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
BS EN 1377:1997

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

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 Amendments issued since publication
15 May 1997

© BSI 09-1999 Amd. No. Date Comments

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

 BS EN 1377:1997

Contents

Page
Committees responsible Inside front cover
National foreword ii
Foreword 2
Text of EN 1377 3
List of references Inside back cover

© BSI 09-1999 i
BS EN 1377:1997

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.
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
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superseded by ISO 5725-1:1994, ISO 5725-2:1994, ISO 5725-3:1994,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.

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.

ii © BSI 09-1999
EUROPEAN STANDARD EN 1377
NORME EUROPÉENNE
September 1996
EUROPÄISCHE NORM

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 Lebensmittel — Bestimmung von Acesulfam-K

l’acésulfame K dans les édulcorants de table — in Tafelsüßen — Spektralphotometrisches
Méthode spectrométrique 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
EN 1377:1996

Foreword Contents
This European Standard has been prepared by the Page
Technical Committee CEN/TC 275, Food analysis — Foreword 2
Horizontal methods, the Secretariat of which is held
1 Scope 3
by DIN.
2 Normative references 3
This European Standard shall be given the status of
a national standard, either by publication of an 3 Principle 3
identical text or by endorsement, at the latest by 4 Reagents 3
March 1997, and conflicting national standards 5 Apparatus and equipment 3
shall be withdrawn at the latest by March 1997.
6 Procedure 3
According to the CEN/CENELEC Internal
Regulations, the following countries are bound to 7 Expression of results 4
implement this European Standard: Austria, 8 Precision 4
Belgium, Denmark, Finland, France, Germany, 9 Test report 4
Greece, Iceland, Ireland, Italy, Luxembourg, Annex A (informative) Figure 5
Netherlands, Norway, Portugal, Spain, Sweden,
Switzerland and the United Kingdom. Annex B (informative) Precision data 6
Annex C (informative) Bibliography 6
Figure A.1 — Absorption spectrum of an
acesulfame K standard solution in water 5
Table B.1 6

2 © BSI 09-1999
 EN 1377:1996

1 Scope 5 Apparatus and equipment

This European Standard specifies a spectrometric Usual laboratory apparatus and, in particular, the
method for the determination of acesulfame K in following.
solid table top sweetener preparations containing it. 5.1 Spectrometer, suitable for measurements in the
An inter-laboratory test has been carried out on ultraviolet (UV) range.
sweetener tablets [1]. 5.2 Quartz cuvettes, with an optical path length
of 1 cm.
2 Normative references
This European Standard incorporates by dated or 6 Procedure
undated reference, provisions from other 6.1 Determination of average tablet mass
publications. These normative references are cited
at the appropriate places in the text and the Determine the mass of at least 20 sweetener tablets
publications are listed hereafter. For dated to the nearest 0,1 mg and calculate the average
references, subsequent amendments to or revisions mass (m2) of one tablet.
of any of these publications apply to this European NOTE For improved accuracy the use of 100 tablets is
recommended.
Standard only when incorporated in it by
amendment or revision. For undated references the 6.2 Preparation of the sample test solution
latest edition of the publication referred to applies. Dissolve an amount of finely ground table top
EN ISO 3696, Water for analytical laboratory use — sweetener preparation (m0), equivalent to
Specification and test methods. about 400 mg of acesulfame K or corresponding
to 20 times the average mass of a tablet (6.1),
3 Principle transfer to a 500 ml volumetric flask with water,
dissolve it in water and dilute to the mark with
Preparation of the sample test solution by dissolving
water.
table top sweetener preparation in water.
Photometric determination of the acesulfame K Allow any undissolved constituents to settle and, if
content at the absorption maximum of necessary, filter the solution, discarding the
about 227 nm. first 100 ml of the filtrate. Then pipette 5,00 ml of
the solution into a 500 ml volumetric flask and
4 Reagents dilute to the mark with water.

