Environmental Monitoring (September-2010) at Swatantra Bharat Mills, Najafgarh
INTRODUCTION
The Environmental Monitoring was carried out by the environment team of Spectro Analytical
Labs Ltd. at Residential cum light service industry at Plot No. 15, Swatantra Bharat Mills
Compound, Najafgarh Road, Delhi. Being a construction and development company DLF is very
much concerned about to reduce the environmental impact due to its Constructional and
Operational activities. The present work is concerning the existing environmental condition with
respect to water, waste water, air and noise levels.
Environmental monitoring programme is a vital process of any management plan of the operational
& development. This helps in signaling the potential problems that result in from the project and
will allow for prompt implementation of effective corrective measures. The environmental
monitoring will be required for both the construction and operational phases. The main objectives
of environmental monitoring are:

Assess the changes in environmental conditions;

Monitor the effective implementation of mitigation measures;

Warn significant deteriorations in environmental quality for further prevention action.
In order to meet the above objectives the following parameters need to be monitored:

Water Quality;

Ambient Air and Noise quality
Scope of work and the detail of the sampling are given in the following paragraphs:-
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SCOPE OF WORK
The scope for performing the environmental monitoring is already mentioned in the work order,
which is briefly given for ready reference.
1. Monitoring of Ambient air quality for the parameters namely PM 10, PM 2.5, Sulphur
dioxide (“SO2”) & Oxides of Nitrogen (“NO2”), Carbon Monoxide (“CO”), Ozone
(“O3”), Lead (“Pb”), Ammonia (“NH3”), Benzene (“C6H6”), Benzopyrene (“BaP”),
Arsenic (“As”), and Nickel (“Ni”), at the project site Monitoring of Ambient Noise Level
Monitoring (24-hrs, day & night Leq) at two locations (one at the project site & other
within the boundary of the project site).
2. Collection and Analysis of the Ground water samples from project site.
3. Collection and Analysis of Soil Sample from project site.
4. Monitoring of Ambient Noise Level (24 hrs) at the project site and at the project boundary
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Abbreviations used in the Report
PM 10 = Particulate Matter (< 10 micron sized particle)
PM 2.5 = Particulate Matter (< 2.5 micron sized particle)
GL = Ground Level;
SO2 = Sulfur Dioxide
NO2 = Nitrogen Dioxide
AAQ = Ambient Air Quality
dB = decibel
N.D = Not detected
MDL = Minimum Detection Limit
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INSTRUMENTS & APPARATUS
Air (Particulate Matter, PM 10) Monitoring Instrument
Instrument
Respirable
Dust Sampler
(RDS)
Make
M/s. Spectro
Instruments
Pvt. Ltd. –
New Delhi
Model No.
SLE -RDS
103/SLE GA 133
Instrument
Identification
No.
SAL/RDS/10, 23
Range and Sensitivity
SPM/RSPM
Gases
0.02 – 01.8
m3/min
0.2 – 3 LPM
± 0.2 LPM
3
±0.02 m /min
Filter Paper Details
APPRATUS
Filter Paper
MAKE SIZE
M/S Whatmann
International Ltd.
SIZE
PRODUCT
CATEGORY NO.
20.3 x 25.4cm
GF/A
CAT NO. 1820-866
Air (Particulate Matter, PM 2.5) Monitoring Instrument
Instrument
Fine
Particulate
Sampler
Make
Model No.
M/s. Spectro
Lab
Equipments
Pvt. Ltd.
SLE-FPS
105
Instrument
Identification
No.
Range and Sensitivity
SAL/FPS/01&2
16.67 LPM
PM
Filter Paper Details
APPRATUS
Filter Paper
MAKE SIZE
M/S Whatmann
International Ltd.
Spectro Analytical Labs Ltd.
SIZE
PRODUCT
CATEGORY NO.
47 mm
GF/A & EPM 2000
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Noise (Sound) Measuring Instrument
Instrument
Integrated Sound
Level Measurement
Instrument Standard
Accessories
Make
Baseline
Technologies
Spectro Analytical Labs Ltd.
Model No.
Instrument
Identification
2001
SAL/NOISE/IN
T/692
A0907-980
Detection
Limit
Lo 30-100dB
Hi 60-130dB
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Testing Methods Followed
S.No.
Particular
1
Testing Method to be Followed
Ambient Air Monitoring Parameter
PM 10
IS-5182 (part – 23) 1973, Handbook of Methods in
PM 2.5
Environment Studies (Vol 2) Published by ABD
A
B
C
SO2 (Sulfur Dioxide)
Publication – Jaipur
IS 5182 (Part – II) 1969, with Improved West &
D
NO2 (Nitrogen Dioxide)
Gaeke Method
Modified Jacobs – Hochheiser Method / Arsenite
Method
E
Carbon Monoxide (as CO),
Gas Chromatography
(mg/m3)
F
G
H
Ozone (as O3) (µg/m3)
Chemical Method
AAS Method after sampling on EPM 2000 or
Lead (as Pb) (µg/m3)
equivalent filter paper
Ammonia (as NH3)
Chemiluminescence
(µg/m3)
I
Benzene (as C6H6)
Gas chromatography based continuous analyzer
(µg/m3)
J
Benzo (O) Pyrene (as BaP)
Solvent extraction followed by HPLC/GC analysis
(ng/m3)
K
L
2
A
Arsenic (as As) (ng/m3)
Nickel (as Ni) (ng/m3)
AAS Method after sampling on EPM 2000 or
continuous 24 hours
SL 5868 issued by Baseline Technologies
equivalent filter paper
Noise Level Measurement
Noise Level in dB (A) for
Operational Manual of Noise level Meter, Model No.
3
Water Analysis
Standard Method for the Examination of Water & Wastewater, 21st Edition, Edited by Lenore S.
Clesceri, Arnold E. Greenberg, Andrew D. Eton is followed for analysis.
4
Soil Analysis: As per Protocol: FAO / IS: 2720
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RESULTS OF AMBIENT AIR QUALITY
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ID:111005079
Ambient Air Analysis Report
Name of the Project
Name & Address of the Company
- Swatantra Bharat Mills Compound
- M/s DLF Commercial Complexes Ltd; Plot No.15, Mills
Compound Najafgarh Road, Delhi.
Name of the Site
- Plot No. 15, Swantra Bharat Mills Compound, Najafgarh
Road.
Location of Sampling Point
- Near the Back Gate of the Project Area.
Date of Sampling
- 24/10/2011
Sampling Started at
- 11.00 P.M. (24.10.11)
Sampling Completed at
- 11.00 P.M. (25.10.11)
Actual Time of Sampling (minutes)
- 1440
3
Av. Flow Rate for SPM (m /min.)
- 1.0
3
Total Volume of Air Sampled for SPM (m ) - 1440
Average Ambient Temperature (oC)
- 26
Purpose of Monitoring
- To Assess Pollution Load
PARAMETERS
RESULTS
Limits as per CPCB (MOEF)
Industrial,
Residential, Rural
& other areas
Particulate Matter PM 2.5 (µg/m3)
122
60
3
Particulate Matter PM 10 (µg/m )
176
100
Sulphur Dioxide (as SO2) (µg/m3)
6.1
80
3
Oxides of Nitrogen (as NO2) (µg/m )
34.5
80
Carbon Monoxide (as CO), (mg/m3)
1.20
02
3
Ozone (as O3) (µg/m )
17.2
100
Lead (as Pb) (µg/m3)
N.D.
1.0
3
Ammonia (as NH3) (µg/m )
19.4
400
3
Benzene (as C6H6) (µg/m )
N.D
05
Benzo (O) Pyrene (as BaP) (ng/m3)
N.D
01
3
Arsenic (as As) (ng/m )
N.D
06
3
Nickel (as Ni) (ng/m )
N.D
20
Protocol – IS: 5182 (Pt - 4, 6 & 23) / IS: 2488, IS-13270
Spectro Analytical Labs Ltd.
Ecologically Sensitive
Area (notified by
Central Government)
60
100
80
80
02
100
1.0
400
05
01
06
20
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ID:111005079
Ambient Air Analysis Report
Name of the Project
Name & Address of the Company
- Swatantra Bharat Mills Compound
- M/s DLF Commercial Complexes Ltd; Plot No.15, Mills
Compound Najafgarh Road, Delhi.
Name of the Site
- Plot No. 15, Swantra Bharat Mills Compound, Najafgarh
Road.
Location of Sampling Point
- Near HSE office
Date of Sampling
- 24/10/2011
Sampling Started at
- 11.15 P.M. (24.10.11)
Sampling Completed at
- 11.15 P.M. (25.10.11)
Actual Time of Sampling (minutes)
- 1440
3
Av. Flow Rate for SPM (m /min.)
- 1.1
3
Total Volume of Air Sampled for SPM (m ) - 1584
Average Ambient Temperature (oC)
- 26
Purpose of Monitoring
- To Assess Pollution Load
PARAMETERS
RESULTS
Limits as per CPCB (MOEF)
Industrial,
Residential,
Rural
& other areas
Particulate Matter PM 2.5 (µg/m3)
128
60
3
Particulate Matter PM 10 (µg/m )
181
100
Sulphur Dioxide (as SO2) (µg/m3)
6.3
80
3
Oxides of Nitrogen (as NO2) (µg/m )
32.1
80
3
Carbon Monoxide (as CO), (mg/m )
1.15
02
Ozone (as O3) (µg/m3)
20.4
100
Lead (as Pb) (µg/m3)
N.D.
1.0
Ammonia (as NH3) (µg/m3)
18.4
400
Benzene (as C6H6) (µg/m3)
N.D
05
3
Benzo (O) Pyrene (as BaP) (ng/m )
N.D
01
Arsenic (as As) (ng/m3)
N.D
06
3
Nickel (as Ni) (ng/m )
N.D
20
Protocol – IS: 5182 (Pt - 4, 6 & 23) / IS: 2488, IS-13270
Spectro Analytical Labs Ltd.
Ecologically Sensitive
Area (notified by
Central Government)
60
100
80
80
02
100
1.0
400
05
01
06
20
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RESULTS OF GROUND WATER
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RESULTS OF GROUND WATER AS PER IS: 10500-1991
TESTS
Colour, Hazen
Units
Odour
Taste
Turbidity, NTU
pH Value
Total Dissolved
Solids, mg/l
T. Hardness
(asCaCO3), mg/l
Residual Free
Chlorine, mg/l
Chlorides (as
Cl), mg/l
Total Iron (as
Fe), mg/l
Fluorides (as F),
mg/l
RESULTS
< 5.0
LIMITS (MAX)
Desirable
Extended
5
25
IS- 3025(Pt-4): 1983
Unobjectionable
Agreeable
< 1.0
7.58
786
Unobjectionable
Agreeable
5
10
6.5 to 8.5
500
2000
IS- 3025(Pt-5): 1983
IS- 3025(Pt-7&8): 1984
IS- 3025(Pt-10): 1984
IS- 3025(Pt-11): 1984
IS- 3025(Pt-16): 1984
404
300
Nil
600
0.2 (Min) When Chlorinate
PROTOCOLS
IS- 3025(Pt-21): 1983
45 of IS-3025: 1964
195.68
250
1000
IS-3025(Pt-32): 1984
0.08
0.3
1.0
32 of IS- 3025: 1964
0.42
1.0
1.5
APHA-4500-D-F
BACTERIOLOGICAL TESTS
TESTS
Total Coli-forms/100ml
(MPN)
E. Coli/100ml
Spectro Analytical Labs Ltd.
