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AMERICAN WOOD PROTECTION ASSOCIATION STANDARD
© 2015 All Rights Reserved
STANDARD METHOD FOR THE DISTILLATION OF CREOSOTE AND CREOSOTE SOLUTIONS
Jurisdiction: AWPA Technical Committee P-5
Adopted in 2011, this standard was developed from AWPA Standard A1, Method 2.
This AWPA Standard is promulgated according to an open, consensus procedure. Using this standard in no way signifies standardization of a
chemical or wood protection system in AWPA Standard U1.
1.0 Scope: This test method is employed to distill creosote
and creosote solutions to determine the amount of water and
weights of different distillation fractions.
2.0 Summary:
2.1 The amount of water in a sample of creosote or creosote
solution is determined, and then the sample is distilled to
determine the percent weight of the fractions in the
following ranges: Up to 210°C, 210 to 235°C, 235 to 270°C,
270 to 315°C, and 315 to 355°C.
2.2 This standard formerly listed as AWPA Standard A1
Method 2.
3.0 Safety Precautions: The collection, handling,
distillation of flammable creosote or creosote solutions, and
disposal of the distillates, should be done in accordance with
standard laboratory safety procedures. Not all general
safety concerns associated with this standard are addressed
here. It is therefore the responsibility of the user to establish
and follow appropriate good laboratory practices and general
safety precautions where applicable.
4.0 Apparatus:
4.1 Flask. A side-neck distillation flask, as shown in Fig. 1,
having the following dimensions:
Diameter of bulb, outside: 86 ± 2 mm
Diameter of neck, inside: 22.0 ± 1.0 mm
Diameter of tubulature, inside: 10.0 ± 0.5 mm
Height of flask, outside: 131.0 ± 1.5 mm
Vertical distance bottom of bulb, outside to horizontal
tangent at tubulature inside: 93.0 ± 1.5 mm
Length of tubulature: 220.0 ± 5.0 mm
Angle of tubulature: 75.0 ± 2 deg
Thickness of tubulature wall: 1.0 to 1.5 mm
4.2 Condenser Tube. A tapered glass condenser, as shown
in Figs. 2 and 3, having the following dimensions:
Diameter of small end, outside:12.5 ± 1.5 mm
Diameter of large end, outside: 28.5 ± 3.0 mm
Length 360.0 ± 4 mm
Length of taper 100 ± 5 mm
Figure 2. - Apparatus Assembly for Flame Distillation
Figure 3. - Apparatus Assembly for Electric Heater
Distillation
Figure 1. - Distillation Flask
4.3 Source of Heat.
4.3.1 Flame. Bunsen or Meker Laboratory gas flame-type
burner, or
4.3.2 Electric Heater. Output variable to 600 or to 750
watts with removable upper and lower refractories, as
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illustrated in Fig. 4, provided with variable transformer or
rheostat suitable for the voltage used and fitted with clamp
for mounting on vertical support rod.
4.4.2 For Electric Heater Distillation. - A metal shield,
should be fitted with heat resistant windows, and cover of
the same construction and dimensions as those used for
flame distillation (4.4.1), except for the height of the shield.
See Fig. 6.
Figure 4. - Upper Part of Electric Heater
Figure 6. - Shield for Use with Electric Heater
4.4 Shield and Cover.
4.4.1 For Flame Distillation. - a metal shield, should be
fitted with mica heat resistant windows, and lined with 1/8"
heat-resistant insulation, of the form and dimensions shown
in Fig 5; with two-part cover made from ¼" "Transite"
ceramic or other flame and heat resistant board, also shown
in Fig. 5.
4.5 Burner Chimney for Flame Distillation. A cylindrical
metal chimney approximately 100 mm high, 95 to 105 mm
in diameter, and having a peephole 25 mm in diameter
centered about 32 mm below the ring support, used to
protect the flame from air currents. The top of the shield
shall be flanged to permit its being suspended from the ring
support. See Fig. 7.
Figure 7. - Burner Chimney for Flame Distillation
4.6 Gauzes for Flame Distillation. Two 6 inch by 6 inch
sheets of approximately 16 mesh heat-resistant wire gauze
made of approximately 0.02" diameter wire.
4.7 Receivers. Erlenmeyer flasks or beakers having a
capacity of 50 to 125 ml tared to the nearest 0.05g.
