STANDARD TESTING AND

OPERATING PROCEDURE FOR

ENVIRONMENTAL MONITORING
(STOP/04)

By: Kushal Sharma

Copy No. : 01 Controlled / Uncontrolled

Issue No. : 01 Date :
Holder Name : HOD
Issued by : Technical Manager
Doc. No.: JMELPL/STOP/04 Doc. Name: STANDARD TESTING AND OPERATING PROCEDURE
Procedure No.: 1.0 Title: RELEASE AUTHORIZATION

ONLY FOR
LABOURATORY USED

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Procedure No.: 2.0 Title: DISTRIBUTION LIST

DISTRIBUTION LIST
The following are the authorized holders of controlled copy of STANDARD TESTING AND OPERATING
PROCEDURE: -

Controlled copy No. Designation of the holder of controlled copy

1. HOD

2. Quality Manager

3. Technical Manager

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Procedure No.: 3.0 Title: AMENDMENT RECORD

AMENDMENT RECORD
Amendments are recorded in the amendment record sheet as below.
S. Page Title/ Clause/ Date of Amendment Reasons of Signature of Quality
No No. Para/ line Amend made Amendment Manager
. (as applicable)

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Procedure No.: 4.0 Title: CONTENTS

CONTENTS
Procedure No. Contents Revision Page No.
No. Date
1.0 RELEASE AUTHORIZATION 00 00 2
2.0 DISTRIBUTION LIST 00 00 3
3.0 AMENDMENT RECORD 00 00 4
4.0 CONTENTS 00 00 5
STOP-01 MONITORING/SAMPLING OF AMBIENT AIR 00 00 6-12
STOP -02 METEOROLOGICAL PARAMETERS 00 00 13
STOP -03 NOISE MONITORING 00 00 14-15
STOP -04 SOIL SAMPLING 00 00 16-17
STOP -05 SOURCE EMISSION MONITORING 00 00 18-24
STOP -06 SAMPLING OF WATER AND WASTE WATER 00 00 25-29

Amend. No.:
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Procedure No.: STOP-01 Title: MONITORING/SAMPLING OF AMBIENT AIR

MONITORING/SAMPLING OF AMBIENT AIR

1. Purpose: Provide guidelines for monitoring and sampling of Ambient Air.
2. Selection of Monitoring Station:
In general the following requirement may be met for sitting the monitoring station.
(i) Height of the inlet must be 3 – 10 m above the ground level.
(ii)The sampler must be more than 20 m from trees.
(iii) Distance of the sampler to any air flow obstacle i.e. buildings, must be more than two times the height
of the obstacle above the sampler.
(iv) There should be unrestricted airflow in three of four quadrants
(v) There should be no nearby furnace or incinerator fumes.
3. Reagents/Chemicals/Filters:
Filter Media for PM10–
A Glass fibre filter of 20.3 X 25.4 cm (8 X 10 in) size
Filter Media for PM2.5–
A PTFE Filter Paper of 47 mm size with pore size of 2 micron.
Absorbing Reagent For SO2, 0.04 M Tetrachloro mercurate (TCM) –Dissolve 10.86 g, mercuric
chloride, 0.066 g EDTA, and 6.0 g potassium chloride or 4.68 gm sodium chloride in water and bring to the
mark in a 1 litre volumetric flask.
Caution: highly poisonous if spilled on skin, flush off with water immediately.
Absorbing Reagent for NO2, –Dissolve 4.0 g of sodium hydroxide in distilled water, add 1.0 g of sodium
Arsenite, and dilute to 1,000 ml with distilled water.
Absorption media for Benzene, Activated Charcoal tube with cap
Absorbing Solution for Ozone (1% KI in 0.1 m Phosphate Buffer): Dissolve 13.6 g of potassium
dihydrogen phosphate (KH2PO4), 14.2 g of disodium hydrogen phosphate (Na 2HPO4) or 35.8 g of the
dodecahydrate salt (Na2HPO2. 12 H2O), and 10.0 g of potassium iodide in sequence and dilute the mixture to
1 L with water. Keep at room temperature for at least 1 day before use. Measure pH and adjust to 6.8 + 0.2
with NaOH or KH2PO4. It should not be exposed to direct sunlight.

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Procedure No.: STOP-01 Title: MONITORING/SAMPLING OF AMBIENT AIR

Filter media for Heavy Metals (As, Ni, Pb):

EPM 2000 or equivalent, 20.3 X 25.4 cm (8 X 10 in)
Absorbing Solution for Ammonia (0.1 N Sulphuric acid):
Dilute 3.0 ml of concentrated H 2 SO 4 ( 1 8 M ) t o 1 L with water to obtain 0.1 H 2 SO 4
Absorbing Solution for Free Chlorine:
Methyl Orange solution (0.005%): Pipette 10 ml of methyl orange solution (0.05 %) and dilute to 100 ml
with distill water. Prepare fresh for use.
Sampling Solution: Pipette 6 ml of 0.005 % methyl orange solution and dilute to 100 ml with distill water.
Add 3 drops of 5.0 N HCl in this solution, and one drop of butanol to increase collection efficiency.
Absorbing Solution for Fluoride (0.1 N NaOH):
Dissolve 4.0 g of sodium hydroxide in distilled water, and dilute to 1,000 ml with distilled water.
4. Sampling Procedures:-
a. Sampling Procedure of Suspended particulate matter:
Tilt back the inlet and secure it according to manufacturer's instructions. Loosen the faceplate wing nuts and
remove the faceplate. Remove the filter from its jacket and centre it on the support screen with the rough
side of the filter facing upwards. Replace the faceplate and tighten the wing nuts to secure the rubber gasket
against the filter edge.
Gently lower the inlet. For automatically flow-controlled units, record the designated flow rate on the data
sheet. Record the reading of the elapsed time meter. The specified length of sampling is commonly 8 hours
or 24 hours. During this period several reading (hourly) of flow rate should be taken, After the required time
of sampling, record the flow meter reading, take out the filter media from the sampler, and put in a container
or envelope.
Inspect the filter for pin holes using a light table. Loose particles should be removed with a soft brush.
Apply the filter identification number . Condition the filter in conditioning room maintained within 20-30° C
and 40-50% relative humidity or in an airtight desiccator for 24 hours. Take initial weight of the filter paper
(Wi) before sampling. Condition the filter after sampling in conditioning room maintained within 20-30° C
and 40-50% relative humidity or in an airtight desiccator for 24 hours. Take final weight of the filter paper
(Wf)