RESULTS
<2.0
LIMITS
10 (Max)
PROTOCOLS
IS: 1622-2003
Absent
Absent
IS: 1622-2003
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RESULTS OF NOISE MONITORING
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ID:111005079
AMBIENT NOISE MONITORING REPORT (Swatantra Bharat Mills Compound)
Date: 24/10/11 to 25/10/11
Location: Near Office Area
Area
A
B
C
D
Time
Hourly Leq
dB (A)
MIDNIGHT
1:00 AM
2
3
4
5
6
7
8
52.3
52.4
51.2
52.1
50.3
51.0
53.2
57.6
61.9
9
65.6
10
67.9
11
69.0
12 NOON
68.6
13
66.6
14
67.5
15
68.4
16
66.8
17
67.5
18
65.8
19
63.9
20
58.9
21
57.3
22
55.7
23
53.3
Category of Area
Industrial
Commercial
Residential
Silence Zone
Spectro Analytical Labs Ltd.
Result dB (A)
Leq
L10
L50
L90
Lday
Lnight
Ldn
Lmax
Lmin
Limits in day (dB)
75
65
55
50
64.3
68.7
67.0
64.8
65.9
53.7
65.3
69
50.3
Limits in Night (dB)
70
55
45
40
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AMBIENT NOISE MONITORING REPORT (Swatantra Bharat Mills Compound.)
Date: 24/10/11 to 25/10/11
Location: Near Boundary Wall
Area
A
B
C
D
Time
Hourly Leq
dB (A)
MIDNIGHT
1:00 AM
2
3
4
5
6
7
8
51.9
50.0
50.4
49.7
48.0
50.4
53.9
56.0
60.9
9
63.1
10
66.6
11
67.6
12 NOON
68.5
13
67.4
14
68.5
15
67.6
16
67.8
17
68.9
18
65.2
19
62.0
20
58.6
21
55.4
22
53.9
Category
of Area
23
Industrial
Commercial
Residential
Silence Zone
Spectro Analytical Labs Ltd.
53.5
Result dB (A)
Leq
L10
L50
L90
Lday
Lnight
Ldn
Lmax
Lmin
Limits in day (dB)
75
65
55
50
64.0
68.6
66.8
64.6
65.7
52.2
64.8
68.9
48.0
Limits in Night (dB)
70
55
45
40
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RESULTS OF SOIL ANALYSIS
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Soil Analysis Report
S.No
TESTS
RESULTS
1
pH value
8.12
2
Conductivity, millimhos/cm
0.146
3
Bulk Density (g/cc)
1.43
4
Total Nitrogen (as N), % w/w
0.16
5
Total Organic Matter, % w/w
0.03
6
Phosphates (as P), mg/kg
4.89
7
Sodium (as Na), mg/kg
39.77
8
Potassium (as K), mg/kg
9.94
9
Calcium (as Ca), mg/kg
810.38
10
Magnesium (as Mg), mg/kg
47.23
11
Water holding capacity, % w/w
44.28
Texture
12
a. Sand, % w/w
62.54
b. Silt, % w/w
23.56
c. Clay, % w/w
13.90
Protocol: FAQ / IS: 2720
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MONITORING AND ANALYSIS METHODOLOGY
The IS methods are followed to decide the monitoring stations, analysis of different sample and
also alternative methods are used, where the cross verification is required.
[A] Ambient Air Quality Monitoring:
Two Respirable Dust Samplers (RDS) with gaseous attachment have been used for RSPM/SPM
Sampling. RDS with Gaseous attachment assembly is used for the collection of gaseous pollutants
such as SO2, NO2 and CO. The details of the instrument used for sampling is mentioned in the
separate annexure under the heading of details of Instruments & Apparatus.
For the measurement of fine particulate matter having an aerodynamic dia. Less than or equal to a
nominal 2.5 micrometer (PM2.5). Draw ambient air at a constant flow rate of 16.67 Lpm .Total
volume of the sampled air is automatically computed by the sampler from the measured sampling
flow rate .the mass concentration of PM 2.5 particles in the ambient air is computed by dividing the
total mass of collected particles by the total volume of sample air and is expressed in micro grams
per cubic meter of air . 37mm glass fiber filter and 1 ml of diffution oil or silicon oil.
For the collection of PM2.5 particulate matter we use 47mm PTFE (polytetrafluoro ethylene). The
ambient air enter the sampler air inlet and pass through the size selective inlet particles larger then
10micro are separated . it then moves through down tube to the impacter where particles larger
then 2.5 micro are cut off.the particles smaller then 2.5 micro are then collected on a filter paper
(47mm PTFE ) mounted in a filter cassette and kept in a holder .
[B] Water Quality Survey:
Water samples were collected in Pre-sterilized sampling container. Chemical and Bacteriological
analysis was carried out as per standard Methods for water and Wastewater Analysis, Published by
IS, APHA, etc.
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[C] Noise Level Measurement:
Instant sound level meter is used for the collection of data related to noise for continuous 24 hours
and for D.G. Set. The details of the instrument used for the sampling is mentioned in the separate
annexure under the heading of Details of instruments & Apparatus.
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METHODOLOGY OF AMBIENT AIR
QUALITY
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RESPIRABLE PARTICULATE MATTER
Principle
Ambient air laden with suspended particulates enters the system through the inlet pipe. As the air
passes through the cyclone, coarse, non-Respirable dust is separated from the air stream by
centrifugal forces acting on the solid particles. The separated particles fall through the cyclone’s
conical hopper and collected in the sampling bottle placed at its bottom. The fine dust forming the
respirable fraction of the total suspended particulate matter passes through the cyclone and is
carried by the air stream to the filter paper clamped between the top filter cover and the filter
adopter assembly. The respirable dust is retained by the filter and the carrier air exhausted from the
system through the blower.
RESPIRABLE SIZE CUT OFF
The repirable dust standard recommended by the Central pollution Control Board is a 10 micron
cut off size for respirable dust measurement. Moreover, the respirable tract like any other
inspection centrifugal separation system retains particulates with varying densities at different
levels. This implies that even relatively finer dust particles of materials having a higher specific
gravit5y are likely to be retained in the upper respiratory tract while large particulates of lighter
materials are likely to pass deeper into the respiratory system.
II) Procedure of sample collection:
Following steps are involved in the collection of samples;
a) Open the shelter of Respirable Dust Sampler (RDS), loosen the wing nuts and remove the
retaining ring from the filter holder.
b) Mount a pre-weighted and numbered glass fibers filter paper in position with the rough
side up and tighten the wing nuts.
c) Allow the RDS to run for the specified length of time (24 hrs)
d) During the sampling time, flow rate should be taken hourly
e) At the end of sampling remove the filter form the mount very carefully.
f) Fold the filter in half upon itself with the collected materials enclosed within.
g) Place the folder filter in a clean, tight envelope and mark it for identification.
h) Place the filter in a desiccator.
ANALYSIS OF SAMPLES:
In a lab, remove the filter from the desiccator and take out the filter paper from the envelope.
Examine the inside surface of filter paper and with the pair of tweezers; remove any accidental
objects such as insects. Dry the filter paper by keeping on watch glass in hot air oven at 105 0 C for
about one hour. Equilibrate the exposed filters for about one hour in desiccator. Carry the
desiccator to the balance and weight on the analytical balance to the nearest 0.1-milligram.
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I) Calculation of volume of air sampled:
V =Q x T
Where
V= Air volume sampled (m3 )
Q = Average flow rate ( m3 per minute)
T = Sampling Time (in minutes)
Q=
( Q1 + Q2)
2
Q1 = Initial sampling rate indicated by the orifice meter at the start of sampling
Q2 = Final sampling rate indicated by the orifice meter just before the end of sampling.
II) Calculations of mass concentration of Responded particulate Matter (RPM):
The mass concentration of RPM may be calculated as follows:
RPM (μg/m )
3
( Fw – Iw ) x 106
= ----------------------V
Where
Fw = Final weight of exposed filter paper in grams.
Iw = Initial weight of unexposed filter paper in grams.
V = Air volume sampled in cubic meter.
SPM (μg/m3) = RPM (μg/m3) +
Spectro Analytical Labs Ltd.
Weight of dust retained by the cyclone
---------------------------------------------------Volume of air sampled, m3
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METHODS FOR DETERMINATION OF OXIDES OF NITROGEN IN AMBIENT
AIR
Principle
The collection and fixation of nitrogen dioxide in air is done by scrubbing a known volume of air
through a solution of basic sodium arsenate. The absorbed nitrogen dioxide is determined
calorimetrically as the azo dye by using it to diazotize sulphanilamide in the presence of
phosphoric acid at a pH of less than 2 and then coupling it with N-(1-Naphthyl)-ethylenediamine
dihydrochloride. The method is standardized statically by using NaNO2 standard. Standardization
is based upon the empirical observation that 0.74 mole of NaNO2 produces same colour as 1 mole
of NO2. The absorbance of the highly colored azo dye is measured on a spectrophotometer at a
wavelength of 540 nm.
Range and Sensitivity
Analysis in the range of 0.04 to 2.0 μg/ml can be performed by this method. The monitoring range
of the method is 9 to 750 μg/ml. However, under certain conditions, with a sampling rate of 2.0
LPM for 24 hours, a sampling efficiency of 82% the range of the method is 9 to 450 μg/m3.
Nitrogen dioxide in the range of 420-750 μg/m3 is accurately measured by 1.1 dilution of the
collected sample.
THE GASEOUS SAMPLING ATTACHMENTS
A trapping is drawn from the suction side of the blower below the orifice plate assembly to provide
suction for sampling air through a set of impingers. These impingers are housed in separate
enclosures and kept in an ice tray.
The separate enclosure and ice tray insulate the impingers from ambient temperature and heat
generated in the motor of the blower. It has Gas Manifold and Rotameter to allow setting up of
independent sampling rates through each of impingers.
The gaseous sampling attachment can easily be detached from the main sampler and transported
and stored independently.
CALCULATION
I)
The concentration of nitrogen dioxide in microgram per meter cube in the sample may
be calculated as follows:
NO2 (μg/m3 ) = (A-Ao) x F x Vf
--------------------Va x Vt x 0.82
Where
A= Sample Absorbance
Ao= Reagent blank absorbance
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INTERFERENCE
Sulphur dioxide is a major interference due to nitric oxide is positive while that due to carbon
dioxide is negative. Interference from sulphur dioxide can be eliminated by converting it to
sulphuric acid by the addition of hydrogen peroxide.
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METHOD FOR DETERMINATION OF SULPHUR DIOXIDE IN AMBIENT AIR
Principle:
When sulphur dioxide from the air is absorbed in a sodium tetrachloromercurate solution it forms a
stable sodium dichloro-sulphitomercurate solution. The amount of sulphur dioxide is then
estimated by the colour produced when pararosaniline hydrochloride is added to the solution. The
magenta colour is produced and estimated at 560 nm.
Range & Sensitivity
The measurement should be reported to the nearest 0.005 ppm at concentration below 0.15 ppm
and to the nearest 0.01 ppm above 0.15 ppm.
Interference
Ozone and nitrogen dioxide interfere if presents in the air sample at concentration greater than
sulphur dioxide. Interference of nitrogen dioxide is eliminated by adding 0.06 percent sulphamic
acid in the absorbing reagent. Nitrogen dioxide interference may also be eliminated by adding 0.1
tuluidine after sample collection. Heavy metals interfere by oxidizing dichloro-sulphitomercurate
during sampling collection. The interference is eliminated by adding EDTA in the absorbing
reagent.
Procedure for gaseous sampling
8 hour sampling:
Place 30 ml of Tetra-Chloro-Mercurate (TCM) absorbing solution in the standard impinger.
Connect the sampling tube leading for manifold of High Volume Sampler. Check the flow rate
from rotameter; maintain the flow rate to accurately 1 LPM throughout the sampling period. Shield
the absorbing reagent from the direct sunlight during the sampling and after sampling. During hot
weather sampling is to be conducted by keeping the impingers impregnated in ice cubes.
