­­­­­
Original
Message­­­­­

From:
David
Word
[
mailto:
d_
word@
src­
ncasi.
org]

Sent:
Tuesday,
June
22,
2004
6:
41
PM
To:
Gary
McAlister
(
Gary
McAlister);
Katie
Hanks;
Becky
(
Rebecca)
Nicholson
Cc:
Tim
Hunt;
Mary
Tom
Kissell
(
Mary
Tom
Kissell);
John
Pinkerton
(
John
Pinkerton)

Subject:
Benzene
and
Impinger
Canister
Gary,
Katie,
and
Becky:

The
AF&
PA
Wood
Products
Environmental
Issues
Task
Group
has
proposed
using
the
NCASI
impinger/
canister
sampling
system
(
NCASI
IM/
CAN/
WP­
99.02)
for
benzene.
I
volunteered
to
send
you
our
QA
data
for
benzene.
Open
mouth
 
insert
foot.
I
forgot
that
toluene
was
our
QA
target,
not
benzene.
We
spiked
toluene,
methylene
chloride,
and
1,2­
dichloroethane
into
the
sample
train
probe
tips
for
train
spikes,
and
directly
into
the
canisters
prior
to
field
sampling
for
the
run
spikes.
So
we
have
toluene
spike
recovery
data,
not
benzene.

However,
benzene
and
toluene
are
similar
compounds,
both
considered
slightly
soluble
and
both
can
be
purged
from
water.
Toluene
is
a
benzene
ring
(
C6H6)
with
a
single
carbon
side
chain
(
C7H8).

I
have
attached
an
excerpt
from
NCASI
Technical
Bulletin
774
regarding
spike
recovery
of
toluene
(
toluene.
pdf).
Our
toluene
spike
recovery
averaged
high
 
133%
for
train
spikes
and
147%
for
run
spikes.
There
is
a
little
discussion
of
this
on
page
15
of
the
attached
file
(
underlined).

When
we
re­
wrote
the
impinger
canister
method
we
added
fairly
stringent
quality
control
criteria.
We
require
that
the
compounds
of
interest
(
benzene
in
this
case)
be
spiked
into
the
sample
train
probe
tip
for
train
spikes
and
into
the
canister
or
first
impinger
for
run
spikes.
The
spike
recovery
is
acceptable
if
it
is
70%
to
130%.
So,
this
builds
in
a
self­
validation
component
and
requires
that
the
samplers
prove
they
can
spike
and
recover
benzene.
Embarrassingly,
we
are
asking
sampling
companies
to
provide
better
spike
recoveries
than
we
obtained,
on
average,
for
the
compounds
we
spiked
as
a
gas.

Please
contact
me
if
you
have
questions.

Thanks,

DW
David
Word,
Ph.
D.
402
SW
140th
Terrace
Newberry,
Fl
32669
(
352)
331
­
1745
x
241
Fax
(
352)
331
­
1766
D_
Word@
src­
ncasi.
org
DRAFT
REVISED
METHOD
IM/
CAN/
WP­
99.02
March
2003
ii
NCASI
METHOD
IM/
CAN/
WP­
99.02
IMPINGER/
CANISTER
SOURCE
SAMPLING
METHOD
FOR
SELECTED
HAPS
AND
OTHER
COMPOUNDS
AT
WOOD
PRODUCTS
FACILITIES
NCASI
SOUTHERN
REGIONAL
CENTER
JANUARY
2004
i
Acknowledgements
This
method
was
prepared
by
Dr.
MaryAnn
Gunshefski,
Senior
Research
Scientist,
Dr.
David
Word,
Program
Manager,
Jim
Stainfield,
Research
Associate,
and
Steve
Cloutier,
Research
Associate,
at
the
NCASI
Southern
Regional
Center.
Other
assistance
was
provided
by
Terry
Bousquet,
Senior
Research
Scientist,
with
the
NCASI
West
Coast
Regional
Center
and
Richard
Law,
Project
Engineer,
with
the
NCASI
Southern
Research
Center.

For
more
information
about
this
method,
contact:

Dr.
David
Word
Richard
W.
Law
NCASI
NCASI
402
SW
140th
Terrace
402
SW
140th
Terrace
Newberry,
FL
32669
Newberry,
FL
32669
(
352)
331­
1745
ext.
241
(
352)
331­
1745,
ext.
254
FAX
(
352)
331­
1766
FAX
(
352)
331­
1766
e­
mail:
dword@
src­
ncasi.
org
email:
rlaw@
src­
ncasi.
org
Jim
Stainfield
NCASI
402
SW
140th
Terrace
Newberry,
FL
32669
(
352)
331­
1745,
ext.
249
FAX
(
352)
331­
1766
e­
mail:
jstainfield@
src­
ncasi.
org
For
more
information
about
NCASI
publications,
contact:

Publications
Coordinator
NCASI
PO
Box
13318
Research
Triangle
Park,
NC
27709­
3318
(
919)
941­
6411
National
Council
for
Air
and
Stream
Improvement,
Inc.
(
NCASI).
2003.
Methods
Manual,
Impinger/
Canister
Source
Sampling
Method
for
Selected
HAPs
at
Wood
Products
Facilities,
Research
Triangle
Park,
N.
C.:
National
Council
for
Air
and
Stream
Improvement,
Inc.

 
2004
by
the
National
Council
for
Air
and
Stream
Improvement,
Inc.

NCASI's
Mission
To
serve
the
forest
products
industry
as
a
center
of
excellence
for
providing
technical
information
and
scientific
research
needed
to
achieve
the
industry's
environmental
goals.
ii
Disclaimer
THE
MENTION
OF
TRADE
NAMES
OR
COMMERCIAL
PRODUCTS
DOES
NOT
CONSTITUTE
ENDORSEMENT
OR
RECOMMENDATION
FOR
USE.
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
1
NCASI
METHOD
IM/
CAN/
WP­
99.02
IMPINGER/
CANISTER
SOURCE
SAMPLE
METHOD
FOR
SELECTED
COMPOUNDS
AT
WOOD
PRODUCTS
FACILITIES
1.0
Introduction
This
test
method
is
intended
to
measure
a
select
group
of
organic
compounds
that
may
be
present
in
air
emissions
from
stationary
sources
at
wood
products
facilities.
The
organic
compounds
are
captured
in
water
filled
impingers
and
an
evacuated
air
sample
canister.
The
analysis
of
the
impinger
contents
is
performed
by
gas
chromatography/
flame
ionization
detection
and
a
colorimetric
method.
The
analysis
of
the
air
sample
canisters
is
performed
by
gas
chromatography/
mass
selective
detection
as
well
as
gas
chromatography/
flame
ionization
detection.

Procedural
steps
outlined
by
this
method
range
from
optional
to
mandated.
Actions
that
are
not
to
be
performed
are
also
specified.
The
following
terms
will
be
used
within
the
text
of
this
method
in
order
to
clarify
these
activities:

Term:
The
action,
activity,
or
procedural
step
is 
 
must
not .
Prohibited
 
may 
Optional
 
should 
Suggested
 
must 
Required
This
NCASI
impinger/
canister
sampling
system
is
capable
of
accurately
measuring
a
large
number
and
wide
variety
of
organic
compounds
in
forest
products
industry
source
exhausts.
Development
of
this
wide
applicability,
however,
resulted
in
a
complicated
field
sampling
system,
lab
analyses,
and
source
concentration
calculations.
This
revision
to
the
method
incorporates
numerous
quality
control
and
quality
assurance
procedures
intended
to
provide
mills,
sampling
contractors,
and
laboratories
clear
feedback
on
the
quality
of
sampling
conducted.

NCASI
strongly
suggests
that
sampling
contractors
and
laboratories
conduct
spiked
train
sample
runs
and
conduct
full
trial
runs
of
all
sample
train
configurations
prior
to
use
of
this
method
in
the
field.
Failure
to
do
so
will
greatly
increase
the
probability
that
mandated
quality
assurance
criteria
will
not
be
achieved
and
the
sample
results
will
not
be
acceptable.

NCASI
recommends
that
mills,
sampling
contractors,
and
laboratories
carefully
review
this
method
and
all
quality
assurance
procedures
and
criteria
prior
to
source
sampling.
Since
spikes
will
be
used
as
one
of
the
quality
assurance
procedures,
evaluation
of
source
concentration
for
the
analytes
of
interest
needs
to
be
carefully
undertaken
prior
to
manufacture
of
the
spike
solutions.
If
multiple
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
2
and
varied
sources
(
for
example,
inlets
and
outlets
of
control
systems)
are
to
be
sampled,
multiple
spike
solutions
or
varied
spike
volumes
will
likely
be
necessary
to
meet
spiking
criteria.

This
method
shall
be
considered
conducted
only
if
all
quality
assurance
procedures
have
been
performed
and
the
results
clearly
reported
in
the
sampling
report.

2.0
Applicability
This
method
is
applicable
to
determining
the
concentration
of
a
select
group
of
organic
compounds
from
stationary
air
emission
sources
at
wood
products
facilities.
The
select
group
of
organic
compounds
listed
in
Table
2.1
include
hazardous
air
pollutants
(
HAPs),
terpene
compounds,
acetone,
and
cis­
1,2­
dichloroethylene.

2.1
This
method
has
been
structured
to
allow
for
the
determination
of
only
the
desired
compounds
of
interest.
While
Table
2.1
provides
a
complete
list
of
the
compounds
that
are
applicable,
this
method
can
be
utilized
for
smaller
sets
of
compounds
such
as
for
"
Total
HAPs"
(
acetaldehyde,
acrolein,
formaldehyde,
methanol,
phenol
and
propionaldehyde)
as
defined
by
the
Environmental
Protection
Agency
(
EPA)
for
the
wood
products
industry.
For
this
case,
only
three
of
the
four
analytical
procedures
included
in
this
method
will
be
required
to
obtain
the
concentration
of
total
HAPs
in
the
source
gas
being
tested.

This
method
is
not
applicable
for
any
emission
source
that
has
a
moisture
content
greater
than
60%­
by
volume.
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
3
Table
2.1.
Target
HAP
and
Non­
HAP
Analytes
Analysis
Techniques
Impinger
Canister
Analysis
Analysis
Analytes
of
Interest:
HAPs
Technique
Technique
acetaldehyde
[
AQU]
GC/
FID
[
MSD]
GC/
MSD
acrolein
[
AQU]
GC/
FID
[
MSD]
GC/
MSD
benzene
[
MSD]
GC/
MSD
bromomethane
[
MSD]
GC/
MSD
chloroethane
[
MSD]
GC/
MSD
chloroethene
[
MSD]
GC/
MSD
1,2­
dichloroethane
[
MSD]
GC/
MSD
formaldehyde
[
FOR]
Colorimetric
methanol
[
AQU]
GC/
FID
[
MSD]
GC/
MSD
methyl
ethyl
ketone
[
AQU]
GC/
FID
[
MSD]
GC/
MSD
methyl
isobutyl
ketone
[
AQU]
GC/
FID
[
MSD]
GC/
MSD
methylene
chloride
[
MSD]
GC/
MSD
phenol
[
AQU]
GC/
FID
[
MSD]
GC/
MSD
propionaldehyde
[
AQU]
GC/
FID
[
MSD]
GC/
MSD
styrene
[
MSD]
GC/
MSD
toluene
[
MSD]
GC/
MSD
1,2,4­
trichlorobenzene
[
MSD]
GC/
MSD
m,
p­
xylene
[
MSD]
GC/
MSD
o­
xylene
[
MSD]
GC/
MSD
Analytes
of
Interest:
Terpenes
cumene
[
TER]
GC/
FID
camphene
[
TER]
GC/
FID
3­
carene
[
TER]
GC/
FID
p­
cymene
[
TER]
GC/
FID
limonene
[
TER]
GC/
FID
p­
mentha­
1,5­
diene
[
TER]
GC/
FID
alpha­
pinene
[
TER]
GC/
FID
beta­
pinene
[
TER]
GC/
FID
Other
Organic
Analytes
of
Interest:

acetone
[
AQU]
GC/
FID
[
MSD]
GC/
MSD
cis­
1,2­
dichloroethylene
[
MSD]
GC/
MSD
3.0
Principle
and
Methodology
3.1
Principle.
A
sample
of
source
gas
is
drawn
through
three
midget
impingers,
each
containing
chilled
organic
free
water.
A
Teflon­
heated
pump
and
a
critical
orifice
are
used
to
maintain
a
constant
flow
through
the
impingers.
A
portion
of
the
gas
exiting
the
impingers
is
drawn
into
an
evacuated
stainless
steel
canister
to
capture
the
compounds
not
trapped
in
the
aqueous
impingers.
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
4
3.2
Methodology.
The
water
from
the
impingers
is
analyzed
by
direct
injection
into
a
gas
chromatograph
equipped
with
a
flame
ionization
detector
(
GC/
FID),
referenced
as
[
AQU]
in
this
method.

The
formaldehyde
concentration
in
the
impinger
solution
is
determined
by
the
acetylacetone
procedure,
referenced
as
[
FOR]
in
this
method.
This
procedure
involves
the
reaction
of
formaldehyde
with
acetylacetone
to
produce
a
colored
derivative
which
is
measured
by
colorimetric
analysis.

Terpenes
in
the
canister
are
measured
by
a
separate
procedure
from
the
one
used
for
the
non­
terpene
analytes
captured
in
the
canister.
The
terpene
concentration
is
determined
by
drawing
a
sample
from
the
canister
into
a
gas
loop.
The
sample
is
then
directly
injected
into
a
GC/
FID,
referenced
by
[
TER]
in
this
method.
The
concentration
of
the
remaining
organic
compounds
is
obtained
by
drawing
another
sample
from
the
canister
for
pre­
treatment
by
a
cryogenic
preconcentrator.
The
sample
is
then
injected
into
a
gas
chromatograph
equipped
with
a
mass
selective
detector
(
GC/
MSD),
referenced
as
[
MSD]
in
this
method.

Figure
1
provides
a
flow
diagram
of
the
four
analytical
procedures
covered
by
this
method.

3.2.1
Interferences
­
Compounds
present
in
the
source
gas
can
coelute
with
the
analytes
of
interest
during
the
chromatographic
analysis.
These
types
of
interferences
can
be
reduced
by
appropriate
choice
of
GC
columns,
chromatographic
conditions,
and
detectors.
Method
interferences
may
also
be
caused
by
contaminants
in
solvents,
reagents,
glassware
and
other
sample
processing
hardware.

3.2.2
Stability
 
A
formal
stability
study
has
not
been
performed,
but
laboratory
tests
show
that
the
impinger
catch
is
stable
for
approximately
2
weeks
if
kept
refrigerated,
at
which
time
acrolein
begins
to
degrade.
At
room
temperature,
the
acrolein
in
the
impinger
catch
degrades
in
a
matter
of
hours.
The
canister
catch,
in
general,
is
stable
for
3
weeks.

3.2.3
Validation
 
This
method
is
designed
to
be
a
self­
validating
method.
The
quality
assurance
procedures
outlined
in
this
method
are
designed
to
validate
the
performance
of
the
measurement
system
by
the
introduction
of
spike
solutions
and
checking
calibrations
using
standard
solutions.
This
procedure
has
not
been
evaluated
using
the
United
States
Environmental
Protection
Agency
(
EPA)
Method
301,
Field
Validation
of
Emission
Concentrations
from
Stationary
Sources
(
Appendix
A
to
CFR
63).

