Document ID: EPA-HQ-OAR-2002-0056-5105
Agency: epa
Document Type: Supporting & Related Material
Title: 
Posted Date: 2004-11-22T05:00Z

Method
101C
­
Determination
of
Elemental
and
Oxidized
Mercury
(
Hg)
from
Stationary
Sources
(
Instrumental
Analyzer
Procedure)
(
Draft
­
For
Review
and
Comment)
RMB
Consulting
&
Research
­
10/
23/
04
1.
APPLICABILITY
AND
PRINCIPLE
1.1
Applicability.
This
method
is
applicable
to
the
determination
of
elemental
(
Hgo)
and
oxidized
(
Hg+
2)
mercury
concentrations
in
emissions
from
stationary
sources
only
when
specified
within
the
regulations.

1.2
Principle.
A
gas
sample
is
continuously
extracted
from
the
effluent
stream;
a
portion
of
the
sample
stream
is
conveyed
to
an
instrumental
analyzer
for
determination
of
Hgo
and
Hg+
2
concentrations
using
a
cold­
vapor
atomic
absorption
(
CVAAS),
cold­
vapor
atomic
fluorescence
(
CVAFS),
ultraviolet
differential
optical
absorption
(
UVDOAS),
atomic
emission
(
AES),
or
x­
ray
fluorescence
(
XRFS)
spectrometer.
Performance
specifications
and
test
procedures
are
provided
to
ensure
reliable
data.

2.
RANGE
AND
SENSITIVITY
2.1
Analytical
Range.
The
analytical
range
is
determined
by
the
instrumental
design.
For
this
method,
a
portion
of
the
analytical
range
is
selected
by
choosing
the
span
of
the
monitoring
system.
The
span
of
the
monitoring
system
shall
be
selected
such
that
the
pollutant
gas
concentration
being
measured
is
not
less
than
30
percent
of
the
span.
If
at
any
time
during
a
run
the
measured
gas
concentration
exceeds
the
span,
then
the
run
shall
be
considered
invalid.

2.2
Sensitivity.
The
minimum
detectable
limit
depends
on
the
analytical
range,
span,
and
signalto
noise
ratio
of
the
measurement
system.
For
a
well
designed
system,
the
minimum
detectable
limit
should
be
less
than
2
percent
of
the
span.

3.
DEFINITIONS
3.1
Measurement
System.
The
total
equipment
required
for
the
determination
of
Hgo
and
Hg+
2
concentrations.
The
measurement
system
consists
of
the
following
major
subsystems:

3.1.1
Sample
Interface.
That
portion
of
a
system
used
for
one
or
more
of
the
following:
sample
acquisition,
sample
transport,
sample
conditioning,
or
protection
of
the
analyzers
from
the
effects
of
the
stack
effluent.

3.1.2
Gas
Analyzer.
That
portion
of
the
system
that
senses
the
gas
to
be
measured
and
generates
an
output
proportional
to
its
concentration.
3.1.3
Data
Recorder.
A
digital
computer/
recorder
for
recording
measurement
data
from
the
analyzer
output.

3.1.4
Hg+
2
to
Hgo
Converter.
A
device
that
converts
the
oxidized
mercury
(
Hg+
2)
in
the
sample
gas
to
elemental
mercury
(
Hgo).

3.2
Span.
The
upper
limit
of
the
gas
concentration
measurement
range
determined
by
the
calibration
gas.

3.3
Calibration
Gas.
A
known
concentration
of
a
gas
in
an
appropriate
diluent
gas.

3.4
Analyzer
Calibration
Error.
The
difference
between
the
gas
concentration
exhibited
by
the
gas
analyzer
and
the
known
concentration
of
the
calibration
gas
when
the
calibration
gas
is
introduced
directly
to
the
analyzer.

3.5
Sampling
System
Bias.
The
difference
between
the
gas
concentrations
exhibited
by
the
measurement
system
when
a
known
concentration
gas
is
introduced
at
the
outlet
of
the
sampling
probe
and
when
the
same
gas
is
introduced
directly
to
the
analyzer.

3.6
Zero
Drift.
The
difference
in
the
measurement
system
output
reading
from
the
initial
calibration
response
at
the
zero
concentration
level
after
a
stated
period
of
operation
during
which
no
unscheduled
maintenance,
repair,
or
adjustment
took
place.

