INTERNATIONAL ISO

STANDARD 939

Second edition
2021-01

Spices and condiments —

Determination of moisture content
Épices et condiments — Détermination de la teneur en eau

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Reference number
ISO 939:2021(E)

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Contents Page

Foreword......................................................................................................................................................................................................................................... iv
1 Scope.................................................................................................................................................................................................................................. 1
2 Normative references....................................................................................................................................................................................... 1
3 Terms and definitions...................................................................................................................................................................................... 1
4 Principle......................................................................................................................................................................................................................... 1
5 Reagents......................................................................................................................................................................................................................... 1
6 Apparatus...................................................................................................................................................................................................................... 2
7 Sampling......................................................................................................................................................................................................................... 2
8 Procedure..................................................................................................................................................................................................................... 2
8.1 Preparation of apparatus................................................................................................................................................................ 2
8.2 Preparation of test sample............................................................................................................................................................. 2
8.3 Test portion................................................................................................................................................................................................. 2
8.4 Determination.......................................................................................................................................................................................... 2
9 Expression of results......................................................................................................................................................................................... 3
10 Test report.................................................................................................................................................................................................................... 3
Annex A (informative) Example of entrainment distillation apparatus........................................................................... 4
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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.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www​.iso​.org/​directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www​.iso​.org/​patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
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World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www​.iso​.org/​
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This document was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 7,
Spices, culinary herbs and condiments. ISO 939:2021
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This second edition cancels and replaces the first edition (ISO 939:1980), which has been technically
c42738c52acd/iso-939-2021
revised. The main changes compared with the previous edition are as follows:
— the Introduction has been deleted;
— definition 3.1 has been revised;
— in 8.1, “a potassium dichromate sulphuric acid cleaning solution” has been replaced by “a laboratory-
grade detergent”;
— in 8.4, “asbestos cloth” has been replaced by “glass fibres, stone wool or ceramic fibres”;
— in 8.4, the instruction to immerse the receiver in water at room temperature has been changed from
“15 min” to “45 min”;
— in Annex A b), the inner tube diameter has been changed from “9,5 to 12,5 mm” to “5 mm to 12,5 mm”.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www​.iso​.org/​members​.html.

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INTERNATIONAL STANDARD ISO 939:2021(E)

Spices and condiments — Determination of moisture

content

1 Scope
This document specifies an entrainment method for the determination of the moisture content of spices
and condiments.

2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 948, Spices and condiments — Sampling
ISO 2825, Spices and condiments — Preparation of a ground sample for analysis

3 Terms and definitions

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For the purposes of this document, the following terms and definitions apply.
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ISO and IEC maintain terminological databases for use in standardization at the following addresses:
ISO 939:2021
— ISO Online browsing platform: available at https://​w ww​.iso​.org/​obp
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— IEC Electropedia: available at http://​c42738c52acd/iso-939-2021
w ww​.electropedia​.org/​
3.1
moisture content
content of water extracted or collected in accordance with the method prescribed in this document
Note 1 to entry: Moisture content is expressed as a percentage by mass.

4 Principle
Determination of the amount of water entrained by azeotropic distillation, using an organic solvent
immiscible with water, and collected in a graduated tube.

5 Reagents

5.1 Toluene.

Saturate the toluene by shaking with a small quantity of water and distil. Use the distillate for the
determination of the moisture.
NOTE Different solvents are used for the determination of moisture.

Unless otherwise specified in the International Standard giving specifications for the spice or condiment
in question, toluene shall be the solvent used for the determination.

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6 Apparatus
Distillation apparatus (a suitable form of apparatus is described in Annex A and shown in Figure A.1),
comprising the following components fitted together by means of ground glass joints.

6.1 Flask, short-necked, of capacity at least 500 ml.

6.2 Reflux condenser.

6.3 Receiver, with a graduated tube, interposed between the flask and the condenser.

6.4 Analytical balance.

7 Sampling
Sample the material by the method specified in ISO 948.

8 Procedure

8.1 Preparation of apparatus

Clean the entire apparatus with a laboratory-grade detergent to minimize the adherence of water
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droplets to the sides of the condenser and the receiver.
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Rinse thoroughly with water and dry completely before use.
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8.2 Preparation of testhttps://standards.iteh.ai/catalog/standards/sist/87846e25-db92-4ccf-a5de-
sample
Prepare the test sample by the method specified c42738c52acd/iso-939-2021
in ISO 2825.

