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Soil Tech Lab Manual

The Soil Technology Laboratory Manual outlines various methods for analyzing soil properties, including pH, electrical conductivity, organic matter, and cation exchange capacity. Each section provides definitions, principles, procedures, and interpretations for the respective tests. The manual serves as a comprehensive guide for soil analysis techniques essential for understanding soil health and nutrient availability.

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0% found this document useful (0 votes)
9 views48 pages

Soil Tech Lab Manual

The Soil Technology Laboratory Manual outlines various methods for analyzing soil properties, including pH, electrical conductivity, organic matter, and cation exchange capacity. Each section provides definitions, principles, procedures, and interpretations for the respective tests. The manual serves as a comprehensive guide for soil analysis techniques essential for understanding soil health and nutrient availability.

Uploaded by

Farhana Tabasum
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
You are on page 1/ 48

Soil Technology Laboratory Manual

(Started on June 22, 2009)


Contents

1 Determination of pH and electrical conductivity of soil


2 Estimation of soil organic matter
3 Estimation of cation exchange capacity
4 Determination of major available nutrients
5 Determination of particle size distribution
6 Estimation of single value soil physical constants
7 Determination of particle and bulk density of soil
8 Measurement of soil strength
9 Evaluation of liquid and plastic limits
10 Compactibility test
11 Determination of soil water contents
12 Evaluation of water retention characteristics of soil
13 Measurement of saturated hydraulic conductivity of soil
14 Measurement of infiltration rate
Determination of pH and electrical conductivity of soil

1.1. Determination of pH

1.1.1. Definition: pH is the negative logarithm to base 10 of the hydrogen ion


activity.
The acidity, neutrality or alkalinity of a soil is measured in terms of H+ ion
concentration or activity. Sorensen (1909) described this term.

1.1.2. Principle: The concept of pH is derived from the ion product of water:

H2O = H+ + OH-

Kw = [H+][OH-] = 10-14

at 25 oC fpr pure water. When H+ and OH- ion activities are equal, we call it a neutral
reaction status with the negative logarithm value for either of the ions returning a
value of 7. Because the dissociated hydrogen ions affect pH, the type of acid present
is important for the interpretation of acidity. Acids are typically either strong or weak
acids depending upon their degree of dissociation. The relationship between the
dissociation constant, hydrogen ion activity and pH may be derived from the simply
law of mass action relationship:

 HA
 H     K a or 2 pH  pK a  pHA
 A 

Note that at a concentration of 1 M, the pH is half of the pKa and hence pKa may be
directly estimated from measured pH in a molar concentration of acid. In soil, pH can
aid estimation of many ions such as Zn, Cu, B, Mn, Fe, and Mo.

pH meter: pH meter is a standard equipment for pH measurement. It has two


electrodes. Glass electrode measure the activity of H+ ion activity. The thin glass
separates the soil suspension from an internal known strength of H+ ion concentration
(HCl). There is an internal reference electrode of AgCl/ Cl- or Hg2Cl2/ Cl-. An
electrometric potential proportional to the H+ ion activity of the solution, in which the
glass electrode dips, develops across the glass membrane.
The description of the electrochemical cell used for the measurement of soil pH is:

H+ ion sensitive electrode Reference buffer Salt Bridge Reference Electrode

E (emf) = Eref – (RT/F) In aH+

= Eref + (2.303RT/F)pH

Or, pH = (E - Eref)/ (2.303RT/F) = (E - Eref)/ 0.059 [at 25 ºC]

In soil solution, pH < 7.0 indicate acid soil and >7.0 alkaline soil.
Soil pH range:
Extremely acidic <4.5
Very strongly acidic 4.5-5.0
Strongly acidic 5.1-5.5
Medium acidic 5.6-6.0
Slightly acidic 6.1-6.5
Neutral 6.6-7.3
Mildly alkaline 7.4-8.0
Strongly alkaline 8.1-9.0
Very strongly alkaline >9.0

1.1.3. Procedure:
 Adjust the pH meter by buffer (known pH solution). Generally, buffer solution
of pH 4.0, 7.0 and 9.2 are used.
 Calibrate the pH meter according to temperature.
 Weigh 10 g. soil.
 Add 25 ml distilled water 1:2.5 (soil: water).
 Mix well with a glass rod, and allow to stand for 30 mins.
 Stir suspension every 10 mins. during this period.
 After 1 hour, stir the suspension.
 Put the combined electrode (after calibrating) in suspension and take the
reading after 30 secs.

1.1.4. Reference:
Indian Society of Soil Science (2002) Fundamentals of Soil Science.
Baruah, T. C., and Barthakur, H. P. (1997) A Textbook of Soil Analysis. Published by
Vikas Publishing House Private Limited.
Basak, R.K. (2006) Soil Testing & Recommendation. Published by Kalyani
Publishers.
Sarkar, D.K., & Haldar, A (2005) Physical and Chemical Methods of Soil Analysis.
Published by New Age International Publishers.
1.2. Determination of Electrical Conductivity

1.2.1. Definition: Electrical conductivity (EC) is the measurement of capacity of a


solution to conduct the electricity.

1.2.2. Principle: In any solution, the conductivity of electricity is due to ions


present. Ions in soils are from salts. Therefore, soil EC is the measurement of
nothing but soil salt concentration or soil salinity.

1.2.3. Procedure

 Set the conductivity meter according to room temperature and then adjust the
EC of a standard solution from chart (generally, 0.01 or 0.1M KCl solution is
used).
 Prepare a 1:2 (soil: water) suspension.
 Stir the mixture with a glass rod occasionally for 30 min. or continuously for 5
min.
 Immerse the conductivity cell into the suspension and take the reading.

1.2.4. Determination of some other soil parameters from EC

When soil solution EC range 0.1-5.0 dS/ m,


Total dissolved Solid (mg/ lt) = EC (dS/ m) × 640
Sum of soluble cations or anions [mmol(p+ or -)/ kg] = EC (dS/ m) × 10
When soil solution EC range 3.0-30.0 dS/ m,
OP (bar) = EC (dS/ m) × (-0.36)

1.2.5. Interpretation:
According to US Soil Salinity Staff (1954),

EC (dS/ m) Comment
> 4.0 Saline Soil
<4.0 Non-saline Soil

1.2.6. Reference:
Indian Society of Soil Science (2002) Fundamentals of Soil Science.
Baruah, T. C., and Barthakur, H. P. (1997) A Textbook of Soil Analysis. Published by
Vikas Publishing House Private Limited.
Basak, R.K. (2006) Soil Testing & Recommendation. Published by Kalyani
Publishers.
Sarkar, D.K., & Haldar, A (2005) Physical and Chemical Methods of Soil Analysis.
Published by New Age International Publishers.
2. Estimation of soil organic matter

2.1. Definition: Soil organic matter (SOM) is considered as the whole non-mineral
fraction of the soil solid. SOM contain two parts: Non-decomposed organic matter
and humas fraction.

2.2. Principle: There is no good scientific method to determine SOM. For its
determination we determine the soil organic carbon (SOC) and multiply with 1.724
(Von Bemmlen factor) as SOC is the main constituent part of SOM.

Titrimetric Determination (Walkly-Black method): A known weight of soil is


treated with an excess volume of standard K2Cr2O7 in the presence of conc. H2SO4. It
results oxidation of SOC to CO2. The excess of K2Cr2O7, which is not reduced by
SOC, is titrated back against standard ferrous ammonium sulphate, in the presence of
NaF or H3PO4 using diphenyl-amine indicator.

Reaction:
Oxidation of carbon:
K2Cr2O7 + 4H2SO4 K2SO4 + Cr2(SO4)3 + 4H2O + 3Ō (×2)
3C + 6 Ō 3CO2

2 K2Cr2O7 + 8H2SO4 + 3C 2K2SO4 + 2 Cr2(SO4)3 + 8H2O + 3CO2

Titration:
FeSO4(NH4)2SO4,6H2O FeSO4 + (NH4)2SO4 + 6H2O (×2)
2FeSO4 + H2SO4 + Ō Fe2(SO4)3 + H2O

2FeSO4(NH4)2SO4,12H2O + H2SO4 + Ō 2(NH4)2SO4 + Fe2(SO4)3 + 13H2O

2.3. Procedure:

 Weigh 1 g soil in a 500 ml. beaker.


 Add 10 ml 1 N K2Cr2O7 and 20 ml concentrated H2SO4. Swirl the beaker to
mix the contents (for saline soil, 1.25% AgSO4 in H2SO4).
 Allow to stand for 30 mins.
 Add 200 ml distilled water, then add 10 ml concentrated H3PO4 and allow the
mixture to cool.
 Add 10-15 drops of diphenylamine indicator [(C6H5) 2NH].
 Titrate with 0.5 M [(NH4)2SO4.FeSO4.6H2O] until the colour changes from
violet-blue to green.
 Simultaneously prepare a blank solution containing all reagents but no soil.