3.2.4
Analytical
Sensitivity
 
The
sensitivity
of
each
analytical
instrument
will
tend
to
vary
depending
on
characteristics
of
the
laboratory
equipment,
analysis
procedure,
and
compound
being
analyzed.
This
method,
therefore,
has
not
established
one
overall
level
of
sensitivity
for
the
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
5
analytes
present
in
both
the
impinger
and
canister
samples.
Instead,
different
sensitivity
requirements
have
been
established
for
the
[
AQU],
[
FOR],
[
MSD],
and
[
TER]
analytical
procedures.

3.2.4.1
[
AQU]
Method
Detection
Limit
 
This
method
will
require
that
a
method
detection
limit
(
MDL)
be
established
for
each
compound
detected
by
the
[
AQU]
analytical
procedure.
MDLs
must
be
established
as
defined
by
EPA1,
and
the
documentation
should
be
kept
on
file
for
reference.
The
MDL
determined
for
each
compound
must
be
clearly
reported
for
this
method
in
terms
of
the
laboratory
concentration
obtained
in
the
aqueous
sample
(
milligrams
per
Liter,
mg/
L).

As
an
example,
NCASI
conducted
a
formal
detection
limit
study
to
establish
the
[
AQU]
method
detection
limits
in
the
source
gas
tested
(
based
on
75
mL
volume
of
aqueous
impinger
sample
and
400
mL/
min
sample
rate)
for
the
compounds
shown
in
Table
2.1
and
listed
below
in
Table
3.2.

Table
3.2.
Example
of
MDLs
Analyte
NCASI
Method
Detection
Limit
(
ppmv)

Acetaldehyde
0.26
Acrolein
0.16
Methanol
0.35
Methyl
Ethyl
Ketone
0.16
Methyl
Isobutyl
Ketone
0.09
Phenol
0.21
Propionaldehyde
0.18
Acetone
0.18
3.2.4.2
[
FOR]
Method
Detection
Level
 
The
laboratory
sensitivity
level
for
formaldehyde
analysis
will
be
determined
in
a
similar
manner
as
the
procedure
used
to
determine
the
[
AQU]
MDLs.
The
formaldehyde
MDL
must
be
clearly
reported
in
terms
of
mg/
L
in
the
aqueous
sample.

1
Federal
Register,
Part
VIII,
EPA,,
40
CRF
Part
136,
Rules
and
Regulations,
"
Appendix
B
to
Part
136­
Definition
and
Procedure
for
the
Determination
of
the
Method
Detection
Limit"
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
6
As
an
example,
the
formal
detection
limit
study
conducted
by
NCASI
established
that
the
MDL
for
formaldehyde
in
the
source
gas
tested
(
based
on
75
mL
volume
of
aqueous
impinger
sample
and
400
mL/
min
sample
rate)
was
0.13
ppmv.

3.2.4.3
[
MSD]
Measurement
Level
 
A
formal
detection
limit
study
will
not
be
required
to
establish
the
level
of
sensitivity
for
the
compounds
determined
by
the
[
MSD]
analytical
procedure.
Instead,
the
measurement
level
(
ML)
established
for
these
compounds
will
be
set
at
50
parts
per
billion
by
volume
(
ppbv)
in
the
canister.
This
ML
will
be
verified
by
the
lowest
calibration
standard.
If
the
analyte
of
interest
is
detected
by
the
GC/
MSD
below
the
ML,
report
the
concentration
as
<
50
ppbv.

Note
that
the
canister
sample
may
or
may
not
require
dilution
prior
to
the
[
MSD]
analytical
procedure.
If
the
canister
sample
is
diluted,
then
the
actual
source
gas
concentration
will
have
to
be
adjusted
for
dilution.
Clearly
report
the
ML,
the
dilution
factor
(
if
applicable),
and
the
source
gas
detection
level.

NCASI
used
approximately
a
2:
1
dilution
ratio
for
the
canister
analysis.
Using
the
50
ppbv
as
the
ML
for
the
diluted
result,
the
actual
detection
level
for
the
analytes
in
the
source
gas
was
approximately
100
ppbv.

3.2.4.4
[
TER]
Measurement
Level
 
The
laboratory
sensitivity
level
for
terpene
analysis
will
be
based
on
the
measurement
level
of
the
lowest
calibration
standard
or
1000
ppbv.
If
the
analyte
of
interest
is
detected
by
the
GC/
FID
below
the
ML,
report
the
concentration
as
<
1000
ppbv.
The
terpene
samples
are
generally
diluted,
therefore
the
ML
of
the
canister
sample
will
have
to
be
adjusted
for
dilution.
Clearly
report
the
ML,
the
dilution
factor
(
if
applicable),
and
the
source
gas
detection
level.

4.0
Apparatus
4.1
Sampling
­
A
diagram
of
the
sample
collection
train
is
shown
in
Figure
2.
Alternative
configurations
for
the
collection
train
may
be
used
if
approved.
Obtain
approval
prior
to
sample
collection
by
demonstrating
that
the
alternative
collection
train
is
capable
of
meeting
the
QA
sampling
criteria
set
forth
by
this
method
(
Section
6.9).

4.1.1
Heated
Sample
Probe
­
The
sample
probe
is
constructed
of
1/
2
inch
OD
stainless
steel
tubing
or
equivalent.
For
wood
products
sources,
the
probe
is
maintained
at
250
±
25
°
F.
The
probe
inlet
is
placed
near
the
center
of
the
stack
or
duct.
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
7
4.1.2
Heated
Filter
Box
­
The
heated
probe
is
directly
connected
to
a
heated
box
containing
a
Teflon
filter.
The
filter
housing
and
connections
are
made
of
stainless
steel.
A
thermocouple
connected
to
or
within
the
filter
housing
is
used
to
record
the
filter
temperature
which
must
be
maintained
at
250
±
25
°
F.

4.1.3
Sample
Line
­
An
unheated
Teflon
line
is
used
to
convey
the
sample
from
the
back
of
the
heated
filter
box
to
the
first
impinger.

4.1.4
Midget
Impingers
 
The
sample
line
is
connected
to
three
midget
impingers
in
series.
The
first
impinger
is
equipped
with
a
stem
that
has
a
frit
on
the
end
to
improve
gas/
liquid
contact.
The
following
two
impingers
have
regular
tapered
stems.
All
impinger
train
connectors
must
be
glass
and/
or
Teflon.

4.1.5
Filter
­
A
second
Teflon
filter
may
be
used
after
the
impingers
to
prevent
any
fiber,
debris,
or
water
from
accidentally
being
drawn
into
the
critical
orifice.

4.1.6
Variable
Area
Flow
Meter
­
A
flow
meter
should
be
placed
in
line
after
the
impingers
for
a
flow
check
during
sampling.

4.1.7
Flow
Control
Device
­
A
critical
orifice
or
other
approved
device
must
be
used
to
maintain
a
steady
flow
rate
through
the
collection
train.
The
flow
rate
must
be
400
±
100
mL/
min.

4.1.8
Vacuum
Gauges
 
Two
vacuum
gauges
placed
on
each
side
of
the
critical
orifice
capable
of
reading
25
inches
of
mercury
gauge
(
in
Hg).

4.1.9
Teflon
Head
Pump
­
The
critical
orifice
is
followed
by
a
pump,
with
a
Teflon
head,
capable
of
providing
a
vacuum
of
about
18
in
Hg.
Pump
capacity
must
be
sufficient
to
obtain
and
maintain
critical
conditions
at
the
orifice.
The
Teflon
diaphragms
used
in
the
pump
must
be
cleaned
or
replaced
prior
to
each
mill
test
effort.

4.1.10
Canister
Sample
Pickup
Point
 
A
tee
with
an
on/
off
valve
must
be
placed
inline
between
the
sample
pump
exhaust
and
the
excess
source
gas
vent
for
the
pump.
The
canister
will
draw
a
slip­
stream
of
source
gas
at
this
location.

4.1.11
Variable
Area
Flow
Meter
with
a
Flow
Controller
­
A
flow
meter
should
be
placed
in
line
before
the
canister
as
a
visual
aid
for
maintaining
the
sample
delivery
rate
to
the
canister
during
sampling.
The
flow
to
the
canister
will
require
adjustment
periodically
during
sampling
to
ensure
that
the
canister
is
filled
at
a
constant
rate
over
the
sample
run.
The
flow
controller
can
be
a
needle
valve.
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
8
4.1.12
Canisters
­
6
L
SUMMA
 
polished
canister
or
6
L
SilcoSteel
 
canister
is
used
to
collect
a
portion
of
the
sample
gas.
Other
types
of
canisters
can
be
used
if
the
canisters
are
shown
to
have
similar
non­
reactive
properties.

4.1.13
Thermometer
­
An
accurate
thermometer
is
used
to
measure
the
ambient
and
canister
temperatures.

4.1.14
Canister
Gauge
 
An
absolute
pressure
gauge
or
a
vacuum
gauge
capable
of
indicating
±
0.1
in.
Hg
is
placed
after
the
canister
sample
pickup
point
and
before
the
canister.
This
gauge
will
indicate
the
canister
pressure
before
and
after
the
sample
run
as
well
as
during
the
leak
check
procedure.
If
an
absolute
pressure
gauge
is
used,
then
the
barometric
pressure
can
be
obtained
before
and
after
each
sample
run.

4.1.15
Sample
storage
bottles
­
Glass
(
i.
e.,
40
mL
or
larger
VOA
vials)
or
polyethylene
bottles
can
be
used
to
store
the
aqueous
impinger
samples.

4.2
[
AQU]
GC/
FID
analysis
4.2.1
Laboratory
glassware
­
Volumetric
pipets,
volumetric
flasks,
2.0
mL
autosampler
vials,
and
syringes
necessary
for
standards
preparation
and
analysis.

4.2.2
Gas
chromatography
system
­
Gas
chromatography
analytical
system
complete
with
a
temperature­
programmable
gas
chromatograph
suitable
for
splitless
injection
and
all
required
accessories
including
an
autosampler,
syringes,
analytical
columns
and
gases.
The
autosampler
must
be
capable
of
maintaining
the
samples
at
4
°
C
to
prevent
degradation
of
acrolein.

4.2.3
Column
­
30
m
x
0.53
mm
x
3
µ
m
bonded
phase
DB­
624
fused
silica
capillary
column
(
J&
W
Scientific
or
equivalent),
or
other
column
shown
to
be
capable
of
separating
the
analytes
of
interest.

4.2.4
GC
detector
­
Flame
ionization
detector
with
appropriate
data
acquisition
system.

4.3
[
FOR]
Formaldehyde
analysis
4.3.1
Laboratory
glassware
 
Borosilicate
test
tubes
(
5­
to
10­
mL)
with
TFEfluorocarbon
lined
screw
caps,
50­
mL
buret,
volumetric
pipets,
volumetric
flasks,
syringes,
and
cuvettes
necessary
for
standards
preparation
and
analysis.
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
9
4.3.2
Spectrophotometer
­
A
spectrophotometer
capable
of
measuring
absorbance
at
a
412
nm
wavelength.

4.3.3
Absorption
Cell
 
The
absorption
cell
must
have
a
minimum
path
length
of
1.0
cm.
Longer
paths
may
be
used
to
improve
the
sensitivity
of
the
photometer.

4.3.4
Heating
Block
 
Heating
block
or
water
bath
that
can
be
regulated
to
maintain
60
°
±
3
°
C
for
the
test
tubes.

4.3.5
Centrifuge
with
capped
tubes.

4.3.6
Magnetic
stirrer
and
stir
bars.

4.3.7
pH
Meter
conforming
to
the
requirements
of
ASTM
Test
Method
D
1293.

4.4
[
MSD]
GC/
MSD
analysis
4.4.1
Laboratory
glassware
­
Volumetric
pipets,
volumetric
flasks,
and
syringes
necessary
for
standards
preparation
and
analysis.

4.4.2
Cryogenic
concentration
system
­
A
cryogenic
preconcentrator
capable
of
trapping
polar
compounds
is
required
to
concentrate
the
sample
prior
to
introduction
into
the
GC/
MSD
system.

4.4.3
Gas
chromatography
system
­
Gas
chromatography
analytical
system
complete
with
a
temperature­
programmable
gas
chromatograph
suitable
for
split/
splitless
injection
and
all
required
accessories
including
syringes,
analytical
columns
and
gases.

4.4.4
Column
­
60
m
x
0.32
mm
x
0.25
µ
m
bonded
phase
DB­
624
fused
silica
capillary
column
(
J&
W
Scientific
or
equivalent),
or
other
column
shown
to
be
capable
of
separating
the
required
analytes.

4.4.5
Mass
selective
detector
 
A
mass
selective
detector
capable
of
scanning
from
29amu
to
300
amu
every
2
seconds
or
less
using
70
volts
electron
energy
in
the
electron
impact
ionization
mode,
and
appropriate
data
system.

4.5
[
TER]
GC/
FID
analysis
4.5.1
Laboratory
glassware
­
Volumetric
pipets,
volumetric
flasks,
and
syringes
necessary
for
standards
preparation
and
analysis.
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
10
4.5.2
Sample
loop
injection
system
­
A
system
capable
of
extracting
a
sample
from
the
canister
into
a
sample
loop.
The
sample
is
then
directly
injected
into
GC/
FID
system.

4.5.3
Gas
chromatography
system
­
Gas
chromatography
analytical
system
complete
with
a
temperature­
programmable
gas
chromatograph
suitable
for
split/
splitless
injection
and
all
required
accessories
including
syringes,
analytical
columns
and
gases.

4.5.4
Column
­
30
m
x
0.32
mm
x
0.25
µ
m
bonded
phase
DB­
1
fused
silica
capillary
column
(
J&
W
Scientific
or
equivalent),
or
other
column
shown
to
be
capable
of
separating
the
terpenes
of
interest.

4.5.5
GC
detector
­
Flame
ionization
detector
with
appropriate
data
acquisition
system.

5.0
Reagents
5.1
DI
Water
 
Organic
free
or
deionized
(
DI)
water,
is
used
in
the
impingers
as
a
capture
solution,
for
rinsing
the
sample
line
and
impingers
at
the
end
of
the
sample
run,
and
for
preparation
of
all
aqueous
calibration
standards
and
spike
solutions.

5.2
Nitrogen
gas
 
Pure
nitrogen
gas
(
99.999%)
must
be
used
for
cleaning
the
canisters
and
as
the
dilution
gas
for
gas
calibration
standards
and
spike
solutions.
When
preparing
the
gas
calibration
standards
and
spike
solutions,
the
nitrogen
gas
must
be
humidified
by
bubbling
through
DI
water
prior
to
being
added
to
a
canister.

5.3
Purity
of
Reagents
 
Reagent
grade
chemicals
shall
be
used
for
all
tests.
The
reagents
required
by
this
method
shall
conform
to
the
specifications
established
by
the
Committee
on
Analytical
Reagents
of
the
American
Chemical
Society,
where
such
specifications
are
available;
otherwise,
use
the
highest
purity
grade
available.

5.4
[
AQU]
Primary
Stock
Solution
 
Reagent
grade
chemicals
must
be
used
in
the
preparation
of
the
aqueous
primary
stock
solution
for
the
[
AQU]
GC/
FID
analysis
portion
of
this
method.
Prepare
the
[
AQU]
Primary
Stock
Solution
by
combining
aliquots
of
the
compounds
of
interest
listed
in
Table
5.1
in
a
100
mL
volumetric
flask.
Dilute
to
100
mL
with
DI
water.
This
stock
solution
will
be
used
to
prepare
the
[
AQU]
Calibration
Standards
and
the
[
AQU]
Spike
Solution.
The
resulting
[
AQU]
Primary
Stock
Solution
will
have
a
concentration
of
1000
mg/
L.
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
11
Table
5.1.
Reagents
for
the
[
AQU]
Primary
Stock
Solution
Compound
Amount
(
µ
L)
to
Add
to
100
mL
Volumetric
Flask
acetaldehyde
128
acetone
128
acrolein
119
methanol
126
methyl
ethyl
ketone
124
methyl
isobutyl
ketone
125
propionaldehyde
124
phenol
(
solid)
100
mg
5.5
[
AQU]
Calibration
Standards
 
Prepare
a
series
of
aqueous
calibration
standards
from
the
[
AQU]
Primary
Stock
Solution
to
develop
a
calibration
curve
for
each
compound
of
interest.
The
lower
limit
[
AQU]
Calibration
Standard
must
be
0.5
mg/
L.
The
upper
limit
of
the
aqueous
calibration
standards
should
be
1000
mg/
L.