3.7
Calibration
Drift.
The
difference
in
the
measurement
system
output
reading
from
the
initial
calibration
response
at
the
span
value
after
a
stated
period
of
operation
during
which
no
unscheduled
maintenance,
repair,
or
adjustment
took
place.

3.8
Response
Time.
The
amount
of
time
required
for
the
measurement
system
to
display
95
percent
of
a
step
change
in
gas
concentration
on
the
data
recorder.

3.9
Interference
Response.
The
output
response
of
the
analyzer
system
to
a
component
in
the
sample
gas,
other
than
the
gas
component
being
measured.

3.10
Interference
Test.
The
comparative
result
of
three
coordinated
test
runs
at
a
particular
source
category
between
the
response
of
a
particular
sampling
system
and
analyzer
model
and
the
measured
result
from
an
ASTM
D6784­
02
(
i.
e.,
Ontario­
Hydro)
sampling
train.
A
unique
source
category
is
defined
1)
by
the
type
of
fuel
combusted
by
the
source
(
e.
g.,
oil,
natural
gas,
anthracite,
lignite
or
bituminous
coal)
and
2)
by
any
additive
emission
controls
downstream
of
the
emission
source
and
upstream
of
the
sample
location
(
e.
g.,
wet
or
dry
scrubber
to
control
SO2
emissions,
selective
catalytic
reduction
(
SCR)
or
selective
non­
catalytic
reduction
(
SNCR)
unit
to
control
NOx
emissions).
(
Note:
I
believe
this
language
covers
"
unique
source"
but
we
may
have
to
be
more
specific.)

4.
MEASUREMENT
SYSTEM
PERFORMANCE
SPECIFICATIONS
(
Note:
The
percent
values
are
just
placeholders
­
we
do
not
know
if
they
can
be
achieved.)

4.1
Analyzer
Calibration
Error.
Less
than

2
percent
of
the
span
for
the
zero,
mid­
range,
and
high­
range
calibration
gases.

4.2
Sampling
System
Bias.
Less
than

5
percent
of
the
span
for
the
zero
and
mid­
range
calibration
gases.

4.3
Zero
Drift.
Less
than

3
percent
of
the
span
over
the
period
of
each
run.

4.4
Calibration
Drift.
Less
than

3
percent
of
the
span
over
the
period
of
each
run.

4.5
Interference
Response.
Less
than
2
percent
of
span.

4.6
Interference
Test.
Less
than

10
percent
of
the
ASTM
D6784­
02
(
i.
e.,
Ontario­
Hydro)
average
result
for
each
three­
run
series.

5.
APPARATUS
AND
REAGENTS
5.1
Measurement
System.
Use
any
measurement
system
for
Hgo
and
Hg+
2
that
meets
the
specifications
of
this
method.
A
schematic
of
an
acceptable
measurement
system
is
shown
in
Figure
101C­
1
of
this
method.
The
essential
components
of
the
measurement
system
are
described
below:

5.1.1
Sample
Probe.
Glass,
stainless
steel?
(
Is
stainless
acceptable?),
teflon
or
equivalent,
of
sufficient
length
to
traverse
the
sample
points.
The
sampling
probe
shall
be
heated
to
prevent
condensation.

5.1.2
Sample
Line.
Heated
(
sufficient
to
prevent
condensation
and/
or
sublimation)
Teflon
tubing,
to
transport
the
sample
gas
to
the
moisture
removal
system.

5.1.3
Sample
Transport
Lines.
Teflon
tubing,
to
transport
the
sample
from
the
moisture
removal
system
to
the
sample
pump,
sample
flow
rate
control,
and
sample
gas
manifold.

5.1.4
Calibration
Valve
Assembly.
A
three­
way
valve
assembly,
or
equivalent,
for
blocking
the
sample
gas
flow
and
introducing
calibration
gases
to
the
measurement
system
at
the
outlet
of
the
sampling
probe
when
in
the
calibration
mode.