2.4. Calculation
Weight of the soil =Wg
0.5 M (NH4)2SO4.FeSO4 solution for blank = B ml
0.5 M (NH4)2SO4.FeSO4 solution for samples = S ml

Volume of K2Cr2O7 used for oxidation of C = 0.5 × (B - S) ml


[1 ml of 1 N K2Cr2O7 = 1 meq = 3 (12/4) mg of organic C = 0.003g of organic C]
So,
% of organic C in soil (uncorrected) = 0.5 × (B - S) × 1 × 0.003 × (100/W) = X
Now, Walkly-Black has an average 77% recovery of SOC. So, correction factor =
100/ 77 = 1.3
Therefore,
% of organic C in soil (uncorrected) = X × 1.3 = R
Hence, % of organic matter in soil = R × 1.724

2.5. Interpretation: In Indian soil,

Organic C % Comment
< 0.50 Low
0.50-0.75 Medium
>0.75 High

2.6. Reference:
Indian Society of Soil Science (2002) Fundamentals of Soil Science.
Baruah, T. C., and Barthakur, H. P. (1997) A Textbook of Soil Analysis. Published by
Vikas Publishing House Private Limited.
Basak, R.K. (2006) Soil Testing & Recommendation. Published by Kalyani
Publishers.
Sarkar, D.K., & Haldar, A (2005) Physical and Chemical Methods of Soil Analysis.
Published by New Age International Publishers.
3. Estimation of Cation Exchange Capacity

3.1. Introduction: In soil, clay minerals and organic matter particles are charged
(dominantly negatively charged). There are two reasons of their charges.
a) Permanent charges due to isomorphous substitution (highest in 2: 1 clay minerals).
b) Non-permanent charges i.e. pH dependent charges (highest in organic matter).
For this charge, these soil particles have capacity to adsorb cations and there exchange
with soil solution cations. This property is called cation exchange capacity (CEC).
It is important as plants uptake maximum of its nutrients as cation form and plant
roots can only uptake cations from soil solution. This uptake results depletion of these
cations in soil solution, which is replenished by cations released from exchange sites
of soil particles. Actually, soil solution and exchange site cations remain in
equilibrium.
Previously CEC was expressed (unit) as meq/ 100 g. Recently the unit becomes cmol
(p+) /kg (though the conversion factor from previous to modern unit is 1).
The % of CEC obtained by basic cations is called percent base saturation (%BS).

There are two widely used methods for CEC determination.


a) Distillation method or NH4 saturation method (1 N NH4OAc, pH 7).
b) Centrifuge method or sodium saturation method (1 N NaOAc, pH 8.2).
Here , only the distillation method is given as that is the simplest as well as less costly
method.

Distillation method
3.2. Principle: In this method, CEC of soil is measured by leaching with neutral 1N
ammonium acetate (NH4OAc). This results saturation of exchange complex with NH4
ions. Then this adsorbed NH4 ions are determined by distillation of soil with magnesia
(MgO). The gas (NH3) evolved during this process is absorbed in known volume of
acid (taken excess amount). Then, the unreacted acid is back titrated with standard
alkali.

Reaction:

CH3COONH4 NH4+ + CH3COO-

X-Soil + NH4+ + CH3COO- NH4-Soil + CH3COOX

MgO + H2O Mg2+ + 2(OH)-

2NH4-Soil + Mg2+ + 2(OH)- 2NH3 + Mg-Soil + 2H2O

3.3. Procedure:
 Preparation of reagents:
1 N NH4OAc, pH 7: Dilute 114 ml glacial acetic acid (99.5%) with water to a
volume of approximately 1 lt. Add 138 ml NH4OH and then water to a volume
of 1980 ml. Adjust pH by adding NH4OH or CH3COOH.
 Determination of CEC:
Weigh exactly 10 g soil sample in 500 ml conical flask.
Add 50 ml NH4OAc solution to soil sample. Mix thoroughly and keep for
overnight (for NH4 saturation of exchange sites).
Transfer the solution onto a moist filter paper, seated inside a Buchner funnel
under suction.
Continue to leach the soil with NH4OAc solution (add 25 ml at a time). Add
more 150 ml to soil on filter paper for leaching.
To the soil on filter paper, add a pinch of NH4Cl crystal and leach with
alcohol. Continue the washing till the filtrate run free with chloride (test with
AgNO3).
After that, transfer the residue with filter paper to a 500 ml distillation flask.
Add 0.5 g MgO and 200-300 ml distilled water.
Connect the flask to the distillation apparatus.
Place a 250 ml beaker, containing 25 ml of 0.1 N H2SO4.
Start distillation.
NH3 evolved during the process can be confirmed by holding a litmus paper
(turned into red) at the end of distillation apparatus.
Back titrate excess acid with 0.1 N NaOH solution.
Run a blank.

3.4. Calculation

Weight of the soil taken = 10 g


Volume of 0.1 N NaOH required for sample titration = S ml
Volume of 0.1 N NaOH required for blank titration = B ml

meq. of NaOH used for sample titration = S × 0.1


meq. of NaOH used for blank titration = B × 0.1
meq. of H2SO4 consumed for NH3 absorption = (B - S) × 0.1
Now, 10 g of soil contain (B - S) × 0.1 meq. of cations
Therefore, 100 g of soil contain (B - S) × 0.1 × 10 meq. of cations = Soil CEC (meq/
100 g)

3.5. Reference
Indian Society of Soil Science (2002) Fundamentals of Soil Science.
Baruah, T. C., and Barthakur, H. P. (1997) A Textbook of Soil Analysis. Published by
Vikas Publishing House Private Limited.
Basak, R.K. (2006) Soil Testing & Recommendation. Published by Kalyani
Publishers.
Sarkar, D.K., & Haldar, A (2005) Physical and Chemical Methods of Soil Analysis.
Published by New Age International Publishers.
4. Determination of major available nutrients

4.1. Nitrogen (Available Nitrogen)


4.1.1. Introduction: In soil, Nitrogen (N) present in organic and inorganic forms.
However, maximum amount of it remains in organic form, which cannot be used by
plants. Amount of plant available N in soil depends upon N mineralization, which
again depends on C: N ratio. Plants can uptake only NH4+ and NO3- forms of N,
though they together hardly occupy 1% of total N in normal soils. It is therefore,
necessary to estimate the different forms of mineralized or available N. The alkaline
potassium permanganate (KMnO4) method (by Subbiah and Asija, 1956) is the
standard one for it.

4.1.2. Principle: A known weight of soil is treated with an excess of alkaline KMnO4,
which extracts easily oxidizable fraction of organic matter. Ammonia evolved is
absorbed in a known volume of standard acid, the excess of which is titrated against
standard alkali using methyl red as an indicator.

Reaction:
Alkaline Medium
2 KMnO4 + H2O 2 MnO2 + 2KOH + 3Ō
Oxidative Deamination
RCH.NH2COOH + Ō R.CO.COOH + NH3
Distillation
NH3 + H2O NH4OH
Absorption
2 NH4OH + H2SO4 (NH4)2SO4 + 2 H2O

H2SO4 + 2NaOH Na2SO4 + 2 H2O

4.1.3. Procedure:
 Preparation of reagents:
0.32% KMnO4: Dissolve 3.2 g of KMnO4 in distilled water and make up the
volume to 1 lt.
2.5% NaOH: Dissolve 25 g of NaOH in distilled water and make up the
volume to 1 lt.
N/ 50 (0.02 N) H2SO4 and N/ 50 (0.02 N) NaOH solution.
Methyl red indicator (0.15%): Dissolve 0.15 g of methyl red power in
absolute alcohol (ethanol) and make up the volume to 100 ml.

 Place 20 g soil in distillation flask.


 Add 20 ml water and 100 ml 0.32% KMnO4 solution.
 Pipette out 25 ml of N/ 50 (0.02 N) H2SO4 in a conical flask. Add 2-3 drops of
methyl red indicator and dip the end of the delivery tube into it.
 Pour 100 ml of 2.5% NaOH solution into the flask and cork it immediately.
 Distill the ammonia gas from the distillation flask and collect in H2SO4
solution. Continue distillation till the evolution of ammonia ceases completely
(test by bringing a moist red litmus paper near the outlet of the condenser,
which will turn blue as long as ammonia is being evolved).
 Titrate the excess of H2SO4 against N/50 (0.02 N) NaOH and note down the
volume of NaOH used. The end point is reached when the colour changes
from pink to yellow.

4.1.4. Calculation:
Weight of soil taken: 20 g
Volume of N/ 50 H2SO4 taken: 25 ml
Volume of N/50 NaOH used (titrate value): X ml
Volume of N/50 acid used for NH3 absorption: (25 - X) ml
Now, I ml of N/50 H2SO4 = 0.02 meq. Of N = 0.28 mg N = 0.00028 g N
Therefore, % of available N = (25 - X) × 0.00028 × 100/20 = Y
Available N in soil (ppm) = Y × 100000 = Z
Available N in soil (kg/ ha) = Z × 2.24

4.1.5. Interpretation:

Amount of N (kg/ ha) Comment


< 272 Low
272-544 Medium
>544 High

4.1.6. Reference:
Indian Society of Soil Science (2002) Fundamentals of Soil Science.
Baruah, T. C., and Barthakur, H. P. (1997) A Textbook of Soil Analysis. Published by
Vikas Publishing House Private Limited.
Basak, R.K. (2006) Soil Testing & Recommendation. Published by Kalyani
Publishers.
Sarkar, D.K., & Haldar, A (2005) Physical and Chemical Methods of Soil Analysis.
Published by New Age International Publishers.
4.2. Phosphorus (Available Phosphorus)
4.2.1. Introduction: Phosphorous (P), which is one of the primary plant nutrients,
present in soil in both organic and inorganic form. A considerable amount of it is
present in inorganic form (52-95%).