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Procedure No.: STOP-01 Title: MONITORING/SAMPLING OF AMBIENT AIR
b. Sampling of particulate matter PM10
Tilt back the inlet and secure it according to manufacturer's instructions. Loosen the faceplate wing nuts and
remove the faceplate. Remove the filter from its jacket and centre it on the support screen with the rough
side of the filter facing upwards. Replace the faceplate and tighten the wing nuts to secure the rubber gasket
against the filter edge.
Gently lower the inlet. For automatically flow-controlled units, record the designated flow rate on the data
sheet. Record the reading of the elapsed time meter. The specified length of sampling is commonly 8 hours
or 24 hours. During this period several reading (hourly) of flow rate should be taken, after the required time
of sampling, record the flow meter reading, take out the filter media from the sampler, and put in a container
or envelope.
Conditioning and inspection of Filter paper
Inspect the filter for pin holes using a light table. Loose particles should be removed with a soft brush.
Apply the filter identification number or a code to the filter if it is not a numbered. Condition the filter in
conditioning room maintained within 20-30° C and 40-50% relative humidity or in an airtight desiccator for
24 hours. Take initial weight of the filter paper (Wi) before sampling. Condition the filter after sampling in
conditioning room maintained within 20-30° C and 40-50% relative humidity or in an airtight desiccator for
24 hours. Take final weight of the filter paper (Wf).
C. Sampling procedure of particulate matter PM2.5
Fine Particulate Sampler with size selective inlet for PM2.5 and Automatic volumetric flow control.
Calibrated flow-measuring device to control the airflow at 16.67 l/min.
On the Field Data Log, fill in the top portion of the form including: the date/time of visit, the site
identification, sampler identification, site name, filter ID number, sample start and stop dates and times, and
field operator initials. Perform all necessary pre-sampling procedures as described above. Record all
maintenance activities in the field log book; include time, date, and any concerns that might affect the
quality of the sample. Remove the filter to be installed from its protective filter cassette carrier. Fix the filter
following manufacturer’s instructions into place against the bottom of the WINS impactor. Check the
system clock and make sure it is within 1 min of NIST time. Strictly follow operator’s manual for setting up
the sampling programme (24 hours).

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Procedure No.: STOP-01 Title: MONITORING/SAMPLING OF AMBIENT AIR
The Filter Setup Screen shows the start date and time and the end date and time for the next sample. To
change the sampling parameters follow the operator’s manual Start Sampling run wait until the auto
diagnosis for all relevant parameters finishes and the sampler automatically switch over to SAMPLING
mode. Check flow (16.67 lpm) and Sample volume displays rightly on screen.
Take out pre-conditioned filters by forceps one by one and weigh Properly. Record the mass in data sheet
and log books against Respective filter numbers or code. Always use gloved hands and blunt tweezers to
handle filters. Replace and close the filter container (Petri dishes). Weigh one Control Filters (Archived
one) with each batch of ten weighing.
Keep separate controls for Pre (Blank filter) and Post (Exposed) sampling filters. Put the values of all
control measurement in Quality Control Charts against dates. Put Lab code on from Plastic petri-slide filter
containers (Filter Cassette). Take out conditioned filter from Plastic petri-slide filter containers (Filter
Cassette). Weigh the preconditioned filter.
Record and store it in laboratory coded filter cassette. Follow the same procedure for exposed filter Place
the weighed filter into a Petri-slide, close tightly.
d. Sampling procedure of Sulphur Dioxide (SO2)
The pH of this reagent should be approximately 4.0 but, it has been shown that there is no appreciable
difference in collection efficiency over the range of pH- 5 to pH- 3. The absorbing reagent is normally
stable for six months. If, a precipitate forms, discard the reagent after recovering the mercury.
Place 30 ml of absorbing solution in an Absorber and sample for 8 to 24 hours at the flow rate of 0.5 L/min.
After sampling measure the volume of sample and transfer to a sample storage bottle.
e. Sampling procedure of Nitrogen Dioxide (NOx)
Place 30 ml of absorbing solution in an Absorber and sample for 8 to 24 hours at the flow rate of 0.5 L/min.
After sampling measure the volume of sample and transfer to a sample storage bottle.
f. Sampling procedure of Carbon Monoxide, Methane and Non- Methane Hydrocarbons:
Sample is collected in Tedlar Beg with a constant flow rate of 1 to 2 LPM for 1 liter of sample volume.
g. Sampling procedure of Benzene, Toluene and Xylene (BTX):
Collect air sample in glass sampling tube filled with a activated charcoal (coconut shell). Sampling flow
rate in the range of 20-100 ml/min is required (+2%) for ambient air.
After sampling sealed the tube with caps, and sent to a laboratory for analysis.
(Note: Activated charcoal tube should be sealed before and after sampling)

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 Procedure No.: STOP-01 Title: MONITORING/SAMPLING OF AMBIENT AIR

h. Sampling procedure of Heavy Metals (Pb, As, Ni)