5.1.5
Moisture
Removal
System.
A
refrigerator­
type
condenser
or
similar
device
(
e.
g.,
permeation
dryer
or
thermoelectric
peltier
chiller),
to
remove
condensate
continuously
from
the
sample
gas
while
maintaining
minimal
contact
between
the
condensate
and
the
sample
gas.
The
moisture
removal
system
is
not
necessary
for
analyzers
that
can
measure
gas
concentrations
on
a
wet
basis;
for
these
analyzers,
(
1)
heat
the
sample
line
and
all
interface
components
up
to
the
inlet
of
the
analyzer
sufficiently
to
prevent
condensation,
and
(
2)
determine
the
moisture
content
and
correct
the
measured
gas
concentrations
to
a
dry
basis
using
appropriate
methods,
subject
to
the
approval
of
the
Administrator.
The
determination
of
sample
moisture
content
is
not
necessary
for
pollutant
analyzers
that
measure
concentrations
on
a
wet
basis
when
(
1)
a
wet
basis
CO2
analyzer
operated
according
to
Method
3A
is
used
to
obtain
simultaneous
measurements,
and
(
2)
the
pollutant/
CO2
measurements
are
used
to
determine
emissions
in
units
of
the
standard.
(
Note
­
This
will
be
problematic
if
EPA
sets
any
Hg
standard
on
a
dry
basis.
Error
propagation
from
moisture
measurement
on
wet
stacks
will
cause
serious
problems.)

5.1.6
Particulate
Filter.
An
in­
stack
or
heated
(
sufficient
to
prevent
water
condensation)
outof
stack
filter.
The
filter
shall
be
borosilicate
or
quartz
glass
wool,
or
glass
fiber
mat.
Additional
filters
at
the
inlet
or
outlet
of
the
moisture
removal
system
and
inlet
of
the
analyzer
may
be
used
to
prevent
accumulation
of
particulate
material
in
the
measurement
system
and
extend
the
useful
life
of
the
components.
All
filters
shall
be
fabricated
of
materials
that
are
nonreactive
to
the
gas
being
sampled.

5.1.7
Sample
Pump.
A
leak­
free
pump,
to
pull
the
sample
gas
through
the
system
at
a
flow
rate
sufficient
to
minimize
the
response
time
of
the
measurement
system.
The
pump
may
be
constructed
of
any
material
that
is
nonreactive
to
the
gas
being
sampled.

5.1.8
Sample
Flow
Rate
Control.
A
sample
flow
rate
control
valve
and
rotameter,
or
equivalent,
to
maintain
a
constant
sampling
rate
within
10
percent.
(
Note:
The
tester
may
elect
to
install
a
back­
pressure
regulator
to
maintain
the
sample
gas
manifold
at
a
constant
pressure
in
order
to
protect
the
analyzer(
s)
from
overpressurization,
and
to
minimize
the
need
for
flow
rate
adjustments.)

5.1.9
Sample
Gas
Manifold.
A
sample
gas
manifold,
to
divert
a
portion
of
the
sample
gas
stream
to
the
analyzer
and
the
remainder
to
the
by­
pass
discharge
vent.
The
sample
gas
manifold
should
also
include
provisions
for
introducing
calibration
gases
directly
to
the
analyzer.
The
manifold
may
be
constructed
of
any
material
that
is
nonreactive
to
the
gas
being
sampled.

5.1.10
Data
Recorder.
A
digital
computer/
recorder,
for
recording
measurement
data.
The
data
recorder
resolution
(
i.
e.,
readability)
shall
be
0.5
percent
of
span.
Alternatively,
a
digital
meter
having
a
resolution
of
0.5
percent
of
span
may
be
used
to
obtain
the
analyzer
responses
and
the
readings
may
be
recorded
manually.
If
this
alternative
is
used,
the
readings
shall
be
obtained
at
equally
spaced
intervals
over
the
duration
of
the
sampling
run.
For
sampling
run
durations
of
less
than
1
hour,
measurements
at
1­
minute
intervals
or
a
minimum
of
30
measurements,
whichever
is
less
restrictive,
shall
be
obtained.
For
sampling
run
durations
greater
than
1
hour,
measurements
at
2­
minute
(
may
need
to
be
as
long
as
6
minutes)
intervals
or
a
minimum
of
96
measurements,
whichever
is
less
restrictive,
may
be
obtained.
Digital
data
collection
systems
may
be
able
to
collect
considerably
more
data
than
the
minimum
requirements
described
above.
This
is
acceptable
so
long
as
the
data
collected
are
equally
spaced
in
time.

