Soil Fertility Research Institute Punjab Lahore

SOIL FERTILITY RESEARCH INSTITUTE PUNJAB, LAHORE
AGRICULTURE DEPARTMENT, GOVERNMENT OF THE PUNJAB

Thoker Niaz baig, Lahore. Email: [email protected]
Issue
SFRI-STM-01 Standard Test Methods 15.01.2021 Revision 0.0
on
SOIL AND WATER ANALYSIS MANUAL

This Soil and Water Analysis Manual achieves the objective of implementing
the standard approved procedures for all divisional and district soil and water
testing laboratories working under the command of the Rapid Soil Fertility
Survey and Soil Testing Institute Punjab, Lahore. Both Divisional
Agricultural Chemists and District Assistant Agricultural Chemists have made
the brain storm these protocols. All these chemists have also been trained for
two days to become acquainted with all the methods, principles and
calculations involved. Even a very thorough compilation has been made in
writing of these methods, if any recent developments or flaws or faults are
revealed, the opinion will be highly appreciated.
DR MUHAMMAD AKRAM QAZI

Agricultural Chemist (Training)/Senior Instructor,
Soil Fertility Research Institute, Lahore
Reviewed & Approved by: DR SHAHZADA MUNAWAR

Prepared by: DR MUHAMMAD AKRAM QAZI
MAHDI
Designation: Agri. Chemist (Trg), Lahore
Designation: Director, SFRI, Punjab, Lahore
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SOIL AND WATER ANALYSIS MANUAL
BASIC GUIDELINES FOR LABORATORY ACTIVITIES
Real knowledge and interpretation of every context of study relies on a diligent correlation of facts
and logical conclusions from them. Efficient laboratory work will give you unique and stimulating
opportunities to learn many details about soil science. Out of such scientific insights, scientists
have established standards that unify the disciplines of soil science and the concepts that offer
existing interpretations. This is the scientific approach to be used. Here are a few tips that will help
you get an outstanding start to your laboratory work.
1. Read carefully safety precautions and laboratory rules and obey them. These will help you to
safeguard not only your interest but also those of other research workers working in the laboratory.
2. Each equipment used in the chemical laboratory is designed for a specific purpose. First become
familiar with the same and then its purpose. For example, a graduated cylinder is intended to be used as a
device for measuring the volume of a liquid and not as a reaction vessel. The objects which you shall use
are shown on the latter pages. Try to learn their names.
3. Before you come to the laboratory, thoroughly read the analysis procedure. Laboratory work is
of much greater value and you can make more efficient use of your time if you are properly
oriented with procedure.
4. Before starting the analysis make sure that all the equipment’s are properly washed and
conveniently arranged.
5. Gain self-reliance by working alone in the laboratory except when directed otherwise.
6. Talk over the analysis to get more precision research workers.
Scientists learn much by discussion with each other.
7. Keep your work bench and locker in a good order so that you can easily find what you need. If
a substance is spilled , clean it up immediately. If you don’t, your clothes, skin, books or papers
may be damaged or ruined.
8. Use care in handling laboratory materials.
9. In all analytical work you should use distilled water.
10. Be economical and specific in the use of all reagents, being costly items also become familiar
with its appearance and properties.

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CHAPTER-1
SOIL SAMPLING
A. SAMPLING IN EXPERIMENTAL PLOTS
a. CORRET PROCEDURE
A zigzag pattern across the plot gives a proper composite of 10-30 cores for a single soil sample.
b. UNSUITABLE PROCEDURE
Regular positioning of the core in plot from which samples are likely to be biased by row
applications. Analysis of these cores separately is an inefficient practice.
c. UNSUITABLE PROCEDURE
Regular positioning of core with a distinct bias towards the end of the plot, too few cores are
presented to make an accurate composite soil sample.
A B C
(correct) (unsuitable) (unsuitable)
* * * * *
*
* * *
*
* * *
*
* * *
*
* * * *
*
* * *
*

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* = X = core sampling positions
B. SAMPLING IN FIELDS.
DIVISION OF FIELD INTO AREA FOR SAMPLING
If soils are fairly uniform , an area upto 10 acre can be sampled as a unit. In case of variation, field
can be subdivided into uniform sampling units and each sampled separately in the form of
composite sample.
SOIL SAMPLING FOR VEGETABLE FIELDS
As vegetables are grown in fertile soil and root remain in furrow slice. So the depth of 0-15,
15-30 and 30-45 cm is sufficient for soil fertility evaluation.
SOIL SAMPLING FOR FIELD CROPS
As roots of crops like wheat, rice, cotton and maize etc. go deeper in sub-soil so it is necessary to
get knowledge about sub soil nutrient status and concretions. Sampling of soil for this purpose
depends on the type of crop grown and study required. Soil sampling should be done upto 0-15 ,
15-30 , 30-45, 45-60 and 60-90 cm depth.
SOIL SAMPLING FOR ORCHARDS/GARDENS
In case of fruit trees samples should be taken at the distance not less than three feet from the trunk
of plant or under the crown of tree. As root system is more extensive than crops sampling should
be done upto the depth of 150 cm to evaluate nutrient status and underlying properties and water
logging. Sampling should be done as follow 0-15,15-30, 30-45,45-60,60-90,90-120 and 120-150
cm depth.
Carefully note the concretions especially. If more that 20%, it will hinder nutrient availability and
free penetration of roots through the soil. In case of sandy soil it will not have positive effect on
fruit trees from nutrient supplying point of view.
PRECAUTIONS FOR SOIL SAMPLE COLLECTION
Samples should not be taken:
1. Along the water channel, roadside, pathway and boundaries

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2. Under the tree shade.

3. Close to the heaps (manure).
4. Areas where plant population is not uniform.
5. Areas where domestic refuse are thrown.
6. Places in the field where fertilizers are dumped.
7. Places where organic matter or plant residues have been accumulated by natural agencies like
wind or water , sampling should be avoided especially for fertility evaluation.
8. For salinity evaluation, if salt crust on the surface is present it should be removed before soil
sample collection or it should be sampled separately.
PRREPARATION OF COLLECTED SOIL SAMPLES
1. BAGGING. Samples are placed in polyethylene bags and then in cloth bags.
2. LABELLING. Labelling should be made with lead pencil or water proof ink.
One small label should be placed inside the bag and same number should be written on the bag.
3. DRYING. Soil samples after collection should be brought to the laboratory. Dry under shade
and where fumes are not present. Higher temperature should be avoided as reversible change may
take place.
4. SIEVING. Air dried soil should be ground and then pass through a sieve of 2mm mesh opening
for general purpose and 100 mesh (0.45mm) for trace elements and for other critical analysis.
5. STORAGE. Soil samples, after passing through 2mm sieve, should be transferred into wide
mouthed screw topped, numbered plastic bottles/jars.
6. Before analysis samples must be uniformly mixed.
REFERENCE / RELATED DOCUMENTS:
Soil and Plant Analysis Laboratory Manual ICARDA, Syria, 2001

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WATER SAMPLING
1. PURPOSE.
To assist the quality of irrigation
2. EQUIPMENTS/APPARATUS REQUIRED:
Plastic bottles
3. REAGENTS/MEDIAS REQUIRED:
4. METHOD:
The minimum quantity of water needed for the chemical analysis is about half liter. Obtain a
representative sample. Collect sample from pipe after the pump has been running for some time.
In general, shorter the elapsed time between collection and analysis of a sample of a sampler,
the more reliable will be the analytical data. Changers resulting from chemical and biological
activity may alter the composition of the sampler
5. CALCULATIONS REQUIRED:
6. CAUTIONS / SAFETY REQUIREMENTS:
Bottle should be clean, never wash bottle with soap. Give detail of tube-well and along with location and
depth.
7. REFERENCE / RELATED DOCUMENTS:
Diagnosis and improvement of saline and alkali soils. USDA Handbook 60. Washington.

