Netel (India) Limited

W-408, Rabale MIDC,

TTC Industrial Area,
Navi Mumbai – 400 701
Ph. (022) 27607 101/102
Website: www.netel-india.com

INSTRUCTION MANUAL
for
STACK MONITORING KIT
MODEL NPM –SMK 1
 Table of contents

Page No.

Standard Warranty ------------------------------------- 1

Introduction ------------------------------------- 2

Principles of Operation ------------------------------------- 3

Unpacking ------------------------------------ 4

Description of Stack Monitoring Kit --------------------------- 5

Pre-assembly and System Check-out -------------------- 7

Selection of Sampling Site and Minimum Number of

Traverse Points ------------------------------------ 10

Method for measurement of emission from stationary source.

a) Determination of Stack Gas Velocity &

Volumetric Flow Rate --------------------------------- 15
b) Determination of Particulate Matter --------------- 22
c) Determination of SO2 --------------------------------- 29
d) Determination of NO/NO2 ----------------------------- 36

Technical Specifications --------------------------------- 50

 STANDARD WARRANTY

STACK MONITORING KIT

We warrant Stack Monitoring Kit manufactured and sold by us to be free from defects in
materials, workmanship and performance for a period of six months from the date of
shipment from NETEL. Any parts found defective within that period will be repaired or
replaced, at our option, free of charge, f.o.b. factory. This warranty does not apply to
those items which by their nature are subject to deterioration or consumption in normal
service, and which must be cleaned, repaired or replaced on a routine basis. Such items
include :-

1) THIMBLES
2) RED OIL
3) BATTERY CELL

Warranty is voided by abuse including rough handling, mechanical damage, and

alteration or repair procedures not in accordance with instruction manual. This
warranty indicates the full extent of our liability, and we are not responsible for removal
or replacement costs, local repair costs, transportation costs, or contingent expenses
incurred without our prior approval.

NETEL’s obligation under this warranty shall be limited to repairing or replacing, and
returning any product which NETEL shall determine to its satisfaction to have been
defective. To receive warranty consideration, all products must be returned to NETEL at
its manufacturing facilities with transportation charges prepaid.

This warranty is expressly in lieu of any and all other warranties and representation,
expressed or implied, and all other obligations or liabilities on the part of NETEL
including but not limited to, the warranty of fitness for a particular purpose.

In no event shall NETEL be liable for direct, incidental or consequential loss or damage
of any kind connected with the use of its product to function or operate properly.

1
 INTRODUCTION

NETEL's STACK MONITORING KIT is designed to measure the total volumetric

discharge of particulate matter and gaseous pollutants from the stacks. It takes
accurate iso-kinetic samples of the effluents in the emissions from chemical and
combustion process. This efficient, flexible system samples all gases stream effluents in
accordance with Central Pollution Control Board's Emission Regulations, Part III
(December 1985). Introduced in 1986, the NETEL's Stack Monitoring Kit was the first
system made to the Central Board specifications for the stationary source sampling.
NETEL's expertise in Air Pollution is reflected in progressive modifications and
improvements to the basic design of the Stack Monitoring Kit. We have also produced a
wide range of accessories that have been developed and adopted to meet specialised
stack sampling requirements.

Designed to operate with its sampling probe in a horizontal or vertical position, this
versatile unit can be used in round or rectangular stacks and ducts with flow velocities
from 1 to 30 m/sec, and temperatures up to 600° C or higher with optional accessories. It
collects particulate samples down to 0.3 µm diameter. Sulphur dioxide gas (SO2),
Sulphur trioxide (SO3), Sulphur Acid mist (H2SO4), Oxides of Nitrogen (NOx), Water
vapours and any other gases which can be measured by Wet Chemical methods.

Engineered for ease of installation, this advanced NETEL's Stack Monitoring Kit meets
all accepted standards for stack sampling operations.

2
 PRINCIPLE OF OPERATION

The purpose of stack monitoring (also called source monitoring) is to extract

sample from the stack or duct a that is representative of emissions from that
source during a time period in which the process is under a desired operating
condition. The scope of stack monitoring includes the following :

i) Determination of stack gas velocity and volumetric flow rate.

ii) Determination of moisture content in stack gases.
iii) Determination of gaseous pollutants such as SO2, SO3,NOx, F, etc.
iv) Determination of Suspended Particulate Matter.

The principle of measurement and the details of operation including the site
selection for a representative sample are described in detail in the following
chapters.

In operation the Pitobe tube consisting of Pitot Tube, Thermocouple and Filter
holder is inserted into a test port and the vacuum pump is operated to maintain
the proper iso-kinetic flow rate as determined by stack velocity, temperature and
pressure. Adjustment of coarse and fine control valves assures that the iso-kinetic
rate is maintained over a wide range of velocity pressures. Within the filter
probe, a contaminated gas enters the high efficiency thimble filter and the
particulate matter is thus collected in the filter thimble. From the filter the gas
goes to the impinger section contained in a double walled impinger module.
After removing the moisture present in the gas stream, the gas now enters the
Control module where a known rate of the gas goes into the dry gas meter
under known temperature and pressure conditions. A suction pump draws the
sample through the entire assembly of Pitobe, Impinger module and Control
module. The collected sample is analysed for its weight gain to calculate the
SPM (Suspended Particulate Matter) concentration. The reagents , which have been
used for absorbing the gaseous pollutants, are analysed for different pollutants, such
as SO2, NOx, etc.

3
 UNPACKING

Open the boxes and check the contents with the packing slip in the envelope
along with this manual. Open the control module and impinger module and
check all components for transit damage.

Check pitot tube and thermocouple etc. for damage such as broken or bent
tubings or connectors. Inspect all glass items for breakage. If damage is found,
Please inform it to us, transport carrier and insurance company and immediately file a
claim.

4
 DESCRIPTION

NETEL's Stack Monitoring Kit consists of Control Module, Dry Gas Meter
Module, Impinger Module with standard glassware set, probe assembly with
hoses and pump.

a) CONTROL MODULE

The control module shown in fig. 1 contains all necessary operational controls,
pressure and temperature measurement displays, flowmeters, etc. mounted in a
sturdy lightweight fibre glass cabinet. The fibre glass cover has been provided to
protect the operational controls from any damage during transportation to site
and sampling platform. The cover is mounted on half hinges and is removable
during operation. The module is battery operated and runs on 4 batteries that
can be changed from the rare side of the control module.

TEMPERATURE

The temperature readout system is a 3 1/2 digit liquid crystal display for
measuring the temperature of stack gas. For measurement of stack gas
temperature, put the main switch ‘ON' of this system and connect the
thermocouple output plug to TC input socket. If the battery get discharged, the
display will loose its contrast.

DIGITAL STOPWATCH

This is four and half digit stopwatch with liquid crystal display to measure
time up to 1 hour 59 minutes and 99 sec. The minimum resolution is 1 sec.
For measurement of time, put the toggle switch to `ON' position. The stop and reset
action is done by a single 2 position toggle switch. The down position is for stop,
while up is for reset action.

INCLINED CUM VERTICAL MANOMETER

This is an acrylic body manometer designed to measure maximum pressure difference of

150 mm, with a resolution of 0.25 mm for inclined up to 50 mm and vertical with 1 mm
resolution from 50 to 150 mm. The manometer has a spirit level , which can be
aligned with adjustable legs provided in the cabinet. The manometer has got two
nylon plugs for making it spill proof during transportation. The specific gravity of the
red oil supplied with the equipment is 0.826. For filling the oil, remove the plug
of right hand side. Open the left sides plug till the hole for the passage of air is
clear. Put the required amount of oil and close the plug.

5
After filling the manometer with Red oil (sp. gravity 0.826) up to zero mark,
rotate nylon plugs clockwise till it is completely closed. While operating, open
the plugs to the extent that the holes at the back for the passage of gas, can be
seen clearly. Do not close the plugs too much because `O' ring will come out and
manometer will start leaking.

