METHODS OF SAMPLING

from Stationary Sources

SOURCE
EMISSION
TESTING
 Purposes of Stack Sampling
• To determine compliance with emission
standards.
• To determine the quantity and type of
pollutants emitted from a specific source.
• To determine the efficiency of the pollution
control device.
• To determine emission factors for use in
emission inventories.
Stack test can be divided into 3
categories
a) isokinetic sampling (generally used for
PM)
b) batch sampling (for gases) &
c) continuous automatic sampling &
analysis
 EMB requirements for compliance
testing

• The IRR of RA-8749 list NESSAP

• Associated w/ these Emission Standards are
Methods of Sampling and Analysis
• The sampling methods in the IRR are Methods
for Stationary Source Sampling of the USEPA
• Sec. 4 of the IRR provides sampling methods
approved by the Bureau as equivalent to this
methods
• Promulgated test methods have been published
in the USEPA federal Register as final rules
 National Emission Standards for Source Specific Air
Pollutants (NESSAP)

Particulates 1. Fuel Burning Equipment USEPA Methods 1 Gravimetric per

a) Urban and industrial area 150 through 5 sampling method
b) Other area 200
2) Cement Plants (Kilns, etc.) 150
3) Smelting Furnaces 150
4) Other stationary sources 200

Sulfur Oxides 1) Existing sources USEPA Methods

a) Manufacture of sulfuric 2,000 as SO3 1 through 4 and 6 or As per sampling
acid and sulfonation 8 as appropriate method
process
b) Fuel burning equipment 1,500 as SO2
c) Other stationary 1,000 as SO3
sources
2) New sources
a) Manufacture of sulfuric 1,500 as SO3
acid and sulfonation
process
b) Fuel burning equipment 700 as SO2
c) Other stationary 200 as SO3
sources
 Before conducting a test
• a pre-site survey should be
conducted
- to check the source to be tested if it
complies w/ method 1 std. such as
sampling port, monorails support,
access ladder, platform installations,
equipment needed during sampling,
electrical outlet, safety, etc.
- plant/facility operations
Process & Operational data requirements
Prior to the conduct of source test, testing agency
should request the facility operator to provide
the following information:
• The operating parameters used to monitor or regulate
the processes or installations that generate the
emissions
• The values of this parameter that indicate normal
operations
• Details of any associated emission control equipment,
including design capacities & efficiencies
• The output of any CEMs
• They should further advice the operator:
- to ensure that processes are operated at an appropriate load
- to use the same type of fuel
- to use the blend that is expected to produce the highest
emissions
 Equipment Calibration
• test results from from a stack emission test are
meaningless w/out calibration of the equipment
components
• w/out calibration, sampling cannot be verified as
having been conducted isokinetically
• components w/c require calibration are:
1. Dry Gas Meter & Orifice Tube
2. Thermocouples & Digital Temperature Indicator
3. Pitot Tube
4. Sampling Nozzels
5. Probe Heater Systems.
 Component Acceptable Limits Frequency
Dry Gas Meter Yi=Y+ 0.05Y Semiannual
Initial 5-point
Post-test 3-point Y=Y+ 0.05 Yave After each field test
Orifice Tube H@=46.7 +6.4mm W/ DGM/Semiannual
H2O(1.84+ 0.25”H2O)
Thermocouples Stack: +1.5% deg K After each field test/
& Digital DGM/P/F:+ 3 deg C Post Test Check
Indicator Exit: + 1 deg C
Pitot Tube Inspect-should be After each field test
level/sharp & not
deformed
Sampling Ave of 3 inner dia.: Quarterly
Nozzles 0.1mm
Probe Heater Capable of maintaining Quarterly
System 120 deg C +14 deg C
 Source Testing Safety
Safety is an attitude that must instilled in all
sample team members. A variety of hazards
must be carefully considered before beginning a
source test.
Hazards which need to be considered are the ff:
• Working at heights or on a temporary platforms
• Exposure to toxic, corrosive or hot gasses
• Electrical hazards
• Trip hazards from cables
• Noise and/or heat from plant equipment
• Objects falling from work platform
• Flammability hazards
• Exposure to the elements
 Safety Organization
Responsibility for Safety
Each has a role to play in safety including:
Source Test Leaders are responsible for:
– day to day implementation of safety procedures,
– supervision of staff,
– safety training specific to source testing; and
– investigation of any accidents or near misses that occur during
testing.
Individual staff are responsible for:
– to arrive fit to work;
– following the established source testing safe working
procedures,
– to act responsibly and carefully at all times; and
– use the supplied personal protective equipment (PPE).
 Introduction
What is Source Testing?