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CHAPTER-2
SOIL ANALYSIS
DETERMINATION OF ELECTRICAL CONDUCTIVITY (ECE) OF SOIL
1. PURPOSE:
Determination of Electrical Conductivity (ECe) of Soil
Conductivity Meter, beaker, suction pump or filter press
0.01 N KCl: Dissolve 0.7456 g KCl in 1 litre of distilled water.
4. METHOD:
SATURATION EXTRACT:
Saturation extract from the soil paste can easily be obtained with the help of suction pump using
negative pressure (pressure is applied from below the soil paste) of 1 atmosphere. However, if the
soil is highly sodic and contains high amount of sodium and clay, saturation extract can not easily
be obtained by the negative suction. For such soils filter press apparatus (pressure from above the
paste) with positive pressure of any desirable magnitude can be used.
PROCEDURE:
Adjust moist filter paper in side the funnel, add paste into it, place bottle below the funnel, apply
vacuum to collect the extract.
In case of filter press, place a moist filter paper in stainless steel cup, add paste to it, closed and air
tight the cup, apply pressure from above the paste gradually till all the extract is collected in the
bottle placed under the cup.
DETERMINAION OF ELECTICAL CONDUCTIVITY OF SATURATION EXTRACT (ECe)
PROCEDURE:
Note and adjust the extract temperature on the conductivity meter with the help of knob provided.
Wash the conductance cell with distilled water and then with extract (if extract
is in reasonable amount). Dip the cell into the extract making sure that there is no air bubble in it.
Conductivity corrected at 25 0C will be displayed in mS cm-1 or dS m-1.
If the sample is very small either use the micro cell or dilute the sample. Sometime salt
concentration is too high to be measured. So make appropriate dilutions and multiply the final
reading with the dilution factor.
SOIL WATER RATIO:

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In case of saline sodic or sodic soils, to get a sufficient amount of extract is difficult. In such cases
soil: water ratio of 1:2, 1:5 or 1:10 should be used.
Vf (total volume of diluted solution)

Dilution Factor (d.f) = ------------------------------------------------
Vi (volume of aliquot taken for dilution
CONVERSION OF 1:10 TO ECe

Divide reading of 1:10 EC by 1.33 to convert into ECe
So EC1 (1:10) / 1.33 = EC2 i.e ECe

6.1 Standardise the conductivity meter before analysis
6.2 Calibrate the instrument with 0.01 N KCl solution. The EC of this standard solution
is 1.413 dS m-1 at 25 0C. The cell constant (K) can be calculated by the formula.
1.413 dS m-1
K = ---------------------------------
Observed reading in dS m-1
6.3 The cell constant is necessary when 0.01 N KCl solution gives an EC values
different from 1.413 dS m-1. In this case, samples readings are multiplied by the
cell constant.
United States Salinity Laboratory Staff. 1954. Diagnosis and improvement of saline and alkali
soils. USDA Handbook 60. Washington, D.C. pp. 89-91.

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DETERMINATION OF SOIL REACTION (pH)

1. PURPOSE:
Determination of soil reaction (pH)
Plastic beaker
Spatula
pH meter
Standard buffer solutions of pH 7.01 and 10.01
-Deionized water
4. CALIBRATION OF pH METER
i. Calibrate the pH meter using at least two buffer solutions of different pH values,
usually7.01 and 10.01. First, measure the temperature of the solution and adjust the
temperature knob, if not auto adjust.
ii. Dip the combined electrode in pH 7.01, buffer solution, check the actual pH at measured
temperature, and adjust with the buffer knob. Then dip the combined electrode in the pH
10.01 buffer solution and adjust with sensitivity knob. Repeat until pH meter gives correct
reading of both buffers.
PROCEDURE:
Give over night stay to the soil paste sample so that it may stabilized. Rejuvenate the paste next
morning if desired. Dip the electrode in the paste, note the reading when it is stabilized. Wash the
electrode with distilled water and dry with tissue paper before dipping in new soil paste sample.
5.1 After completion of work, wash and immerse the electrode in distilled water or in saturated
KCl solution.
Schofield, R. K. and A. W. Taylor. 1955. The measurement of soil pH. Soil Sci. Soc. Amer.
Proc. 19:164-167.

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DETERMINATION OF SOIL SATURATION PERCENTAGE

1. PURPOSE:
Determination of Soil Saturation Percentage
Balance
China Dish
Spatula
Plastic beaker
Oven
3. METHOD:
PREPARATON OF STAURATED SOIL PASTE
Take desirable amount of sieved soil in a plastic beaker (500 ml capacity), add distilled water
gradually while continuously stirring with spatula till the desirable paste is prepared. Note the
following points.
1. Soil paste should glisten and reflect light from the surface.
2. Soil paste should slide freely from the spatula.
3. Water should not stand on the surface when placed for some time.
4. When small hole is made on the surface with glass rod, water should not accumulate in it and
hole so made will be filled with paste under slow gravity movement.
5. Cover the beaker with lid for 30 minutes or one hour to reach equilibrium.
If the saturated soil paste fulfils the above points, it will be ready for the determination of different
parameters.
Weight of china dish =M g
Weight of china dish + paste =U g
Weight of paste =U-M = S g
Place the china dish in an oven at 105 0C for 24 hours. Remove and cool in a desiccator until
constant dry weight.
Weight of china dish + paste (oven dried) =T g
Weight of paste (oven dried) =T – M = A g
Loss in weight =S-A = F g
Saturation percentage =F/A x 100
or Loss in weight of soil
= ------------------------------x 100
Oven dry weight of soil
Soil paste and tarred china dish is placed in an oven at 105 0C for 24 hours, remove, cool and
record the weight. Same china dish with paste is again placed in an oven at 105 0C for some time,

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remove, cool and weight is recorded. If there is no difference in previous and new weight, then it
will be constant oven dry weight.
soils. USDA Handbook 60. Washington.

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DETERMINATION OF CARBONATES AND BICARBONATES IN SOIL
1. PURPOSE:
Determination of Carbonates and Bicarbonates in soil
Pipette, 50 ml
Conical flask, 100ml
Cylinder, 50 ml
Wash bottle
Burette, 50 ml
A. Phenolphthalein 1%: Dissolve 1.0 g phenolphthalein in 100 ml ethanol with constant stirring.
Filter if needed.
B. Methyl orange 0.1%: Dissolve 0.1 g methyl orange in 100 ml distilled water.
C. Sulphuric Acid 0.1 N (standardised).
4. METHOD:
Pipette out 50 ml aliquot in conical flask, add 1-3 drops of reagent A. If no colour appears,
carbonates are absent. If pink colour appears, carbonates are present. Titrate it against 0.1 N H2SO4
to a colourless end point. Take three readings. Reserve the flask along with its contents for
bicarbonates determination.
To the same conical flask (after colourless endpoint), add 1-2 drops of methyl orange, titrate
against 0.1N H2SO4 from golden yellow to a light pink or light orange colour endpoint. Take three
readings. Reserve the flask for chloride determination.
2R1 x Normality of H2SO4
-2 -1
CO3 (me L ) = ---------------------------------- ×1000
aliquot(ml)
or
Volume of aliquot taken = × ml (50 ml)
Volume of 0.1 N H2SO4 used = Final reading - blank reading
= R1
Actual volume of 0.1 N H2 SO4 used = 2× R1
= 2R1*
2R1 x 0.1 N H2SO4

-1
Carbonates (me L ) = ------------------------ x 1000 = 4 R1
50

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(R2-R1) x Normality of H2SO4

Bicarbonates (me L-1) = ------------------------------------ × 1000
aliquot (ml)
or
Volume of aliquot taken = 50 ml
Volume of 0.1 N H2SO4 used = Final reading -Initial reading
** = R2
Actual volume of 0.1 N H2SO4 used = R2 - R1
(R2-R1) × 0.1 N H2SO4

Bicarbonates (me L-1) = ------------------------------- × 1000
50
= 2 (R2-R1)
* This reaction is completed in two steps as shown by the chemical reaction
Na2CO3 + H2SO4--------------------2 NaHCO3 + Na2 SO4-------i

2 NaHCO3 + H2SO4 ----------------Na2SO4 + 2 H2 O+ 2 CO2--------ii
R1 is the amount of acid used to convert the carbonates to bicarbonates (equation i,
phenolphthalein part of reaction, while for the completion of the reaction, same amount of acid
will be still needed to further convert bicarbonates so produced during step i to form CO2 and H2O
as shown in equation ii. Thus R1 is the amount of acid for half reaction and 2R1 will represent the
amount of complete reaction. Hence R1 is multiplied by a factor of 2.
** R2 is the total amount of acid used to neutralise the bicarbonates present in the sample after
titration. Which means that sample contains bicarbonates coming form conversion of CO3 as well
as originally present in the sample. Therefore the actual amount of acid used for neutralising the
originally present HCO3 would be R2-R1.
Always run blank for accuracy.
soils. USDA. Handbook 60. Washington, D.C. pp. 89-91.