5.1.11
Hg+
2
to
Hgo
Converter.
That
portion
of
the
system
that
converts
Hg+
2
in
the
sample
gas
to
Hgo.

5.1.12
Hgo
Analyzer.
A
cold­
vapor
atomic
absorption
(
CVAAS),
cold­
vapor
atomic
fluorescence
(
CVAFS),
ultraviolet
differential
optical
absorption
(
UVDOAS),
atomic
emission
(
AES),
or
x­
ray
fluorescence
(
XRFS)
spectrometer,
to
determine
continuously
the
Hgo
concentration
in
the
sample
gas
stream.
The
analyzer
shall
meet
the
applicable
performance
specifications
of
Section
4.
A
means
of
controlling
the
analyzer
flow
rate
and
a
device
for
determining
proper
sample
flow
rate
(
e.
g.,
precision
rotameter,
pressure
gauge
downstream
of
all
flow
controls,
etc.)
shall
be
provided
at
the
analyzer.
(
Note:
Housing
the
analyzer(
s)
in
a
clean,
thermally­
stable,
vibration­
free
environment
will
minimize
drift
in
the
analyzer
calibration.)

5.2
Hgo
and
Hg+
2
Calibration
Gases.
The
calibration
gases
for
the
Hgo
analyzer
shall
be
Hgo
and
HgCl2.
(
Note
­
May
need
to
come
up
with
calibration
gas
mixture
standards
for
fluorescence­
based
analyzers.)
Alternative
Hg0
and
Hg+
2
calibration
devices
that
are
traceable
to
NIST
with
an
accuracy
of
2%
or
better
may
also
be
used
instead
of
calibration
gases
in
pressurized
cylinders.
Use
three
calibration
gases
or
a
calibration
device
to
provide
calibration
levels
as
specified
below:

5.2.1
High­
Range
Gas.
Concentration
equivalent
to
80
to
100
percent
of
the
span.

5.2.2
Mid­
Range
Gas.
Concentration
equivalent
to
40
to
60
percent
of
the
span.

5.2.3
Zero
Gas.
Concentration
of
less
than
0.25
percent
of
the
span.
Purified
ambient
air
may
be
used
for
the
zero
gas
by
passing
air
through
an
activated
charcoal
filter.

6.
MEASUREMENT
SYSTEM
PERFORMANCE
TEST
PROCEDURES
Perform
the
following
procedures
before
measurement
of
emissions
(
Section
7).

6.1
Calibration
Gas
Concentration
Verification.
(
Note
­
This
requires
additional
development
for
Hg+
2
.
In
fact,
we
may
want
to
eliminate
the
entire
section
and
just
replace
it
with
the
alternative
Section
6.1
below.)
There
are
two
alternatives
for
establishing
the
concentrations
of
calibration
gases.
Alternative
No.
1
is
preferred
Alternative
6.1
Calibration
Gas
Concentration
Verification
The
calibration
gases
used
for
Hg0
and
Hg+
2
must
be
a
NIST/
EPA
approved
certified
reference
material,
standard
reference
material
or
Protocol
1
calibration
gas
certified
by
the
vendor
to
be
within
2%
of
the
tag
value.
Alternatively,
the
calibration
gases
may
be
generated
by
a
device
traceable
to
NIST
certified
to
deliver
calibration
gases
within
2%
accurate.
The
manufacturer
of
the
calibration
device
is
responsible
for
providing
documentation
and
certification
of
NIST
traceability.
Operate
the
calibration
devices
in
accordance
with
the
manufacturer's
instructions.

6.1.1
Alternative
No.
1­­
Use
of
calibration
gases
that
are
analyzed
following
the
Environmental
Protection
Agency
Traceability
Protocol
No.
1
(
see
Citation
1
in
Bibliography).
Obtain
a
certification
from
the
gas
manufacturer
that
Protocol
No.
1
was
followed.