24 hourly sampling
Place 50 ml of (TCM) solution in a large impinger and collect the sample at 1 LPM. Determine the
air volume by multiplying the airflow rate by the time in minutes. The solution after the sample
collection are relatively stable. At the temperature of 250C and above, the losses of SO2 occurs.
Therefore, it is advisable to store the samples at 50 C till the analysis.
Analysis of samples
After receiving the sample in the lab, check the volume of absorbing media and record it. Normally
the volume of absorbing reagent is likely to be reduced as a result of evaporation losses. Make up
the evaporation loss by adding fresh, boiled cooled distill water.
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Pipette 10 ml of aliquot from the sample into a 25 ml volumetric flask. Prepare a blank solution by
measuring 10 ml of unexposed Tetra-Chloro-Mercurate (TCM) solution into 25 ml volumetric
flask. Then add 1 ml sulphamic acid and allow to stand for 10 minutes for reaction, then ad 2 ml of
formaldehyde and 2 ml of working parasaniline solution. Mix up thoroughly and make up it with
freshly boiled and cooled distilled water to the volume. Take absorbance of the sample after 30
minutes at 560 nm on a spectrophotometer after setting the spectrophotometer at 0.00 absorbance
with blank.
Calculation
I)
The concentration of sulphur dioxide in microgram per meter cube in the sample may
be calculated as follows:
(A-Ao) x F x Vf
SO2 (/m3) = --------------------Va x Vt
Where
A= Sample Absorbance
Ao = Reagent blank absorbance
F = Calibration factor (g / absorbance unit)
Vf = Final volume of Sample (ml)
Va = Volume of air sampled (cubic meter)
Vt = Volume of sample taken for analysis
II)
Conservation of microgram/m3 sulphur dioxide to parts per million (PPM) may be
calculated as follows:
SO2 ppm = g SO2/3 x 3.82 x 10-4
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Ammonia (as NH3)
Principle: Ammonia is collected in 0.1 N Sulphuric Acid Solution (H2SO4) in a midget impinger to
form ammonium sulphate. The solution reacted with nessler reagent to produce a yellow brown
complex & determine by colorimetric method at the wavelength 440 nm.
Procedure:
Sampling: Take 20 ml of absorbing solution in midget impinger. Attach the impinger to air
sampling pump & draw air through impinger at a rate of 1 lpm for 1hr to 24 hrs. Record the volume
of air sample.
Analysis: Take the sample in 50 ml volumetric flask containing 2 ml of alkaline tartrate and
makeup to the mark with distilled water. Add 2 ml of nessler reagent to the flask & determine
absorbance after 10 minutes at 440 nm in a spectrophotometer. Treat the blank in the same manner
as the sample.
Calculation:
Ammonia, g/m3 = Abs  F  106
V
F- Factor
V- Volume of air sampled, liter
106 – Conversion from liter to cubic meter
Carbonmonoxide (as CO)
SAMPLING: Take the gaseous sample into a bladder through a suction pump.
ANALYSIS: Analyze it on the Gas Chromatograph.
CALCULATION:
Concentration of CO (ppm) = Sample Area x conc. of CO2 in Standard x vol. of standard
Standard Area x vol. of sample
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Ozone in Ambient Air (O3)
Principle: Micro amounts of ozone and other oxidant librated iodine when absorbed in a 1%
solution of potassium iodide buffered at pH 6.8 ± 0.2. The iodine is determined
spectrophotometrically by measuring the absorption of triiodide ion at 352 nm.
Range and Sensitivity: This method covers the manual determination of oxidant concentration
between 0.01 to 10 ppm (0.019-19.6mg/m3) as Ozone.
Reagent:
1. Double Distilled Water
2. Absorbing Solution: (1% KI in 0.1 M Phosphate Buffer). Dissolve 13.6 gm of potassium
dihydrogen phosphate (KH2PO4), 14.2 gm of disodium hydrogen phosphate (NaHPO4) or
35.8 gm of the dodecahydrate salt (NaHPO4.12H2O) and 10 gm of potassium iodide in
sequence and dilute the mixture to 1 lt with double distilled water.
3. Stock Solution: (0.025M) I2 Dissolve 16gm potassium iodide and 3.173gm of resublimed
iodine successively and dilute the mixture to exactly 500ml with DDW.
4. 0.001M I2 Solution: Take 4ml of the 0.025 M stock solution into a 100ml low volumetric
flask and dilute to the mark with absorbing solution.
Procedure:Take 10ml of the absorbing solution to a midget impinger. Sample at 0.5 to 3 l/m for up
to 30 minutes. Calculate the total volume of the air sample, also measure the air temperature and
pressure. Do not expose the absorbing reagent to direct sunlight.
Analysis: If appreciable evaporation of the absorbing solution occurs during sampling, add double
distilled water to bring the liquid volume to 10ml.
Within the 30 to 60 minutes after sample collection, read the absorbance in a cuvette at 352 nm
against a reference cuvette containing DDW.
Measure the absorbance of the unexposed reagent and subtract the value from the absorbance of the
sample.
Calculation: The concentration of O3 (ppm) = Total µl ozone per 10 ml
Volume of air sample in liter
Lead in Ambient Air (as Pb)
Principle of the Method: Airborne dust samples are collected on cellulose membrane filters
(EPM 2000). The filters samples are ashed using nitric acid to destroy the organic matrix and
solubilize the lead. The lead content of the ashed material is determined by atomic absorption
spectroscopy.
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Range and Sensitivity: By atomic absorption the detection limit for lead in aqueous solution about
Reagents:
1. Purity. ACS reagent grade chemicals or equivalent shall be used in all tests. References to
water shall be understood to mean double distilled water or equivalent.
2. Care in selection of reagents and in following listed precautions is essential if low blank
values are to be obtained.
3. Conc. Nitric acid (68 to 71%) redistilled specific gravity 1.42.
Nickel in Ambient Air (as Ni)
Principle of the Method: Samples are collected by drawing a known volume of air through a
membrane or glass fiber filter. The filter samples are ashed, extracted with acid, and the analysis is
subsequently made by atomic absorption spectroscopy using 23.9 nm nickel line.
Range and Sensitivity: This method is applicable to the determination of nickel in quantities of
Reagents:
1. Purity. ACS reagent grade chemicals or equivalent shall be used in all tests. References to
water shall be understood to mean double distilled water or equivalent.
2. Care in selection of reagents and in following listed precautions is essential if low blank
values are to be obtained.
3. Conc. Hydrochloric Acid (36.5 – 38.0%).
4. Conc. Nitric Acid (69.0-71.0%).
5. Nickel Shot.
6. Perchloric acid 72%.
7. Hydrochloric acid 1:10. Dilute 100 ml of conc acid to one liter with water.
8. Perchloric-Nitric acid Mixture. Add 10 ml of conc perchloric to 90 ml of conc nitric.
9.
Benzo[a]Pyrene (BaP) in Ambient Air
Principle of the Method: This rapid method, for the measurement of Benzo[a]Pyrene (BaP) in air
samples, is based on the chromatographic separation of air samples extracts on and activated
alumina column using a polar solvent, toluene, as the eluting agent. The concentration of
hydrocarbon in the eluates is determined from fluorescence emission measurements made on the
eluates.
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Range and Sensitivity: The method can measure concentrations in a prepared air sample extract or
fraction over the range of 0 to 0.25 micrograms of BaP of solution.
Reagents:
1.
2.
3.
4.
5.
6.
Cyclohexane. Spectrograde Cyclohexane.
Activated carbon.
Alumina. 100 to 200 mesh size, is heated for 24 hrs in an oven at 1400C before use.
Toluene.
Benzo[a]Pyrene(BaP).
Standard solutions of BaP. Solutions of BaP are prepared containing 0.005, 0.010, 0.015,
-free toluene. Weigh accurately 1.25 mg of BaP on
a micro balance and dissolve in 250 ml of Spectrograde toluene. Measure accurately 1.0 ml
of this stock solution and dilute to 1000 ml with Spectrograde toluene. Repeat this with
2.0, 3.0, 4.0 and 5.0 ml portions of stock solution, diluted in each case to 1000 ml.
Procedure: The chromatographic columns are setup in a fume hood and complete preparation of
column and elution procedure is carried out there. Fluorescence readings are made while the
elutions are in progress.
Using a clean metal punch of cork borer, 4 corcles of 35.5 mm diameter are cut from the high
volume glass fiber sample. These represent 1/10.5 of the total effective area of the filter. These are
placed in a microsoxhlet extractor on top of a wad of glass wool which prevents the carbon
particles from being washed over into the extract and avoids subsequent filtration. The area chose,
in this case, amounts to ca 10% of the filter. After 6 to 8 hr extraction with fluorescence-free
cyclohexane, the solvent extract is evaporated carefully in a current of nitrogen to 2 ml.
A chromatographic column is then prepared by slurrying the activated alumina with toluene and
filling the tube to a depth of 12.0 cm. the concentrated extract is placed on the alumina and after
rinsing with a further 1 ml of toluene, elution os carried out using toluene from beginning to end.
The first 25 ml of eluate are discarded and 3 ml fractions are collected thereafter up to a total of
about 30 fractions. Each fraction is scanned separately in the fluorimeter and those fractions
containing BaP and BkF are combined for further measurement.
Having combined all the fractions containing BaP and BkF, these are carefully evaporated and
made up to a final volume of 5.0 mol in toluene. Fluorescence emission measurements of peak
heights are now made using excitation wavelength 307 and 384 nm.
A blank determination is carried out on the glass fiber filter, glassware and reagents.
Calibration and Standards: Standards curves of fluorescence emission, in arbitrary units, are
prepared for the various concentrations of both BaP and BkF at the two exciting wavelengths 384
and 307 nm. i.e., the optimum excitation wavelengths for BaP and BkF. These are prepared by
plotting the height of the peaks against the concentration. The fluorescence emission intensities of
air sample extracts or fractions are also measured using the same two exciting wavelengths.
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Similar calibration curves are obtained when standard solutions are made up in eyelohexane. The
sensitivity is noticeable less in toluene than in cyclohexane solution. The emission of BaP with 384
excitation, is higher than the emission of BkF with 384 excitation, so that the toluene based BaP
measurement is somewhat better than a measurement made in cyclohexane.
Calculation:
Since the fluorescence emission intensity of BkF is much greater than that of BaP when a mixture
of the two is excited at 307 nm, the reading at this wavelength is essentially due to BkF. Having
determined the concentration of BkF, one can calculate the effect of this hydrocarbon when a
mixture is excited at 384 nm after which the BaP concentration may be calculated. Thus:The concentration of BkF
Emission of Sample at 307 nm excitation
Slope of BkF standard curve at 307 nm excitation
The concentration of BaP
Emission of Sample at 384 nm – (conc. BkF X Slope BkF standard curve at 384 nm excitation)
Slope of BaP standard curve at 384 nm excitation
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METHODOLOGY OF STACK
MONITORING & ANALYSIS
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Methods for Measurement of Emission from Stationary Sources
General Determination of PM Concentration consist essentially of sampling isokinetically a
measured amount of gas from the flue and separating the particle from the gas and hence
determining the particulate concentration to obtain a representative particulate sample the sampling
should be carried out i.e. the kinetic energy of the gas stream, in the stack should be equal to
kinetic energy of the gas stream through the sampling nozzle.
Procedure
1. Temperature& Pressure Measurement Take the temperature with the thermocouple&
pressure with pressure gauge.