ROTAMETERS:

The rotameters have been provided for measuring the flow for Particulate Matter (PM)
and gaseous pollutants. The flow-controller fitted on the pump is to control the iso-
kinetic flow-rate of particulate matter, which is measured on left side large rotameter. If
the gases are sampled simultaneously ball valve should be used and flow rate is
adjusted with the help of right side fine rotameter. In this case, flow rate passing
through the thimble and DGM will be total of both the rotameters, which should be
considered for iso-kinetic flow-rate and volume calculation of particulate matter.

b) FLOW TOTALISER / DRY GAS METER MODULE:

This is a diaphragm type dry gas meter housed in a separate fibre glass box shown in
fig.2 and is used to measure the total volume of gas collected. It has got a display with a
resolution of 1 litre. The difference between final and initial reading gives the volume of
the gas, which has passed through the flow totaliser. The meter has been calibrated at
25 deg. C and 760 torr and any change in operating conditions should be corrected by
measuring the temperature and pressure of the gas going in the meter. The temperature
of dry gas meter can be measured on dial type thermometer. The pressure is measured
with the vacuum gauge provided on the panel. The gauge gives the vacuum in inches of
Hg/mm of Hg with respect to atmospheric pressure (760 torr).

c)IMPINGER MODULE:

The impinger module shown in fig.3 is a double walled thermally insulated fibreglass
cabinet for housing six impinger tubes. Two impinger tubes are of modified
Greenburg Smith design with a capacity of 250 ml while four impinger tubes
are of midget impinger type with 120 ml capacity. The inner compartment can
be filled with ice/water. An adapter with a closing arrangement has been
provided to drain out the water from inner compartment. There is one inlet and
two outlet ports so that different set of impinger tubes in different
configurations can be connected to these ports.

6
 PRE- ASSEMBLY AND SYSTEM CHECK-OUT

PRE - ASSEMBLY

The entire sampling train should be assembled as shown in fig.7.

FILTER HOLDER ASSEMBLY

The arrangement of assembling the thimbles in filter holder has been shown
in fig. 5. Two types of thimble assembly have been provided, smaller one is
used for Glass Fibre thimbles of 19 mm OD while bigger assembly is used for
28 mm OD Cellulose thimbles. Place first the appropriate outer taper ring on
the thimble and bring it up to the open end. Now put the thimble along with the
outer ring on to the tapered cone and press it slowly. The thimble will get
flared up and make a seal between the two metal surfaces. Put the threaded
ring and tighten it. The thimble will not normally tear off as long as the outer
ring is covering the open end. Now thread the assembly into holder cover. Make
sure that silicon `O' ring has been inserted for leak tight connection.

Note: All thimbles must be prepared by desiccating at 25° C ambient

pressure for atleast 24 hours prior to use. Alternatively, they may be
dried in an oven 120° C for two hours and desiccated for two hours and
then weighed.

7
 NOZZLES WITH BEND PIPE

The bend- type pipe to be fixed to the filter holder assembly as shown in fig. 6.
Ensure that silicon `O' ring has been inserted in the 1/2" BSP female union of
filter holder before threading the bend pipe. Three types of nozzles (i.e. 1/4", 3/8"
and 1/2" dia opening) have been provided for fixing to the bend type pipe. Select
the right size of nozzle depending on the stack gas velocity i.e. smaller nozzle for
high velocities and bigger nozzle for low velocities. The thimble pipe is to be
connected along with silicon `O' ring to the thimble holder. Ensure that nozzle
and bend pipes are clean (i.e. without any dust particles) before fixing.

IMPINGER BOX

Assemble all the impinger tubes as shown in fig.3. Be careful in assembling all
glassware. Clean all them with acetone or trichloroethylene. To help in sealing the
system, a light coating of silicon stopcock grease may be used on the ground
glass joints. Grease only the outer portions of the joints to avoid the possibility of
contaminating the sampling system.

CONTROL MODULE

Ensure that 4 nos. “D” type dry batteries have been fixed in the battery box provided at
the back of control module. Make sure that sufficient quantity of red oil has been
filled in the manometer. Connect the control module to the pump and impinger
box and make all the connections for tubing as shown in fig. 7.

PITOT TUBE

Check the Pitot Tubes and ensure that the tips are not damaged. Make sure
that tubes are not blocked, by blowing air through both the ends. (fig. 8)

SYSTEM CHECKOUT

We recommend that a pre-test leak check to be performed at all times before

starting the sampling. To perform leak checks proceed as follows after
assembling the sampling train.

8
1) Plug the inlet nozzle using a rubber stopper.

2) Plug the power cord of vacuum pump into a power outlet and
put the mains switch ‘ON’.

3) Open the coarse valve fully and observe the vacuum on the gauge. It should
be better than 20" of mercury.

4) Observe the dry gas meter dial and determine the leak rate by taking the
difference of the reading over a particular time. A leakage rate of less than 3 lpm
is acceptable.

5) If the leak rate does not exceed this value, carefully remove the plug from the
inlet of the nozzle and immediately shut-off the vacuum pump. Care must be
exercised in this operation so that water is not sucked out of the impingers nor
excessively bubbled through the impingers.

6) If the leakage rate exceeds 3 lpm, remove the plug from the nozzle and shut-
off the vacuum pump.

7) Disconnect the tubings from the control unit and leak check the control unit by
plugging the sample inlet connection. Follow steps 2 & 3.

8) If the leakage rate in the control unit does not exceed 3 lpm, then proceed to
connect control module to the impinger unit. Follow steps 2 & 3.

9) In succession, leak checks should then be performed on the impingers, the filter
holder and probe. In each case, observe the dry gas meter flow rate. Any flow
indicates leakage in the unit isolated working from the rear.

10) Correct the leakage whenever it occurs. We suggest, since most of the leakage
will occur in the filter holder, that is to be isolated first. From past experience we have
found that it is necessary to adequately seal the filter holder first when assembling the
unit.

9
SELECTION OF SAMPLING SITE AND MINIMUM NUMBER OF TRAVERSE
POINTS

As mentioned earlier, emission testing is based on the assumption that the

sample obtained at a given point is representative of the concentration at that
point. Therefore, a system in which the concentrations are non uniform with respect
to the stack-cross sectional area will require more sampling points compared to a
system with uniform concentrations. Usually gaseous concentrations are fairly
uniform across a duct's cross-section and a single sampling point is sufficient. To
obtain representative gas velocities and particulate concentrations traversing of
stack's cross-sectional area is a must and the number of traverse point required
in different cases are given below.

Particulate sampling or velocity measurement is performed at a site located at

least eight stack or duct diameters downstream and two diameter upstream
from any flow disturbance such as bend, expansion or contraction in the stack or
from visible flame. For rectangular cross section an equivalent diameter (De)
shall be calculated from the following equation to determine the upstream and
downstream distances
2 LW
De = ---------
L+W

where L = Length & W = Width of Stack.

When the above sampling site criteria can be met, determine the minimum
number of traverse points required, from Table 1. The minimum required
number of traverse points is a direct function of stack or duct diameter.

When a sampling site such as described above is not available, choose a

convenient sampling location and use Table 1 and fig. 9 to determine the
minimum required number of traverse points. First, measure the distance from
the chosen sampling location to the nearest upstream and downstream
disturbance. Then, from fig. 9 determine the corresponding sample point multiples
for both distances and select the greater of these. Multiply it by the number
obtained from Table 1.

10
The result of this calculations is the minimum number of traverse points
required. This number may have to be increased such that for circular stacks
the number is a multiple of 4 and for rectangular stacks the number is one of
those shown in Table 2.

Cross-sectional Layout and Location of Traverse Points

For circular stacks divide the cross section into equal parts by two right-angle
diameters. Locate half the traverse points symmetrically along each diameter
according to fig. 10 and Table 3.

For rectangular stacks determine the number of traverse points as described

earlier. From Table 2 determine the grid configuration. Divide the cross section
into as many equal rectangular areas as there are traverse points. Locate the
traverse points at the centroid of each area according to fig. 10.

Under no conditions shall a sampling point be selected within 3 cm of the stack

wall.