5.6
[
AQU]
Internal
Standards
 
The
aqueous
internal
standard
is
added
to
every
standard,
blank,
matrix
spike,
and
sample
before
analysis
to
compensate
for
variations
in
sample
size
and
is
used
in
determining
relative
response
factors
for
the
target
compounds
analyzed
by
the
[
AQU]
GC/
FID
procedure
used
in
this
method.
The
recommended
[
AQU]
internal
standard
for
this
method
is
cyclohexanol.
Another
internal
standard
that
may
be
used
in
place
of
cyclohexanol
is
2,2,2­
triflouroethanol.

5.6.1
[
AQU]
Internal
Standard
Stock
 
This
internal
standard
will
be
added
to
each
laboratory
blank
and
quality
control
sample
and
calibration
standard.
If
cyclohexanol
is
to
be
added
to
autosampler
vials,
prepare
the
aqueous
internal
standard
stock
solution
by
using
0.312
mL
of
pure
cyclohexanol
and
diluting
to
100
mL
with
DI
water
in
a
100
mL
volumetric
flask.
The
resulting
concentration
of
this
stock
solution
will
be
3000
mg/
L
cyclohexanol.

5.6.2
[
AQU]
Intermediate
Internal
Standard
 
This
internal
standard
will
be
added
to
each
field
sample
bottle
along
with
a
known
volume
of
DI
water
in
the
laboratory
prior
to
sampling.
If
using
cyclohexanol,
prepare
this
intermediate
internal
standard
by
using
3.12
mL
of
pure
cyclohexanol
and
diluting
to
2.0
L
with
DI
water
in
a
2.0
L
volumetric
flask.
The
resulting
concentration
of
this
internal
standard
will
be
1500
mg/
L
cyclohexanol.

5.7
[
FOR]
Primary
Stock
Solution
 
For
this
method,
the
preparation
of
the
primary
stock
solution
for
formaldehyde
will
be
based
on
the
ASTM
Method
D
6303­
98,
"
Standard
Test
Method
for
Formaldehyde
in
Water."
The
formalin
solution
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
12
called
for
by
the
ASTM
method
contains
37%
formaldehyde
by
weight
or
40g
formaldehyde/
100
mL
formalin
solution.
Note
that
formalin
solutions
contain
methanol.

The
[
FOR]
Primary
Stock
Solution
is
made
by
placing
a
2.7
mL
aliquot
of
formalin
solution
(
37%
formaldehyde
by
weight)
in
a
1000
mL
volumetric
flask
and
dilute
to
1000
mL
with
DI
water.
The
formalin
solution
must
be
standardized
per
the
ASTM
method
to
verify
the
formaldehyde
content.
The
primary
stock
solution
should
be
stored
at
room
temperature,
in
the
dark,
and
must
be
standardized
every
six
months.
The
solution
appears
to
be
reasonably
stable.

5.8
[
FOR]
Intermediate
Stock
Solution
­
The
intermediate
stock
solution
must
be
prepared
from
the
[
FOR]
primary
stock
solution
each
time
the
calibration
standards
are
prepared.
Prepare
the
[
FOR]
intermediate
stock
solution
by
placing
a
1.0
mL
aliquot
of
the
[
FOR]
primary
stock
solution
in
a
100
mL
volumetric
flask
and
dilute
to
100
mL
with
DI
water.
The
resulting
[
FOR]
intermediate
stock
solution
will
have
a
formaldehyde
concentration
of
10
mg/
L.

5.9
[
FOR]
Calibration
Standards
 
The
spectrophotometer
used
in
the
colorimetric
analysis
procedure
must
be
calibrated
using
six
different
formaldehyde
concentrations.
The
calibration
standards
will
be
prepared
in
six
screw
capped
test
tubes.
Leave
the
first
test
tube
empty
and
place
0.1,
0.2,
0.4,
1.0,
and
1.5
mL
of
the
[
FOR]
secondary
stock
solution
in
the
second
through
sixth
test
tubes,
respectively.
Fill
all
six
test
tubes
to
2.0
mL
with
DI
water.
The
resulting
concentration
in
the
test
tubes
will
be
0.0,
0.5,
1.0,
2.0,
5.0,
and
7.5
mg/
L
formaldehyde,
respectively.

5.10
[
FOR]
Acetylacetone
Reagent
 
Prepare
by
dissolving
15.4
g
of
ammonium
acetate
in
50
mL
of
DI
water
in
a
100
mL
volumetric
flask.
To
this
solution,
add
0.20
mL
of
pure
acetylacetone
and
0.30
mL
of
aldehyde­
free
glacial
acetic
acid
(
specific
gravity
1.05).
Mix
thoroughly
and
dilute
to
100
mL
with
DI
water.
This
reagent
must
be
stored
in
a
brown
glass
bottle
and
refrigerated.
This
reagent
is
stable
for
a
maximum
of
two
weeks.

5.11
[
MSD]
Primary
Stock
Gas
Mixtures
and
Calibration
Standards
 
The
compounds
that
are
analyzed
by
the
GC/
MSD
technique
are
either
partially
purged
from,
or
not
captured
in,
the
aqueous
impinger
sample.
As
a
consequence,
two
separate
primary
stock
mixtures
will
be
required
to
prepare
the
calibration
standards
for
the
GC/
MSD
analytical
technique.
In
either
case,
the
primary
stock
mixtures
shall
consist
of
the
compounds
of
interest
that
will
be
captured
in
the
canister.

5.11.1
[
MSD]
Aqueous
Analyte
Primary
Stock
Gas
Mixture
 
This
primary
stock
gas
mixture
shall
consist
of
the
compounds
of
interest
that
have
the
potential
to
be
purged
from
the
aqueous
impinger
sample.
These
compounds
are
analyzed
by
both
the
[
AQU]
and
[
MSD]
procedures.
This
primary
stock
gas
mixture
is
made
in
two
steps,
first
an
aqueous
solution
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
13
is
prepared
and
then
an
aliquot
of
the
aqueous
solution
is
converted
to
a
gas
mixture.

The
aqueous
solution
is
prepared
by
adding
the
aliquot
for
each
compound
of
interest
shown
in
Table
5.2
into
a
100
mL
volumetric
flask.
Dilute
this
solution
to
100
mL
with
DI
water.

Table
5.2.
Reagents
for
the
[
MSD]
Aqueous
Analyte
Primary
Stock
Solution
(
gas
phase)

Compound
Amount
(
µ
L)
to
Add
to
100
mL
Volumetric
Flask
acetaldehyde
281
acetone
369
acrolein
334
methanol
202
methyl
ethyl
ketone
(
2­
butanone)
448
methyl
isobutyl
ketone
628
propionaldehyde
360
phenol
(
solid)
439
mg
Then
inject
10
µ
L
of
this
aqueous
stock
solution
into
a
clean
evacuated
canister
(
below
1.0
in
Hga)
along
with
170
µ
L
of
DI
water.
Fill
the
canister
to
60
in
Hga
with
a
nitrogen
gas.
The
resulting
concentration
for
each
compound
in
the
[
MSD]
aqueous
analyte
primary
stock
solution
will
be
1000
ppbv
in
the
canister.

5.11.2
[
MSD]
Aqueous
Analyte
Calibration
Standards
­
Prepare
a
series
of
gas
calibration
standards
for
the
[
MSD]
analysis
technique.
The
lower
limit
of
the
gas
calibration
standards
must
be
50
ppbv.
The
upper
limit
of
the
gas
calibration
standards
should
be
500
ppbv.
The
concentration
of
each
calibration
standard
shall
be
prepared
by
adding
the
appropriate
amount
of
[
MSD]
aqueous
analyte
primary
stock
gas
mixture
to
a
clean
evacuated
(<
1.0
in
Hga)
canister
and
dilute
with
nitrogen
gas
to
40
in
Hga
or
above.

5.11.3
[
MSD]
Gas
Analyte
Primary
Stock
Gas
Mixture
 
This
primary
stock
gas
mixture
shall
consist
of
the
compounds
in
Table
2.1
that
are
not
captured
in
the
aqueous
impinger
sample
as
indicated
by
the
[
MSD]
analysis
technique
only.
The
compounds
of
interest
can
be
obtained
in
gas
phase
directly.
Refer
to
EPA
Compendium
Method
TO­
14
for
possible
list
of
available
compounds.
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
14
The
concentration
of
each
compound
should
be
1000
ppbv
at
a
certified
level
of
Environmental
Protection
Agency
(
EPA)
Traceability
Protocol
Number
1
or
other
approved
certified
level.

5.11.4
[
MSD]
Gas
Analyte
Calibration
Standards
 
Prepare
a
series
of
gas
calibration
standards
for
the
[
MSD]
analysis
technique.
The
lower
limit
of
the
gas
calibration
standards
must
be
50
ppbv.
The
upper
limit
of
the
gas
calibration
standards
should
be
500
ppbv.
The
concentration
of
each
calibration
standard
shall
be
prepared
by
adding
the
appropriate
amount
of
[
MSD]
gas
analyte
primary
stock
gas
mixture
to
a
clean
evacuated
(<
1.0
in
Hga)
canister
and
dilute
with
nitrogen
gas
to
40
in
Hga
or
above.

5.12
[
MSD]
Internal
Standard
 
An
internal
standard
must
be
added
to
the
gas
samples
analyzed
by
the
GC/
MSD
technique.
The
commonly
used
internal
standards
are
bromochloromethane,
1,4­
diflourobenzene,
and
d5­
chlorobenzene.
For
additional
guidance,
refer
to
EPA
Compendium
Method
TO­
14.

The
gas
concentration
of
the
[
MSD]
internal
standard
will
be
at
an
appropriate
level
as
determined
by
the
laboratory
conducting
the
analysis
with
a
recommended
concentration
range
between
100
and
300
ppbv.

5.13
[
TER]
Primary
Stock
Gas
Mixture
 
The
primary
stock
gas
solution
for
the
terpene
compounds
will
be
used
to
make
calibration
standards
for
the
[
TER]
GC/
FID
analysis
technique
in
this
method.
This
stock
solution
is
prepared
in
two
steps,
first
add
the
amount
of
each
terpene
compound
of
interest
shown
in
Table
5.3
into
a
10
mL
volumetric
flask
and
dilute
to
10
mL
with
reagent
grade
ethyl
ether.
Then,
inject
100
µ
L
of
the
terpene/
ethyl
ether
solution
into
a
clean
evacuated
canister
(
below
1.0
in
Hga).
Fill
the
canister
to
60
in
Hga
with
nitrogen
gas.
The
resulting
[
TER]
primary
stock
solution
will
have
a
canister
concentration
of
100
ppmv
for
each
terpene
compound.

Table
5.3.
Reagents
for
the
[
TER]
Primary
Stock
Solution
Compound
Amount
(
µ
L)
to
Add
to
10
mL
Volumetric
Flask
p­
mentha­
1,5­
diene
810
3­
carene
786
cumene
694
p­
cymene
780
limonene
811
 ­
pinene
795
 ­
pinene
793
camphene
(
solid)
809
mg
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
15
5.14
[
TER]
Calibration
Standards
­
Prepare
a
series
of
calibration
standards
from
the
[
TER]
Primary
Stock
Solution.
The
calibration
standards
will
be
used
to
develop
a
calibration
curve
for
each
terpene
compound
of
interest.
The
lowest
calibration
standard
must
have
a
concentration
of
1.0
ppmv.
The
highest
calibration
standard
should
be
300
ppmv.
For
each
concentration,
the
appropriate
amount
of
[
TER]
Primary
Stock
Solution
shall
be
added
to
a
clean
evacuated
gas
cylinder
(
below
1.0
in
Hga)
and
diluted
with
nitrogen
gas
to
60
in
Hga.

5.15
Spike
Solutions
 
This
method
requires
that
quality
assurance
procedures
be
carried
out
to
ensure
that
the
measurement
system
is
capable
of
capturing
the
compounds
of
interest
from
the
emission
source
and
preserving
those
compounds
until
analysis
can
be
conducted.
Spike
solutions
are
used
to
introduce
a
known
quantity
of
reagent(
s)
into
the
measurement
system
operating
under
normal
sampling
conditions.
The
spike
samples
are
collected
and
analyzed
along
with
the
source
samples
collected
by
the
measurement
system.

5.15.1
Aqueous
Spike
Solution
­
The
aqueous
spike
solution
shall
have
the
appropriate
concentration
for
each
compound
of
interest
that
is
equivalent
to
±
50%
of
the
expected
source
gas
concentration.
The
expected
source
gas
concentration
can
be
obtained
from
historical
test
results,
test
results
from
similar
emission
sources,
or
published
emission
factors.
Alternatively,
both
"
low"
and
"
high"
spike
solutions
can
be
used.
In
this
case,
the
two
spike
solutions
are
intended
to
bracket
the
expected
source
gas
concentration.

All
of
the
compounds
of
interest,
except
formaldehyde,
can
be
obtained
from
diluting
the
[
AQU]
primary
stock
solution.
The
formaldehyde
portion
of
the
Aqueous
Spike
Solution
will
come
from
a
dilution
of
the
[
FOR]
primary
stock
solution.
Note
that
the
liquid
volume
contributed
by
the
[
FOR]
primary
stock
solution
will
contain
methanol,
therefore,
the
resulting
methanol
concentration
will
be
higher
than
expected
from
just
methanol
in
the
[
AQU]
primary
stock
solution.

It
is
recommended
that
the
volume
of
the
aqueous
spike
introduced
into
the
spiked
sample
run
(
Section
6.9.3)
and
spiked
train
sample
run
(
Section
6.9.4)
be
1.0
mL.

5.15.2
Prepare
Gas
Spike
Solution
­
The
gas
spike
solution
shall
have
the
appropriate
concentration
of
each
compound
of
interest
that
is
equivalent
to
±
50%
of
the
expected
concentration
for
the
source
gas
being
tested.
The
expected
source
gas
concentration
can
be
obtained
from
historical
test
results,
test
results
from
similar
emission
sources,
or
published
emission
factors.

The
gas
spike
solution
can
be
prepared
by
diluting
the
[
MSD]
gas
analyte
primary
stock
gas
mixture,
the
[
TER]
primary
stock
gas
mixture,
or
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
16
purchasing
a
cylinder
with
the
compounds
of
interest
at
the
desired
concentration.
The
gas
mixtures
can
then
be
diluted
or
stored
undiluted
in
a
cleaned
canister
that
is
pressurized
between
40
and
60
in
Hga
that
will
be
used
as
a
spike
transfer
container.

5.16
Reference
Standards
 
A
reference
standard
is
used
to
validate
each
calibration
curve
developed
for
the
analytical
procedures
in
this
method.
The
reference
standard
can
be
certified
or
from
a
secondary
source.
A
second
source
reference
standard
is
purchased
from
a
different
vendor
than
was
used
to
purchase
the
reagent
used
to
make
the
primary
stock
solution.

The
concentration
for
each
reference
standard
shall
be
equivalent
to
the
midpoint
of
the
reagent's
calibration
curve.
Note
that
an
aliquot
of
internal
standard
solution
must
be
added
to
the
reference
standard
prior
to
analysis.