2. Selection of location of sampling
Sample for particulate concentration at same traverse point where velocity measurement
were carried out
3. Gas velocity Measure gas velocity with probe along with sampling nozzle Sampling
Volume of gases (for 1.4m3)
4. Monitoring & Analysis For Particulate Matter (g/m3)
Insert the thimble in thimble holder & insert the probe in porthole of the stack at least 30
min.
Calculations:
Final wt. of filter paper – Initial wt. of filter paper / vol. x 103
For Volume
sampling time x flow rate / 100
Area of stack 3.14 d2/4
Quantity of emission: vel. Of flue gases x area of nozzle x 3600 x298 /Ts 0(k)
Where Ts is temp. in Kelvin & 298 is atmospheric pressure
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TEST: Sulphur dioxide (as SO2)
Principle: A gas sample is extracted from the sampling point in the stack. The acid mist,
including sulphur trioxide, is separated from the separated from the sulphur dioxide & the
sulphur dioxide fraction is measured by the barium thorin titration method.
Procedure:
Preparation of collection train: Measure 15 ml of 80% iso-propanol into the
impinger & 15 ml of 3% hydrogen peroxide into each of the first two Impingers.
Leave the final impinger dry & assemble the train. Check the sampling train for
leakage at the sampling site by plugging the probe inlet & pulling a vacuum
corresponding to pressure manometer. A leakage rate not in excess of 1% of the
sampling rate is acceptable. Carefully release the probe inlet plug & Impingers and
add more ice during the run to keep the temperature of the gases leaving the last
impinger at 200C or less.
Sample collection: Adjust the sample flow rate as required. Disconnect the Impingers
after purging discard the sample from the impinger into a polyethylene bottle.
Sample analysis: Pipette a 10 ml sample into a Erlenmeyer flask. Add 40 ml of isopropanol & add 2-4 drops of thorin indicator. Titrate to a pink end point using 0.01 N
barium per chlorate/ barium chlorides. Run a blank with each series of samples.
Calculation: Calculate the concentration of sulphur dioxide using the following formulaC= B-S  N32Vs103
Vs
Where,
B - Volume of barium per chlorate titrant used for blank, ml
S - Volume of barium per chlorate titrant used for sample, ml
Va- Volume of sample titrated, ml
Vs- Volume of absorbing reagent, ml
103- Conversion factor from liters to cubic meter.
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TEST: Nitrogen dioxide (as NO2)
Phenoldisulphonic Acid Method:
Principle:
Nitric oxide (NO), nitrous anhydride (N2O3), nitrogen dioxide (NO2), nitrogen tetraoxide (N2O4),
also vapor or mist of nitric acid (HNO3) and nitrous acid (HNO2), but not nitrous oxide (N2O) may
be collected and oxidized to the nitrate ion in an evacuated flask containing sulfuric acid and
hydrogen peroxide. The yellow compound resulting from reaction of the nitrate ion with
phenoldisulphonic acid is measured calorimetrically at 400 nm.
Range and Sensitivity:
a) The phenoldisulphonic acid method is sensitive to 1 µg of nitrate in a water sample.
b) A 1000 – ml air sample as collected in an evacuated flask of this volume will permit
accurate determination of 50 or more ppm (by volume) of oxides of nitrogen as nitrogen
dioxide (NO2). Accordingly, the application of this method to ambient air is appropriate
only to industrial locations where the concentration may exceed 50 ppm.s
Reagents:
Nitrate and Nitrite Free Water, Hydrogen peroxide (3%), Sulfuric Acid, Ammonium Hydroxide.
Absorbent Solution:
1.0 ml of H2O2 (3%) in 100 ml of H2SO4 (3:997). For high concentrations of oxides of nitrogen, the
amount of H2O2 should be increased to 3 ml. Since dilute H2O2 may be unstable, these solutions
should not be kept for a prolonged period.
Phenoldisulphonic Acid Reagent:
Dissolve 25 g of phenol in 150 ml of conc. sulfuric acid (H2SO4 sp. gr. 1.84) by heating on a steam
bath (100 C). Cool, add 75 ml of fuming sulfuric acid (15% SO2) and heat on the water bath for 2
hr. Cool and store in a brown glass bottle. The solution should be colorless; in deteriorates on long
standing.
Procedure:
Sampling: Sampling may be conducted by use of an evacuated flask or bottle. Pipet 25.0 ml of
absorbent solution into the sampling container. The T-tube is connected to the tube of the container
cap. The mercury manometer or accurate vaccum gauge is attached to one branch of the T-tube and
the three-way Y stopcock to the other. The vaccum pump is attached to a second branch of the
stopcock and the sampling probe to the third. By successive of the stopcock plug, the container is
first evacuated to the incipient boiling point of the absorbing solution, and the manometer reading
recorded, then air is drawn through the sampling line or probe to flush it, and finally the sample is
collected in the evacuated container. The cap of the container is turned to seal the sample and the
T-tube disconnected. The temperature is recorded.
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Analysis:
1. The glass flask or bottle in which the sample has been collected should remain in contact
with the absorbent overnight to complete oxidation to nitrate.
2. Transfer the absorbent solution quantitatively from the container into a 200 ml
evaporating dish.
3. A blank should be treated in the same manner as the sample.
4. Add NaOH solution to the sample solution and to the blank in the evaporating dish until
just basic to litmus paper.
5. Avoid adding excess NaOH as this may dissolve some silicate from the dish and later
cause turbidity. Evaporate the contents of the evaporating dish to dryness on a hot water
or steam bath and allow to cool. Using the glass rod rub the residue thoroughly with
2.0ml phenoldisulphonic acid reagent to insure solution of all solids.
6. Cool and add 20 ml distilled water, stir, and then add sufficient fresh, cool NH4OH
dropwise (about 6 or 7 ml) with constant stirring to give a basic reaction with litmus. If
turbidity should occur, filter the solution through 7-cm, rapid, medium-texture filter
paper into a 50 – ml volumetric flask.
7. Wash the evaporating dish three times with 4 to 5 ml of water and pass the washings
through the filter. Since some yellow color may be left on the filter paper.
8. Instead of filtering to remove the turbidity, the EDTA reagent may be added dropwise
with stirring until the turbidity redissolves. Make up the volume to 50 ml in a volumetric
flask with water and mix thoroughly.
9. Read the absorbance of the sample against the blank in the photometer at 400 nm. If a
greater dilution is required, dilute the blank to the same volume.
10. Convert the absorbance found by means of the calibration curve to mg of NO2.
Calculations:
The volume of gas sample may be corrected to standard conditions by the following calculations:
(Vf - Vr) P.298.2
V=
760 (t – 273.2)
Where
Vs = Volume of gas sample corrected to standard conditions of 760 torr and 25 C, in milliliters.
Vf = Volume of sampling flask upto stopcocks in milliliters,
Vr = Volume of absorbent reagent,
P = Vaccum in sampling container as measured by the manometer, in mm and t = Sample
temperature, C.
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Calculation of concentration of NO2 in Parts per Million by Volume
Oxides of nitrogen as NO2
24.47W x 106
=
ppm
46.0 Vs
532W x 103
Vs
Where
=
ppm
Vs = volume of gas sample corrected to standard conditions, in milliliters.
W = milligrams of oxides of nitrogen found (as NO2).
24.47 x 103 = standard molar volume (760 Torr at 25 0C), in milliliters.
and
146.0 = formula weight of NO2
DETERMINATION OF CARBON MONOXIDE
SAMPLING Take the gaseous sample into a Tedller Beg through a suction pump.
ANALYSIS Analyze it on the Gas Chromatograph.
CALCULATIONS:
Concentration of CO (ppm) = Sample Area x conc. of CO2 in Std. x vol. of std.
Standard Area x vol. of sample
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METHODOLOGY OF SOIL
ANALYSIS
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METHODOLOGY FOR PHYSICO-CHEMICAL ANALYSIS OF SOIL
pH
Soils may be acidic, neutral or alkaline in reaction. The pH of soils is significant in crop production
and soil management practices because the various degrees of soil reaction are produced by the
chemical conditions which exist in soils. pH of soils affects plant growth due to either a depressed
solubility of some elements or to an increased solubility of others. It is useful in diagnosing the
feasibility of soil. The pH can be taken as negative logarithm of hydrogen ion activity. pH values
from 0 to 7 are diminishingly acidic, 7 to 14 are increasingly alkaline and 7 is neutral.
The pH of the soil generally varies from 4 to 8. In humid regions, it is usual to find a soil with
a pH of more than 7.5 or 8 but in arid regions where soluble salts of sodium carbonate accumulate
a pH of 9.5 to 11 is sometimes attained. Usually pH of agricultural soils in the humid regions varies
from 5 to 6.8. It is also possible to find mineral soils whose pH is 4. Soils having pH < 8.3 are
termed alkaline soils.
The determination of pH by conventional chemical means is not practicable and the equilibrium
which are involved depend to some extent on temperature. The precise accepted scale of pH can be
used only if approximate pH values are required.
The pH determination is usually done by electrometric method which is the most accurate method
and free of interference.
ELECTROMETRIC METHOD:
The pH is determined by measurement of the electromotive force of a cell comprising an indicator
electrode (an electrode responsive to hydrogen ions such as glass electrode (immersed in the test
solution) and a reference electrode (usually a mercury calomel electrode) contact between the test
solution and the reference electrode is usually achieved by means of a liquid junction, which forms
a part of the reference electrode. The EMF of this cell is measured with pH meter. This is a high
impedance electrometer calibrated in terms of pH.
Apparatus:
Glass Electrode:
This must be compatible with the pH meter used and must be suitable for the particular application.
Special electrodes are available for pH values greater than 10 and for use at temperature greater
than 600 C. Combined glass/reference electrodes are also available and are convenient to use.
Reference Electrode:
The mercury /calomel electrode is widely used but the silver/silver chloride electrode may be
preferably used on account of it being more reproducible and more reliable. Les-s .concentrated
solutions of KCI (e.g. 3.5 M KCI or 350 gm/litre) are more satisfactory as filling solutions than the
saturated solution often used because problems due to clogging of the electrode or the liquid
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junction will be avoided. To prevent dissolution of the silver chloride film, the potassium chloride
filling solution of Ag/AgCI electrodes should be saturated with AgCI.
pH Meter:
Both mains and battery operated models are available; the later type can be used for field’s
measurements. The most accurate pH meters can be read to better than = 0.005 pH unit.
Reagents:
1. Buffer solution for pH 4.0
2. Buffer solution of pH 6.8
3. Buffer solution of pH 9.2
NOTE:
In general analytical reagent grade chemicals are satisfactory for the preparation of these solutions.
Commercial buffer tablets are available in the market for the preparation of
solution of above pH values (each tablet dissolved in 100 ml gives the buffer solution of required
pH),
Procedure:
1. Standardize the pH meter according to the manufacturer's instructions.
2. Select a standard buffer solution with a pH value close to that of the soil to be tested.
3. Set the temperature control to the temperature of the buffer.
4. Set the meter to the pH of the buffer at that temperature.
5. Check the electrode response by measuring a second standard buffer solution of different pH.
6. Wash the electrode thoroughly first with distilled water and then with the sample.
7. Set the temperature control to the temperature of the sample.
8. Add 100 ml distilled water to 40 g soil.
9. Stir the mixture for 10 minutes, allow to stand for 30 minute, stir again for 2 minutes.
10. Measure the pH of the soil suspension.
11. Immerse electrodes in the sample and record the pH after stabilising the system.
Note:
Between measurements, the electrodes are kept in distilled water. New or dried out glass electrodes
should be prepared for the use by soaking in 0.1 N HCI for 8hours or according to the
manufacturer's instructions.
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CONDUCTIVITY
Conductivity is a capacity of water to carry an electrical current and varies both with the number
and types of ions the solution contains, which in turn is related to the concentration I of ionized
substances in the water. Most dissolved inorganic substances in water are in the ionized form and
hence contribute to conductance. The electro- conductivity measurement identifies soils which are
potentially saline. The electro- conductivity of saturated paste I extract is measured to determine
the level of salinity.