Tilt back the inlet and secure it according to manufacturer's instructions. Loosen the face-plate wing-nuts
and remove the face plate. Remove the filter from its jacket and centre it on the support screen with the
rough side of the filter facing upwards. Replace the face-plate and tighten the wing-nuts to secure the rubber
gasket against the filter edge. Gently lower the inlet. For automatically flow-controlled units, record the
designated flow rate on the data sheet. Record the reading of the elapsed time meter. The specified length
of sampling is commonly 8 hours or 24 hours. During this period, several reading (hourly) of flow rate
should be taken. After the required time of sampling, record the flow meter reading and take out the filter
media from the sampler and put in a container or envelope.
i. Sampling procedure of Benzo (a) pyrine
Tilt back the inlet and secure it according to manufacturer's instructions. Loosen the face-plate wing-nuts
and remove the face plate. Remove the filter from its jacket and centre it on the support screen with the
rough side of the filter facing upwards. Replace the face-plate and tighten the wing-nuts to secure the rubber
gasket against the filter edge. Gently lower the inlet. For automatically flow-controlled units, record the
designated flow rate on the data sheet. Record the reading of the elapsed time meter. The specified length
of sampling is commonly 8 hours or 24 hours. During this period, several reading (hourly) of flow rate
should be taken. After the required time of sampling, record the flow meter reading and take out the filter
media from the sampler and put in a container or envelope.
j. Sampling procedure of Ozone:
Place 10 ml of absorbing solution in a standard impinger and sample for one hour at the flow rate of 1
L/min. Do not expose the absorbing reagent to direct sunlight. After sampling measure the volume of sample
and transfer to a sample storage bottle.
k. Sampling procedure of Fluoride:
Place 30 ml of (0.1 N NaOH) absorbing solution in a standard impinger and sample for 8 hour at the flow
rate of 1 L/min. Do not expose the absorbing reagent to direct sunlight. After sampling measure the volume
of sample and transfer to a sample storage bottle.
l. Sampling procedure of Ammonia:
Place 10 ml of absorbing solution in a standard impinger and sample for one hour at the flow rate of 1
L/min. Do not expose the absorbing reagent to direct sunlight. After sampling measure the volume of sample
and transfer to a sample storage bottle.

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Procedure No.: STOP-01 Title: MONITORING/SAMPLING OF AMBIENT AIR
m. Sampling procedure of Free Chlorine:
Place 100 ml of absorbing solution in a impinger for 1 – 4 hour at the flow rate of 1 L/min. Do not expose
the absorbing reagent to direct sunlight. After sampling measure the volume of sample and transfer to a
sample storage bottle.

FLOW CHART FOR SAMPLING OF AMBIENT AIR

Select the location as per physical requirement and representative site.

Place the RDS, FPS HVS and OVS at 3-10 m height and distance as per requirement.

Place the 8*10 PM10 filter for in RDS

Place PTFE 47 mm PM2.5 filter in FPS

Place 30 ml of 0.1 N NaOH absorbing solution for NO2 in gases attachment of RDS

Place 30 ml of 0.04 M TCM absorbing solution for SO2 in gases attachment of RDS

Place 10 ml of 1 % KI absorbing solution for O3 in RDS or gases attachment at flow rate of 1.0 lpm

Place 10 ml of 0.1N H2SO4 absorbing solution for NH3 in RDS or gases attachment at flow rate of 1.0
lpm

Place the EPM 2000 filter for metals in HVS

Connect Activated charcoal tube with OVS.

Connect the low flow rate vacuum pump with Tedlar bag for CO at the flow rate of 1 LPM for 1 liter of
sample volume

Start the sampler and Note down the flow rate, manometer reading before the starting the monitoring.

Note down the flow rate with interval of time.

After the monitoring note down the final reading and collect the filter media in filter cassette and
absorbing solution in PVC sampling bottle.

Preserve the absorbing solution with ice or dry ice

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 Procedure No.: STOP-01 Title: MONITORING/SAMPLING OF AMBIENT AIR

5. PRECAUTIONS:-

i. Site should be representative and available for long time.

ii. Site should be selected on the basis of Source emissions data, demographic information and
meteorological parameters
iii. Site Should be away from source & other interferences (Inlet 15 meter away from source\ traffic
artery)
iv. Site Should be at Height of inlet >3 Meter (Preferably 3-10mtr)
v. Site Should be at double the height of nearby wall/obstructed
vi. Site Should be Free flowing & well mixed
vii. Site Should be at Elevation angle <30(inlet to top of building)
viii. Site for Collected sampler should be 20 mtr apart
ix. Site of sampler must be more than 20m from trees.
x. Site should be in such that these in to obstacle air flow i.e. building, must be more than two times the
height of the obstacle above the sampler
xi. Site Should be unrestricted air flow in three of four quadrants
xii. Site should be away from furnace or incinerator fumes.
xiii. Flow rate should be in between 0.9-1.4 m3/min(free flow condition without filter)
xiv. Check Leakage of the Sampler before use.
xv. Uses Recommended filter paper Whatman GF/A for better result
xvi. Use preconditioned filter paper.
xvii. Hourly flow rate should be recorded.
xviii. Ensure Power requirements for instrument operation i.e. nominal 220 V, single phase,50-Hz AC
mains Supply
xix. Use of PPE during Monitoring viz. Hand Gloves, Safety goggles, Safety jackets, Safety shoes, safety
helmet and Safety Belt

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Procedure No.: STOP-02 Title: MONITORING OF METEOROLOGICAL PARAMETERS
Standard Operating Procedure for Meteorological Parameters
1. Purpose
This SOP is applicable for the sampling and determination of Wind Direction, Wind Velocity, Temperature,
Relative Humidity and Rain Fall..
2. Principle
Through real time electronic monitoring, storing of met. Parameter with time weighted Digital display.
3. Instrument/Equipment
Wind Monitor 271
4. Procedure
Connect and assemble the entire sensor with data logger and as per instruction manual WM 271. The sensors
get connected with data logger from a bottom and are mounted on a rooftop. A logger can be kept on a table
on its stand or mounted on a wall/pole. The battery charger should be Connected to the instrument and left to
fully charge the NiMH battery. Once the battery is charged, the instrument can work without mains supply
for approximately 20 hours. A GSM modem is connected to the instrument, by mounting it on instrument’s
left side wall. The power supply to the modem can be provided by a wind monitor’s in built battery through
a power cord. The LCD on the instrument shows instantaneous sensor values and one can scroll through
using the Cursor keys available on the keypad. It should be noted all the sensors are analog sensors, expect
the rainfall and the wind speed sensor which are digital.
After all the sensors get connected then ON the instrument via data logger, to ON the instrument press ON
key and hold key for couple of seconds till a welcome message “Envirotech WM 271” appears on the
Screen. Up & Down Keys : these keys is used to scroll through different sensor values captured by the data
Logger. Note that one needs to press and hold the arrow key for 1 second to scroll to the next value.
The order in which instantaneous sensor values will be displayed in LCD is as follows:
a. Wind Direction
b. Temperature
c. Relative Humidity
d. solar
e. Barometric Pressure
f. Wind Speed
g. Rain fall

