Bsi bs en 01377 1997 (1999)

00971287 PDF BRITISH STANDARD BS EN 1377 1997 Foodstuffs — Determination of acesulfame K in table top sweetener preparations — Spectrometric method The European Standard EN 1377 1996 has the status of[.]

BRITISH STANDARD BS EN

1377:1997

Foodstuffs —

Determination of

acesulfame K in table

top sweetener

preparations —

Spectrometric method

The European Standard EN 1377:1996 has the status of a

British Standard

ICS 67.180.10

This British Standard, having

been prepared under the

direction of the Consumer

Products and Services Sector

Board, was published under

the authority of the Standards

Board and comes

into effect on

15 May 1997

© BSI 09-1999

The following BSI references

relate to the work on this

standard:

Committee reference AW/-/3

Draft for comment 94/501925 DC

ISBN 0 580 27123 4

Committees responsible for this British Standard

The preparation of this British Standard was entrusted to Technical Panel AW/-/3, Food analysis — Horizontal methods, upon which the following bodies were represented:

Association of Public Analysts Food and Drink Federation Institute of Food Science and Technology Laboratory of the Government Chemist Ministry of Agriculture, Fisheries and Food Royal Society of Chemistry

Amendments issued since publication

BS EN 1377:1997

Contents

Page

ii © BSI 09-1999

National foreword

This British Standard has been prepared by Technical Panel AW/-/3 and is the

English language version of EN 1377:1996 Foodstuffs — Determination of

acesulfame K in table top sweetener preparations — Spectrometric method,

published by the European Committee for Standardization (CEN) EN 1377 was produced as a result of international discussions in which the United Kingdom took an active part

ISO 5725:1986, to which informative reference is made in the text, has been superseded by ISO 5725-1:1994, ISO 5725-2:1994, ISO 5725-3:1994,

ISO 5725-4:1994 and ISO 5725-6:1994 which are identical with BS ISO 5725

Accuracy (trueness and precision) of measurement methods and results,

BS ISO 5725-1:1994 General principles and definitions, BS ISO 5725-2:1994

Basic method for the determination of repeatability and reproducibility of a standard measurement method, BS ISO 5725-3:1994 Intermediate measures of the precision of a standard measurement method, BS ISO 5725-4:1994 Basic method for the determination of the trueness of a standard measurement method,

and BS ISO 5725-6:1994 Use in practice of accuracy values.

A British Standard does not purport to include all the necessary provisions of a contract Users of British Standards are responsible for their correct application

Compliance with a British Standard does not of itself confer immunity from legal obligations.

Cross-references

Publication referred to Corresponding British Standard

EN ISO 3696:1995 BS EN ISO 3696:1995 Water for analytical laboratory

use Specification and test methods

Summary of pages

This document comprises a front cover, an inside front cover, pages i and ii, the EN title page, pages 2 to 6, an inside back cover and a back cover

This standard has been updated (see copyright date) and may have had amendments incorporated This will be indicated in the amendment table on the inside front cover

EUROPEAN STANDARD

NORME EUROPÉENNE

EUROPÄISCHE NORM

EN 1377

September 1996

ICS 67.180.10

Descriptors: Food products, intense sweeteners, chemical analysis, determination of content, spectrometric analysis

English version

Foodstuffs — Determination of acesulfame K in table top sweetener preparations — Spectrometric method

Produits alimentaires — Dosage de

l’acésulfame K dans les édulcorants de table —

Méthode spectrométrique

Lebensmittel — Bestimmung von Acesulfam-K

in Tafelsüßen — Spektralphotometrisches Verfahren

This European Standard was approved by CEN on 1996-06-09 CEN members

are bound to comply with the CEN/CENELEC Internal Regulations which

stipulate the conditions for giving this European Standard the status of a

national standard without any alteration

Up-to-date lists and bibliographical references concerning such national

standards may be obtained on application to the Central Secretariat or to any

CEN member

This European Standard exists in three official versions (English, French,

German) A version in any other language made by translation under the

responsibility of a CEN member into its own language and notified to the

Central Secretariat has the same status as the official versions

CEN members are the national standards bodies of Austria, Belgium,

Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy,

Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and

United Kingdom

CEN

European Committee for Standardization Comité Européen de Normalisation Europäisches Komitee für Normung