Conductivity measurement is affected by:
1. The nature of the various ions, their relative concentration and the ionic strength of water.
2.
Dissolve CO2
3. Temperature (for precise work, the conductivity must be determined at 250 C.
Instruments:
Most of the instruments commercially available for measurement of conductivity consist of.
1.
A source of alternating current.
2.
A wheat-stone bridge, a null indicator, and,
3.
A conductivity cell consisting of a pair of rigidly mounted electrodes, each conductivity
cell has its own cell constant: depending on its shape, size and the position of the
electrodes. Either the cell constant is mentioned by the supplier or can be determined by
using standard solution of KCl (0.01 M). Alternatively, by comparison with a cell of
known cell constant. Other instruments measure the ratio of I ~ alternating current through
the cell to voltage across it and have advantage of linear reading of conductance. Portable
battery operated instruments for both pH and conductivity are also available for field
studies.
Conductivity can be measured as per the instruction manual supplied with the instrument and the
results may be expressed as siemens I metre or 11 siemens I cm at temperature say 250 C at which
measurement was made. With reasonable care I conductivity meter needs very little maintenance
and gives accurate results. However few important points in this respect are:
1. Adherent coating formation of the sample substances on the electrodes should be -avoided
which requires thorough washing of cell with distilled water at the end of each measurement.
2. Keep the electrode immersed in distilled water.
3. Organic material coating can be removed with alcohol or acetone followed by washing with
distilled water.
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Reagents:
1.
Dissolve 0.7456 g of KGl in 1000 ml of distilled water. It is equivalent to 1.412 mhos/cm
conductivity at 250 G.
2.
Dissolve 7.456 g of KGI in 1000 ml of distilled water. It is equivalent to 12890 Jlmhos/cm.
Procedure:
1. Add 100 ml distilled water to 40 g soil.
2. Stir the mixture for 10 minutes, allow to stand for 30 minutes, stir again for 2 minute.
3. Allow to settle for 1 hour then measure the conductivity of the supernatant liquid.
Calculation = Observed conductance x Cell constant x temperature factor at 250 C.
Temperature
Factor
Temperature
Factor
3
1.62
18
1.14
4
1.58
19
1.12
5
1.54
20
1.10
6
1.50
21
1.08
7
1.46
22
1.06
8
1.42
23
1.04
9
1.39
24
1.02
10
1.36
25
1.00
11
1.33
26
0.98
12
1.30
27
0.97
13
1.27
28
0.95
14
1.24
29
0.93
15
1.21
30
0.92
16
1.19
31
0.90
17
1.16
32
0.89
BULK DENSITY
Bulk density of the soil is the dry weight of a unit volume of it. It is expressed as g/cm3. Generally,
the bulk density has been found in the range of 1.1 to 1.5 g/cm3 for medium to fine textured soil
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and from 1.2 to 1.65 g/cm3 for coarse textured soil. However, it has been slightly higher in case of
alkaline soils. The soils having high bulk density have been found to be inhibitive to root
penetration and have low permeability and infiltration. The bulk density is inversely related to pore
space of soil.
Apparatus
Oven, Measuring Cylinder and Chemical Balance.
Method
Collect the sample the dry it in an over at 1050 C until constant weight. Now put a little dried soil in
a measuring cylinder and record the volume. Now find out the weight of this volume of soil in a
chemical balance.
Calculations:
Bulk Density =
Weight of dry soil (g) = g/cm3
Volume of dry soil g/cm3
Bulk Density = W2 -W1 = g/cm3
V
W1 = Weight of empty watch glass in gm.
W2 = Weight of empty watch glass and soil in gm.
V = Volume of soil in cm3
WATER HOLDING CAPACITY
When soil is soaked with water, water fills all the pores between the par1icles of soil and no air
space exists as in the case of aquatic sediments. Such a soil is said to be at its maximum water
holding capacity or saturation.
Apparatus :Perforated Circular Soil boxes, Filter Paper Whatmann No. 1, Petri Dish, Oven and Chemical
Balance
Method
Collect the soil sample and crush it. Dry this sample in an oven at 105 0C. Keep a filter paper
(Whatmann No.1) inside the perforated bottom of the circular soil box. Then weigh the box. Now
fill it with dried soil sample. Then, find out the weight of the box filled with dried
soil. Keep the box in petri dish of 10 cm diameter having water for about 12 hours, so that water
enters the box and gets saturated the soil. Remove the box out of water from petridish, wipe it dry
on the outside and find out its weight.
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Calculations
Water Holding Capacity = (W3 -W2) - (W2 -W1)
W2 -W1
Where
W1 = Weight of empty box
W2 = Weight of box filled with dried soil
W3 = Weight of box with water saturated soil.
SOIL PARTICLE SIZE ANALYSIS
Principle
The particle size analysis of soil estimates the percentage sand, silt and clay contents of the soil and
is often reported as percentage by weight of oven-dry and organic matter-free soil.
The analysis is usually performed on air-dry soil. Based on the proportions of different particle
sizes, a soil textural category may be assigned to the sample.
The first stage in a particle size analysis is the dispersion of the soil into the individual particles.
These are the sand (2.00 -0.5 mm), silt (0.05 -0.002 mm) and clay «0.002 mm) fractions. Individual
soil particles are often bound into aggregates hence the requirement for dispersion.
The hydrometer method of silt and clay measurement relies in the effects of particle size on the
differential settling velocities within a water column. The setting velocity is also a function of
liquid temperature, viscosity and specific gravity of the falling particles. Theoretically the particles
are assumed to be spherical and to have a specific gravity of 2.65. If all other factors are constant
then the settling velocity is proportional to the square of the radius of the particle (Stoke's law). In
practice, therefore, correction for the for the temperature of the liquid is made. Greater
temperatures result in reduced viscosity due to, liquid expansion and a more rapid descent of
falling particles.
Reagents and equipment
Calgon (sodium hexametaphosphate) solution 10%. Dissolve 100 gm of calgon in 1 litre of distilled
water. This solution should not be kept over one month, when too o1d it loses its dispersing
efficiency because if will be converted to another compound.
Amyl Alcohol
Hydrometer with Bouyoucos scale in gm litre.
Soil dispersing stirrer. A high speed electric stirrer with a cup receptacle.
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Procedure
1. Weigh out 50 9 of air -dry <2 mm soil (100 gm in case of very sandy soil) into a 400 ml
beaker.
2. Saturate the soil with distilled water and add 10 ml of 10% Calgon solution. Allow to stand for
10 minutes.
3. Transfer the suspension to the dispersing cup and make to the mark in the cup with distilled
water.
4. Mix the suspension of 2 minutes with an electric high speed stirrer. Use ordinary bottles if a
cup is not available. Shake the suspension overnight if no stirrer is available.
5. Transfer the suspension into a graduated cylinder and rinse remaining soil into the cylinder
with distilled water. Insert the hydrometer into the suspension and add water to 1130 ml, then
remove the hydrometer.
6. Cover the cylinder with a tight fitting rubber bung and mix the suspension by inverting the
cylinder carefully ten (10) times. Note the time.
7. Quickly add 2-3 drops of amyl alcohol to the soil suspension in order to remove froth and after
20 seconds place the hydrometer gently into the column.
8. At 40 seconds take the hydrometer reading and measure the temperature of the suspension.
9. Repeat step 6 (mixing of the soil suspension 10 times) and allow the cylinder to stand
undisturbed for 2 hours.
10. After two hours take both hydrometer and temperature readings.
11. Make the necessary temperature corrections (Table 1). Temperature affects the hydrometer
readings and, because the hydrometer has been calibrated at 680 F (200 C), either correction
factors must be applied or the determination conducted in a temperature controlled room kept
at the correct temperature.
Calculations
Percent Sand: After 40 seconds, the sand present in 1 liter of the suspension, subtract this value
from the original sample weight. For example, if the hydrometer reading after 40 seconds corrected
for temperature is 18.0 g/liter, then silt + clay weight 18.0 g in the 1 liter soil suspension.
Therefore, the sand weights 50.0 -18.0 = 32.0 g in the 1 liter suspension (of the original 50.0 gm
air-dry soil sample). The percentage sand is calculated by dividing the sand content (32 g) by the
total (50 g) and multiplying by 100 as follows:
Sand % = 32.0 x 100 = 64%
50.0
Percent Clay: After 2 hours, the silt has settled. The hydrometer reading now reflects the -clay
content of the original suspension. For example, if hydrometer reading after temperature correction
is 4.7 g/litter, then the percentage of clay in soil is
Clay % = 4.7 x 100 = 9.45
50.0
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Percent Silt: The silt content is calculated by subtracting the sum of the clay and sand contents
from 100% or:
Silt % = 100 - (9.4% clay + 64% sand) = 26.6%
Soil Texture: Once the sand, silt and clay distribution is measured, the soil may be assigned to a
texture class based on the soil textural triangle (Figure 1). Within the textural triangle are various
soil textures which depend on the relative proportions of soil particles. Users simply obtain the
appropriate texture based on the particle size distribution. In the example, above (64% sand, 27%
silt and 9% clay), the corresponding soil texture is a sandy loam.
Table 1: Temperature correction for hydrometer readings of soil texture.
Temperature (0C)
Hydrometer correction g/liter
15
-
2.0
16
-
1.5
17
-
1.0
18
-
1.0
19
-
0.5
20
Nil
21
+ 0.5
22
+ 0.5
23
+ 0.5
24
+ 0.5
25
+ 0.5
Procedural notes
1. Cylinders for particle size analysis are calibrated depending upon the volume of the
hydrometer in use.
AVAILABLE NITROGEN
Principle:
Nitrogen is a major element essential for plant growth and it is a constituent of all proteins and
nucleic acids, It is generally taken up by plants as ammonium (NH4) and nitrates (NO3) ions, The
ammonium ions and nitrates ions are jointly make up to available nitrogen in soil, The two major
forms of available nitrogen, ammonium and nitrate produces a more rapid and spectacular effect on
the growth of plants than any other nutrients, This reflects the need to measure the herds and
subsequent movement patterns of these ions in soils during cropping in order to give firm
recommendations on fertilizer N/manure/crop residue uses,
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Because of rapid transformations of N to various forms, many procedures have been developed to
measures these have two ions (NH4 + NO3) in soils, These include the biological and chemical
methods, It has been demonstrated that the chemical methods is suitable for predicting the natural
available soil over a wide range of soils, The method gives measurements of NH4 N and NO3 N in
a single soil extract.
Extraction Procedure:
Weigh 10 gm freshly sampled soil (or soil kept in the refrigerator) into a plastic shaking bottle.
Add 100 ml of 2 N KCl extracting solution. Stopper and shake contents for 1 hour.
Filter through whatman no. 42 filter paper if analysis will not be completed in one day, store the
filtrate in the refrigerator. Microbial activity associated with N mineralization may also be
suppressed by storing the extract in a refrigerator when the distillation cannot be conducted
immediately.
Ammonia Distillation
1. Set up the ammonia distillation apparatus.
2. Pass steam through the apparatus for 30 min. Check the steam blank by collecting 50 ml
distillate and titrating with 0.002 N H2SO4. The steam blank should not require more than 0.2
ml of acid.
3. Check also the 2 M KCI for possible contamination by steam distilling 10 ml of this solution.
4. Add 25 ml of boric acid indicator solution to a 250 ml conical flask.
5. Place the flask under the condensor of the steam distillation apparatus so that the tip of
the condensor is within the surface of the boric acid indicator solution.