6.0
Sample
Procedure
Reliable
emission
data
can
be
obtained
through
properly
configuring
and
operating
the
sample
collection
train.
Quality
assurance
measures
provide
verification
that
appropriate
sampling
techniques
were
utilized.
This
section
will
describe
the
assembly
and
operation
of
the
sample
collection
train
and
the
quality
assurance
requirements.

6.1
Preparation
of
the
Sample
Bottles
 
Add
1.0
mL
[
AQU]
intermediate
internal
standard
stock
to
each
sample
bottle
and
dilute
with
74
mL
of
DI
water.
Record
the
pre­
sample
weight
of
each
bottle.

6.2
Sample
Run
 
A
sample
collection
period
preceded
and
followed
by
quality
assurance
checks
as
specified
in
this
method.
It
is
recommended
that
the
duration
of
each
sample
run
be
one
hour.
Sampling
or
source
specific
conditions
may
require,
however,
that
the
collection
time
be
adjusted
to
a
shorter
or
longer
interval.

For
source
types
with
multiple
vents
such
as
press
vents,
a
sample
run
shall
refer
to
all
collection
trains
that
operate
simultaneously.
Control
device
inlets
and
outlets
are
considered
separate
sources.

6.3
Sampling
Event
 
Three
consecutive
sample
runs
conducted
at
one
source
type.

6.4
Preparation
of
the
Collection
Train
 
Prior
to
testing
each
new
emission
source,
clean
the
probe
and
filter
housing
with
DI
water
and
replace
the
filter.
Use
one
pre­
weighed
sample
bottle
for
each
impinger
set.
Record
the
ID
of
the
sample
bottle
and
divide
the
contents
between
the
three
midget
impingers
so
that
each
contains
approximately
25
mL
of
the
aqueous
solution.

Assemble
the
impinger/
canister
collection
train
as
shown
in
Figure
2.
For
sources
that
are
expected
to
have
very
high
amounts
of
moisture
(
40%
to
60%­
by
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
17
volume),
a
fritless
empty
impinger
can
be
used
as
the
first
impinger
(
for
a
total
of
four
impingers)
to
act
as
a
water
drop
out.
Keep
both
the
impingers
and
canister
out
of
direct
sunlight.
Attach
a
thermocouple
to
the
outside
of
the
canister
and
keep
the
canister
valve
closed.

6.5
Leak­
Check
Procedure
 
An
optional
leak
check
can
be
conducted
when
the
collection
train
is
first
assembled
before
the
system
is
brought
up
to
operating
temperature.
A
leak
check
prior
to
starting
the
sample
run
is
mandatory
with
the
collection
train
at
operating
temperature.

The
method
used
for
leak
checking
the
collection
train
will
be
dependent
on
the
configuration
of
the
train.
The
collection
train
shown
in
Figure
2,
for
instance,
has
two
sections
to
leak
check;
the
probe/
impinger
section
and
the
canister
section.
The
probe/
impinger
section
includes
components
from
the
probe
to
the
pump.
The
canister
section
is
from
the
canister
sample
pickup
point
to
the
canister.

The
probe/
impinger
section
and
the
canister
section
will
have
an
acceptable
leak
check
when
the
loss
of
vacuum
is
not
greater
than
1.0
in
Hg
over
a
2.0
minute
period.

6.5.1
Probe/
Impinger
Section
Leak
Check
­
The
leak
check
procedure
shall
be
conducted
when
all
of
the
heated
components
have
reached
operating
temperature
(
250
°
F
±
25
°
F).
The
probe
and
impinger
section
of
the
collection
train
is
leak
checked
by
turning
on
the
sample
pump,
plugging
the
probe
tip,
and
drawing
a
vacuum
of
at
least
15
in.
Hg.
After
15
in.
Hg
has
been
reached,
close
the
inlet
side
of
the
sample
pump
and
turn
the
sample
pump
off.
After
the
pressure
reading
has
stabilized,
note
the
beginning
and
ending
pressure
on
the
vacuum
gauge
over
a
two
minute
period.

Leak
Check
Troubleshooting:
presence
of
bubbles
in
the
first
impinger
indicates
a
leak
located
between
the
probe
and
the
first
impinger:
a
leak
between
the
impingers
or
behind
the
impingers
will
be
indicated
by
aqueous
solution
being
drawn
up
one
of
the
impinger
stems
(
flow
direction
is
backwards
through
the
system).

When
this
section
of
the
collection
train
has
passed
the
leak
check,
slowly
remove
the
plug
at
the
probe
tip.
Bringing
this
section
up
to
ambient
pressure
slowly
will
ensure
that
the
aqueous
solution
remains
distributed
evenly
between
the
impingers.

6.5.2
Canister
Section
Leak
Check
 
Close
the
on/
off
valve
at
the
canister
sample
pickup
point.
Open
the
needle
valve
of
the
flow
meter
to
the
canister.
Open
the
canister
valve
and
allow
the
canister
to
bring
this
section
under
vacuum.
After
the
pressure
reading
in
this
section
equalizes,
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
18
note
the
beginning
and
ending
pressure
readings
on
the
canister
vacuum
gauge
over
a
two
minute
period.
An
alternative
procedure
might
include
a
second
evacuated
canister
that
could
be
used
to
draw
a
vacuum
on
this
section.
This
will
alleviate
the
necessity
for
using
the
sample
canister
for
leak
checking.

If
this
section
passes
the
leak
check,
close
the
canister
valve
and
slowly
open
the
on/
off
valve.
There
should
be
very
little
loss
of
vacuum
(
less
than
0.5
in
Hga)
in
the
canister
since
the
air
volume
in
this
section
of
the
collection
train
is
minimal.

6.6
Pre­
Sample
Run
Procedures
 
6.6.1
Verify
that
the
probe
and
filter
housing
are
at
operating
temperature.
Place
crushed
ice
and
water
around
the
impingers.

6.6.2
Obtain
the
average
of
five
flow
rate
readings
taken
at
the
probe
tip
of
the
collection
train.
The
average
flow
rate
should
be
400
±
100
mL/
min.
Record
the
ambient
temperature
and
pressure
at
this
measurement
location.

6.6.3
Obtain
the
flow
rate
of
the
source
gas
at
the
test
port
using
appropriate
stack
measurement
methods.
Other
source
gas
parameters
required
must
include
stack
gas
temperature,
moisture
content,
static
pressure,
and
percent
O2
and
CO2.

6.6.4
Insert
probe
into
test
port
and
align
perpendicular
to
source
gas
flow.
Recheck
the
operating
temperature.
Close
the
on/
off
valve
at
the
slipstream
pickup
point
for
the
canister
sample,
open
the
canister
valve
to
verify
that
the
canister
pressure
is
less
than
1.0
in
Hga,
and
adjust
the
canister
flow
meter
so
that
it
is
just
barely
open
(
this
will
prevent
excessive
flow
to
the
canister
at
the
start
of
the
sample
run).
Record
the
beginning
canister
pressure
and
temperature.

6.7
Sample
Collection
 
Prior
to
the
start
of
each
sample
run,
coordinate
with
process
operators
to
verify
that
the
production
unit
and
source
gas
being
tested
are
under
steady
state
conditions.

The
collection
train
will
be
started
in
two
steps.
The
first
step
will
involve
purging
ambient
air
from
the
collection
train
by
drawing
sample
gas
through
the
impingers.
The
second
step
will
then
establish
sample
flow
to
the
canister.

6.7.1
Start
the
impinger
sample
pump.
Record
start
time
and
flow
rate
at
the
flow
meter.
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
19
6.7.2
After
one
minute,
open
the
on/
off
valve
at
the
canister
sample
pickup
point
and
adjust
the
flow
rate
to
the
canister.
An
appropriate
flow
rate
will
deliver
a
constant
amount
of
sample
gas
over
the
entire
sample
run.
For
the
6­
L
canisters
and
a
1­
hour
sample
run,
it
is
recommended
that
the
flow
rate
be
100
ml/
min.

6.7.3
At
various
intervals
during
the
sample
run,
record
the
impinger
flow
rate,
canister
flow
rate,
and
the
canister
pressure
and
temperature.

6.7.4
At
the
end
of
the
sample
run,
turn
off
both
the
slip­
stream
valve
and
impinger
sample
pump.
Record
ending
canister
pressure
and
temperature.
Close
the
canister
valve.

6.8
Post­
Sample
Run
Procedures
 
6.8.1
Remove
probe
from
test
port.

6.8.2
Turn
on
the
sample
pump
only
long
enough
to
obtain
the
average
of
five
flow
rate
measurements
at
the
probe
tip.

6.8.3
Verify
that
the
differences
between
pre­
and
post­
average
flow
rate
measurements
are
within
20%.

6.8.4
If
the
difference
is
greater
than
20%
then
examine
the
collection
train
and
determine
if
the
sample
run
is
valid.
A
post­
sample
run
leak
check
may
be
conducted
in
order
to
examine
flow
rate
differences.

6.9
Sample
Recovery
 
6.9.1
Disconnect
the
sample
line
at
the
exit
to
the
heated
filter
box.
Rinse
the
sample
line
with
a
small
amount
of
DI
water
(
approximately
10
mL).
Operate
the
sample
pump
long
enough
to
draw
the
rinse
into
the
first
impinger.

6.9.2
Transfer
the
contents
of
the
impingers
into
the
original
sample
bottle.
Label
the
sample
bottle
appropriately,
mark
water
level,
and
obtain
the
post­
sample
weight
of
the
bottle.
For
high
moisture
sources,
two
sample
bottles
can
be
used.

6.9.3
The
sample
bottles
must
be
stored
on
ice
or
in
a
refrigerator
set
at
approximately
4
°
C.
If
the
water
samples
are
required
to
be
shipped
to
the
laboratory
for
analysis,
pack
the
sample
bottles
in
ice,
do
not
use
frozen
packs.
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
20
6.9.4
Disconnect
the
canister
sample
line
from
the
canister
and
place
the
protection
cap
on
the
canister
valve.
Label
the
canister
appropriately.
Ship
the
canisters
in
a
container
that
will
keep
the
canister
valve
protected.

6.10
Quality
Assurance
Procedures
for
the
Collection
Train
 
The
quality
assurance
(
QA)
measures
used
to
verify
the
performance
of
the
collection
train(
s)
include
conducting
duplicate
sample
runs
and
spiked
sample
runs.
A
QA
sample
run
will
be
conducted
at
the
same
time
as
the
normal
sample
run.

6.10.1
Field
blank
sample
 
There
should
be
at
least
one
field
blank
sample
per
source
tested.
The
first
field
blank
will
be
one
of
the
pre­
weighed
sample
bottles
containing
75
mL
of
solution
(
DI
water
and
internal
standard).
The
field
blank
must
be
analyzed
along
with
the
other
aqueous
samples
collected
by
this
method.

6.10.2
Equipment
blank
sample
 
A
75
mL
sample
of
the
DI
water
must
be
used
for
rinsing
the
collection
train
components
in
the
field.
Note
that
the
internal
standard
will
need
to
be
added
to
the
equipment
blank
at
the
laboratory
prior
to
analysis.
The
equipment
blanks
must
be
analyzed
along
with
the
other
aqueous
samples
collected
by
this
method.

6.10.3
Duplicate
Sample
Run
­
One
duplicate
sample
run
must
be
conducted
per
mill
visit
or
per
sampling
event
for
each
source
type
at
a
mill,
whichever
is
more
stringent.
The
optimal
sampling
configuration
used
to
conduct
a
duplicate
sample
will
be
to
connect
two
separate
collection
trains
to
a
single
probe
and
filter
box
as
shown
in
Figure
3.
Alternative
configurations
for
conducting
a
duplicate
sample
run
can
be
used
if
shown
to
meet
the
QA
criteria.
Duplicate
sample
trains
must
be
configured
such
that
independent
leak
checks
and
flow
rate
measurements
can
be
conducted.

For
source
types
with
multiple
emission
points
being
tested
simultaneously
such
as
press
vents,
this
method
requires
that
a
duplicate
sample
run
be
conducted
at
only
one
of
the
emission
points.
To
provide
additional
QA,
however,
it
is
recommended
that
duplicate
samples
be
collected
at
more
than
one
emission
point
during
a
sampling
event.
Control
device
inlets
and
outlets
are
considered
separate
sources.

6.10.3.1
Duplicate
Sample
Run
Procedure
­
Prepare
both
collection
trains
as
per
Section
6.3.
To
leak
check
the
duplicate
train
shown
in
Figure
3,
disconnect
one
of
the
trains
from
the
outlet
of
the
heated
filter
box.
Cap
that
connection
and
follow
Section
6.4
to
conduct
the
leak
check
procedure
for
the
probe,
filter
box,
and
impinger/
canister
assembly
for
one
train.
For
the
disconnected
impinger/
canister
train,
again
follow
Section
6.4
but
disregard
the
probe
and
filter
portion
of
the
leak
check
procedure.
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
21
Follow
Section
6.5
through
Section
6.8
to
complete
a
duplicate
sample
run
making
sure
that
both
collection
trains
are
started
simultaneously
and
operate
in
a
similar
manner.

The
normal
and
duplicate
samples
are
separate
samples
whereby
the
duplicate
is
collected,
labeled,
and
analyzed
separately
from
the
normal
sample.

6.10.3.2
Duplicate
QA
Criteria
­
Calculate
the
difference
between
the
source
gas
concentration
as
determined
by
the
normal
and
duplicate
trains.
This
difference
is
calculated
by
the
absolute
value
of
the
dry
source
concentration
determined
by
one
sample
train
minus
the
dry
source
concentration
determined
by
the
other
sample
train
divided
by
the
average
dry
source
concentration
determined
from
both
trains
(
Equation
6.1).

(
)
(
)
100
,
%
×
 
=

SD
SN
SD
SN
C
C
Average
C
C
ABS
difference
(
Equation
6.1)

CSN
=
dry
source
gas
concentration
determined
by
the
normal
train,
ppmvd
CSD
=
dry
source
gas
concentration
determined
by
the
duplicate
train,
ppmvd
The
result
is
expressed
as
a
percent
difference
for
each
analyte
and
should
be
less
than
40%.
The
percent
difference
should
not
be
calculated
if
the
concentration
of
the
analyte
determined
by
the
normal
train
or
duplicate
train
has
been
detected
below
the
method
detection
limit.

Results
of
the
duplicate
sample
analysis
must
be
clearly
calculated
and
reported
for
each
analyte.
Identify
each
analyte
that
did
not
meet
the
40
percent
acceptance
criteria.

6.10.3.3
Source
Gas
Concentration
­
The
source
gas
concentration
reported
for
duplicate
sample
runs
will
be
based
on
the
average
of
the
dry
source
gas
concentrations
determined
by
each
collection
train
even
if
the
QA
criteria
is
not
met.

6.10.4
Spiked
Sample
Run
and
Field
Spike
Samples
 
One
spiked
sample
run
must
be
conducted
per
mill
visit
or
per
sampling
event
for
each
source
type
at
a
mill,
whichever
is
more
stringent.
For
the
spiked
sample
run,
a
known
spike
solution
is
introduced
into
one
of
the
two
collection
trains
to
determine
the
percent
recovery
of
the
spike.
The
optimal
sampling
configuration
used
to
conduct
a
spiked
sample
run
will
be
to
connect
two
separate
collection
trains
to
a
single
probe/
filter
box
as
shown
in
Figure
3.
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
22
One
of
the
collection
trains
will
be
equipped
with:
(
1)
a
spike
tee
at
the
inlet
to
the
first
impinger
and
(
2)
an
evacuated
spiked
canister.
The
two
sampling
trains
must
be
configured
such
that
independent
leak
checks
and
flow
rate
measurements
can
be
conducted.

