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IS 15108 (2002): Pretreatment of Samples for

Physico-Chemical Analyses [FAD 7: Soil Quality and
Gertilizers]

! $ ' +-
Satyanarayan Gangaram Pitroda
Invent a New India Using Knowledge

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BharthariNtiatakam
Knowledge is such a treasure which cannot be stolen
 IS 15108:2002
ISO 11464:1994

Indian Standard
PRETREATMENT OF SAMPLES FOR
PHYSICO-CHEMICAL ANALYSES

ICS 13.080

.,

42 BIS 2002

BUREAU OF INDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

March 2002 Price Group 5

Soil Quality and Improvement Sectional Committee, FAD 27

NATIONAL FOREWORD

This Indian Standard which is identical with ISO 11464:1994 Soil quality Pretreatment of samples
for physico-chemical analyses issued by the International Organization for Standardization ( ISO )
was adopted by the Bureau of Indian Standards on the recommendation of the Soil Quality and Improvement
Sectional Committee and approval of the Food and Agriculture Division Council.

In the adopted standard, certain terminology and conventions are not identical to those used in Indian
Standards. Attention is particularly drawn to the following:

a) Wherever the words International Standard appear referring to this standard, they should be
read as Indian Standard.

b) Comma (, ) has been used as a decimal marker while in Indian Standards, the current practice
is to use a point ( . ) as the decimal marker.

CROSS REFERENCES

/international Standard Corresponding Indian Standard Degree of Equivalence

1S0 565:1990 Test sieves Metal IS 460 ( Part 1 ) : 1985 Test Equivalent
wire cloth, perforated metal plate sieves : Part 1 Wke cloth test sieves
and electroformed sheet Nominal ( third revision)
sizes of openings

In reporting the result of a test or analysis made in accordance with this standard, if the final value,
observed or calculated, is to be rounded off, it shall be done in accordance with IS 2:1960 Rules for
rounding off numerical values ( revised ).
 IS 15108:2002
ISO 11464:1994

Indian Standard
PRETREATMENT OF SAMPLES FOR
PHYSICO-CHEMICAL ANALYSES

1 Scope temperature not exceeding 40 C, or freezedried (see

5.2 ). If necessary, the soil sample is crushed while
This International Standard specifies the pretreat- still damp and friable and again after drying (see 5.3).
ment required for soil samples that are to be sub The soil is sieved (see 5.4) and the fraction smaller
jetted to physico-chemical analyses and describes the than 2 mm is divided into portions mechanically or by
following five types of pretreatment of samples: dry- hand, to enable representative subsampling for analy-
ing, crushing, sieving, dividing and milling. sis (see 5.5). If small subsamples (< 2 g) are required
for analysis, the size of the particles of the fraction
The pretreatment procedures described in this inter- smaller than 2 mm is further decreased (see 5.6 ). The
national Standard are not applicable if they affect the necessaty procedures are given in the flow diagram
results of the determinations to be made. In general, in figure 1.
International Standards for analytical methods will
state when it is necessaty to adopt other procedures. NOTES

1 A drying temperature of 40 C in an oven is preferable

2 Normative reference to air drying at room temperature because the increased
speed of the drying limits changes due to microbial activity.
The following standard contains provisions which,
2 It should be noted that every type of pretreatment will
through reference in this text, constitute provisions
have an influence on several soil properties. I
of this International Standard. At the time of publi-
cation, the edition indicated was valid. All standards 3 Storing soil samples, including samples that are as re-
are subject to revision, and parties to agreements ceived, air dried, refrigerated or stored in the absence of
based on this International Standard are encouraged light, for a long time may have an influence on a number
to investigate the possibility of applying the most re- of soil parameters, especially solubilities of both inorganic
cent edition of the standard indicated below. Mem- and organic fractions. See [1].
bers of IEC and ISO maintain registers of currently
4 Special measures should usually be taken for samples
valid International Standards.
from contaminated soils. It is important to avoid contact
with the skin and special measures should be taken when
ISO 565:1990, Test sieves Metal wire cloth, per- drying such samples (ventilation, air removal, etc.). Samples
forated metal plate and electroformed sheet Nom- may be hazardous because of the presence of chemical
inal sizes of openings. contaminants etc., fungal spores, or pathogens such as
Ieptospirosis, and appropriate safety precautions should be
taken.
3 Principle
5 In this International Standard, it is generally assumed
Soil samples are dried in the air, or in an oven at a that at least 500 g of fresh soil is available.