• only provides the “snap shot” of the emission

from a source at the time of testing
• a sample is drawn from the stack in conditions
that represent those in the source
• It is performed to collect a representative
sample from a specific source such as from a
stack or duct
 How the sample be
representative?

By means of collecting sample in

isokinetic sampling condition
What is Isokinetic sampling
condition?

The velocity of flue gas in the nozzle is

equal to the velocity of stack gas and
particulate mixture
Definition of Isokinetic Sampling

Super Isokinetic Under Isokinetic Isokinetic

 METHOD 1

Sample and Velocity Traverses for

Stationary Sources
Principle and Applicability

A measurement site where the effluent stream is

flowing in known direction is selected, and the
cross-section of the stack is divided into a
number of equal areas.
Sampling port installations
Condition to meet for isokinetic
sampling

• The stack inside diameter is more

than 12 inches or 30 cm
• Sampling location must be at least
0.5 x stack diameter upstream and 2
x diameter downstream from the
nearest disturbance
• Flow of flue gas is not cyclonic
 Procedure
• Selection of measurement site
• Find the number of traverse point
• Compute the distance of equal areas
• Mark the probe to denote the proper
distance of each sampling point
Measurements
 Traverse point location
Diameters No. of traverse points
A B
2 8
A>2Di
12
1.8 7
16
1.5 6
20
B>8Di 1.3 5
Di
24
0.5 2

Draw horizontal lines through A & B

diameters & use the higher no. of points.
-If more than 8 & 2 dia. & if duct dia. less
than 0.6 meter use 8 or 9 points
 Cyclonic flow check

probe angle locator pitot tube

 METHOD 2

Stack Gas Velocity and

Volumetric Flow Rate
Principle and Applicability

• The average velocity head is measured

using Type S pitot tube;
• Applicable of measuring average velocity
of a gas stream and for quantifying gas
flow;
• The procedure cannot be used if fail to
meet the criteria of Method 1.
 Procedure
• Inspect or calibrate Type S pitot tube
• Set up the apparatus
• Leak check the manometer connected to
Type S pitot tube
• Measure the cyclonic flow
• Measure the velocity head and
temperature at each traverse point
• Measure the static pressure
 Pitot tube Inclined manometer

Angle locator
Note: Purge pitot/sample lines then leak check the + & - side of
the pitot tube before taking measurements (delta H)
 METHOD 3

Determination of dry Molecular

Weight
 CO2 and O2 determination
• Measurement of dry molecular weight of
the stack gas in order to calculate the
stack gas volumetric flow rate
• use to correct to a specific CO2 & O2
concentration basis
Equipment used: Orsat/Fyrite Analyzer, sample
pump & tedlar bag
Applicability

• Determination of carbon dioxide and

oxygen content of flue gas and dry
molecular weight from the fossil fuel
combustion process.
Principle

A gas sample is extracted from the stack

and the percent CO2 and percent O2 is
analyzed using either an Orsat or a Fyrite
analyzer.
 Procedure
• Leak check the flexible bag
• Place tip of the probe inside the stack
• Draw a sample into the flexible bag and
immediately analyze it for %CO2 and %O2.
• Repeat the sampling, analysis, and calculation
procedures until the dry molecular weights of
any three grab samples differ from their mean by
no more than 0.3 g/g-mole
Tedlar bag Orsat analyzer
Meter console
Fyrite analyzer
Probe
 METHOD 4