For
source
types
with
multiple
emission
points
being
tested
simultaneously
such
as
press
vents,
this
method
requires
that
a
spiked
sample
run
be
conducted
at
only
one
of
the
emission
points.
To
provide
additional
QA,
however,
it
is
recommended
that
a
spiked
sample
run
be
collected
at
more
than
one
emission
point
during
a
sampling
event.
Control
device
inlets
and
outlets
are
considered
separate
sources.

If
the
analytes
of
interest
are
limited
to
acetaldehyde,
acrolein,
acetone,
formaldehyde,
methanol,
phenol,
methyl
ethyl
ketone,
methyl
isobutyl
ketone,
and
propionaldehyde,
then
substitute
an
unspiked
evacuated
canister
for
the
spiked
canister.

Alternative
configurations
for
conducting
a
spike
sample
run
can
be
used
if
shown
to
meet
the
QA
criteria.

6.10.4.1
Aqueous
Field
Spike
 
For
each
spiked
sample
run,
prepare
an
aqueous
field
spike
by
injecting
an
aliquot
(
1.0
mL)
of
aqueous
spike
solution
(
Section
5.14.1)
into
one
of
the
sample
bottles
containing
DI
water
and
[
AQU]
Internal
Standard.
Clearly
label
the
aqueous
field
spike
and
analyze
with
the
corresponding
aqueous
sample
from
the
spiked
sample
run.
Results
of
the
aqueous
field
spike
must
be
clearly
reported.

6.10.4.2
Spiked
Canisters
and
Gas
Field
Spike
 
Prior
to
going
to
the
field,
prepare
two
spiked
canisters
for
each
spiked
sample
run.
A
spiked
canister
is
prepared
by
injecting
an
aliquot,
for
example
25
mL
at
ambient
pressure,
of
the
gas
spike
solution
(
Section
5.14.2)
into
a
clean
evacuated
canister.
The
gas
spike
solution
can
be
transferred
to
each
spike
canister
using
a
gas
syringe
with
a
valve.
It
is
very
important
to
use
a
consistent
gas
spike
volume
or
record
the
volume
of
spike
(
both
at
ambient
conditions)
that
is
injected
into
each
canister.
Clearly
label
each
spike
canister.

A
gas
field
spike
will
be
required
for
each
spiked
sample
run.
Choose
one
of
the
spiked
canisters
to
be
the
gas
field
spike
and
label
it
as
such.
The
gas
field
spike
will
be
analyzed
along
with
the
spiked
canister
used
for
the
spiked
sample
run.
Results
of
the
gas
field
spike
must
be
clearly
reported.

6.10.4.3
Spiked
Sample
Run
Procedure
 
Prepare
both
collection
trains
as
per
Section
6.3
choosing
one
as
the
spiked
train.
To
leak
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
23
check
the
collection
trains
shown
in
Figure
3,
disconnect
one
of
the
trains
from
the
outlet
of
the
heated
filter
box.
Cap
that
connection
and
follow
Section
6.4
to
conduct
the
leak
check
procedure
for
the
probe,
filter
box,
and
impinger/
canister
assembly
for
one
train.
For
the
disconnected
impinger/
canister
train,
follow
Section
6.4
but
disregard
the
probe
and
filter
portion
of
the
leak
check
procedure.

Follow
Section
6.5
through
Section
6.8
to
complete
a
spiked
sample
run
making
sure
that
both
collection
trains
start
simultaneously
and
operate
in
a
similar
manner.

After
the
start
of
the
run,
inject
an
aliquot
of
the
aqueous
spike
solution
(
Section
5.14.1)
into
the
first
impinger
of
the
spiked
train.
Note
that
the
canister
has
already
been
pre­
spiked.
The
normal
and
spiked
samples
are
separate
samples
whereby
the
spiked
sample
is
collected,
labeled,
and
analyzed
separately
from
the
normal
sample.

6.10.4.4
Spike
Recovery
QA
Criteria
 
The
percent
recovery
of
the
aqueous
spike
and
the
gaseous
spike
will
be
based
on
the
mass
recovered
in
the
spiked
train
(
after
subtraction
of
the
source
gas
contribution
as
shown
in
Figure
4)
divided
by
the
mass
obtained
from
the
field
spikes
(
Equation
6.2).
The
method
used
to
calculate
the
percent
recovery
for
Equation
6.2
is
outlined
in
Figure
4.

Account
for
all
laboratory
and
field
dilutions
in
the
computation
of
the
mass.

100
mass
mass
%

)
i
(
)
i
(
)
i
(
×
=

FS
recovered
Recovery
(
Equation
6.2)

massrecovered(
i)
=
mass
of
analyte
(
i)
recovered
by
the
spiked
collection
train
massFS(
i)
=
mass
of
analyte
(
i)
in
the
aqueous
and
gas
field
spike
The
spike
recovery
is
acceptable
if
the
percent
recovery
is
between
70%
and
130%.
Results
of
the
spiked
sample
run
must
be
clearly
calculated
and
reported
for
each
analyte.
If
the
70
to
130
%
percent
recovery
criteria
are
not
met,
the
analyte(
s)
failing
the
criteria
must
be
listed
and
the
results
clearly
stated
in
the
report.

6.10.5
Spiked
Train
Sample
Run
 
One
spiked
train
sample
run
must
be
conducted
for
each
mill
visit.
This
QA
procedure
can
be
conducted
prior
to
source
testing,
while
in
the
field,
or
after
source
testing.
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
24
If
the
analytes
of
interest
are
limited
to
acetaldehyde,
acrolein,
acetone,
formaldehyde,
methanol,
phenol,
methyl
ethyl
ketone,
methyl
isobutyl
ketone,
and
propionaldehyde
the
gas
spike,
gas
field
spike,
and
spiked
canister
discussed
in
this
section
are
not
needed.

The
spiked
train
sample
run
will
be
conducted
using
only
one
collection
train
attached
to
the
heated
probe
and
filter
box
as
shown
in
Figure
3.
Use
an
unspiked
evacuated
canister.
This
collection
train
will
be
operated
outside
or
independent
of
the
source(
s)
tested.
For
the
spiked
train
sample
run,
both
an
aqueous
spike
and
a
gas
spike,
if
applicable,
are
injected
into
the
probe
tip
of
the
collection
train
to
determine
the
percent
recovery
of
the
spikes.
Care
must
be
taken
to
prevent
introduction
of
any
ambient
organic
contaminants
during
this
procedure;
activated
charcoal
tubes
may
be
used
for
this
purpose.

6.10.5.1
Aqueous
Field
Spike
 
Prepare
an
aqueous
field
spike
by
injecting
an
aliquot
(
1.0
mL)
of
aqueous
spike
solution
(
Section
5.14.1)
into
one
of
the
sample
bottles
containing
DI
water
and
[
AQU]
Internal
Standard.
Clearly
label
the
aqueous
field
spike
and
analyze
with
the
corresponding
aqueous
sample
from
the
spiked
sample
run.

6.10.5.2
Spiked
Canisters
and
Gas
Field
Spike
 
Prior
to
going
to
the
field,
prepare
one
spiked
canister
for
the
spiked
train
sample
run
unless
the
analytes
are
limited
to
the
list
provided
above
in
bold.
A
spiked
canister
is
prepared
by
injecting
an
aliquot,
for
example
25
mL
at
ambient
pressure,
of
the
gas
spike
solution
(
Section
5.14.2)
into
a
cleaned
evacuated
(<
1.0
in
Hga)
canister.
The
gas
spike
solution
can
be
transferred
to
the
canister
using
a
gas
syringe
with
a
valve.
Use
the
same
gas
spike
volume
as
injected
into
the
spiked
canisters
prepared
for
the
spiked
sample
run
(
Section
6.9.3.2).
Clearly
label
this
spike
canister.

The
gas
field
spike
will
be
injected
into
the
probe
tip
of
the
collection
train
using
a
gas
syringe
with
a
valve.
Use
the
same
gas
spike
volume
that
was
injected
into
the
spiked
canister.

6.10.5.3
Spiked
Train
Sample
Run
Procedure
 
Prepare
the
collection
train
as
per
Sections
6.3
and
6.4.
Then
follow
Section
6.5
through
Section
6.8
to
complete
the
spiked
train
sample
run.
The
sample
flow
rate
and
duration
should
be
similar
to
the
sample
runs
conducted
at
the
source.

Note
that
two
spikes
will
be
injected
into
the
probe
tip
of
this
collection
train
unless
the
analytes
are
limited
to
the
list
provided
above
in
bold.
After
the
start
of
the
run,
inject
the
gas
spike
first
NCASI
METHOD
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January
2004
25
over
a
period
of
at
least
5
minutes.
Then
follow
with
the
injection
of
the
aqueous
spike
over
a
period
of
at
least
10
minutes.
It
is
recommended
that
the
aqueous
spike
be
injected
slowly
into
the
heated
probe
tip
over
the
duration
of
the
remaining
sample
run.
Prepare
the
aqueous
and
gas
field
spikes.

6.10.5.4
Spike
Recovery
QA
Criteria
 
The
percent
recovery
of
the
aqueous
spike
and
the
gaseous
spike
will
be
based
on
the
mass
recovered
in
the
spiked
train
divided
by
the
mass
obtained
from
the
field
spikes
(
Equation
6.3).
The
method
used
to
calculate
the
percent
recovery
is
outlined
in
Figure
5.
Account
for
all
laboratory
and
field
dilutions
in
the
computation
of
the
mass.

100
mass
mass
Recovery
%

FS(
i)
ST(
i)
(
i)
×
=
(
Equation
6.3)

massST(
i)
=
mass
of
analyte
(
i)
recovered
by
the
spiked
collection
train
massFS(
i)
=
mass
of
analyte
(
i)
in
the
aqueous
and
gas
field
spike
The
spike
recovery
is
acceptable
if
the
percent
recovery
is
between
70%
and
130%.
Results
of
the
spiked
train
sample
run
must
be
clearly
calculated
and
reported
for
each
analyte.
If
the
70
to
130
%
criteria
are
not
met,
the
analyte(
s)
failing
the
criteria
must
be
listed
and
the
results
clearly
stated
in
the
report.

7.0
Sample
Analysis
Complete
analysis
of
the
impinger
and
canister
samples
will
require
four
analytical
techniques.
If
a
select
group
of
compounds
are
to
be
determined,
then
only
use
the
analytical
techniques
that
are
required
to
obtain
the
desired
concentrations
in
the
aqueous
and
gas
samples.

7.1
Sample
Preparation
 
7.1.0
Aqueous
Impinger
Samples
­
Record
the
laboratory
weight
and
verify
water
level
mark
for
each
sample
bottle
prior
to
analysis.
Note
any
differences.
The
sample
bottles
do
not
need
to
be
at
room
temperature
before
weighing
and
must
remain
cold.

7.1.1
Gas
Canister
Samples
­
Record
the
pressure
of
each
canister
when
delivered
to
the
lab.
If
the
canister
samples
require
dilution,
add
nitrogen
gas
and
record
the
final
pressure
of
the
canister.
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January
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26
7.2
[
AQU]
GC/
FID
Analysis
 
Perform
the
analysis
of
the
compounds
of
interest
in
the
aqueous
impinger
samples
by
direct
aqueous
injection
into
a
GC/
FID.

7.2.1
[
AQU]
GC/
FID
Operating
Parameters
 
Table
1
lists
the
recommended
operating
parameters
for
the
GC/
FID
analysis
of
the
aqueous
samples.
Other
chromatographic
columns
and
conditions
may
be
used
if
it
has
been
established
that
the
compounds
are
adequately
separated,
quality
control
parameters
are
met,
and
no
other
interferences
are
present.
Once
the
GC/
FID
system
has
been
optimized
for
analytical
separation
and
sensitivity,
the
operating
conditions
must
remain
constant
for
the
analysis
of
all
samples,
blanks,
calibration
standards
and
quality
assurance
samples.

Optimal
GC/
FID
operating
conditions
will
produce
distinct
separate
peaks
for
each
analyte
at
established
retention
times.
Verification
of
the
GC/
FID
performance
is
recommended
by
running
an
analysis
of
a
solution
containing
a
high
level
[
AQU]
calibration
standard
and
the
[
AQU]
internal
standard
stock.
Determine
the
retention
time
of
each
analyte
relative
to
the
internal
standard.
If
using
the
recommended
[
AQU]
internal
standard
stock
solution
(
Section
5.6),
place
10
µ
L
into
a
2.0
mL
autosampler
vial
and
fill
the
vial
with
a
high
concentration
[
AQU]
calibration
standard.
The
resulting
concentration
of
the
[
AQU]
internal
standard
in
the
autosampler
vial
will
be
15
mg/
L.

Compare
the
results
with
previously
established
retention
times
for
the
GC/
FID
instrument.
If
the
retention
times
are
significantly
different,
then
adjust
the
[
AQU]
GC/
FID
operating
parameters
to
return
the
retention
times
to
the
established
values.

Troubleshooting
tips:
The
temperature
of
the
samples
in
the
autosampler
must
be
kept
at
4
°
C
to
inhibit
the
degradation
of
acrolein.
Some
possible
interfering
compounds
include
ethanol,
methyl
mercaptan,
dimethyl
sulfide,
and
dimethyl
disulfide.
Also
note
that
constant
injections
of
aqueous
samples
can
cause
water
to
buildup
in
the
system.
This
will
cause
the
retention
times
to
shift
and
the
peaks
to
broaden.
It
is
recommended
that
after
approximately
50
injections
a
bakeout
of
the
system
be
performed.
This
should
consist
of
heating
the
injector
to
250oC,
the
oven
to
over
200oC,
and
the
detector
to
275oC
for
several
hours.

7.2.2
[
AQU]
GC/
FID
Calibration
Curves
 
The
calibration
curves
will
be
based
on
the
analysis
of
the
[
AQU]
calibration
standards
prepared
in
Section
5.5.
Obtain
a
2.0
mL
autosampler
vial
for
each
calibration
standard
and
place
10
µ
L
of
the
[
AQU]
internal
standard
stock
(
Section
5.6)
into
each
vial.
Then
fill
each
vial
with
a
different
[
AQU]
calibration
standard.
The
NCASI
METHOD
IM/
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99.02
January
2004
27
resulting
concentration
of
the
internal
standard
in
the
vials
will
be
15
mg/
L.

Most
analytical
software
will
automatically
generate
calibration
curves
and
verify
the
accuracy
of
each
curve.
Verification
of
a
calibration
curve
shall
be
based
on
the
determination
of
the
relative
standard
deviation
of
the
relative
response
factors
obtained
for
each
analyte
of
interest.
Each
point
on
a
calibration
curve
will
have
a
relative
response
factor
(
RRFM).
The
RRFM
is
calculated
by
Equation
7.1
using
a
relationship
between
the
responses
obtained
for
the
internal
standard
and
analyte.

M
IS
IS
M
M
C
C
x
A
A
RRF
=
(
Equation
7.1)

RRFM
=
Relative
response
factor
for
an
analyte
AM
=
area
of
analyte
peak
AIS
=
area
of
internal
standard
peak
CM
=
concentration
of
analyte
injected
(
mg/
L)
CIS
=
concentration
of
internal
standard
injected
(
mg/
L)

A
calibration
curve
will
be
acceptable
when
the
relative
standard
deviation
of
the
RRFMs
are
less
than
20%.
The
average
RRFM
will
then
be
used
to
calculate
the
concentration
of
an
analyte
in
an
aqueous
sample
by
Equation
7.2.

