First Commission Directive of 26 July 1979 laying down Community methods of analysis for testing certain sugars intended for human consumption (79/796/EEC)

EU Directive 1979/796 · Adopted 26 July 1979 · Extends to United Kingdom

X1First Commission Directive

of 26 July 1979

laying down Community methods of analysis for testing certain sugars intended for human consumption

(79/796/EEC)

THE COMMISSION OF THE EUROPEAN COMMUNITIES,

Having regard to the Treaty establishing the European Economic Community,

Having regard to Council Directive 73/437/EEC of 11 December 1973 on the approximation of the laws of the Member States concerning certain sugars intended for human consumption^f1, and in particular Article 11 thereof,

Whereas Article 11 of that Directive lays down that the composition of certain sugars shall be verified by Community methods of analysis;

Whereas it is desirable to adopt an initial series of methods in respect of which studies have been completed;

Whereas the method of determining the colour type for sugar or white sugar and for extra-white sugar, the method of measuring the conductivity ash in extra-white sugar, in sugar solution, in invert sugar solution and in invert sugar syrup, and the method of determining the colour in solution of extra-white sugar and sugar solution are laid down in the Annex to Directive 73/437/EEC;

Whereas, on the other hand, pending the formulation of further Community methods for the determination of reducing sugars, it would be advisable to allow the Member States the option of continuing to authorize the use of the Lane and Eynon method (methods 7 and 8 in Annex II, III.3 and III.4) instead of the Luff-Schoorl method (method 6 in Annex 11, III.3 and III.4);

Whereas the methods of analysis provided for in this Directive are in accordance with the opinion of the Standing Committee on Foodstuffs,

HAS ADOPTED THIS DIRECTIVE:

Annotations to the whole text

Editorial notes

X1: Substituted by Corrigendum to First Commission Directive 79/796/EEC of 26 July 1979 laying down Community methods of analysis for testing certain sugars intended for human consumption (Official Journal of the European Communities L 239 of 22 September 1979).

Footnotes

f1: OJ No L 356, 27. 12. 1973, p. 71.

