International S andard

INTERNATIONAL ORGANIZATION FOR STANDARDIZATION~ME~YHAPOAHAR OPI-AHM3ALWlR I-IO CTAH~APTM3ALWl.ORGANISATiON INTERNATIONALE DE NORMALISATION

Agricultural food products - Determination of crude fibre

content - Modified Scharrer method
Produits agricoles alimen taires - Determination de l indice d’insoluble dit ocellulosique>~ - AMhode de Scharrer modifike

First edition - 1981-06-01

UDC 664: 543.868 Ref. No. ISO 6541-1981 (EI

Descriptors
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of
national Standards institutes (ISO member bedies). The work of developing Inter-
national Standards is carried out through ISO technical committees. Every member
body interested in a subject for which a technical committee has been set up 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.

Draft International Standards adopted by the technical committees are circulated to

the member bedies for approval before their acceptance as International Standards by
the ISO Council.

International iTeh STANDARD PREVIEW

Standard ISO 6541 was developed by Technical Committee ISO/TC 34,
Agricultural food products, and was circulated to the member bodies in September
1979. (standards.iteh.ai)
lt has been approved by the member bodies of the following ISO 6541:1981
countries :
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Austria Hungary 1c781a9fc1d1/iso-6541-1981
Portugal
Brazil India Romania
Bulgaria Israel South Africa, Rep. of
Canada Korea, Rep. of Spain
Cyprus Libyan Arab Jamahiriya Thailand
Czechoslovakia Malaysia Turkey
Egypt, Arab Rep. of Mexico United Kingdom
Ethiopia Netherlands USSR
France New Zealand Y ugoslavia
Germany, F. R. Poland

No member body expressed disapproval of the document.

This International Standard has also been approved by the International Union of Pure
and Applied Chemistry (IUPAC).

NOTE - This International Standard is based on Standard No. 113 of the International Associ-
ation for Cereal Chemistry ( ICC).

International Organkation for Standardkation, 1981

Printed in Switzerland
INTERNATIONAL STANDARD ISO 6541-1981 (E)

Agricultural food products - Determination of crude fibre

content - Modified Scharrer method

1 Scope 6.1 Scharrer reagent, consisting of a mixture having the

following composition :
This International Standard specifies a conventional method for
the determination of the crude fibre content of agricultural food - acetic acid Solution, prepared by diluting 730 g
products. of 96 % (mlm) glacial acetic acid with water to
loow 900 ml
- nitric acid, concentrated, ~20 = 138 g/ml 60 ml
2 Field of application
- trichloroacetic acid, crystalline 24 g
The method is applicable to cereals and cereal products, as well
as to certain products containing less than 1 % of crude fibre,
6.2 Acetone.
for example yeasts, which are excluded from the field of
application of ISO 5498.
6.3 Diethyl ether.
iTeh STANDARD PREVIEW
3 Reference 6.4 Sea sand, prepared as follows.

ISO 5498, Agricultural foodproducts

(standards.iteh.ai)
- Determination of crude Sieve the sand successively through sieves of wire gauze of
fibre content - General method. aperture sizes 160 Fm and 125 Pm, complying with the re-
ISO 6541:1981quirements of ISO 3310/1.
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4 Definition 1c781a9fc1d1/iso-6541-1981
Boil the sand retained by the125 Pm aperture size sieve for
30 min in 4 mol/1 hydrochloric acid Solution. Rinse the sand
crude fibre content : Conventionally, the whole of the with water until the rinsing water is free from chloride, as in-
substances which are insoluble and combustible under the dicated by the absence of a reaction with silver nitrate Solution,
operating conditions described in this International Standard. and incinerate in the muffle furnace (7.9) at 550 + 25 OC to
constant mass (usually at least 6 h are required).
The crude fibre content is expressed as a percentage by mass,
referred either to the product as received or to the dry matter 6.5 Boiling aid : crushed porcelain.
content of the product.

NOTE - In French, the term “indice d’insoluble dit cellulosique” has 7 Apparatus
been adopted for “crude fibre” rather than the alternative “cellulose
brute”. Usual laboratory apparatus, and in particular

