Document ID: EPA-HQ-RCRA-2002-0029-0009
Agency: epa
Document Type: Supporting & Related Material
Title: 
Posted Date: 2003-01-29T05:00Z

EVALUATION
OF
VALUATION
TREATMENT
OF
REATMENT
BULK
ULK
ELEMENTAL
LEMENTAL
MERCURY
ERCURY
D­
1
APPENDIX
D.
ANALYTICAL
PROTOCOLS,
TECHNICAL
BACKGROUND
DOCUMENT:
MERCURY
WASTES,
EVALUATION
OF
TREATMENT
OF
BULK
ELEMENTAL
MERCURY,
FINAL
REPORT
FEBRUARY
8,
2002
SUBMITTED
FOR:
U.
S.
ENVIRONMENTAL
PROTECTION
AGENCY
ARIEL
RIOS
BUILDING
OFFICE
OF
SOLID
WASTE
1200
PENNSYLVANIA
AVENUE,
N.
W.
WASHINGTON,
D.
C.
20460
SUBMITTED
BY:
SCIENCE
APPLICATIONS
INTERNATIONAL
CORPORATION
ENGINEERING
AND
ENVIRONMENTAL
MANAGEMENT
CORP.
11251
ROGER
BACON
DRIVE
RESTON,
VIRGINIA
20190
EPA
CONTRACT
NO.
68­
W­
98­
025
WORK
ASSIGNMENT
NO.
3­
8
SAIC
PROJECT
NO.
06­
0758­
08­
1373­
000
ANALYTICAL
NALYTICAL
PROTOCOLS
ROTOCOLS
D­
2
APPENDIX
D.
ANALYTICAL
PROTOCOLS
SOP
Titles
Procedure
for
the
Determination
of
Ammonium
Acetate
Extractable
Calcium,
Magnesium,
Sodium
and
Potassium
in
SoilD­
3
Undisturbed
Bulk
Density
Analytical
ProcedureD­
10
Determining
the
Cation
Exchange
Capacity
(
CEC)
of
SoilD­
12
pH
Analytical
ProcedureD­
14
Determining
the
Acidity
of
SoilD­
17
Hydraulic
Conductivity
 
Constant
Head
MethodD­
20
Texture
Procedure
 
Pipette
MethodD­
23
Redox
Potential
of
a
Soil
SampleD­
28
Cation­
Exchange
Capacity
by
Sodium
Saturation
in
Calcareous
SoilsD­
31
Determination
of
Total
Organic
Carbon
in
Soil
by
CombustionD­
35
1/
3
Bar
 
German
MethodD­
38
ChloridesD­
39
EVALUATION
OF
VALUATION
TREATMENT
OF
REATMENT
BULK
ULK
ELEMENTAL
LEMENTAL
MERCURY
ERCURY
D­
3
This
page
intentionally
left
blank.
D­
4
AGVISE
Laboratories,
Inc.
NORTHWOOD,
ND
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.12.13
SOP
TITLE:
Procedure
for
the
Determination
of
Ammonium
Acetate
Extractable
Calcium,
Magnesium,
Sodium
and
Potassium
in
Soil
REVISED
BY:
Larry
Wikoff
TITLE:
Nutrient
Laboratory
Manager
REPLACES
SOP
NUMBER:
NUT.
02.12.12
REASON
FOR
REVISION:
Add
use
of
ICP
to
method.

APPROVALS:

Larry
Wikoff
Date
Julie
M.
Johnson
Date
Nutrient
Laboratory
Manager
Quality
Assurance
Manager
Robert
Deutsch
Date
Robert
Wallace
Date
President
CEO
Effective
Date
PURPOSE:
To
define
the
analytical
method
used
to
determine
soil
cation
exchange
capacity.
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.12.13
SOP
TITLE:
Procedure
for
the
Determination
of
Ammonium
Acetate
Extractable
Calcium,
Magnesium,
Sodium
and
Potassium
in
Soil
D­
5
PROCEDURE:
1.
To
extract
the
samples,
use
a
1.0
gm
soil
scoop
to
transfer
the
sample
to
50
ml
Erlenmeyer
flasks
in
Potassium
extraction
tray,
according
to
SOP
NUT.
06.02
 
"
Soil
Scoop
Procedure."
Scoop
a
check
sample
after
the
last
sample
in
each
tray.

2.
Use
an
appropriate
dispenser
or
a
dispenser
pump
to
add
10.0
ml
of
Potassium
Extracting
Solution
to
each
sample.
For
each
batch
of
samples,
check
one
aliquot
with
a
graduated
cylinder
to
determine
the
actual
volume
dispensed
and
record
the
volume
on
the
raw
data
lab
sheet.
This
volume
is
to
be
at
10.0
ml
or
reject
and
recalibrate
and
check
volume
again.

3.
Shake
for
5
minutes
at
200
(
±
10%)
epm
on
a
mechanical
shaker.

4.
Filter
through
sodium­
free
9
cm
filter
paper
into
an
ICP
filtering
tray
or
into
plastic
cups
in
Potassium
filter
trays,
labeled
the
same
as
the
extracting
tray.

5.
Remove
the
filter
papers
and
read
the
extract
on
the
ICP
according
to
SOP
NUT.
01.25
 
"
Optima
3000
&
3100
Operating,
Calibration
and
Maintenance
Procedure"
and
SOP
NUT.
02.93
 
"
Determination
of
Ammonium
Acetate
Extractable
Calcium,
Magnesium,
Sodium,
and
Potassium
for
Cation
Exchange
Capacity
using
ICP".
Record
the
results
on
the
raw
data
lab
sheet
or
capture
electronically.
For
all
samples:
Read
the
standards
after
every
tray.
If
the
read
standard
is
more
than
±
10%
of
the
known
standard,
the
run
must
be
retested
Record
the
standard
readings
on
the
raw
data
lab
sheet.
The
check
sample
must
fall
within
the
limits
set
in
SOP
NUT.
04.03
 
"
The
Use
and
Ranges
of
Check
Soil".

6.
Samples
may
also
be
analyzed
using
the
Atomic
Absorption
Spectrophotometer.
Use
Steps
6
through
10
when
using
the
Atomic
Absorption
Spectrophotometers.
Read
the
extracts
for
Potassium
and
Sodium
on
the
Atomic
Absorption
Spectrophotometer,
according
to
SOP
NUT.
01.21
 
"
Atomic
Absorption
Spectrophotometer
Operating
Procedure
 
Buck
Scientific
Models"
&
NUT.
01.23
 
"
Atomic
Absorption
Spectrophotometer
Operating
Procedure
 
Perkin­
Elmer
100".