6.1.2
Alternative
No.
2­­
Use
of
calibration
gases
not
prepared
according
to
Protocol
No.
1.
If
this
alternative
is
chosen,
obtain
gas
mixtures
with
a
manufacturer's
tolerance
not
to
exceed

2
percent
of
the
tag
value.
Within
6
months
before
the
emission
test,
analyze
each
of
the
calibration
gases
in
triplicate
using
an
ASTM
D6784­
02
or
Method
29
sampling
train.
Record
the
results
on
a
data
sheet.
Each
of
the
individual
Hg
analytical
results
for
each
calibration
gas
shall
be
within
5
percent
of
the
triplicate
set
average,
otherwise,
discard
the
entire
set
and
repeat
the
triplicate
analyses.
If
the
average
of
the
triplicate
analyses
is
within
5
percent
of
the
calibration
gas
manufacturer's
cylinder
tag
value,
use
the
tag
value;
otherwise,
conduct
at
least
three
additional
analyses
until
the
results
of
six
consecutive
runs
agree
within
5
percent
of
the
average.
Then
use
this
average
for
the
cylinder
value.
6.2
Interference
Response.
Conduct
an
interference
response
test
of
the
analyzer
prior
to
its
initial
use
in
the
field.
Thereafter,
recheck
the
measurement
system
if
changes
are
made
in
the
instrumentation
that
could
alter
the
interference
response
(
e.
g.,
changes
in
the
gas
detector).
Conduct
the
interference
response
in
accordance
with
procedures
below:

6.2.1
Introduce
the
gaseous
components
listed
in
Table
101C­
3
directly
into
the
analyzer
system
(
analyzer
plus
Hg
converter)
separately,
or
as
gas
mixtures.
For
analyzer
systems
that
will
be
used
with
dilution
probes,
correct
the
concentrations
in
Table
101C­
3
consistent
with
the
dilution
ratio.
Determine
the
total
interference
output
response
of
the
system
to
these
components
in
concentration
units;
record
the
values
on
a
form
similar
to
Figure
101C­
4.
If
the
sum
of
the
interference
responses
of
the
test
gases
for
either
the
Hgo
or
Hg2+
analysis
is
greater
than
2
percent
of
the
applicable
span
value,
take
corrective
measures
on
the
measurement
system.

6.2.2
Conduct
an
interference
response
test
of
each
analyzer
before
its
initial
use
in
the
field.
Thereafter,
recheck
the
measurement
system
if
changes
are
made
in
the
instrumentation
that
could
alter
the
interference
response,
e.
g.,
changes
in
the
type
of
gas
detector.

6.2.3
In
lieu
of
conducting
the
interference
response
test,
instrument
vendor
data,
which
demonstrate
that
for
the
test
gases
of
Table
101C­
3
the
interference
performance
specification
is
not
exceeded,
are
acceptable.

6.3
Measurement
System
Preparation.
Assemble
the
measurement
system
by
following
the
manufacturer's
written
instructions
for
preparing
and
preconditioning
the
gas
analyzer
and,
as
applicable,
the
other
system
components.
Introduce
the
Hg0
calibration
gases
in
any
sequence,
and
make
all
necessary
adjustments
to
calibrate
the
analyzer
and
the
data
recorder.
Adjust
system
components
to
achieve
correct
sampling
rates.

6.4
Analyzer
Calibration
Error.
Conduct
the
analyzer
calibration
error
check
by
introducing
calibration
gases
to
the
measurement
system
at
any
point
upstream
of
the
gas
analyzer
as
follows:

6.4.1
After
the
measurement
system
has
been
prepared
for
use,
introduce
the
zero,
mid­
range,
and
high­
range
Hg0
gases
to
the
analyzer.
During
this
check,
make
no
adjustments
to
the
system
except
those
necessary
to
achieve
the
correct
calibration
gas
flow
rate
at
the
analyzer.
Record
the
analyzer
responses
to
each
calibration
gas
on
a
form
similar
to
Figure
101C­
5.
Note:
A
calibration
curve
established
prior
to
the
analyzer
calibration
error
check
may
be
used
to
convert
the
analyzer
response
to
the
equivalent
gas
concentration
introduced
to
the
analyzer.
However,
the
same
correction
procedure
shall
be
used
for
all
effluent
and
calibration
measurements
obtained
during
the
test.