6. Pipette an aliquot of 10 ml of the soil extract into the distillation flask and add sodium
hydroxide solution directly to the bulk of the distillation flask. Start distillation by closing the
stop cock on the steam by pass tube.
7. When the distillate is collected about 50 ml in the conical flask. Stop the distillation by opening
the stop cock removing the burner. Rinse the tip of the condensor with a little distilled water.
8. Determine the ammonia nitrogen content in the distillate by titration with 0.002 N H 2SO4 .the
colour change at the end point is from green to a permanent faint pink. At the end point 1 ml of
0.002 N H2SO4 = 28 I.1g NH3 N2.
Calculation
Since 100 ml KGI is used to extract NH4 – N and NO3 -N from 10 g soil, then 10 ml KCl
(aliquot in distillation) is used to extract:
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10 x 10g Soil = 1 gm of soil
100
from titration 1 ml of 0.002 N H2SO4 = 28 I.1g NH3 -N
Therefore quantity of NH4 -N in 1 gm soil = ml of 0.002 N H2SO4
for data correction on soil dry (1030 G) basis. The procedure is as follows:
W1 = Weight of empty crucible.
W2 = Weight of empty crucible + fresh soil
W3 = Weight of empty crucible + dry soil
W3 - W1
W2 - W1
Hence the quantity of NH4 -N in 1 gm of oven dry.
Soil = ml of 0.002 N H2SO4 = 28 X (W3 -W1)/(W2 -W1) g
AVAILABLE PHOSPHORUS
Principle
The availability of soil phosphorus to plants varies greatly depending on reaction, mineralogical
composition, type of colloids present and content of organic matter in the soil. In many instances.
phosphorus occurs in the soil in the form of ion and aluminium phosphorus. These compounds are
only slowly or partially available to plants. The fluoride ion has the special property of complexing
aluminium and ferric ions in acid solution with consequent release of phosphorus held in the soil
by these trivalent ions. The dilute acid fluoride procedure is extensively used for the extraction of
available phosphorus of soils with -0.03 N NH4 F and 0.05 N HCI and has been found to give
results that are highly correlated with crop response to phosphate fertilization.
Reagents:
Ammonium fluoride. NH4 F. 1 N: Dissolve 37 g of AR NH4 F in distilled water and dilute the
solution to one litre. Store the solution in a polythene bottle.
Hydorchloric acid. HC/. 0.5 N: Dilute 44.2 ml of AR conc. HCI (11.2 N approx.) to 1000 ml with
distilled water
Soil extracting solution. or Bray p2 solution: Add 150 ml of 1 N NH4 F solution and 1000 ml of 0.5
N HCI to 3850 ml of distilled water placed in a 5 litre container. This gives a solution which a 0.03
N NH4 F and 0.1 N HCI. It keeps in glass more than one year.
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Boric acid. H3BO3. 0.8 M: Weight out 49.4 g of AR H3 B03 powder (AR) into 1 litre volumetric
flask Dissolve and dilute to mark with distilled water.
Ammonium molybdate antimony potassium tartrate solution (mixed reagent): Dissolve 6 g ammonium molybdate (AR) in 125 ml of warm (50 0C) distilled water. Dissolve 0.1455 g of 'wi
antimony potassium tartrate in 50 ml of distilled water. Add both solutions to 500 ml of 5 N
H2SO4 which has been transferred to a 1 litre volumetric flask. Mix thoroughly and dilute with
distilled water to 1 liter. Transfer to a brown reagent bottle. Store in a dark, cool place. The mixture
keeps for 2 months.
Ascorbic acid reducing agent: Dissolve 1.054 g ascorbic acid in 200 ml of ammonium required on
the day of analysis. The solution keeps of about 24 hours.
Phosphate standard stock solution: Weigh accurately 1.0982 g of dry KH2P04 (AR).
Transfer to a one litre volumetric flask. Dissolve in distilled water and make up to volume (1000
ml). The concentration of P is 250 mg/P/1000 ml, or 0.250 mg/P/ml.
Procedure:
1. Soil extraction: Weight accurately 2.5 g of dry soil (2 mm) into a 250 ml plastic bottle. Add 50
ml of Bray P-2 extracting solution and shake for 5 minutes. Filter through Whatmann NO. 42
filter paper. If filter is not clear, pour the solution back through the filter.
2. Pipette 10 ml of each phosphorus standard solution and 10 ml of soil extract into 50 ml
volumetric flasks.
3. Add about 20 ml of distilled water to each flask.
4. Add 5 ml of 0.8 M boric acid solution to each flask.
5. Add 10 ml of ascorbic acid solution to each flask.
6. Make to the mark with distilled water.
7. Stopper and shake contents well.
8. Measure the intensity of blue color at 880 nm after 10 minutes and before 30 minutes.
Preparation of Calibration curve: Pipette 1, 2, 5, 10, 15 and 20 ml of phosphate standard
solution into a 100 ml volumetric flask. Add 10 ml of soil extracting solution, 10 ml of
ascorbic acid reagent to each flask and fill upto the mark. After at least 10 minute but not more
than 30 minute, measure the absorbance of each sample at 880 nm using reagent blank as the
reference solution. Plot absorbance Vs phosphate concentration to give a straight line passing,
through the origin. Test at least one phosphate standard with each set of samples.
Calculations:
mg/P/100 gm of soil = Phosphate reading in mg from the graph x 100 gm of soil.
0.5
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CALCIUM CARBONATE
Introduction:
Inorganic carbonates either accumulates in the soil by pedogenic processes or inherited from
calcareous parent materials. It is used to define carbonatic, particle size, calcareous soil classes,
calcic and petrocalcic soil horizons. Its presence may lead to some nutrient deficiencies in the soil.
Methods of quantitative determination of calcium carbonate includes dissolution of carbonates in
acid and determination of carbon dioxide by titrimetry and by measuring the volume of evolved
carbon dioxide.
Principle
The dried soil sample 2 mm is reacted with hydrochloric acid and evolved carbon dioxide gas is
absorbed in dilute hydrochloric acid and the remaining hydrochloric acid is titrated with sodium
hydroxide.
Reagents & Apparatus: Chemical Balance
i)
Standard 1N HCI. Dilute 88 ml of concentrated HCI to 1000 ml standardize it against standard
NaOH.
ii) Standard in NaOH. Solution 1 N; Dissolve 40 gm NaOH to 1000 ml of distilled water and
standardize using methyl red indicator.
iii) Phenolphthalein Indicator: Dissolve 0.5 g of phenolphthalein in 50 ml 95% ethyl alcohol and
50 ml of distilled water.
Procedure:
Weigh 5 g of dry soil accurately and transfer to 250 ml beaker and add 100 ml of 1 N HCI solution.
Cover with a watch glass and stir several times for one hour at interval of 10 minutes. After settling
for 10 minutes, pipette off 20 ml of supernatant liquid and take into a conical flask. Add 6 to 8
drops of phenolphthalein indicator and titrate with 1 N sodium hydroxide solution till the solution
turns pink.
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Calculations:
1 ml of 1N HCI is equivalent to 0.05 gm of CaCO3 present in the soil sample.
Carbonate present in soil percent =
Volume of hydrochloric acid consumed for 5 gm of soil x 0.05 x 100
5
ORGANIC CARBON
Principle
Organic carbon present in the soil is determined by digestion with excess of potassium dichromate
and sulphuric acid and the unutilized potassium dichromate is then titrated with ferrous ammonium
sulphate using diphenylamine as indicator. The used potassium dichromate the difference between
added and residual potassium dichromate gives a, measure of organic carbon content of soil.
The elementary carbon present as graphite, charcoal etc. is not attacked in this method. The
recovery of the carbon in this method is not 100 percent. Only about 60-90 percent of the total
organic carbon is recovered depending upon the kind. For example in most cases, the proteins
remain unaffected by this method.
Reagents
1. Potassium Dichromate Solution 1 N. Dissolve 49.04 gm of K2Cr2O7 in distilled water and
dilute to 1000 ml.
2. Sulphuric Acid concentrated H2SO4 (Sp gravity 1.84)
3. Phosphoric Acid H3PO4 concentrated (Sp gravity 1.71).
4. Ferrous Ammonium Sulphate 0.4 N.
5. Dissolve 156.86 g Fe (NH4)2 (SO4)3 6H2O in distilled water and add 14 ml conc. H2SO4
and dilute to 1000 mi.
6. Diphenylamine Indicator
7. Dissolve 0.5 diphenylamine in a mixture of 20 ml distilled water and 100 ml conc.
sulphuric acid.
8. Sodium Fluoride
Procedure
1. Take oven dried soil sample and pass through 0.2 mm non ferrous screen.
2. Weigh a suitable quantity of soil not exceeding 10 gm (containing about 10-25 mg
carbon) and transfer to a dried 500 ml conical flask.
3. Add 10 ml 1 N K2Cr2O7 solution and 20 ml conc. H2SO4 and mix by gentle swirling.
4. Keep the flask to react the mixture for about 30 minutes.
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5. After the reaction is over, dilute the contents with 200 ml of distilled water and add 10 ml
of phosphoric acid and 0.2 gm sodium fluoride followed by 1 ml of diphenylamine
indicator.
6. Titrate the sample with 0.4 N ferrous ammonium sulphate till the dull green color changes
to brilliant green.
7. Run a blank with same quantity of chemical but without soil.
8. If more than 8 ml of the 10 ml added K2Cr2O7 is consumed (ml titrant less than 5 ml),
repeat with less quantity of the sample.
Calculation
Percent Carbon = 3.939 1 - T
g
S
g = weight of soil sample in gms.
S = ml ferrous ammonium sulphate solution with blank titration.
T = ml of ferrous ammonium sulphate solution with sample titration.
% Organic matter = % C x 1.724
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METHODOLOGY OF WATER
ANALYSIS
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METHODOLOGY OF PHYSIO-CHEMICAL ANALYSIS OF
WATER
pH
For most practical purposes, the pH of aqueous solutions can be taken as negative logarithm of
hydrogen ion activity. pH values from 0 to 7 are disminishingly acidic, 7 to 14 increasingly
alkaline and 7 is neutral.
The pH of nature water usually lies in the range of 4.4 to 8.5. its value is governed largely by the
carbon dioxide / bicarbonate / carbonate equilibrium. It may be affected by humic substances by
changes in the carbonate equilibria due to the bio-activity of plants and in some cases by
hydrolysable salts. The effect of pH on the chemical and biological properties of liquids makes its
determination very important. It is used in several calculations in analytical work and its
adjustment is necessary for some analytical procedures.
The determination of pH by conventional chemical means is not practicable and the equilibria,
which are involved, depend to some extent temperature. The precise accepted scale of pH must
therefore be based on an agreed primarily standard. The colorimetric indicator methods can be used
only if approximate pH values are required. The pH determination is usually done by electrometric
method, which is the most accurate method and free of interferences.
Electrometric Method:
The pH is determined by measurement of the electromotive force of cell comprising an indicator
electrode (an electrode responsive to hydrogen ions such as glass electrode) immersed in the test
solution and a reference electrode (usually a mercury calomel electrode) contract between the test
solution and the reference electrode is usually achieved by means of a liquid junction, which forms
a part of the reference electrode. The emf of this cell is measured with pH meter. This is a high
impedance electrometer calibrated in terms of pH.
Apparatus:
Glass Electrode:
This must be compatible with the pH meter used and must be suitable for the particular application.
Special electrodes are available for pH values greater than 10 and for use at temperature greater
than 600 C. combined glass/reference electrodes are also available and are convenient to use.