Determination of Moisture Content of Stack

Gases
Principle

A gas sample is extracted at the stack with

a constant rate; moisture is removed from
the sample and determined either
volumetrically or gravimetrically.
A. Preliminaries
• Follow Method 1 & 2
• Place known volume of water in the first
two impingers
• Leave the third impinger blank
• On the fourth impinger place silica gel
about 200 to 250 gram
B. Sampling
• Set up the sampling train.
• Turn on the probe heater and the filter heating system to
temperatures of about 120 deg.C +/- 10 deg.C; allow
time for the temperatures to stabilize. Place crushed ice
in the ice bath container.
• Optional: Leak-check the sampling train from the inlet of
the first impinger inlet or, the filter holder.
• Position the probe tip at the first traverse point. Sample
at a constant (10%) flow rate. Record data.
• Select a total sampling time such that a min. total
volume of 0.6 scm at a rate no greater than 0.021
cum/min
B. Sampling
• Traverse the cross section, sampling at
each traverse point for an equal length of
time.
• Add more ice and, if necessary, salt to
maintain  20 deg.C at the silica gel outlet.
• At completion of sampling, disconnect the
probe from the filter holder (or from the
first impinger).
• Mandatory: Leak-check the sampling train.
C. Sample Recovery
• Measure the volume of the moisture
condensed to the nearest mL.
• Determine the increase in weight of the
silica gel (or silica gel plus impinger) to
0.5g. Record data.
• Calculate the moisture percentage.
Weighing of Impingers
 METHOD 5

Determination of Particulate Emissions

from Stationary Sources
Method 5 Sampling Train
Principle

Particulate matter is withdrawn isokinetically

from the stack and collected on a glass
fiber filter maintained at a temperature
range of 120+/-14oC.
A. Pretest Preparations
• Weigh several 200- to 300-g portions of
silica gel in air-tight containers to  0.5g.
• Check filters visually against light for
irregularities and flaws or pinhole leaks.
• Dessicate the filters at 20  5.6oC and
ambient pressure for  24hr, and weigh at
intervals of  6hr to a constant weight.
B. Preliminary Determinations
• Select the sampling site and the number of
sampling points
• Determine the stack pressure,
temperature, and the range of velocity
heads
• Optional: Leak-check the pitot lines
• Determine the moisture content
• Determine or estimate the dry molecular
weight
B. Preliminary Determinations
• Select a nozzle size. Do NOT change nozzle
size during the sampling run
• Calculate the proper differential pressure gauge
• Select a suitable probe liner and probe length
such that all traverse points can be sampled
• Select the total sampling time and standard
sample volume specified in the test procedure to
the specified industry. Select equal sampling
times of  2min per point
C. Preparation of Collection Train
• During preparation and assembly of the
sampling train, keep all openings covered to
avoid contamination
• Prepare impingers as follows:
- Impingers 1 and 2: 100mL water in each
- Impinger 3: Empty.
- Impinger 4: 200 to 300 g of preweighed silica
gel.
• Place the silica gel container in a clean place
C. Preparation of Collection Train
• Using a tweezer or clean disposable surgical
gloves, place filter in the filter holder
• Mark the probe with heat resistant tape to
denote the proper distance into the stack or duct
for each sampling point
• Setup the train. Turn on and set probe and filter
box heaters. Placed crushed ice around
impingers
• Optional: Leak-check the sampling train
D. Sampling
• Record the initial dry gas meter (DGM) reading.
• Remove the nozzle cap, verify that the filter and
probe heating systems are up to temperature,
and check pitot tube, temperature gauge, and
probe alignments and clearances.
• When the probe is in position, block off the
openings around the probe and porthole.
• Traverse the stack cross-section
 barometer