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 Procedure No.: STOP-03 Title: NOISE MONITORING

1. Purpose
To provide guidelines for Ambient Noise Monitoring and Source specific noise.
2. Principle
Determine the sound pressure Level by using noise meter and calculate Continuous equivalent sound
Pressure level (Leq) in dB (A).
3. Instrument/Equipment
Noise Meter
4. Procedure for Ambient Noise
Select the location as per Ambient Noise standards or requirements and place the instrument with
minimum of 1 meter height to known the actual sound pressure on human hearing and Switch ON
the instrument. Determine proper measuring range by selecting the range to minimize the tolerance
of readout. Note down the reading in dB (A) with the interval of 6 minutes or minimum 10 values in
an hours and for the ambient noise monitoring should be done for 24 hours.
Situate the instrument minimum 1.0 meter from the source and Switch ON the instrument and wait
for few seconds and then note down the reading which in display on Noise meter in dB (A) with the
interval of 6 minutes and collect minimum 10 values in hour for accurate results
5. Procedure for Source Specific or point source Noise
Situate the instrument minimum 1.0 meter from the source and Switch ON the instrument and wait
for few seconds and then note down the reading in field data sheet which is display on Noise meter
in dB (A) with the interval of 1 minute and collect maximum values in 30 minutes for accurate
results
6. Calculation
Calculate the Continuous equivalent sound Pressure level (Leq) by using the following Formula:
n

Leq dB (A) = 10 log [1/n ∑i=1 (10L/10)

L10 = Percentile (reading, x 0.9)
L50 = Percentile (reading, x 0.5)
L90 = Percentile (reading, x 0.1)
LDay = Avg. Leq values of day time
LNight = Avg. Leq values of day time
Ldn =10*Log (16/24*10Lday/10+8/24*10(Lnight+10/10))

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Procedure No.: STOP-03 Title: NOISE MONITORING

Precautions:-

a. Representative site should be selected for noise monitoring.

b. The Sampler should be proper height (5feet from ground level and 1 meter from walls etc.)
c. Site should be away from trees to know the exact level of noise
d. For Source Monitoring minimum 5 meter distance should be kept.
e. Sound Level should be calibrated.
f. During point source noise monitoring ear plug should be wear.
g. For the actual Noise monitoring of source other sources should be Off
h. Weighting Frequency should be ‘A’ for Human hearing Ambient noise monitoring

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Procedure No.: STOP-04 Title: SAMPLING OF SOIL

1. Purpose:-
To provide guidelines for collection of representative soil sample.
2. Principle of the method:-
3. Grab Sampling:-
Collect the sample from a particular location at a distinct point in time. Before Soil Sampling we
have removed 10 cm surface litter & vegetation covered in sampling area than taken soil samples
with the help of Auger tool of a 15-30 cm depth Collect in 2 kg Polythene bag.
4. Composite Sampling:-
a. Random Sampling
Sample represents nos. more than 10-15 cores composited to produce one sample Collected in a
zigzag pattern across the field.
b. Grid Sampling
Field is divided into equal areas generally 300’ x 300’ (2 a) 10 cores (min.) composited within each
grid cell in a 10’ radius around a georeferenced point.
c. Zone Sampling
Divides field into areas that are < 10-15 a 20 cores composited to produce 1 sample/zone collected in
a zig-zag pattern across the zone, Zone borders & sampling points can be georeferenced.
5. Instrument/Equipment
Buckets
Probes
Augers
6. Procedure
Collection of samples from near-surface soil can be accomplished with tools such as spades,
shovels, trowels, and scoops. Surface material is removed and collect the sample from 15-30 cm of
depth with a stainless steel or plastic scoop or auger. This method can be used in most soil types but
is limited to sampling at or near the ground surface. Accurate, representative samples can be
collected with this procedure depending on the care and precision demonstrated by the sample team
member. If volatile organic analysis is to be performed, transfer the sample directly into an
appropriate, labeled sample container with a stainless steel lab spoon, or equivalent and secure the
cap tightly. Place the remainder of the sample into a stainless steel, plastic, or other appropriate
homogenization container, and mix thoroughly to obtain a homogenous sample representative of the
entire sampling interval.

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Procedure No.: STOP-04 Title: SAMPLING OF SOIL
Then, either place the sample into appropriate, labeled containers and secure the caps tightly; or, if
composite samples are to be collected, place a sample from another sampling interval or location into
the homogenization container and mix thoroughly.
7. Quartering & Coning
Thoroughly mix the soil sample and spread the sample into a conical pile.
Further mix the soil by circumventing the cone symmetrically, repeatedly taking a spatula-full of soil
from the base and transferring the soil to the apex of the cone.
Ensure the spatula is large enough to reach to centre of the cone. Circumvent the cone twice.
Flatten the cone to a height of about 1 cm.
Use a flat spatula or ruler; divide the pile into quarters along two lines intersecting 90° to each other.
Select one pair of opposite quarters as the sample to be retained.
If the sample is still too large then repeat the procedure from the beginning.
After Coning and Quartering collect the sample in a PTFE sampling begs with proper identification.
8. Precautions

a. Representative site should be selected.