M
IS
IS
averageRRF
x
A
C
x
S
S
A
C
=
(
Equation
7.2)

CS
=
Concentration
of
the
analyte
in
the
sample,
mg/
L
AS
=
Area
of
the
analyte
peak
in
the
sample
CIS
=
Concentration
of
the
internal
standard,
mg/
L
AIS
=
Area
of
the
internal
standard
peak
in
the
sample
averageRRFM
=
Relative
response
factor
of
analyte
If
the
calibration
curve
is
not
acceptable,
then
reanalyze
the
calibration
solutions
by
developing
another
calibration
curve
and
evaluating
the
relative
standard
deviation.
If
that
evaluation
also
fails,
then
prepare
new
calibration
standards
and/
or
perform
instrument
maintenance.

7.2.3
[
AQU]
GC/
FID
QA
Requirements
 
The
GC/
FID
aqueous
analytical
technique
includes
both
mandatory
and
recommended
laboratory
QA
procedures.
Laboratories
must
report
the
appropriate
QA
results
along
with
the
source
sample
results.
NCASI
METHOD
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99.02
January
2004
28
7.2.3.1
Laboratory
Blank
Sample
­
A
laboratory
blank
sample
must
be
analyzed
prior
to
analysis.
Additional
laboratory
blanks
must
be
included
for
every
20
source
samples
analyzed.
Blank
samples
are
prepared
from
the
DI
water
used
to
prepare
the
internal
and
calibration
standards.
Blank
samples
must
include
the
appropriate
internal
standard.

7.2.3.2
Laboratory
Duplicates
 
One
laboratory
duplicate
of
a
source
sample
will
be
required.
Additional
laboratory
duplicates
will
be
required
for
every
10
source
samples
analyzed.
Duplicates
are
a
replicate
injection
of
the
same
source
sample.
Note
that
these
samples
already
contain
the
internal
standard.

The
percent
difference
of
the
duplicate
concentrations
should
be
within
10%
(
Section
6.9.2.2).

7.2.3.3
Calibration
Verification
Standard
 
The
calibration
verification
standard
shall
be
the
mid­
range
[
AQU]
calibration
standard.
This
calibration
check
must
be
performed
prior
to
analysis,
after
every
10
source
samples
analyzed,
and
at
the
end
of
the
analysis.

Compare
the
concentration
reported
by
the
instrument
with
the
known
concentration
of
the
standard
to
verify
instrument
calibration.
The
percent
recovery
of
the
concentrations
must
be
within
80%
and
120%.
If
it
is
not,
either
prepare
a
new
standard
or
perform
instrument
maintenance.
If
necessary,
re­
calibrate
the
instrument.

7.2.3.4
Reference
Standard
 
Analysis
of
a
reference
standard
(
Section
5.15)
is
required
for
each
analyte
following
the
initial
analysis
of
the
calibration
verification
standard.
The
reference
standard
should
match
the
results
obtained
for
the
calibration
verification
standard
to
demonstrate
optimum
analytical
performance.

Compare
the
concentration
of
the
reference
standard
with
the
concentration
of
the
calibration
verification
standard.
The
percent
recovery
of
the
concentrations
must
be
within
80%
and
120%.
If
it
is
not,
either
prepare
a
new
standard
or
perform
instrument
maintenance.
If
necessary,
re­
calibrate
the
instrument.

7.2.3.5
Laboratory
matrix
spike
samples
­
A
laboratory
matrix
spike
sample
may
be
prepared
with
each
group
of
similar
matrix
type.
Using
the
mean
concentration
determined
by
the
replicate
analyses,
or
the
background
level
determined
from
a
single
measurement,
determine
the
spiking
level
which
will
give
one
to
four
times
the
background.
If
the
background
sample
does
not
NCASI
METHOD
IM/
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99.02
January
2004
29
have
detectable
levels
of
analytes,
spike
the
sample
at
approximately
five
times
the
lowest
calibration
level
of
the
instrument.
Spike
the
sample
with
the
determined
amount
of
the
calibration
standard/
matrix
spike
solution
and
proceed
to
analyze
the
sample
in
the
normal
manner.
The
results
are
acceptable
if
the
calculated
spike
recovery
is
80
to
120%.
In
cases
where
multiple
analytes
are
present,
the
analyte
with
the
highest
concentration
should
govern
the
acceptance
criteria.

7.2.4
[
AQU]
GC/
FID
Source
Sample
Analysis
 
The
concentration
of
the
source
samples
must
be
determined
from
the
calibration
curves
derived
for
the
[
AQU]
GC/
FID
analytical
technique.
Note
that
the
internal
standard
has
already
been
added
to
the
source
samples.

7.3
[
FOR]
Acetylacetone
Colorimetric
Procedure
 
This
analytical
procedure
will
determine
the
concentration
of
formaldehyde
in
the
aqueous
samples.
It
is
based
on
the
ASTM
Method
D
6303­
98.
Note
that
this
procedure
does
not
require
the
use
of
an
internal
standard.
Laboratories
must
report
the
appropriate
QA
results
along
with
the
source
sample
results.

7.3.1
Spectrophotometer
Operating
Parameters
 
The
spectrophotometer
must
be
capable
of
measuring
absorbance
at
412
nanometer
wavelength.

7.3.2
[
FOR]
Calibration
Curve
 
Prepare
the
six
[
FOR]
Calibration
Standards
as
described
in
Section
5.8.
Add
2.0
mL
of
the
acetylacetone
reagent
to
each
test
tube
and
mix
thoroughly.
Place
test
tubes
containing
the
calibration
standards
in
the
water
bath
for
10
minutes
at
60oC.
Then
allow
the
test
tubes
to
cool
to
room
temperature.

The
same
spectrophotometer
absorption
cell
will
be
used
to
analyze
the
six
[
FOR]
calibration
standards.
The
six
concentrations
will
represent
0.0,
0.5,
1.0,
2.0,
5.0,
and
7.5
mg/
L
formaldehyde,
respectively.
Follow
the
spectrophotometer
manufacturer's
instructions
for
calibrating
the
instrument
by
measuring
the
absorbance,
at
412
nm,
for
each
calibration
standard.

The
calibration
curve
should
yield
a
linear
plot
of
the
absorbance
value
versus
the
corresponding
formaldehyde
concentration.
The
linear
plot
must
have
a
correlation
coefficient
that
is
greater
than
0.995.
Determine
the
slope
and
y­
intercept
of
the
curve
to
develop
a
linear
equation
that
must
be
used
to
determine
the
concentration
of
formaldehyde
in
the
source
samples.

Verification
of
the
formaldehyde
calibration
curve
is
not
required
because
the
titration
process
to
determine
the
formaldehyde
content
of
the
formalin
solution,
called
for
by
the
ASTM
method,
is
a
primary
standard.
NCASI
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99.02
January
2004
30
7.3.3
[
FOR]
Formaldehyde
Laboratory
QA
Requirements
 
The
formaldehyde
analysis
includes
both
mandatory
and
recommended
laboratory
QA
procedures.

7.3.3.1
Laboratory
Blank
Sample
­
A
laboratory
blank
sample
must
be
analyzed
prior
to
analysis.
Additional
laboratory
blanks
must
be
included
for
every
20
source
samples
analyzed.
Blank
samples
are
prepared
from
the
DI
water
used
to
prepare
the
internal
and
calibration
standards.
Note
that
the
blank
samples
for
this
analytical
technique
do
not
contain
an
internal
standard.

7.3.3.2
Laboratory
Duplicates
 
One
laboratory
duplicate
of
a
source
sample
will
be
required.
Additional
laboratory
duplicates
will
be
required
for
every
10
source
samples
analyzed.
Duplicates
are
a
replicate
analysis
of
the
same
source
sample.

The
percent
difference
of
the
duplicate
concentrations
should
be
within
10%
(
Section
6.9.2.2).

7.3.3.3
Calibration
Verification
Standard
 
The
calibration
verification
standard
shall
be
the
mid­
range
[
FOR]
calibration
standard.
This
calibration
check
must
be
performed
prior
to
analysis,
after
every
10
source
samples
analyzed,
and
at
the
end
of
the
analysis.

Compare
the
concentration
reported
by
the
instrument
with
the
known
concentration
of
the
standard
to
verify
instrument
calibration.
The
percent
recovery
of
the
concentrations
must
be
within
80%
and
120%.
If
it
is
not,
either
prepare
a
new
standard
or
perform
instrument
maintenance.
If
necessary,
re­
calibrate
the
instrument.

7.3.3.4
Reference
Standard
 
Analysis
of
a
reference
standard
(
Section
5.15)
is
required
following
the
initial
analysis
of
the
calibration
verification
standard.
The
reference
standard
should
match
the
results
obtained
for
the
calibration
verification
standard
to
demonstrate
optimum
analytical
performance.

Compare
the
concentration
of
the
reference
standard
with
the
concentration
of
the
calibration
verification
standard.
The
percent
recovery
of
the
concentrations
must
be
within
80%
and
120%.
If
it
is
not,
either
prepare
a
new
standard
or
perform
instrument
maintenance.
If
necessary,
re­
calibrate
the
instrument.

7.3.4
[
FOR]
Formaldehyde
Source
Sample
Analysis
 
Refer
to
the
ASTM
Method
06303­
98
for
complete
details.
In
summary,
remove
a
2.0
mL
NCASI
METHOD
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99.02
January
2004
31
aliquot
of
the
impinger
sample
and
transfer
to
a
screw­
capped
test
tube.
Add
2.0
mL
of
the
acetylacetone
reagent
and
mix
thoroughly.
Place
test
tube
in
a
water
bath
for
10
minutes
at
60oC.
Allow
test
tubes
to
cool
to
room
temperature.
Transfer
the
cooled
solution
to
an
absorption
cell
and
place
in
the
spectrophotometer
to
measure
the
absorbance
at
412
nm.

Use
the
absorbance
value
obtained
for
each
source
sample
to
calculate
the
formaldehyde
concentration
from
the
calibration
curve
developed
by
this
procedure.

If
the
concentration
of
a
sample
is
above
7.5
mg/
L
after
the
initial
analysis,
remove
an
aliquot
of
the
original
aqueous
sample
and
dilute
accordingly.
Start
the
procedure
over
by
using
the
diluted
source
sample.
Confirm
that
this
concentration
is
within
the
operating
range
of
the
instrument.
Always
dilute
the
aliquot
of
original
source
sample
instead
of
diluting
the
colored
(
derivatized)
solutions.

7.4
[
MSD]
GC/
MSD
Analysis
 
Perform
the
analysis
of
the
canister
samples
by
using
a
cryogenic
preconcentrator
to
concentrate
the
sample
for
injection
into
a
gas
chromatograph
followed
by
a
mass
selective
detector.
The
delivery
of
the
[
MSD]
Internal
Standard
should
be
automated
by
the
preconcentrator.
The
lab
must
insure
that
that
pretreatment
of
the
gas
sample
does
not
remove
the
polar
compounds
of
interest.

7.4.1
[
MSD]
GC/
MSD
Operating
Parameters
 
Table
2
lists
the
recommended
operating
parameters
for
the
preconcentrator
and
the
GC/
MSD
instrument.
Other
chromatographic
columns
and
conditions
may
be
used
if
it
has
been
established
that
the
compounds
are
adequately
separated,
quality
control
parameters
are
met,
and
no
other
interferences
are
present.
Once
the
[
MSD]
GC/
MSD
system
has
been
optimized
for
analytical
separation
and
sensitivity,
the
operating
conditions
must
remain
constant
for
the
analysis
of
all
samples,
blanks,
calibration
standards
and
quality
assurance
samples.

Optimal
[
MSD]
GC/
MSD
operating
conditions
will
produce
distinct
separate
peaks
for
each
analyte
at
established
retention
times.
Verification
of
the
[
MSD]
GC/
MSD
performance
is
recommended
by
running
an
analysis
of
a
solution
containing
a
high
level
[
MSD]
Calibration
Standard
and
the
[
MSD]
Internal
Standard.
Determine
the
retention
time
of
each
analyte
relative
to
the
internal
standard.

Compare
the
results
with
previously
established
retention
times
for
the
[
MSD]
GC/
MSD
instrument.
If
the
retention
times
are
significantly
different,
then
adjust
the
[
MSD]
GC/
MSD
operating
parameters
to
return
the
retention
times
to
the
established
values.
NCASI
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January
2004
32
7.4.2
[
MSD]
GC/
MSD
Calibration
Curves
 
Develop
a
separate
calibration
curve
for
each
compound
being
analyzed
by
the
GC/
MSD
technique.
The
calibration
curves
will
be
based
on
the
analysis
of
the
[
MSD]
Calibration
Standards
prepared
in
Section
5.11.
The
delivery
of
the
[
MSD]
Internal
Standard
should
be
automated
by
the
preconcentrator
for
all
samples
and
QA
requirements.
Most
analytical
software
will
automatically
generate
calibration
curves
and
verify
the
accuracy
of
each
curve.

Verification
of
a
calibration
curve
shall
be
based
on
the
determination
of
the
relative
standard
deviation
of
the
RRFMs
obtained
for
each
analyte
of
interest.
Refer
to
Equation
7.1
(
Section
7.2.2)
to
calculate
the
RRFM
for
each
calibration
point
along
a
calibration
curve.
A
calibration
curve
will
be
acceptable
when
the
relative
standard
deviation
of
the
RRFMs
are
less
than
20%.
Use
the
average
RRFM
to
calculate
the
concentration
of
an
analyte
in
a
gas
sample
by
Equation
7.2
(
Section
7.2.2).

If
the
calibration
curve
is
not
acceptable,
then
reanalyze
the
calibration
solutions
by
developing
another
calibration
curve
and
evaluating
the
relative
standard
deviation.
If
that
evaluation
also
fails,
then
prepare
new
calibration
standards
and/
or
perform
instrument
maintenance.

7.4.3
[
MSD]
GC/
MSD
QA
Requirements
 
The
GC/
MSD
technique
includes
both
mandatory
and
recommended
laboratory
QA
procedures.
Laboratories
must
report
the
appropriate
QA
results
along
with
the
source
sample
results.

7.4.3.1
Laboratory
Blank
Sample
­
A
laboratory
blank
sample
must
be
analyzed
prior
to
analysis.
Additional
laboratory
blanks
must
be
included
for
every
20
source
samples
analyzed.
Blank
samples
are
prepared
from
the
nitrogen
gas
used
to
prepare
the
calibration
standards.

7.4.3.2
Laboratory
Duplicates
 
One
laboratory
duplicate
of
a
source
sample
will
be
required.
Additional
laboratory
duplicates
will
be
required
for
every
10
source
samples
analyzed.
Duplicates
are
a
replicate
injection
of
the
same
source
sample.

The
percent
difference
of
the
duplicate
concentrations
should
be
within
10%
(
Section
6.9.2.2).

7.4.3.3
Calibration
Verification
Standard
 
The
calibration
verification
standard
shall
be
the
appropriate
mid­
range
[
MSD]
calibration
standard.
This
calibration
check
must
be
performed
prior
to
analysis,
after
every
10
source
samples
analyzed,
and
at
the
end
of
the
analysis.
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
33
Compare
the
concentration
reported
by
the
instrument
with
the
known
concentration
of
the
standard
to
verify
instrument
calibration.
The
percent
recovery
of
the
concentrations
must
be
within
80%
and
120%.
If
it
is
not,
either
prepare
a
new
standard
or
perform
instrument
maintenance.
If
necessary,
re­
calibrate
the
instrument.

7.4.3.4
Reference
Standard
 
Analysis
of
a
reference
standard
(
Section
5.15)
is
required
for
each
analyte
following
the
initial
analysis
of
the
calibration
verification
standard.
The
reference
standard
should
match
the
results
obtained
for
the
calibration
verification
standard
to
demonstrate
optimum
analytical
performance.