11
 Table 1

MINIMUM REQUIRED NUMBER OF TRAVERSE POINTS FOR

SAMPLING SITES WHICH MEET SPECIFIED CRITERIA

=========================================================
Inside diameter or equivalent Number of Points
dia. De of stack or duct (m) for circular for rectangular
stacks stacks
=========================================================
I.D. ≤ 0.3 4 4

0.3 ≤ I.D. ≤ 0.6 8 9

0.6 ≤ I.D. ≤ 1.2 12 12

1.2 ≤ I.D. ≤ 2.4 20 20

2.4 ≤ I.D. ≤ 5.0 32 32

========================================================

12
 Table 2

CROSS-SECTIONAL LAYOUT FOR RECTANGULAR STACKS

=========================================================
Number of Traverse Points Matrix Layout
=========================================================

9 3 x3
12 4 x3
16 4 x4
20 5 x4
25 5 x5
30 6 x5
36 6 x6
42 7 x6
49 7 x7
=========================================================

13
 Table 3

LOCATION OF TRAVERSE POINTS ON DIAMETERS OF CROSS

SECTIONS OF CIRCULAR STACKS

Traverse

Point PERCENT OF STACK DIAMETER FROM

Number INSIDE WALL TO TRAVERSE POINT
On a
Diameter

Number of traverse points on a diameter

2 4 6 8 10 12 14 16 18 20 22 24

1 14.6 6.7 4.4 3.3 2.5 2.1 1.8 1.6 1.4 1.3 1.1 1.1
2 8.4 25.0 14.7 10.5 8.2 6.7 5.7 4.9 4.4 3.9 3.5 3.2
3 75.0 29.5 19.4 14.6 11.8 9.9 8.5 7.5 6.7 6.0 5.5
4 93.3 70.5 32.3 22.6 17.7 14.6 12.5 10.9 9.7 8.7 7.9
5 85.3 67.7 34.2 25.0 20.1 16.9 14.6 12.9 11.6 10.5
6 95.6 80.6 65.8 35.5 26.9 22.0 18.8 16.5 14.6 13.2
7 89.5 77.4 64.5 36.6 28.3 23.6 20.4 18.0 16.1
8 96.7 85.4 75.0 63.4 37.5 29.6 25.0 21.8 19.4
9 91.8 82.3 73.1 62.5 38.2 30.6 26.1 23.0
10 97.5 88.2 79.9 71.7 61.8 38.8 31.5 27.2
11 93.3 85.4 78.0 70.4 61.2 39.3 32.3
12 97.9 90.1 83.1 76.4 69.4 60.7 39.8
13 94.3 87.5 81.2 75.0 68.5 60.2
14 98.2 91.5 85.4 79.6 73.9 67.7
15 95.1 89.1 83.5 78.2 72.8
16 98.4 92.5 87.1 82.0 77.0
17 95.6 90.3 85.4 80.6
18 98.6 93.3 88.4 83.9
19 96.1 91.3 86.8
20 98.7 94.0 89.5
21 96.5 92.1
22 98.9 94.5
23 96.8
24 98.9

14
METHOD FOR MEASUREMENT OF EMISSION FROM STATIONARY SOURCE.

DETERMINATION OF STACK GAS VELOCITY AND VOLUMETRIC FLOW

RATE (TYPE ‘ S ’ PITOT TUBE)

1) Principle

The average gas velocity in a stack is determined from the gas density and from
measurement of average velocity head with a Type S (Stausscheilbe or reverse
type) pitot tube.

2) Applicability

This method is applicable for measurement of the average velocity of a gas

stream and for quantifying gas flow.

This procedure is not applicable at measurement sites, which fail to meet the
criteria of selection of sampling points. Also, the method cannot be used for direct
measurement in cyclonic or swirling gas streams. When unacceptable conditions exist,
alternative procedures, subject to the approval of State / Central Pollution Control
Boards, must be employed to make accurate flow rate determinations; examples of
such alternative procedures are :

(1)To install straightening vanes

(1)To calculate the total volumetric flow rate stoichiometrically, or

(1)To move to another measurement site at which the flow is acceptable.

15
3) Procedure

i.Set up the apparatus as shown in fig.7. Capillary tubing or surge tanks

installed between the manometer and Pitot tube may be used to dampen (∆P)
fluctuations. It is recommended, but not required, that a pre-test leak-check be
conducted, as follows:

a. Blow through the pitot impact opening until at least 2.5 cm (1

in) of velocity pressure registers on the manometer, then, close off the
impact opening. The pressure shall remain stable for at least 15 seconds.

b. Do the same for the static pressure side, except using suction to
obtain the minimum of 2.5 cm (1 in.). The pressure shall remain stable
for at least 15 seconds.
i. Level and zero the manometer: Because the manometer level and zero may
drift due to vibrations and temperature changes, make periodic checks during the
traverse. Record all necessary data.

i. Measure the stack gas velocity pressure (∆P) on the inclined manometer by
inserting pitot tube in to the stack at all traverse points specified earlier. For
measurement of the stack gas velocity pressure, connect static tip of Pitot tube to (-ve)
inlet of inclined manometer & dynamic tip of Pitot tube to (+ve) end of the manometer
inlet. Ensure that the proper differential pressure gauge is being used for the range of ∆P
values encountered. Conduct a post-test as described above, to validate the
traverse run.

∆P = Manometer reading x Sp. Gravity of liquid (USED)

i. Measure temperature on the temperature readout (stack) at the traverse

points specified earlier, by connecting thermocouple inlet pin in to the TC input.

i. Measure the Static Pressure (Ps) in the stack with the help of inclined
Manometer, by disconnecting dynamic tip from the main module at the same traverse
points specified earlier, if static pressure difference is within 40 mm of W.G. For positive
pressure stacks, connect static tip (-ve) of Pitot tube to (+ve) of inlet of inclined
manometer. For negative pressure stacks, connect static tip to (-ve) inlet of inclined
manometer. For stacks with more than 40mm W.G. differential use `U' tube
manometer filled with water. One reading is usually adequate.

16
 Sp. Gravity of liquid (USED) x (Manometer Reading)
Pu = -------------------------------------------------------------------- (Hg)
13.5

Static pressure (Ps) will be calculated as,

Ps = 760 ± Pu (mm-Hg)

Where 13.5 = Sp. Gravity of the mercury. Addition will take place for +ve
pressure stack & Subtraction for –ve pressure stack.

i. Determine the atmospheric pressure with a barometer or use data available

with meteorological stations.

i. Determine the stack gas dry molecular weight. For combustion processes or
processes that emit essentially CO2, O2, CO, and N2, use method given below.
For processes emitting essentially air, analysis need not be conducted; use a dry
molecular weight of 29.0

i. Obtain the moisture content by the method given below.

i. Determine the cross-sectional area of the stack or duct at the sampling location.
Whenever possible, physically measure the stack dimensions rather than using
blueprints.

17
4) Determination of molecular weight
The average molecular weight the gas mixture is described by the expression:

n
M= ∑ Xi × Mi
i=1

where Xi is the mole fraction and Mi is the mole weight of each constituent in the
mixture of n number of constituents.

4.1) Dry and Wet Molecular Weights

For the majority of sources, Equation 1 is used to calculate the dry
molecular weight of the sample. This equation may be modified with
additional terms if other gaseous constituents that will influence the
molecular weight of the sample are present. Equation 2 is used to
calculate the molecular weight of the stack gas on a wet basis.

Md = 0.44 (% CO2) + 0.32 (%O2) + 0.28 (% N2 + % CO) .......... 1

Ms = Md (1-Bwo) + 18 Bwo .......... 2

0.44 - molecular weight of carbon dioxide divided by 100, kg/kg-mole

0.32 - molecular weight of oxygen divided by 100, Kg/Kg-mole

Bwo - proportion by volume of water vapour in stack gas

18 - molecular weight of water, Kg/Kg - mole

NOTE - In the majority of cases, the following equation may be used

% N2 = 100 - (% CO2 avg + % O2 avg + % CO avg)

Where
Md = Molecular weight of stack gas on dry basis, kg/kg - mole
Ms = Molecular weight of stack gas on wet basis, kg/kg - mole
% CO2 = percent carbon dioxide by volume, dry basis
% O2 = percent oxygen by volume, dry basis
%N = percent nitrogen by volume, dry basis

18
5) Determination of moisture in gas stream

1.1 Condenser Method - The condenser method, in principle, involves extracting

a sample of the stack gases through a filter for removal of the
particulate matter, then through a condenser, accumulating the condensate
formed in process, and finally through a gas meter. The object of the test is to
collect and measure the volume of all the condensate formed at the condensing
temperature from a measured amount of gas.