7.
For
Calcium
and
Magnesium:
A)
To
prepare
samples,
use
either
step
a),
b),
or
c).
a)
Use
a
1000
µ
l
auto­
pipet
to
take
a
1.00
ml
aliquot
of
each
sample,
transferring
them
to
cups
in
a
CEC
tray,
numbered
the
same
as
the
Potassium
tray.
Use
a
pipet
or
dispenser
to
add
1.00
ml
of
2%
Lanthanum
Chloride
Solution.
Use
a
dispenser
to
add
8.00
ml
of
deionized
water.
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.12.13
SOP
TITLE:
Procedure
for
the
Determination
of
Ammonium
Acetate
Extractable
Calcium,
Magnesium,
Sodium
and
Potassium
in
Soil
D­
6
b)
Use
the
Hamilton
Microlab
Dilutor
to
dispense
1000
µ
l
of
sample
and
9000
µ
l
of
the
1:
9
Dilution
of
2%
Lanthanum
Chloride
Solution.
c)
Use
a
1000
µ
l
auto­
pipet
to
take
a
1.00
ml
aliquot
of
each
sample,
transferring
them
to
cups
in
a
CEC
tray,
numbered
the
same
as
the
Potassium
tray.
Use
a
dispenser
to
add
9.00
ml
of
the
1:
9
Dilution
of
2%
Lanthanum
Chloride
Solution.

B)
Read
on
the
Atomic
Absorption
Spectrophotometer,
according
to
SOP
NUT.
01.21
 
"
Atomic
Absorption
Spectrophotometer
Operating
Procedure
 
Buck
Scientific
Models"
&
NUT.
01.23
 
"
Atomic
Absorption
Spectrophotometer
Operating
Procedure
 
Perkin­
Elmer
100".

C)
Record
the
results
on
the
raw
data
lab
sheet
or
capture
electronically.
a)
If
the
samples
are
low
in
calcium
and/
or
magnesium
and
levels
can
not
be
detected,
the
following
procedure
may
be
used:
1)
Use
a
1
gm
soil
scoop
and
transfer
soil
two
times
for
a
total
of
2
gm
of
soil
to
an
Erlenmeyer
flask
in
a
potassium
extraction
tray.
Use
an
appropriate
dispenser
and
add
20
ml
of
Potassium
Extracting
Solution
to
each
sample.
Shake
for
5
minutes
on
a
mechanical
shaker.
Filter
through
11
cm
filter
paper
into
plastic
cups.
This
extracting
method
is
needed
in
order
to
have
at
least
10
ml
of
extract.
2)
Use
a
pipet
to
transfer
9
ml
of
each
sample
to
a
plastic
cup.
Use
a
pipet
or
dispenser
to
add
1.0
ml
of
2%
Lanthanum
Chloride
to
each
sample.
3)
Read
on
the
AA
and
calculate
by:
Sample
(
ppm)
=
AA
Reading/
9
Record
the
calculated
reading
on
the
raw
data
lab
sheet.

D)
Check
all
pipets
and
dispensers
with
a
graduated
cylinder
to
determine
actual
volume
dispensed
and
record
the
volume
on
the
raw
data
lab
sheet.
This
should
be
at
exact
volumes,
dispensed
or
reject
and
calibrate
pipets
and
check
volumes
again.

8.
For
all
samples:
Read
the
standards
after
every
tray.
If
the
read
standard
is
more
than
±
10%
of
the
known
standard,
the
run
must
be
re­
tested.
Record
the
standard
readings
on
the
raw
data
lab
sheet.

9.
If
the
sample
exceeds
the
highest
standard
by
more
than
10%,
an
appropriate
dilution
is
made.
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.12.13
SOP
TITLE:
Procedure
for
the
Determination
of
Ammonium
Acetate
Extractable
Calcium,
Magnesium,
Sodium
and
Potassium
in
Soil
D­
7
10.
The
check
sample
must
fall
within
the
limits
set
in
SOP
NUT.
04.03
 
"
The
Use
and
Ranges
of
Check
Soil".
If
the
check
soil
does
not
fall
within
these
limits,
the
lab
manager
or
technician
III
may
approve
the
check
soil(
s)
or
may
have
the
samples
re­
tested.

REAGENTS:
·
POTASSIUM
EXTRACTING
SOLUTION
(
1N
Ammonium
Acetate):
10
L
50
L
Ammonium
Hydroxide
690
ml
3450
ml
Acetic
Acid
600
ml
3000
ml
1.
Rinse
out
the
carboy
with
deionized
water
then
fill
about
3/
4
full.
2.
IN
(
OR
IN
FRONT
OF)
THE
FUME
HOOD
use
a
graduated
cylinder
to
add
the
Ammonium
Hydroxide.
Rinse
the
cylinder
with
Deionized
Water
into
the
carboy.
3.
Use
the
graduated
cylinder
to
add
the
Acetic
Acid.
Rinse
the
cylinder
with
Deionized
Water
into
the
carboy.

DANGER:
Ammonium
Hydroxide
and
Acetic
Acid
both
are
corrosive
and
produce
corrosive
fumes.
Use
gloves
and
face
protection
when
handling.
Work
in
(
or
in
front
of)
the
fume
hood
to
avoid
inhaling
the
fumes.

4.
Mix
the
solution
by
shaking
with
the
lid
on,
with
an
electric
mixer,
or
a
magnetic
stir
plate
and
bar.
5.
Fill
the
carboy
to
volume
with
deionized
water
and
mix
again.
6.
Check
the
pH
and
adjust
to
8.5.
If
the
pH
is
over
8.5,
add
Acetic
Acid.
If
under
8.5,
add
Ammonium
Hydroxide.

(
1.0
N
Ammonium
Acetate
Concentrate):
1.
Add
400
ml
of
concentrate
to
a
2000
ml
volumetric
flask.
2.
Dilute
to
volume.
Mix
the
solution
thoroughly.
3.
Adjust
the
pH
of
this
solution
to
8.5.
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.12.13
SOP
TITLE:
Procedure
for
the
Determination
of
Ammonium
Acetate
Extractable
Calcium,
Magnesium,
Sodium
and
Potassium
in
Soil
D­
8
·
2%
LANTHANUM
CHLORIDE
SOLUTION:
2000
ml
Lanthanum
Oxide
47.00
g
Cesium
Chloride
12.60
g
Hydrochloric
Acid
72.0
ml
1.
Weigh
the
Lanthanum
Oxide
and
transfer
it
to
a
flask.
2.
Weigh
the
Cesium
Chloride
and
add
it
to
the
flask.
3.
Fill
about
2/
3
full
with
Deionized
Water
and
swirl
to
mix.
4.
Use
a
graduated
cylinder
to
measure
the
Hydrochloric
Acid
and
add
it
to
the
flask.
5.
Swirl
until
dissolved.
6.
Bring
to
volume
with
deionized
water
and
mix
thoroughly.

·
1:
9
DILUTION
OF
2
%
LANTHANUM
CHLORIDE
SOLUTION:
Dilute
250
ml
of
2
%
Lanthanum
Chloride
solution
to
2000
ml
with
deionized
water
in
a
volumetric
flask.

STANDARDS:
FOR
THE
ICP:
·
ICP
High
CEC
Std.
 
(
Calcium
1500
ppm,
Magnesium
300
ppm,
Sodium
40
ppm,
and
Potassium
72
ppm
in
solution)
(
Calcium
15,000
ppm,
Magnesium
3000
ppm,
Sodium
400
ppm,
and
Potassium
720
ppm
in
soil)
1.
80
mls
of
1000
ppm
Sodium
Standard.
2.
144
mls
of
1000
ppm
Potassium
Standard.
3.
7.492gms
of
oven
dried
Calcium
Carbonate.
4.
0.995
gms
of
oven
dried
Magnesium
Oxide.
5.
20
mls
of
concentrated
Hydrochloric
Acid.
6.
Dilute
to
2000
mls
with
Potassium
Extraction
Solution.

