Stack Emission Testing Workshop

CTS Chemical & Technical Services

Cairo - Egypt
USEPA METHOD 5 & 17
Particulates
 Selection of USEPA M5 or 17
• Both methods can are used for the determination of
Total particulate Matter(TPM)/Total Suspended
Particulate(TSP)
• Captures Solid Phase Particulate ONLY…
• Like all Isokinetic methods, it incorporates USEPA
Methods 2, 3A and 4.
• USEPA Method 5 is an extractive OUT-STACK method
which means that the gas is extracted to be captured
on a filter outside the stack.
• USEPA Method 17 is an IN-STACK method which means
that the filter apparatus is placed in-situ of the stack in
direct contact with the gas.
 Selection of USEPA M5 or 17
It is important to note that the results generated can be
different due to method bias. Both results reported are
correct in their own right.

This can occur in high temperature stacks (especially with

significant levels of HF, HCl and NH3)where the pollutant is
in a gaseous state in the stack but when it cools it becomes
a solid. If in-stack monitoring is done then the particulate
passes through the filter and is not captured, conversely
the extractive sampling filter is at 120oC so may capture
more.
 Condensable Particulates
Definition:
Condensable PM (CPM) means material that is vapor
phase at stack conditions, but condenses and/or reacts
upon cooling and dilution in the ambient air to form solid
or liquid PM immediately after discharge from the stack.
Note that all condensable PM is assumed to be in the
PM2.5 size fraction.

USEPA Method 202 – Dry Impinger Method is the most

commonly used to determine condensable particulate
matter. It is operated in conjunction with either Method 5
or 17 in order to get a true Total Particulate Matter
Concentration.
 Particle Size Determination
Method – USEPA Method 201

• Uses an In-stack Cyclone Filter head to separate

different sized particles.
• Unlike other Isokinetic testing, a single steady
calculated flow rate is used to sample at all points
across the duct.
• Requires a larger port size (6’’ to insert equipment).
• Can determine TPM, PM10 and PM2.5 results.

• Alternative methods include Particle Size Diffraction

analysis of the filters and the use of a Cascade
Compactor.
 Selection of USEPA M5 or 17
USEPA Method 17 Pros and Cons

• Cannot use in wet stacks with temperatures <120oC

• Easier to use than Method 5 with less equipment
required.
• Samples particulate at stack conditions
• Improved samples recovery as no probe washing
required. Only nozzle rinse.

USEPA Method 5 Pros and Cons

• Full equipment including hot probe required

• Can change the composition of particulate state
• Can use to sample in any stack conditions
• Greater chance of in-accurate probe wash recovery
 Selection of USEPA M5 or 17
Particulate Abatement Technology

• Wet Scrubber
Useful for high particulate loaded gas streams and high
acid gas content.
Use Method 5 extractive sampling due to low stack
temperature and high liquid moisture content
Effectiveness of removal >95%
 Selection of USEPA M5 or 17

• Bag House Filtration

• Most Commonly used to remove particulates from various
process gas streams.
• Can use Method 5 or 17
• Effectiveness of removal >99% IF PROPERLY MAINTAINED!
 Selection of USEPA M5 or 17
Particulate Abatement Technology

• Electrostatic Precipitator(ESP)
Can handle high volume air flows and commonly used in
large scale industrial process such as cement kilns or
particle board manufacture.
Can use either Method 5 or 17 unless it is a Wet
Electrostatic Precipitator(WESP), in which case Method 5.
Effectiveness of removal >95%
 USEPA METHOD 5
• Applicability Statement
• Principle
• The Orifice Meter
• Isokinicity
• The Isokinetic Calculation (I)
• Delta H Calculation (ΔH)
• Ideal Nozzle Size Calculation (Dn)
• k-factor Calculation (k)
• Sampling Equipment List
a)Dry gas meter – console
b)Probe and attachments
c)Pitot Tubes – specifications
d)Filter Holder – specifications
e)Heating - specifications
f)Condenser - specifications
 USEPA METHOD 5
• Sampling
a) Preliminary Determinations
b)Sample Train Preparation
c) Pre & Post Sampling Leak-Check
d)Operating the sample Train
e)Sample Recovery
 Why do USEPA Method 5?
To determine isokinetically the concentration of particulate
in the stack gas stream.