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DETERMINATION OF CALCIUM AND MAGNESIUM
PURPOSE:
Determination of Calcium and Magnesium
China dish
Pipette, 10 ml
Cylinder, 50 ml
Glass rod
Wash bottle
A. NH4Cl -NH4 OH buffer solution
Dissolve 67.5 g NH4Cl in 570 ml concentrated NH4OH, make the volume upto l litre..
B Sodium hydroxide (NaOH), 4 N
Dissolve 160 g NaOH in distilled water, make the volume of the solution to 1 litre .
C. Standard calcium chloride solution (CaCl2) , 0.01 N
Dissolve 0.5 g CaCl2 pure (calcite crystals ) in 10 ml of approx. 3 N (1+3) HCl and dilute to a
volume of exactly 1 litre.
D. Eriochrome black-T indicator (EBT)
Dissolve 0.4 g of EBT and 4.5 g hydroxyl amine hydrochloride (NH2O.H. HCl, H3NO.HCl, m. wt.
69.49) in 100 ml of 95 % ethanol.
E. Ammonium purporate indicator (C8H4N5O6. NH4)
Thoroughly mix 0.5 g ammonium purporate with 100 g of powdered potassium sulphate (K2SO4)
F. EDTA (Versenate ) solution, 0.01 N
Dissolve 2.0 g of disodium salt and 0.5 g magnesium chloride hexahydrate ( MgCl2. 6H2 O ) in
distilled water and dilute to a volume of 1 litre . Standardised the solution against reagent C using
given titration procedure.
4. METHOD:
Pre-treatment of soil extract .
Ammonium acetate and dispersed organic matter present in appreciable amount must be removed
from soil extracts prior to titration wit versenate. For this purpose soil extract is dried by
evaporation after treating with aqua regia (3 part conc. HCl + 1 part conc. HNO3) Second dryness
is considered sufficient for the removal of ammonium acetate and organic matter. (Soil extract
with dark colours require additional treatment with aqua regia).
CALCIUM:
Pipette out 10 ml of pre-treated aliquot in a conical flask. Add 5 drops of reagent B and add 50 mg
of E. Titrate against F from orange red to lavender/purple and point. When closed to the endpoint,

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reagent F should be added drop wise (each drop after 5-10 second ) as the colour change is not
instantaneous.
CALCIUM PLUS MAGNESIUM:
Pipette out 10 ml of aliquot in a conical flask. Add 10 drops of reagent A, 3-4 drops of reagent D.
Titrate against reagent F to a change in colour from wine red to bluish green.
ml of ETDA sol. for sample -ml of EDTA for blank
x N x 1000
++ ++ ++ -1
Ca / Ca + Mg (me L )=-------------------------------------------------------------------
aliquot in ml
R1-R2 x 0.01 x 1000

= -----------------------
10
= (R1-R2) = R me L-1
Mg++ (me L-1) = Ca++ + Mg++ –Ca++ (All expressed as meL-1)
soils. USDA. Handbook 60. Washington, D.C.

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DETERMINATION OF CHLORIDE IN SOIL
1. PURPOSE:
Determination of soil chloride
Pipette, 50 ml
Cylinder, 50 ml
Wash bottle
Burette, 50 ml
A. Potassium Chromate (K2CrO4), 5 % solution
Dissolve 5.0 g of potassium chromate in 50 ml distilled water and add l N (saturated solution)
AgNO3 drop wise until red precipitate is produced. The solution is filtered and filtrate is diluted
to 100 ml.
B. Silver Nitrate (AgNO3), 0.05 N (F. wt. 169.888)
Dissolve 8.494 g silver nitrate in distilled water and dilute to 1 litre. Keep in a brown bottle away
from light to avoid photolysis.
4. METHOD
To the same conical flask after light orange yellow end point, add 3-4 drops of reagents A. While
stirring, titrate under bright light with reagent B., to a brick red precipitate./permanent reddish
brown colour..
NaCl + AgNO3-----------NaNO3 +AgCl
As soon as the amount of NaCl is used up, AgNO3 reacts with potassium chromate.
K2CrO4 + 2 AgNO3--------------2 KNO3 + Ag2CrO4 (ppt.)
(ml of AgNO3 for sample -ml of AgNO3 for blank) x N
-1
Cl (me L ) = --------------------------------------------------------------------x 1000
aliquot (ml)
or
Volume of 0.05 N AgNO3 used = Final reading - initial reading = R3
Cl (me L-1) = R3 x 0.05 N AgNO3 x 1000/50
6. CAUTIONS / SAFETY REQUIREMENTS.
Always run a blank with actual titration.
soils. USDA. Handbook 60. Washington, D.C.

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DETERMINATION OF ORGANIC MATTER

1. PURPOSE:
Organic matter determination in soil
A. 1 N Potassium dichromate (K2Cr2O7, f. wt. 294. 18): Dissolve oven dried 49.04 g potassium
dichromate in distilled water, mix well and dilute to 1litre.
B. 1.0 N ferrous sulphate standardised: Dissolve 278.02 g ferrous sulphate (FeSO4.7H2O), in
distilled water, add 15 ml concentrated sulphuric acid and dilute to one litre.
C. Sulphuric Acid (96 %, specific gravity 1.84)
D. Phosphoric acid (H3PO4) 85 % or sodium fluoride (NaF)
E. Barium diphenylamine sulphonate, 0.16 %: Dissolve 0.16 g barium diphenylamine sulphonate
indicator in 100 ml conc. H2SO4 of 4:1 ratio.
500 ml conical flask
Pipette, 10 ml
Burette, 50 ml
Beaker, 500 ml
Cylinder, 50 ml
Wash bottle
Weighing balance
4. METHOD:
Weigh 1.0 g air dried, ground soil sample into 500 ml conical flask, add 5 ml K 2Cr2O7 and mix
well. Add 10 ml sulphuric acid and mix. Allow the flask to stand for 30 minutes to cool. Then add
100-150 ml distilled water. Add 3 ml phosphoric acid or 0.5 g sodium fluoride, 5-10 drops of
indicator and finally titrate against standardised ferrous sulphate to sharp green end point through
blue colour. Run a blank and subtract sample reading from blank to get the actual volume of ferrous
sulphate used to reduce potassium dichromate.
ml for blank - ml for sample
%OM = -------------------------------------x 0.698*
weight of sample (g)
me of K2 Cr2O7 reduced
% OM= ----------------------------------- x 0.698
weight of sample ( g)
me of K2Cr2O7 reduced = ( me of K2Cr2O7 added - me of FeSO4 used)

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me of K2Cr2O7 added = (ml of K2Cr2O7 added x N)

me of FeSO4 used = (ml of FeSO4 used x N )
ml for blank - ml for sample
% O C = ---------------------------------------x N FeSO4 x 0.337
weight of sample (g)
% O C = % organic matter / 1.724
100 100
*0.698 = 0.003 x ---------- x ---------- x 100
74 58
How = 0.003
1 me of C of OM in soil = 1 x Eq. wt. of C / 1000
m. wt. 12 3
Eq. Wt. of C = ------------ x --------- = ------ = 0.003 g of C of OM in soil
valency 4 1000
So
1 ml of 1 N K2Cr2O7 when reduced = 0.003 g of C of OM in soil
100 / 74= 1.3514, efficiency factor for determining O. C. of soil
100 / 58 = 1.724, for conversion of % OM of soil to % O.C. (If divided).
100 = for converting O.M. in percentage
**0.337
Walkley, s rapid method (1935, 1947) for the determination of organic carbon in soils has been
found to give app. 89 % recovery of carbon as compared to dry combustion method. The
conversion factor, 0.337 was obtained by dividing 0.003, the milliequivallent weight of carbon by
89 and multiplying by 100 to convert to percent.
Always run blank along with samples.
Walkley, A. 1947. A critical examination of a rapid method for determining organic carbon in
soils – effect of variations in digestion conditions and of inorganic soil constituents. Soil Sci.
63:251-264.