6.4.2
The
analyzer
calibration
error
check
shall
be
considered
invalid
if
the
gas
concentration
displayed
by
the
analyzer
exceeds

2
percent
of
the
span
for
any
of
the
calibration
gases.
If
an
invalid
calibration
is
exhibited,
take
corrective
action
and
repeat
the
analyzer
calibration
error
check
until
acceptable
performance
is
achieved.

6.5
Sampling
System
Bias
Check.
Perform
the
sampling
system
bias
check
by
introducing
Hg0
calibration
gases
at
the
calibration
valve
installed
at
the
outlet
of
the
sampling
probe.
A
zero
gas
and
either
the
mid­
range
or
high­
range
gas,
whichever
most
closely
approximates
the
effluent
concentrations,
shall
be
used
for
this
check
as
follows:

6.5.1
Introduce
the
upscale
calibration
gas,
and
record
the
gas
concentration
displayed
by
the
analyzer
on
a
form
similar
to
Figure
101C­
6.
Then
introduce
zero
gas,
and
record
the
gas
concentration
displayed
by
the
analyzer.
During
the
sampling
system
bias
check,
operate
the
system
at
the
normal
sampling
rate,
and
make
no
adjustments
to
the
measurement
system
other
than
those
necessary
to
achieve
proper
calibration
gas
flow
rates
at
the
analyzer.

6.5.2
The
sampling
system
bias
check
shall
be
considered
invalid
if
the
difference
between
the
gas
concentrations
displayed
by
the
measurement
system
for
the
analyzer
calibration
error
check
and
for
the
sampling
system
bias
check
exceeds

5
percent
of
the
span
for
either
the
zero
or
upscale
calibration
gases.
If
an
invalid
calibration
is
exhibited,
take
corrective
action,
and
repeat
the
sampling
system
bias
check
until
acceptable
performance
is
achieved.
If
adjustment
to
the
analyzer
is
required,
first
repeat
the
analyzer
calibration
error
check
and
then
repeat
the
sampling
system
bias
check.

Alternately
introduce
the
zero
and
upscale
gases
until
a
stable
response
is
achieved.
The
tester
shall
determine
the
measurement
system
response
time
by
observing
the
times
required
to
achieve
a
stable
response
for
both
the
zero
and
upscale
gases.
Note
the
longer
of
the
two
times
as
the
response
time.

6.6
Hg+
2
to
Hgo
Conversion
Efficiency.
Introduce
the
Hg+
2
calibration
gas
into
the
analyzer's
Hg+
2
 
Hgo
converter
until
the
analyzer's
response
stabilizes.
Then,
record
the
instrument
response
and
calculate
converter
efficiency.
If
the
instrument
indicates
at
least
95
(
90?)
percent
Hg+
2
to
Hgo
conversion,
the
converter
is
acceptable.
If
the
instrument
response
indicates
less
than
95
percent
Hg+
2
to
Hgo
conversion,
the
converter
is
unacceptable
and
repair
or
replacement
is
required
before
repeating
the
check.
Conversion
efficiency
tests
shall
be
conducted
prior
to
beginning
any
reference
method
test
series
or
once
a
day,
whichever
is
most
frequent.