Reference Electrode:
The mercury/ calomel electrode is widely used but the silver/ silver chloride electrode may be
preferably on account of it being more reproducible and more reliable. Less concentrated solutions
of KCL (3.5 M KCL or 350 gm/litre) are more satisfactory as filling solutions than the saturated
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solution often used because problems due to logging of the electrode or the liquid junction will be
avoided. To prevent dissolution of the silver chloride film, the potassium chloride filling solution
of Ag/ AgCl electrodes should be saturated with AgCl.
PH Meter:
Both mains and battery operated models are available, the alter type can be used for field
measurements. The most accurate pH meters can be read to better than ± 0.005 pH unit.
Reagents:
1.Buffer solution for pH 4.0: Dissolve 10.12 gm potassium dihydrogen phthalate dried at 1100 C
in freshly distilled water and dilute to one litre at 250C.
2. Buffer solution for pH 6.8: dissolve 3.388 gm anhydrous KH2PO4 and 3.533 gm Na2HPO4 both
of which have been dried overnight at between 1100C and 1300C in water an dilute to 1 litre at
250C. The distilled water should be freshly boiled, cooled and free from CO2.
3. Buffer Solution for pH 9.2: Dissolve 3.80 gm Na2B4O7. 10 H2O in water dilute to 1 litre to
250C.
NOTE: In general analytical reagent grade chemicals are satisfactory for the preparation of these
solutions. Commercial buffer tablets are available in the market for the preparation of solution of
above pH values (Each tablet dissolved in 100 ml gives the buffer solution of required pH).
Procedure:
1. Standardize the pH meter according to the manufacturer’s instructions.
2. Select a standard buffer solution with a pH value close to that of the water to be tested.
3. Set the temperature control to the temperature of the buffer.
4. Set the meter to the pH of the buffer at that temperature.
5. Check the electrode response by measuring a second standard buffer solution of different pH.
6. Wash the electrode thoroughly first with distilled water and then with the sample.
7. Set the temperature control to the temperature of the sample.
8. Immerse electrodes in the sample and record the pH after stabilizing the system.
Note:
Between measurements, the electrodes are kept in distilled water. New or dried out glass electrodes
should prepared for the use by soaking in 0.1 N HCL for 8 hours or according to the maker’s
instructions.
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COLOUR
Out line:
Colour is measured by visual comparison of the sample with colour standard. One
unit of colour is that produced by 1 mg of platinum per litre in the form of
chloroplatinate ion.
Procedure: Prepare standard colour solution of various Hazen units by diluting standard
chloroplatinate solution with distilled water to 50 ml, observe the colour of the
sample by filling a matched nessler cylinder to the 50 ml mark with water and
compare it with standard.
Calculation:
Colour unit = (50 x A)/ B
Where, A = Estimated colour of diluted sample
B = Volume in ml of sample taken for dilution
ODOUR
Out line:
The type of odours present in water & wastewater will vary widely. The types of
odour shall be described by judging the degrees of sweetness, pungency, smokiness
and rottenness of the odour.
Procedure: As soos as possible after collection of sample, fill a bottle half full of sample, insert the
stopper and shake for 2-3 second and then quickly observed the order. The sample
taken observation of odour shall be at room temperature.
TASTE
Procedure: Prepare dilution series, take the 15 ml sample in a 50 ml beaker and pair each sample
with known blank sample and present to each panelist. Ask the panelist to hold water
at 400C in as much quantity as is comfortable to several second and discharg it with
out swallowing.
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TURBIDITY
Outline:
It is based on comparison of the intensity of light scattered by the sample under
defined conditions with the intensity of light scattered by a standard reference
suspension under the sample conditions. The higher the intensity of scattered light,
the higher the turbidity.
Procedure: Shake the sample to disperse the solids wait until air bubbles disappear. Pour sample
into turbidity meter tube and read turbidity directly from the instrument scale, which is calibrated
by standard solution.
TOTAL DISSOLVED SOLIDS (FILTRABLE) SOLIDS
Principle:
A known volume of filterable sample is evaporated and dried in a weighing dish at 105 0 C to
constant weight the increase in weight over the empty dish represent the dissolved solids.
Apparatus:
1. Evaporating dishes, 50, 100ml capacity (Preferably porcelain or silica).
2. Pipettes 25, 50 ml capacity.
3. Water bath and oven.
4. Balance to weigh up to 4th decimal.
Procedure:
The known volume (V) of filtered sample in a previously ignited and weighted basin (W1).
Evaporate to dryness on a steam bath and further dry at 1500 C for one or two hours in an oven.
Cool in desicator and weight (W2). Repeat by further heating for 15 minutes and cooling unit
successive results do not differ by more than about 0.4 mg.
Calculation:
Dissolved solids mg/l =
(W2 – W1) x 1000
V
Where
W2 = Weight of residue and dish
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W1 = Weight of empty and dry dish
V = Weight of sample
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(TSS)TOTAL SUSPENDED SOLIDS
Procedure:
Take well-mixed 100 ml sample and filter through a pre-weighed standard glass
fiber filter paper and the residue retained on the filter is dried to a constant weight
at 103 to 1050C. The increase in weight represents the total suspended solids.
(BOD) BIOCHEMICAL OXYGEN DEMAND
The biochemical oxygen demand test is based on mainly bio assay procedure which
measures the Dissolved oxygen consumed by micro organism while assimilating and
oxidizing the organic matter under aerobic conditions.
Procedure: Take appropriate quantity of water sample in one liter. Volumetric flask and dilute
upto mark with dilution water. Mix well. Rinse BOD bottles with diluted sample and fill up these
bottles with diluted sample. Stopper the bottles immediately after removing the air bubbles.
Determine the dissolve oxygen of one bottle. And keep one set of bottle for 3 days incubation at
270±10C. After three days determine the Dissolve oxygen. Carry out a blank determination along
with each sample.
(COD) CHEMICAL OXYGEN DEMAND
A sample is refluxed is strongly acid solution with a known excess of K2Cr2O7. After digestion, the
remaining unreduced K2Cr2O7 is titrated with ferrous ammonium sulphate to determine the amount
of K2Cr2O7 consumed. And oxidizable organic matter is calculated in terms of oxygen equivalent.
Procedure:
Calculation:
Place 50 ml sample or smaller sample portion diluted to 50ml in a refluxing flask.
Add 1g HgSO4 and very slowly add 5 ml sulphuric acid reagent with mixing to
dissolve HgSO4. Add 25 ml of K2Cr2O7 solution and mix. Attach flask to
condenser and then on cooling water add remaining sulphuric acid reagent (70 ml)
through open end of condenser. Mix reflux mixture, cover open end of condenser
with beaker and reflux for 2 hrs cool and wash down condenser with 50 ml D/W.
Dilute and cool the room temterature. Titrate excess K2Cr2O7 with FAS using 0.1
to 0.15 ml (2-3 drops) ferroin indicator up to reddish brown end point. In the same
manner reflux and titrate a blank with same reagents and a volume of D/W.
COD as mg O2 / L = (A-B) X M X 8000
ml Sample
A= ml FAS used for blank
B= ml FAS used for Sample.
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M= Molarity of FAS
OIL & GREASE
Dissolved and emulsified oil and grease is extracted from water by solvent trichlorotrifluorethane
or petroleum benzene and estimation is made gravimetrically.
Procedure:
Transfer suitable quantity of sample to a separating funnel. Acidify to pH 2 by
adding Conc HCl. Carefully rinse the measuring cylinder with 30 ml solvent and
add the solvent washings to the separating funnel. Shake vigorously for 2 minutes
or gently for 5-10 minutes. Let the layers separate. Drain the solvent layer through
a funnel containing solvent moistened filter paper and Na2SO4 into a clean tared
flask or beaker, wash filter or beaker. Extract two more times with 30 ml solvent
each time. Collect extracts in tared flask or beaker. Wash filter paper with 10-20ml
solvent. Distill off solvent over water bath at 70°C and evaporate of all solvent.
Cool the beaker in a desiccator and weigh.
Calculation:
Oil & Grease mg/l = M x 1000
V
M = Mass in mg of residue
V = Volume in ml of sample taken
HARDNESS
Water hardness is the traditional measure of the capacity of water to react with soap, hard water
requiring a considerable amount of soap to produce lather. Hardness of water is not a specific
constituent but a variable and complex mixture of cations and anions. The principle hardness
causing ions are calcium and magnesium. The degree of hardness of drinking water has been
classified in term of the equivalent CaCO3 concentration as follows:
Soft 0-60 mg/l, Medium 60-120 mg/l, Hard 120-180 mg/l & Very Hard > 180 mg/l
Hardness many also be discussed in term of carbonate (Temporary) & non-carbonate (Permanent)
hardness. Carbonate hardness can be removed or predicated by boiling. This type of hardness is
responsible for the deposition of scale in hot water pipes and kettles. Non-carbonate hardness is
caused by the association of the hardness causing cations with Sulphate, chloride or nitrate. It
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cannot be removed by boiling public acceptability of the degree of hardness may vary considerably
from community to community, depending on local condition.
EDTA TITRIMATRIC METHOD
Principle:
In alkaline condition EDTA reacts with Ca and Mg to form a soluble chelated complex. Ca & Mg
ions develop wine red color with Eriochrom Black T under alkaline condition. When EDTA is
added as a titrant, the Ca & Mg divalent ions get complexed resulting in sharp change from wine
red to blue, which indicates end point of the titration. The pH for this titration has to be maintained
at 10 + 0.1. At a high pH i.e. about 12 Mg ion of color from pink to purple which indicates the end
point of the reaction.
Interferences:
Metal ions do interfere but can be overcome by addition of inhibitors.
Reagents:
1. Buffer Solution:
Dissolve 16.9 gm NH4Cl in NH4OH. Add 1.25 gm magnesium salt of EDTA to obtain sharp
change in indicator and to 250 ml. If magnesium salt of EDTA is unavailable, dissolve 1.179 gm
disodium salt of EDTA (AR grade) and 780 mg MgSO4. 7H2O or 644 mg MgCl2 6H2O in 50 ml
distilled water. Add to above solution of NH4Cl in NH4OH and dilute to 250 ml.
2. Inhibitor:
Dissolve 4.5 gm hydroxylamine hydrochloride in 1000 ml 95% ethyl alcohol or isopropyl alcohol.
3. Erichrom Black T Indicator:
Mix 0.5 gm dye with 100gm. NaCl to prepare dry powder.
4. Murexide Indicator:
Prepare a ground mixture of 200 mg of murexide (ammonium purpurate) with 100gm
NaCl.
of solid
5. Sodium Hydroxide 2 N:
Dissolve 80 gm NaOH and dilute to 1000 ml.
6. Standard EDTA solution 0.01 M:
Dissolve 3.723 gm EDTA sodium salt and dilute to 1000ml. Standardize against standard calcium
solution, 1 ml = 1mg CaCO3.
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7. Standard calcium solution:
Weight accurately 1.0 gm AR grade CaCO3 and transfer to 250 ml conical flask. Place a funnel in
the neck of a flask and add 1+1 HCl till CaCO3 dissolves completely. Add 200 ml distilled water
and boil for 20-30 min. to expel CO2. Cool and add methyl red indicator. Add NH4OH3 N dropwise
till intermediate orange color develops. Dilute 1000 ml to obtain 1 ml = 1 mg CaCO3.
Procedure:
A. Total Hardness:
1. Take 25 or 50 ml mixed in porcelain dish or conical flask.
2. Add 1-2 ml buffer solution followed by 1 ml inhibitor.
3. Add a pinch of Eriochrome Black T and titrate with standard EDTA (0.01 M) till wine red color
changes to blue. Note down the volume of EDTA required. (A)
4. Run a reagent blank. Note down the volume of EDTA…………….(B).
5. Calculate volume of EDTA required by sample, from volume of EDTA required in step 3 & 4.
C = (A-B)
6. Calculate as follows:
Total hardness
As CaCO3 mg/l = CxDx1000
ml sample
Where C = Volume of EDTA required by sample.