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DETERMINATION OF SOIL TEXTURAL CLASS
1. PURPOSE:
Soil Textural Class Determination
Hydrometer
Graduated cylinder 1000 ml
Thermometer
Stop watch
Stirrer with cup
Beaker 500 ml
Perforated brass plunger
Wash bottle
i. Sodium haxametaphosphate (4%), dispersing reagent (NaPO3)6: Dissolve 40 g of sodium
hexametaphosphate and 10 g of sodium carbonate in distilled water, mix well and make
the volume one litre (new solutions should be prepared after 1 – 2 weeks).
ii. Amyl Alkohol
4. METHOD:
1. Weight 40g air-dry soil (2-mm) into a 600mL beaker.
2. Add 60-mL dispersing solution
3. Cover the beaker with a watch-glass, and leave overnight
4. Quantitatively transfer contents of the beaker to a soil-stirring cup, and fill the cup to about
three-quarters with water.
5. Stir suspension at high speed for 3 minutes using the special stirrer. Shake the suspension
overnight if no stirrer is available.
6. Rinse stirring paddle into a cup, and allow to stand for 1 minute.
7. Transfer suspension quantitatively into a 1-L calibrated cylinder (hydrometer jar), and
bring to volume with water.
A. Determination of Blank
 Dilute 60 mL dispersing solution to 1-L hydrometer jar with water
 Mix well, and insert hydrometer, and take hydrometer reading Rb.
 The blank reading must be re-determined for temperature changes of more than 2oC from
20oC
B. Determination of Silt plus Clay.
 Mix suspension in the hydrometer jar, using a special paddle carefully, withdraw the paddle,
and immediately insert the hydrometer.
 Disperse any froth, if needed, with one drop of amyl alcohol, and take hydrometer reading 40
seconds after withdrawing the paddle. This gives reading Rsc.

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CALCULATIONS
Percentage Silt plus Clay in soil
% [Silt +Clay] (w/w) = (Rsc-Rb) × 100
Oven –dry soil (g)
C. Determination of Clay
 Mix suspension in the hydrometer jar with paddle, withdraw the paddle, with great care,
leaving suspension undisturbed
 After 4 hours, insert the hydrometer, and take hydrometer reading Rc.
Percentage Clay in soil:
% Clay (w/w)= (Rc-Rb) × 100
Percentage Silt in soil:
% Silt (w/w) = % [Silt +Clay (w/w)] – [% Clay (w/w)]
D. Determination of Sand
 After taking readings required for clay and silt, poor suspension quantitatively through a 50um
sieve.
 Wash sieve until water passing the sieve is clear.
 Transfer the sand quantitatively from sieve a 50 mL beaker of known weight.
 Allow the sand in the beaker to settle, and decant excess water.
 Dry beaker with sand overnight at 105oC
 Cool in a desiccator, and re-weigh beaker with sand.
Percentage Sand in soil:
% Sand (w/w) = Sand weight × 100
Where: Weight of sand follows from
Sand weight (g) = [Beaker + Sand (g)] – [Beaker (g)]
Note:
1. If possible, all hydrometer jars should be placed in a water bath at constant temperature (20oC);
in that case, temperature corrections are not needed.
2. For temperature correction, use a value of 0.4 for each degree temperature difference from
20oC. Add or subtract this factor if the temperature is more or less than 20oC, respectively.
3. All results of mechanical analysis should be expressed on the basis of oven-dry soil (24 hours
drying at 105oC).
4. In the above procedure, carbonates and organic matter are not removed from the soil.
5. The Hydrometer method, as described in this section, cannot be applied to soils that contain
free gypsum (gypsiferous soils). For gypsiferous soils, see Hesse (1971).
6. Sum of % silt and clay + % sand should be 100%. The magnitude of deviation from 100 is an
indication for the degree in accuracy.

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Soil Texture
Once the percentage of sand, silt, and clay is measured, the soil may be assigned a textural class
using the USDA textural triangle (Fig.4). Within the textural triangle are various soil textures
which depend on the relative proportions of the soil fractions.
Bouyouces, G. J. 1962. Hydrometer method improved for making particle size analysis of soils.
Agron. J., 53:464-465.

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DETERMINATION OF EXTRACTABLE POTASSIUM IN SOIL
1. PURPOSE:
Extractable potassium determination in soil
Mechanical Shaker, reciprocating
Flamephotometer
Beaker, 50 ml
Pipette, 10 ml
Wash bottle
Volumetric flasks
A.1 N NH4OAC: Dissolve 77.1 g ammonium acetate (F.W. 77.1, CH3COONH4) in 800 ml distilled
water and make the volume to 1 litre. Adjust pH 7.0 using either NH4OH or HCl.
B. Stock solution : Dissolve 1.907 g oven dried KCl in distilled water and make volume 1-2. This
solution contains 1000ppm K.
ii. Prepare standard solutions from stock solution in 100ml volumetric flask.
4. METHOD: Wight 2.5 g air dried, ground, passed through 2 mm sieve soil sample into a 250ml
conical flask, add 50 ml extracting reagent, shake on a flat bed recipro shaker for 30 minutes and
filter the extract. Determine K by flame photometer in ppm using graph readings.
Extractable K (ppm) = reading (ppm) × 20

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DETERMINATION OF EXTRACTABLE SOIL PHOSPHORUS (OLSEN’S METHOD)
1. PURPOSE:
Soil Extractable Phosphorus Determination (The Olsen Method)
Spectrophotometer
Standard laboratory glassware, Beaker, Volumetric flasks pipettes funnels
Extraction bottles
A. Sodium bicarbonate solution, 0.5 M NaHCO3: Dissolve 42.0 g NaHCO3 in app. 700 ml distilled
water, shake well and make the volume 1000 ml . Adjust pH 8.5 using 5 N NaOH.
5 N NaOH = Dissolve 200g NaOH in distilled water and let it cool and make volume 1 L.
B. Mixed reagent:
(a) Ammonium hepta molybdate 4.8 % (NH4)6MO7O24 4HO2 (f. wt. 1235.9)
Dissolve 12.0 g in distilled water and make volume 250 ml
(b) Potassium antimony tartrate (KsbO. C4 H2O6)
Dissolve 0.291 g make volume to 100 ml with distilled water
(c) 5N H2SO4. Dilute 148 ml concentrated sulfuric acid (in fume hood) in distilled water, let it cool
and make volume 1 L.
(d) Add both the dissolved reagents (a + b) in 1000 ml 5 N H2SO4 and make volume 2000 ml with
distilled water. Store in a Pyrex bottle in a dark, cool place
C. Colour developing reagent: Weigh 0.528g ascorbic acid to 100 ml of mixed reagent. This
reagent should be prepared freshly as required because it does not give accurate results after 24
hours.
D. Stock solution (1000 ppm): Dissolve 4.3937 g potassium dihydrogen phosphate (KH2PO4) in
distilled water and make volume to 1 liter.
STANDARDS (0.05-1.5ppm):
Making 5 ppm sub-stock solution
4. METHOD:
Weigh 2.5 g air dried and ground soil, add 50 ml extracting solution. Shake for 30 minutes and
filter with Whatman No. 42. Pipette out 5 ml aliquot. Add 5 ml of colour developing reagent, in
25 ml volumetric flask. Shake to remove gas bubbles. Let stand for 15 minutes. Make volume up
to mark. Bluish colour will develop. Concentration of phosphorus in soil is directly proportional
to the intensity of blue color developed. Take reading on concentration mode at 880 nm wavelength
on Spectrophotometer.

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5. CALCULATIONS:- Extractable phosphorous in soil (ppm)=ppm p*x A x 50

wt v
A= Total volume of Extractant (ml)

Wt= Wight of air-dry soils (g)
V= Volume of extract used (ml)

Olsen, S. R., C. V. Cole, F. S. Watanabe and L. A. Dean. 1954. Estimation of available
phosphorus in soils by extraction with sodium bicarbonate. USDA Circ. 939. pp. 19.

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DETERMINATION OF SODIUM IN SOIL
1. PURPOSE:
Sodium Determination of Soil
Flame Photometer
Volumetric flask
Conical flask
Preparation of stock solutions
Stock solution of sodium (1000 ppm) can be prepared by dissolving oven dried NaCl (2.5435 g)
in distilled water and making the volume to exactly one litre. Store in a cool and dry place.
Preparation of working standards:
Stock solution so prepared will be used for the preparation of working standards by using the
formula:
C1V1 =C2V2
Where
C1 = Concentration of stock solution in ppm
V1 = Volume to be taken of stock solution in ml
C2 = Concentration of Na to be required in ppm
V2 = Total volume to be required in ml
V1(ml of known solution) x C1 (ppm of known solution)

C2 (ppm required) = -------------------------------------------------------------------
V2 (Total volume to be made)
Working standard solution can be prepared of 10,20,30,------100 ppm concentration and for plant
0-10 ppm concentration or as desired.
4. METHOD:
All Flamephotometers have approximately the same procedure but this procedure is mainly based
on PFP 7 Flamephotometer.
Steps are as follow
1. After ignition of flame photometer wait for 5 – 10 minutes to stabilize the instrument.
2. Adjust zero with extractant.
3. Run desired standards and draw calibration curve.
4. If the sample to be analysed have higher concentration (ppm)than the highest working
standard solution concentration, dilute the sample solution and multiply the reading with dilution
factor.

