SIST EN ISO 11215:1999

Modified starch - Determination of adipic acid content of acetylated di-starch adipates - Gas-chromatographic method (IS0 11215:1998)

Migrated from Progress Sheet (TC Comment) (2000-07-10): According to a PC4 recommendation, CEN/BT agreed to launch a parallel voting ++ procedure on the draft international standard derived from the above ++ mentionned subject (Ref.nr. in ISO 11215).

Modifizierte Stärke - Bestimmung des Gehalts an Adipinsäure in acetylierten Di-Stärke-Adipaten - Gaschromatographisches Verfahren (ISO 11215:1998)

Diese Internationale Norm legt ein Verfahren zur gaschromatographischen Bestimmung des Gesamtgehalts an Adipat und des Gehalts an freier Adipinsäure in acetylierten Di-Stärke-Adipaten fest.

Amidons et fécules modifiés - Détermination de la teneur en acide adipique dans les adipates de diamidon acétylés - Méthode par chromatographie en phase gazeuse (ISO 11215:1998)

L'IEC 61340-5-1:2016 s'applique aux activités concernant: la fabrication, le traitement, l'assemblage, l'installation, l'emballage, l'étiquetage, l'entretien, l'essai, l'examen, le transport ou bien la manipulation des pièces, des ensembles et des équipements électriques ou électroniques présentant des tensions de tenue supérieures ou égales à 100 V sur le modèle du corps humain (HBM), 200 V sur le modèle de dispositif chargé (CDM) et 35 V sur les conducteurs isolés. Des ESDS possédant des tensions de tenue inférieures peuvent nécessiter des éléments de contrôle supplémentaires ou des limites ajustées. Les processus conçus pour manipuler des éléments présentant une ou plusieurs tensions de tenue aux ESD inférieures peuvent toujours déclarer être conformes à la présente norme. La présente norme fournit les exigences nécessaires à un programme de maîtrise des ESD. L'IEC TR 61340-5-2 [9] donne des lignes directrices pour la mise en eouvre de la présente norme. La présente norme ne s'applique pas aux dispositifs explosifs à déclenchement électronique ni aux liquides, gaz et poudres inflammables. L'objectif de la présente norme est de fournir les exigences administratives et techniques pour l'établissement, la mise en oeuvre et la maintenance d'un programme de maîtrise des ESD (ci­après dénommé "programme"). Cette édition inclut les modifications techniques majeures suivantes par rapport à l'édition précédente:
a) Des exigences techniques ont été modifiées afin d'aligner l'IEC 61340-5-1 avec les autres normes de l'industrie relatives aux décharges électrostatiques (ESD);
b) Les documents de référence ont été mis à jour afin de refléter les normes IEC récemment publiées;
c) Un paragraphe sur la qualification produit a été ajouté;
d) Le Tableau 4 a été supprimé, et les exigences relatives aux emballages sont désormais décrites dans l'IEC 61340-5-3;
e) L'Article A.1 a été supprimé et figure désormais dans l'IEC 61340-4-6.

Modificiran škrob - Določevanje vsebnosti adipinske kisline v acetiliranih di-škrob adipatih - Plinskokromatografska metoda (ISO 11215:1998)

General Information

• Status: Published
• Publication Date: 30-Apr-1999
• ICS: 67.180.20 - Starch and derived products
• Technical Committee: KŽP - Agricultural food products
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 01-May-1999
• Due Date: 01-May-1999
• Completion Date: 01-May-1999
• Ref Project: EN ISO 11215:1998 - Modified starch - Determination of adipic acid content of acetylated di-starch adipates - Gas-chromatographic method (IS0 11215:1998)

Overview

EN ISO 11215:1998 specifies a validated gas‑chromatographic method to determine the total and free adipic acid content of acetylated di‑starch adipates (modified starch). The method is intended for laboratories performing quality control and regulatory testing of starch derivatives used in food and industrial applications. The procedure uses silylation and capillary GC with an internal standard (pimelic acid) to achieve reliable quantification.