Central Secretariat: rue de Stassart 36, B-1050 Brussels

© 1996 Copyright reserved to CEN members

Ref No EN 1377:1996 E

© BSI 09-1999

2

Foreword

This European Standard has been prepared by the

Technical Committee CEN/TC 275, Food analysis —

Horizontal methods, the Secretariat of which is held

by DIN

This European Standard shall be given the status of

a national standard, either by publication of an

identical text or by endorsement, at the latest by

March 1997, and conflicting national standards

shall be withdrawn at the latest by March 1997

According to the CEN/CENELEC Internal

Regulations, the following countries are bound to

implement this European Standard: Austria,

Belgium, Denmark, Finland, France, Germany,

Greece, Iceland, Ireland, Italy, Luxembourg,

Netherlands, Norway, Portugal, Spain, Sweden,

Switzerland and the United Kingdom

Contents

Page

Figure A.1 — Absorption spectrum of an acesulfame K standard solution in water 5

EN 1377:1996

1 Scope

This European Standard specifies a spectrometric

method for the determination of acesulfame K in

solid table top sweetener preparations containing it

An inter-laboratory test has been carried out on

sweetener tablets [1]

2 Normative references

This European Standard incorporates by dated or

undated reference, provisions from other

publications These normative references are cited

at the appropriate places in the text and the

publications are listed hereafter For dated

references, subsequent amendments to or revisions

of any of these publications apply to this European

Standard only when incorporated in it by

amendment or revision For undated references the

latest edition of the publication referred to applies

EN ISO 3696, Water for analytical laboratory use —

Specification and test methods

3 Principle

Preparation of the sample test solution by dissolving

table top sweetener preparation in water

Photometric determination of the acesulfame K

content at the absorption maximum of

about 227 nm

4 Reagents

During the analysis, unless otherwise stated, use

only reagents of recognized analytical grade and

water of at least grade 3 as defined in EN ISO 3696

4.1 Acesulfame K standard substance, with a known

content of at least 99 % in dry matter

NOTE For further information on identification and purity,

see [2].

4.2 Acesulfame K stock solution,

Ô(C4H4NO4SK) ë 0,8 g/l1)

Dissolve about 400,0 mg of the acesulfame K

standard substance (4.1) weighed to the

nearest 0,1 mg, in water in a 500 ml volumetric

flask, and dilute to the mark with water

4.3 Acesulfame K standard solution,

Ô(C4H4NO4SK) ë 8 mg/l

Pipette 5,00 ml of the acesulfame K stock

solution (4.2) into a 500 ml volumetric flask and

dilute to the mark with water

NOTE Additional solutions with concentrations within the

linear range may be prepared for the calibration graph.

5 Apparatus and equipment

Usual laboratory apparatus and, in particular, the following

5.1 Spectrometer, suitable for measurements in the

ultraviolet (UV) range

5.2 Quartz cuvettes, with an optical path length

of 1 cm

6 Procedure

6.1 Determination of average tablet mass

Determine the mass of at least 20 sweetener tablets

to the nearest 0,1 mg and calculate the average

mass (m2) of one tablet

NOTE For improved accuracy the use of 100 tablets is recommended.

6.2 Preparation of the sample test solution

Dissolve an amount of finely ground table top

sweetener preparation (m0), equivalent to about 400 mg of acesulfame K or corresponding

to 20 times the average mass of a tablet (6.1),

transfer to a 500 ml volumetric flask with water, dissolve it in water and dilute to the mark with water

Allow any undissolved constituents to settle and, if necessary, filter the solution, discarding the first 100 ml of the filtrate Then pipette 5,00 ml of the solution into a 500 ml volumetric flask and dilute to the mark with water

6.3 Determination 6.3.1 Measure the absorption spectrum of the standard acesulfame K solution between 200 nm

and 280 nm in quartz cuvettes (5.2) with water as

reference and determine the absorption (A1) at the wavelength of the absorption maximum

(about 227 nm)

Check the linearity range with a series of solutions

of suitable concentrations (calibration graph)

6.3.2 Measure the absorption spectrum of the

sample test solution as described in 6.3.1 and

determine the absorption (A2) at the absorption

maximum as determined in 6.3.1.

If the shape of the absorption curve obtained for the

sample test solution (6.2) differs from that of the

standard solution, it is probable that an interfering substance is present In this case, the method is not applicable

1) Ô is the mass concentration.