·
ICP
Medium
CEC
Std.
 
(
Calcium
1000
ppm,
Magnesium
200
ppm,
Sodium
20
ppm,
and
Potassium
36
ppm
in
solution)
(
Calcium
10,000
ppm,
Magnesium
2000
ppm,
Sodium
200
ppm,
and
Potassium
360
ppm
in
soil)
1.
40
mls
of
1000
ppm
Sodium
Standard.
2.
72
mls
of
1000
ppm
Potassium
Standard.
3.
4.995gms
of
oven
dried
Calcium
Carbonate.
4.
0.663
gms
of
oven
dried
Magnesium
Oxide.
5.
20
mls
of
concentrated
Hydrochloric
Acid.
6.
Dilute
to
2000
mls
with
Potassium
Extraction
Solution.
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.12.13
SOP
TITLE:
Procedure
for
the
Determination
of
Ammonium
Acetate
Extractable
Calcium,
Magnesium,
Sodium
and
Potassium
in
Soil
D­
9
·
ICP
Low
CEC
Std.
 
(
Calcium
500
ppm,
Magnesium
100
ppm,
Sodium
10
ppm,
and
Potassium
16
ppm
in
solution)
(
Calcium
5000
ppm,
Magnesium
1000
ppm,
Sodium
100
ppm,
and
Potassium
160
ppm
in
soil)
1.
20
mls
of
1000
ppm
Sodium
Standard.
2.
32
mls
of
1000
ppm
Potassium
Standard.
3.
2.497gms
of
oven
dried
Calcium
Carbonate.
4.
0.332
gms
of
oven
dried
Magnesium
Oxide.
5.
20
mls
of
concentrated
Hydrochloric
Acid.
6.
Dilute
to
2000
mls
with
Potassium
Extraction
Solution.

FOR
THE
ATOMIC
ABSORPTION
SPECTROPHOTOMETER:
·
Potassium
and
Sodium:
1.
Pipet
1000
ppm
Potassium
and
Sodium
Standards
into
500
ml
volumetric
flasks,
according
to
the
chart
below.
2.
Dilute
to
volume
with
Potassium
Extracting
Solution,
and
mix
thoroughly.

STANDARD
#
1
STANDARD
#
2
ml
ppm
ppm
in
soil
ml
ppm
ppm
in
soil
Potassium
8
16
160
18
36
360
Sodium
5
10
100
10
20
200
STANDARD
#
3
ml
ppm
ppm
in
soil
Potassium
36
72
720
Sodium
20
40
400
·
Calcium
and
Magnesium:
1.
Pipet
1000
ppm
Calcium
and
Magnesium
Standards
into
500
ml
volumetric
flasks,
according
to
the
chart
below.
2.
Add
50
ml
Lanthanum
Chloride
Solution.
3.
Add
50
ml
Extracting
Solution.
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.12.13
SOP
TITLE:
Procedure
for
the
Determination
of
Ammonium
Acetate
Extractable
Calcium,
Magnesium,
Sodium
and
Potassium
in
Soil
D­
10
4.
Dilute
to
volume
with
Deionized
Water
and
mix
thoroughly.

STANDARD
#
1
STANDARD
#
2
ml
ppm
ppm
in
soil
ml
ppm
ppm
in
soil
Calcium
25
50
50
50
100
100
Magnesium
5
10
100
10
20
200
STANDARD
#
3
ml
ppm
ppm
in
soil
Calcium
75
150
150
Magnesium
15
30
300
REFERENCES:
Brown,
J.
R.,
and
Darryl
Warncke.
1988.
Recommended
Cation
Tests
and
Measures
of
Cation
Exchange
Capacity.
In
W.
C.
Dahnke,
(
ed.).
Recommended
Chemical
Soil
Test
Procedures
for
the
North
Central
Region.
North
Central
Region
Publication
No.
221
(
Revised).
North
Dakota
Agricultural
Experiment
Station
Bulletin
499
(
Revised).
D­
11
AGVISE
Laboratories,
Inc.
NORTHWOOD,
ND
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.02.05
SOP
TITLE:
Undisturbed
Bulk
Density
Analytical
Procedure
REVISED
BY:
Lucinda
S.
Moen
TITLE:
Laboratory
Technician
III
REPLACES
SOP
NUMBER:
NUT.
02.02.04
REASON
FOR
REVISION:
Update
Cover
Page.

APPROVALS:

Robert
Deutsch
Date
Julie
M.
Johnson
Date
President/
Nutrient
Laboratory
Manager
Quality
Assurance
Manager
Robert
Wallace
Date
CEO
Effective
Date
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.02.05
SOP
TITLE:
Undisturbed
Bulk
Density
Analytical
Procedure
D­
12
PURPOSE:
To
define
the
analytical
method
for
determining
the
bulk
density
of
undisturbed
soil
samples
received
in
sampling
tubes.

PROCEDURE:
1.
Determine
the
diameter
of
the
soil
tube.
Use
the
inside
diameter
of
the
soil
probe
used
to
take
the
sample
if
it
is
known.
Otherwise
use
a
ruler
or
caliper
to
measure
the
inside
diameter
of
the
soil
tube
itself.
Record
the
value
to
the
nearest
0.1cm.

2.
Measure
the
length
of
the
soil
core
and
record
the
total
length
to
the
nearest
0.1cm.
If
multiple
cores
represent
the
sample,
sum
the
lengths
of
the
individual
cores
that
make
up
the
sample.

3.
Calibrate
the
balance
following
SOP
NUT.
01.01
 
"
Use
and
Maintenance
of
Laboratory
Balances."

4.
Weigh
a
tray
(
or
several
trays)
suitable
to
hold
all
the
soil
from
the
core,
and
record
the
weight(
s)
to
at
least
the
nearest
0.1g.

5.
Place
all
the
soil
on
the
tray(
s)
and
dry
in
restricted
access
soil
dryer
at
105
±
5
°
C
for
at
least
12
hours.

6.
Weigh
the
tray(
s)
containing
the
dry
soil
and
record
the
weight(
s)
to
at
least
the
nearest
0.1g.

7.
Calculate
the
bulk
density:

Bulk
Density
=
Dry
Soil
Weight
Pi
*
(
Core
Radius)
2
*
(
Core
Length)

REFERENCE:
Blake,
G.
R.
1965.
Bulk
Density.
In
Methods
of
Soil
Analysis,
Part
1.
American
Society
of
Agronomy.
Madison,
WI.
D­
13
AGVISE
Laboratories,
Inc.
NORTHWOOD,
ND
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.03.03
SOP
TITLE:
Determining
the
Cation
Exchange
Capacity
(
CEC)
of
Soil
REVISED
BY:
Julie
M.
Johnson
TITLE:
Quality
Assurance
Manager
REPLACES
SOP
NUMBER:
NUT.
02.03.02
REASON
FOR
REVISION:
Update
Cover
Page
and
Minor
Revisions.

APPROVALS:

Robert
Deutsch
Date
Julie
M.
Johnson
Date
President/
Nutrient
Laboratory
Manager
Quality
Assurance
Manager
Robert
Wallace
Date
CEO
Effective
Date
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.02.03
SOP
TITLE:
Determining
the
Cation
Exchange
Capacity
(
CEC)
of
Soil
D­
14
PURPOSE:
Determining
the
Cation
Exchange
Capacity
(
CEC)
of
a
soil
sample.