Key Topics

• Scope and principle: Hydrolysis of adipyl linkages with NaOH releases adipic acid from the starch matrix. After acidification, adipic acid is extracted into ethyl acetate, concentrated, silylated (BSTFA + 1% TMCS) and analysed by GC with flame ionization detection.
• Reagents and reference materials: water (ISO 3696 grade), waxy maize starch as base material, adipic acid and pimelic acid standard solutions (50 mg/l), NaOH (4 mol/l), concentrated HCl, ethyl acetate, acetonitrile, BSTFA/TMCS, and carrier gases (He, H2, N2, air).
• Apparatus: capillary GC with FID and on‑column injection, ultrasonic bath, centrifuge, rotary shaker, nitrogen evaporation device and standard lab glassware.
• Calibration and quantification: Use calibration tubes containing known adipic acid masses added to waxy maize starch and pimelic acid as the internal standard. Plot adipic/pimelic peak area ratios vs. mass to derive the calibration curve and determine sample adipic content.
• Precision: The standard includes interlaboratory precision data. Example values from the collaborative trial: for a mean total adipic acid content of about 430 mg/kg, repeatability standard deviation s(r) = 22 mg/kg and reproducibility limit R = 142 mg/kg.

Applications

• Routine quality control of modified starch (acetylated di‑starch adipates) in food ingredient manufacturing and ingredient supply chains.
• Verification of free vs. bound adipic acid to assess hydrolysis, storage stability, or processing effects.
• Regulatory compliance testing where quantification of residual adipic acid is required for safety and labelling.

Practical value: The method provides a clear analytical workflow - extraction, concentration, silylation and GC - using commonly available reagents and instrumentation. The internal standard approach (pimelic acid) improves accuracy and compensates for extraction/derivatisation variability.

Related Standards

• ISO 1666:1996 - Starch - Determination of moisture content (oven‑drying method).
• ISO 3696:1987 - Water for analytical laboratory use - Specification and test methods.
• ISO 5725 - Precision of measurement methods (referenced for interlaboratory statistics).

For laboratories implementing EN ISO 11215:1998, following the described sample preparation, calibration and reporting requirements ensures reproducible, traceable results for adipic acid analysis in modified starch products.

Standards Content (Sample)

SLOVENSKI STANDARD
01-maj-1999
0RGLILFLUDQãNURE'RORþHYDQMHYVHEQRVWLDGLSLQVNHNLVOLQHYDFHWLOLUDQLKGLãNURE
DGLSDWLK3OLQVNRNURPDWRJUDIVNDPHWRGD,62
Modified starch - Determination of adipic acid content of acetylated di-starch adipates -
Gas-chromatographic method (IS0 11215:1998)
Modifizierte Stärke - Bestimmung des Gehalts an Adipinsäure in acetylierten Di-Stärke-
Adipaten - Gaschromatographisches Verfahren (ISO 11215:1998)
Amidons et fécules modifiés - Détermination de la teneur en acide adipique dans les
adipates de diamidon acétylés - Méthode par chromatographie en phase gazeuse (ISO
11215:1998)
Ta slovenski standard je istoveten z: EN ISO 11215:1998
ICS:
67.180.20 Škrob in izdelki iz njega Starch and derived products
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