Forms of Soil P:
Soil P

Organic P Inorganic P

Ca-P, Fe-P, Al-P Occluded and


Reductant Soluble P

Plant can only absorb P in primary (H2PO4-) and secondary (HPO4=) orthophosphate
ions. In availability of these two types of orthophosphate ions are dependent on soil
properties mainly soil reaction. H2PO4- ions dominate in acidic range of pH (4.0-7.5)
while HPO4= ions dominate in alkaline range of pH (8.0-12.0). At pH 7.2, these two
ions have equal activity.
There are three standard worldwide-accepted soil P extraction and determination
methods.
Bray and Kurtz’s 1 (for acidic to near neutral soils).
Bray and Kurtz’s 2 (for tea, coffee, hilly rice soils).
Olsen’s Method (for neutral, alkaline and calcareous soils).

Bray and Kurtz 1


4.2.2.1. Principle: In this method, the soil is shaken with an extracting solution of
0.03 N NH4F in 0.025 N HCl (at pH 3.5), which dissolves the fractions of soil P (Al-P
and Fe-P). HCl results in the dissolution of Ca-P in addition to this, though it is in
negligible amount in this pH range.

Reaction:

3 NH4F + 3 HF + AlPO4 = H3PO4 + (NH4)3AlF6

3 NH4F + 3 HF + FePO4 = H3PO4 + (NH4)3FeF6

4.2.3.1. Procedure
 Preparation of reagents:
NH4F 1 N: Dissolve 37 g of NH4F in distilled water and make up the volume
to 1 lt.
HCl 0.5N: Dilute 20.2 ml conc. HCl to a volume of 500 ml with distilled
water.
Extracting solution (0.03 N NH4F in 0.025 N HCl): Add 15 ml of 1 N NH4F
and 25 ml of 0.5 N HCl to 460 ml of distilled water.
Dickman and Bray’s reagent: Dissolve 15 g ammonium molybdate
[(NH4)6MO7O24, 4H2O], in 300 ml distill water, warm about 60 ºC and filter, if
necessary, after cooling. Add 342 ml conc. HCl and make up the volume to 1
lt.
Stannous chloride (SnCl2, 2H2O) solution: Dissolve 10 g SnCl2, 2H2O crystals
in 25 ml conc. HCl, (40% SnCl2 stock solution) and store in brown bottle.
Then dilute 0.5 ml of the stock solution to 66 ml with distilled water (prepare
this solution just before use).

 Extraction: weigh 5 g soil and transfer to 100 ml conical flask.


Add 50 ml extracting solution to it.
Shake for 5 min.
Filter through Whatman 1.
Prepare a blank.

 Preparation of P solution of known concentration for standard curve:


Dissolve 0.439 g potassium dihydrogen orthophosphate (KH2PO4), in about
500 ml distilled water and add 25 ml 7 N H2SO4 and make up the volume to 1
lt. This gives a 100 ppm stock solution.
Then prepare 2 ppm by 50 times dilution of stock solution.
Take 5 ml of the different conc. of P solutions by pipetting out 0 (blank), 1, 2,
3, 4, 5 and 10 ml of 2 ppm solution in 25 ml volumetric flasks.
Add 5 ml of extracting solution to each of the P standard solution.
Add 5 ml Dickman and Bray’s reagent to all standard solutions (development
of yellow colour).
To avoid fluoride interference, 7.5 ml 0.8 M boric acid (50 g H3BO3 per lt)
may be added. The reaction is,

4 F- + H3BO3 + 3H+ = (BF4)- + 3H2O

Mix with about 5 ml of distilled water.


Add 1 ml of SnCl2 solution and make up to the mark with distill water
(development of blue colour).
Measure the intensity of the blue colour after 10 min, using 660 nm red filter
in colorimeter.
Plot the transmittance reading (%T) of the standard on the ordinate against the
conc. in ppm. In semi logarithmic graph paper for a straight line relationship.

 Colorimetric estimation of P:
Take 5 ml of the soil extracts in 25 ml volumetric flasks.
Add 5 ml Dickman and Bray’s reagent to all test solutions (development of
yellow colour).
To avoid fluoride interference, add 7.5 ml 0.8 M boric acid.
Mix thoroughly the content of the flask with about 5 ml of distilled water,
washing the neck of the flash down, to remove the adhering ammonium
molybdate.
Finally add 1 ml of SnCl2 solution (development of blue colour) and make up
to the mark with distill water. Mix thoroughly.
Measure the %T by colorimeter after 10 min, using 660 nm red filter and
determine the conc. of P from standard curve. Must take the reading within 15
min as colour started to fade after 15-20 min. Plot the reading on standardized
graph and get the ppm value.
4.2.4.1. Calculation
Weight of soil taken: 5g
Volume of extractant added: 50 ml
First dilution: 10 times (50/ 5)
Volume of the extract taken for colour development: 5 ml
Final volume made: 25 ml
Second dilution: 5 times (25/ 5)
Total dilution: 10 × 5 = 50 times
Transmittance (%T) of test solution: T
Conc. of P as read from standard curve: A ppm
Available P in soil: A × 50 ppm = A × 50 × 2.24 kg/ha
Available P2O5 in soil: A × 50 × 2.24 × 2.29 kg/ha

Olsen’s Method
4.2.2.2. Principle: In this method, soil is shaken with 0.5 M NaHCO3, at pH 8.5, in 1:
20 ratio, for 30 min. with Darco-G 60 (activated charcoal). Darco-G 60 absorbs the
organic matter in the sample and therefore gives clear extract. P in this solution is then
treated with ammonium molybdate [(NH4)6MO7O24, 4H2O], resulting formation of
heteropoly complex phosphomolybdate (yellow colour). Then it is reduced by SnCl2
(blue colour). The intensity of blue colour is proportional to P conc. in solution.
NaHCO3 mainly extract P from Ca-P through precipitation of CaCO3. However, it
also extract P from Al-P and Fe-P.

Reaction:
Exchange Reaction:

Exchange Exchange
Complex Phosphate+ HCO3 Complex HCO3 + Phosphate

Chemical Reaction:

Ca3(PO4)2 + 6NaHCO3 3Ca(HCO3)2 + 2Na3PO4

3Ca(HCO3)2 3CaCO3 + 3H2CO3

2Na3PO4 + 3H2CO3 2H3PO4 + 3Na2CO3

Ca3(PO4)2 + 6NaHCO3 3CaCO3 + 2H3PO4 + 3Na2CO3

4.2.3..2. Procedure:
 Preparation of reagents:
0.5 M NaHCO3: Dissolve 42.0 g of NaHCO3 in distilled water and make up
the volume to 950 ml approximately. Adjust the pH to 8.5 with dilute NaOH
solution and make up the volume to 1 lt.
Dickman and Bray’s reagent: Dissolve 15 g ammonium molybdate
[(NH4)6MO7O24, 4H2O], in 300 ml distill water, warm about 60 ºC and filter, if
necessary, after cooling. Add 400 ml 10N HCl and make up the volume to 1 lt.
Stannous chloride (SnCl2, 2H2O) solution: Dissolve 10 g SnCl2, 2H2O crystals
in 25 ml conc. HCl, (40% SnCl2 stock solution) and store in brown bottle.
Then dilute 0.5 ml of the stock solution to 66 ml with distilled water (prepare
this solution just before use).

 Extraction:
Weigh 1 g soil in 100 ml conical flask.
Add a pinch of Darco-G powder.
Add 20 ml 0.5 M NaHCO3 solution.
Shake the flask for 30 min. in electric shaker.
Filter the suspension through Whatman 1.
Prepare a blank.

 Preparation of P solution of known concentration for standard curve:


Dissolve 0.439 g potassium dihydrogen orthophosphate (KH2PO4), in about
500 ml distilled water and add 25 ml 7 N H2SO4 and make up the volume to 1
lt. This gives a 100 ppm stock solution.
Then prepare 2 ppm by 50 times dilution of stock solution.
Take 5 ml of the different conc. of P solutions by pipetting out 0 (blank), 1, 2,
3, 4, 5 and 10 ml of 2 ppm solution in 25 ml volumetric flasks.
Add 5 ml of extracting solution to each of the P standard solution.
Add 5 ml ammonium molybdate solution to all standard solutions
(development of yellow colour).
Shake the flask to avoid direct contact of SnCl2 with ammonium molybdate
solution.
Add 1 ml of SnCl2 solution and make up to the mark with distill water
(development of blue colour).
Measure the intensity of the blue colour after 10 min, using 660 nm red filter
in colorimeter.
Plot the transmittance reading (%T) of the standard on the ordinate against the
conc. in ppm. In semi logarithmic graph paper for a straight-line relationship.

