GUIDELINES FOR MANUAL SAMPLING

AND ANALYSES
RESPIRABLE DUST SAMPER
IMPINGER
 Stack sampling
To determine the quantity and quality of the pollutant emitted
by the source.
To measure the efficiency of the control equipment by
conducting a survey before and after installation.
To determine the effect on the emission due to changes in raw
materials and processes.
To compare the efficiency of different control equipments for a
given condition.
To acquire data from an innocuous individual source so as to
determine the cumulative effect of many such sources.
To compare with the emission standards in order to assess the
need for local control.
 Planning the study
Familiarity of the process and operations to determine
the time of cyclic operations, peak loading that might
cause variations in the characteristics.
Methods of sampling
Methods of analysis of samples
Sampling time because certain industries undergo
cyclic changes
Sampling frequency.
 Representative sample
It is highly important that the sample collected must truly
represent the conditions prevailing inside the stack. The important
considerations for accurate representative sample collection :
Accurate measurement of pressure, moisture, humidity and gas
composition
The selection of suitable locations for samplings
Determination of the traverse points required for a velocity and
temperature profile across the cross-section of the stack and
sampling for particulate matter
The measurement of the rate of flow of gas or air through the stack
Selection of a suitable sampling train
Accurate isokinetic sampling rate especially for particulate
sampling
Accurate measurement of weight and volume of samples collected
 objective
The main tasks involved are to determine the pollutant
concentration, stack gas flow rate and pollutant mass
emission rate. These terms are related as shown in eq
PMRs=Cs*Qs
Where,
PMRs=is the average pollutant mass emission rate from
the stack
Cs=is the average stack concentration of the
pollutant, and
Qs=is the average volumetric stack gas flow rate
Hence, the overall objective is to determine PMRs by
measuring Cs and Qs. The average volumetric stack
gas flow rate , Qs is determined by measuring the
average gas velocity, Vs and the area of the stack As
Qs=VsxAs
The basic equation to determine the velocity of flow
inside the stack is given by eq
Vs=Kp*Cp{Tsx
where,
P=is the velocity head, mm H2O
O
Ts=is the stack temperature K
Ps=is the absolute stack gas pressure, mm Hg
Ms=is the molecular weight of the stack gas
Kp=is the dimension constant
Cp=is the pitot coefficient
 Selection of sampling location
The sampling point should be as far as possible from
any disturbing influence, such as elbows, bends,
transition pieces, baffles or other obstructions.

The sampling point, wherever possible should be at a

distance 5-10 diameters down-stream from any
obstructions and 3-5 diameters up-stream from similar
disturbance.
 Size of sampling point
Usually, there will not be any opening in the stack.
Hence for collection of samples, an opening has to be
made to an extent of accommodating the probes.

 The size of sampling point may be made in the range

of 7-10cm, in diameter.

A flange may be riveted so that the opening may be

closed during the non-sampling period.
 Traverse points
For the sample to become representative, it should be
collected at various points across the stack.
 This is essential as there will be changes in velocity and
temperature (hence the pollutant concentration) across
the cross-section of the stack.
 Traverse points have to be located to achieve this.
These points are to be located at the centre of each of a
number of equal areas in the selsected cross-section of
the stack.
The number of traverse points may be selected with
reference to table
 Rectangular Stack
C/S AREA OF THE STACK NO.OF POINTS
SQ.M

0.2 4
0.2-2.5 12
2.5 and above 20
Circular stack
 Circular stack
Minimum required no of traverse points for sampling
site which meet sampling criteria
Inside diameter of stack or Number of points
duct (m)
I.D. ≤ 0.3 4

0.3 ≤ I.D. ≤ .6 8 8

0.6 ≤ I.D. ≤ 1.2 12 12

1.2 ≤ I.D. ≤ 2.4 20 20

2.4 ≤ I.D. ≤ 5 32
Circular stack
Pitot Tube
Assembly
sampling technique
 Isokinetic conditions
The efficiency of the sampling depends on the conditions
at which sampling was carried out.
The sample collected must be representative like a
composite waste water collection.
 This can be achieved by isokinetic sampling.
 Isokinetic conditions exist when the velocity in the stack
Vs equals the velocity at the top of the probe nozzle Vn at
the sample point.
 This is especially important when the particle size is
greater then 3m as it presents a problem in that, the
inertial effect on the particles can result in erroneus
samples.
Gas sampling
 Determination of gas composition
The first step in the field work of stack sampling is to
determine the gas composition. This can be
determined by using ORSAT APPARATUS
The gas is collected in the orsat apparatus and
analysed for the composition of CO2, O2 and CO in
the same order, and the remaining is assumed to be
nitrogen.
 Molecular weight of gas= sum of ( Mx*Bx)
Mx is the molecular weight of CO2,O2,CO and N2 resp.
Bx- represents % of gases.
 Determination of moisture content
The moisture content in the stack may be determined by
any one of the following methods:

wet bulb and dry bulb temperature technique

condenser technique
silica gel tube
The wet and dry bulb technique is used when the moisture
content is less than 18% and dew point is less than 51
degree Celcius and cannot be used for acid streams.
As the moisture content in the stack is usually less than
18%, the wet bulb and dry bulb technique is being
adopted.
 Determination of temperature
The temperature has to be measured across the cross-
section of the stack at predetermined traverse points.
 The temperature probe is inserted into the stack and
the reading are taken with the help of a pyrometer.
care should be taken in selecting the probe.