INTERNATIONAL ISO
STANDARD 11215
First edition
1998-05-15
Modified starch — Determination of adipic
acid content of acetylated di-starch
adipates — Gas chromatographic method
Amidons et fécules modifiés — Détermination de la teneur en acide
adipique dans les adipates de diamidon acétylés — Méthode par
chromatographie en phase gazeuse
A
Reference number
ISO 11215:1998(E)
ISO 11215:1998(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide
federation of national standards bodies (ISO member bodies). The work of
preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which
a technical committee has been established has the right to be represented
on that committee. International organizations, governmental and non-
governmental, in liaison with ISO, also take part in the work. ISO
collaborates closely with the International Electrotechnical Commission
(IEC) on all matters of electrotechnical standardization.
Draft International Standards adopted by the technical committees are
circulated to the member bodies for voting. Publication as an International
Standard requires approval by at least 75 % of the member bodies casting
a vote.
International Standard ISO 11215 was prepared by Technical Committee
ISO/TC 93, Starch (including derivatives and by-products).
Annexes A to C of this International Standard are for information only.
©  ISO 1998
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced
or utilized in any form or by any means, electronic or mechanical, including photocopying and
microfilm, without permission in writing from the publisher.
International Organization for Standardization
Case postale 56 • CH-1211 Genève 20 • Switzerland
Internet [e-mail]
X.400 c=ch; a=400net; p=iso; o=isocs; s=central
Printed in Switzerland
ii
©
INTERNATIONAL STANDARD  ISO ISO 11215:1998(E)
Modified starch — Determination of adipic acid content of
acetylated di-starch adipates — Gas chromatographic method
1  Scope
This International Standard specifies a method for the gas chromatographic determination of total adipic content
and free adipic acid content of acetylated di-starch adipates.
2  Normative references
The following standards contain provisions which, through reference in this text, constitute provisions of this
International Standard. At the time of the publication, the editions indicated were valid. All standards are subject to
revision, and parties to agreements based on the International Standard are encouraged to investigate the
possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain
registers of currently valid International Standards.
ISO 1666:1996, Starch — Determination of moisture content — Oven-drying method
ISO 3696:1987, Water for analytical laboratory use — Specification and test methods
3  Principle
The test portion is dispersed in moderately concentrated sodium hydroxide solution, to hydrolyse fully the adipate
from the starch. After acidification, the free adipic acid is extracted with ethyl acetate. The ethyl acetate is removed,
and the dry residue is silylated. An aliquot portion of this solution is injected into a gas chromatograph equipped with
a capillary column. Pimelic acid is used as internal standard.
Free adipic acid is extracted by washing out the starch with water, acidifying the extract, and extracting the free acid
with ethyl acetate.
The determination is performed by silylation and gas chromatography as described above.
4  Reagents and materials
Use only reagents of recognized analytical grade.
4.1 Water, complying with at least grade 3 in accordance with ISO 3696.
4.2 Waxy maize starch, commercial grade.
NOTE  Waxy maize starch is chosen as the base material, as it represents the bulk of starch adipate on the market. This may
be substituted with another native starch, if appropriate.
©
ISO
ISO 11215:1998(E)
4.3 Adipic acid solution, r(C H O ) = 50,0 mg/l.
6 10 4
4.4 Pimelic acid solution, r(C H O ) = 50,0 mg/l.
7 12 4
4.5 Sodium hydroxide solution, c(NaOH) = 4 mol/l.
4.6 Hydrochloric acid, concentrated, c(HCl) = 12 mol/l.
4.7 (C H O ).
Ethyl acetate
4 8 2
4.8 Nitrogen gas, purity 99 %.
4.9 Acetonitrile
4.10 Silylation reagent: bis(trimethylsilyl)trifluoroacetamide (BSTFA) which includes 1 % trimethylchlorosilane
(TMCS).
4.11 Helium gas, purity 99,9999 % (e.g. grade N60).