6.7
Interference
Test
(
if
performed).
If
an
interference
test
has
not
previously
been
performed
on
any
unique
source
category,
this
test
must
be
performed
prior
to
the
use
of
a
given
analyzer
system
as
a
reference
method.
This
test
is
intended
to
demonstrate
that
the
analyzer
system
accurately
represents
the
Hg
measurement
in
the
presence
of
the
unique
source's
flue
gas
matrix.
A
unique
source
category
is
defined
1)
by
the
type
of
fuel
combusted
by
the
source
(
e.
g.,
oil,
natural
gas,
anthracite,
lignite
or
bituminous
coal)
and
2)
by
any
additive
emission
controls
downstream
of
the
emission
source
and
upstream
of
the
sample
location
(
e.
g.,
wet
or
dry
scrubber
to
control
SO2
emissions,
selective
catalytic
reduction
(
SCR)
or
selective
non­
catalytic
reduction
(
SNCR)
unit
to
control
NOx
emissions).
To
conduct
the
test,
perform
three
comparative,
coordinated
test
runs
at
a
particular
source
category
using
a
particular
sampling
system
and
analyzer
model,
operated
as
a
reference
method,
and
an
ASTM
D6784­
02
(
i.
e.,
Ontario­
Hydro)
sampling
train.
For
this
interference
test
traversing
is
not
required
for
either
the
instrumental
reference
method
or
the
Ontario­
Hydro
method.
It
is
recommended
that
the
sampling
probes
for
both
methods
be
located
as
close
as
possible
to
each
other,
but
at
least
1
meter
from
the
stack
wall.
Recover
and
analyze
the
contents
of
the
ASTM
D6784­
02
sampling
train
for
each
run,
and
determine
the
Hgo
and
Hg+
2
gas
concentrations
using
the
procedures
in
ASTM
D6784­
02.
Determine
the
average
gas
concentration
exhibited
by
the
analyzer
system
for
each
run.
Average
the
results
of
the
three
analyzer
system
runs
and
the
three
ASTM
D6784­
02
runs.
If
the
Hg0
plus
Hg+
2
gas
concentrations
provided
by
the
analyzer
system
and
the
ASTM
D6784­
02
sampling
train
differ
by
more
than
10
percent
from
the
average
ASTM
D6784­
02
result,
the
analyzer
system
does
not
pass
the
interference
check
test
and
cannot
be
used
to
perform
reference
method
tests
on
the
unique
source
category.

7.
EMISSION
TEST
PROCEDURE
7.1
Selection
of
Sampling
Site
and
Sampling
Points.
Select
a
measurement
site
and
sampling
points
using
the
same
criteria
that
are
applicable
to
tests
performed
using
ASTM
D6784­
02.

7.3
Sample
Collection.
Position
the
sampling
probe
at
the
first
measurement
point,
and
begin
sampling
at
the
same
rate
as
used
during
the
response
time
test.
Maintain
constant
sampling
rate
(
i.
e.,

10
percent)
during
the
entire
run.
The
sampling
time
per
run
shall
be
at
least
30
minutes
plus
twice
the
average
system
response
time.
For
each
run,
use
only
those
measurements
obtained
after
twice
the
response
time
of
the
measurement
system
has
elapsed
to
determine
the
average
effluent
concentration.

7.4
Zero
and
Calibration
Drift
Test.
Immediately
preceding
and
following
each
run,
or
if
adjustments
are
necessary
for
the
measurement
system
during
the
run,
repeat
the
sampling
system
bias
check
procedure
described
in
Section
6.5.
(
Make
no
adjustments
to
the
measurement
system
until
after
the
drift
checks
are
completed.)
Record
the
analyzer's
responses
on
a
form
similar
to
Figure
101C­
6.

7.4.1
Sample
System
Bias.
If
either
the
zero
or
upscale
calibration
value
exceeds
the
sampling
system
bias
specification
(
i.
e.,
5%
of
span
from
the
last
analyzer
calibration
error
check
response),
then
the
run
is
considered
invalid.
Repeat
both
the
analyzer
calibration
error
check
procedure
(
Section
6.4)
and
the
sampling
system
bias
check
procedure
(
Section
6.5)
before
repeating
the
run.
If
both
the
zero
and
upscale
calibration
values
are
within
the
sampling
system
bias
specification,
then
use
the
average
of
the
pre­
test
run
and
post­
test
run
bias
check
values
to
calculate
the
gas
concentration
for
the
run.

7.4.2
Analyzer
Drift.
If
the
difference
between
either
the
pre­
test
and
post­
test
run
sample
system
bias
test
zero
or
upscale
calibration
value
exceeds
the
bias
test
drift
limit
(
i.
e.,
3%
of
span,
pre­
test
compared
to
post­
test),
then
repeat
both
the
analyzer
calibration
error
check
procedure
(
Section
6.4)
and
the
sampling
system
bias
check
procedure
(
Section
6.5)
before
conducting
additional
runs.

