INTERNATIONAL IS0

STANDARD 18414
First edition
1996-07-o 1

Meat and meat products - Determination

of chloride content -
Part 1:
iTeh STANDARD PREVIEW
Volhard method
(standards.iteh.ai)
ISO 1841-1:1996
Viande et produits ;j base de viande - D&termination
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enbfab93312a26/iso-1841-1-1996
chlorures -
Partie I: M&hode de Volhard

Reference number
IS0 1841-1:1996(E)
IS0 1841-1:1996(E)

Foreword

IS0 (the International Organization for Standardization) is a worldwide fed-

eration of national standards bodies (IS0 member bodies). The work of
preparing International Standards is normally carried out through IS0
technical committees. Each member body interested in a subject for
which a technical committee has been established has the right to be rep-
resented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. IS0 col-
laborates closely with the International Electrotechnical Commission (IEC)
on all matters of electrotechnical standardization.

Draft International Standards adopted by the technical committees are cir-

culated to the member bodies for voting. Publication as an International
Standard requires approval by at least 75 % of the member bodies casting
a vote.
iTeh STANDARD PREVIEW
International Standard IS0 1841-1 was prepared by Technical Committee
ISOnC 34, Agricultural food products, Subcommittee SC 6, Meat and
meat products. (standards.iteh.ai)
This first edition of IS0 1841-I cancels and replaces ISOIS0 1841 :I 981 which
1841-1:1996
has been technically revised.https://standards.iteh.ai/catalog/standards/sist/f7a5c841-dbb3-46c1-a30d-
bfab93312a26/iso-1841-1-1996
IS0 1841 consists of the following parts, under the general title Meat and
meat products - Determination of chloride con tent:

- Part 7: Volhard method

Part 2: Po ten tiome tric method

Annex A of this part of IS0 1841 is for information only.

0 IS0 1996
All rights reserved. Unless otherwise specified, no part of this publication may be repro-
duced or utilized in any form or by any means, electronic or mechanical, including photo-
copying and microfilm, without permission in writing from the publisher.
International Organization for Standardization
Case Postale 56 l CH-121 1 Geneve 20 l Switzerland
Printed in Switzerland

II
INTERNATIONAL STANDARD @ IS0 IS0 1841-1:1996(E)

Meat and meat products - Determination of chloride content -

Part I:
Volhard method

1 Scope to 100 ml of water. No more than a slight turbidity

shall be produced.
This part of IS0 1841 specifies a method for the de-
termination of the chloride content of meat and meat 4.2 Nitrobenzene or nonan-l-01.
products, including poultry, with sodium chloride con-
tents equal to or greater than I,0 % (m/m). 4.3 Nitric acid, c(HNO$ = 4 mol/l.
iTeh STANDARDMixPREVIEW 1 volume of concentrated nitric acid
(standards.iteh.ai)
(13 g/ml c ~20 G I,42
water.
g/ml) with 3 volumes of
2 Definition
ISO 1841-1:1996
4.4 Solutions for precipitation of proteins
For the purposes of this https://standards.iteh.ai/catalog/standards/sist/f7a5c841-dbb3-46c1-a30d-
part of IS0 1841, the follcw-
ing definition applies. bfab93312a26/iso-1841-1-1996
4.4.1 Reagent A

2.1 chloride content of meat and meat products: Dissolve in water 106 g of potassium hexacyanofer-
Total chloride content determined by the method rate(ll) trihydrate [K4Fe(CN)6.3H20]. Transfer quantitat-
specified in this part of IS0 1841. It is expressed as ively to a 1 000 ml one-mark volumetric flask (5.2) and
sodium chloride as a percentage by mass. dilute to the mark with water.

4.42 Reagent B

Dissolve in water 220 g of zinc acetate dihydrate

3 Principle [Zn(CH3COO)2.2H201 and add 30 ml of glacial acetic
acid. Transfer quantitatively to a 1 000 ml one-mark
Extraction of a test portion with hot water and precipi- volumetric flask (5.2) and dilute to the mark with
tation of the proteins. After filtration and acidification, water.
addition of an excess of silver nitrate solution to the
extract, and titration of this excess with potassium 4.5 Silver nitrate, standard volumetric solution,
thiocyanate solution. c(AgNOs) = 0,l mol/l.

