade.

2 REFERENCES

2.1 The following Indian Standards are necessary adjuncts to this standard:

IS No. Title

1070 : 1992 Reagent grade water (third revision)

1699 : 1995 Methods for sampling and tests for synthetic food colours (second revision)

2362 : 1973 Determination of water by the Karl Fischer method (first revision)

characteristic acid taste. Fumaric acid is soluble in alcohol, slightly soluble in water and ether and very slightly soluble in chloroform.

NOTE - The solubility is intended only as information regarding approximate solubiiity and is not to be considered as a quality requirement and is of minor significance as a means of identification or determination of purity and de- pendence must be placed on other specifications.

4 REQUIREMENTS

4.1 Identification Tests

3 DESCRIPTION

Place 50 mg of fumaric acid in a test tube, add 2 to 3 mg of resorcinol and 1 ml of sulphuric acid, stir, heat at 120 to 130°C for 5 minutes and cool. Dilute with water to 5 ml, and add sodium hydroxide solu- tion (2 : 5) dropwise while cooling to make the solution alkaline. Dilute with water to 10 ml. The solution shall have a greenish blue flourescence under ultravoilet light.

The material may be in the form of white, odour- 4.2 The materials shall also conform to the re- less granules or as a crystalline powder with quirements given in Table 1.

Table 1 Requirements for Fumaric Acid, Food Grade

Sl No.

Chnrncterlslic Requirement Melhod_of Test, Ref to C&wax of Other Indian>

This Standard

Standards

(1) (2) (3) (4) (5)

i) Purity as C4H404, 99.5 A-l -

percent by mass, (on anhydrous basis), Mm

ii) Moisture, percent by 0.5 - IS 2362 : 1973 mass, Max

iii) Sulphated ash, percent 0.1 A-2 -

by mass, Max

iv) Maleic acid, percent 0.1 A-3 -

by mass, lMax

v) Arsenic (as As), 3 - 15 of

mg/kg, Ma IS 1699 : 1995

vi) Heavy metals (as Pb), 10 - 16 of

mglkg, Mar IS 1699 : 1995

1

IS 6793 : 1996

5 PACKING, STORAGE AND MARKING

5.1 Packing

The material shall be securely packed in well-filled containers with minimum access to light and mois- ture. The containers shall be such as to preclude contamination of the contents with metals or other impurities.

5.2 Storage

The material shall be stored in a cool and dry place so as to avoid excessive exposure to heat.

5.3 Marking

Each container shall be legibly and indelibly marked with the following information:

a>

b) 4 4 e) f)

Name of the material including the words, ‘Food Grade’; Indication of the source of manufacture; Minimum net mass of the contents; Batch or code number; Date of manufacture; and Any other requirements as specified under the Standards of Weights and Measures (Packaged Commodities) Rules, 19771 Prevention of~Food AdulterationRules, 1955.

5.3.1 BIS Certification Marking

The product may also be marked with the Standard Mark.

5.3.2 The use of the Standard Mark is governed by the provisions of Bureau of Indian Standard Act, 1986 and the Rules and Regulations made there- under. The details of conditions under which the licence for the use of Standard Mark may be granted to manufacturers or producers may be obtained .from the Bureau of Indifn Standards.

6 SAMPLING .

6.1 The representative sample of the material shall be drawn according to the method prescribed in 4 of iS 1699 : 1995.

7 TESTS

7.1 Quality of Reagents

Unless specified otherwise, pure chemicals and dis- tilled water (see IS 1070 : 1992) shall be employed in tests.

NOTE - ‘Pure chemicals’ shall mean chemicals that do not contain impurities which affect the test results.

ANNEX A

[Table 1, Items (i), (iii) arzd (iv)]

METHOD OF TEST FOR FUMARIC ACIDS

A-l PURITY

A-l.1 Procedure

Transfer about 2 g, accurately weighed previously dried material into a 250-ml conical flask, add 50 ml of methanol and dissolve the sample by warming gently on a steam-bath. Cool, add phenolphthalein indicator and titrate with 1 N sodium hydroxide solution. Perform a blank determination and make any necessary correction. Each ml of 1 N sodium hydroxide is equivalent to 58.04 mg of fumaric acid.