1Article 1
2Article 2
3Article 3
Annex ISCOPE OF TOE COMMUNITY METHODS OF ANALYSIS FOR CERTAIN SUGARS INTENDED FOR HUMAN CONSUMPTION
Annex II: METHODS OF ANALYSIS TO VERIFY THE COMPOSITION OF CERTAIN SUGARS INTENDED FOR HUMAN CONSUMPTION
INTRODUCTION
1Preparation of the sample for analysis
2Reagents and apparatus
3Expression of results
METHOD 2
1Scope and field of application
2Definition
3Principle
Reagents
4.1Division 4.1
Apparatus
5.1Division 5.1
5.2Division 5.2
5.3Division 5.3
5.4Division 5.4
5.5Division 5.5
5.6Division 5.6
5.7Division 5.7
Procedure
6.1Pour approximately 30 g of kieselguhr (4.1) into the weighing dish (5.4) equipped with a glass rod (5.5). Place the whole in the oven (5.1) at 70 ± 1 oC and reduce the pressure to 3·3 kPa (34 mbar) or less.
6.2Division 6.2
63Division 63
6.4Division 6.4
6.5Place the dish containing the test portion and the glass rod in the oven and reduce the pressure to 3.3 kPa (34 mbar) or less. Dry at 70 ± 1 oC, allowing a slow stream of dry air to pass through the oven.
6.6Division 6.6
6.7Division 6.7
6.8Division 6.8
Expression of results
7.1Formula and method of calculation
7.2Repeatability
METHOD 3
1Scope and field of application
2Definition
3Principle
Apparatus
4.1Division 4.1
4.2Division 4.2
Procedure
5.1Division 5.1
5.2Division 5.2
6Expression and calculation of results
6.1Division 6.1
6.2Division 6.2
6.3Repeatability
METHOD 4
Scope and field of application
1Division 1
2Definitions
3Principle
Reagents
4.1Copper II solution (Muller's solution)
4.2Division 4.2
4.3Division 4.3
4.4Division 4.4
4.5Division 4.5
Apparatus
5.1Division 5.1
5.2Division 5.2
Procedure
6.1Weigh a portion of the sample (10 g or less) containing not more than 30 mg of invert sugar in a 300 ml conical flask and dissolve in about 100 ml of water.
6.2Division 6.2
6.3Division 6.3
Expression of results.
7.1Formula and method of calculation
7.1.1Division 7.1.1
7.1.2Division 7.1.2
7.1.3A value of 2·0 ml for every 10 g of sucrose present in the aliquot used, or a proportionate quantity where the sample contains less than 10 g sucrose (correction for sucrose).
7.2Repeatability
METHOD 5
1Scope and field of application
2Definition
3Principle
Reagents
4.1Division 4.1
4.2Division 4.2
Alkaline copper reagent: dissolve 25 g of anhydrous sodium carbonate and 25 g of potassium sodium tartrate tetrahydrate in about 600 ml of water containing 40 ml of 1.0 mol/litre sodium hydroxide. Dissolve 6·0 g of copper II sulphate pentahydrate (CuSO4.5H2O) in about 100 ml of water, and add to the tartrate solution. Dilute to one litre with water.
Division
4.4Standard invert sugar solution: dissolve 23·750 g of pure sucrose (4.5) in about 120 ml of water in a 250 ml graduated flask, add 9 ml of hydrochloric acid (ζ = 1·16) and allow to stand for eight days at room temperature. Make the solution up to 250 ml and check for completion of hydrolysis by a polarimeter or saccharimeter reading in a 200 mm tube. This should be - 11·80o ± 0·05 oS (see Note 8). Pipette 200 ml of this solution into a 2 000 ml graduated flask. Dilute with water and while shaking (to avoid excessive local alkalinity) add 71·4 ml of sodium hydroxide solution (1 mol/litre) in which 4 g of benzoic acid has been dissolved. Make up to 2 000 ml to give a 1 g/100 ml solution of invert sugar. This solution should be approximately pH 3.
4.5Division 4.5
Apparatus
5.1Division 5.1
5.2Division 5.2
5.3Division 5.3
Procedure
6.1Division 6.1
6.2Transfer quantitatively the solution in the test tube to the white porcelain dish (5.2) using as little water as possible, add three drops of indicator (4.2) and titrate with EDTA solution (4.1). Vo is the number of ml of EDTA used in the titration.
6.3Division 6.3
Expression of results
7.1Method of calculation
7.2Division 7.2
7.3Repeatability
8Note
METHOD 6
1Scope and field of application
1.1The reducing sugars content expressed as invert sugar in:
1.2The reducing sugar content, expressed and calculated (on the dry matter) as the dextrose equivalent in:
1.3The reducing sugar content expressed as D-glucose in:
2Definition
3Principle
Reagents
4.1Division 4.1
4.2Division 4.2
4.3Luff-Schoorl reagent: prepare the following solutions:
4.4Division 4.4
4.5Division 4.5
4.6Division 4.6
4.7Division 4.7
4.8Division 4.8
4.9Division 4.9
4.10Division 4.10
4.11Division 4.11
4.12Division 4.12
Apparatus
5.1Division 5.1
5.2Division 5.2
Procedure
6.1Standardization of the Luff-Schoorl reagent (4.3)
6.2Preparation of the solution
6.3Titration by the Luff-Schoorl method
Expression of results
7.1Formula and method of calculation
7.2Repeatability
8Note
METHOD 7
1Scope and field of application
2Definition
3Principle
Reagents
4.1Fehling's solution:
4.2Division 4.2
4.3Standard invert sugar solution: dissolve 23·750 g of pure sucrose in about 120 ml of water in a 250 ml graduated flask, add 9 ml of hydrochloric acid (ζ = 1·16) and allow to stand for eight days at room temperature. Make the solution up to 250 ml and check for completion of hydrolysis by a polarimeter or saccharimeter reading in a 200 mm tube. This should be - 11·80o ± 0·05 oS (see note 8). Pipette 200 ml of this solution into a 2 000 ml graduated flask. Dilute with water and while shaking (to avoid excessive local alkalinity) add 71·4 ml of sodium hydroxide solution (1 mol/litre) (4.2) in which 4 g of benzoic acid has been dissolved. Make up to 2 000 ml to give a 1 g/100 ml solution of invert sugar. This solution should be a pH of approximately 3.