1.1 Apparatus - The apparatus necessary for determination of moisture content by

the condensate method is provided with stack monitoring kit. Particulate Sampling
Apparatus - consisting of a probe of stainless steel is equipped with a filter to
remove particulate matter will be required.

5.3 A glass condenser or 120 ml midget impingers may be used to

condense the water vapours. Assemble the equipment as shown in fig. 4.
Fill the impinger module inner compartment with ice/water bath.
Measure the temperature of the bath.

5.4 Gauges - two thermometer (range 0-100 °C), two calibrated vacuum gauges
or U-tube mercury manometers (range 0-500 mm)

1.1 Procedure - Except in unusual circumstances, the water vapour is

uniformly dispersed in the gas stream and therefore sampling for moisture
determination need not be iso-kinetic and is not sensitive to position in the duct.
The sampling nozzle may be positioned down-stream to minimise the build-up of
pressure drop across the thimble due to particulate catch. Sample the gas at the
rate of about 500 ml/sec. run the test until enough condensate has been collected
to enable an accurate measurement. Measure the temperature and pressure of
condenser close to the meter, as an insignificant pressure loss in the line
between them is expected. The meter pressure may be substituted for
condensate pressure. Measure the volume of gas sampled and barometric
pressure also in order to calculate the moisture content. Measure the volume of
condensate collected in a graduated measuring cylinder.

19
5.6 Calculations

Calculate the volume of water vapour collected using the following equations.

(Vc x 22.4) Tm 760

Vv = --------------- x ---------- x -----------
1000 x 18 273 Pbar-Pm

Where

Vv = Equivalent vapour of condensate under sampling

conditions, m3

Vc = Volume of condensate in condenser, ml

Tm = Absolute condenser temperature, ° K

Pm = Suction at meter, mm mercury column

Pbar = Barometric pressure, mm mercury column

Calculate the moisture content of the gases using the following

equation :

M = Bwo × 100 (%)

Where
Vv
Bwo = -------------------------
Vv + Vm

M = Moisture in the flue gases, percent

Vv = Equivalent vapour volume of condensate under

sampling condition

Vm = Volume of gas sampled (m3)

20
6) Calculations

6.1) Stack Gas Velocity

Stack gas velocity Us in m/sec is given by the following equation :

(∆P) x Ts
Us = Kp Cp ----------------
(Ps x Ms)
where

Us = Stack gas velocity, m/s

( kg. mm Hg )1/2
Kp = Constant, 33.5 m/s -----------------------------
( Kg-mole °K mm H20)

Cp = S-type pitot tube coefficient

Ts = Absolute stack gas temperature, ° K

∆P = Stack gas velocity pressure, mm water column or inclined manometer

reading in terms of mm multiplied by 0.826

Ps = Absolute Static pressure, mm Hg

Ms = Molecular weight of stack gas on wet basis kg/kg-mole

The nomographs given on the following pages will provide you the calculated
stack gas velocity for different velocity heads (∆P) at different stack gas
temperatures. These are based on the presumption that stack gas composition is
air (i.e. M=29) and static pressure is 760.

21
6.2) Stack gas volumetric flow rate

The following equation is used to calculate the stack gas volumetric flow rate
Qs (m3/hr)

298 Ps
Qs = 3600 (Us) x As (1-Bwo) x ------- x -------
Ts 760

where

As = Area of the stack (duct), m2

Bwo = Proportion by volume of water vapour in stack gas

Ts = Absolute stack gas temperature, K

Ps = Absolute stack gas pressure in mm of Hg

DETERMINATION OF PARTICULATE MATTER

This method is for sampling of particulate matter in a moving gas stream in a duct
or a stack. The methods for determining the sulphur dioxide and total oxides of
nitrogen are given later.

The collector recommended for use, under specified field condition to obtain
satisfactory results is described. These procedures utilise particulate filtering systems
, which are located within the stack. If properly used, these systems are
satisfactory for determining the mass concentration of particulate matter in the gas
stream at stack conditions. The use of collection system located outside the
stack for collecting samples at other than in-stack conditions is an alternative.

Determination of the particulate concentration consists of sampling isokinetically,

a measured amount of gas from the flue and separating the particles from the
gas and hence determining the particulate concentration. To obtain a
representative particulate sample, the sampling should be carried out
isokinetically, that is, the velocity of the gas stream through the sampling nozzle
should be equal to the velocity of gas stream in the stack.

22
Sampling at other than isokinetic velocities induces error. The particles of size
greater than 3 to 5 micron in size have sufficient inertia so that particle motion
may deviate significantly from the gas flow streamline pattern. In that case,
particles are selectively drawn into the probe in a size distribution different from
that existing in the duct or flue. It has been observed that, if sampling
velocity is greater than the isokinetic rate the sampling will have a lower mass
concentration of particulate material than the main stream because of collecting
greater percentage of fine particles. However, if the sampling velocity is less
than the isokinetic rate, the particulate sample has a higher mass
concentration than actually present, with lower percentage of fine particles.

PROCEDURE

Selection of Location of Sampling - Sample for particulate concentration shall be

done at the same traverse points where velocity measurement were carried out.

Calculation of Iso Kinetic Sampling Rate - The dry gas meter for measuring the
gas sample, measures the gas at conditions of temperature, pressure and
moisture content which are different than those in the flue gas. Therefore,
calculate the Iso Kinetic sampling rate at the gas meter for each sampling point
before starting the test and record on the log the required rate (Table 4). Calculate the
Iso Kinetic sampling rate at the gas meter as follows :

Tm (Pbar – Pu) Vm
Rm = Us An -------- x --------------- x ------------
Ts (Pbar – Pm) Vm + Vv

where
Rm = Iso Kinetic flow rate through meter, m3/S

Us = Velocity of flue gas at sampling point m/s

23
An = Area of sampling nozzle, m2

= 3.17 x 10-5 m2 for 1/4" bore nozzle

= 7.12 x 10-5 m2 for 3/8" bore nozzle

= 1.267 x 10-4 m2 for 1/2" bore nozzle

Tm = Absolute meter temperature, ° K

Ts = Absolute stack gas temperature, ° K

Pu = Suction in stack, mm mercury column

Pbar = Barometric Pressure, mm mercury column

Pm = Suction at meter, mm mercury column

Vm = Volume of gas sampled at meter conditions, m3

Vv = Equivalent vapour volume of condensate at meter
conditions, m3

Select the nozzle size, which will provide a meter sampling rate between 4 to 60
litres/min. Charts relating sampling rate with stack and meter conditions may be
prepared for the range of conditions expected.

24
 TABLE 4

DUST CONCENTRATION MEASUREMENT LOG SHEET

Sampling Dry Gas Meter Reading Rotameter Details

point
Temp. Static Meter Reading m3
C Pressure
Tm mm, Hg Pm
INL FNL Vol. Sampling Flow
Sampled Period Rate
sec. T m3/sec
Vm

25
Duration of Sampling-Plan the sampling run to be of sufficient length if one of the
following criteria have been obtained :

a) A minimum of 1 m3 of dry gas has been withdrawn for sampling. That will be
calculated by following equation.

1000
Time = --------- (sec.)
Rm

b) The mass of particulate matter amounts to at least 20 percent of the mass of

the filtering medium in the sampler.

Experience and intelligent judgement should be applied in determining the

sampling time. Too short a time may give unreliable results and too long a time
may cause the resistance of the sampling train to exceed the pump's limits.

Preparation of the sampling train :

After proper nozzle and filtering medium have been selected assemble the sample
train as shown in fig. 6. Mark the sampling probe (including nozzle and filter
holder) with the same traverse points used for conducting the velocity traverse.
Place a clean, preweighed thimble in the filter holder and tighten securely.

Start the test after sampling rates have been calculated and train assembled and
checked for leakages. When the equipment is ready in all respects, record the
initial dry gas meter reading and push the sampling probe carefully into the duct
to the point nearest to the back wall. This will allow the probe to cool in hot
stack as it comes out, shortening the time required for cooling after the sample is
taken. It is advisable to allow the nozzle and filter holder to preheat so that
moisture present in the gases do not condense in the filter during initial part of
the sampling.