PROCEDURE:
1.
Determine
the
calcium,
magnesium,
sodium
and
potassium
of
the
soil
sample
by
following
the
procedures
described
in
SOP
NUT.
02.12
 
"
Procedures
for
the
Determination
of
Ammonium
Acetate
Extractable
Calcium,
Magnesium,
Sodium
and
Potassium
in
Soil".

2.
Determine
the
acidity
of
the
soil
sample
by
following
the
procedures
described
in
SOP
NUT.
02.11
 
"
Determining
the
Acidity
of
Soil".

3.
Calculate
the
CEC
using
one
of
the
following
methods:

Method
1:
lbs
per
acre
Ca
/
400
=
Meq
per
100
gm
Ca
lbs
per
acre
Mg
/
240
=
Meq
per
100
gm
Mg
lbs
per
acre
K
/
780
=
Meq
per
100
gm
K
lbs
per
acre
Na
/
460
=
Meq
per
100
gm
Na
8
×
(
8.00
 
buffer
pH)
=
Meq
per
100
gm
H
CEC
=
sum
of
the
Meq
per
100
gm
(
Ca
+
Mg
+
K
+
Na
+
H)

Method
2:
ppm
Ca
/
200
=
Meq
per
100
gm
Ca
ppm
Mg
/
120
=
Meq
per
100
gm
Mg
ppm
K
/
390
=
Meq
per
100
gm
K
ppm
Na
/
230
=
Meq
per
100
gm
Na
8
×
(
8.00
 
buffer
pH)
=
Meq
per
100
gm
H
CEC
=
sum
of
the
Meq
per
100
gm
(
Ca
+
Mg
+
K
+
Na
+
H)
D­
15
AGVISE
Laboratories,
Inc.
NORTHWOOD,
ND
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.05.08
SOP
TITLE:
pH
Analytical
Procedure
REVISED
BY:
Linda
M.
Anderson
TITLE:
Laboratory
Technician
III
REPLACES
SOP
NUMBER:
NUT.
02.05.07
REASON
FOR
REVISION:
Update
Title
Page
and
Minor
Revisions.

APPROVALS:

Robert
Deutsch
Date
Julie
M.
Johnson
Date
President/
Nutrient
Laboratory
Manager
Quality
Assurance
Manager
Robert
Wallace
Date
CEO
Effective
Date
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.05.08
SOP
TITLE:
pH
Analytical
Procedure
D­
16
PURPOSE:
To
define
the
analytical
method
used
to
determine
soil
pH.

EQUIPMENT:
°
pH
Meter
°
Soil
Scoop
PROCEDURE:
1.
Set
up
pH/
Salt
trays,
putting
small
plastic
cups
in
each
space.

2.
Mark
each
cup
with
its
appropriate
sample
number.

3.
Using
a
5
gm
soil
scoop,
scoop
the
soil
samples
into
the
cups,
according
to
SOP
NUT.
06.02
 
"
Soil
Scoop
Procedure."
Scoop
at
least
one
check
sample
per
10
samples.

4.
Use
a
dispenser
to
add
5
ml
of
deionized
water
to
each
sample.
For
each
batch
of
samples,
check
one
aliquots
of
water
with
a
graduated
cylinder
to
determine
the
actual
volume
dispensed,
and
record
the
volume
on
the
raw
data
lab
sheet.

5.
Stir
the
samples,
and
then
wait
10
minutes
before
reading
them.

6.
Calibrate
the
pH
meter
before
reading
each
batch:
a.
Use
the
appropriate
instruction
manual
for
the
pH
meter
being
used
and
follow
the
instructions
for
calibrating
the
meter.
b.
Use
pH
buffers
4.00,
7.00
and
10.00
to
calibrate
the
pH
meter.
c.
Enter
the
buffers
at
the
end
of
the
run
on
the
raw
data
lab
sheet
to
see
if
the
meter
held
the
calibration.
Acceptable
Ranges
are
as
follows:

4.00
7.00
10.00
Min
3.94
6.94
9.94
Max
4.06
7.06
10.06
7.
Fill
an
adequately
large
enough
beaker
with
deionized
water
for
rinsing
the
electrode.
Put
clean
water
in
the
beaker
for
each
run.

8.
RINSE
THE
ELECTRODE
IN
THE
DEIONIZED
WATER
BEAKER
BEFORE
EACH
SAMPLE.
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.05.08
SOP
TITLE:
pH
Analytical
Procedure
D­
17
9.
Read
each
sample
by
stirring
it
with
the
electrode
until
a
fairly
steady
reading
is
obtained.
THE
READING
SHOULD
BE
TAKEN
WHILE
THE
SAMPLE
IS
BEING
STIRRED.

10.
Record
the
reading
for
each
sample
on
the
raw
data
lab
sheet.

11.
Turn
off
the
pH
meter
after
all
the
samples
are
read
and
store
the
electrodes
in
pH
7
or
pH
4
buffer.

REAGENTS:
pH
ELECTRODE
FILLING
SOLUTION
(
4M
KCl):
500
ml
Potassium
Chloride
150
g
1.
Weigh
the
Potassium
Chloride
into
a
beaker.
2.
Add
about
400
ml
deionized
water
and
stir
on
a
magnetic
stirrer
until
dissolved.
Warm
slightly
if
necessary.
3.
Dilute
to
volume
with
deionized
water
and
stir
until
mixed.

REFERENCES:
Ecken,
D.
J.
1988.
Recommended
pH
and
Lime
Requirement
Tests.
W.
C.
Dahnke,
(
ed.).
Recommended
Chemical
Soil
Test
Procedures
for
the
North
Central
Region.
North
Central
Region
Publication
No.
221
(
Revised).
North
Dakota
Agricultural
Experiment
Station
Bulletin
499
(
Revised).

Peck,
T.
R.
1988.
Standard
Soil
Scoop.
W.
C.
Dahnke,
(
ed.).
Recommended
Chemical
Soil
Test
Procedures
for
the
North
Central
Region.
North
Central
Region
Publication
No.
221
(
Revised).
North
Dakota
Agricultural
Experiment
Station
Bulletin
499
(
Revised).
D­
18
AGVISE
Laboratories,
Inc.
NORTHWOOD,
ND
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.11.09
SOP
TITLE:
Determining
the
Acidity
of
Soil
REVISED
BY:
Linda
Anderson
TITLE:
Laboratory
Technician
III
REPLACES
SOP
NUMBER:
NUT.
02.11.08
REASON
FOR
REVISION:
Update
Cover
Page
and
Method
APPROVALS:

Julie
Johnson
Date
Mary
Thingelstad
Date
Nutrient
Laboratory
Manager
Quality
Assurance
Manager
Robert
Deutsch
Date
Robert
Wallace
Date
President
CEO
Effective
Date
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.11.09
SOP
TITLE:
Determining
the
Acidity
of
Soil
D­
19
PURPOSE:
To
determine
the
acidity
of
a
soil
sample
for
use
in
calculating
the
CEC
of
the
soil.

SCOPE:
Using
the
Adam­
Evans
method
to
determine
the
Acidity
of
a
soil
sample.
Ref.:
Soil
Testing
and
Plant
Analysis
Laboratory
Manual,
1989,
J.
Benton
Jones,
Jr.