Hot box Cold box Meter console

E. Sample Recovery
• Place 200mL acetone from the wash bottle being used
for cleanup in a glass sample container
• Inspect the train prior to and during disassembly, and
note any abnormal conditions
• Container No. 1 (filter)
- Using a pair of tweezers and/or clean disposable surgical gloves,
carefully remove the filter from the filter holder, and place it in its
identified petri dish container.
- Using a dry Nylon bristle brush and/or a sharp-edged blade,
carefully transfer to the petri dish any PM and/or filter fibers that
adhere to the filter holder gasket. Seal the container
E. Sample Recovery
• Container No. 2 (Acetone Rinses)
Recover particulate matter from the probe nozzle, Swagelock fitting,
probe liner, front half of the filter holder, and cyclone, and recover
all rinses in a glass container as follows:
- Rinse with acetone, brush with a Nylon bristle brush, and rinse with
acetone until there are no visible particles. Make a final acetone
rinse.
- For probe liner, repeat rinse, brush, rinse sequence at least 3x for
glass liners, and 6x for metal liners.
- Make a final rinse of the brush with acetone.
- After completing the rinse, tighten the lid on the sample container.
Mark the height of the fluid level. Label the container.
Particulate Matter Sample Recovery
PARTICULATE MATTER
EPA Method-5/6
- for determination of PM & SO2
Sample recovery for SO2
• Pour the contents of the 1st and 2nd
impinger into a storage container.
• Rinse the 1st, 2nd, & 3rd impingers and
the connecting tubes with de-ionized
water, and add the washings to the same
storage container.
• Seal and identify the storage container
• Properly label the samples & mark the
sample level.
Sulfur Dioxide Sample Recovery
 Sulfur Dioxide Sample Preparation
SAMPLE DILUTED SAMPLE ADDITION OF INDICATOR

1.0 L

AFTER ADDITION
Sulfur Dioxide Sample Preparation
TITRATION

0.01 N BaCl2 . .2H2O

ENDPOINT: SALMON PINK

 METHOD 7

Determination of Nitrogen Oxides Emissions

from Stationary Sources
Method 7 Sampling Train
Principle

A grab sample is collected in an evacuated

flask containing a dilute sulfuric acid-
hydrogen peroxide absorbing solution and
are measured colorimetrically using
phenoldisulfonic acid procedure.
Procedure
• Turn the flask valve and the pump valve to
their “evacuate” positions.
• Evacuate the flask valve to 75 mm Hg or
3 in Hg.
• Turn the pump valve to its “vent” position.
• Turn off the pump when the 75 mm Hg or
3 in Hg achieved.
Procedure
• Check for leakage, any variation greater
than 10 mm Hg or 0.4 in Hg over a period
of 1 min is not acceptable.
• 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.
Procedure
• If condensation occurs, heat the probe and
purge until the condensation disappear.
• Turn the pump valve to its “vent” position.
• Turn the flask valve clockwise to its
“evacuate” position, record the difference
in manometer reading.
• Immediately turn the flask valve to the
“sample” position.
Procedure
• Allow the gas to enter the flask until
pressures in the flask and sample line are
equal. This will usually require about
15sec.
• After collecting the sample, turn the flask
valve to its “purge” position, disconnect the
flask from the sampling train.
• Shake the flask for at least 5 min
Procedure
• Record the volume of flask flask valve,
(Vm) flask temperature, (Tf) , absolute
internal pressure (Pi), where: absolute
internal pressure is equal to the barometric
pressure less the manometer reading.
Procedure
• If the gas being sampled contains
insufficient oxygen for the conversion of
NO to NO2, then oxygen may be introduce
by terminating sampling with a minimum of
50 mm Hg or 2 in Hg vacuum remaining in
the flask, vent the flask to the atmosphere
until the flask pressure is almost equal to
atmospheric pressure.
Sample Recovery
• Let the flask set for a minimum of 16 hours
and then shake the contents for 2 mins.
• Connect the flask to a mercury filled U-
tube manometer.
• Open the valve from the flask to the
manometer and record the flask
temperature, barometric pressure, and
absolute internal pressure.
Sample Recovery
• Transfer the contents of the flask to a
polyethylene bottle.
• Rinse the flask twice with 5 ml portions of
the deionized distilled water and add the
rinse water into the sampling bottle.
• Adjust the pH to bet. 9-12 by adding
sodium hydroxide.
• Label the container.
Nitrogen Oxides Sample Preparation
EVAPORATING DISH