4.4Division 4.4
Apparatus
5.1Division 5.1
5.2Division 5.2
5.3Division 5.3
5.4Division 5.4
5.5Division 5.5
5.6Division 5.6
Procedure
Standardization of Fehling's solution
6.1.1Division 6.1.1
6.1.2Division 6.1.2
6.1.3Division 6.1.3
6.1.4Heat the flask and contents till boiling and allow to boil for exactly two minutes; the flask must not be removed from the heat source during the course of the rest of the procedure, or allowed to cease boiling.
6.1.5Division 6.1.5
6.1.6Division 6.1.6
6.2Preparation of sample solutions
Preliminary test
6.3.1A preliminary test must be carried out to ensure that the quantity of water to be added to the 20 ml of mixed solutions A and B is sufficient to ensure that a final volume after titration of 75 ml is obtained.
6.3.2If, after the addition of the methylene blue solution, the reddish colour persists, the sample solution used is too concentrated. In this case, the test is discarded but repeated using a less concentrated sample solution.
Final analysis of sample solution
6.4.1Division 6.4.1
6.4.2Division 6.4.2
Expression of results
7.1Formula and method of calculation
Note:
7.2Repeatability
8Note
METHOD 8
1Scope and field of application
Definition
2.1Division 2.1
2.2Division 2.2
3Principle
Reagents
Fehling's solution:
4.1.1Solution A:
4.1.2Solution B:
Note:
4.1.3Preparation of the mixed Fehling's solution
Note:
4.2Anhydrous dextrose (D-glucose) (C6H12O6)
4.3Standard dextrose solution, 0·600 g/100 ml
4.4Methylene blue solution, 0·1 g/100 ml
Apparatus
5.1Division 5.1
5.2Division 5.2
5.3Division 5.3
5.4Division 5.4
5.5Division 5.5
5.6Division 5.6
Procedure
Standardization of the Fehling's solution
6.1.1Division 6.1.1
6.1.2Division 6.1.2
6.1.3Division 6.1.3
6.1.4Place the boiling flask on the heating device (5.5), previously adjusted so that boiling commences in 120 ± 15 seconds.
6.1.5Division 6.1.5
6.1.6Boil the contents of the flask for 120 seconds, as timed by the stop-watch.
6.1.7After boiling has continued for 120 seconds (by the stop-watch) start adding standard dextrose solution to the boiling flask (5.1) from the burette (6.1.2) in 0·5 ml increments until the colour of the methylene blue is discharged (see notes 2 and 3).
6.1.8Division 6.1.8
6.1.9Division 6.1.9
6.1.10Division 6.1.10
6.1.11After boiling has continued for 120 seconds (by the stop-watch), start adding standard dextrose solution to the boiling flask (5.1) from the burette, initially in 0·2 ml increments and finally dropwise, until the colour of the methylene blue is just discharged.
6.1.12Division 6.1.12
6.1.13Vo shall be between 19·0 and 21·0 ml standard dextrose solution (4.3).
6.1.14Division 6.1.14
Note 1:
Note 2:
Note 3:
Note 4:
Preliminary examination of the prepared sample
6.2.1Unless the reducing power (2.1) of the prepared sample is known approximately, it is necessary to carry out a preliminary examination in order to obtain an approximate figure for it so that the mass of the test portion (6.3) can be calculated.
6.2.2Division 6.2.2
6.2.3Division 6.2.3
6.2.4Division 6.2.4
6.2.5Division 6.2.5
6.2.6Division 6.2.6
6.2.7Division 6.2.7
6.2.8Immediately boiling has started, start the stop-watch (5.6) from zero and commence adding sample solution to the flask from the burette in 1·0 ml increments at intervals of approximately 10 seconds until the blue colour of the methylene blue is discharged.
6.2.9Division 6.2.9
6.2.10The approximate reducing power of the prepared sample in percent by mass is given by:
6.3Test portion
6.4Test solution
Determination
6.5.1Division 6.5.1
6.5.2Division 6.5.2
6.5.3Division 6.5.3
6.5.4Division 6.5.4
6.5.5Division 6.5.5
6.5.6Division 6.5.6
6.5.7Division 6.5.7
6.5.8Division 6.5.8
6.5.9Division 6.5.9
6.5.10Division 6.5.10
6.5.11Division 6.5.11
6.5.12Division 6.5.12
6.5.13V1 shall be between 19·0 and 21·0 ml test solution.
6.5.14Division 6.5.14
6.6Dry matter content
Expression of results
Formulae and method of calculation
7.1.1Reducing power
7.1.2Dextrose equivalent
7.1.3Division 7.1.3
7.2Repeatability
DETERMINATION OF POLARIZATION
1Scope and field of application
2Definition
3Principle
Reagents
4.1Clarification agent: basic lead acetate solution.
4.2Division 4.2
Apparatus
5.1Saccharimeter graduated for the normal weight of 26 g of sucrose, or polarimeter
5.2Division 5.2
5.3Division 5.3
5.4Division 5.4
5.5Division 5.5
5.6Division 5.6
Procedure
6.1Preparation of the solution
6.2Polarization
6.2.1Division 6.2.1
6.2.2Division 6.2.2
6.2.3Division 6.2.3
6.2.4Fill the tube carefully at 20 ± 0·1 oC with the sample solution to be examined.
6.2.5Division 6.2.5
Expression of results
7.1Formula and method of calculation
7.2Repeatability

First Commission Directive of 26 July 1979 laying down Community methods of analysis for testing certain sugars intended for human consumption (79/796/EEC)

Annotations to the whole text

Editorial notes

Footnotes

Contents