EQUIPMENT
REQUIRED:
1.
pH
meter
BUFFER
SOLUTION:
1.
Using
a
one­
Liter
flask
with
a
magnetic
stirrer,
dissolve
74
g
of
potassium
chloride
in
approximately
500
ml
of
water.

2.
Add
10.5
g
of
potassium
hydroxide,
stir
and
dissolve.

3.
Add
20
g
of
p­
nitrophenol,
stir
and
dissolve.

4.
Add
15
g
of
boric
acid.

5.
Dilute
to
1
L
with
water
and
stir.
You
may
need
to
heat
to
dissolve.

METHOD:
1.
To
the
5
grams
of
soil
and
5
ml
of
deionized
water
used
for
pH
of
soil
(
Refer
to
SOP
NUT.
02.05
 
pH
Analytical
Procedure),
add
5
ml
of
Adams­
Evans
buffer.
Scoop
a
check
sample
after
the
last
sample
in
each
tray.
Check
the
dispenser
with
a
graduated
cylinder
and
record
this
amount
on
the
raw
data
lab
sheet.

2.
Shake
or
stir
for
10
minutes.

3.
Let
stand
for
30
minutes.

4.
Prepare
a
standard
by
mixing
5
ml
of
deionized
water
with
5
ml
of
Adams­
Evans
buffer
solution.
Use
this
solution
to
calibrate
the
pH
meter
to
8.00.
The
Acceptable
Range
is
as
follows:
Min
 
7.92
Max
 
8.08
5.
Read
samples
and
record
pH
to
nearest
0.01
on
the
raw
data
lab
sheet
for
Acidity.
This
reading
is
the
buffer
pH.
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.11.09
SOP
TITLE:
Determining
the
Acidity
of
Soil
D­
20
CALCULATIONS:
meq
acidity
(
H+)
/
100
g
=
8
×
(
8.00­
buffer
pH)
D­
21
AGVISE
Laboratories,
Inc.
NORTHWOOD,
ND
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.34.03
SOP
TITLE:
Hydraulic
Conductivity
 
Constant
Head
Method
REVISED
BY:
Garis
Pollert
TITLE:
Nutrient
Laboratory
Analyst
REPLACES
SOP
NUMBER:
NUT.
02.34.02
REASON
FOR
REVISION:
Update
Cover
Page,
Procedures
and
Minor
Revisions
APPROVALS:

Robert
Deutsch
Date
Julie
M.
Johnson
Date
President/
Nutrient
Laboratory
Manager
Quality
Assurance
Manager
Robert
Wallace
Date
CEO
Effective
Date
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.34.03
SOP
TITLE:
Hydraulic
Conductivity
 
Constant
Head
Method
D­
22
PURPOSE:
To
define
the
analytical
method
for
determining
the
hydraulic
conductivity
of
a
saturated
soil.

EQUIPMENT:
°
Constant­
Head
Hydraulic
Conductivity
Apparatus
(
See
Figure
1).
°
Container
to
hold
water.

PROCEDURE:
1.
Set
up
an
apparatus
similar
to
Figure
1.

2.
Scoop
each
sample
into
a
plastic
cylinder
that
has
a
cover
of
cloth
on
one
end.
Cover
the
cloth
end
with
a
cover
or
cap
and
tap
on
the
counter
10
times
to
settle
the
disturbed
sample,
remove
cover.
If
the
sample
arrives
in
an
acetate
or
metal
tube,
the
hydraulic
conductivity
is
performed
on
the
sample
undisturbed.
Cut
the
tubes
into
appropriate
lengths
using
a
saw.
Place
a
cylinder
extension
on
top
of
the
soil
tube
and
seal.
Make
sure
that
the
seal
is
watertight.
Place
a
cloth
on
the
bottom
of
the
soil
tube.

3.
Place
samples,
cloth­
covered
end,
down
into
water.
Allow
the
samples
to
soak
at
least
16
hours
until
they
are
saturated.

4.
Turn
on
the
water
supply
for
the
upper
trough.

5.
Transfer
the
samples
to
the
rack
and
start
the
siphons
to
maintain
a
constant
head
of
water
on
each
of
the
samples.

6.
After
the
water
level
on
top
of
a
sample
becomes
stabilized,
collect
the
percolate
in
a
suitable
container
for
a
known
amount
of
time.

7.
Record
the
time
and
the
amount
of
water
in
the
container.
Measure
and
record
the
hydraulic
head
difference
(
DH).
Record
the
temperature
of
the
water.
Measure
the
length
of
the
soil
column
and
the
diameter
of
the
cylinder
used.

CALCULATIONS:
Hydraulic
conductivity
=
(
Q/
A*
t)
×
(
L/
D
H)
Q
=
Water
that
passes
through
the
sample
at
a
known
time
t
=
Known
time
A
=
Cross
sectional
area
of
the
sample
L
=
Length
of
the
sample
D
=
Hydraulic
head
difference
across
sample
(
See
Figure
1)
*
Figure
1:
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.34.03
SOP
TITLE:
Hydraulic
Conductivity
 
Constant
Head
Method
D­
23
*
Drawing
taken
from
reference
listed
below
REFERENCES:

Black,
C.
A.
(
ed).
1965.
Methods
of
Soil
Analysis,
Part
1,
American
Society
of
Agronomy,
Inc.,
Madison,
Wisconsin.
D­
24
AGVISE
Laboratories,
Inc.
NORTHWOOD,
ND
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.56.04
SOP
TITLE:
Texture
Procedure
 
Pipette
Method
REVISED
BY:
Garis
Pollert
TITLE:
Laboratory
Nutrient
Analyst
REPLACES
SOP
NUMBER:
NUT.
02.56.03
REASON
FOR
REVISION:
Update
Cover
Page,
Clarify
Procedure
Order
&
Minor
Revisions
APPROVALS:

Robert
Deutsch
Date
Julie
M.
Johnson
Date
President/
Nutrient
Laboratory
Manager
Quality
Assurance
Manager
Robert
Wallace
Date
CEO
Effective
Date
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.56.04
SOP
TITLE:
Texture
Procedure
 
Pipette
Method
D­
25
PURPOSE:
To
define
the
analytical
procedure
used
to
determine
soil
texture
(%
sand,
silt,
and
clay)
using
a
pipette
method.

EQUIPMENT:
°
Pipettes
°
Thermometer
°
Stop
watch
or
clock
with
second's
hand
°
Balance
°
Shaker
REAGENTS:
°
10%
Sodium
hexametaphosphate
Solution:
Dissolve
100
GM
of
sodium
hexametaphosphate
in
1
L
H
2
0.

Determine
a
correction
factor
by
pipetting
or
dispensing
10
ml
of
the
solution
into
a
preweighed
container.
Place
the
container
in
an
oven
at
105
±
5oC
until
dry.
Weigh
the
container
on
a
balance
to
at
least
three
decimal
places.
Calculate
the
correction
factor
and
write
it
on
the
container.