b. For the study of nutrients circulation in various ecosystem in rooting depth (10-15 cm)
c. The area is usually inspected and if Considerable differences in color, texture, elevation act
d. Each 5m or 10m interval soil sample taken for analysis
e. As a precautionary measure, uniform portion is to be taken from surface to their desired depth and
secondly, same volume of soil volume to be taken from each location of same depth.
f. Collect the soil sample in a polyethylene bag with proper seal & ID No.
g. Sampling type of soil is composite
h. Protocol used for IS-2720, IS-14684, USDA and APHA methods.
i. Use of durring ppe at monitoring
Hand Gloves, Safty gogles, Safty jackets, Safty shoes, Safty helmet, Ear plug

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Procedure No.: STOP-05 Title: MONITORING/SAMPLING OF SOURCE EMISSION

1. Purpose:
To provide guidelines for monitoring of Source Emissions for Particulate Matter and Gases.
2. Principle of the method:-
To collect a known volume of air at the constant flow rate for particulate matter by using a specify
glass Fiber/cellulose/Silica thimble and to trap gases in specific absorbing solutions.
3. Instrument/Equipment:-
Stack Sampler
Analytical balance
NOx Assembly Flask
Vacuum Pump
Capable of maintaining an air pressure differential greater than 3 to 30 LPM atmosphere at the
desired flow rate.
Pre -Calibrated flow-measuring device to ensure airflow from 0.2 to 1l/min.
Absorber
All glass midget impinger with specific absorbing solutions.
4. Reagents/Thimbles/Requirements:-
Thimbles for particulate matter:-
Glass Fiber/Cellulose/Silica thimble
Silica Gel
Distilled Water
Absorbing Solutions for SO2:
Iso- Propanol (80 % by Volume):-
Mix 80 ml of Iso Propanol with 20 ml of distilled water.
Hydrogen Peroxide (3 %):-
Add 10 ml of 30 % hydrogen peroxide and make up to 100 ml with distill water. Prepare Fresh daily.
Absorbing Solution for NOx:-
Cautiously add 2.8 ml concentrated H 2SO4 to a 1-liter flask partially filled with water. Mix well, and
add 6 ml of 3 percent hydrogen peroxide, freshly prepared from 30 percent hydrogen peroxide.
Absorbing Solution for Fluoride (0.1 N NaOH):
Dissolve 4.0 g of sodium hydroxide in distilled water, and dilute to 1,000 ml with distilled water.

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 Procedure No.: STOP-05 Title: MONITORING/SAMPLING OF SOURCE EMISSION

Absorbing Media for Carbon Monoxide, Methane and Non- Methane Hydrocarbons:
Tedlar Beg with a constant low flow sampler.

Absorbing Solution for Hydrogen Sulphide (0.1 N NaOH):-

Dissolve 10 gm of cadmium chloride in 450 ml of distill water to which 10 ml of 0.5 N NaOH is
added.
Absorbing Solution for Carbon Disulphide (0.1 N NaOH):-
Dissolve 5 gm of KOH in 2-3 ml of distill water and make up to 100 ml with ethyl alcohol.
Absorbing Solution for Ammonia (0.1 N H2SO4):-
Dilute 2.8 ml of concentrated H2SO4 (18M) to 1oo ml with distill water.
5. Procedure:-

Minimum required number of traverse points for sampling sites which meet specified criteria
S. Diameter of stack No. of Traverse points
No.
1. I.D. ≤ 0.3 4
2. 0.3 ≤ I.D. ≤0 .6 8
3. 0.6 ≤ I.D. ≤ 1.2 12
4. 1.2 ≤ I.D. ≤ 2.4 20
5. 2.4 ≤ I.D. ≤ 5 32
Stack gas velocity determination:-
For velocity determination, connect thermocouple to the stack monitoring kit and wait for
stabilization and note down the temperature in different points as per traverse point selection and
then connect Pitot tube to the stack and dynamic and a static pressure are measured by using the
manometer. The velocity of gas in the duct and the air quantity are determined using the following
formula.
Preliminary determination
Preliminary determination requires for the parameters like Temperature (Stack & ambient
temperature OC), velocity pressure Head ΔP, Ambient Barometric pressure, Static pressure as
mentioned as above
V = C √ (ΔP × Ts)

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Procedure No.: STOP-05 Title: MONITORING/SAMPLING OF SOURCE EMISSION

Where
V = Stack gas velocity, m/s
C = Combined pitot tube coefficient.
Ts = absolute stack gas temperature, °K
Δ P = Stack gas velocity pressure, mm water column
After the velocity determination calculate the Iso-kinetic flow rate by using the following Formula:
= (V×An×60×1000) × (Ta/Ts)
Where
An = Area of Nozzle in m2
Ta = Ambient Temperature in ̊ K
Ts = Stack Temperature in ̊ K
Stack gas volumetric flow Rate:
The following equation is used to calculate the stack gas volumetric flow rate,
Qs (m3/hr).
Qs = 3600 (V) × As × [Tref* Ps/ Pref* Ts]
As = Area of the stack (duct), m2
Tref = 298 °K
Pref = 760 mmHg
Ts = Absolute stack gas temperature, °K
Ps = Absolute stack gas pressure, mmHg

Sampling Procedure for Particulate Matter:-

After the calculation of iso-kinetic flow rate place the preweighted glass fiber/silica/cellulose thimble
as per desired temperature into the thimble holder and and insert the probe in to first sampling
traverse point and and start the flow pump and monitor at different- different traverse point at per
internal dia of the stack and collect the gas sampled about 1 m3. After the monitoring kept the
thimble in thimble container.