7.1 Grinding device, easy to clean, suited to the nature of

5 Principle the product and allowing grinding of the product without caus-
ing undue heating or significant Change in the moisture
After any necessary grinding and defatting, boiling with a mix-
content.
ture of acetic acid, nitric acid and trichloroacetic acid (Scharrer
reagent). Separation and washing sf the insoluble residue on a
filter crucible. 7.2 Sieve, of metal wire cloth, aperture size 1 mm, comply-
ing with the requirements of ISO 3310/1.
Drying and weighing of the insoluble residue, and determina-
tion of the loss of mass on incineration. 7.3 Wide-mouthed vessel, provided with a condenser, for
example a conical flask of capacity 200 to 300 ml, fitted with a
reflux condenser.
6 Reagents and materials
7.4 Suction flask.
All reagents shall be of recognized analytical quality and the
water used shall be distilled water or water of at least equivalent
purity. 7.5 Water-jet pump.
ISO 6541-1981 (E)

7.6 Filter crucible, of silica, having a fritted silica plate of 9.1.3.3 Determine the dry matter content ot the test Sample
porosity grade P 100 (Pore diameter 40 to 100 Pm), prepared as (9.1.3.2) by an appropriate method.
indicated in 11 .l.

7.7 Desiccator, containing an efficient desiccant. 9.2 Test portion

Weigh, to the nearest 1 mg, a mass of the prepared test Sample

7.8 Drying oven, capable of being controlled at (9.1) corresponding to 0,05 to OJ5 g of crude fibre [i.e. 1 to 3 g
130 + 2 OC. for a crude fibre content of 5 % (n7/~1)1.

7.9 Muffle furnace, capable of being controlled at For products with low crude fibre contents, and in particular
550 I!I 25 OC. those having crude fibre contents less than 1 % (HZ/IYI), take a
test Portion of 3 g.
7.18 Analytical balance.

9.3 Determination

8 Sampling NOTE - Products rich in fatty substances r-nay require defatting

beforehand (methods are described in annex A of ISO 5498). This
Refer to the International Standard appropriate to the product Operation is not required for cereal and cereal products or for yeasts.
concerned.
9.3.1 Digestion

9 Procedure Transfer the test Portion to the digestion vessel (7.3) and sus-
pend it in about one-third of the total volume of the Scharrer
9.1 Reparation of test Sample reagent (6.1). Generally, the total volume, in millilitres, of the
iTeh STANDARD PREVIEW Scharrer reagent is numerically twenty times the mass, in
grams, of the test Portion (in no case shall the volume used be
9.1.1 Preliminary drying
(standards.iteh.ai) less than 40 ml).
In the case of products having moisture contents too high for
Using a glass rod, which shall be left in the d igestion vessel,
them to be mixed or ground as received, carry out a preliminary ISO 6541:1981
drying of the product at an appropriate temperature. In this break UP anY large lumps that may ha ve been formed.
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case, weigh the product before the preliminary drying and
1c781a9fc1d1/iso-6541-1981
again just before preparation of the test Sample (9.1.2 or 9.1.3). Carefully rinse the interior Walls of the digestion vessel with the
remaining two-thirds sf the Scharrer reagent in Order to remove
any particles of the product adhering to the Walls. Fit the con-
9.1.2 Products no% requiring grinding denser. Bring the contents of the vessel to the boil in
3 k 0,5 min and maintain boiling for 30 ? 1 min (sec 11.2).
9.1.2.1 Products of which 95 % pass through the sieve (7.2) DO not stir or Shake while boiling.
do not need to be ground before the determination.
9.3.2 Separation and washing of the residue
Mix well before taking the test Portion.
After the specified boiling period, transfer the boiling Solution
9.1.2.2 If the results are to be expressed relative to the dry to the filter crucible (7.6) prepared as described in 11 .l, and
matter content, determine beforehand the dry matter content filter under reduced pressure using the suction flask (7.4) and
of the test Sample (9.1.2.1) by an appropriate method. the water-jet pump (7.5).

Rinse the vessel and the glass rod with 50 to 70 ml portions of

9.1.3 Products requiring grinding
water (temperature between 95 and 100 “C) and quantitatively
transfer the insoluble residue to the filter crucible using a glass
Products of which less than 95 % pass through the sieve (7.2)
rod fitted with a rubber cap. Repeat the washing until the
shall be ground.
filtrate is substantially neutral to litmus Paper; this usually re-
quires 300 to 400 ml water.
9.1.3.1 If the results are to be expressed relative to the
product as received, determine beforehand the dry matter con- After washing, disconnect the water-jet pump, immediately
tent of the Sample by an appropriate method. empty the suction flask and fill the filter crucible three times
with the acetone (6.21, allowing the solvent to drain through
9.1.3.2 Grind the laboratory Sample in the grinding device under gravity. If this Operation requires too much time, apply
gentle suction to obtain a flow rate not exceeding one drop per
(7.1) so that at least 95 % of the product Passes through the
second.
sieve (7.2).