When starting the test, the nozzle should be facing in the up stream direction,
start operating the suction source, open the control valve (coarse) and start the
stopwatch. Note the time and record it in the log sheet. Adjust the flow rate
with the help of the roatmeter and control valve until the desired flow rate for
isokinetic conditions is obtained.

26
As the test proceeds, dust build-up in the thimble will increase the amount of
suction required to maintain the proper meter rate, the valve should be adjusted
accordingly. This suction should not exceed 150 mm of mercury for paper
thimbles. In case it exceeds this value before the completion of sampling, replace
the same with a new thimble and restart sampling. During the test if the
mercury suction pressure at the meter drops suddenly, it indicates that a leak
has developed in the equipment or that thimble has cracked or burst. In this
event, discard the test and repeat. Record the initial gas meter reading and
pressure and temperature in the sampling train as well as condenser temperature
at half-minute interval during the test.

When sampling at one point has been completed, move the sampling probe to the
next point as quickly as possible. At the completion of test, close the control
valve, turn the direction of the probe so that the sampling nozzle is facing down-
stream and record the final gas volume and time. Remove the sampler carefully
from the flue gas and plug the nozzle to prevent the loss of sample.

Sample Recovery

After the sampler has cooled, brush down the dust on the inside of the nozzle
carefully into the thimble, using a small brush, remove the thimble and place it in a
dust-tight container for transportation to the weighing room. In case, the filter
holder is kept outside during the sampling, the dust from the sampling probe before
the filter holder should be brushed down into the thimble.

Determine the mass of dust collected in the thimble by difference, that is, by
weighing the thimble before and after the run. Dry the thimble in an oven for
about 2 hours at 120° C prior to sampling. After sampling, cool, dry and again
weigh the thimble alongwith dust maintaining the same conditions as prior to
sampling.

27
Calculations

Calculate the volume of gas sampled using the following equations :

Volume of dry gas through the sampling train ( 25 ° C, 760 mm Hg)
Pbar - Pm 298
Vstd = Vm x Y x ----------------- x ------------
760 Tm + 273
where
Tm = Absolute temperature of gas at dry gas meter conditions, °K
Vm = Volume of gas sampled at dry gas meter conditions, m3
(Pbar - Pm)= Actual pressure in sampling train, mm mercury column
Pbar = Barometric pressure, mm mercury column
Pm = Static pressure in sampling train, mm of mercury

Y = Calibration factor of Dry gas meter.

Dust concentration - Calculate the dust concentration using the following

equations :
Mn
Dust concentration in mg/ Nm3 , S = ---------
Vstd
where
Mn = Mass of the dust in the thimble in mg
Vstd = Volume of dry gas through the meter
(25° C, 760 mm Hg), Nm3

Emission Rate - Calculate the dust emission rate as follows :

S x Qs
Dust Emission Rate = ---------
(kg/hr) 106

where
Qs = Flue gas flow rate (25° C, 760 mm Hg) Nm3

All stack emission test results shall be given in dry basis as above, i.e. at zero
percent moisture.

28
DETERMINATION OF SULPHUR DIOXIDE EMISSION FROM STATIONERY
SOURCES (EPA METHOD)

Principle

A gas sample is extracted from the sampling point in the stack. The sulphuric
acid mist (including sulphur trioxide) and the sulphur dioxide are separated. The
sulphur dioxide fraction is measured by the barium-thorin titration method.

Applicability

This method is applicable for the determination of sulphur dioxide emissions from
stationery sources. The minimum detectable limit of the method has been
determined to be 3.4 milligrams (mg) of SO2 per cubic meter. Although no upper
limit has been established tests have shown that concentrations as high as
80,000 mg per cubic meter of SO2 can be collected efficiently in two midget
impingers, each containing 15 millilitres of 3 percent hydrogen peroxide at a
rate of 1.0 lpm for 20 minutes. Based on theoretical calculations, the upper
concentration limit in a 20 litre sample is about 93,300 mg per cubic meter.
Possible interference are free ammonia, water soluble cautions and fluorides. The
cautions and fluorides are removed by glass wool filters and an isopropanol
bubbler, and hence do not effect the SO2 analysis.

29
Apparatus

1) Probe
Borosilicate glass, or stainless steel, approximately 6 mm inside diameter,
with a heating system to prevent water condensation and a filter (either in stack
or heated outside stack) to remove particulate matter, including sulphuric acid
mist. A plug of glass wool is a satisfactory filter.

2) Bubbler and Impingers

One midget bubbler, with medium coarse glass frit and borosilicate or quartz
glass wool packed in top to prevent sulphuric acid mist carry over, and three 30
ml midget impingers. The bubbler and midget impingers must be connected in
series with leak free glass connectors. Silicon grease may be used, if necessary, to
prevent leakage.

3) Glass Wool
Borosilicate or quartz.

4) Stop Cock Grease

Acetone - insoluble heat stable silicon grease may be used, if necessary.

5) Temperature Gauge
Dial thermometer or equivalent, to measure temperature of gas leaving impinger
train to within 1° C.

6) Drying Tube

Tube packed with 6 to 16 mesh indicating type silica gel, or equivalent, to dry the gas
sample and to protect the meter and pump. If the silica gel has been used
previously, dry at 175° C for 2 hours. New silica gel may be used as received.

7) Valve

Fine control needle valve to regulate sample gas flow rate.

8) Pump
Use vacuum pump to pull the gas through sample train

30
9) Rotameter
Rotameter, or equivalent capable of measuring flow rate to within 2 % of the
selected flow rate about 1000 cc/min (1 lpm). Use 0.6 to 6 lpm rotameters on
control module.

10) Dry Gas Meter

Dry gas meter in dry gas meter module.

11) Barometer
Mercury, aneroid, or other barometer capable of measuring
atmospheric pressure to within 2.5 mm Hg (0.1 in. Hg). In many cases, the
barometric reading may be obtained from nearby meteorological station.
12) Reagents
Only AR grade reagents for sampling and analysis should be used. Other
specifications for sampling material is as given below.

13) Water
Deionized water

14) Isopropanol, 80 percent

Mix 80 ml of isopropanol with 20 ml of deionized, distilled water. Check

each lot of Isopropanol for peroxide impurities as follows:
Shake 10 ml of isopropanol with 10 ml of freshly prepared 10 percent potassium
iodide solution. Prepare a blank by similarly treating 10 ml of distilled water After
1 minute, read the absorbance at 352 manometers on a spectrophotometer. If
absorbance exceeds 0.1, reject alcohol for use.

15) Hydrogen peroxide, 3 percent

Dilute 30 percent hydrogen peroxide 1:9 ( v/v) deionized, distilled water (30
ml is needed per sample). Prepare fresh daily.

31
16) Potassium Iodide (KI) Solution : 10 percent

Dissolve 10.0 gram KI in deionized distilled water and dilute to 100 ml, prepare
when needed.

Specification for analytical materials are as given below :

1.Water : Deionized water

2.Isopropanol : 100 percent
3.Thorin Indicator : 1 - (0-arsenophenylazo)-2-naphthol-3, 6-dis-ulphonic acid, disodium
salt, or equivalent. Dissolve 0.20 gm in 100 ml of deionized, distilled water.
4.Barium Perchlorate Solution (0.01) N : Dissolve 1.95 gm of barium perchlorate
trihydrate Ba(CIO4)2. 3 H20 in 200 ml distilled water and dilute to 1 litre with
isopropanol. Alternatively, 1.22 gm of Bacl2. 2H2O may be used instead of the
perchlorate.
5.Sulphuric Acid Standard: (0.01) N: Standardised to 0.0002 N against
6.0.01 N NaOH which has been previously standardised against potassium acid
phthalate.

Procedure

1. Sampling
Preparation of Collection Train : Measure 15 ml of 80 % isopropanol into the
midget bubbler and 15 ml of 3 percent hydrogen peroxide into each of the first
two midget impingers. Leave the final midget impinger dry. Assemble the train
as shown in Fig. 3. Adjust probe heater to a temperature sufficient to prevent water
condensation. Place crushed ice and water around the impingers and bubbler.

2. Leak Check Procedure

A leak check prior to the sampling run is optional, however, a leak check after the
sampling run is mandatory.