Applicability Statement

This method is applicable for determination of particulate

emissions from stationary sources. It is also the basis for all
isokinetic techniques.
 Principle

Particulate matter is withdrawn isokinetically from the

source and collected on a glass fibre filter maintained at
120oC +/- 14oC.

The particulate mass which includes any material which

condenses at or above filtration temperature is determined
gravimetrically.
 Isokinicity
The whole basis behind the theory lies in the name itself. Isokinetic
breaks down to “Iso” same as or equal to and “kinetic” as in
movement or in this application, flow. The importance of collecting
a representative sample gave rise to sampling at the same flow
rate as the gas stream itself, as particles and droplets vary in size
and concentration dependent on the stack flow rate.
As determined whilst conducting the preliminary measurements,
the velocity and temperature across the stack may vary which is
why multiple sampling positions are calculated and predetermined
to obtain the most representative result.
In order to pull a sample of stack gas Isokinetically at each
position, information relating to the gas composition such as
moisture, dry molecular weight, temperature and velocity are
required to calculate the appropriate nozzle size and subsequent
sampling rate.
 Isokinicity
Isokinetic sampling conditions exist when the velocity of
the gases entering the probe nozzle tip (Vn) is exactly equal
to the velocity of the approaching stack gases (vs).

Isokinetic sampling = (Vn = vs)

Percent isokinetic = vs x 100

Vn

When Vn ≠ vs (anisokinetic) conditions exist.

“Final dust concentrations can become biased due to the

inertial effects of particulates”
 Isokinicity

200 % Isokinetic Sampling Rate

Tends to underestimate the particulate load due to bias of
smaller sized particulate and larger gas volumes.
 Isokinicity

50 % Isokinetic Sampling Rate

Tends to over-estimate load due greater number of larger
particles and lower gas volume.
 Isokinicity

100% Isokinetic Sampling Rate

Sampling performed at the 100% isokinetic rate will not
bias the uptake of the particulate. That is particulate will be
sampled equally irrespective of particle size.
100 % Isokinetic Sampling Rate
Particulate Entering The Nozzle.
 Isokinetic Calculation
I = 100 x Ts [0.003454 x Vic + (VmY/Tm) (Pbar+dH/13.6)]
60 x θ x Vs x Ps x An

I = Isokinetic sampling rate.

Ts = Temperature of the stack.
0.003454 = constant mmHg- m3/ml
Vm (std) = Total gas volume.
Y = gas meter calibration constant.
Vic = total water collected (grams)
Pbar = barometric pressure.
ΔH = Average delta H of test
13.6 = conversion from mmH20 to mmHg
60 = 60 seconds in a minute.
Vs = Stack gas velocity.
Ps = Absolute stack pressure.
An = Area of nozzle.
Ө = minutes sampled

The acceptable final isokinetic range is 90% - 110%

 Ideal Nozzle Size Calculation

Tm = Temperature of meter (Kelvin).

Ts = Temperature of stack (Kelvin).
Pm = Meter pressure (Pbar + deltaH@/13.6)
Ps = Absolute stack pressure (Ps=Pbar+Pg/13.6)
Md = Dry molecular weight.
Bws = Stack gas moisture fraction.
Ms = Wet gas molecular weight.
Cp =Pitot-tube coefficient.
Δp = average velocity head in mmH2O
Qm = Sampling flow rate.
0.6071 = constant mmHg/oK

“Assumes that the moisture fraction at the gas meter is

 K FACTOR

Dn = Nozzle diameter.
ΔH@ = Calibration constant for DGM
Cp = Pitot-tube coefficient.
Bws = Stack gas moisture fraction.
Md = Dry gas molecular weight.
Ms = Wet gas molecular weight.
Tm = Meter temperature.
Ts = Stack temperature.
Ps = Absolute stack pressure.
Pm = meter pressure.
 DELTA H CALCULATION

“This calculation is used to set the velocity of the gas

entering the nozzle (ΔH) to exactly same velocity of the gas
in the stack (Δp), using the derived K factor”
USEPA METHOD 5 – Sampling Train
 EQUIPMENT LIST
• Nozzles / Unions
• Pitot Tubes
• Heated Probe
• Liner (Glass)
• Cyclone (optional)
• Filter Assembly
• Glass Fibre Filter
• Heater Box
• Impingers (Impinger Case)
• Greenburg-Modified Impingers
• Greenburg-Impingers (No2)
 EQUIPMENT LIST