 Colorimetric estimation of P:
Pipette out 5 ml extract in 25 ml volumetric flask.
Add 5 ml ammonium molybdate solution (development of yellow colour).
Shake the flask to avoid direct contact of SnCl2 with ammonium molybdate
solution.
Add 1 ml SnCl2 solution (development of blue colour) and make up volume.
Measure the %T by colorimeter after 10 min, using 660 nm red filter and
determine the conc. of P from standard curve. Must take the reading within 15
min as colour started to fade after 15-20 min. Plot the reading on standardized
graph and get the ppm value.

4.2.4.2. Calculation
Weight of soil taken: 5g
Volume of 0.5 M NaHCO3 solution added: 20 ml
First dilution: 20 times (20/ 1)
Volume of the extract taken: 5 ml
Final volume made: 25 ml
Second dilution: 5 times (25/ 5)
Total dilution: 20 × 5 = 100 times
Transmittance (%T) of test solution: T
Conc. of P as read from standard curve: A ppm
Available P in soil: A × 100 ppm = A × 100 × 2.24 kg/ha
Available P2O5 in soil: A × 100 × 2.24 × 2.29 kg/ha

4.2.5. Interpretation:

Amount of P2O5 (kg/ ha) Comment


< 22.5 Low
22.5-56.0 Medium
>56.0 High

4.2.6. Reference:
Indian Society of Soil Science (2002) Fundamentals of Soil Science.
Baruah, T. C., and Barthakur, H. P. (1997) A Textbook of Soil Analysis. Published by
Vikas Publishing House Private Limited.
Basak, R.K. (2006) Soil Testing & Recommendation. Published by Kalyani
Publishers.
Sarkar, D.K., & Haldar, A (2005) Physical and Chemical Methods of Soil Analysis.
Published by New Age International Publishers.
4.3. Potassium

4.3.1. Introduction: K is one of the macro nutrient required by plant. It plays a


variety role in plant body and therefore called as master cation. Plants can uptake
potassium (K) in only K+ form. Total K content of soil varies 0.5-2.5% but only 1-2%
of them are in available to plants (soil solution K). The total K in soil remains in the
following forms:
i) Mineral K as structural lattice (e.g. in mica, vermiculite etc.): 92-98%
ii) Non-exchangeable K (fixed in clay lattice): 1-10%
iii) Exchangeable K (in the exchangeable sites of clay): 1-2%
iv) Solution K (in soil solution):

iii + iv = Plant available K pool.


These two pools of K remains in equilibrium and when plant uptake results decrease
the solution K, K released from exchangeable sites.

4.3.2. Principle: The available K in soil can be extracted by CH3COONH4


(ammonium acetate). The diameter of K+ is 0.233 nm. NH4 is the ion of nearest
diameter (0.286 nm). Therefore, it can replace the K+ in the exchange sites (clay) and
release them into solution. After extraction, K+ (solution + exchangeable K+) is
measured in flame photometer.

K NH4

K NH4

Clay K + 5CH3COONH4 Clay NH4 + 5CH3COOK


K NH4

Flame photometer is a device used to determine the concentration of certain metal


ions e.g. sodium, potassium, lithium, and calcium. It is a controlled flame test with the
intensity of the flame colour quantified by photoelectric circuitry. The sample is
introduced to the flame at a constant rate. Filters select which colours the photometer
detects and exclude the influence of other ions. Flame photometer works in the
emission spectrometry principle. When K+ in the solution is exited, the electron from
outer orbital of K goes to the higher energy state (for fraction of a second). When it
returns back to stable state, it releases the energy which is specific.
Before use, the device requires calibration with a series of standard solutions of the
ion to be tested.

4.3.3. Procedure
 Preparation of standards for K (minimum 5):
Prepare a bulk 1000 ppm K solution (dissolve 1000 mg K i.e. 1.908 g KCl
in 1 lt).
Then prepare K solution of different strength (5, 10, 15, 20 and 30 ppm)
from that bulk solution by dilution.
 Preparation of reagents:
Neutral normal CH3COONH4 solution: Dissolve 77.09 g CH3COONH4 in
distilled water the make the volume to 1 lt. Use NH4OH or CH3COOH for
neutralization.
 Standardization of flame photometer.
 Weight 5 g soil in a 150 ml conical flask.
 Add 25 ml of neutral normal CH3COONH4 solution.
 Shake (in shaker for 5 min.).
 Filter using Whatman 1.
 Feed the filtrate into the atomizer of flame photometer.
 Get the reading from flame photometer.

4.3.4. Interpretation:

Amount of K2O (kg/ ha) Comment


< 136 Low
36-337.5 Medium
>337.5 High

4.3.5. Reference:
Indian Society of Soil Science (2002) Fundamentals of Soil Science.
Baruah, T. C., and Barthakur, H. P. (1997) A Textbook of Soil Analysis. Published by
Vikas Publishing House Private Limited.
Basak, R.K. (2006) Soil Testing & Recommendation. Published by Kalyani
Publishers.
Sarkar, D.K., & Haldar, A (2005) Physical and Chemical Methods of Soil Analysis.
Published by New Age International Publishers.
5. Determination of particle size distribution

5.1. Definition
The relative proportion of sand, silt and clay particles in soil is called soil texture. The
size of soil particles range over six orders of magnitude (Table 5.1) from boulders (1
m) to submicroscopic clays (<10-6 m).

Table 5.1: Size specification for different soil particles


Name Constitution Diameter (mm)
Coarse fragment Rock or mineral fragments > 2.0
Boulders Rock fragments > 600
Stone Rock fragments 250-600
Cobble stone Fully/partially rounded 75-250
rock or mineral fragment
Gravel Rock fragments 2-75
Soil separates Mineral particles < 2.0
Sand Soil particle 0.02-2.0
Silt Soil particle 0.002-0.02
Clay Soil particle < 0.002

The mineral fraction of soil is characterized with three major soil size classes: sand,
silt, and clay fractions with sizes 0.02-2.0 mm, 0.002-0.02 mm, and < 0.002 mm,
respectively. These fine earth fractions, also called as soil separates, have special
properties, which are associated with their large surface area. Mineral particle size
profoundly affects the physical, chemical and biological properties of soil including
soil aeration and drainage, soil water holding capacity, and habitable pore space in
soil. Based on the relative proportion of soil separates, twelve textural classes are
recognized the ranges for which are shown in Table 5.2.

Table 5.2: Textural classes with per cent composition


of sand, silt, and clay fraction
Sand (%) Silt (%) Clay (%)
Sand 85-100 0-15 0-10
Loamy sand 70-90 0-30 0-15
Sandy loam 40-80 0-50 0-20
Loam 23-52 28-50 7-27
Silt loam 0-50 50-88 0-27
Silt 0-20 80-100 0-12
Sandy clay loam 45-80 0-28 20-35
Clay loam 20-45 15-53 27-40
Silty clay loam 0-20 40-73 27-40
Sandy clay 45-65 0-20 35-45
Silty clay 0-20 40-60 40-60
Clay 0-45 0-40 40-100

5.2. Principle
The principle of sedimentation is used to determine percent composition of sand, silt,
and clay fraction in the laboratory. When fully dispersed and dilute suspension
containing spherical soil particles is allowed to settle, the particles fall freely in the
suspension with a terminal velocity (v). The expression for v may be derived by
equating the drag and buoyancy forces:
2 gr 2 (  p   l )
v
9
where r is the particle radius, p is the particle density, l is the density of the liquid, 
is the coefficient of viscosity, and g is the constant acceleration due to gravity. Once
the terminal velocity is reached, the time taken to travel a certain distance (usually top
10 cm of the suspension in a suspension cylinder of 1 L capacity) is calculated from
the diameter of particles of certain size. For example, it may be estimated that the time
taken for sand-sized particle to travel 10 cm of distance is about 5 minutes and that for
the silt-sized particle is about 5 hours. This information is utilized to sample
suspension from the top 10 cm of the soil suspension, oven dry the sample, and
estimate the mass of sample left after 5 minutes or 5 hours. The 5-minute sample
gives the mass of silt+clay fraction and the 5-hour sample gives the mass of clay
fraction. Knowing the initial mass of soil, one can then estimate the mass fraction of
different size fractions.

5.3. Procedure

Texture by Pipette Method:


 Take 20 g soil and 20 mL of water in a 100 mL glass beaker.
 Add 5 mL of 30% hydrogen peroxide and heat the content until effervescence
stops. If needed, add 5 mL additional peroxide.
 Add 10 mL 5% sodium hexametaphosphate solution. The whole content is
then transferred to a mixer. DO NOT fill the cup within 2 inches of the top,
otherwise it will splash over while being mixed. Attach the cup to the stirrer.
The top of the cup should be raised straight upwards and hooked securely
under the switch finger, with the base hooked over the lower finger support.
 Transfer the soil sample to the cylinder using the wash bottle. Make certain
that all of the soil is transferred from the cup to the cylinder. Make up the
volume to 1000 mL and mix the content with a plunger.
 After desired time is over, carefully pipette out 25 mL of solution from a depth
of 10 cm below the suspension surface.
 Oven dry the solution and take dry weights.

