9060A
)
1
Revision
1
August
2002
METHOD
9060A
TOTAL
ORGANIC
CARBON
1.0
SCOPE
AND
APPLICATION
1.1
Method
9060
is
used
to
determine
the
concentration
of
organic
carbon
in
ground
water,
surface
and
saline
waters,
and
domestic
and
industrial
wastes.
Some
restrictions
are
noted
in
Sections
2.0
and
3.0.

1.2
Method
9060
is
most
applicable
to
measurement
of
organic
carbon
above
1
mg/
L.

2.0
SUMMARY
OF
METHOD
2.1
Organic
carbon
is
measured
using
a
carbonaceous
analyzer.
This
instrument
converts
the
organic
carbon
in
a
sample
to
carbon
dioxide
(
CO
2)
by
either
catalytic
combustion
or
wet
chemical
oxidation.
The
CO
2
formed
is
then
either
measured
directly
by
an
infrared
detector
or
converted
to
methane
(
CH
4)
and
measured
by
a
flame
ionization
detector.
The
amount
of
CO
2
or
CH
4
in
a
sample
is
directly
proportional
to
the
concentration
of
carbonaceous
material
in
the
sample.

2.2
Carbonaceous
analyzers
are
capable
of
measuring
all
forms
of
carbon
in
a
sample.
However,
because
of
various
properties
of
carbon­
containing
compounds
in
liquid
samples,
the
manner
of
preliminary
sample
treatment
as
well
as
the
instrument
settings
will
determine
which
forms
of
carbon
are
actually
measured.
The
forms
of
carbon
that
can
be
measured
by
Method
9060
are:

1.
Soluble,
nonvolatile
organic
carbon:
e.
g.,
natural
sugars.

2.
Soluble,
volatile
organic
carbon:
e.
g.,
mercaptans,
alkanes,
low
molecular
weight
alcohols.

3.
Insoluble,
partially
volatile
carbon:
e.
g.,
low
molecular
weight
oils.

4.
Insoluble,
particulate
carbonaceous
materials:
e.
g.,
cellulose
fibers.

5.
Soluble
or
insoluble
carbonaceous
materials
adsorbed
or
entrapped
on
insoluble
inorganic
suspended
matter:
e.
g.,
oily
matter
adsorbed
on
silt
particles.

2.3
Carbonate
and
bicarbonate
are
inorganic
forms
of
carbon
and
must
be
separated
from
the
total
organic
carbon
value.
Depending
on
the
instrument
manufacturer's
instructions,
this
separation
can
be
accomplished
by
either
a
simple
mathematical
subtraction,
or
by
removing
the
carbonate
and
bicarbonate
by
converting
them
to
CO
2
with
degassing
prior
to
analysis.

3.0
INTERFERENCES
3.1
Carbonate
and
bicarbonate
carbon
represent
an
interference
under
the
terms
of
this
test
and
must
be
removed
or
accounted
for
in
the
final
calculation.
9060A
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August
2002
3.2
This
procedure
is
applicable
only
to
homogeneous
samples
which
can
be
injected
into
the
apparatus
reproducibly
by
means
of
a
microliter­
type
syringe
or
pipet.
The
openings
of
the
syringe
or
pipet
limit
the
maximum
size
of
particle
which
may
be
included
in
the
sample.

3.3
Removal
of
carbonate
and
bicarbonate
by
acidification
and
purging
with
nitrogen,
or
other
inert
gas,
can
result
in
the
loss
of
volatile
organic
substances.

4.0
APPARATUS
AND
MATERIALS
4.1
Apparatus
for
blending
or
homogenizing
samples:
Generally,
a
Waring­
type
blender
is
satisfactory.

4.2
Apparatus
for
total
and
dissolved
organic
carbon:

4.2.1
Several
companies
manufacture
analyzers
for
measuring
carbonaceous
material
in
liquid
samples.
The
most
appropriate
system
should
be
selected
based
on
consideration
of
the
types
of
samples
to
be
analyzed,
the
expected
concentration
range,
and
the
forms
of
carbon
to
be
measured.

4.2.2
No
specific
analyzer
is
recommended
as
superior.
If
the
technique
of
chemical
oxidation
is
used,
the
laboratory
must
be
certain
that
the
instrument
is
capable
of
achieving
good
carbon
recoveries
in
samples
containing
particulates.

5.0
REAGENTS
5.1
ASTM
Type
II
water
(
ASTM
D1193):
Water
should
be
monitored
for
impurities,
and
should
be
boiled
and
cooled
to
remove
CO
2.