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5. After completion of analysis aspirate the distilled water for at least 15 minutes to remove all the
elemental particles and to avoid the chance of chocking.
6. In case of chocking the instrument, aspirate semi hot distilled water or very dilute HCl in semi
hot distilled water. However in case of still chocking very dilute HCl in semi hot distilled water
should be used for aspirating.
7. Clean the table, wash all the apparatus and place at proper place before leaving the laboratory.
Na (ppm) = R × Dilution factor
Where
R = Flame photometer reading in concentration made
soils. USDA Handbook 60. Washington.

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DETERMINATION OF SULPHATE IN SOIL
1. PURPOSE:
Soil Sulphate Determination
Spectrophotometer
Electronic balance
Pipette
A. 0.001 M CaCl2: 0.147 g CaCl2 L-1
B. Acid Mixture: 125 ml HNO3 + 250 ml Acetic Acid + 100 ml H3PO4 (85 %) Dilute to one litre
with deionized water.
C. Acid Sulphate solution (20ppm S): 86ml conc. HCl+100ml S solution (100ppm). Make volume
upto 500 ml with Deionized water.
D. BaCl2.2H2O Crystal: 20-60 mesh crystal
E. Gum Acacia Solution: Dissolve 0.5 g gum acacia in 50 ml Deionized water. Mix and filter. Add
50 ml acetic acid. Filter if necessary.
F. Dissolve 0.5434 g potassium Sulphate in distilled water and bring to 1-L volume. This solution
contains 100ppm SO4-S (stock solution).
G. SO4 – Standards from 100 ppm standard: 0, 5, 10, 15 and 20 ppm solutions
4. METHOD:
Weigh 25 g soil and add 50 ml CaCl2 extracting solution. Shake for 30 minutes and filter through
Whatman No. 42 filter paper. Take 5 ml sample in a 50 ml volumetric flask. Add 5 ml mixed
acid reagent and 1 ml acid Sulphate solution and mix. Add 0.5 g BaCl2.2H2O crystals. Let stand
undisturbed for 3 minutes and then mix.
Add 1 ml gum acacia reagent and mix. Make 50 ml volume with distilled water. Take readings
of samples and standards at 420-450 nm between 3 to 8 minutes after final shaking. Run reagent
blank.
Sulphate concentration (ppm) = Sulphate conc. (ppm) × Dilution factor
Bardsley, C. E. and J. D. Lancaster. 1965. Chapter 79. C. A. Black. Ed. Methods of soil analysis.

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DETERMINATION OF CALCIUM CARBONATE IN SOIL
1. PURPOSE:
Soil Calcium Carbonate Assessment
Pippete, 10 ml
Flask
Balance
Hydrochloric Acid (1 + 3, Acid + Water)
4. METHOD:
Weigh the flask. Add 10 ml HCl 3 N (1:3 acid, water) and weigh it. Add 10 g soil and weigh again.
Shake gently and stay for two hours. Note the final weight of flask after 2 hours.
Wt. of flask = A
Wt. of flask + acid = B
Wt. of flask + acid + soil = C
Wt. of flask + acid + soil after 2 hours = D
Wt. of CO2 lost = Initial Wt. (C) – Final Wt. (D) = E
E × 227.4
% CaCO3 = ----------------------------------
Wt. of soil taken
soils. USDA Handbook 60. Washington, D.C.

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GYPSUM REQUIREMENT OF SALINE SODIC AND SODIC SOIL

1. PURPOSE:
Assessment of Gypsum Requirement for Saline Sodic and Sodic Soil
Weighing balance
Volumetric flask, 1000 ml
Mechanical shaker
Conical flask, 250 ml
Plastic bottle, 250 ml
Funnel with stand
Pipette, 10 ml
Burette, 50 ml
A. Saturated gypsum solution: Dissolve 5.0 g CaSO42H2O in 1 litre distilled water. Stopper the
volumetric flask and shake by hand for one hour or for 10 minutes on reciprocating shaker. Filter
and determine the calcium concentration of solution by versenate method. The calcium
concentration should be at least 28 me L-1.
B. EDTA 0.01 N. Dissolve 2.0g of EDTA and 0.05g MgCl2-6H2O in water and dilute to volume
of 1-L.
C. Buffer solution: Ammonium chloride – ammonium hydroxide solution. Dissolve 67.5g
of ammonium chloride in 570ml of concentration ammonium hydroxide and make volume to
1-L.
D. EBT indicator. Dissolve 0.5g of EBT and 4.5g of hydroxylamine hydrochloride in 100ml of
95% ethanol.
4. METHOD:
Weigh 5.0 g air dried soil in a 250 ml capacity plastic bottle, add 100 ml saturated gypsum solution,
stopper the bottle, shake by hand several times for half an hour or for 5 minutes in a mechanical
shaker. Filter the suspension and. Take 5 ml of aliquot, add 7 – 10 drops of C and D each. Titrate
against B from wine red to bluish end point.
5. CALCULATIONS :
Blank Reading – Sample Reading x 0.01 x 1000 x 2
-1
Gypsum Req. (me100 g )= --------------------------------------------------------------
5.0
5 g soil was added in 100 ml of gypsum saturated solution.

So, 1000 ml soil filtrate will correspond to 50 g air dry soil.

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Therefore, in 50 g soil, Ca conc. = Ca conc. (me L-1) of gyp. sol. - Ca+Mg conc. (me L-1) of
filtrate.
Ca conc. in 100 g soil = 100/50 = 2
Conversions:
Say
100 g soil has gypsum requirement = M me
Then gyp. req. for
Tonnes per acre 15 cm of soil = M x 0.86
Tonnes per ha 15 cm of soil = M x 2.12
Tonnes per acre 30 cm of soil = M x 1.72
Tonnes per ha 30 cm of soil = M x 4.25
6.1 Never use oven dry soil sample as heating promotes the conversion of CaSO 4 2HO2 to
CaSO4.1/2 H2O (plaster of Paris) which is more soluble than that of CaSO4. 2H2. Hence the
gypsum requirement will be more than the actual.
Schoonover, W. R. 1952. Examination of soil for alkali. Univ. of Calif. Ext. Service Berkely
California. (Mimeographed).

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DETERMINATION OF TOTAL NITROGEN IN SOIL
1. PURPOSE:
Total Nitrogen Evaluation in Soil
Kjeldhal distillation unit
Balance
Volumetric flasks, 100, 1000 & 2000ml
Pipette, 10 ml
Conical flask, 250 ml
Burette, 50 ml
Beaker, 50 & 1000 ml
Wash bottle
Digestion Block
A. Sulphuric acid Conc. (reagent grade N free).
B. Digestion mixture: K2SO4+CuSO4 in 9:1
C. Sodium hydroxide solution (40%): Dissolve 400g sodium hydroxide in one litre distilled water.
D. Bromocresol green and Methyl red indicator : Dissolve 0.5 g BCG and 0.1 g methyl red in 100
ml of 95 % ethanol
E. Boric acid solution (4%): Dissolve 40 g of boric acid in 1.0 litres of CO2 free distilled water.
F. 0.1 N H2SO4 solution
G. Phenolphthalein indicator
STANDARDISATION OF NaOH 0.1 N:

REAGENTS:
A Potassium acid phthalate 0.1 N: Weigh 20.423 g of oven dried potassium acid phthalate, dissolve
in distilled water and make the volume 1.0 litre.
B. Phenolphthalein indicator. Dissolve 1 g of phenolphthalein in 100 ml 50% ethanol (50 ml of
ethanol and 50 ml distilled water) with constant stirring. Filter if precipitates are formed.
C. Sodium hydroxide 0.1 N: 4.0 g of sodium hydroxide is dissolved in distilled water and make
volume one litre.
Pipette 10 ml of 0.1 N potassium acid phthalate into a titration flask and add 1-2 drops of
phenolphthalein, titrate against solution of sodium hydroxide to light pink colour end point. Note
the reading and adjust the normality of the base by
Na x Va = Nb x Vb
Standardisation of H2SO4 0.1 N:

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Pipette out 10 ml of 0.1 N standardised base in a titration flask, add 1-2 drops of phenolphthalein
indicator titrate against the acid to be standardised, to colourless endpoint. Note the volume of acid
used. By suing the above formula adjust the normality i.e. 0.1N. If less volume of acid to be
standardised is used for 10 ml of standardised base then dilute the acid or vice versa.
4. METHOD:
Weigh 5 g air dried, passed through 2.0 mm sieve soil sample and 1.0 g digestion mixture into
clean and dry digestion tube. Add 10-15 ml concentrated commercial sulphuric acid and heat at
4200C. Continue to heat until the colour of the material changes from black to white/greenish
white. Solidification should be avoided.
Distille digested material in same flask on the distillation unit. Collect distillate in 20-25 ml 4%
boric acid in the receiver. Add few drops of indicator. Purple color will form and will be changed
to golden yellow on distillation. Which is then titrated against 0.1 N H2SO4 for soil from golden
yellow to a purple end point.
14.1 × ml of titrant for sample - ml of titrant for blank × N of acid
%N= ------------------------------------------------------------------------------------
weight of sample (g) ×10
0.00141 × R ×100
= ----------------------------
5
Factor for soil if weight of soil is 5.0 g
% N = R - blank ×0.0282

6.1 Always run blank along with samples.
Bremner, M. 1960. Kjeldhal Method. Agronomy – 9, 2nd Ed.

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DETERMINATION OF CATION EXCHANGE CAPACITY OF SOIL

1. PURPOSE:
Determination of the Capacity of the Cation Exchange of Soil
Flame photometer
Centrifuge machine
Volumetric flask, 100 ml
Cylinder, 50 ml
Weighing balance
Funnel with stand
Burette, 50 ml
A. Sodium acetate solution (saturating solution), 1.0 N: Dissolve 136 g sodium acetatetrihydrate
in distilled water and make volume upto 1 litre. Adjust pH approximately 8.2 using NaOH or
CH3COOH.
B. Ethanol 95%
C. Ammonium acetate solution (replacing solution) 1.0 N: Dissolve 77.08g in distilled water and
make volume up to 1L and adjust pH at 7.0 with Ammonium Sulphate.
D. Sodium Stock Solution (1000 ppm) Dissolve dried 2.5418 g of NaCl in 1 L deionized water
(Desired working standards be prepared from it).
4. METHOD:
Weigh 5.0 g soil sample in a centrifuge tube. Add 33 ml of reagent A, stopper the tube, shake for
5-7 minutes, centrifuge for 5 minutes or till the clear supernatant solution in centrifuge at 1200-
2000 rpm. Decant and discard. Repeat same process further two times with 33 ml of reagent A.
Centrifuge, decant and discard the supernatant solution. Now add 33ml of B regent to the tube,
stopper, shake for 5-7 minutes. Decant and discard supernatant solution. Repeat the same
procedure further two times with 33 ml of reagent B. Now add 33 ml of reagent C to the same
tube, stopper, shake and centrifuge at 2000 rpm for 5-7 minutes. Decant the supernatant solution
in the 100 ml volumetric flask. Repeat the same procedure for further two times with 33 ml of
reagent C. Make the volume 100 ml with distilled water. This solution is ready for the
determination of replaced Na by flame photometer.
5. CALCULATIONS:
Na conc. of ext. (me L-1)
Cation exchange capacity (CEC) C mol (+) Kg-1 = ------------------------------ × 10
wt. of sample (g)

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soils. USDA Handbook 60. Washington, D.C. pp. 101.

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DETERMINATION OF EXTRACTABLE MICRONUTRIENTS IN SOIL
1. PURPOSE:
Determination of Plant Available Micronutrients in Soil
Atomic Absorption Spectrophotometer
Plastic beaker
Mechanical Shaker
Filter paper
Funnel
Test tubes
0.005 M DTPA, 0.01 M CaCl2, and 0.1 M TEA (tri-ethanol amine, adjusted to pH 7.3 with dilute
HCl. Dissolve 3.934 g of DTPA and 2.94 g of CaCl2 and 25.3 ml of TEA in approximately 200
ml of distilled water. After sufficient time for DTPA to dissolve, make the volume 2 litre. Adjust
the pH 7.3 with 1:1 HCl while stirring.
4. METHOD:
Weigh 20 g of soil and add 40 ml of DTPA solution. Shake continuously for 2 hours on horizontal
shaker and filter. A blank solution (0 ppm) containing all reagents except soil should be run with
samples as blank. Read on concentration mode by atomic absorption spectrophotometer Prepare
at least 4 standard using DTPA as matrix for each element with a range as following
For Zn and Cu 0.05.1.0,1.5,2.0 ppm
For Fe and Mn 0,5,10,20, 30, ppm
5. CALCULATIONS:
Micronutrients (ppm) = reading × 2
Always run blank along with samples.
Lindsay and Norvell. 1978.

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DETERMINATION OF BORON IN SOIL

1. PURPOSE:
Boron Assessment in Soil
Spectrophotometer.
Weighing balance
Poly propylene volumetric flask
Pipette
Funnel with stand
Wash bottle
Water bath
Burner
Beaker, 50 ml
A. Buffer solution: Dissolve 250 g ammonium acetate and 15 g of ethylenediamine tetra acetic
acid (EDTA) in 400 ml of distilled water. Slowly add 125 ml glacial acetic acid and mix.
B. Azomethine – H reagent: Dissolve 0.45 g of reagent in 100 ml of 1 % L-ascorbic acid solution.
Fresh reagent should be prepared and store in a refrigerator.
C. Boron standard solution: Dissolve 5.709 g of boric acid (H3BO3) in distilled water (for hot
water extraction) or in 0.05 M HCl for HCl extraction and adjust the volume 1000 ml . This will
be of 1000 ppm of boron solution. Make sub-stock solution to 100 ml of 100 ppm B. Then make
working standard as desired.
C1V1 = C2V2
100 x V1 = 0.5 x 100
5 x 100
V1 = ---------- = 0.5 ml of sub-stock solution to make 0.5 ppm B working standard.
1000
D. 0.05 M HCl
4. METHOD:
HOT WATER EXTRACTION
Boil 10g soil in 20ml distilled water for 5 minutes in boron free apparatus (Polypropylene) and
then filter. If boron free apparatus is not available then pyrex glass apparatus should be dipped in
concentrated HCl for a week and then used.
HCl EXTRACTION
Ten grams soil was shaken with 20 ml of 0.05 M HCl for 5 minutes and then filter. Transfer 1 ml
aliquot in 50 ml polypropylene volumetric flask, add 2 ml buffer solution, add 2 ml azomethine-
H reagent and mix. After 30 minutes read absorbance at 430 nm on spectrophotometer at
concentration mode or by graph using standard curve prepared Boron standards are prepared in
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0.05 M HCl for HCl extraction and in distilled water for hot water extraction. Using 420 nm
wavelength determine boron (ppm) by spectrophotometer using color developing method.
5. CALCULATIONS:
B (ppm) = R x 100*
Where
R = spectrophotometer reading
100* = total dilution factor.

6.1 Always run blank for accuracy.
Bingham. 1982. Methods of soil analysis. Part II. Amer. Soc. Agron. USA.

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CHAPTER-3
WATER ANALYSIS
ELECTRICAL CONDUCTIVITY (EC) OF WATER
PURPOSE:
Determination of Electrical Conductivity (EC)
Conductivity Meter
0.01 N KCl: Dissolve 0.7456 g KCl in 1 litre of distilled water.
4. METHOD:
The instrument must be standardised with 0.01 N KCl solution. The EC of this standard solution
is 1.413 dS m-1 at 25 0C. The cell constant (K) can be calculated by the formula.
1.413 dS m-1
K = ---------------------------------
Observed reading in dS m-1
The cell constant is necessary when 0.01 N KCl solution gives an EC values different from 1.413
dS m-1. In this case, samples readings are multiplied by the cell constant.
EC of water = Observed EC × K
The conductivity meter should be standardised daily or as desired depending upon the number of
samples being tested.