1
 ,
,%

IS 15108:2002
ISO 11464:1994

t
I Sampledescription I
I (5.1) I

Drying of the complete sample

.mEEzlEEzl

Removal and weighing of gravel, glass, roots, etc.

I (5.3.1) I

Sieving 2 mm
(5.3.2 and 5.4)

m m
1

,
yes

No

+- w
Subdividing the sample

=-=

t
I 4

Subdividing the sample

mm=

Figure 1 Diagram for sample pretreatment

2
 - e%

IS 15108:2002
ISO 11464:1994

4 Apparatus have resulted in segregation of different sized par-

ticles) has been carried out.
It is essential that the apparatus used does not add
or remove any of the substances under investigation WARNING Take special precautions with sam-
(e.g. heavy metals). If the use of certain equipment ples from potentially hazardous soil. Avoid any
and/or materials is not permitted in pretreatment of contact with the skin and make special provisions
samples required for particular physico-chemical concerning drying (discharge of air, ventilation
analysis, this should be mentioned in the relevant etc.).
International Standards on analysis (see note 6).
NOTES

4.1 Drying oven, thermostatically controlled, with 7 Care should be taken to avoid contamination of the
forced ventilation, capable of maintaining a tempera- sample via the air or by dust (e.g. from the ambient labora-
ture of 40 C * 2 C. tory atmosphere or between samples stored or processed
close to one another).
4.2 Freeze-drier, optional.
8 It is recommended that pretreatment of soil material al-
ways be performed in a separate room used only for this
4.3 Crusher(s), mill(s), mortar and pestle, wooden purpose.
or other soft-faced hammer (see note 6).
9 If the sample has a dust-like consistency, part of it may
be lost and this may alter its physico-chemical properties.
4.4 Plate sieve, complying with ISO 565, with an
aperture of 2 mm.
5.1 Sample description
4.5 Mechanical mixer(s).
Examine the sample as received and record the de-
scription according to a nationally, or preferably inter-
4.6 Mechanical sieve shaker, optional (see note 6).
nationally, accepted terminology, including details of
extraneous matter, remains of vegetation, and other
4.7 Subsampler or sample divider, (see note 6). noticeable or relevant features.

4.8 Mesh sieve, complying with ISO 565, with ap- 5.2 Drying
ertures of 250 ~m or of the size specified in the rel-
evant test method. Dty the complete sample in air or in a ventilated dry-
ing oven from which the moist air has been removed
4.9 Analytical balance, readable and accurate to or in a freeze dryer. Depending on the chosen method
0,1 g. of drying, follow the procedure set out in 5.2.1, 5.2.2
or 5.2.3. Dry until the loss in mass of the soil sample
4.10 Balance, readable and accurate to 1 g. is not greater than 5 YO (nAm) per 24 h.

NOTE 6 The apparatus to be used is not specified in de- To accelerate the drying process, break down the size
tail, although drawings of some suitable items of equipment of larger clods (greater than 15 mm) during the pro-
are provided in figures A. 1 to A,4. Most comparable national cess. When samples are dried in air, crush them
standards contain detailed equipment specifications and lightly by hand using a wooden hammer or a mortar
these may be used, provided they meet the basic perform- and pestle. When samples are dried in an oven, re-
ance requirements indicated in this International Standard.
move them temporarily from the oven and treat them
in the same way. This procedure also makes it easier
5 Procedure to separate the particles greater than 2 mm.

The procedures for drying, fraction separation and size Freeze-d~ing has the advantage that the sample to
reduction are set out in 5.2 and 5.3. At several stages be dried rarely dries into clods; it usually breaks up
in the procedure, the analyst will be required to make into parts.
decisions, referring in particular to whether size frac-
tions are to be combined or treated separately: this 5.2.1 In air
will depend on the nature of the soil and the objec-
tives of the analytical programme. Spread all the material, in a layer not thicker than
15 mm, on a tray which does not absorb any moisture
The sample shall be rehomogenized after any separ- from the soil and which does not cause con-
ation, sieving, crushing or milling operation (that may tamination.