5.2
Potassium
hydrogen
phthalate,
stock
solution,
1,000
mg/
L
carbon:
Dissolve
0.2128
g
of
potassium
hydrogen
phthalate
(
primary
standard
grade)
in
Type
II
water
and
dilute
to
100.0
mL.

NOTE:
Sodium
oxalate
and
acetic
acid
are
not
recommended
as
stock
solutions.

5.3
Potassium
hydrogen
phthalate,
standard
solutions:
Prepare
standard
solutions
from
the
stock
solution
by
dilution
with
Type
II
water.

5.4
Carbonate­
bicarbonate,
stock
solution,
1,000
mg/
L
carbon:
Weigh
0.3500
g
of
sodium
bicarbonate
and
0.4418
g
of
sodium
carbonate
and
transfer
both
to
the
same
100­
mL
volumetric
flask.
Dissolve
with
Type
II
water.

5.5
Carbonate­
bicarbonate,
standard
solution:
Prepare
a
series
of
standards
similar
to
Step
5.3.

NOTE:
This
standard
is
not
required
by
some
instruments.

5.6
Blank
solution:
Use
the
same
Type
II
water
as
was
used
to
prepare
the
standard
solutions.
9060A
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2002
6.0
SAMPLE
COLLECTION,
PRESERVATION,
AND
HANDLING
6.1
Sampling
and
storage
of
samples
in
glass
bottles
is
preferable.
Sampling
and
storage
in
plastic
bottles
such
as
conventional
polyethylene
and
cubitainers
is
permissible
if
it
is
established
that
the
containers
do
not
contribute
contaminating
organics
to
the
samples.

NOTE:
A
brief
study
performed
in
the
EPA
Laboratory
indicated
that
Type
II
water
stored
in
new,
1­
qt
cubitainers
did
not
show
any
increase
in
organic
carbon
after
2
weeks'
exposure.

6.2
Because
of
the
possibility
of
oxidation
or
bacterial
decomposition
of
some
components
of
aqueous
samples,
the
time
between
sample
collection
and
the
start
of
analysis
should
be
minimized.
Also,
samples
should
be
kept
cool
(
4
E
C)
and
protected
from
sunlight
and
atmospheric
oxygen.

6.3
In
instances
where
analysis
cannot
be
performed
within
2
hr
from
time
of
sampling,
the
sample
is
acidified
(
pH
<
2)
with
HCl
or
H
2
SO
4.

7.0
PROCEDURE
7.1
Homogenize
the
sample
in
a
blender.

NOTE:
To
avoid
erroneously
high
results,
inorganic
carbon
must
be
accounted
for.
The
preferred
method
is
to
measure
total
carbon
and
inorganic
carbon
and
to
obtain
the
organic
carbon
by
subtraction.
If
this
is
not
possible,
follow
Steps
7.2
and
7.3
prior
to
analysis;
however,
volatile
organic
carbon
may
be
lost.

7.2
Lower
the
pH
of
the
sample
to
2.

7.3
Purge
the
sample
with
nitrogen
for
10
min.

7.4
Follow
instrument
manufacturer's
instructions
for
calibration,
procedure,
and
calculations.

7.5
For
calibration
of
the
instrument,
a
series
of
standards
should
be
used
that
encompasses
the
expected
concentration
range
of
the
samples.

7.6
Quadruplicate
analysis
is
required.
Report
both
the
average
and
the
range.

8.0
QUALITY
CONTROL
8.1
All
quality
control
data
should
be
maintained
and
available
for
easy
reference
or
inspection.

8.2
Employ
a
minimum
of
one
blank
per
sample
batch
to
determine
if
contamination
or
any
memory
effects
are
occurring.

8.3
Verify
calibration
with
an
independently
prepared
check
standard
every
15
samples.

8.4
Run
one
spike
duplicate
sample
for
every
10
samples.
A
duplicate
sample
is
a
sample
brought
through
the
whole
sample
preparation
and
analytical
process.
9060A
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Revision
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August
2002
9.0
METHOD
PERFORMANCE
9.1
Precision
and
accuracy
data
are
available
in
Method
415.1
of
Methods
for
Chemical
Analysis
of
Water
and
Wastes.

10.0
REFERENCES
1.
Annual
Book
of
ASTM
Standards,
Part
31,
"
Water,"
Standard
D
2574­
79,
p.
469
(
1976).

2.
Standard
Methods
for
the
Examination
of
Water
and
Wastewater,
14th
ed.,
p.
532,
Method
505
(
1975).
9060A
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Revision
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August
2002
A