8.3 Test portion

Weigh, to the nearest 0,01  g, about 40  g of the test sample (see 8.2), such that the quantity of water
collected will not exceed 4,5 ml.

8.4 Determination
Transfer quantitatively the test portion (see 8.3) to the distillation flask (6.1), add sufficient toluene
(5.1) (about 75  ml in all) to cover the sample completely and swirl to mix. Assemble the apparatus
and fill the receiver (6.3) with the toluene by pouring it through the condenser (6.2) until it begins to
overflow into the distillation flask. If necessary, insert a loose cotton plug in the top of the condenser
or attach to it a small calcium chloride tube to prevent condensation of atmospheric moisture within
the condenser tube. In order to control refluxing, wrap the flask and tube leading to the receiver with
glass fibres, stone wool or ceramic fibres. Heat the flask so that the distillation rate is about 100 drops
per minute. When the greater part of the water has distilled over, increase the distillation rate to
about 200 drops per minute and continue until no more water is collected. Purge the reflux condenser
occasionally during the distillation with 5  ml portions of the toluene to wash down any moisture
adhering to the walls of the condenser. The water in the receiver may be made to separate from the
toluene by occasionally moving a spiral copper wire up and down in the condenser and receiver, thus
causing the water to settle at the bottom of the receiver. Reflux until the water level in the receiver
remains unchanged for 30 min and then shut off the source of heat.
Flush the condenser with toluene as required, making use of the spiral copper wire to discharge any
moisture droplets. Immerse the receiver in water at room temperature for at least 45 min or until the
toluene layer is clear. Then read the volume of water.

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9 Expression of results
The moisture content (w), in percentage by mass, can be expressed by Formula (1):
100×V
w= (1)
m
where

  V is the volume of water collected, in ml;

  m is the mass of the test portion, in g.

It is assumed that the density of water is 1 g/ml exactly.

10 Test report
The test report shall show the method used and the result obtained. It shall also mention all operating
conditions not specified in this document, or regarded as optional, as well as any circumstances that
may have influenced the result.
The report shall include all details required for complete identification of the sample.

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Annex A
(informative)

Example of entrainment distillation apparatus

The apparatus consists of a glass flask heated by a suitable means and provided with a reflux condenser
discharging into a receiver connected to the flask. The connections between the receiver, the condenser
and the flask are interchangeable ground glass joints. The receiver serves to collect and measure the
condensed water, and to return the solvent to the flask. The assembly of the apparatus is shown in
Figure A.1 and the various components are described below.
a) Flask, of capacity 500 ml, made of heat-resistant glass, well annealed, as free as possible from striae
and defects, and similar to the shape shown in Figure A.1.
b) Reflux condenser, water cooled, made of glass, having a jacket approximately 400 mm long and an
inner tube of diameter 5 mm to 12,5 mm. The tip of the condenser to be inserted in the receiver
may be ground off at an angle of 30° from the vertical axis of the condenser. When inserted into the
receiver, the tip of the condenser is 6 mm to 7 mm above the surface of the liquid in the receiver
after distillation conditions have been established.
c) Receiver, of capacity 5 ml, made of heat-resistant glass, well annealed and as free as possible from
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striae and similar defects, provided with ground glass joints, with the shape, dimensions and
tolerances given in Figure A.1, and consisting essentially of the upper chamber, together with the
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tube and ground joint leading to the flask, and the graduated tube. The graduated portion has a
capacity of 5 ml when filled to the highest graduation mark.
ISO 939:2021
The scale covers the range of 0 ml to 5 ml and is graduated at intervals of 0,1 ml. The graduation
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are numbered and carried completely round the tube. The
graduation marks midway between the numbered marks are carried three-quarter way, and the
remaining marks are carried half-way, around the tube. The error at any indicated capacity does
not exceed 0,05 ml.
d) Heat source, either an oil bath or an electric heater provided with a sliding rheostat or other means
of heat control.
The temperature of the oil in the bath should not be very much higher than the boiling point of
toluene.
e) Copper wire, long enough to extend through the condenser and with one end twisted into a spiral.
The diameter of the spiral is such that it fits snugly within the graduated portion of the receiver
and yet can be moved up and down.

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Dimensions in millimetres

Key
1 reflux condenser (6.2) iTeh STANDARD3 PREVIEW
graduated tube
2 receiver (6.3) 4 flask (6.1)
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NOTE Volume: 5 ml, graduations: 0,10 ml.
ISO 939:2021
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Figure A.1 — Assembly of the entrainment distillation apparatus
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