The leak check procedure is as follows:

Temporarily attach a suitable (e.g. 0 to 3 lpm) rotameter to the outlet of the dry
gas meter and place a vacuum gauge at or near the probe inlet. Plug the
probe inlet, pull a vacuum of at least 250 mm Hg and note the flow rate as
indicated by the rotameter. A leakage rate not in excess of 2 % of the average
sampling rate is acceptable.

Note: Carefully release the probe inlet plug before turning off the pump.

32
3. Sample Collection

Record the initial dry gas meter reading and barometric pressure. To begin
sampling, position the tip of the probe at the sampling point. Adjust the sample
flow rate to a constant rate of approximately 1.0 litre/minute as indicated by the
rotameter. Maintain this constant rate (within +/- 10 %) during the entire sampling
run. Take readings (dry gas meter, and rotameter) at least every 5 minutes. Add
more ice during the run to keep the temperature of the gases leaving the last
impinger at 20° C or less. At the end of each run, turn off the pump, remove probe
from the stack and record the final readings.

4. Sample Recovery

Disconnect the impingers after purging. Discard the contents of the midget
bubbler. Pour the contents of the midget impingers into a leak-free polyethylene
bottle for shipment. Rinse the three midget impingers and the connecting tubes
with deionized distilled water, and add the washings to the same storage
container. Mark the fluid level, seal and identify the sample container.

5. Sample Analysis.

Transfer the contents of the storage container to a 100 ml volume with

deionized, distilled water. Pipette a 20 ml aliquot of this solution into a 250 ml-
Erlenmeyer flask, add 80 ml of 100 percent isopropanol and two to four drops of
thorin indicator, and titrate to a pink end point using 0.01 N barium perchlorate.
Repeat and average the titration volumes. Run blank with each series of samples.
Replicate titrations must agree within 1 percent or 0.2 ml whichever is larger.

6. Calculations

Carry out calculations, retaining at least one extra decimal figure beyond
that of the acquired data.

33
7. Nomenclature

C - Concentration of sulphur dioxide, dry basis converted to

SO2 standard conditions, mg/meter cube (at N.T.P.)

N - Normality of barium perchlorate titrant milliequivalents/ml.

Pbar - Barometric pressure.

Pstd - Standard absolute pressure, 760 mm Hg

Tm - Average dry gas meter temperature ° K

Tstd - Standard Temperature, 298° K

Va - Volume of sample aliquot- tritrated, ml

Vm - Dry gas volume as measured by the dry gas meter, m3

Vm(std) - Dry gas volume measured by the dry gas meter, corrected
to standard conditions, Nm3 (at N.T.P.)

Vsoln - Total volume of solution in which the SO2 sample is

contained, 100 ml.
V2 - Volume of barium perchlorate titrant used for the sample,
ml (average of replicate titration)

Vtb - Volume of barium perchlorate titrant used for the blank, ml

8. Dry sample gas volume, corrected to standard conditions

Tstd Pbar
Vm(std) = Vm --------- x ----------
Tm Pstd
K1 Vm Pbar
= ------------------------
Tm
Where
K1 = 0.38580 K/mm Hg

34
9. Sulphur dioxide concentration

Vsoln
K2(Vt-Vtb) N ----------
C Va
SO2 = ---------------------------------
Vm(std)

where

K2 = 32.03 mg/meq.

35
DETERMINATION OF NITROGEN OXIDE EMISSIONS FROM
STATIONARY SOURCES (EPA METHOD)

Alkaline - Permanganate / Calorimetric Method

1.Applicability, Principle, Interference, Precision, Bias and

Stability

1.1 Applicability

The method is applicable to the determination of NOx emissions from

fossil-fuel fired steam generators, electric utility plants, nitric acid plants, or
other sources as specified in the regulations. The lower detectable limit is 13
mg NOx/m3, as NO2 (7 PPM NOx) when sampling at 500 cc/ min for 1 hour. No
upper limit has been established : however, when using the recommended sampling
conditions, the method has been found to collect NOx emissions quantitatively up
to 1,782 mg NOx/ m3, as NO2 (932 PPM NOx).

1.2 Principle

An integrated gas sample is extracted from the stack and collected in alkaline
- potassium permanganate solution : NOx (NO + NO2) emissions are oxidised to NO2
and NO3. The NO3 is reduced to NO2 with cadmium, and the NO2 is analysed
colorimetrically.

1.3 Interferences

Possible interferences are SO2 and NH3. High concentrations of SO2 could
interfere because SO2 consumes MnO4 - (as does NOx) and, therefore could reduce the
NOx collection efficiency. However, when sampling emissions from a coal fire electric
utility plant burning 2.1% sulphur coal with no control of SO2 emissions,
collection efficiency was not reduced. In fact, calculations show that sampling 3000
PPM SO2 will reduce the MnO4 concentration by only 5 % percent if all the SO2
is consumed in the first impinger.

36
 NH3 is slowly oxidised to NO3 by the absorbing solution. At 100 PPM NH3 in
the gas stream an interference of 6 PPM NOx (11 mg NO2/m3) was observed
when the sample was analysed 10 days after collection. Therefore, the method may not
be applicable to plants using NH3 injection to control NOx emissions unless means
are taken to correct the results.

1.4 Precision

The within - laboratory relative standard deviation for a single

measurement is 2.8 and 2.9 % at 201 and 268 PPM, NO2, respectively.

1.5 Stability

Collected samples are stable for atleast 4 weeks.

2. Apparatus

2.1 Sampling and Sample Recovery

The sampling train is shown in fig. 3, and component parts are discussed
below.

Alternative apparatus and procedures are allowed provided acceptable

accuracy and precision can be demonstrated.

2.1.1 Probe

Borosilicate glass tubing, sufficiently heated to prevent water

condensation and equipped with an instack or outstack filter to remove particulate
matter (a plug of glass wool is satisfactory for this purpose). Stainless steel or
teflon tubing may also be used for the probe.

2.1.2 Impingers

Three restricted - orifice glass impingers, are required for each

sampling train. The impingers must be connected in series with leak-free glass
connectors. Stopcock grease may be used, if necessary, to prevent leakage.

37
2.2 Sample preparation and Analysis

2.2.1 Hot plate

Stirring type with 50 by 10 mm teflon coated stirring bars.

2.2.2 Beakers

400, 600 and 1000 ml capacities.

2.2.3 Filtering Flask

500 ml capacity with side arm

2.2.4 Buchner Funnel

75 mm ID, with spout equipped with a 13 mm ID by 90 mm long piece

of Teflon tubing to minimise possibility of aspirating sample solution during
filtration.

2.2.5 Filter Paper

Whatman GF/C. 7 cm diameter.

2.2.6 Stirring Rods

2.2.7 Volumetric Flasks

100, 200 or 250, 500 and 1000 ml capacity.

2.2.8 Watch Glass

To cover 600 and 1000 ml beakers.

2.2.9 Graduated Cylinders

50 and 250 ml capacities

38
 2.2.10 Pipettes

Class A.

2.2.11 pH Meter

To measure pH from 0.5 to 12.0

2.2.12 Burette

50 ml with a micrometer type stopcock. Place a glass wool plug in bottom of

burette. Cut of glass burette at a height of 43 cm from the top of plug. And have a
glass blower attach a glass funnel to top of burette such that the diameter of the
burette remains essentially unchanged. Other means of attaching the funnel are
acceptable.

2.2.13 Glass Funnel

73 mm ID at the top.

2.2.14 Spectrophotometer

Capable of measuring absorbance at 540 nm. One cm cells are adequate.

2.2.15 Metal Thermometers

Bimetallic thermometers, range 0 to 150° C

2.2.16 Culture Tubes

20 x 150 mm kimax No. 45048

39
3. Reagents

Use the best available grade.

3.1 Sampling

3.1.1. Water

Deionised distilled to confirm to ASTM specification

3.1.2. Potassium Permanganate

Potassium Permanganate 4 percent (w/w); Sodium Hydroxide 2 percent

(w/w) Dissolve 40 g of KMnO4 and 20 g of NaOH in 940 ml of water.