A-2 SULPI-IATED ASII

A-2.1 Reagent

A-2.1.1 Concentrated Sulphuric&id

A-2.2 Procedure

Weigh accurately about 2 g of the material in a tared crucible. Ignite, gently at first until the material is thoroughly charred. Cool, moisten the residue with 1 ml sulphuric acid and ignite gently till the carbon is completely consumed. Cool the crucible ina desiccator and weigh.

NOTE- Cany out the ignition in a place protected from air currents and use as low temperature as possible to effect the combustion of carbon.

A-2.3 Calculation

Sulphated ash, percent by mass = 2 x 100

where Ml = mass, in g, of the residue; and M2 = mass, in g, of the material taken

for the test.

A-3 MALEIC ACID

A-3.1 Reagents

A-3.1.1 Buffer Solution

Dissolve 53.5 g of ammonium chloride in about 900 ml of water, adjust the pH to, 8.2 with approximately 0.3 N ammonium hydroxide, and dilute with water to 1000 ml.

A-3.1.2 Standard Solution

Transfer to a lOO-ml volumetric flask about 100 mg, accurately weighed, maleic acid of the highest

2

% IS 6793 : 1996

purity available, dissolve in about 10 ml of water, then dilute to volume with water and mix.

A-3.1.3 Sample Solution

Transfer about 50 g of the sample, accurately weighed, into a 250-ml beaker, add 80 ml of water, and stir for 10 minutes with a mechanical stirrer. Filter, using suction, and wash with about 40 ml of water. Transfer the combined filtrate and washings to, a 250-ml beaker, add an additional 50 g sample, accurately weighed, to the beaker and repeat the stirring, filtration, and washing procedure. Trans- fer the combined filtrate and washings to a 250-ml volumetric flask, add 2 drops of phenolphthalein indicator, then add sodium hydroxide solution with stirring, until a light pink colour persists for at least 30 seconds, and dilute to volume with water.

A-3.2 Procedure

Transfer 10.0 ml of the sample solution into a lOO-ml volumetric flask, add 20 ml of buffer solu- tion, dilute to volume with water, and mix (solution A). Rinse a polarographic cell with a portion of the

solution, then add a suitable volume of the solution to the cell, immerse it in a water-bath regulated at 24.5 to 25.5’C, and deaerate by bubbling purified nitrogen through the solution for at least 6 minutes. Insert the dropping mercury electrode of a suitable polarograph, and record the polarogram from - 1 to -2 volts, using a saturated calomel electrode as the reference electrode. Determine the height of the wave occurring at the halfwave potential near -1.36 volts. In the same manner polarograph a solution prepared by adding 10.0 ml of the sample solution, 20 ml of the buffer qolution and 2.0 ml of the standard solution to a ldO-ml volumetric flask and diluting to volume with water (solution B).

A-3.3 Calculation

Calculate the mass, in mg, of maleic acid in the total mass of sample taken by the formula 2500 C x A/(B -A), in which A is the wave height of solution A, B is the wave height of solution B, and C is the concentration in mg/ml of added maleic acid in solution B.

Bureau of Indian Standards

BIS is a statutory institution established under the Bureau ofIndian Standards Act, 1986 to promote harmonious development of the activities of standardization, marking and quality certification of goods and attending to connected matters in the country.

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Review of Indian Standards A

Amendments are issued to standards as the need arises on the basis of comments. Standards are also reviewed periodically; a standard along with amendments is reaffirmed when such review indicates that no changes are needed; if the review indicates that changes are needed, it is taken up for revision. Users of Indian Standards should ascertain that they are in possession of the latest amendments or edition by referring to the latest issue of ‘BIS Handbook’ and ‘Standards Monthly Additions’.

This Indian Standard ha5 been developed from Dot : No. FAD 8 ( 415 ).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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