Dissolve in water 16,989 g of silver nitrate, previously

dried for 2 h at 150 “C + 2 “C and allowed to cool in a
4 Reagents desiccator. Transfer quantitatively to a 1 000 ml one-
mark volumetric flask (5.2) and dilute to the mark with
Use only reagents of recognized analytical grade un- water.
less otherwise specified.
Store this solution in a dark glass container out of
4.1 Water, distilled and halogen-free. direct sunlight
Halogen-free test: Add 1 ml of silver nitrate [c(AgN03) 4.6 Potassium thiocyanate, standard volumetric
= 0,l mol/l] and 5 ml of nitric acid [c(HNOs) = 4 mol/l] solution, c(KSCN) = 0,l mol/l.

1
IS0 1841-1:1996(E) @ IS0

Dissolve in water about 9,7 g of potassium thio- ture of the sample material does not rise above 25 “C.
cyanate. Transfer quantitatively to a 1 000 ml one- If a mincer is used, pass the sample at least twice
mark volumetric flask (5.2) and dilute to the mark with through the equipment.
water. Standardize the solution to the nearest
0,000 1 mol/l against the silver nitrate solution (4.5) 7.2 Fill a suitable airtight container with the prepared
using the ammonium iron(lll) sulfate solution (4.7) as sample. Close the container and store in such way
indicator. that deterioration and change in composition are pre-
vented. Analyse the sample as soon as practicable,
4.7 Ammonium iron(lll) sulfate but always within 24 h of homogenization.

Prepare a saturated aqueous solution at room

temperature from the dodecahydrate
[NH4Fe(S04)2.1 2H20]. 8 Procedure
NOTE 1 If it is required to check whether the repeatability
requirement is met, carry out two single determinations in
5 Apparatus accordance with 8.1 to 8.4 under repeatability conditions.

Usual la boratory apparatus and, in particular, the fol- 8.1 Test portion
lowing.
Weigh, to the nearest 0,001 g, about 10 g of the test
5.1 Homogenizing equipment, mechanical or elec- sample and transfer it quantitatively to a conical flask
trical, capable of homogenizing the test sample. This (5.3).
includes a high-speed rotational cutter, or a mincer fit-
ted with a plate with holes not exceeding 4,5 mm in
8.2 Deproteination
diameter.
Add 100 ml of hot water (4.1) to the test portion (8.1).
5.2 One-mark volumetric flasks, of capacity
1 000 ml and 200 ml. iTeh STANDARD PREVIEW Heat the flask and its contents for 15 min in the
boiling water bath (5.6). Periodically shake the con-

5.3 Conical flasks,

(standards.iteh.ai)
of capacity about 250 ml.
tents of the flask.

Allow the flask and its contents to cool to room tem-

5.4 Burette, of capacity 25 ml or 50 ml. ISO 1841-1:1996
perature, then add successively 2 ml of reagent A
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(4.4.1) and 2 m I o f reagent B (4.4.2). Mix thoroughly
55. One-mark pipettes, of capacity 20 ml. after each addition.
bfab93312a26/iso-1841-1-1996
Allow the flask to stand for 30 min at room tem-
5.6 Boiling water bath. perature. Transfer the contents quantitatively to a
200 ml volumetric flask (5.2) and dilute to the mark
5.7 Analytical balance, capable of weighing to an with water. Mix the contents thoroughly and filter
accuracy of + 0,001 g. through a fluted filter paper.

NOTE 2 If this method is used for the determination of the

nitrate and nitrite content or if ascorbic acid is present in
6 Sampling the sample in concentrations higher than 0,l %, it is
necessary to add also 0,5 g of activated charcoal to the test
portion (8.1). After mixing reagents A and B, adjust the pH
It is important that the laboratory receive a sample to between 7,5 and 8,3 by means of a sodium hydroxide
which is truly representative and has not been dam- solution.
aged or changed during transport or storage.
8.3 Determination
Sampling is not part of the method specified in this
part of IS0 1841. A recommended sampling method Transfer 20 ml of the filtrate to a conical flask (5.3) by
is given in IS0 3100-I. means of a pipette (5.5) and add, from a graduated
measuring cylinder, 5 ml of the dilute nitric acid (4.3)
Proceed from a representative sample of at least
and 1 ml of the ammonium iron(lll) sulfate solution
200 g.
(4.7) as indicator.