(
Container
+
Residue
 
Container
Empty)
Blank
Factor
=
(
20
)

°
30%
Hydrogen
Peroxide
(
H
2
O
2)
°
Acetic
Acid
PROCEDURE:
1.
Weigh
out
approximately
10
g
of
soil.
Record
the
weight
on
the
raw
data
lab
sheet.
Weigh
in
or
transfer
to
a
container,
such
as
a
fleaker,
that
has
been
weighed
to
at
least
three
decimal
places.
Follow
SOP
NUT.
01.01
 
"
Use
and
Maintenance
of
Laboratory
Balances"
to
calibrate
the
balance.

2.
If
the
%
Organic
Matter
is
1.0
%,
Step
2
and
3
are
not
necessary,
skip
to
step
4.
To
the
samples
that
are
>
1.0%,
add
10
ml
of
deionized
water,
10
ml
of
30%
Hydrogen
Peroxide,
and
1
drop
of
Acetic
Acid.
Swirl
the
mixture;
cover
with
a
watch
glass
and
heat
at
approximately
60
°
C.
When
the
temperature
is
reached,
add
Hydrogen
Peroxide
in
5­
ml
increments
approximately
every
15
minutes
until
the
organic
matter
is
oxidized.
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.56.04
SOP
TITLE:
Texture
Procedure
 
Pipette
Method
D­
26
3.
After
the
organic
matter
is
removed,
the
containers
are
oven
dried
at
105
±
5
°
C,
and
then
weighed
to
at
least
three
decimal
places.

4.
Add
10
ml
of
the
10%
Sodium
Hexametaphosphate
to
each
container
and
bring
the
volume
up
to
approximately
150
ml
with
deionized
water.

5.
Cap
and
shake
the
containers
on
a
horizontal
shaker
overnight
(
12
hours
minimum).

6.
Add
10
ml
of
the
10%
Sodium
Hexametaphosphate
solution
to
a
container
and
bring
the
volume
up
to
approximately
150­
ml.
This
sample
is
referred
to
as
a
BLANK.

7.
The
stoppers
are
then
removed
and
the
volume
of
each
container
is
brought
up
to
400
ml
with
deionized
water.

8.
The
temperature
of
the
BLANK
is
taken
and
recorded
on
the
raw
data
lab
sheet.

9.
Cap
the
container
and
shake
vigorously
for
10
seconds
to
ensure
that
no
soil
adheres
to
the
bottom
of
the
container.

10.
Shake
the
container
vigorously
for
15
seconds,
end­
over­
end.
Note
the
time
and
allow
the
container
to
stand
for
the
desired
settling
time
based
on
the
temperature
of
the
BLANK
(
See
Table
1).

11.
Run
the
pipette
calibration
by
pipetting
DI
water
into
a
tarred
container
and
recording
the
weigh
in
the
appropriate
spaces
provided
on
the
form.
Do
this
for
three
consecutive
readings.
The
average
is
taken
for
the
calibration
figure.

12.
Pipette
20
ml
of
the
samples,
at
a
depth
of
3
cm,
at
the
time
corresponding
with
the
temperature
of
the
BLANK
(
See
Table
1).
Rinse
the
pipette
by
sampling
20
mls
of
DI
water.

13.
Each
aliquot
is
discharged
into
a
tarred
weighing
dish,
along
with
the
deionized
water
used
to
rinse
the
pipette.

14.
Place
the
weighing
dishes
in
an
oven
at
105
±
5
°
C.
When
the
samples
are
dry,
weigh
on
a
balance
to
at
least
three
decimal
places
and
record
the
weight
under
the
"
Can
Dry
Wt."
on
the
raw
data
lab
sheet.
These
containers
can
be
dried
with
the
sand
containers.

15.
Using
deionized
water,
wash
the
remaining
sample
through
a
45
m
m
sieve.
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.56.04
SOP
TITLE:
Texture
Procedure
 
Pipette
Method
D­
27
16.
Transfer
the
soil
from
the
sieve
to
a
tarred
container.
Place
the
sample
in
a
drying
oven
at
105
±
5
°
C
until
dry.
Weigh
the
container
with
the
sample
on
a
balance
to
at
least
three
decimal
places
and
record
the
weight
under
the
"
Sand
Dry
Wt."
on
the
raw
data
lab
sheet.

Table
1.
Settling
times
at
corresponding
temperatures
for
pipetting
<
2­
µ
m
fraction
at
3
cm
depth.

Temperature
Settling
Times
E
C
hr:
min
17
2:
37
18
2:
33
19
2:
29
20
2:
26
21
2:
22
22
2:
18
23
2:
16
24
2:
13
25
2:
10
26
2:
7
27
2:
4
28
2:
1
29
1:
58
30
1:
56
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.56.04
SOP
TITLE:
Texture
Procedure
 
Pipette
Method
D­
28
CALCULATIONS:
%
Sand
=
100
(
Total
Sand
Weight
/
Total
Soil
Weight)

%
Clay
=
(
Clay
Weight)
(
400/
Pipet
Volume)
(
100/
Total
Soil
Weight)

%
Silt
=
100
 
(%
Sand
+
%
Clay)

Where:
Clay
Weight
=
(
Can
Dry
Wt.
 
Can
Tare
Wt.)
 
(
Blank
Factor)

Total
Sand
Weight
=
(
Sand
Dry
Wt.)
 
(
Sand
Can
Tare
Wt.)

Soil
Classification
is
determined
from
Textural
Triangle
REFERENCES:
Indorante,
S.
J.
March
 
April
1990.
Particle­
Size
Analysis
is
a
Modified
Pipette
Procedure.
Soil
Science
Society
of
America
Journal.
Volume
54.

Black,
C.
A.
(
Ed).
1965.
Methods
of
Soil
Analysis,
Part
1,
American
Society
of
Agronomy,
Inc.,
Madison,
Wisconsin.

Isaac,
Robert.
1984.
Methodology
for
the
Analysis
of
Soil,
Plant,
Feed,
Water
and
Fertilizer
Samples.
Georgia
Soil
Testing
and
Plant
Analysis
Laboratory.

Liegel,
E.
A.,
Simson
and
Schulte
(
Ed).
1980.
Wisconsin
Procedures
for
Soil
Testing,
Plant
Analysis,
and
Feed
and
Forage
Analysis.
Department
of
Soil
Science,
University
of
Wisconsin
 
Madison.
D­
29
AGVISE
Laboratories,
Inc.
NORTHWOOD,
N.
D.

STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.58.02
SOP
TITLE:
Redox
Potential
of
a
Soil
Sample
REVISED
BY:
Garis
Pollert
TITLE:
Nutrient
Laboratory
Analyst
REPLACES
SOP
NUMBER:
NUT.
02.58.01
REASON
FOR
REVISION:
Update
Title
Page
and
Update
Procedures.

APPROVALS:

Robert
Deutsch
Date
Julie
M.
Johnson
Date
President/
Nutrient
Laboratory
Manager
Quality
Assurance
Manager
Robert
Wallace
Date
CEO
Effective
Date
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.58.02
SOP
TITLE:
Redox
Potential
of
a
Soil
Sample
D­
30
PURPOSE:
To
define
the
analytical
method
for
determining
the
oxidation­
reduction
potential
of
a
soil
sample.

EQUIPMENT:
°
Redox
Electrode
°
Millivolt
meter
°
Thermometer
CALIBRATION:
1.
Prepare
a
Solution
of:
105
ml
Deionized
Water
+
3
ml
H
2
SO
4
2.000
grams
of
Fe(
NH
4)
2(
SO
4)
2
*
6H
2
O
0.081
grams
KMnO
4
Prepare
in
a
beaker
and
stir
with
a
magnetic
stir
bar.