4.12 Hydrogen gas, purity 99,99 % (e.g. grade N400 or better).
4.13 Air, purity 99,999 % (e.g. grade S).
5  Apparatus
Usual laboratory apparatus and, in particular, the following.
5.1 Glass reaction tubes, 100 mm x 16 mm, with screw caps fitted with polytetrafluoroethylene (PTFE) covered
rubber seals resistant to concentrated hydrochloric acid (4.6).
5.2 Pipettes, adjustable, of 1,00 ml and 5,00 ml capacity, accurate to 0,01 ml.
NOTE  The pipettes should be tested to see if they comply to manufacturer's tolerance. Calibration may be required.
5.3 Rotary shaker.
5.4 Pasteur pipettes.
5.5 Heating device, capable of being maintained at (30 ± 2) °C.
1)
5.6 Evaporation device, based on solvent removal with a stream of nitrogen (e.g. Pierce Reacti-Vap III) .
5.7 Ultrasonic bath, power 120 W.
5.8 Gas chromatograph, accommodating capillary columns, fitted with a flame ionization detector, on-column
injector, and a computer integrator. See annex A for typical conditions for chromatography.
5.9 Sieve, 800 μm.
5.10 Blade mill.
5.11 Laboratory centrifuge, capable of operating at a radial acceleration of 1 100 g .
n
___________
1)
Pierce Reacti-Vap III is an example of suitable apparatus available commercially. This information is given for the
convenience of users of this International Standard and does not constitute an endorsement by ISO of this apparatus.
©
ISO
ISO 11215:1998(E)
6  Sampling
It is important that the laboratory receive a sample which is truly representative and has not been damaged or
changed during transport or storage.
Sampling is not part of the method specified in this International Standard.
7  Preparation of test sample
Sieve the laboratory sample through the 800 μm sieve (5.9). If the material does not pass through the sieve, then
grind the sample with a blade mill (5.10) until it passes completely through the 800 μm sieve. Homogenize the
sample.
8  Procedure
8.1  Calibration for total adipic acid content
8.1.1 Weigh, to the nearest 0,1 mg, approximately 50 mg of waxy maize starch (4.2) into each of four glass
reaction tubes (5.1).
8.1.2 Into one tube, pipette (5.2) 1,00 ml of adipic acid solution (4.3) and into the others 0,75 ml, 0,50 ml and
0,25 ml, respectively, of adipic acid solution (4.3).
8.1.3 Adjust the volume in each tube to 1,5 ml with water (4.1) and add 1,00 ml of pimelic acid solution (4.4) to
each tube. Each tube then contains 50 μg of pimelic acid, and 50,0 μg, 37,5 μg, 25,0 μg and 12,5 μg respectively of
adipic acid.
NOTE  It is possible that pimelic acid contains some adipic acid. If this is proven, a fifth tube should be prepared in a similar
fashion but without addition of adipic acid solution (4.3).
8.1.4 Agitate the tubes manually to disperse the starch fully. Add 2,5 ml of sodium hydroxide solution (4.5).
8.1.5 Seal the tubes well and place on the rotary shaker (5.3) for 5 min.
8.1.6 Remove the tubes and, with cooling, add 1,0 ml of hydrochloric acid (4.6). Mix well.
8.1.7 Add 5 ml of ethyl acetate (4.7). Seal the tubes tightly and shake vigorously for 1 min.
8.1.8 Let the tubes stand until good phase separation is achieved. With a Pasteur pipette (5.4), transfer the
supernatant layer (ethyl acetate) to a clean screw-top tube.
Make sure that none of the aqueous layer is carried over with the organic layer.
8.1.9 Place the tubes in the heating device (5.5) set at 30 °C, and evaporate the ethyl acetate completely under a
stream of nitrogen (4.8) with the evaporation device (5.6).
8.1.10 Repeat steps 8.1.7 to 8.1.9 three times more, accumulating the dried residue in the same tube.
8.1.11 Dissolve the total residue in 0,6 ml of acetonitrile (4.9) and place the closed tubes in the ultrasonic bath
(5.7) for 2 min.
8.1.12 Add 0,3 ml of the silylation reagent (4.10). Close the tubes and homogenize in the ultrasonic bath for 2 min.
8.1.13 Place the tubes in the heating device (5.5) set at 30 °C, for 30 min to complete derivatization.
©
ISO
ISO 11215:1998(E)
8.1.14 Inject 0,5 μl of the solution into the gas chromatograph. See annex A for typical conditions for
chromatography.
8.2  Total adipic acid content
8.2.1 Weigh, to the nearest 0,1 mg, approximately 50 mg of the prepared test sample into a glass reaction tube
(5.1).
8.2.2 Add 1,5 ml of water (4.1) a
...