The relative amounts of sand, soil, and clay in the < 2 mm fraction of the component
layer is then estimated using the principle outlined in the principle.

Texture by Hydrometer Method:

Texture by ‘Feel Method


5.4. Data Sheet
Measurements
Symbol Item Value Units
(2 places behind decimal point)
W1 Weight of dry soil g
Weight of suspension sample after 5 minute of sedimentation
W2 Weight of moisture box g
W3 Weight of moisture box + g
sample before drying
W4 Weight of moisture box + g
sample after drying
o
T1 Temperature of suspension C
Weight of suspension sample after 5 hours of sedimentation
W5 Weight of moisture box g
W6 Weight of moisture box + g
sample before drying
W7 Weight of moisture box + g
sample after drying
o
T2 Temperature of suspension C

5.5. Sample Data and Calculation


Calculations
Symbol Item Value Units
(2 places behind decimal point)
W8 % of silt + clay particles %
= (W4 – W2)*1000*100 /
(W1*25)
W9 % of clay particles = (W7 – %
W5)*975*100/(W1*25)
W10 % of silt particles = (W8 – W9) %
W11 % of sand particles = (100 – %
W8)
Texture

5.6. Remarks

Note that the sedimentation time is approximately 5 minutes and 5 hours. One should
use exact sedimentation time depending on the viscosity and density measurements in
the blank samples for the solution and soil combinations used.

5.7. Reference

Gee, G.W., Bauder, J.W., 1986. Particle size analysis. In: A. Klute (Editor), Methods
of soil analysis, Part 1, Agronomy Monograph No. 9. ASA and SSSA, Madison, WI,
pp. 383–412.Agronomy Monograph 9.
6. Estimation of single value soil physical constants

6.1. Definition
The following physical properties may be estimated using a ‘keen box’ (also, called as
Keen Raczkowski box):
a) apparent density
b) absolute specific gravity
c) maximum water holding capacity
d) percentage of pore space
e) volume expansion
A Keen box is a cylindrical brass core with a perforated screen fitted in the middle.

6.2. Principle
Simple mass volume relationships may be used to estimate the above physical
constants for soils.

6.3. Procedure
 Weigh the Keen box fitted with a filter paper
 Pack the box with air dry soil sample (ensure uniform packing by gently
tapping the box on its side)
 Fill the box completely and level it using knife by removing extra soil at the
top of the box. Add extra soil and tap it to ensure that the box is full
 Take the weight of box and air dry soil
 Place the box on a tray containing water over-night. Water level in the tray
should be such that a portion of soil at the bottom is under water (about 0.5 cm
of water in the tray may be sufficient).
 After equilibration, remove the box from the tray and wipe excess water from
the outside of the box
 Weigh the box immediately
 Scrap out expanded portion of the soil at the top of the box to a pre-weighed
moisture can
 Weigh the Keen box with residual soil and the moisture box
 Dry both the soils in an oven
6.4. Data Sheet
Symbol Item Value Units
W1 Weight of Keen box + filter paper g
W2 Weight of Keen box + filter paper + air dry soil g
W3 Weight of Keen box + filter paper + saturated soil g
W4 Weight of Keen box + filter paper + residual g
saturated soil
W5 Weight of Keen box + filter paper + residual soil g
after drying
W6 Weight of empty moisture can g
W7 Weight of moisture can + wet soil g
W8 Weight of moisture can + oven dry soil g
Symbol Item Value Units
z Gravimetric water content of air dry soil %
r Radius of the Keen box cm
d Height of Keen box above filter paper cm

6.5. Sample Data and Calculation


Symbol Item Value Units
v Volume of soil = r h
2 cm3
AD Apparent density = (W2 – W1)/v g/cm3
Bulk density = (W2 – W1) x (100 –z)/v g/cm3
Spg Absolute specific gravity = (W5 – W1)/{v – g/cm3
(W4 - W1)}
Maximum = {(W3 – W1) – (W2 – W1)} x 100/(W2 – W1) %
water holding
capacity
% pore space = (W4 – W5) x 100/v %
Volume =[{(W7 – W8) + (W8 – W6)/Spg}/v] x 100 %
expansion of
100 mL soil

6.6. Remarks

Carefully check the definitions for the apparent density and specific gravity and
explore their relationship with soil bulk density and particle density. Also, pay
attention to the units. Attention also is required on careful removal of soil after
saturating the Keen box and also the moisture retained in the filter paper.

6.7. Reference

Sarkar, D. and A. Haldar. 2005. Physical and Chemical Methods in Soil Analysis,
New Age International.
7. Determination of particle and bulk density of soil

7.1. Soil Particle Density


7.1.1. Definition
Soil particle density (p) is defined as the mass of oven dry soil (105° C) per unit
volume of soil solids. Volume soil solids is the difference between the bulk volume
and the volume of soil pores. Particle density (p) of a soil changes little from year to
year and place to place, as it is dependent mainly upon its mineralogical composition
and humus content. Particle density for kaolinite and quartz is 2.65 g/cm3, however, it
can go as high as 5.02 for pyrite rich soils and as low as 1.5 g/cm3 for humus.

7.1.2. Principle
Determination of particle density of soil requires that the volume of soil solids is
known or in other words, the total soil pore volume is known. The difference between
bulk volume and pore volume will yield the volume of soil solids. Generally, liquid
displacement following the Archimedes’ principle in a pycnometer (pycn meaning
dense) is applied to determine the volume of soil solids.

7.1.3. Procedure
 Weigh the clean, dry specific gravity bottle.
 Place about 10 g of oven dry soil in the bottle.
 Weigh bottle with contents and record.
 Fill bottle about half-full with distilled water and swirl well.
 Take top off and heat bottle in water bath to 50-60° C for about 10 minutes.
 De-air in vacuum for 10-15 minutes.
 The purpose in swirling, heating and boiling is to remove all traces of
entrapped air. Failure to remove the air is the greatest source of error. Exercise
care in boiling so that the suspension does not boil over. If it boils over you
must start all over again!
 Fill pycnometer to the top and replace the stopper carefully (water should
overflow through the capillary hole in the top) Wipe bottle dry.
 Weigh the bottle and its contents.
 Empty and clean the bottle.
 Fill the bottle with water of known temperature and record that temperature.
 Weigh the water-filled bottle
 Clean, and store the bottle.
7.1.4. Data Sheet
Measurements
Symbol Item Value Units
(2 places behind decimal point)
W1 Bottle (empty) g
W2 Bottle + Soil g
W3 Bottle + Soil + Water g
W4 Bottle + Water (only) g
o
T Temperature of Water C

7.1.5. Sample Data and Calculation


Calculations
Symbol Item Value Units
(2 places behind decimal point)
W5 Mass of soil (= W2 - W1) g
W6 Mass of displaced H2O g
(= W4 + W5 - W3)
w Density of Water g cm-3
Vdw Volume of displaced H2O cm3
(= W6/w)
p Particle density (=W5/Vdw) g cm-3

7.1.6. Remarks
Particle density is the average density of the soil particles present and is usually
expressed in grams per cubic centimeter (g cm-3). The suggested S.I. units are Mg m-3.
Note that the numerical value is the same in both unit systems.

7.1.7. Reference

7.2. Soil Bulk Density

7.2.1. Definition
Soil bulk density (b) is defined as the mass of oven dry soil (105° C) per unit bulk
volume of soil. Bulk volume includes pore space. Bulk density of the surface
horizons of cultivated soils varies widely in time and space, as it reflects the degree of
soil packing. The b of surface soil decreases with increasing aggregation and
increases with increasing compaction. The b decreases immediately after tillage due
to soil loosening (fragmentation), but generally increases over time, as compared to
untilled soil, due to loss of organic stabilizing materials. The b also increases with
increasing depth because of the increasing weight of overburden and decreasing
disturbance. Bulk densities for soil materials range from 0.5 g/cm3 for organic soils to
1.9 g/cm3 for sandy soils.

7.2.2. Principle
The procedures used to determine b can be grouped as follows: clod methods, core
methods, excavation methods and radiation methods (Chapter 2, Dane and Topp,
2002). In this Lab we will take "undisturbed" soil samples for determination of b by
the core method. In this method, a soil core of known volume is dried at 105 oC for
24 hours to get oven dry mass whose volume equals the volume of the core.

7.2.3. Procedure
Field Sampling: Establish a transect, with sampling locations spaced 1 m apart. Each
student is responsible for collecting one undisturbed soil cores (5 cm long by 5 cm in
diameter) according to the following procedure:

 Scrape away any vegetation to expose the mineral soil surface.


 Place a soil core sandwiched between two spacer rings in the barrel of a soil
core sampler.
 Orient the sampler vertically on the soil surface.
 Hammer until the top of barrel is flush with soil surface
 To remove, push sampler sideways, so that barrel comes out of soil on an
angle.
 Extract soil core from barrel; carefully remove upper and lower spacer rings.
 Using a knife (with the blade set at 20° to the core) trim the soil flush on both
ends of the core
 Place sample in an aluminum can for drying in the oven
 Identify your samples by writing your name and field location.

Repeat the above procedure to obtain a second undisturbed core.