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Procedure No.: STOP-05 Title: MONITORING/SAMPLING OF SOURCE EMISSION

Sampling Procedure for Sulphur Dioxide:-

For the sampling of SO2 Pour 15 ml of 80% Iso-Propanol into the impinger and 15 ml of 3% of
Hydrogen peroxide into each of the first two Impingers. Leave the final impinger dry and assemble
the sampling train as shown in figure. Check the leakage in sampling train and leakage rate not to
exceed to 1 percent of sampling rate.
After the setting of sampling train adjust the sampling flow rate in the range of 1 to 2 LPM, and start
the sampling. After the sampling turn off the pump and disconnect the Impingers.
Transfer the sample into a polyethylene shipment bottle with proper labeling.
Sample Collection Procedure for NO2:-
Flask Volume. The volume of the collection flask and flask valve combination must be known prior
to sampling. Assemble the flask and flask valve, and fill with water to the stopcock. Measure the
volume of water to ± 10 ml. Record this volume on the flask. Pipette 25 ml of absorbing solution into
a sample flask, retaining a sufficient quantity for use in preparing the calibration standards. Insert the
flask valve stopper into the flask with the valve in the "purge"
position. place the probe at the sampling point. Make sure that all fittings are tight and leak-free, and
that all ground glass joints have been greased properly with high vacuum, high temperature
chlorofluorocarbon-based stopcock grease. Turn the flask valve and the pump valve to their
"evacuate" positions. Evacuate the flask to 75 mm Hg absolute pressure, or less. Evacuation to a
pressure approaching the vapor pressure of water at the existing temperature is desirable. Turn the
pump valve to its "vent"
position, and turn off the pump. Check for leakage by observing the manometer for any pressure
fluctuation. (Any variation greater than 10 mm Hg over a period of 1minute is not acceptable, and
the flask is not to be used until the leakage problem is corrected.
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Procedure No.: STOP-05 Title: MONITORING/SAMPLING OF SOURCE EMISSION

Pressure in the flask is not to exceed 75 mm Hg absolute at the time sampling is commenced.)
Record the volume of the flask and valve (Vf), the flask temperature (Ti), and the barometric
pressure. Turn the flask valve counterclockwise to its "purge" position, and do the same with the
pump valve.
Purge the probe and the vacuum tube using the squeeze bulb. If condensation occurs in the probe and
the flask valve area, heat the probe, and purge until the condensation disappears. Next, turn the pump
valve to its "vent" position. Turn the flask valve clockwise to its "evacuate" position, and record the
difference in the mercury levels in the manometer. The absolute internal pressure in the flask (Pi) is
equal to the barometric pressure less the manometer reading. Immediately turn the flask valve to the
"sample" position, and permit the gas to enter the flask until pressures in the flask and sample line
(i.e., duct, stack) are equal. This will usually require about 15 seconds; a longer period indicates a
plug in the probe, which must be corrected before sampling is continued. After collecting the sample,
turn the flask valve to its "purge" position, and disconnect the flask from the sampling train. 8.1.3
Shake the flask for at least 5 minutes. 8.1.4 If the gas being sampled contains insufficient oxygen for
the conversion of NO to NO2 (e.g., an applicable subpart of the standards may require taking a
sample of a calibration gas mixture of NO in N 2), then introduce oxygen into the flask to permit this
conversion. Oxygen may be introduced into the flask by one of three methods: (1) before evacuating
the sampling flask, flush with pure cylinder oxygen, then evacuate flask to 75 mm (3 in.) Hg absolute
pressure or less; or (2) inject oxygen into the flask after sampling; or (3) terminate sampling with a
minimum of 50 mm (2 in.) Hg vacuum remaining in the flask, record this final pressure, and then
vent the flask to the atmosphere until the flask pressure is almost equal to atmospheric pressure.

Sampling procedure of Carbon Monoxide, Methane and Non- Methane Hydrocarbons:

Sample is collected in Tedlar Beg with a constant low flow rate of 1 LPM for 1 liter of sample
volume.
Sampling procedure of Ammonia:
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Procedure No.: STOP-05 Title: MONITORING/SAMPLING OF SOURCE EMISSION
Place 30 ml of absorbing solution into each of the first two impingers. Leave the final impingerdry.
Connect all the three impingers in series and place in the ice bath. Check the sampling train for
leakage and start the sampling for 30 min. at the flow rate of 2 L/min. Do not expose the absorbing
 reagent to direct sunlight. After sampling transfer the first two impinger content into PTFE sampling
storage bottle.

Sampling procedure of Hydrogen Sulphide:

Place 30 ml of absorbing solution into first three impingers. Connect all the three impingers in series
and place in the ice bath. Check the sampling train for leakage and start the sampling at the flow rate
of 0.5 L/min for collect the volume about 8 liter. Do not expose the absorbing reagent to direct
sunlight. After sampling transfer the first two impinger content into PTFE sampling storage bottle.
Sampling procedure of Carbon Di-sulphide:
Place 30 ml of absorbing solution into last two impingers. Connect all the three impingers in series
and place in the ice bath. Check the sampling train for leakage and start the sampling at the flow rate
of 0.5 L/min for collect the volume about 8 liter. Do not expose the absorbing reagent to direct
sunlight. After sampling transfer the first two impinger content into PTFE sampling storage bottle.
Sampling procedure of Fluoride:
Place 30 ml of absorbing solution into each of the PTFE impingers. Connect all impingers in series
and place in the ice bath. Check the sampling train for leakage and start the sampling for 30 min. at
the flow rate of 2 L/min. Do not expose the absorbing reagent to direct sunlight. After sampling
transfer the first two impinger content into PTFE sampling storage bottle.
Sampling Procedure for Free Chlorine:-
Pour 50 ml of the acidic absorbing solution into each one of the first pair of impingers, and 50 ml of
the alkaline absorbing solution into each one of the second pair of impingers. Connect the impingers
in series with the knockout impinger first, if used, followed by the two impingers containing the
acidic absorbing solution and the two impingers containing the alkaline absorbing solution. Place a
fresh charge of silica gel, or equivalent, in the drying tube or impinger (after the one more empty
impinger) at the end of the impinger train. Adjust the probe temperature and the temperature of the
filter and the stopcock, i.e., the heated area in Figure – 1 to a temperature sufficient to prevent water
condensation. This temperature should be at least 20̊C above the source temperature, but not greater
than 120̊ C. The temperature should be monitored throughput run to ensure that the desired
temperature is maintained.