• Silica Gel
• Umbilical Cord (Vacuum Line)
• Vane Pump
• Gas Metering System
• Dual Liquid Vein Manometers
• Thermocouples
• Monorail Supports / Guy Ropes
• Residual Current Devices
• Measuring Cylinders / Wash Bottles
• Esky – 3 Bags of ice per run.
 Dry Gas Meter Console.
• Calibrated Dry Gas Meter
• Dual Vein Liquid Manometer for delta-P and delta-H
adjustments.
• System vacuum gauges.
• Quick connections for the Pitot-tube.
• Typical console has thermostats which regulate the probe
and filter box temperatures.
• Quick fit connections for flow of dry gas from (umbilical)
sampling train to DGM.
• Quick fit connections for the pump.
 The Orifice Meter.
The Orifice meter is the basis of an isokinetic test. In
practice the orifice meter is calibrated to provide a
calibration constant (ΔH@). This calibration factor is used to
determine the gas flow rates through the orifice meter
relative to the nozzle. Hence velocity at the nozzle is
equivalent (equals) the velocity of the gas flow up the
stack.

The k-factor is determined so that isokinetic sampling can

be performed. It is based on the calibration constant of the
Orifice Meter and atmospheric and stacks conditions.
Orifice Meter – a circular hole in a thin flat plate held
between flanges a joint in a pipe, located 8 diameters
upstream and 2 diameters downstream from any
disturbance, perpendicular to the pipe axis, with the hole
concentric to the pipe. The orifice creates a pressure
differential between the two sides of the plate. This
pressure differential is related to the flow rate through the
orifice device.
 Probe
• Made from suitable material. Consider temperature and
stack atmosphere.
• Has attached to it an S-Type Pitot-Tube.
• It has a heating element built into the inner body.
• Available in variable lengths.
• Holds glass, quartz, titanium or steel liners dependant on
method and stack requirements
• Has a union for the attachment of the nozzle.
 Pitot
• Impact plane: equal to or above the nozzle entry plane
• Usually attached to the probe sheath
• Type S with a known coefficient
• At least ¾ inch between the outsides of the probe nozzle
and the Pitot
• Thermocouple mounted either 2 inch behind or ¾ inch to
the side of the sensing head or over the top of the nozzle
 Filter Holder
• Holds Pre-weighed glass fibre filter in place during
sampling
• Usually made of borosilicate glass
• Positioned on glass, Teflon, or stainless steel
• Maintained at 120 0C +/- 140C
 Sampling Testing Approaches
Examples:

USEPA Method 17 USEPA Method 17 glass

sampling tip and fibre thimbles
thimble holder
 Filter / Probe Heating System
• Must reach and maintain 120 ± 14oC
• Filter heat prevents condensation, organics, and SO2 on
the filter.
• Criteria may differ from state to state and with certain
processes.
• Filter temperature should be monitored with a gage that
has 1oC increments.
 Condenser

• Minimum of Four impingers connected in series.

• Can be glass, stainless steel, or Teflon.
• Impingers 1, 3 and 4 have straight ½ inch ф tips.
• Impinger number two has Greenburg-Smith tip.
• Impinger 4 has 1oC increment thermometer at exit.
• Maintained below 200C for duration of stack test.
SAMPLING - Preliminary Determinations
• Determine sampling location – M1
• Determine number of sampling points – M1.
• Preliminary velocity and temperature traverse – M2.
• Determine gas molecular weight – M3.
• Determine the moisture content – M4.
• Select suitable probe liner type (quartz or Borosilicate
glass etc...)
• Select suitable length of probe and liner.
• Select appropriately sized nozzle based on previous
calculations – Ideal Nozzle.
• Determine total test time / time per point - θ.
• Perform a 10-minute DGM check.
 SAMPLING Leak Checks
It is a mandatory step and vitally important to ensure that
the sample train is leak free. This is done by blocking the
sample nozzle to build pressure and identify air ingress.

Any leak leads to underestimation of the final result.

• Performed at highest vacuum pressure of the run.

• Conducted pre and post test.
• Acceptable leak<0.00057m3 or 4% of the average.
• Void run if greater than <0.00057m3 or 4% of the average.