In the laboratory: Store cores at 4° C until they can be processed. Remove one 6 cm
long by 5.35 cm in diameter core from the refrigerator. Process this core as follows:

 Weigh the trimmed soil core and record weight (W1).


 Dry the trimmed soil core in oven at a temperature of 105° C for 24 hours.
 Remove trimmed soil core from oven and record weight immediately (W2).
 Remove soil from core and record weight of the empty core (W3).
 Complete the calculations on the attached data sheet.

7.2.4. Data Sheet


Symbol Item Value (2 places behind Units
decimal point)

W1 Mass of moist soil and core g

W2 Mass of oven dry soil and g


core

W3 Mass of core g
V Volume of core cm3

7.2.5. Sample Data and Calculation

Symbol Item Value Units

W4 Mass of water g
(W1 – W2)

W5 Mass of oven dry soil g


(W2 – W3)

b Bulk density g cm-3

WBD Wet bulk density g cm-3


(W5 + W4)/V

g Gravimetric water content g g-1


(W4/W5)

v Volumetric water content cm3 cm-3


g *b

7.2.6. Remarks
The customary unit for bulk density is g cm-3. The suggested unit based on SI unit
usage is Mg m-3. Note that the number remains unchanged.

7.2.7. Reference

7.3. Sample Questions

1. Obtain data sheets from other students and prepare graphs showing b as a
function of distance along the transect. Discuss any trends that you observe.

2. A contractor needs 200 m3 of field moist topsoil for a construction site. When
loaded to capacity his trucks can carry 6,000 kg of field moist soil. Calculate
the number of truckloads needed to transport this soil from your sampling
location to the construction site.

3. Assuming erosion is occurring at a rate of 7 Mg ha-1 y-1, calculate the


thickness of the soil layer that will be lost from your sampling location over
the next year.

4. Derive the following relationship between porosity (Vp/V) and bulk density:
Vp/V = 1 - b/p

where V is the bulk volume of soil, Vp is the volume of pores; given your
estimate of b and p this lab, calculate the porosity for your soil.

5. Verify the formula used for calculating the particle density.

6. Calculate the error (expressed as a percentage) in your estimate of p assuming


a 0.2 cm3 air bubble had been trapped in the pycnometer.
8. Measurement of soil strength

8.1. Definition

8.2. Principle

8.3. Procedure

8.4. Data Sheet

8.5. Sample Data and Calculation

8.6. Remarks

8.7. Reference
9. Evaluation of liquid and plastic limits

9.1. Definition
Liquid limit: boundary between the liquid and the plastic state, also called as upper
plastic limit. This is the water content above which a mixture of soil and water flows
as a viscous liquid and below which soil is plastic.

Plastic limit: boundary between the plastic and the semi-solid state. Also, called as
lower plastic limit. This is the water content at which the soil will start to crumble
when rolled into a thread under the palms of the hand.

Plasticity is defined as that property of material, which allows it to be


deformed rapidly, without rupture, without plastic rebound, and without
volume change when the material is subjected to an external force.

Shrinkage limit: boundary between the semi-solid and the solid state. This is the
lower limit of the volume change at which there is no further decrease in volume
when wetted with water.

Plasticity Index=upper plastic limit – lower plastic limit

Knowing at which moisture content these limits occur for a given soil is a basic
geotechnical principle it is obvious why one would want to know at which moisture
content a soil reached it's liquid limit.

It is not appreciated as much in this country but in places like Hong Kong regular
liquid limit tests are carried out to determine whether hills will remain stable during
rain seasons in an effort to alleviate the problems of land slides.

9.2. Principle
The liquid, plastic and shrinkage limits apply to fine grained soils in which the water
content affects the physical properties, changing a clay soil from solid to liquid or
slurry. In 1911 A. Atterberg suggested the concept of boundaries to the four states in
which a soil may exist.

9.3. Procedure
 Any coarse articles present need to be removed, by hand or by wet sieving
(coarse particles are defined as any particles retained on a 425 micron sieve).
 Next a representative sample is required weighing around 200g. This sample
should be cut into small pieces using a knife or shredder and any coarse
particles removed with tweezers.
 Then the sample is transferred to a flat glass plate, distilled water is added and
the soil and water are mixed thoroughly with two palette knives until the mass
becomes a thick homogenous paste. The paste is then transferred to an air
tight container for 24 hrs to allow the water time to penetrate the soil fully.
 Use the grooving tool to divide the sample (in the cup) into two sections, do
this by running the grooving tool along the base of the cup from the hinge to
front edge of the cup in a continuous circular movement.
 Turn the crank handle at a rate of approximately 2 rotations/s so that the cup is
lifted and dropped, counting the number of bumps.
 Continue until the two parts of the sample come into contact at the bottom of
the groove along a distance of 13mm, measured with the end of the grooving
tool or with a rule.
 Record the number of bumps required.
 Add more water and repeat until the number of bumps for contact is the same
for two consecutive runs.
 This must be repeated at least three more times with varying amounts of
distilled water added, proceed from the dryer to the wetter condition of the
soil the amount of water to be added shall be such that when the four or more
moisture contents are plotted they are distribnuted evenly over the range 10-50
bumps, each time the soil is removed from the cup for the addition of water
the cup and grooving tool must be thouroughly cleaned, if the soil is to be left
for any length of time it should be covered with a damp cloth to prevent it
drying out.
 NOTE, if a number of tests are to be carried out they should be performed by
the same operator in an attempt to decrease the chance of operator error
creeping in.
 Calculate the moisture content of each test sample, plot the relationship
between the moisture content and the corresponding number of bumps
recorded on a semi-logarithmic chart, with the percentage moisture content as
ordinates on the linear scale and the number of bumps on the logarithmic
scale.
 Draw the line of best fit this is the flow curve. From the flow curve read off
the moisture content corresponding to 25 blows, to the first decimal place.
 Express this moisture content to the nearest whole number and report it as the
liquid limit.

9.4. Data Sheet


9.5. Sample Data and Calculation

9.6. Remarks

9.7. Reference
10. Compactibility test

10.1. Definition
The Proctor test provides a means of determining the optimum moisture content at
which a given amount of energy will compact a soil to its densest state (the maximum
bulk density). This test was developed in 1932 by R.R. Proctor. Proctor's basic
procedure is widely accepted and has been adopted as the standard criterion for soil
compaction in engineering practice (ASTM, 1991). It is included here to demonstrate
the relationships that exist between the volume fractions of air, soil and water when
all three fractions are varied.

10.2. Principle

It should be recognized that the bulk density versus water content curve determined
by the Proctor test is only valid for the particular amount of energy applied. The
maximum bulk density increases and is attained at lower values of optimum moisture
content with increasing compactive effort. However, the optimum gravimetric water
content at which maximum bulk density occurs always approximately 80% of the
gravimetric water content at saturation (Hillel, 1980).

10.3. Procedure

Five points will be determined on the bulk density versus water content curve for a
Maury silt loam soil using standard Proctor molds and rammers. Each point will be
measured by a different group of students. The data thus obtained will be shared
among the groups.

 Weight the proctor mold


 Prepare wet soils with water contents ranging from 8 to 22%.
 Use 200 g of soil for this purpose.
 Mix soil and water thoroughly with a trowel.
 Add one third of the moistened soil to the Proctor mold.
 Drop the fully-extended rammer 25 times in a concentric pattern on the soil
surface.
 Add another one third of the moistened soil to the mold and repeat step #6.
 Add the last one third of the moistened soil to the mold and repeat step #6.
 Remove the extension collar, level off the excess soil and clean the outside of
the mold.
 Re-weigh the soil-filled mold.
 Detach cylinder from base plate.
 Take duplicate soil samples from the top and bottom of the cylinder for
determination of gravimetric water content.
 Break up soil and remove from cylinder
 Calculate gravimetric water content and bulk density. Obtain additional values
of bulk density and water content from other groups. Complete data sheet.

10.4. Data Sheet


OBSERVATIONS

1. Cylinder number

2. Cylinder mass g

3. Cylinder volume cm3 944

4. Cylinder + moist soil g

5. Can number

6. Can mass g

7. Can + soil + H2O g

8. Can + O.D. soil g

10.5. Sample Data and Calculation

9. Moist soil (in cylinder) g

10. Weight of H2O in can g

11. Weight of O.D. soil g

12. Water content g g-1

13. Average of (12) g

14. Weight of O.D. soil in cylinder g

15. Bulk density g cm-3

Note: O.D. signifies oven dry

10.6. Remarks

10.7. Reference
11. Determination of soil water contents

11.1. Definition
Water content is the amount of water present in soil and is expressed either on mass

Massof water
g 
Massof soil
Massof water
v    g b
Volumeof soil
where b is the soil bulk density. Mass of water can be determined by several
different methods. A summary of these methods are given below.

11.2. Principle
Thermo-gravimetric method

Convective oven drying method: In the gravimetric method, the water initially present
in a sample is determined by recording the loss of mass in response to heating of the
sample at 105 0C for 24 hours.

Microwave oven drying method: In this gravimetric method, a microwave is used to


dry the soil. Microwaves penetrate the samples giving more rapid heating and drying.