During the analysis, unless otherwise stated, use 6.3 Determination

only reagents of recognized analytical grade and 6.3.1 Measure the absorption spectrum of the
water of at least grade 3 as defined in EN ISO 3696. standard acesulfame K solution between 200 nm
4.1 Acesulfame K standard substance, with a known and 280 nm in quartz cuvettes (5.2) with water as
content of at least 99 % in dry matter. reference and determine the absorption (A1) at the
wavelength of the absorption maximum
NOTE For further information on identification and purity,
see [2]. (about 227 nm).
4.2 Acesulfame K stock solution, Check the linearity range with a series of solutions
Ô(C4H4NO4SK) ë 0,8 g/l1) of suitable concentrations (calibration graph).
Dissolve about 400,0 mg of the acesulfame K 6.3.2 Measure the absorption spectrum of the
standard substance (4.1) weighed to the sample test solution as described in 6.3.1 and
nearest 0,1 mg, in water in a 500 ml volumetric determine the absorption (A2) at the absorption
flask, and dilute to the mark with water. maximum as determined in 6.3.1.
4.3 Acesulfame K standard solution, If the shape of the absorption curve obtained for the
Ô(C4H4NO4SK) ë 8 mg/l sample test solution (6.2) differs from that of the
Pipette 5,00 ml of the acesulfame K stock standard solution, it is probable that an interfering
solution (4.2) into a 500 ml volumetric flask and substance is present. In this case, the method is not
dilute to the mark with water. applicable.
NOTE Additional solutions with concentrations within the
linear range may be prepared for the calibration graph.

1)
Ô is the mass concentration.

© BSI 09-1999 3
EN 1377:1996

Verify the applicability by determining the 8 Precision

absorptions 12 nm above and 12 nm below the
Details of the inter-laboratory test of the precision of
wavelength of the absorption maximum
the method according to ISO 5725:1986 [3] are
(about 227 nm). Absorption ratios between these
summarized in Annex B. The values derived from
values and the maximum absorption shall not differ
from those obtained when using the acesulfame K the inter-laboratory test may not be applicable to
standard solution (4.3). analyte concentration ranges and matrices other
than given in Annex B.
An example for an absorption spectrum of
acesulfame K is given in Annex A. 8.1 Repeatability
The absolute difference between two single test
7 Expression of results results found on identical test material by one
operator using the same apparatus within the
7.1 Calculate the mass fraction, w1, of acesulfame K,
shortest feasible time interval will exceed the
in milligrams per kilogram, using the following
repeatability limit r in not more than 5 % of the
equation:
cases.
The value is:
(1)
r = 3,2 mg/100 mg for commercially available
acesulfame K tablets.
Where:
8.2 Reproducibility
A2 is the absorption of the sample test
The absolute difference between two single test
solution (6.3.2);
results on identical test material reported by two
A1 is the absorption of the acesulfame K laboratories will exceed the reproducibility limit R
standard solution (6.3.1); in not more than 5 % of the cases.
m0 is the initial sample mass (6.2) in The value is:
milligrams;
R = 3,7 mg/100 mg for commercially available
m1 is the mass of the acesulfame K standard
substance in 500 ml standard solution acesulfame K tablets.
(4.3) in milligrams (here: 4,0 mg);
9 Test report
F is the dilution factor (here: 100).
The test report shall contain at least the following
7.2 Calculate the mass fraction, w2 of acesulfame K, data:
in milligrams per tablet, using the following — all information necessary for the identification
equation: of the sample;
— a reference to this European Standard or to the
(2) method used;
— the results and the units in which the results
where: have been expressed;
m2 is the average tablet — if the repeatability of the method has been
mass (6.1), in milligrams; verified;
A2, F, m1, A1, m0 see equation (1). — any particular points observed in the course of
the test;
If the calculation is based on a calibration graph, an — any operations not specified in the method or
alternative calculative evaluation using the regarded as optional which might have affected
regression graph may be used. the results.
Report the result after rounding to one decimal
place.

4 © BSI 09-1999
 EN 1377:1996

Annex A (informative)
Figure

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

© BSI 09-1999 5
EN 1377:1996

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
Sample Commercially available acesulfame tablets
Year of inter-laboratory test 1986
Number of laboratories 8
Number of samples 1
Number of laboratories retained after eliminating outliers 7
Number of outliers (laboratories) 1
Number of accepted results 38
Mean value x 98,0 mg/100 mg
Repeatability standard deviation sr 1,1 mg/100 mg
Repeatability relative standard deviation RSDr 1,2 %
Repeatability limit r 3,2 mg/100 mg
Reproducibility standard deviation sR 1,3 mg/100 mg
Reproducibility relative standard deviation RSDR 1,3 %
Reproducibility limit R 3,7 mg/100 mg

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.

6 © BSI 09-1999
 BS EN 1377:1997

List of references

See national foreword.

© BSI 09-1999
BS EN
1377:1997
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