3.2 Sample Preparation and Analysis

3.2.1. Water

Same as in section 3.1.1

3.2.2 Sulphuric Acid

Concentrated H2SO4

3.2.3 Oxalic Acid Solution

Dissolve 48 g of Oxalic Acid (COOH)2. 2H2O) in water and dilute to 500

ml. Do not heat the solution.

3.2.4. Sodium Hydroxide 0.5 N

Dissolve 20 g of NaOH in water and dilute to 1 litre.

3.2.5 Sodium Hydroxide 10 N

Dissolve 40 g of NaOH in water and dilute to 100 ml.

3.2.6 Ethylenediamine Tetraacetic Acid (EDTA) Solution 6.5%

Dissolve 6.5 ml of EDTA (disodium salt) in water, and dilute
to 100 ml. Solution is best accomplished by suing a magnetic
stirrer.

40
 3.2.7 Column Rinse Solution

Add 20 ml of 6.5 percent EDTA solution to 960 ml of water

and adjust the pH to 11.7 to 12.00 with 0.5 N NaOH.

3.2.8 Hydrochloric Acid (HCL) 2N

Add 86 ml of concentrated HCL to a 500 ml volumetric flask

containing water, dilute to volume and mix well. Store in glass
stoppered bottle.

3.2.9 Sulphanilamide Solution

Add 20 g Sulphanilamide (melting point 165 to 167 deg.

C) to 700 ml water. Add, with mixing, 50 ml concentrated
phosphoric acid (85 percent), and dilute to 1000 ml. This
solution is stable for atleast one month, if refrigerated.

3.2.10 N - (1-Napthyl) - Ethylenediamine Dihydrochloride

(NEDA) Solution

Dissolve 0.5 g of NEDA in 500 ml of water. An aqueous

solution should have one absorption peak at 320 nm over
the range of 260 to 400 mm. This solution is stable for
atleast 6 months under laboratory conditions.

NEDA, showing more than one absorption peak over this

range, is impure and should not be used. This solution is
stable for atleast one month if protected from light and
refrigerated.

3.2.11 Cadmium

Prepare by rinsing in 2N HCL for 5 minutes until the colour

is silver grey. Then rinse the cadmium with water until
the rinsing are neutral when tested with pH paper.
Caution : H2 is liberated during preparation. Prepare in a
exhaust hood away from any flame.

41
3.2.12 NaNO2 Standard Solution Nominal Concentration,
100 µg NO2/ml.

Desiccate NaNO2 overnight. Accurately weigh 1.4 to 1.6 gm of

NaNO2 (essay of 97 % NaNO2 or greater), dissolve in water
and dilute to 1 litre. Calculate the exact NO2 concentration
from the following relationship :

Purity, % 46.01
µg NO2 / ml = gm of NaNO2 x ------------- x 10 x --------
3

1000 69.01

3.2.13 KNO2 Standard Solution

Dry KNO3 at 110 deg.C for 2 hrs. and cool in a dissector.

Accurately weigh 9 to 10 g of KNO3 to within 0.1 mg, dissolve
in water, and dilute to 1 litre. Calculate the exact NO3 -
concentrations from the following relationship :

62.01
µg NO3 -/ml = gm of KNO3 x 103 x -----------
101.10

This solution is stable for 2 months without preservative

under laboratory conditions.

3.2.14 Spiking Solution

Pipette 7 ml of the KNO3 standard into a 100 ml volumetric

flask, and dilute to volume.

3.2.15 Blank Solution

Dissolve 2.4 gm of KMnO4 and 1.2 gm of NaOH in 96 ml of
water. Alternatively, dilute 60 ml of KMnO4 / NaOH solution
to 100 ml.

42
4. Procedure

4.1 Sampling

4.1.1. Preparation of Collection Train

Add 200 ml of KMnO4 / NaOH solution (3.1.2) to each of

three impingers, and assemble the train as shown in Figure 11.

4.1.2 Leak - Check Procedure

A leak-check prior to the sampling run should be carried out :

a leak check after the sampling run is mandatory.

4.1.3 Check of Rotameter Calibration Accuracy (Optional)

Disconnect the probe from the first impinger, and connect

the filter (2.1.6). Start the pump, and adjust the rotameter
to read between 400 and 500 cc/ min. After the flow rate has
stabilised, start measuring the volume sampled, as recorded by
the dry gas meter (DGM), and the sampling time. Collect
enough volume to measure accurately the flow rate and
calculate the flow rate. This average flow rate must be
less than 500 cc/ min. For the sample to be valid : therefore,
it is recommended that the flow rate can be checked as
above prior to each test.

4.1.4 Sample Collection

Record the initial DGM reading and barometric pressure.

Determine the sampling point or points according to the
appropriate regulations. Position the tip of the probe at the
sampling points, connect the probe to the first impinger,
and start the pump. Adjust the sample flow to a value
between 400 to 500 cc/ min.

43
Caution : Higher flow rates will produce low results. Once adjusted, maintain a
constant flow rate during the entire sampling run. Sample for 60 minutes. For
relative accuracy (RA) testing of continuous emission monitors, the minimum
sampling time is one hour, sampling 20 minutes at each traverse point. (Note
when the SO2 concentration is greater than 1200 PPM, the sampling time may
have to be reduced to 30 minutes to eliminate plugging of impinger orifice with
MnO2. For RA tests with SO2 greater than 1200 PPM, sample for 30 minutes (10
minutes at each point). Record the DGM temperature, and check the flow rate
atleast every 5 minutes. At the conclusion of each run, turn off the pump, remove
probe from the stack and record the final readings. Divide the sample volume by
sampling time to determine the average flow rate. Conduct a leak-check as in
Section. 4.1.2 If a leak is found, void the test run or use procedures acceptable
to the Administrator to adjust the sample volume for the leakage.

4.2 Sample Recovery

Disconnect the impinger. Pour the contents of the impingers into a 1 litre
polyethylene bottle using a funnel and a stirring rod (or other means) to prevent
the spillage. Complete the quantitative transfer by rinsing the impingers and
connection tubes with water until the rinsing that are clear to light pink and add
the rinsing to the bottle. Mix the sample, and mark the solution level. Seal and
identify the sample container.

4.3 Sample Preparation for Analysis

Prepare a Cadmium reduction column as follows : Fill the burette with water. Add
freshly prepared Cadmium slowly with tapping until no further settling occurs. The
height of the cadmium column should be 39 cm. When not in use, store the column
under rinse solution (Note - The column should not contain any bands of
cadmium fines. This may occur if regenerated column is used and will greatly reduce
the column lifetime.)

44
 Note the level of liquid in the sample container, and determine whether
any sample was lost during shipment. If a noticeable amount of leakage has
occurred, the volume lost can be determined from the difference between initial and
final solution levels, and this value can be used to correct the analytical result.
Quantitatively transfer the contents to a 1 litre volumetric flask, and dilute to volume.

Take a 100 ml aliquot of the sample and blank ( unexposed KMnO4⁄ NaOH)
solutions, and transfer to 400 ml beakers containing magnetic stirring bars. Using a
pH meter, add concentrated H2SO4, with stirring until a pH of 0.7 is obtained.
Allow the solutions to stand for 15 minutes. Cover the beakers with watch
glasses, and bring the temperature of the solution to 50 ° C. Keep the
temperature below 60° C. Dissolve 4.8 g of oxalic acid in a minimum volume of
water, approximately 30 ml, at room temperature. Do not heat the solution. Add this
solution slowly, in increments until the KMnO4 solution becomes colourless. If
the colour is not completely removed, prepare some more of the above oxalic
acid solution, and add until a colourless solution is obtained. Add an excess of
oxalic acid by dissolving 1.6 g of oxalic acid in 50 ml of water and add 6 ml of
this solution to the colourless solution. If suspended matter is present, add
concentrated H2SO4 until a clear solution is obtained.

Allow the samples to cool to near room temperature being sure that the
samples are still clear. Adjust the pH to 11.7 to 12.0 with 10 N NaOH.
Quantitatively transfer the mixture to a Buchner funnel containing GF/C filter
paper and filter the precipitate. Filter the mixture into a 500 ml filtering flask.
Wash the solid material four times with water. When filtration is completed wash the
Teflon tubing quantitatively transfer the filtrate to a 500 ml volumetric flask, and
dilute to volume. The samples are now ready for cadmium reductions. Pipette a 50 ml
aliquot of the sample into a 150 ml beaker and add a magnetic stirring bar. Pipette
1.0 ml of 6.5 % EDTA solution and mix.