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DETERMINATION OF CARBONATES AND BICARBONATES IN WATER

PURPOSE:
Determination of the concentration of carbonates and bicarbonates in water
Pipette, 50ml
Cylinder, 50ml
Wash bottle
Burette, 50ml
A. Phenolphthalein 1%: Dissolve 1.0 g phenolphthalein in 100 ml ethanol with constant stirring,
Filter if needed.
B. Mehtyl Orange 0.1%: Dissolve 0.1g methyl orange in 100ml distilled water.
C. Sulphuric Acid 0.1 N (standardized)
4. METHOD:
Pipette 50ml aliquot in conical flask, add 1-3 drops of reagent A. If no colour appears,
carbonates are absent. If pink colour appears, carbonates are present. Titrate it against 0.1 N
H2SO4 to colorless end point. Take three readings. Reserve the flask along with its contents for
bicarbonates determination.
To the same conical flask (after colorless end point), add 1-2 drops of methyl orange, titrate
against 0.1 N H2SO4 from golden yellow to a light pink or light orange colour end point. Take
three readings. Reserve the flask for chloride determination.
2R1 ×Normality of H2SO4
-2 -1
CO3 (me L ) = ---------------------------------- ×1000
Aliquot (ml)
Or
Volume of 0.1 N H2SO4 used = Final Reading - Blank Reading
= R1
Actual Volume of 0.1 N H2 SO4 used = 2 x R1= 2R1
* 2R1 x 0.1 N H2SO4
Carbonates (me L-1) = ---------------------------- x 1000 = 4 R1
50
(R2-R1) x Normality of H2SO4
-1
Bicarbonates (me L ) = -------------------------------------- x 1000
Aliquot (ml)
Or

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Volume of 0.1 N H2SO4 used = Final reading -Initial reading
= R2
Actual volume of 0.1 N H2SO4 used = R2 - R1
(R2-R1) x 0.1 N H2SO4
-1
Bicarbonates (me L ) = ------------------------------- x 1000
50
= 2 (R2-R1)
* This reaction is completed in two steps:
R1 is the amount of acid used to convert the carbonates to bicarbonates.
R2 is the total amount of acid used to neutralise the bicarbonates present in the sample after
titration. Therefore the actual amount of acid used for neutralising the originally present HCO3
would be R2-R1.

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DETERMINATION OF CHLORIDE IN WATER

1. PURPOSE:
Determination of Chloride in Water
Pipette, 50ml
Cylinder, 50ml
Wash bottle
Burette, 50ml
A. Potassium Chromate (K2CrO4), 5 % solution: Dissolve 5.0 g of potassium chromate in 50 ml
distilled water and add l N (saturated solution) AgNO3 drop wise until red precipitate is produced.
The solution is filtered and filtrate is diluted to 100 ml.
B. Silver Nitrate (AgNO3), 0.05 N. Dissolve 8.494 g silver nitrate in distilled water and dilute to 1
litre. Keep in a brown bottle to avoid photolysis.
4. METHOD:
To the same conical flask after light orange yellow end point, add 3-4 drops of reagents A. While
stirring, titrate under bright light with reagent B., to a brick red precipitate./permanent reddish
brown color.
(ml of AgNO3 for sample -ml of AgNO3 for blank) x N
-1
Cl (me L ) = --------------------------------------------------------------------x 1000
Aliquot (ml)
Or
Volume of 0.05 N AgNO3 used = Final reading - initial reading
= R3
-1
Cl (me L ) = R3 x 0.05 N AgNO3 x 1000/50
= R3
Note: Always run a blank along with actual titration.
Q. Why we first neutralize CO3 & HCO3 before Cl titration?

If we don't neutralize CO3 & HCO3, AgNO3 will react with CO3 & HCO3 to form AgHCO3. So
more AgNO3 will be utilize for chloride titration.
Always run blank for accuracy.

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DETERMINATION OF CALCIUM AND MAGNESIUM IN WATER

PURPOSE:
Determination of Calcium and Magnesium in Water
Burette
China dish
Pipette, 10 ml
Cylinder, 50 ml
Glass rod
Wash bottle
A. NH4Cl -NH4 OH buffer solution: Dissolve 67.5 g NH4Cl in 570 ml concentrated NH4OH, make
the volume up to l litre.
B Sodium hydroxide (NaOH), 4 N: Dissolve 160 g NaOH in distilled water, make the volume of
the solution to 1 litre .
C. Standard calcium chloride solution (CaCl2) , 0.01 N: Dissolve 0.5 g CaCl2 pure (calcite crystals
) in 10 ml of approx. 3 N (1+3) HCl and dilute to a volume of 1 litre.
D. Eriochrome black-T indicator (EBT): Dissolve 0.5 g of EBT and 4.5 g hydroxyl amine
hydrochloride (NH2O.H. HCl, H3NO.HCl) in 100 ml of 95 % ethanol.
E. Ammonium purporate indicator (C8H4N5O6. NH4): Thoroughly mix 0.5 g ammonium purporate
with 100 g of potassium sulphate (K2SO4).
F. EDTA (Versenate) solution, 0.01 N: Dissolve 2.0 g of EDTA and 0.05 g magnesium chloride
hexahydrate (MgCl2.6H2O) in distilled water and dilute to a volume of 1 litre . Standardized the
solution against reagent C using given titration procedure.
4. METHOD:
Calcium: Pipette 10 ml of pre-treated aliquot in a conical flask. Add 5 drops of reagent B and add
50 mg of E. Titrate against F from orange red to lavender/purple end point. When closed to the
endpoint, reagent F should be added drop wise (each drop after 5-10 second) as the colour change
is not instantaneous.
Calcium + Magnesium: Pipette 10 ml of aliquot in a conical flask. Add 10 drops of reagent A, 3-
4 drops of reagent D. Titrate against reagent F to a change in colour from wine red to bluish green.
ml of ETDA sol. for sample -ml of EDTA for blank x N

++ ++ ++ -1
Ca or Ca + Mg (me L ) =------------------------------------------------------------------- x1000
Aliquot in ml

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R1-R2 x 0.01 x 1000

= -----------------------
10
= (R1-R2) = R me L-1
Mg++ (me L-1) = Ca++ + Mg++ –Ca++ (All expressed as meL-1)

Always run a blank.

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DETERMINATION OF SULPHATE IN WATER

1. PURPOSE:
Determination of Sulphate in Water
2. EQUIPMENTS/APPARATUS
Spectrophotometer
Electric balance
Volumetric flask
Pipette
3. REAGENTS/MEDIAS:
A. Acid Mixture: 125 ml HNO3 + 250 ml Acetic Acid + 100 ml H3PO4 (85 %) Dilute to one litre
with deionized water.
B. Acid Sulphate solution (20 ppm S): 86 ml conc. HCl + 100 ml S solution (100 ppm). Make
volume upto 500 ml with deionized water.
C. BaCl2.2H2O Crystal: 20-60 mesh crystal
E. Gum Acacia Solution: Dissolve 0.5 g gum acacia in 50 ml deionized water. Mix and filter. Add
50 ml acetic acid. Filter if necessary.
F. SO4 – Standards: Standards of 5, 10, 15 and 20 ppm from 100 ppm stock solution
4. METHOD:
Take 5 ml sample in a 50 ml volumetric flask. Add 5 ml mixed acid reagent and 1 ml acid
sulphate solution and mix. Add 0.5 g BaCl2.2H2O crystals. Let stand undisturbed for 3 minutes
and then mix. Add 1 ml gum acacia reagent and mix. Make total volume 50 ml. Take readings of
samples and standards at 420-450 nm between 3 to 8 minutes after final shaking. Run reagent
blank.
5. CALCULATIONS:
Sulphate concentration (ppm) = Sulphate conc. (ppm) × Dilution factor
Verma, B. C. 1977.

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DETERMINATION OF SODIUM (Na) AND POTASSIUM (K) IN WATER
1. PURPOSE:
Determination of Sodium (Na) and Potassium (K) in water
Flame Photometer
Preparation of stock solutions
Sodium: Dissolve 2.5435g dry NaCl in 1-L, it will be 1000ppm Na.
Potassium: Dissolve 1.9103 g dry KCl in 1-L, it will be 1000ppm K.
However, both the stock solutions in combined form can easily be prepared by dissolving the said
amounts of both the salts in exactly one litre distilled water. Store in a cool and dry place.
Preparation of working standards:

Stock solutions so prepared will be used for the preparation of working standards by using the
formula:
C1V1 =C2V2
Where
C1 = Concentration of stock solution in ppm
V1 = Volume to be taken of stock solution in ml
C2 = Concentration of Na or K to be required in ppm
V2 = Total volume to be required in ml
V1 (ml of known solution) x C1 (ppm of known solution)

C2 (ppm required) = -------------------------------------------------------------------
V2 (Total volume to be made)
Working standard solution can be prepared of 10, 20, 30,------100 ppm concentration and for plant
0-10 ppm concentration or as desired.
4. METHOD:
CALIBRATION AND OPERATION:
1. "On" the fuel (gas).
2. Ignition
3. During ignition rotate the fuel knob clockwise for more gas supply to make ignition easy.
4. After the ignition rotate the knob anticlockwise and adjust the fuel in such a way that small
cones should be formed in flame (blue flame).
5. Aspirate the distilled water for at least 10-15 minutes before aspirating the working standard
solutions.
6. Be sure that you have adjusted the required filter i.e., sodium filter for Na or potassium filter

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for K by the knob provided.