Vmc = Vm x (Lp – La) x Θ

Lp = post leak rate

La = acceptable leak rate
Θ = run time
 SAMPLING-Particulate Train Operation

• Maintain +20% of 100% isokinetic average at each point.

• Maintain +10% of 100% isokinetic as total average for test.

• Average >21 L/min (for example, collect >1.2 m3/hour)

• Maintain probe and filter +/-14o of 120oC.

• Ensure no vacuum >15 inch Hg (384 mmHg).

SAMPLING Particulate Train Operation

• Make sure all data recorded

• Impinger 4 < 20oC at all times.
• Read and record required data for duration of test.
• Make a note of any unusual circumstances or changes in
processes during the testing period.
 Isokinetic Spreadsheets
Sampling – Spreadsheets used
Isokinetic Spreadsheets
 Sample Recovery
• To be performed in a clean area.
• Probe liner and nozzle brushes made of nylon and Teflon
• Polyethylene or Teflon wash bottles
• Glass sample containers with screw lids and Teflon or
scrubber lid liners
• Graduated cylinder
• Tweezers and spatula
• Move probe and sample box to clean area
• Disconnect and seal probe, filter holder, and impingers
 Sample Recovery
Pour liquid from first three impingers into a jar, weigh, and
mark the level on outside of jar.

Place silica gel into another jar.

Rinse back half as directed

Save a portion of the acetone in another jar for a blank.

“USEPA Method has been successfully completed”

 Samples Generated
• A filter (this is either made of quartz or glass micro fibre)
and sho
• A probe wash/nozzle rinse. (this is approximately 100ml of
Deionised water and Acetone)

A Blank Filter and Probe wash should be generated for

quality assurance purposes for each stack tested. These are
taken on-site as a control to identify contamination or
analysis problems. THE BLANKS ARE NOT SUBTRACTED
FROM THE FINAL RESULT!

The rule of thumb should be approximately 1/3 of the Total

Particulate captured is in the probe rinse. This only applies
to extractive sampling and not in all circumstances.
 Calculations

The particulates are collected on the filter cartridge and

also deposited on the probe liner.

The final expression of particulate concentration is as

follows:

TPM = Dust collected on filter (PM) + Dust collected on

Probe (ACW)
Dry Standard Cubic Meters

TPM = mg/dscm
 Consecutive Vs Parallel Sampling
Definition
Consecutive Sampling is performing one test after another
and is related to completing duplicate or triplicate testing
using Isokinetic methods.
It is important to recognise that multiple tests can be run at
the same time and is necessary on occasion. However this
only applies to non-isokinetic techniques ie. Gas Analysers
Parallel Sampling is performing multiple isokinetic tests
concurrently in the same stack at the same time.
 Consecutive Vs Parallel Sampling
The USEPA recommends that only a single isokinetic
sampling train(probe) can be used at a sampling location at
any one time. This is based on the following facts:
1. Sample flow disturbances generated from the probes
can occur causing non-representative sampling.
2. Safety concerns with added equipment in
tight/confined areas on platform.
3. Representative sampling potentially not occurring due
to sample probe cross over.
The importance of replicate sampling
Currently the author is unaware of any stipulations through
regulatory operating licences regarding the number of tests
required to obtain a reasonable level of confidence.

It is standard industry practice although not mandatory, but

vital in terms of Quality Assurance that multiple (at least 2)
samples are taken for each pollutant .
Acceptable Variations between Tests
Testing and respective results are heavily influenced by
process conditions and plant stability, especially when the
testing is conducted on non-continuous processes (Batch).
Accounting for the standard method uncertainty, and
assuming stable plant conditions, attributed to the methods
(USEPA Method 5 & 17 are approximately +/- 10%) then an
acceptable criteria would be a variation of +/- 20% between
multiple runs.
 Acceptable Variations between Tests
An important note is that method uncertainty, and in turn the
acceptable criteria of comparing runs increases as you get nearer the
Method Detection Limit(MDL).
Where replicate runs are out with this acceptable criteria, the process
conditions and type of plant tested must come into consideration.
Example include:
• Batch Processes (Brick Kilns, spray booths etc)
• Electrostatic Precipitator Abatement plants
• Variable Feed rate processes/Electrical Generation Loads
• The variable results caused by the unstable nature of processes as
described above can be mitigated by increasing the number of
tests conducted.