Time domain reflectrometry

This is an electromagnetic method in which the applied signal is guided along a


transmission line through a soil sample. The time delay between the reflection of the
pulse from the beginning and end of the soil transmission line is used to determine the
velocity of propagation through the soil along the transmission line. The relative
dielectric permittivity of the soil controls the velocity. Because water is the dominant
dielectrics in soil, the amount of water present is correlated with the bulk dielectric
constant of soil. This method is an indirect method.

 v  5.3x10 2  2.92 x10 2   5.5x10 4  2  4.3x10 6  3

Ground penetrating radar

In Ground penetrating radar, radio frequency signals are generated and radiated in a
wide range of angles from an antenna into the ground and a separate antenna receives
both the transmitted and reflected signals. The reflected signal in this method is
correlated with the dielectric constant of the soil.

Capacitance device

In capacitance probe designed for soil water content measurements, the measurement
electrodes are placed in the soil in such a manner that the soil acts as the dielectric of
a capacitor in a capacitive-inductive resonant circuit.

Neutron Thermalization
Density/Water probe

Principle

Density/water neutron-gamma probe (CPN Corporation) has a radioactive source


(Americium-241: Beryllium) of high- energy neutron. (mean energy of 5 Mev) and a
detector of slow neutrons (0.025 ev). High-energy neutrons emitted from the source
are slowed through repeated collisions with the nuclei of atoms in the soil. A small
fraction will be deflected back to the detector. Their energy level slowed to thermal
(room temperature) energy level. The concentration of thermal neutrons changes
mainly with hydrogen ions present in soil water.

The counter contains 10BF3 gas. On absorption of neutron, 10B isotope of B (boron)
emits  particles. When the  particles strike on the charged filaments of the counter,
electric impulses are counted.

To determine density, the cesium-137 source emits gamma radiation into the soil.
Some of the gamma radiation will pass through the soil and be detected by detector. A
soil of low density will give a higher count. A soil of high density will give a low
count for the same time, as the high density soil absorbs more gamma radiation.

Water calibration

Calibration equation for soil water determination

M=Ar+B

M = water content
A, B are calibration coefficient
r = count ratio

A = (MH-ML)/(RH-RL)

MH, ML are high and low water contents


RH, RL are probe count ratio value at high and low water level, respectively.

Sample Calibration Curve for the moisture/density probe:

11.3. Procedure
Gravimetric Sampling:
 Weigh the empty moisture box.
 Take the soil samples at desired depths.
 Put it in moisture box and seal it.
 Weigh the moisture box with wet soil.
 Dry it for 24 hours at 105 0C temperature in oven.
 Weigh it after oven heating.
Moisture/Density Probe:
Calibration of moisture density probe
 Place the moisture/density probe above the access tube.
 Switch on the depth probe by pressing start.
 Insert the probe at desired depth (it should be equal or more than 30 cm from
ground surface).
 Set units and time.
 Press CALIB key.
 Select MCALIB for moisture calibration.
 Select Moisture calibration no. like MCAL 2-16 (As MCAL 1 is occupied for
factory calibration).
 Display MCOEFF?.
 Press STEP to get MSLFCAL (self calibration).
 Press ENTER.
 Display R2….
 Feed value of R2 (As calculated manually by taking samples from that depth.
This can be fed in lab, right now feed any arbitrary value to continue for next
step).
 Press ENTER.
 Display C2….
 Press START (Be 10 ft away after pressing START).
 Display C2 count (Note this count).
 Below the probe at lower depth.
 Repeat the same procedure and note the second count.

Standard count
 Place the gauge on the CPN name plate depression on the top of the case. (no
other radioactive source should be within 30 feet of gauge).
 Switch on the depth probe by pressing start.
 Press STD switch.
 By pressing STEP key go to NEW STD?.
 Press ENTER.
 By Pressing STEP key come at DISP MCT (display moisture counts).
 Press ENTER (It will start taking new standard counts and will display count
value against each count no. 1-32).
 AVERAGE COUNT Value will display after completion.

11.4. Data Sheet

Symbol Item Value units


W1 Weight of empty box g
W2 Weight of moisture box g
and wet soil
W3 Weight of moisture box g
and dry soil
C1 Count value at first
depth
C2 Count value at second
depth
Cs Standard count (average)

11.5. Sample Data and Calculation

Symbol Item Value units


W4 Mass of water(W2-W1) g
W5 Mass of oven dry soil g
(W3-W1)
Өg Gravimetric water g
content (W4/W5)
ρb Bulk density of soil g/cm3
Өv Volumetric water cm3/cm3
content

Symbol Item Value units


MH Moisture content at first g/cm3 or cm3/cm3
depth
ML Moisture content at
lower depth
A Moisture calibration
coefficient
B Moisture calibration
coefficient
r Count ratio

11.6. Remarks
11.7. Reference
12. Evaluation of water retention characteristics of soil

12.1. Definition
A water retention curve is generated by plotting measured water contents as a function
of corresponding soil matric potentials. The relation is also called as matric potential
curve, water characteristic curve, water content-matric potential curve, and capillary
pressure-saturation relation. A WRC is a constitutive property of soil.

The water retentation curve depends on soil texture and soil structure. Organic matter
also affects the shape of the retentation curve.

12.2. Principle
Laboratory methods
Hanging water column
The hanging water column is a simple measurement technique for WRC wherein a
saturated soil column is kept in hydraulic contact with a porous plate of nonzero air
entry pressure. The bottom of the plate is connected to a hanging water column either
left open or form a U-tube as in a manometer. This column length may be varied to
achieve different target suctions. After soil gets equilibrated with the applied suction
its weight is taken to measure water contents gravimetrically. To determine a water
retentation curve is performed in a Buchner funnel, also referred to as a Haines
apparatus.
Tempe Pressure cell
In a pressure cell, the body of water under the porous plate is kept at about
atmospheric pressure, while a gas pressure, Pa > atmospheric pressure, is applied to
the soil sample. Total pressure head, h, is given by
h= ha + hm
When the wet soil sample is in contact with the wetted porous plate in a pressure cell
and the gas pressure is raised above atmospheric, water flows out of the sample
through the porous plate due to driving force caused by the increase in ha. As the soil
drains, hm and h decrease. Eventually, static equilibrium is established between the
soil water and the bulk water in the system below the porous plate.
Pressure plate extractor
Both the hanging water column and pressure cell method are limited to a minimum hm
value of about -850 cm of water column. The use of pressure plate apparatus avoids
this limitation. Principle is same as is for pressure cell.

12.3. Procedure
Sample preparation
For undisturbed soil samples
 Take the few core boxes (5 to 8 cm in diameter, 1 to 6 cm in height) to collect
the soil samples.
 Remove the weeds and level the ground surface.
 Place the core on ground surface and hammer carefully (soil should not
compact).
 Remove excess soil and transfer these cores to lab carefully.
 Place the sample on the porous plate for saturation.
 Let the water imbibe from the bottom of the soil sample.
 Slowly raise the water level outside the sample ring up to near top of the
sample ring (this procedure may take from several hours to many days).
 Once the wetting solution has wetted the surface of the soil, sample can be
assumed to be saturated
 If undisturbed soil samples are to be stored for extended periods of time at
their field water content, add few drops of propylene oxide to each sample, cap
them, and store in a refrigerator to prevent bacterial growth.

For disturbed soil samples


 Dry the soil in oven and pass through a 2 mm sieve.
 Place enough soil to pack the desired number of cores in a plastic bag.
 Add sufficient water to the soil to make it slightly cohesive (gravimetric water
content, of about 0.05 for sands, 0.08 to 0.1 is suitable for soils of finer
texture).
 Close the bag to minimize evaporation and mix the soil thoroughly 3-5 times
to allow the water to redistribute throughout the soil.
 Determine the gravimetric water content of soil in the bag from 3-5 random
samples.
 For the volume of the sample ring, calculate the required soil to get desired
bulk density.
 Place the ring on a flat surface and pore the required amount of soil in to the
ring.
 Insert the packing piston into the piston ring and compress the soil into the
sample ring.
 Saturate the soil (as mentioned for undisturbed soil sample).

Experimental steps
 Take a porous plate with the desire bubbling pressure and saturate it
completely.
 Drain most of the water from the space between the plate and the rubber sheet
and place the plate in the pressure chamber.
 Connect the pressure tubing to the plate at one end and to the inside end of the
pressure chamber outlet at the other end.
 Place the soil samples (saturated previously), on the top of the porous plate.
 Close the pressure chamber and apply the desired pressure.
 Water will start to flow of the pressure chamber (observe it from the water
level in the burette or glass beaker).
 When outflow has ceased, disconnect the outflow tubing from the pressure
chamber.
 Reduce the applied pressure to atmospheric and open the pressure chamber.
 Remove the soil samples and take weight of moist samples.
 Transfer the samples to tin cans and dry in oven for 24 hours at 1050C.
 Calculate the volumetric water content.
 Repeat this procedure for other pressure plates and get the moisture content
corresponding to each value of hm.