4.8 Suitable Analytical Balance.
4.9 Thermometer. An ASTM High Distillation
thermometer having a range of -2º to 400º C and conforming
the requirements for Thermometer 8ºC as prescribed in the
specifications for ASTM Thermometers (ASTM
FLANGED OPEN-END
MADE OF 22 GUAGE
STAINLESS STEEL
AND WITH 1/8-IN HEAT
RESISTANT
INSULATION LINING
TWO MICA CYLINDER
WINDOWS ARE
PROVIDED AT
RIGHT ANGLES
TO THE END SLOT
Figure 5. - Shield and Cover for Flame Distillation
Designation: E1).
4.10 Apparatus Assembly.
4.10.1 For Flame Distillation. Suspend the burner chimney
by its flange from a support ring, place the specified two
sheets of wire gauze on the burner chimney, and set the flask
shield on the upper sheet of gauze. Insert the thermometer
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through a regular-length tightly-fitting cork, rolled prior to
use, in the neck of the distillation flask so that the bottom of
the cork is from 23 to 28 mm above the lowest point of the
juncture between the tubulature and the neck of the flask,
and the bottom of the bulb is 12 to 13 mm from the surface
of the liquid in the flask. The exact location of the
thermometer bulb may be determined by calculating the
number of divisions on the thermometer which are equal to
12 to 13 mm, lowering the thermometer through the cork
until the tip of its bulb touches the surface of 100 g of
sample in the flask, and then raising the thermometer the
calculated number of degrees to give the correct distance
from the surface of the liquid. Align the stem on the axis of
the bulb through the neck of the flask. Place the distillation
flask in the flask shield with its bulb resting on the gauze
and connect the condenser tube to the tubulature of the flask
with a tight cork joint, having the tubulature project 30 to 50
mm through the cork. The distance from the neck of the
flask to the outlet end of the condenser tube shall be not
more than 600 nor less than 500 mm. Support the condenser
tube in a position such that it is in alignment with the
tubulature of the flask, and the thermometer is vertical.
Place the shield cover on the flask shield around the neck of
the flask.
4.10.2 For Electric Heater Distillation. Attach the electric
heater to a vertical support so that, at the end of the
distillation, it can be lowered for a distance of at least six
inches (15 cm). Place the upper refractory on the heater
with its larger opening facing upwards. Set the flask shield
on the upper refractory. Position the thermometer in the
distillation flask as described the second paragraph of 4.10.1.
Connect the condenser tube to the tubulature of the
distillation flask with a tight cork joint, having the tubulature
project 30 to 50 mm through the cork. The distance from the
neck of the flask to the outlet end of the condenser tube shall
be not more than 600 mm nor less than 500 mm. Place the
distillation flask in the flask shield and support the assembly
so that the bottom of the flask is between 4 and 7 mm above
the heating coils, the condenser tube is in alignment with the
tubulature of the flask, and the thermometer is vertical.
Place the shield cover on the flask shield around the neck of
the flask.
5.0 Reagents: Not applicable.
6.0 General Method Procedures:
6.1 Sampling. Thoroughly stir or otherwise mix the sample
immediately before removing the portion for testing, to
ensure that such portion will be representative of the sample.
If crystallized solids are present warm the sample to dissolve
the crystals, taking care to avoid loss of volatile material.
6.2 Dehydration. If not more than 3.0 percent of water is
present, the sample may be tested as is. If the water content
is above 3.0 percent, the sample should be re-tested and, if
still above 3.0 percent, the suitability of the material for the
particular application should be carefully considered before
proceeding.
6.3 Distillation. Weigh the distillation flask to the nearest
0.05 g. and then weigh 100.0 ± 0.1 g. of the sample into it.
Weigh five flasks of 50 ml to 100 ml to collect the various
distillate fractions. Assemble the distillation apparatus in an
appropriate and safe manner. Apply heat to the flask so that,
45 seconds after the first drop of distillate falls from the end
of the condenser, the distillation rate is 80 to 100 drops per
minute. Maintain this rate throughout the distillation. If the
sample contains over 1% of water, heat the flask and
contents slowly until the vapor temperature reaches 170°C to
distill over water before continuing the distillation as
described above. Warm the condenser tube whenever
necessary to prevent accumulation of solid distillates in the
tube. Collect the distillate fractions in the tared receiver
flasks at the points designated by the specifications below,
changing receivers as the thermometer indicates the
maximum temperature, corrected as described in the
following paragraph, for each fraction. The following
fractions are specified:
• Up to 210°C
• 210° to 235°C
• 235° to 270°C
• 270° to 315°C
• 315° to 355°C
Do not change the position of