NOTE - Such a degree of fineness of grinding is unnecessary for Rinse twice with the diethyl ether (6.3) and remove the ether by
products containing Parts which are rich in cellulosic substances, such filtration under reduced pressure using the suction flask and
as grains in husk or husks of grain. water-jet pump.

2
 ISO 6!541-1981 (E)

9.3.3 Drying 10.1.2 Crude fibre content relative’ to the dry matter
Conte nt of the prod uct
Dry the filter crucible with its contents in the drying oven (7.8)
maintained at 130 + 2 OC. The crude fibre content, expressed as a percentage by mass
relative to the dry matter content of the product, is given by the
Allow them to cool to room temperature in the desiccator (7.7) formula
and weigh them rapidly to the nearest 0,5 mg. 100 100
b-n, - m2) x KX M’
S
Repeat these operations until the differente between two suc-
cessive weighings, separated by a period in the oven followed where mg, ml, m2 and MS have the same meanings as
by cooling in the desiccator, does not exceed 1 mg. in 10.1.1.

NOTE - Drying for 1 h is generally sufficient. 10.1.3 Case of preliminary drying

If a preliminary drying was carried out (sec 9.1 .l), the crude
9.3.4 Incineration fibre content, expressed as a percentage by mass relative to the
product as received, is obtained by multiplying the result
After drying, incinerate the dry residue in the muffle furnace calculated according to 10.1.1 by the ratio
(7.9) at 550 I!I 25 OC for 30 min.

Place the crucible on a refractory plate and allow to cool to

room temperature in the desiccator (7.7). Weigh rapidly to the
nearest 0,5 mg.

m4 is the mass, in grams, of the initial moist Sample before

9.3.5 Number sf determinations preliminary drying;

Carry out at least two determinations

iTeh STANDARD PREVIEW
on the same test Sample.
‘n5 is the mass, in grams, of the Sample after
(standards.iteh.ai) preliminary drying .

10.1.4 Result
10 Expression of results ISO 6541:1981
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Take as the result the arithmetic mean of the two determina-
1c781a9fc1d1/iso-6541-1981
tions (9.3.51, provided that the requirements for repeatability
IQ.1 Method of calculation and formulae (see 10.2) are satisfied.

10.1.1 Crude fibre content relative to the product as

received 10.2 Repeatability

The crude fibre content, expressed as a percentage by mass The differente between the results of the two determinations
relative to the product as received, is given by the fo lrmula (9.3.51, carried out simultaneously or in rapid succession by the
same analyst, shall not exceed :
a) for products not requiring grinding
0,l (absolute value) for crude fibre contents below
100
(ml - m2) x - 2 % (mlm);
m0
5 % (relative value) for crude fibre contents greater than
b) for products requiring grinding
2 % (mlm).
100 100 MS
(m, - m2) x - x - x 100
mg Mk

where
11 Notes on procedure

is the mass, in grams, of the test Portion (9.2);

11.1 Preparation of filter crucibles
mg

is the total mass, in grams, of the dry residue and its 11.1.1 Prior to first use, carefully clean the filter crucibles
ml
(7.6) and heat in the muffle furnace (7.91, controlled at
support after drying (9.3. ‘3);
550 + 25 OC, for 6 h.
m2 is the total mass, in grams, of the dry residue and its
support after incineration (9.3.4); 11.1.2 Spread on the crucible plate 5 to 6 g of the sea sand
(6.4). Level the surface and spread over the top 4 to 5 g of
MS is the dry matter content of the product as received, crushed porcelain (6.5) and again level the surface. Using
determined as indicated in 9.1.3.1; gentle pressure, place a perforated porcelain disc on top of
these two layers. This filling may be reused without cleaning or
Mk is the dry matter content of the test Sample, deter- preliminary treatment, but care should be taken to ensure that
mined as indicated in 9.1.2.2 or 9.1.3.3. the layers remain in their initial positions.

3
ISO 6541-1981 (El

11.2 Precautions 1

During digestion (see 9.3.11, heating shall be performed with The test report shall show the method used and the result
care in Order to avoid over-heating and too rapid boiling. The obtained (in particular, whether it is expressed relative to the
foam formed in the vessel shall never be allowed to exceed a product as received or to the dry matter content). lt shall also
height of 10 mm. Control is exerted by varying the intensity of mention all operating conditions not specified in this lnter-
heating . national Standard or regarded as optional, as weil as any
circumstances that may have influenced the result.

The test report sha ll include all the details required for the com-
plete identification of the sam ple.

iTeh STANDARD PREVIEW

(standards.iteh.ai)
ISO 6541:1981
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ISO 6541:1981
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ISO 6541:1981
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