7. Now adjust the "ZERO" on the scale by rotating the knob "BLANK".
8. Aspirate the standard working solution and record the reading in ppm e.g. when you feed 100
ppm, standard solution the reading on the scale should be 100. If it is not 100 then use "
COARSE” or "FINE” adjustment to make the reading 100. Use desired maximum standard to
adjust 100.
9. Without disturbing the blank, check whether there is "ZERO" on the scale when distilled water
is aspirated after aspiring working standard solutions. If so instrument is standardised according
to the given Na or K filter. If not so then adjust "ZERO" by adjustment "BLANK" and repeat all
the above procedure with standard working solution.
10. Before aspirating the next sample, always aspirate the distilled water until reading becomes
ZERO
11. If the sample to be analyzed have higher concentration (ppm) than the highest working standard
solution concentration, dilute the sample solution and multiply the reading with dilution factor.
12. After finishing the work aspirate the distilled water for at least 15 minutes for cleaning to avoid
the chance of chocking.
K or Na (ppm) =ppm from calibration cure of standards.

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DETERMINATION OF SODIUM ADSORPTION RATIO (SAR) AND RESIDUAL

SODIUM CARBONATE (RSC) OF WATER
PURPOSE:
Determination of Sodium Adsorption Ratio (SAR) and Residual Sodium Carbonate (RSC) of
Water
SAR = Na+ / [(Ca ++ + Mg++)/2]1/2
All the cations are expressed as me L-1.
Residual sodium carbonate can be calculated by using following equation
RSC, me L-1 = (CO3-- + HCO3-) – (Ca++ + Mg++)
All expressed in me L-1.

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DETERMINATION OF HEAVY METALS IN WATER

PURPOSE:
Determination of Heavy Metals in Water
Atomic Absorption Spectrophotometer / ICP-OES
Standard solutions for the respective heavy metals
4. METHOD:
Determine the heavy metals concentration using atomic absorption spectrophotometer / ICP-OES
after standardizing. Dilute the sample if necessary.
Direct concentration is given on these instruments
Standard method for the examination of water and waste water. (APHA, AWWA WEF) 20th
Edition, 1998.

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DETERMINATION OF BORON IN WATER

1. PURPOSE:
Determination of Boron in Water
Poly propylene volumetric flask, 50 ml
Pipette, 2 ml
Weighing balance
Funnel with stand
Wash bottle
Beaker, 50 ml
Spectrophotometer.
A. Buffer solution: Dissolve 250 g ammonium acetate and 15 g of ethylenediamine tetra acetic
acid (EDTA) in 400 ml of distilled water. Slowly add 125 ml glacial acetic acid and mix.
B. Azomethine – H reagent: Dissolve 0.45 g of reagent in 100 ml of 1 % L-ascorbic acid solution.
Fresh reagent should be prepared and store in a refrigerator.
C. Boron standard solution: Dissolve 5.709 g of boric acid (H3BO3) in distilled water (for hot water
extraction) and in 0.05 M HCl for HCl extraction and adjust the volume 1000 ml . This will be of
1000 ppm of boron solution. Make sub-stock solution to 100 ml of 100 ppm B. Then make
working standard as desired.
C1V1 = C2V2
100 x V1 = 0.5 x 100
5 x 100
V1 = ---------- = 0.5 ml of sub-stock solution to make 0.5 ppm B working standard.
1000
4. METHOD:
Filter water sample in boron free apparatus (Polypropylene). If boron free apparatus is not
available then pyrex glass apparatus should be dipped in concentrated HCl for a week and then
used.
Boron standards (0.5, 1.0, 1.5, 2.0 and 2.5 ppm) were prepared in distilled water. At 420 nm
wavelength determine boron (ppm) by spectrophotometer after developing color using
azomethine – H.
Transfer 1 ml sample in 50 ml polypropylene volumetric flask, add 2 ml buffer solution, add 2

ml azomethine- H reagent and mix. After 30 minutes read absorbance by specrophotometer
directly at concentration mode or by graph using standard curve prepared from standards
readings.

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B (ppm) = R × dilution factor

Where
R = spectrophotometer reading
Gaines, T. P. and G. A. Mitchell. 1979. Commun. Soil Sci. Plan Anal. 10:1099-1108.

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SOIL FERTILITY RESEARCH INSTITUTE PUNJAB, LAHORE

AGRICULTURE DEPARTMENT, GOVERNMENT OF THE PUNJAB

SOIL AND WATER ANALYSIS MANUAL

DR MUHAMMAD AKRAM QAZI

Reviewed & Approved by: DR SHAHZADA MUNAWAR

SOIL AND WATER ANALYSIS MANUAL

BASIC GUIDELINES FOR LABORATORY ACTIVITIES

Reviewed & Approved by: DR SHAHZADA MUNAWAR

Reviewed & Approved by: DR SHAHZADA MUNAWAR

* = X = core sampling positions

Reviewed & Approved by: DR SHAHZADA MUNAWAR

2. Under the tree shade.

Reviewed & Approved by: DR SHAHZADA MUNAWAR

Reviewed & Approved by: DR SHAHZADA MUNAWAR

DETERMINAION OF ELECTICAL CONDUCTIVITY OF SATURATION EXTRACT (ECe)

Reviewed & Approved by: DR SHAHZADA MUNAWAR

Vf (total volume of diluted solution)

CONVERSION OF 1:10 TO ECe

So EC1 (1:10) / 1.33 = EC2 i.e ECe

Reviewed & Approved by: DR SHAHZADA MUNAWAR

DETERMINATION OF SOIL REACTION (pH)

Reviewed & Approved by: DR SHAHZADA MUNAWAR

DETERMINATION OF SOIL SATURATION PERCENTAGE

Reviewed & Approved by: DR SHAHZADA MUNAWAR

Reviewed & Approved by: DR SHAHZADA MUNAWAR

DETERMINATION OF CARBONATES AND BICARBONATES IN SOIL

2R1 x 0.1 N H2SO4

Reviewed & Approved by: DR SHAHZADA MUNAWAR

(R2-R1) x Normality of H2SO4

(R2-R1) × 0.1 N H2SO4

* This reaction is completed in two steps as shown by the chemical reaction

Na2CO3 + H2SO4--------------------2 NaHCO3 + Na2 SO4-------i

Reviewed & Approved by: DR SHAHZADA MUNAWAR

DETERMINATION OF CALCIUM AND MAGNESIUM

Reviewed & Approved by: DR SHAHZADA MUNAWAR

R1-R2 x 0.01 x 1000

Reviewed & Approved by: DR SHAHZADA MUNAWAR

DETERMINATION OF CHLORIDE IN SOIL

Reviewed & Approved by: DR SHAHZADA MUNAWAR

DETERMINATION OF ORGANIC MATTER

me of K2Cr2O7 reduced = ( me of K2Cr2O7 added - me of FeSO4 used)

Reviewed & Approved by: DR SHAHZADA MUNAWAR

me of K2Cr2O7 added = (ml of K2Cr2O7 added x N)

% O C = % organic matter / 1.724

1 me of C of OM in soil = 1 x Eq. wt. of C / 1000

Reviewed & Approved by: DR SHAHZADA MUNAWAR

DETERMINATION OF SOIL TEXTURAL CLASS

Reviewed & Approved by: DR SHAHZADA MUNAWAR

Reviewed & Approved by: DR SHAHZADA MUNAWAR

Reviewed & Approved by: DR SHAHZADA MUNAWAR

DETERMINATION OF EXTRACTABLE POTASSIUM IN SOIL

Reviewed & Approved by: DR SHAHZADA MUNAWAR

DETERMINATION OF EXTRACTABLE SOIL PHOSPHORUS (OLSEN’S METHOD)

Reviewed & Approved by: DR SHAHZADA MUNAWAR

5. CALCULATIONS:- Extractable phosphorous in soil (ppm)=ppm p*x A x 50

A= Total volume of Extractant (ml)

6. REFERENCE / RELATED DOCUMENTS:

Reviewed & Approved by: DR SHAHZADA MUNAWAR

DETERMINATION OF SODIUM IN SOIL