45
 Determine the correct stopcock setting to establish a flow rate of 7 or 9
ml/min of column rinse solution through the cadmium reduction column. Use a 50 ml
graduated cylinder to collect and measure the solution volume. After the last of the
rinse solution has passed from the funnel into the burette, but before air entrapment
can occur, start adding the sample and collect it in a 250 ml graduated cylinder,
Complete the quantitative transfer of the sample to the column as the sample
passes through the column. After the last of the sample to the column as the
sample passes through the column. After the last of the sample has passed from the
funnel into the burette, start adding 60 ml of column rinse solution, and collect the
rinse solution until the solution just disappears from the funnel.

Quantitatively transfer the sample to a 200 ml volumetric flask (250 ml may be

required), and dilute to volume. The samples are now ready for NO2 analysis. (Note :
Both the samples and blank should go through this procedure. Additionally, two
spiked samples should be run with every group of samples passed through the
column. To do this, prepare two additional 50 ml aliquots of the sample
suspected to have the highest NO3 concentration, and add 1 ml of the spiking
ssolution to these aliquots. If the spike recovery or column efficiency (see 6.2.1) is below
95 percent prepare a new column and repeat the cadmium reduction.

4.4 Sample Analysis

Pipette 10 ml of a sample into a culture tube. (Note - Some test tubes give a high
blank NO2 - value but culture tubes do not) Pipette in 10 ml of sulphanilamide
solution and 1.4 ml of NED solution. Cover the culture tube with parafilm, and mix
the solution. Prepare a blank in the same manner using the sample from treatment
of the unexposed KMnO4/ NaOH solution (3.1.2). Also prepare a calibration
standard to check the slope of the calibration curve. After a 10 minute colour
development interval measure the absorbance at 540 nm against water. Read gm NO2
/ ml from the calibration curve, if the absorbance is greater than that of highest
calibration standard, pipette less than 10 ml, of sample and enough water to make the
total sample volume 10 ml, and repeat the analysis. Determine the NO2 concentration
using the calibration curve in section 5.

46
5. Calibration Curve for Spectrophotometer

Dilute 5.0 ml of the NaNO2 standard solution to 200 ml with water. This solution
nominally contains 25 µg NO2/ml. Use this solution to prepare calibration standards
to cover the range of 0.25 to 3.00 µg NO2/ ml. Prepare a minimum of three
standards each for the linear and slightly non-linear (described below) range of
the curve. Use pipettes for all additions.
Run standards and a water blank as instructed in 4.4. Plot the net absorbance
Vs µg NO2-/ml. Draw a smooth curve through the points. The curve should be linear up
to an absorbance of approximately 1.2 with a slope of approximately 0.53
absorbance units/µg NO2/ml. The curve should pass through the origin. The curve is
slightly non-linear from an absorbance of 1.2 to 1.6

6. Calculations

Carry out calculations retaining at least one extra decimal figure beyond that
of the acquired data. Round off figures after final calculation.

6.1 Sample volume, Dry Basis Corrected to Standard Conditions

T std Pbar Vm Pbar

Vm(std) = Vm XY ------- --------- = K1 XY -------------
Tm Pstd Tm

Where

Vm(std) = Dry as volume measured by the dry gas meter,

corrected to standard conditions, dscm
Vm = Dry as volume as measured by the dry gas meter,
dcm.
Y = Dry as meter calibration factor
X = Correction factor for CO2 collection

100
-------------------------
100 - % CO2 (v/v)

Pbar = Barometric pressure mm Hg.

Pstd = Standard absolute pressure 700 mm Hg.

Tm = Average Dry Gas Meter absolute temperature,°K.

Tstd = Standard absolute temperature, 293° K.

K1 = 0.3858 K./mm H.

47
6.2 Total µg NO2 per sample

6.2.1 Efficiency of Cadmium Reduction Column

Calculate this value as follows :

(x - y) 200 269.6 (x-y)

E = --------------------- = ------------------
S x 1.0 x 46.01 6
--------
62.01

Where:
E = Column Efficiency, unit less

x = Analysis of spiked sample, µg NO2 /ml.

y = analysis of unspiked sample µg NO2 /ml.

200 = Final volume of sample and blank after passing through the
column ml.

S = Concentration of spiking solution µg NO2 / ml.

1.0 = Volume of spilling solution added ml.

46.01 = µg NO2 / µ mole

62.01 = µg NO2 / µ mole

6.2.2 Total µg NO2

(S-B) 500 1000 (2 x 104 ) (S-B)

m = ------- x 200 x ------ x -------- = ---------------------
E 50 100 E

48
 Where

m = Mass of NOx as NO2 in sample µg.

S = Analysis of sample. µg NO2 -/ml.

B = Analysis of blank µg NO2-/ml

500 = Total volume of prepared sample ml.

50 = Aliquot of prepared sample processed through Cadmium

column ml.

100 = Aliquot of KMnO4 / NaOH Solution. Ml.

1000 = Total volume of KMnO4 / NaOH solution ml.

6.3 Sample Concentration

m
C = K2 ------------
Vm (std)

Where :

C = Concentration of NO2 as NO2 dry basis.

-3
K2 = 10 mg/µs.

6.4 Conversion Factor

1.0 PPM NO = 1.247 mg NO/m3 at STP

1.0 PPM NO2 = 1.912 NO2/ m3 as STP
1 Ft = 2.832 x 10-2 m3
1000 mg = 1 gm

49
7. TECHNICAL SPECIFICATIONS OF NETEL'S STACK
MONITORING KIT

1.General
1.Stack velocity range : 0 to 30 mtrs. / sec.
2.Stack temperature range : 0 to 600 ° C
3.Particulate flow meter : At 0 to 100 lpm.
4.Filter paper (Thimble) : Collection of particulate down to 0.3 µ
5.Gaseous flow meter : at 0 to 6 lpm, collection on a set of
Impingers containing selective reagents

1.Pitot Tube
Modified S-type Pitot tube fabricated from S.S. 304 as per US EPA regulations /
CPCB Doc. No. Emission Regulation (Dec. 1985). Individually calibrated from I. I. T.,
Mumbai

1.Sampling Probe
Fabricated from S.S. 304 tube (I.D. more than 15 mm) standard length 1 mtr, other
lengths optional.

1.Nozzles
A set of 3 nozzles of SS 304 with I.D. 1/4", 3/8" & 1/2" (other bore sizes available on
request)

1.Thimble Holder
Tapper design thimble holder of S.S. suitable to hold cellulose /
glass fibre thimble.

1.Thermocouple
Cr/Al Thermocouple sensor 1mtr. Long with digital LCD readout to measure stack
temperatures from 0 to 600OC covering with S.S. casing.

1.Control Module
Fabricated out of fibre glass with baked stove-enamel finish for with suitable
arrangements for housing stop watch, manometer, rotameters, temperature read
out, etc.

50
1.Inclined-cum-vertical Manometer

Fabricated out of solid acrylic sheets with resolution of 0.25 mm spirit

level attached for levelling, velocity range 0 to 30 meters/Sec.

1.Rotameters

Glass tube rotameters with 0 to 100 lpm of particulate sampling

and 0 to 6 lpm for gaseous monitoring.

10. Stop - Watch

LCD read-out stop watch for 0 to 120 minutes. With 1 sec.

resolution and hold facility.

11. Impinger Tubes

4 nos. 120 ml and 2 nos. 250 ml capacity impinger tubes. Double

walled impinger tube box for keeping impinger tubes at low
temperature.

12. Vacuum Pump

Rotary design, mono-block type vacuum pump with a capacity of 0 to 100 lpm gas
flow, single phase motor operating at 220 V.

13. Dry Gas Meter

Dry Gas meter with the facility of measuring temperature and static pressure of the
gas. Minimum read-out of 1 ltr. in separate glass fibre box.

14. Hose

5Hoses (4 PVC and 3 SS braided ) with suitable end connections.

15. Tools

The kit contains the essential tools required for connecting various components,
silicon grease, red oil for manometer etc.

------×-----

51