D = mg CaCO3 per 1.0 ml. EDTA (0.01m) used as titrant.
B. Calcium Hardness:
1. Take 25 or 50 ml sample in porcelain dish.
2. Add 1 ml NaOH to raise ph to 12.0 and a pinch of murexide indicator.
3. Titrate immediately with EDTA till pink color changes to purple. Note the volume of EDTA
used (A’).
4. Run a reagent blank. Note the ml of EDTA (B’) required and keep it aside to compare end points
of sample titrations.
5. Calculate as follows:
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Calcium hardness as CaCO3 = C x D x 1000
ml sample
Where C’ = Volume of EDTA used by sampled (A’- B’)
D = mg Caco3 per 1.0 ml EDTA (0.01 M) used for titration.
C. Magnesium Hardness as CaCO3 mg/l = total hardness as
CaCO3 mg/l- Ca hardness as CaCO3 mg/l.
D. Alkaline (Carbonate) Hardness and Non Alkaline (Non Carbonate) Hardness.
These types of hardness can be calculated from hardness and alkalinity data as follows:
If total hardness as CaCo3
>
Total alkalinity as Caco3
Then
1. Alkalinity Hardness = Total Alkalinity
2. Non-alkaline hardness = Total hardness- Total alkalinity
If total hardness as CaCO3
<
Total alkalinity as CaCO3
=
Total Hardness
Then,
i)
Alkaline Hardness
ii)
Non-Alkaline Hardness =
Nil
FLUORIDE
Outline:
The Spadns colorimetric method is based on the reaction between fluoride and
zirconium dye lake, Fluoride reacts with dye lake, dissociating a portion of it into
a colorless complex anion and the dye. As the amount of fluoride increases, the
color produced becomes progressing lighter.
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Procedure:
1)
2)
Prepare fluoride standards in the range of 0 to 1.4 mg/l by diluting standards
fluoride solution. Add 10 ml mixed acid zirconyl spadns reagent, mix and
dilute to 50 ml with D/W. Set photometer to zero absorbance with reference
solution and absorbance readings of standards. Plot a curve of mg fluoride absorbance relationship.
Take 25 ml sample or a portion of sample, add 10 ml mixed acid zirconyl spadns
reagent, mix and dilute to 50 ml with D/W and read absorbance at 570 nm. Determine
concentration of fluoride from curve.
Calculation:
mg F/l
=
A .
ml sample
A = µg F from Curve
CHLORIDE
Chloride ion is generally present in natural water. The presence of chloride in natural waters can be
attributed to dissolution of salt deposits, discharges of effluents from chemical industries, irrigation
drainage, contamination from refuge leachates and sea water intrusion in coastal areas. The salty
taste produced by chloride depends on the chemical composition of the water. A concentration of
250 mg/L may be detectable in some waters containing sodium ions. A high chloride content has a
deleterious effect on metallic pipes as structure as well as on agricultural plants.
Principle:
Chloride is determined in a neutral or slightly alkaline solution by titration with standard silver
nitrate using potassium chromate as an indicator. Silver chloride is quantitatively precipitated
before red silver chromate is formed.
Interference: If the sample is too colored or turbid to allow the end point to be readily detected.
This interference may be reduced by alum flocculating followed by filtration prior to the estimation
of chloride.
Reagents:
1. Potassium Chromate Indicator: Dissolve 50 g K2crO4 in distilled water. Add AgNO3 till
definite red precipitate is formed. Allow standing for 12 hrs. filter and dilute to 1000 ml
2. Silver nitrate (0.0141 N): Dissolve 2.395 gm AgNO3 and dilute to 1000 ml standardize against
NaCl, 0.141 N. 1 ml of 0.141 N AgNO3 = 0.5 mg Cl.
3. Sodium Chloride 0.141 N: Dissolve 824.1 mg NaCl (dried at 1400 C) and dilute to 1000 ml. 1
ml = 0.5 mg Cl
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4. Special reagent to remove color and turbidity: Dissolve 125 g A1K (SO4)2, 12 H2O or AINH4
(SO4)2,.12 H2O and dilute to 1000 ml Warm to 600 C and ad 5 ml conc.NH4OH slowely.Allow to
stand for 1 hr. Solution should be free from Cl.
Procedure:
1. Take 100 ml sample and adjust the pH between 7.0 and 8.0
2. Take 50 ml well mixed sample adjusted to pH 7.0 – 8.0 and add 1.0 ml K2CrO4.
3. Titrate with standard AgNo3 solution till AgCrO4 starts precipitating.
4. Standardize AgNO3 against standard NaCl.
5. For better accuracy titrate distilled water (50 ml) in the same way to establish reagent blank.
6. Calculate the follows:
Chloride mg/l = (A-B x N x 35.45 x 1000)
ml sample
Where A = ml AgNO3 required for sample.
B = ml AgNO3 required for sample.
N = Normality of AgNO3 used.
RESIDUAL FREE CHLORINE
Out line:
Residual chlorine reacts under acid conditions with o-tolidine to give a yellow colour
which is matched against standard colours.
Procedure: Use 5 ml neutral ortho-toludine and 5 ml buffer stabilizer reagent with 100ml sample.
Place the neutral ortho-toludine and buffer stabilizer mixture in a beaker on a
magnetic stirrer. Mix and add sample to the reagents with gentle stirring, Measure
the absorbance at 625 nm.
Calculation: (OD x GF x 1000)/ Sample taken = Residual free chlorine, mg/l
IRON
Being the fourth most abundant element by weight in the earth's crust, it occurs mainly in the
divalent and trivalent state in water. The presence of iron in natural water can be attributed to the
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dissolution of rocks and minerals, acid mines drainage, landfill leachates, sewage and engineering
industries. The presence of iron in drinking water supplies is objectionable for a number of reasons.
Under pH condition existing in drinking water supply. ferrous sulphate is unstable and precipitate
as insoluble ferric hydroxide which settles out as a rust colored silt. Such water often tastes
unpalatable even at low concentration (0.3 mg/L) and stains laundry and plumbing fixtures. Iron
also promotes the growth of 'Iron bacteria'. These microorganisms serive their energy from the
oxidation of ferrous to ferric and in the process deposit a slimy coating on the piping.
Principle:
The ferric form of iron is reduced to ferrous form by boiling with hydrochloric acid and
hydroxylamine hydrochloride. Upon adding 1, 10 phenanthroline (between pH 3.3 and 3.3) form a
soluble chelated complex of orange red color. Intensity of the color is directly proportional to
concentration of iron present in the sample.
Interference:
Strong oxidizing agents such as CN, KO2, polyphosphates, Cr, Zn in conc. exceeding 10 times the
Fe conc. Co and Cu if 5 mg/L Ni if 2 mg/L color and organic matter.
constitutes sources of interference in the development of color. Boiling with HCI and addition of
hydroxylamine -hydrochloride remove interference due to CN, PO4 and other oxidizing agents. The
metal ions get complexed with phenanthroline.
Apparatus:
1) HCl conc.
2) Hydroxylamine HCl solution -Dissolve 10 gm NH2OH. HCl in 100 ml distilled water.
3) Ammonium acetate buffer: Dissolve 250 gm ammonium acetate in 150 ml distilled water. Add
700 ml conc. glacial acetic acid. Final volume will be slightly more than 1000 ml.
4) Phenanthroline solution: Dissolve 100 mg 1, 10 -phenanthroline monohydrate = in 100 ml
distilled water. Warm slightly or add 2 drops conc. HCl if necessary. 1 ml of this solution can
chelate 100 mg iron.
5) Stock iron solution: Add 20 ml conc. H2SO4 to 50 ml distilled water and dissolve -1.404 gm Fe
(NH4) (504) 2.6H2O add dropwise 0.1N KMnO4 till faint pink color persists. Dilute to 100 ml.,
1 ml. = 200 g Fe
Procedure:
1. Take suitable aliquot about 50 ml (having 2 mg/L Fe) of well-mixed sampled in 125 ml conical
flask.
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2. Add 2 ml conc. HCl followed by 1 ml Hydroxylamine -hydrochloride solution.
3. Add 2-3 glass beads and boil for 20-25 min. to ensure dissolution of Fe.
4. Cool to room temp. and transfer to nessler's tube.
5. Add 10ml ammonium acetate buffer and 2 m11, 10-phenanthroline solutions.
6. Dilute to 100 ml and mix well.
7. Prepare blank by substituting the sample by distilled water.
8. For soluble iron determination, take known volume of filtered sample, acidify by adding 2 ml
conc. HCl per 100 ml of sample and treat form step 5 onwards for color developing.
9. Prepare calibration curve taking standard iron solution in the same way in the range, 1 000-4000
g /L with 1 cm light path.
10. Measure the developed color after 10 min. at 510 nm.
11. Calculate the conc. 0 total or soluble Fe present in the sample form calibration curve and
express as mg/L.
TOTAL COLIFORMS
The coliform group consists of several genera of bacteria belonging to the family of
Enterobacteriaceae. This group is defined as all facultative anaerobic, gram (-), nor-spore forming
rod shaped bacteria, lactose fermenting with acid and gas within 48 hrs. at 370C.
“When multiple tubes are used in the fermentation technique results at the examination of replicate
tubes and dilutions are reported in the term of the Most Probable Number (MPN) of organisms
present”.
Procedure:
(a) Presumptive testi) Inculate a 5 tube series having 10 ml. Mac’Conkey broth double strength and 10 tube
having 10 ml Macconkey broth single strength and Durham’s tubes by adding water
sample 10 ml. in 5 tubes of double strength, and 1 ml. & 0.1 ml in each 5 tube of single
strength respectively.
ii) Incubate all the tubes at 370C for 24-48 hrs.
iii) Examine each tube after the end of the incubation period for acid and gas formation.
iv) Production of gas within 48 hrs in the inner fermentation tubes constitutes a positive
presumptive test and absence of gas shows negative test.
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(b) Confirmatory testi) Transfer a loopful of suspension by the all-primary fermentation tubes showing acid
and gas to a 10-ml. tube of BGB broth containing Durham’s tube.
ii) Incubate the tubes at 370C for 48 hrs.
iii) Formation of acid and gas in Durham’s tube shows positive test.
(c) Completed testi) Positive BGB tubes streak with the help of a loop on Mac’ Conkey Agar plate.
ii) Incubate all the tubes at 37 for 24 hrs.
iii) Typical pink, pale yellow color colonies show positive results that will ferment the
lactose broth.
iv) Gram Staining – Gram negative bacilli.
Computing and Recording
Number of the Coliform can be obtained by using MPN table.
E-Coli
E-Coli is gram (-), aerobic, facultative anaerobic, rod shaped, lactose, fermenting and belongs to
Enterobacterioaceae family. It is a member of indigenous fecal flora of warm blooded animals. Its
occurrence is considered a specific indicator of fecal contamination and possible presence of
enteric pathogen.
Media:
1) Mac’ Conkey Broth
2) Mac’ Conkey Agar
3) Peptone Water
4) BGB Broth
5) Kovac’s Reagent
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Procedure:
1. Submit all the presumptive fermentation tubes from Coliform tests showing growth, gas or
acidity within 48 + 3 hours.
2. Sub culture from all the positive Mac Conkey Broth tube on to BGB Broth tubes and
incubate at 44.5 0C for 48 hours.
3. Sub culture from all the positive tubes of BGB Broth into tubes of peptone water.
4. Incubate at 44.5 0C for 48 hours.
5. At the end of incubation period test for indole production by adding a few drops of
Kovac’s reagent.
Results:
Positive tubes will give pink color or reddish ring while negative tubes will give yellow color rings
with Kovac’s reagent.
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