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Procedure No.: STOP-05 Title: MONITORING/SAMPLING OF SOURCE EMISSION

6. Precautions:
a. Select the sampling site at any cross section of the stack or duct that is at least Eight stack or duct
diameters downstream and two diameters upstream from any flow disturbance such as bend,
expansion, contraction, visible flame, or stack exit.
b. Pitot tube, temperature and sampling probe are to be inserted together into the sampling port for
monitoring purposes.
c. Under no condition shall sampling points be selected within 3 cm of the stack Wall.
d. Molecular Weight Determination Before Calculate the Velocity
e. Traverse Point Criteria and Selection
f. Port should extend outward from the exterior stack wall not less than 50 mm and not more than 200
mm only when additional length is required for gate valve installation. Ports should be installed at a
height between 0.90 and 1.2m above the floor of the working platform.
g. Power Supply Should Be 220 V/Single Phase at the Platform.
h. The work platform should be able to support at least three men (Average 80 Kg each) and 91 Kg of
test equipment (stack monitoring kit, etc.).
i. Wear Safety Helmet Safety Shoes and Double Clamp Safety Belt and Goggles and Vehicle and First
Aid Should Be at the Site.
j. Thimble should be Pre-weighted and Clean.
k. When starting the test, the nozzle should be facing in the upstream direction.
l. Iso Kinetic Sampling Conditions Should be Maintain during Monitoring.

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Procedure No.: STOP-06 Title: SAMPLING OF WATER AND WASTE WATER

1. Purpose
The purpose of this SOP is to provide guidelines for Sampling of water and waste water.
2. Principle
A sufficient numbers of composite sampling with small amounts of grab sample helps in collecting a
reasonably representative sample.
3. Instruments/Equipments/ General Requirements and safety considerations
Ensure that all sampling equipments are clean and quality assured before use. Bake at 450̊ C all
bottles to be used for organic analysis.
Fill the container full for most organic compounds and Leave space for aeration and mixing for
microbiological and inorganic analysis.
Precautions may be limited to wearing gloves or may include coveralls, aprons or other protective
apparel. Often, the degree of protection is provided by chemical protective clothes. Always wear eye
protection (e.g., safety glasses with side shields or goggles).
When toxic vapors may be present, sample only in well ventilated areas, In a Laboratory open
sample container in a fume hood.
Always prohibit eating, drinking or smoking near samples
4. Type of sampling
Grab Sampling:
Grab samples are single samples collected at a specific spot at a site over a short period of time
(typically seconds or minutes). Thus, they represent a snapshot in both space and time of a sampling
area. Discrete grab samples are taken at a selected location, depth, and time.
A sample can represent only the composition of its source at the time and place of collection.
However, when a source is known to be relatively constant in composition over an extended time or
over substantial distances in all directions.
The same principles apply to sampling waste water, sludges, sludge bank and muds, although these
matrices are not specifically addressed in this Title.
Composite Sampling:
Composite sample should provide a more representative sampling of heterogeneous matrices in
which the concentration of the analytes of interest may very over short periods of time and or/space.
Composite samples can be obtained by combining portions of multiple grab samples or by using
specially designed automatic sampling devices.
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Procedure No.: STOP-06 Title: SAMPLING OF WATER AND WASTE WATER

Composite samples are collected by using continuous, constant sample pumping or mixing equal
water volumes collected at regular time intervals.
Integrated Sampling:
 For Certain Purposes the information is needed is best provided by analyzing mixture of grab
samples collected from different point simultaneously, or as nearly so as possible, using discharge
weighed method such as equal width increment or equal discharge increment procedures and
equipment.
Preparation of integrated samples usually requires equipment designed to collect a sample water
uniformly across the depth profile. Collecting integrated samples is a complicated and specialized
process that must be described adequately in a sampling plan.
Sampling of different sample matrix: Sample is collected manually from various type of
sampling location by method describe below-
a) River Streams and canals: Sample should be collected as far as possible form mid stream and
at mid depth, sample near the bank should be avoided, it may be collected from the bridge or
by boat where feasible.
b) Ground water: sample should be collected after pumping the bore hole or well for a period of
at least one hour.
c) Drinking Water: The sample should be collected from tap or pipeline directly as close as
possible to the reservoir in the container.
d) Sewage/ETP Effluent: sample should be collected at the point where the Effluent enter in
treatment plant and at the point after various stages of treatments. Sample may also becollected
from each step of treatment if required.
5. Sampling for microbiological examination:
Collect sample of water with utmost care to ensure that no contamination occurs at the time of
collection and prior to examination.During sampling, the stopper and the neck of the bottle do not
touches .Hold the bottle at the base with one hand and hold the stopper with the other hand .Immerse
the bottle beneath the water surface , slowly open the stopper allowing water to enter the bottle . Fill
the bottle without rinsing and once filled place the stopper quickly in its place .Remove the bottle
from the water . Label It.

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Procedure No.: STOP-06 Title: SAMPLING OF WATER AND WASTE WATER

Sampling from tap: Avoid leaking taps,as flow cannot be controlled.Close the tap tightly with no
dripping of water . Flame the tap ( in case of plastic tap, apply alcohol or spirit, preferably rectified,
 and allow it to dry). Open the tap fully and allow water to run for two to three minutes.Reduce the
flow and gently fill the bottle and place the stopper .