4 © BSI 09-1999

Verify the applicability by determining the

absorptions 12 nm above and 12 nm below the

wavelength of the absorption maximum

(about 227 nm) Absorption ratios between these

values and the maximum absorption shall not differ

from those obtained when using the acesulfame K

standard solution (4.3).

An example for an absorption spectrum of

acesulfame K is given in Annex A

7 Expression of results

7.1 Calculate the mass fraction, w1, of acesulfame K,

in milligrams per kilogram, using the following

equation:

Where:

7.2 Calculate the mass fraction, w2 of acesulfame K,

in milligrams per tablet, using the following

equation:

where:

If the calculation is based on a calibration graph, an

alternative calculative evaluation using the

regression graph may be used

Report the result after rounding to one decimal

place

8 Precision

Details of the inter-laboratory test of the precision of the method according to ISO 5725:1986 [3] are summarized in Annex B The values derived from the inter-laboratory test may not be applicable to analyte concentration ranges and matrices other than given in Annex B

8.1 Repeatability

The absolute difference between two single test results found on identical test material by one operator using the same apparatus within the shortest feasible time interval will exceed the

repeatability limit r in not more than 5 % of the

cases

The value is:

r = 3,2 mg/100 mg for commercially available

acesulfame K tablets

8.2 Reproducibility

The absolute difference between two single test results on identical test material reported by two

laboratories will exceed the reproducibility limit R

in not more than 5 % of the cases

The value is:

R = 3,7 mg/100 mg for commercially available acesulfame K tablets

9 Test report

The test report shall contain at least the following data:

— all information necessary for the identification

of the sample;

— a reference to this European Standard or to the method used;

— the results and the units in which the results have been expressed;

— if the repeatability of the method has been verified;

— any particular points observed in the course of the test;

— any operations not specified in the method or regarded as optional which might have affected the results

(1)

A2 is the absorption of the sample test

solution (6.3.2);

A1 is the absorption of the acesulfame K

standard solution (6.3.1);

m0 is the initial sample mass (6.2) in

milligrams;

m1 is the mass of the acesulfame K standard

substance in 500 ml standard solution

(4.3) in milligrams (here: 4,0 mg);

F is the dilution factor (here: 100)

(2)

mass (6.1), in milligrams;

A2, F, m1, A1, m0 see equation (1)

EN 1377:1996

Annex A (informative)

Figure

Figure A.1 — Absorption spectrum of an acesulfame K standard solution in water

6 © BSI 09-1999

Annex B (informative)

Precision data

In accordance with ISO 5725:1986 [3], the following parameters have been defined in an inter-laboratory test The test was conducted by the Max von Pettenkofer Institute of the Federal Health Office, Food Chemistry Department, Berlin, Germany [1]

Table B.1

Annex C (informative)

Bibliography

[1] Untersuchung von Lebensmitteln: Bestimmung des Acesulfam-K-Gehaltes in acesulfam-K-haltigen

Süßstoff-Tabletten L 57.22.99-3, Mai 1989 (Food Analysis: Determination of acesulfame K content in sweetener tablets containing it L 57.22.99-3, 1989-05) In: Amtliche Sammlung von Untersuchungsverfahren nach § 35 LMBG: Verfahren zur Probenahme und Untersuchung von Lebensmitteln, Tabakerzeugnissen, kosmetischen Mitteln und Bedarfsgegensänden/Bundesgesundheitsamt (In: Collection of official methods under article 35 of the German Federal Foods Act; Methods of sampling and analysis of foods, tobacco products, cosmetics and commodity goods, Federal Health Office) Loseblattausgabe, Stand Mai 1994

Bd 1 (Loose-leaf edition of 1994-05 Vol I.) Berlin, Köln: Beuth Verlag GmbH

[2] FAO Food and Nutrition Paper 28 of the Joint FAO/WHO Expert Committee on Food Additives, April 1980

[3] ISO 5725:1986 Precision of test methods — Determination of repeatability and reproducibility for a

standard test method by inter-laboratory tests.

Sample Commercially available acesulfame tablets

Number of laboratories retained after eliminating outliers 7

Reproducibility relative standard deviation RSDR 1,3 %

x

BS EN 1377:1997

© BSI 09-1999

List of references

See national foreword

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