8.
EMISSION
CALCULATION
The
average
gas
effluent
concentration
is
determined
from
the
average
gas
concentration
displayed
by
the
gas
analyzer
and
is
adjusted
for
the
zero
and
upscale
sampling
system
bias
checks,
as
determined
in
accordance
with
Section
7.4.
The
average
gas
concentration
displayed
by
the
analyzer
may
be
determined
by
averaging
all
of
the
effluent
measurements.
Alternatively,
the
average
may
be
calculated
from
measurements
recorded
at
equally
spaced
intervals
over
the
entire
duration
of
the
run.
For
sampling
run
durations
of
less
than
1
hour,
measurements
at
1­
minute
intervals
or
a
minimum
of
30
measurements,
whichever
is
less
restrictive,
may
be
used.
For
sampling
run
durations
greater
than
1
hour,
measurements
at
2­
minute
intervals
(
may
need
to
increase
these
time
intervals)
or
a
minimum
of
96
measurements,
whichever
is
less
restrictive,
shall
be
used.
Calculate
the
effluent
gas
concentration
using
Equation
101C­
1
below.

(
)
C
C­
C
C
C
C
gas
o
ma
m
o
=
 

Equation
101C­
1
Where:
Cgas
=
Effluent
gas
concentration,
ppm.
(
µ
g/
m3)
Cavg
=
Average
gas
concentration
indicated
by
gas
analyzer,
ppm.
(
µ
g/
m3)
Co
=
Average
of
initial
and
final
system
calibration
bias
check
responses
for
the
zero
gas,
ppm.
(
µ
g/
m3)
Cm
=
Average
of
initial
and
final
system
calibration
bias
check
responses
for
the
upscale
calibration
gas,
ppm.
(
µ
g/
m3)
Cma
=
Actual
concentration
of
the
upscale
calibration
gas,
ppm.
(
µ
g/
m3)

BIBLIOGRAPHY
1.
Traceability
Protocol
for
Establishing
True
Concentrations
of
Gases
Used
for
Calibrations
and
Audits
of
Continuous
Source
Emission
Monitors:
Protocol
Number
1.
U.
S.
Environmental
Protection
Agency,
Quality
Assurance
Division.
Research
Triangle
Park,
N.
C.
June
1978.

2.
Westlin,
Peter
R.
and
John
W.
Brown.
Methods
for
Collecting
and
Analyzing
Gas
Cylinder
Samples.
Source
Evaluation
Society
Newsletter.
3(
3):
5­
15.
September
1978.
Figure
101C­
1.
Measurement
System
Schematic.
Ice
Water
Bath
Midget
Impingers
Dry
Gas
Meter
Rotameter
Drying
Tube
Needle
Valve
3%
H
O
(
15
ml
each)
2
2
Excess
Sample
Vent
Sample
By­
pass
Vent
Figure
101C­
2.
Interference
Check
Sampling
Train.
Table
101C­
3.
Interference
Test
Gas
Concentrations
CO
500
±
50ppm
CO2
10
±
1%

SO2
200
±
20ppm
O2
20.9
±
1%
ppm
Date
of
Test:
_____________

Analyzer
Type:
_______________________________________________________

Serial
Number:
_______________________________________________________

Test
Gas
Type
Concentration
ppm
Analyzer
Output
Response
%
of
Span
%
of
span
=
Analyzer
Output
Response
Instrument
Span
X
100
Figure
101C­
4.
Interference
Response
Source
Identification:
Runs:

Test
Personnel:
Span:

Date:

Analyzer
Calibration
Data
for
Sampling
Cylinder
Value
(
indicate
units)
Analyzer
Calibration
Response
(
indicate
units)
Absolute
Difference
(
indicate
units)
Difference
(
percent
of
span)

Zero
Gas
Mid­
Range
Gas
High­
Range
Gas
Figure
101C­
5.
Analyzer
Calibration
Data.

Source
Identification:
Run
Number:

Test
Personnel:
Span:

Date:

Initial
Values
Final
Values
Analyzer
Calibration
Response
System
Calibration
Response
System
Cal.
Bias
(
percent
of
span)
System
Calibration
Response
System
Cal.
Bias
(
percent
of
span)
Drift
(
percent
of
span)

Zero
Gas
Upscale
Gas
System
Calibration
Bias
=
System
Cal.
Response
­
Analyzer
Cal.
Response
Span
Drift
=
Final
System
Cal.
Response
­
Initial
System
Cal.
Response
Span
X
X
100
100
Figure
101C­
6.
System
Calibration
Bias
and
Drift
Data.