Note:
It
is
important
that
the
solution
is
stirred
slowly,
to
prevent
air
bubbles.

2.
Take
a
millivolt
reading
of
the
above
solution
when
all
the
solids
have
dissolved.
The
millivolt
reading
should
be
474
±
10
millivolts.

PROCEDURE:
1.
Set
up
small
plastic
cups
in
trays.

2.
Mark
each
sample
with
its
appropriate
sample
number.

3.
Scoop
the
soil
samples
into
the
cups
using
the
15
gram
soil
scoop,
according
to
SOP
NUT.
06.02,
"
Soil
Scoop
Procedure."
Scoop
a
check
sample
after
the
last
sample
in
each
tray.

4.
Add
15
ml
of
deionized
water
to
each
sample.
For
each
batch
of
samples,
check
one
aliquot
of
water
with
a
graduated
cylinder
and
record
the
volume
on
the
lab
sheet.

5.
Slowly
stir
the
samples
with
a
glass
stir
rod.

6.
Insert
a
stir
bar
into
the
beaker
and
record
the
stabilized
millivolt
reading
while
the
sample
is
being
stirred
slowly.
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.58.02
SOP
TITLE:
Redox
Potential
of
a
Soil
Sample
D­
31
7.
Record
the
temperature
of
the
sample.

8.
The
pH
may
also
be
required.
Follow
the
appropriate
SOP
and
record
the
stabilized
reading.

REFERENCE:
Platinum
Redox
Electrode
Instruction
Manual.
Model
96­
78­
00,
97­
78­
00.
Orion
Research
Incorporated,
1991.
D­
32
AGVISE
Laboratories,
Inc.
NORTHWOOD,
ND
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.66.03
SOP
TITLE:
Cation­
Exchange
Capacity
by
Sodium
Saturation
in
Calcareous
Soils
REVISED
BY:
Gail
Ducioame
TITLE:
Quality
Control
Specialist
REPLACES
SOP
NUMBER:
NUT.
02.66.02
REASON
FOR
REVISION:
Update
Title
Page
and
Procedures
APPROVALS:

Julie
Johnson
Date
Mary
Thingelstad
Date
Nutrient
Laboratory
Manager
Quality
Assurance
Manager
Robert
Deutsch
Date
Robert
Wallace
Date
President
CEO
Effective
Date
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.66.03
SOP
TITLE:
Cation­
Exchange
Capacity
by
Sodium
Saturation
in
Calcareous
Soils
D­
33
PURPOSE:
To
determine
the
cation
exchange
capacity
of
calcareous
soil
by
sodium
saturation.

EQUIPMENT:
1.
Atomic
Absorption
Spectrophotometer
2.
Vortex
mixer
3.
Centrifuge
REAGENTS:
SODIUM
ACETATE,
1.0N
1.
Dissolve
136
g
of
NaC2H3O2*
3H2O
in
water
and
dilute
to
1000
ml.
2.
Adjust
the
pH
to
8.2
with
acetic
acid
or
sodium
hydroxide
solution.

ETHANOL,
95
percent
AMMONIUM
ACETATE,
1.0N
(
1.0
N
Ammonium
Acetate
Concentrate)

1.
Add
400
ml
of
concentrate
to
a
2000
ml
volumetric
flask.
2.
Dilute
to
volume.
Mix
the
solution
thoroughly.
3.
This
makes
a
1.0
N
Ammonium
Acetate
solution
with
a
working
pH
of
7.0.
1.0
N
AMMONIUM
ACETATE:
10
L
50
L
Ammonium
Hydroxide
690
ml
3450
ml
Acetic
Acid
600
ml
3000
ml
1.
Rinse
out
the
carboy
with
deionized
water,
then
fill
about
3/
4
full.
2.
IN
(
OR
IN
FRONT
OF)
THE
FUME
HOOD
use
a
graduated
cylinder
to
add
the
Ammonium
Hydroxide.
Rinse
the
cylinder
with
Deionized
Water
into
the
carboy.
3.
Use
the
graduated
cylinder
to
add
the
Acetic
Acid.
Rinse
the
cylinder
with
Deionized
Water
into
the
carboy.
DANGER:
Ammonium
Hydroxide
and
Acetic
Acid
both
are
corrosive
and
produce
corrosive
fumes.
Use
gloves
and
face
protection
when
handling.
Work
in
(
or
in
front
of)
the
fume
hood
to
avoid
inhaling
the
fumes.

4.
Mix
the
solution
by
shaking
with
the
lid
on
or
with
an
electric
mixer
or
a
magnetic
stir
plate
and
bar.
5.
Fill
the
carboy
to
volume
with
deionized
water
and
mix
again.
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.66.03
SOP
TITLE:
Cation­
Exchange
Capacity
by
Sodium
Saturation
in
Calcareous
Soils
D­
34
6.
Check
the
pH.
If
the
pH
is
over
7.0,
add
Acetic
Acid.
If
under
7.0,
add
Ammonium
Hydroxide.

PROCEDURE:
1.
Weigh
out
4.0
g
of
soil
into
a
50
ml
conical
centrifuge
tube.

2.
Add
33
ml
of
sodium
acetate
solution.

3.
Vortex
the
sample
for
approximately
10
 
30
seconds.
Shake
the
sample
for
5
minutes.

4.
Centrifuge
for
5
minutes
or
until
the
supernatant
is
clear.

5.
Decant
the
liquid
and
discard.

6.
Repeat
this
extraction
(
Steps
2
 
4)
three
more
times.

7.
Add
33
ml
of
95%
Ethanol.

8.
Vortex
the
sample
for
approximately
10
 
30
seconds.
Shake
the
sample
for
5
minutes.

9.
Centrifuge
for
5
minutes
or
until
the
supernatant
is
clear.

10.
Decant
the
liquid
and
discard.

11.
Repeat
this
extraction
(
Steps
7
 
10)
two
more
times.

12.
Add
33
ml
of
ammonium
acetate
solution
to
the
sample.

13.
Vortex
the
sample
for
approximately
10
 
30
seconds.
Shake
the
sample
for
5
minutes.

14.
Centrifuge
for
5
minutes
or
until
the
supernatant
is
clear.

15.
Decant
the
liquid
into
a
100
ml
volumetric
flask.

16.
Repeat
this
extraction
(
Steps
12
 
15)
two
more
times.
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.66.03
SOP
TITLE:
Cation­
Exchange
Capacity
by
Sodium
Saturation
in
Calcareous
Soils
D­
35
17.
Dilute
the
ammonium
acetate
extract
to
volume
and
mix.

18.
Determine
the
sodium
by
using
the
method
and
standards
in
SOP
NUT.
02.12.
 
"
Procedures
for
the
Determination
of
Ammonium
Acetate
Extractable
Calcium,
Magnesium,
Sodium
and
Potassium
in
Soil."