Transfer 20 ml of the silver nitrate solution (4.5) to the

conical flask by means of a pipette (5.5). Add 3 ml of
7 Preparation of test sample the nitrobenzene or nonan-l-01 from a graduated
measuring cylinder and mix thoroughly. Shake vigor-
7.1 Homogenize the laboratory sample with the ap- ously to coagulate the precipitate. Titrate the contents
propriate equipment (5.1). Take care that the tempera- of the conical flask with the potassium thiocyanate

2
@ IS0 IS0 1841=1:1996(E)

(4.6) until the appearance of a persistent pink colora- 10.1 Repeatability

tion. Record the volume of the potassium thiocyanate
solution required, to the nearest 0,05 ml. The absolute difference between two independent
single test results, obtained using the same method
8.4 Blank test on identical test material in the same laboratory by the
same operator using the same equipment within a
Carry out a blank test, in accordance with 8.2 and 8.3, short interval of time, should not be greater than
using the same volume of silver nitrate solution (4.5). 0,15 % (m/m) for sodium chloride contents between
1 ,O % and 2,0 %;
0,20 % (m/m) for sodium chloride contents greater
9 Calculation
than 2,0 %.
Calculate the chloride content of the sample from the
following equation: 10.2 Reproducibility
200 100 The absolute difference between two single test re-
wcI = 0,058 44(v2 - 4) x 2. x - x c
m sults, obtained using the same method on identical
test material in different laboratories with different
Y2 - v1
= 58,44 x -XC operators using different equipment, should not be
m greater than:
0,20 % (m/m) for sodium chloride contents between
where
I,0 and 2,0 %;
wcI is the chloride content of the sample, ex- 0,30 % (m/m) for sodium chloride contents greater
pressed as sodium chloride as a percentage’ than 2,0 %.
by mass;
V, is the volume, in millilitres, of the potassium
iTeh STANDARD11PREVIEW
thiocyanate solution (4.6) used in the deter-
Test report
mination (8.3);
V2 is the volume,
(standards.iteh.ai)
in millilitres, of the potassium The test report shall specify:
thiocyanate solution (4.6) used in the blank
test (8.4); ISO 1841-1:1996 - the method in accordance with which sampling
c
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is the concentration of the potassium thio- was carried out, if known;
cyanate solution (4.6), in moles per bfab93312a26/iso-1841-1-1996
litre; - the method used;
m is the mass, in grams, of the test portion. - the test result(s) obtained; and

Report the result to the nearest 0,05 % (m/m). - if the repeatability has been checked, the final
quoted result obtained.

10 Precision It shall also mention all operating details not specified

in this part of IS0 1841, or regarded as optional,
The precision of the method has been established by together with details of any incidents which have in-
an interlaboratory test (see reference [4]), carried out fluenced the test result(s).
in accordance with IS0 5725. For the values obtained
for the repeatability limit, r, and the reproducibility The test report shall include all information necessary
limit, R, a probability level of 95 % holds. for the complete identification of the sample.

3
IS0 1841-1:1996(E)

Annex A
(informative)

Bibliography

[I I IS0 3100-I :1991, Meat and meat products - nach Par. 35 LMBG. Bestimmung des Kochsalz-
Sampling and preparation of test samples - gehaltes in Fleisch und Fleischerzeugnissen.
Part 1: Sampling. L 06.00-5, September 1980.

[2] IS0 5725:1986, Precision of test methods - De- 141 BELJAARS, P.R and HORWITZ, W, Comparison of
termination of repeatability and reproducibility for the Volhard and potentiometric methods for the
a standard test method by inter-laboratory tests determination of chloride in meat products: Col-
(now withdrawn) was used to obtain the precision laborative study. J. Assoc. Off. Anal. Chem., 68,
data. 1985, pp. 480-484.

[3] Amtliche Sammlung von Untersuchungsverfahren

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IS0 1841-1:1996(E)

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ISO 1841-1:1996
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ICS 67.120.10
Descriptors: agricultural products, animal products, food products, meat, meat products, chemical analysis, determination of content,
chlorides.

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