3
 ,*

IS 15108:2002
ISO 11464:1994
--4

It is essential that direct sunlight be avoided. b) crush the entire sample (see 5.3.3). --

NOTE 10 Direct sunlight could create large temperature

5.3.3 Size reduction of material greater than
differences in the sample, especially between the partly or
2 mm
completely dried top layer and the lower layers which are
still wet. :,
Crush the dried soil into particles no larger than
2 mm using suitable apparatus (4.3). The necessaw .,+
5.2.2 In a drying oven
apparatus shall be adjusted or used in such a way that
crushing of the original particles (concretions and
Spread all the material, in a layer not thicker than
conglomerates) is minimized. {
15 mm, on a tray which does not absorb any moisture
from the soil and which does not cause con-
tamination. Put the tray in the drying oven (4.1) and 5.4 Sieving
dry at a temperature that is not higher than 40 C.
Sieve the dried and crushed sample by hand or using
a mechanical shaker. Remove and weigh stones and
5.2.3 Freeze-drying
fresh plant fragments, glass, etc. from the fraction
Dry all the material in the freeze-drier (4.2) according remaining on the sieve (see 5.3.1). Crush any clods
to the procedures recommended by the manufacturer left behind on the sieve separately and return them
of the apparatus. to the sample. Collect all or part of the material left
on the sieve and treat it separately if required (see
NOTE 11 The drying time depends on the type of ma- note 12). Take care to minimize the amount of fine
terial, the thickness of the layer, the initial moisture content material adhering to the separated stones, etc.
of the material and of the air, and on the rate of ventilation.
In a drying oven, the drying time for sandy soils is normally
not more than 24 h and for clay soils more than 48 h. For 5.5 Subsampling
soils containing a large proportion of fresh organic matter
(e.g. plant roots etc.), 72 h to 96 h may be required. Subsampling is necessary when the sample cannot
be stored (Iaboratoty sample and archive sample) or
used (test sample) completely, because of its size. For
5.3 Crushing and removal of coarse
the preparation of a laboratory sample, divide the
materials dried, crushed and sieved sample (now <2 mm) into .- -

representative portions of 200 g to 300 g according

5.3.1 Separation of stones, etc. to 5.5.1 or 5.5.2 or another suitable procedure. For the
preparation of a test sample, split up the laboratory
If soil samples have dried into clods, crushing is nec- sample into representative portions until the required
essary. Before crushing, remove stones, fragments sizes of samples are obtained. Avoid the production
of glass and rubbish etc., which are larger than of dust as much as possible.
2 mm by sieving (5.4) and hand picking (see note 12).
Take care to minimize the amount of fine material NOTE 13 It may be necessary to mill the material (5.6)
adhering to the separated stones, etc. Determine and between subsampling stages, to ensure homogeneity as
record the total mass of the dried sample, and the the mass of the subsample is decreased. The procedures
mass of any material removed at this stage. described in 5.5.1 and 5.5.2 may be used to produce
subsamples/test portions of the materials less than 2 mm
NOTE 12 If the material under examination is a contami- and not less than 2 g in mass.
nated soil or waste, the analyst may wish to grind the
complete sample, including for example pieces of slag, to Select the method of subsampling (5.5.1, 5.5.2 or
pass the 2 mm mesh sieve. 5.5.3) according to the nature of the sample, the re-
quirements of the subsequent determinations and the
5.3.2 Separation of material naturally less than equipment available.
2 mm
5.5.1 Subsampling by hand (quartering)
After removal of extraneous matter, either
Mix the soil sample thoroughly using a suitable me-
a) sieve out the material smaller than 2 mm, re- chanical mixer (4.5) and spread it into a thin layer on
cording the masses greater and smaller than a tray of a type which will not influence the compo-
2 mm, crush the material greater than 2 mm (see sition of the sample. Separate the soil into four equal
5.3.3) and recombine the fractions using a me- portions (quadrants). Combine two of the four
chanical mixer (4.5); or portions diagonally, rejecting the other two. Repeat

4
 _d+

IS 15108:2002
ISO 11464:1994

this procedure until the desired amount of soil is ob- Mill a representative subsample (see 5.5) of the dried,
tained. pulverized and sieved soil until the complete sub
sample just passes through a sieve of 250 ~m or a
5.5.2 Use of the sample divider size otherwise specified in the test method (see 4.8).