Type of probe Temperature range

(degree celcius)
Chromel/alumel 148.8-1260
Copper/constantan 148.8-348.9
Iron//constantan 115.5-1010
platinum 0-1537.7
 Determination of velocity

Velocity measurement is the most essential part of

stack sampling. This measurement is not only required
for establishing the gas flow rate but also for fixing
isokinetic conditions.
 Gaseous sampling

The procedure adopted for gaseous sampling in a stack

differs little from particulate matter sampling.
 Isokinetic sampling principles are not required for
gaseous sampling.
However, the success of gaseous sampling depends on
the proper collecting device, since different gases,
mists and vapours exhibit a wide variety of physical
and chemical characteristics.
 Methods for collection of gaseous samples

Gaseous sampling may be carried out by any one of the following methods:
absorption
adsorption
freezeout/condensation
Whenever the flow rate and the process operation are uniform and whenever
analytical equipment of extreme sensitivty is available it is possible to take a
grab sample from the stock by any one of the following methods:
use of an evacuated container
purging (displacement of air)
inflation of flexible bag
use of a syinge
 Proportional sampling
Whenever the source conditions, especially flow rate
changes, with time, the sampling must be done
proportionally so that the sample is representative.
This requires the velocity measurement as explained
and correction to standard conditions.
wt.of gaseous sample
concentration of pollutant=
volume of gas sample
For analysis of various gaseous pollutants standard
books may be referred
Conditions for stack sampling
Flow rate much lower with particulate sampling
App 1-5lit/min
Sampling method which is used has its special
application,depending on temperature,humidity and
gaseous constituent being analysed.
No all purpose collection system/device exists for
gaseouse sampling.
For ex. Of gasoline vapors,activated carbon serves as an
effective adsorption medium,where its collection
effeciency falls sharply for butane.
Freezeout sampling
In this method air samples are passed through cold
traps,maintained at progressively low temperatures

Sl.no Coolant temp

1 Ice water 0
2 Ice salt -21
3 Dry ice and acetone -79
4 Liquid air -147
5 Liquid oxygen -1832
 STANDARD OPERATING PROCEDURE FOR SAMPLING OF
METALS AND NONMETALS
This method is applicable for determination of
antimony (Sb), arsenic (As), barium (Ba),
beryllium (Be), cadmium (Cd), chromium (Cr), cobalt
(Co), copper (Cu), lead (Pb),manganese (Mn), mercury
(Hg), nickel (Ni), phosphorus (P), selenium (Se), silver
(Ag),thallium (Tl), and zinc (Zn) emissions from
stationary sources.
This method may be used
to determine particulate emissions in addition to the
metals emissions if the prescribed
Preparation of sampling train

Assemble the sampling train as shown in the Figure –

1.
 Select First impinger as a moisture trap.
 Put 100 ml of the HNO3 /H2O2 solution in the
second and the third impinger.
 Keep fourth impinger empty.
 Place 100 ml of the acidic KMnO4 absorbing solution
in each 5th and 6th impingers
 Take 200 to 300 g of pre-weighed silica gel in the last
impinger.
If Hg analysis will not be performed, the fourth, fifth,
and sixth impingers as shown in
Figure -1 are not required.
Precaution: Prevent the acidic KMnO4 from
contacting any glassware that contains sample
material to be analyzed for Mn. Prevent acidic H2O2
from mixing with the
acidic KMnO4. Uses of amber glass impinger are
recommended for acidic
KMnO4 Solution.
 Field activity
Perform leak check. Determine the stack pressure,
temperature, calculation of Isokinetic velocity,
volumetric flow rate, flow at nozzle/ selection of nozzle,
adjustment of flow rate at rotameter, temperature at
metering point and volume of gas sampled, pressure drop
during sampling as described in the SOP of the
particulate matter.

Note:
Calculate isokinetic velocity and collect the sample
following the SOP prescribed for
Particulate monitoring.
Sample Recovery
Cool the probe, Transfer the probe and filter assembly to
a clean area, cap all the open outlet with the non-
contaminated glass stoppers or plastic cap.
Take special precautions to assure that all the items
necessary for recovery do not contaminate the samples.