Compare
the
concentration
of
the
reference
standard
with
the
concentration
of
the
calibration
verification
standard.
The
percent
recovery
of
the
concentrations
must
be
within
80%
and
120%.
If
it
is
not,
either
prepare
a
new
standard
or
perform
instrument
maintenance.
If
necessary,
re­
calibrate
the
instrument.

7.4.3.5
Laboratory
matrix
spike
samples
­
A
laboratory
matrix
spike
sample
may
be
prepared
with
each
group
of
similar
matrix
type.
Using
the
mean
concentration
determined
by
the
replicate
analyses,
or
the
background
level
determined
from
a
single
measurement,
determine
the
spiking
level
which
will
give
one
to
four
times
the
background.
If
the
background
sample
does
not
have
detectable
levels
of
analytes,
spike
the
sample
at
approximately
five
times
the
lowest
calibration
level
of
the
instrument.
Spike
the
sample
with
the
determined
amount
of
the
calibration
standard/
matrix
spike
solution
and
proceed
to
analyze
the
sample
in
the
normal
manner.
The
results
are
acceptable
if
the
calculated
spike
recovery
is
80
to
120%.
In
cases
where
multiple
analytes
are
present,
the
analyte
with
the
highest
concentration
should
govern
the
acceptance
criteria.

7.4.4
[
MSD]
GC/
MSD
Source
Sample
Analysis
 
7.4.4.1
Record
the
temperature
and
pressure
of
each
canister
at
laboratory
conditions.

7.4.4.2
If
dilution
of
a
canister
sample
is
required
for
analysis,
then
fill
the
appropriate
canisters
to
40
in
Hga
or
above
with
nitrogen
gas.
Record
the
final
pressure
and
temperature
of
each
diluted
canister.

7.4.4.3
Using
a
preconcentrator,
inject
a
sample
from
each
canister
into
the
GC/
MSD.
The
concentration
of
the
samples
analyzed
must
be
NCASI
METHOD
IM/
CAN/
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99.02
January
2004
34
determined
from
the
calibration
curves
developed
for
this
procedure.

7.5
[
TER]
GC/
FID
Analysis
 
Perform
the
analysis
of
the
terpene
compounds
collected
in
the
canister
by
using
a
gas
sample
loop
to
introduce
the
gas
sample
into
the
GC/
FID.
Note
that
there
is
no
internal
standard
for
terpene
analysis.

7.5.1
[
TER]
GC/
FID
Operating
Parameters
 
Table
3
lists
the
recommended
operating
parameters
for
the
GC/
FID
analysis
for
terpene
compounds.
Other
chromatographic
columns
and
conditions
may
be
used
if
it
has
been
established
that
the
compounds
are
adequately
separated,
quality
control
parameters
are
met,
and
no
other
interferences
are
present.
Once
the
[
TER]
GC/
FID
system
has
been
optimized
for
analytical
separation
and
sensitivity,
the
operating
conditions
must
remain
constant
for
the
analysis
of
all
samples,
blanks,
calibration
standards
and
quality
assurance
samples.

Optimal
[
TER]
GC/
FID
operating
conditions
will
produce
distinct
separate
peaks
for
each
analyte
at
established
retention
times.
Verification
of
the
[
TER]
GC/
FID
performance
is
recommended
by
running
an
analysis
of
a
solution
containing
a
high
level
[
TER]
calibration
standard.
Determine
the
retention
time
of
each
terpene
compound.
Note
that
there
is
no
internal
standard
used
in
the
terpene
analysis.

Compare
the
results
with
previously
established
retention
times
for
the
[
TER]
GC/
FID
instrument.
If
the
retention
times
are
significantly
different,
then
adjust
the
[
TER]
GC/
FID
operating
parameters
to
return
the
retention
times
to
the
established
values.

7.5.2
[
TER]
GC/
FID
Calibration
Curves
 
Develop
a
separate
calibration
curve
for
each
compound
being
analyzed
by
the
[
TER]
GC/
FID
technique.
The
calibration
curves
will
be
based
on
the
analysis
of
the
[
TER]
calibration
standards
prepared
in
Section
5.14.
Most
analytical
software
will
automatically
generate
the
calibration
curves
and
verify
the
accuracy
of
each
curve.

Verification
of
a
calibration
curve
shall
be
based
on
the
linear
plot
of
the
terpene
concentration
versus
corresponding
GC/
FID
area
count.
Calibration
will
be
acceptable
if
the
correlation
coefficient
for
the
curve
is
greater
than
0.995.
Determine
the
slope
and
y­
intercept
of
the
curve
to
develop
a
linear
equation
that
must
be
used
to
determine
the
concentration
of
terpenes
in
the
source
samples.

If
the
calibration
curve
is
not
acceptable,
then
reanalyze
the
calibration
gas
mixtures
by
developing
another
calibration
curve
and
evaluating
the
NCASI
METHOD
IM/
CAN/
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99.02
January
2004
35
correlation
coefficient.
If
that
evaluation
also
fails,
then
prepare
new
calibration
standards
and/
or
perform
instrument
maintenance.

7.5.3
[
TER]
GC/
FID
QA
Requirements
 
The
[
TER]
GC/
FID
procedure
includes
both
mandatory
and
recommended
laboratory
QA
procedures.
Laboratories
must
report
the
appropriate
QA
results
along
with
the
source
sample
results.

7.5.3.1
Laboratory
Blank
Sample
­
A
laboratory
blank
sample
must
be
analyzed
prior
to
analysis.
Additional
laboratory
blanks
must
be
included
for
every
20
source
samples
analyzed.
Blank
samples
are
prepared
from
the
nitrogen
gas
used
to
prepare
the
calibration
standards.

7.5.3.2
Laboratory
Duplicates
 
One
laboratory
duplicate
of
a
source
sample
will
be
required.
Additional
laboratory
duplicates
will
be
required
for
every
10
source
samples
analyzed.
Duplicates
are
a
replicate
injection
of
the
same
source
sample.

The
percent
difference
of
the
duplicate
concentrations
should
be
within
10%
(
Section
6.9.2.2).

7.5.3.3
Calibration
Verification
Standard
 
The
calibration
verification
standard
shall
be
the
appropriate
mid­
range
[
TER]
calibration
standard.
This
calibration
check
must
be
performed
prior
to
analysis,
after
every
10
source
samples
analyzed,
and
at
the
end
of
the
analysis.

Compare
the
concentration
reported
by
the
instrument
with
the
known
concentration
of
the
standard
to
verify
instrument
calibration.
The
percent
recovery
of
the
concentrations
must
be
within
80%
and
120%.
If
it
is
not,
either
prepare
a
new
standard
or
perform
instrument
maintenance.
If
necessary,
re­
calibrate
the
instrument.

7.5.4
[
TER]
GC/
FID
Source
Sample
Analysis
­
Obtain
a
gas
sample
from
each
canister
and
analyze
using
the
GC/
FID.
The
concentration
of
the
samples
analyzed
must
be
determined
from
the
calibration
curves
developed
for
this
procedure.

7.5.4.1
Record
the
temperature
and
pressure
of
each
canister
at
laboratory
conditions.

7.5.4.2
If
dilution
of
a
canister
sample
is
required
for
analysis,
then
fill
the
appropriate
canisters
to
40
in
Hga
or
above
with
nitrogen
gas.
Record
the
final
pressure
and
temperature
of
each
diluted
canister.
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
36
7.5.4.3
Inject
a
sample
from
each
canister
into
the
GC/
FID.
The
concentration
of
the
samples
analyzed
must
be
determined
from
the
calibration
curves
developed
for
this
procedure.

8.0
Calculations
The
stack
gas
concentration
of
each
analyte
will
be
determined
by
combining
the
data
collected
from
the
sample
train
and
laboratory
analyses.
The
following
calculation
procedure
has
been
provided
as
guidance.
Other
calculation
methods
may
be
used
if
shown
to
be
valid.

This
method
has
been
developed
to
determine
the
emission
source
gas
concentration
of
the
compounds
listed
in
Tables
2.1
and
2.2.
Some
of
these
compounds
will
be
captured
in
the
aqueous
impinger
sample,
some
will
be
collected
in
both
the
aqueous
and
canister
sample,
and
the
rest
will
be
collected
in
the
canister.
The
calculations
provided
determine
the
mass
of
each
compound
captured
in
the
impinger
and
canister
samples
and
the
corresponding
source
gas
concentration.

8.1
Total
Mass
Captured
by
the
Collection
Train
The
total
mass
of
a
compound
is
determined
by
combining
the
mass
captured
in
the
aqueous
sample
with
the
corrected
mass
captured
in
the
canister
sample.
The
procedure
used
to
calculate
the
total
mass
can
also
be
used
to
determine
the
mass
for
the
percent
recovery
calculations
required
by
the
QA
procedures
in
this
method.

8.1.1
Mass
Collected
in
the
Aqueous
Sample
 
The
mass
of
an
analyte
in
the
aqueous
sample
is
determined
by
multiplying
the
aqueous
concentration
of
the
analyte
by
the
volume
of
the
aqueous
sample.

8.1.1.1
Mass
of
Formaldehyde
­
The
formaldehyde
concentration
is
determined
by
a
different
analytical
procedure
than
the
other
compounds
of
interest
in
the
aqueous
sample.
Therefore,
the
mass
of
formaldehyde
in
Equation
1
is
calculated
using
the
final
volume
of
the
aqueous
sample
obtained
by
the
collection
train
(
sample
plus
rinse).

Equation
1:

aqueous
f,
HCOH
aqueous
HCOH,
V
x
mass
C
=

massHCOH,
aqueous
=
mass
of
formaldehyde
in
the
aqueous
sample,
µ
g
CHCOH
=
concentration
of
formaldehyde
in
aqueous
sample,
µ
g/
mL
Vf,
aqueous
=
final
volume
of
aqueous
sample,
mL
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
37
8.1.1.2
Mass
of
[
AQU]
Compounds
­
The
determination
of
the
mass
for
the
remaining
compounds
in
the
aqueous
sample
is
based
on
a
fixed
sample
volume,
100
mL,
and
the
concentration
(
Equation
2).

Equation
2:
mL
100
x
mass
[
AQU]
aqueous
[
AQU],
C
=

mass[
AQU],
aqueous
=
mass
of
[
AQU]
analyte
in
the
aqueous
sample,
µ
g
C[
AQU]
=
concentration
of
analytei
in
the
aqueous
sample,
µ
g/
mL
The
final
volume
of
the
[
AQU]
samples
are
fixed
at
100
mL
because
both
the
[
AQU]
internal
standard
and
the
[
AQU]
primary
stock
solution
were
prepared
in
100
mL.

8.1.2
Mass
Collected
in
the
Canister
 
The
collection
train
only
captures
a
slipstream
of
the
source
gas
in
the
canister
while
the
total
sample
of
the
source
gas
passes
through
the
impingers.
Because
of
this,
the
resulting
mass
collected
in
the
canister
will
have
to
be
adjusted
by
a
correction
factor.

First,
however,
the
mass
of
each
compound
captured
in
the
canister
is
determined
by
multiplying
the
volume
of
the
sample
gas
at
standard
conditions
by
the
concentration
as
determined
by
the
[
MSD]
GC/
MSD
or
[
TER]
GC/
FID
analytical
procedures.
Note
that
the
dry
concentration
in
the
canister
will
only
be
equivalent
to
the
dry
concentration
in
the
source
gas
for
those
compounds
that
are
not
partially
captured
in
the
aqueous
sample
and
for
canister
samples
that
have
not
been
diluted
prior
to
laboratory
analysis.

8.1.2.1
Volume
of
Gas
Sample
in
Canister
 
The
interior
volume
of
the
canister
used
in
this
method
is
6.0
Liters.
Equation
3
calculates
the
volume
of
the
gas
sample
in
the
canister
at
standard
conditions.

Equation
3:

















=
Hg
in
92
.
29
R
528
L
0
.
6
V
std
GS,
GS
GS
P
T

VGS,
std
=
wet
standard
volume
of
gas
sample
at
standard
conditions,
wsL
TGS
=
temperature
of
gas
sample
(
equivalent
to
canister
temperature)
at
laboratory
conditions,
°
R
PGS
=
pressure
of
the
gas
sample
prior
to
analysis,
in
Hga
8.1.2.2
Mass
of
[
MSD]
or
[
TER]
Compounds
in
Canister
Sample
 
Obtain
the
concentration
of
the
compounds
of
interest
in
the
canister
gas
sample
by
the
[
MSD]
GC/
MSD
or
[
TER]
GC/
FID
analytical
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
38
procedures.
Then
combine
the
concentration
with
the
standard
sample
gas
volume
to
calculate
the
mass
of
analyte(
i)
in
the
canister
using
in
Equation
4.

Equation
4:

(
)
(
)

























=
g
g
10
MW
L
24.055
gmole
1
V
10
C
mass
6
(
i)
,
G
9
[
TER]
or
[
MSD]
i,
canister
i,
µ
std
S
massi,
canister
=
mass
of
analyte(
i)
in
the
canister,
µ
g
Ci,
[
MSD]
or
[
TER]
=
concentration
of
[
MSD]
or
[
TER]
analyte
in
wet
canister
sample
gas,
ppbvw
VGS,
std
=
wet
standard
volume
of
gas
sample
at
standard
conditions,
wsL
(
one
atmosphere
and
68
°
F)
MW(
i)
=
molecular
weight
of
analytei,
g/
gmole
8.1.3
Canister
Mass
Correction
Factor
 
A
mass
correction
factor
is
used
to
adjust
the
mass
collected
in
the
canister.
This
correction
factor
is
based
the
ratio
of
the
total
dry
volume
of
source
gas
sampled
through
the
collection
train
to
the
dry
volume
of
the
sample
collected
in
the
canister
at
the
end
of
the
sample
run.

8.1.3.1
Total
Dry
Volume
of
Source
Gas
Sampled
 
This
method
assumes
that
the
flow
rate
of
the
collection
train
is
measured
at
the
probe
tip
using
a
soap­
bubble
meter.
The
ambient
air
entering
the
bubble
meter,
however,
becomes
saturated
from
passing
over
the
surface
of
the
liquid
reservoir.
Therefore,
the
flow
will
have
to
be
corrected
to
dry
conditions
assuming
saturated
conditions
using
the
vapor
pressure
of
water
at
the
ambient
temperature.
Calculate
the
dry
standard
flow
rate
measured
prior
to
and
after
the
sample
run
using
Equation
5.

Equation
5:

















 
=

meas
vap
bar
meas
probe
drystd
probe
T
R
Hg
in
P
P
Q
Q

528
92
.
29
,
,

Qprobe,
drystd
=
dry
standard
flow
rate
measured
at
the
probe
tip
of
the
sample
collection
train,
dsL/
min
Qprobe,
meas
=
actual
flow
rate
measured
at
the
probe
tip
of
the
sample
collection
train,
L/
min
Pbar
=
barometric
pressure
at
flow
rate
measurement
site,
in
Hga
Pvap
=
water
vapor
pressure
in
the
gas
stream
being
measured,
assumed
to
be
saturated
at
ambient
dry
temperature,
in
Hga.
Tmeas
=
ambient
temperature
at
flow
rate
measurement
site,
°
R
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
39
Then,
calculate
the
total
volume
of
source
gas
sampled
by
multiplying
the
average
flow
rate
of
the
collection
train
by
the
duration
of
the
sample
run
using
Equation
6.