12.4. Data Sheet


S.N. Pressure applied Wt of soil mass Wt of soil mass Moisture content (Ө)
(cm of water) before oven drying after oven drying (W -W )
1 2
(W1) (W2)

12.5. Sample Data and Calculation

Symbol Item Value units


V Volume of soil sample g/cm3
Өs Saturated water content cm3/cm3
Ρ Bulk density g/cm3

12.6. Remarks

12.7. Reference
13. Measurement of saturated hydraulic conductivity of soil

13.1. Definition
When the saturated hydraulic conductivity is measured via infiltration into initially
unsaturated soil, it is referred to field saturated hydraulic conductivity, Kfs. Air
interrupt in a porous media when the porous medium is saturated by infiltrating water,
especially during downward infiltration under ponded conditions. The water content
of a porous media at field saturation is consequently lower than at complete or true
saturation.

13.2. Principle
Double or Concentric- Ring Infiltrometer
The double ring infiltrometers are used for measuring field saturated hydraulic
conductivity, infiltration rate, and cumulative infiltration. A double-ring infiltrometer
consists of two cylinders pounded to ground to a depth of 10 to 20 cm. Two cylinders
are placed concentrically with the outer cylinder serving as a buffer zone. The inner
cylinder is about 10 to 20 cm in diameter by 10 to 20 cm long, while the buffer
cylinder is about 50 cm in diameter and the same length as selected for the measuring
cylinder. These cylinders should be thin-walled with sharp outside beveled cutting
edge at the base to minimize resistance and soil compaction or shattering during
cylinder insertion.

13.3. Procedure
 Select the place and clean the weeds.
 Insert the cylinders vertically.
 Fix the hook gauge or some types of pointer at desired depth for ponding.
 Pond a constant head of water inside the measuring cylinder.
 Maintain the same ponding depth of water in buffer cylinder.
 Measure the quantity of water needed to maintain the constant head with
respect to time (when the water surface in the cylinder drops to the pointer or
hook gauge level, water is manually added to bring the water surface back up
to a preset mark).

13.4. Data Sheet

Symbol Item Value units


A Ring radius cm
H Head cm

13.5. Sample Data and Calculation

Cumulative time, t Water added Infiltration rate (R)


(min) (cm3) Cm/hr
13.6. Remarks

13.7. Reference
14. Measurement of infiltration rate

14.1. Definition

14.2. Principle

14.3. Procedure

14.4. Data Sheet

14.5. Sample Data and Calculation

14.6. Remarks

14.7. Reference
APPENDIX

THINGS TO KNOW ABOUT WATER


 At 4°C pure water has a density (weight or mass) of about 1 g/cu.cm, 1 g/ml, 1
kg/litre, 1000 kg/cu.m, 1 tonne/cu.m or 62.4 lb/cu.ft
 At 4°C pure water has a specific gravity of 1. ( Some reference the s.g. base
temperature as 60F.)
 Water is essential for life. Most animals and plants contain more than 60 % water
by volume.
 More than 70 % of the Earth's surface is covered with about 1.36 billion cubic
kilometers of water / ice
 The density of pure water is a constant at a particular temperature, and does not
depend on the size of the sample. That is, it is an intensive property. The density
of water varies with temperature and impurities.
 Water is the only substance on Earth that exists in all three physical states of
matter: solid, liquid and gas.
 When water freezes it expands rapidly adding about 9 % by volume. Fresh water
has a maximum density at around 4° Celsius. Water is the only substance where
the maximum density does not occur when solidified. As ice is lighter than water,
it floats.
 Water has a very simple atomic structure. This structure consists of two hydrogen
atoms bonded to one oxygen atom - H2O
 Note; kg/m3 divided by 16.02 = lbs/cu.ft. kg/m3 divided by 1,000 = g/ml
Convert g/cm3 = g/cc = g/ml = g/mL - they are all the same.
Table of Density of Pure & Tap* Water and Specific Gravity
Density Density Density Specific
Density Specific
Temp pure tap pure Gravity
pure water Gravity
( °C ) water water water 60°F
( kg/m3 ) 4°C reference
( g/cm3 ) ( g/cm3 ) lb/cu.ft reference
0 (solid) 0.9150 915.0 - - 0.915 -

0 (liquid) 0.9999 999.9 0.99987 62.42 0.999 1.002

4 1.0000 1000 0.99999 62.42 1.000 1.001


20 0.9982 998.2 0.99823 62.28 0.998 0.999
40 0.9922 992.2 0.99225 61.92 0.992 0.993
60 0.9832 983.2 0.98389 61.39 0.983 0.985
80 0.9718 971.8 0.97487 60.65 0.972 0.973

100 (gas) 0.0006 see steam tables ... - -

This is for average, clean drinking water. It will vary from area to area.

The Expansion of Water at Various Temperatures


The following table shows the volume that 1 gram of water occupies as temperature varies. Data
corrected for buoyancy and for the thermal expansion of the container.

Temperature (°C) Volume (mL)

17.0 1.0022

18.0 1.0024
19.0 1.0026

20.0 1.0028

21.0 1.0030

22.0 1.0033

23.0 1.0035

24.0 1.0037

25.0 1.0040

26.0 1.0043

The thermal coefficient of expansion of water is 0.00021 per 1° Celsius at 20° Celsius.

Density of Water (g/cm3) at Temperatures from 0°C (liquid state) to 30.9°C by 0.1°C inc.

0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9

0 0.999841 0.999847 0.999854 0.999860 0.999866 0.999872 0.999878 0.999884 0.999889 0.999895

1 0.999900 0.999905 0.999909 0.999914 0.999918 0.999923 0.999927 0.999930 0.999934 0.999938

2 0.999941 0.999944 0.999947 0.999950 0.999953 0.999955 0.999958 0.999960 0.999962 0.999964

3 0.999965 0.999967 0.999968 0.999969 0.999970 0.999971 0.999972 0.999972 0.999973 0.999973

4 0.999973 0.999973 0.999973 0.999972 0.999972 0.999972 0.999970 0.999969 0.999968 0.999966

5 0.999965 0.999963 0.999961 0.999959 0.999957 0.999955 0.999952 0.999950 0.999947 0.999944

6 0.999941 0.999938 0.999935 0.999931 0.999927 0.999924 0.999920 0.999916 0.999911 0.999907

7 0.999902 0.999898 0.999893 0.999888 0.999883 0.999877 0.999872 0.999866 0.999861 0.999855

8 0.999849 0.999843 0.999837 0.999830 0.999824 0.999817 0.999810 0.999803 0.999796 0.999789

9 0.999781 0.999774 0.999766 0.999758 0.999751 0.999742 0.999734 0.999726 0.999717 0.999709

10 0.999700 0.999691 0.999682 0.999673 0.999664 0.999654 0.999645 0.999635 0.999625 0.999615

11 0.999605 0.999595 0.999585 0.999574 0.999564 0.999553 0.999542 0.999531 0.999520 0.999509

12 0.999498 0.999486 0.999475 0.999463 0.999451 0.999439 0.999427 0.999415 0.999402 0.999390

13 0.999377 0.999364 0.999352 0.999339 0.999326 0.999312 0.999299 0.999285 0.999272 0.999258

14 0.999244 0.999230 0.999216 0.999202 0.999188 0.999173 0.999159 0.999144 0.999129 0.999114

15 0.999099 0.999084 0.999069 0.999054 0.999038 0.999023 0.999007 0.998991 0.998975 0.998959

16 0.998943 0.998926 0.998910 0.998893 0.998877 0.998860 0.998843 0.998826 0.998809 0.998792

17 0.998774 0.998757 0.998739 0.998722 0.998704 0.998686 0.998668 0.998650 0.998632 0.998613

18 0.998595 0.998576 0.998558 0.998539 0.998520 0.998501 0.998482 0.998463 0.998444 0.998424

19 0.998405 0.998385 0.998365 0.998345 0.998325 0.998305 0.998285 0.998265 0.998244 0.998224

20 0.998203 0.998183 0.998162 0.998141 0.998120 0.998099 0.998078 0.998056 0.998035 0.998013

21 0.997992 0.997970 0.997948 0.997926 0.997904 0.997882 0.997860 0.997837 0.997815 0.997792
22 0.997770 0.997747 0.997724 0.997701 0.997678 0.997655 0.997632 0.997608 0.997585 0.997561

23 0.997538 0.997514 0.997490 0.997466 0.997442 0.997418 0.997394 0.997369 0.997345 0.997320

24 0.997296 0.997271 0.997246 0.997221 0.997196 0.997171 0.997146 0.997120 0.997095 0.997069

25 0.997044 0.997018 0.996992 0.996967 0.996941 0.996914 0.996888 0.996862 0.996836 0.996809

26 0.996783 0.996756 0.996729 0.996703 0.996676 0.996649 0.996621 0.996594 0.996567 0.996540

27 0.996512 0.996485 0.996457 0.996429 0.996401 0.996373 0.996345 0.996317 0.996289 0.996261

28 0.996232 0.996204 0.996175 0.996147 0.996118 0.996089 0.996060 0.996031 0.996002 0.995973

29 0.995944 0.995914 0.995885 0.995855 0.995826 0.995796 0.995766 0.995736 0.995706 0.995676

30 0.995646 0.995616 0.995586 0.995555 0.995525 0.995494 0.995464 0.995433 0.995402 0.995371

0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9

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