Sampling direct from a source : Do not take sample too far from a point of far off or too
close.Avoid areas of relative stagnation in a stream .Collect Samples from a river , stream by
holding the bottle in the hand near its base and plunging it neck downward,below the surface. Turn
the bottle until the neck points slightly upward, the mouth being directed against the current . If it is
not possible to collect samples in this way , attach a weight to the base of the bottle lower the bottle
with weight into the water. If the sample is to be taken from a well , flame the mouth of the hand-
pump and pump the water to waste for four to five minutes before the collection of sample . If the
well is fit with a mechanical pump , collect the sample from a tap on the discharge. ( If the tap is
connect to an overhead storage tank , this fact is record in the sampling report ). If there is no
pumping machinery, collect the sample directly from the well in a sterilize bottle fit with a weight at
the base. In this case , care is to taken to avoid contamination of the supply by any surface scum.

Size of the sample : Do not fill the sample up to the brim and Leave some space in bottle for
effective mixing of the sample .

Preservation & storage: Preserve the sample at 1-4°C and analyse within 30 hrs of collection.

Identifying data: Label all samples with the source , date and time of collection , and the name and
designation of the person who collected sample .

6. Sampling for biological examination:

Collect sample of natural plankton producing water in a clean, neutral glass bottles of 2-litre
capacity. Leave small air space between the bottle & the stopper . Collect the concentrate sample of
the plankton organisms from water with the aid of a plankton net. Haul the plankton net
horizontally in the water for 2 metres .Lift the net and wash off the collected organisms in net into
the bottle,
Preservation: The samples is examine within 2 to 3 hrs after collection. If the examination is to be
done late , preserve the samples as follows:
To each 100 ml of the sample , add about 3 ml of 2 percent formaldehyde soln. (made by diluting 5
ml of 37-40 percent aqueous formaldehyde solution to 100 ml with distilled water ), 0.5ml of 20
percent detergent solution made by diluting 20 ml of liquid . detergent to 100 ml with distilled water
and 5-6 drops of copper sulphate soln. 21 percent (v/v).This preservation maintains cell colouration
and is effective indefinitely. Store the preserved sample in the dark.

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Procedure No.: STOP-06 Title: SAMPLING OF WATER AND WASTE WATER
7. Preservation and Storage:
The sample should be preserve and store by the process define as under-
S. Determination Container Minimum Preservation Maximum storage
No. sample size (ml) Recommended Regulatory
 1. Acidity P/G 100 Refrigerate 24 hrs. 14 days
2. Alkalinity P/G 200 Refrigerate 24 hrs. 14 days
3. B O D. P/G 1000 Refrigerate 6 hrs. 48 hrs.
4. Boron P/G 1000 HNO3 to pH<2 28 days 6 months
5. C O D. P/G 100 H2SO4 to pH<2 7 days 28 days
6. Chloride P/G 100 Non required N. S. 28 days
7. Chlorine P/G 500 Analyzed 0.25 h. 0.25 h.
(Residual) immediately
8. Color P/G 500 Refrigerate 48 hrs. 48 hrs.
9. Specific P/G 500 Refrigerate 28 hrs. 28 hrs.
Conductance
10. Fluoride P/G 100 Non required 28 hrs. 28 hrs.
11. Hardness P/G 100 HNO3 or H2SO4 6 months 6 months
to pH<2
12. Chromium P/G 1000 Refrigerate 24 hrs. 24 hrs.
13. Copper P/G 1000 Refrigerate 24 hrs. 24 hrs.
14. Nitrate P/G 100 Analyzed 48 hrs. 48 hrs.
immediately
15. Nitrite P/G 100 Refrigerate None 48 hrs.
16. Oil & Grease P/G 1000 H2SO4 to pH<2 28 days 28 days
Refrigerate
17. Phenol P/G 500 H2SO4 to pH<2 As soon as 28 days
Refrigerate possible
18. Dissolve Oxygen P/G 300 Analyzed 0.25 h. 0.25 h.
immediately
19. pH P/G 50 Analyzed 0.25 h. 0.25 h.
immediately
20. Phosphate P/G 100 Refrigerate 48 hrs. N. S.
21. Silica P/G 200 Refrigerate, 28 days 28 days
Don’t Freeze
22. Sulphate P/G 100 Refrigerate 28 days 28 days
23. Turbidity P/G 100 Analyze same 24 hrs 24 hrs
day Refrigerate
P- PVC, G-Glass

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Procedure No.: STOP-06 Title: SAMPLING OF WATER AND WASTE WATER

8. Precautions:

a. Drinking water intake points, bathing Ghats, irrigation canal off-take points should be considered
for monitoring.
b. Sites for biological sampling should match with sites for chemical sampling.
c. In case of groundwater sampling select only wells (tube well, dug-well, Handpump)
d. Rinse the sample container three times with the sample before it is filled.
e. Leave a small air space in the bottle to allow mixing of sample at the time of analysis.
f. Label the sample container properly, preferably by attaching an appropriately Inscribed tag or
label.
g. The sample code and the sampling date should be clearly marked on the sample container or the
tag.
h. For bacteriological samples, when collected from tube wells/hand pump, the spout/outlet of the
pump should be sterilized under flame by spirit lamp before Collection of sample in container.
i. Sample identification forms should all be kept in a master file at the laboratory where Surface
water Samples will be collected from well-mixed section of the river (main stream) 30 cm Below
the water surface using a weighted bottle.
j. Samples from reservoir sites will be collected from the outgoing canal, power channel or water
intake structure, in case water is pumped. When there is no discharge in the Canal, sample will be
collected from the upstream side of the regulator structure, Directly from the reservoir.
k. Some parameter Should be analyzed on site (D.O, pH. Temp.TDS,RFC etc.)
l. Samples for groundwater quality monitoring would be collected from one of the following three
types of wells: • Open dug wells, Tube wells, hand pump or a power-driven pump Pyrometers,
m. Samples from the production tube wells will be collected after running the well for about 5
minutes.
n. For bacteriological samples, when collected from tubewells/hand pump, the spout/outlet of the
pump should be sterilized under flame by spirit lamp before collection of sample in container.
o. Precautions: Prior to sample preservation, put on protective disposable gloves supplied in the
sampling kit. Also wear supplied chemical safety glasses, unless you are already wearing
eyeglasses.

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