Equation
6:

t
Q
Q
drystd
probe
f
drystd
probe
i
drystd
sourcegas
×








+
=
2
V
,
)
(
,
)
(
,

Vsourcegas,
drystd
=
Total
dry
standard
volume
of
source
gas
sampled
by
the
collection
train,
dsL
Q(
i)
probe,
drystd
=
Pre­
sample
run
dry
standard
flow
rate
measured
at
the
probe
tip
of
the
sample
collection
train,
dsL/
min
Q(
f)
probe,
drystd
=
Post­
sample
run
dry
standard
flow
rate
measured
at
the
probe
tip
of
the
sample
collection
train,
dsL/
min
t
=
duration
of
sample
run,
minutes
8.1.3.2
Dry
Volume
of
Canister
Sample
Collected
 
This
parameter
represents
the
volume
of
the
gas
sample
collected
at
the
end
of
the
sample
run.
Determine
the
volume
of
gas
present
in
the
canister
at
the
start
and
end
of
the
of
the
sample
run
using
Equations
7
and
8.
It
is
assumed
that
no
moisture
is
present
in
the
evacuated
canisters.

Equation
7:

















×
=

can
o
can
o
drystd
s
canisterga
o
T
R
Hg
in
P
L
,
,
,
)
(
528
92
.
29
0
.
6
V

V(
o)
canistergas,
drystd
=
dry
standard
canister
gas
volume,
dsL,
at
start
of
sample
run
Po,
can
=
pressure
of
the
canister,
in
Hga,
at
start
of
sample
run
To,
can
=
temperature
of
canister
gas
sample,
°
R,
at
start
of
sample
run
Equation
8:

















 
×
=

can
f
F
vap
can
f
drystd
s
canisterga
f
T
R
Hg
in
P
P
L
,
38
@
,

,
)
(
528
92
.
29
0
.
6
V


V(
f)
canistergas,
drystd
=
dry
standard
canister
gas
volume,
dsL,
at
the
end
of
the
sample
run
P(
f)
can
=
Measured
pressure
of
the
canister,
in
Hga,
at
the
end
of
the
sample
run
Pvap@
38
°
F
=
moisture
correction
for
water
vapor
in
canister
equivalent
to
0.2292
in
Hga;
gas
stream
assumed
saturated
leaving
the
impinger
train
at
38
°
F
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
40
T(
f)
can
=
temperature
of
canister
gas
sample,
°
R,
at
the
end
of
the
sample
run
Then
calculate
the
difference
in
the
pre­
and
post­
canister
volumes
using
Equation
9.

Equation
9:

drystd
s
canisterga
o
drystd
s
canisterga
f
drystd
ple
anistersam
,
)
(
,
)
(
,
c
V
V
V
 
=

Vcanistersample,
drystd
=
dry
standard
volume
of
canister
sample
collected,
dsL
V(
f)
canistergas,
drystd
=
dry
standard
canister
gas
volume
at
the
end
of
the
sample
run,
dsL
V(
o)
canistergas,
drystd
=
dry
standard
canister
gas
volume
at
the
start
of
the
sample
run,
dsL
8.1.3.3
Canister
Mass
Correction
Factor
 
Since
the
volume
of
source
gas
sampled
through
the
probe
tip
of
the
collection
train
is
greater
than
the
sample
volume
sent
to
the
canister,
the
resulting
mass
of
each
analyte
detected
in
the
canister
has
to
be
corrected.
This
mass
correction
factor
is
calculated
by
Equation
10.

Equation
10:

drystd
ple
anistersam
drystd
sourcegas
,
c
,

V
V
CF=

CF
=
canister
mass
correction
factor
Vsourcegas,
drystd
=
Total
dry
standard
volume
of
source
gas
sampled
by
the
collection
train,
dsL
Vcanistersample,
drystd
=
dry
standard
volume
of
canister
sample
collected,
dsL
8.1.4
Total
Mass
Captured
by
the
Collection
Train
 
The
mass
of
the
compounds
collected
in
the
aqueous
sample
will
be
combined
with
the
corrected
mass
collected
in
the
canister
sample
using
Equation
11.
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
41
Equation
11:

(
)
CF
x
mass
mass
canister
i
aqueous
i
,
,
total
,
i
mass
+
=

massi,
total
=
total
mass
of
analyte(
i)
captured
by
the
collection
train,
µ
g
massi,
aqueous
=
mass
of
analyte(
i)
in
the
aqueous
sample,
µ
g
massi,
canister
=
mass
of
analyte(
i)
in
the
canister
sample,
µ
g
CF
=
canister
mass
correction
factor
8.2
Concentration
in
the
Source
Gas
Sample
The
source
gas
concentration
for
each
compound
of
interest
can
be
determined
by
converting
the
total
mass
captured
into
a
dry
gas
volume
equivalent
of
the
pure
compound
and
then
dividing
by
the
total
dry
volume
sampled
by
the
collection
train,
as
shown
by
Equation
12.

8.3
Equation
12:

drystd
sourcegas
i
L
L
,
6
6
total
i,

gas
source
i,
V
10
gmole
L
055
.
24
MW
1
g
10
g
mass
C
































×
=
µ
µ
Ci,
sourcegas
=
concentration
of
analyte(
i)
in
the
source
gas,
ppmvd
massi,
total
=
total
mass
of
analyte(
i)
captured
by
the
collection
train,
µ
g
MW(
i)
=
molecular
weight
of
analytei,
g/
gmole
Vsourcegas,
drystd
=
Total
dry
standard
volume
of
source
gas
sampled
by
the
collection
train,
dsL
9.0
References
Wight,
Gregory
D.
1994.
Fundamentals
of
Air
Sampling,
Lewis
Publishers,
Boca
Raton,
FL.

EPA
Compendium
Method
TO­
14,
"
Determination
of
Volatile
Organic
Compounds
(
VOCs)
in
Ambient
Air
Using
SUMMA
®
Passivated
Canister
Sampling
and
Gas
Chromatographic
Analysis,"
EPA/
600/
4­
89/
017,
June
1988.

Federal
Register,
Part
VIII,
EPA,,
40
CRF
Part
136,
Rules
and
Regulations,
"
Appendix
B
to
Part
136­
Definition
and
Procedure
for
the
Determination
of
the
Method
Detection
Limit."

American
Society
For
Testing
and
Materials,
Designation:
D
6303­
98,
"
Standard
Test
Method
for
Formaldehyde
in
Water,"
March
1999.
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
42
Table
1.
Recommended
Operating
Conditions
for
the
[
AQU]
GC/
FID
Analysis
of
the
Impinger
Samples
Injection:
Direct
(
Splitless)
Injector
Temperature:
170
°
C
Injection
Volume:
1
µ
L
Injection
Liner
Size:
2
mm
id
(
no
packing)
Syringe
Rinse
10
rinses
with
VOC
free
DI
water
FID
Detector
Temperature:
275
°
C
H2
Flow
Rate:
Approx.
50
mL/
min
Air
Flow
Rate:
Approx.
500
mL/
min
Makeup
Gas:
Helium
Makeup
Gas
Flow
Rate:
Approx.
25
mL/
min
Carrier
Gas:
Helium
Carrier
Gas
Flow
Rate:
Constant
pressure
mode
to
give
6
mL/
min
at
room
temperature
Column:
J&
W
DB­
624,
30
m
x
0.53
mm
id
x
3
micron
fused
silica
capillary
column
with
10
m
deactivated
fused
silica
guard
column
Cryogenics:
On
Temperature
Program
°
C:
Initial:
0
°
C
for
3
min
Ramp
1:
5
°
C/
min
to
50
°
C
for
0
minutes
Ramp
2:
70
°
C/
min
to
105
°
C
for
17
minutes
Ramp
3:
70
°
C/
min
to
220
°
C
for
3
minutes
Retention
Time
Order:
Acetaldehyde,
Methanol,
Acrolein,
Propionaldehyde,
Methyl
Ethyl
Ketone,
Methyl
Isobutyl
Ketone,
Cyclohexanol,
Phenol
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
43
Table
2.
Recommended
Operating
Conditions
for
the
Preconcentrator
and
[
MSD]
GC/
MS
Analysis
of
the
Canister
Samples
Cryogenic
Preconcentrator
Sample
Volume
for
Calibration:
500
mL
Module
1
Trap
Temperature:
­
150oC
Module
1
Desorb
Temperature:
20oC
Module
2
Trap
Temperature:
­
10oC
Module
2
Desorb
Temperature:
180oC
Module
3
Trap
Temperature:
­
170oC
Module
3
Inject
Temperature:
100oC
Transfer
Line
Temperature:
100oC
Gas
Chromatograph/
Mass
Selective
Detector
Inlet
Temperature:
180oC
Carrier
Gas:
Helium
Carrier
Gas
Flow
Rate:
Constant
flow
mode
at
2.0
mL/
min
Column:
J&
W
DB­
624,
60
m
x
0.25
mm
id
x
1.4
micron
fused
silica
capillary
column
with
10
m
deactivated
fused
silica
guard
column
Cryogenics:
On
Temperature
Program
°
C:
Initial:
20
°
C
for
3
min
Ramp
1:
3
°
C/
min
to
100
°
C
for
3
minutes
Ramp
2:
5
°
C/
min
to
140
°
C
for
2
minutes
Ramp
3:
7
°
C/
min
to
240
°
C
for
0
minutes
Total
Run
Time:
57
min
Mass
Range
Scan:
29­
250
amu
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
44
Table
3.
Recommended
Operating
Conditions
for
the
[
TER]
GC/
FID
Analysis
of
the
Canister
Samples
Injection:
Split
Injector
Temperature:
180
°
C
Injection
Volume:
2
mL
 
sample
loop
Split
Ratio:
1.5:
1
Split
Flow:
4.8
mL/
min
Total
Flow:
9.8
mL/
min
FID
Detector
Temperature:
250
°
C
H2
Flow
Rate:
40
mL/
min
Air
Flow
Rate:
450
mL/
min
Makeup
Gas:
Helium
Makeup
Gas
Flow
Rate:
45
mL/
min
Carrier
Gas:
Helium
Carrier
Gas
Flow
Rate:
Ramped
pressure
mode.
Initial
pressure
14.0
psi.
Ramp
7
psi/
min
to
9.3.
Initial
flow
3.2
mL/
min.
Column:
J&
W
DB­
1,
30
m
x
0.32
mm
id
x
0.25
micron
fused
silica
capillary
column
with
10
m
deactivated
fused
silica
guard
column
Cryogenics:
Off
Temperature
Program
°
C:
Initial:
55
°
C
for
16
min
Ramp
1:
120
°
C/
min
to
240
°
C
for
2
minutes
Retention
Time
Order:
Cumene,
 ­
pinene,
camphene,
 ­
pinene,
p­
mentha­
1,5­
diene,
3­
carene,
p­
cymene,
limonene
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
45
Figure
1.
Schematic
of
Sample
Analyses
and
Analytes
[
MSD]
GC/
MSD
Analysis
Canister
Analysis
Sampling
Train
[
TER]
GC/
FID
For
Terpenes
[
FOR]
Acetylacetone
Procedure
[
AQU]
GC/
FID
Analysis
Impinger
Analysis
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
46
Figure
2.
Chilled
Impinger/
Canister
Sample
Collection
Trains
Heated
Probe
(
250
F)
Ice
Water
Bath
Heated
Filter
Box
(
250
F)
Filter
Optional
Variable
Area
Flow
Meter
Critical
Orifice
400
mL/
min
Teflon
Head
Pump
Variable
Area
Flow
Meter
Needle
Valve
6L
Canister
Excess
Sample
Gas
Stream
Canister
Sample
On/
Off
Valve
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
47
Figure
3.
Quality
Assurance
Sample
Collection
Trains
Heated
Probe
Filter
Box
F
Pump/
Control
Box
Aqueous
Impingers
SUMMA
Canister
N
Spiked
Train
Sample
Run
Heated
Probe
Filter
Box
F
Pump/
Control
Box
Aqueous
Impingers
D
Run
Duplicate
Duplicate
Sample
Run
F
Pump/
Control
Box
Aqueous
Impingers
N
Run
Normal
Heated
Probe
Filter
Box
F
Pump/
Control
Box
Spike
Tee
(
for
introduction
of
liquid
spike
solution)

S
Run
Spike
Spiked
Sample
Run
F
Pump/
Control
Box
Aqueous
Impingers
N
Run
Normal
Previously
spike
SUMMA
Canister
D
N
S
N
N
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
48
Figure
4.
Percent
Recovery
for
the
Spiked
Sample
Run
Source
Gas
Impingers
Aqueous
Spike
Spike
Canister
ppmvdST(
i)
Convert
to
Source
Gas
Concentration
mg/
L(
i)
ppbvd(
i)
+
Spike
Train
(
ST)

S
Source
Gas
Impingers
Non­
spiked
Canister
ppmvdNT(
i)
Convert
to
Source
Gas
Concentration
mg/
L(
i)
ppbvd(
i)
+
Normal
Train
(
NT)

N
Mass
Recovered
by
Spiked
Train
ppmvdrecovered(
i)
=
ppmvdST(
i)
ppmvdNT(
i)

ppmvdrecovered(
i)
Convert
to
Massrecovered(
i)

Combine
Field
Spike
Mass
(
FS)

Sample
Bottle
Aqueous
Field
Spike
mg/
LAFS(
i)
MassAFS(
i)
S
ppbvdGFS(
i)
MassGFS(
i)
Gas
Field
Spike
MassFS(
i)
=
MassAFS(
i)
+
MassGFS(
i)

%
Recovery(
i)
=
Massrecovered(
i)

MassFS(
i)
Calculate
%
Recovery
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
49
Figure
5.
Percent
Recovery
for
the
Spiked
Train
Sample
Run
Convert
to
Gas
Spike
Concentration
Impingers
Non­
spiked
Canister
ppmvdST(
i)
mg/
L(
i)
ppbvd(
i)
+
Spiked
Train
(
ST)

N
Aqueous
Spike
Gas
Spike
Convert
to
ppmvdST(
i)
Mass
ST(
i)

Sample
Bottle
Aqueous
Field
Spike
mg/
LAFS(
i)
MassAFS(
i)
S
ppbvdGFS(
i)
MassGFS(
i)
Gas
Field
Spike
MassFS(
i)
=
MassAFS(
i)
+
MassGFS(
i)
Combine
Field
Spike
Mass
(
FS)

%
Recovery(
i)
=
MassFS(
i)
MassST(
i)
Calculate
%
Recovery
NCASI
METHOD
IM/
CAN/
WP­
99.02
January
2004
50
EXAMPLE
FIELD
DATA
COLLECTION
SHEET
SAMPLER
DATE:
CANISTER
ID#
CAN
CODE:

SAMPLING
CODE:
FIELD
SPKIE
Y
N
gas____
mL
aqueous_____
mL
DESCRIPTION:

SECTION
1a
SECTION
1b
SECTION
2
SECTION
3
SECTION
4
SECTION
5
LEAK
CHECK
1
2
3
4
5
AVG
%
DIFFERENCE
%
DIFFERENCE
°
F
in.
Hga
°
F
in.
Hga
LEFT
VAC.
GA.
VENT
TIME
FLOW
(
mL/
min)
(
in.
Hga)
TIME
P
(
in
Hga)
FLOW
(
mL/
min)
TEMP
°
F
FLOW
(
mL/
min)

START
5
10
15
20
25
30
35
40
45
50
55
STOP
COMMENTS:
AMBIENT
TEMPERATURE
/
PRESSURE
IMPINGER
CANISTER
PRE­
RUN
POST­
RUN
PRE­
RUN
POST­
RUN
PRE­
RUN
POST­
RUN
FINAL
DIFFERENCE
PROBE
SAMPLE
FLOW
RATES
COMBINED
TRAIN
FLOW
RATES
PRESSURE
INITIAL
TRAIN
SPIKE
NCASI
HAPS
TRAIN
FIELD
DATA
SHEET