19.
If
the
samples
exceed
the
highest
standard
by
more
than
10
%,
an
appropriate
dilution
is
made
and
calculated.

CALCULATION:
Cation
Exchange
Capacity
by
Sodium
Saturation
(
meq/
100g)
=
Atomic
Absorption
Reading(
ppm)
*
.01087
REFERENCES:
Homer
D.
Chapman
and
Parker
F.
Pratt.
1978.
Methods
of
Analysis
for
Soil,
Plants,
and
Waters.
Division
of
Agricultural
Sciences.
pp.
35
 
36.
D­
36
AGVISE
Laboratories,
Inc.
NORTHWOOD,
ND
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.92.00
SOP
TITLE:
Determination
of
Total
Organic
Carbon
in
Soil
by
Combustion
SUBMITTED
BY:
Larry
Wikoff
TITLE:
Nutrient
Laboratory
Manager
REVISED
BY:

TITLE:

REPLACES
SOP
NUMBER:

REASON
FOR
REVISION:

APPROVALS:

Larry
Wikoff
Date
Julie
M.
Johnson
Date
Nutrient
Laboratory
Manager
Quality
Assurance
Manager
Robert
Deutsch
Date
Robert
Wallace
Date
President
CEO
Effective
Date
PURPOSE:
To
describe
the
procedure
for
determining
total
organic
carbon
in
calcareous
and
noncalcareous
soils
using
the
LECO
CR­
412
Carbon
Analyzer.
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.92.00
SOP
TITLE:
Determination
of
Total
Organic
Carbon
in
Soil
by
Combustion
D­
37
EQUIPMENT:
°
LECO
CR­
412
Carbon
Analyzer
°
Weigh
Boats
PROCEDURE:
1.
Instrument
Set­
Up:
A.
Check
the
O2
supply
to
furnace
and
set
regulator
to
40
psi
as
stated
in
the
manual.
B.
Power
up
the
furnace
and
allow
it
to
come
to
temperature,
about
1400oC.
C.
Check
for
proper
gas
flow
as
stated
in
the
user
manual
for
this
system.
D.
Replace
Anhydrone
 
if
instrument
indicates
it
is
wet.
E.
Check
the
Ambient
Monitor
for
proper
instrument
conditions.
Print
table
and
place
it
in
the
appropriate
calibration
logbook.
All
data
must
be
signed
and
dated
by
the
individual
generating
the
data.

2.
Calibration:
A.
Calibration
data
is
stored
in
the
calibration
logbook.
B.
Check
current
calibration
curve
by
combusting
three
replicates
(
approximately
0.2g
of
a
known
low
standard)
as
detailed
in
the
system
calibration
logbook.
Document
information
on
the
standard
such
as
supplier,
lot
number,
and
ppm
concentration
in
the
calibration
logbook.
3.
System
should
be
recalibrated
if:
1.
The
value
of
standard
varies
more
than
5%
relative
to
the
expected
value.
2.
Carbon
content
of
unknown
samples
is
expected
to
be
above
the
current
calibration
curve.
3.
The
oxygen
tank
is
changed.
4.
The
CR­
412
Carbon
Analyzer
has
sat
idle
for
four
weeks
or
more.
D.
Calibrate
by
combusting
at
least
7
replicates
of
the
known
low
and
high
ppm
standard,
0.2g
within
5%
and
0.09g
within
5%,
respectively.
E.
Record
calibration
data
in
the
appropriate
calibration
logbook.
All
data
must
be
signed
and
dated
by
the
individual
generating
the
data.

3.
Sample
Analysis:
A.
All
samples
tested
for
organic
carbon
content
must
be
checked
for
inorganic
carbon
by
placing
several
drops
of
2M
HCl
on
a
small
amount
of
soil
(
approximately
0.2g)
to
check
for
carbonates.
If
no
carbonates
are
present
(
no
effervescence
observed),
place
approximately
0.25g
into
a
weighing
dish
and
heat
at
104oC
(
2
to16
hours)
to
allow
carbon
to
be
determined
on
an
oven
dry
weight
basis.
Store
samples
in
a
desiccator
until
ready
to
weigh.
STANDARD
OPERATING
PROCEDURE
SOP
NUMBER:
NUT.
02.92.00
SOP
TITLE:
Determination
of
Total
Organic
Carbon
in
Soil
by
Combustion
D­
38
B.
Follow
this
procedure
if
carbonates
are
present
as
indicated
by
effervescence.
Place
enough
soil
in
a
weighing
dish
for
the
desired
reps
allowing
0.25g/
rep.
Next,
add
2M
HCl
until
effervescence
stops.
Oven
dry
the
samples
as
in
Step
A
for
noncalcareous
soils.
C.
Weigh
about
0.200g
of
the
oven
dried
soil
into
a
combustion
crucible
and
record
the
weight.
Manually
enter
the
recorded
weight
in
the
instruments
analysis
screen
menu.
D.
Percent
carbon
is
calculated
by
the
instrument
and
printed.
Record
this
value
on
the
appropriate
lab
sheet.

4.
System
Shutdown:
A.
Shutdown
the
system
by
choosing
"
LOG
OFF"
on
the
screen.
The
furnace
temperature
will
be
reduced
and
oxygen
flow
through
the
instrument
will
be
stopped.

REFERENCES:
LECO
CR­
412
Instrument
manual,
revised
1995.
STANDARD
OPERATING
PROCEDURE
SOP
TITLE:
1/
3
Bar
 
German
Method
1
The
MWC
is
frequently
described
in
American
literature
as
FC
(
field
capacity,
pF
#
0.3)

2
The
FC
is
frequently
described
in
American
literature
as
1/
3
bar­
FMC
(
field
moisture
capacity,
pF
#
2.5)

D­
39
Subsequently,
the
following
operations
are
carried
out:

1)
Taring
of
Buchner
funnels
with
premoistened
filter
(
A,
A',
A")

MWC1­
determination:

2)
One
aliquotes
of
approx.
100
g
each
(
filled
to
the
rim)
are
divided
into
tared
Buchner
funnels.
Soil
allowed
again
to
drip
off.
Soil
is
saturated
and
allowed
to
stand
overnight.
Funnels
to
be
covered
with
a
reversed
watch
glass
in
order
to
prevent
drying
out
of
the
soil.

FC2­
determination:
1/
3
Bar
4)
Covering/
sealing
of
Buchner
funnels
with
1
 
2
layers
of
parafilm
and
slight
pressing
down
of
film
on
soil.
Tightness
of
parafilm
at
the
Buchner
funnel
to
be
checked
so
that
no
air
current
can
go
through
the
soil.
This
step
serves
to
prepare
for
the
FC­
determination.

5)
Application
of
a
saturation
potential
of
1/
3
bar
to
the
suction
bottles
(
vacuum
regulator
setting:
 
0.33
bar,
manometer
setting:
666
mbar),
°
0.33
bar
should
not
fall
below
otherwise
high
pressure
is
exerted
on
the
soil
via
the
parafilm
membrane
and,
thus,
too
much
water
is
pressed
out.
Increase
vacuum
only
slowly
from
0
to
 
0.33
bar.
With
this
procedure
the
water
starts
to
emerge.
Suction
to
be
used
until
dripping
off
speed
is
only
approx.
1
drop/
15
minutes
(
at
least,
however,
2
hours,
attention
to
be
paid
to
tightness
of
the
parafilm).

6)
Balance
of
the
low
pressure
to
be
established
and
parafilm
removed.

7)
The
funnels
with
the
partially
wet
soils
to
be
weighed.

8)
Soil
is
dried
in
the
Buchner
funnels.