A suitable example of a sample divider of the If more than one analysis is to be made , sufficient
multiple-slot type (riffle box) is shown in figure A,2. material should be ground to the smallest particle size
This splits the sample into two equal parts. specified, to enable all the analyses to be made on
this one subsample.
NOTE 14 The dimensions of the equipment should be
chosen in such a way as to suit the amount and particle size NOTES
of the materials to be divided (see figure A.2 and table A.1).
15 For the determination of some parameters based on
chemical extractions, milling is not permitted because it in-
5.5.3 Mechanical subsempiing
creases the specific surface and thus the reactivity of the
sample,
A varkty of appropriate equipment for subsampling is
available, often manufactured according to national 16 If required, the fraction greater than 2 mm can be
standards. These may be used for subsampling in ac- milled and mixed with the fraction less than 2 mm before
cordance with the appropriate national standard and chemical analysis is performed.
the manufacturers instructions.
6 Test report
An example of mechanical subsampling equipment is
illustrated in figure A.3. This operates according to the The test report shall include the following information:
following procedure.
a) a reference to this International Standard;
Pdur the soil sample into the funnel of the subsampler
(figure A.3) and screw the sample bottles into place.
b) which processes, procedures and apparatus were
Start the subsampler. After subsampling, pour the
used, including the drying temperature;
contents of the bottles into other sample containers.
Repeat this procedure, if necessary, with the contents
c) a complete identification and description of the
of one of the containers until the desired amount of sample, including the presence (and if necessav
soil is obtained. The material should be relative masses) of stones, fragments of glass,
rehomogenized between each stage of subsampling.
detritus, etc., odour (if any) and colour;
The contents of more than one container may be
thoroughly mixed and used for subsequent phases of d) any details not specified in this International
the subsampling routine. Standard or which are optional, and any other
factors which may have affected the results.
5.6 Miiiing

If a test sample of less than 2 g is to be taken for the

analysis, it is essential to further comminute the frac-
tion less than 2 mm.

5
 .. ,
J%_

IS 15108 :2OO2
ISO 11464:1994

Annex A
(informative)

Examples of apparatus

Examples of apparatus given in clause 4 are illustrated in figures A.1 to A.4 .

The design of a mechanical sample divider illustrated in figure A.2 has been found satisfactory but alternative de-
signs may be employed, provided that the essential requirements are fulfilled.

M
7lr#r
. ..> {.+.) --- ...

,-: ...

~ =&$ . .
+
% h\\\\\\\\\\\\\\\\\\+
,.
y.;
.p:;
.,,,:
....
.,,,..
,.
..:.,.
.,..:,,
.:,
,.,

Figure A.1 Example of a mechanical soil crusher

6
 IS 15108:2002
ISO 11464:1994

/-
/-

Figure A.2 Example of a mechanical sample divider

Table A.1 Dimensions of a mechanical sample divider

All !?,
-,7
riimancinnc
!l, -,! 1-,
aveant p.
nws.
A
n,
arn yprlal
1
snnrnvimatn
l...
nnlv
01!, .

Maximum
Number of Internal dimensions of the boxes (three
size of Internel dimensions
slots required)
sample
A B c D E F
mm mm m In mm mm mm mm

40 8 50 150 70 230 150 400

20 10 30 130 40 150 100 300

10 12 15 80 30 120 90 200

5 12 7 20 i5 50 50 90

2 12 5 20 15 50 50 90
IS 15108:2002
ISO 11464:1994 .
i
I

1- -

bringbeti I

Sample bottle

u
//////////////////////////////// /

Figure A.3 Example of a mechanical subsampler

...

. .

>

....;
.....
,.. ..
.....
..
....
.: ...

Figure A.4 Example of a mechanical mill

 - e+<

IS 15108:2002
ISO 11464:1994

Annex B
(informative)

Bibliography

[1] BARTLE~, R.J. Oxidation-reduction status ofaerobic soils (Chapter 5), in: Chemisty of the soil environment,
pp. 77-103. American Society of Agronomy. Soil Science Society of America. ASA Special Publication
No. 40 (1981), Madison, Wisconsin.

,.

9
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of BIS Catalogue and Standards : Monthly Additions.

This Indian Standard has been developed from Doc : No. FAD 27 ( 1036 ).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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