WATER BATH

CALIBRATION STANDARDS
 Nitrogen Oxides Sample Preparation

UV-VIS SPECTROPHOTOMETER CUVETTES

 METHOD 10

Determination of Carbon Monoxide

Emissions from Stationary Sources
Tedlar bag
Meter console
Non Dispersive Infrared Analyzer
(NDIR)
 METHOD 23

Determination of Dioxins and Furans

Emissions from Stationary Sources
Principle

A sample is withdrawn isokinetically from the

gas stream and collected in the sample
probe, on a glass fiber filter, and on a
packed column adsorbent material.
Pre-test Preparation

Same as procedure outlined in Method 5

Glassware Preparation
• All glassware shall be cleaned by soaking
for several hours in a chromic acid
cleaning solution.
• Special care shall be devoted to the
removal of silicone grease sealants on
ground glass connections of used
glassware.
• Rinse all the glassware’s by acetone,
followed by methylene chloride and finally
by toluene
Sampling Train Preparation
• Place 100 ml of water in the second and
third impingers, leave the first and fourth
impinger empty.
• Place 200 to 300 g of silica gel in the fifth
impinger
• Assemble the sampling train
• Turn on the adsorbent module and
condenser coil recirculating pump
• Make sure the required temperature is
achieved before sampling is commenced.
• Temperature at the XAD-2 must not
exceed 20 oC
• Sampling train operation is the same as
Method 5
Sample Recovery
• Container No.1 Remove the filter from the
filter holder and place it in petri dish.
• Adsorbent Module Remove the module
and tightly cap both ends, label it and
store it on ice for transport to the
laboratory.
• Container no. 2 Wash the nozzle, probe
liner and front half of the filter holder three
times by acetone and then three times
with methylene chloride.
• Container No. 3 Wash the nozzle, probe
liner and front half of the filter holder three
times by toluene
Actual Method 23 Sampling
 METHOD 29
Determination of Heavy Metals
Emissions from Stationary
Sources
Principle
• A stack sample is withdrawn isokinetically,
particulate are collected on a heated filter,
and gaseous emissions are then collected
in an aqueous acidic solutions.
Pre-test Preparation

Same as procedure outlined in Method 5

Glassware Preparation
• All glassware shall be cleaned by rinsing
with hot water, then wash with hot soapy
water followed by rinsing 3 times with tap
water.
• Soak all glassware in a 10% (V/V) nitric
acid solution for a minimum of 4 hours,
then rinse 3 times with water and finally
rinse with acetone
Sampling Train Preparation
• Place 100 ml of HNO3/H2O2 solution in
each second and third impingers
• Place 100 ml of KMnO4 absorbing solution
in each of the fifth and sixth impingers
• Place 200 to 300 g of silica gel to the last
impinger
• Leave the fourth impinger blank
• First impinger will be eliminated if the
moisture content is less than 100 ml
Sampling

• Assemble the sampling train and follow

the sampling procedure of Method 5
Sample Recovery
• Container No.1 Remove the filter from the
filter holder and place it in petri dish.
• Container no. 2 Wash the nozzle, probe
liner and front half of the filter holder three
times by acetone
• Container no. 3 Wash the nozzle, probe
liner and front half of the filter holder
thoroughly with a total of 100 ml of 0.1N
HNO3
• Container No. 4 Rinse the impingers 1
through 3 as well as the back half of filter
holder with 100 ml of 0.1N HNO3
• Container No. 5A Rinse the impinger 4
with 100 ml of ).1N HNO3
• Container No. 5B Rinse impingers 5 & 6 of
100 ml fresh KMnO4 solution 3 times
• Container No. 5C If deposits remains on
the impinger surfaces, wash them with
25ml of 8N HCl
Mabalos!!!