Astm D 611-04 Punto Anilina
Astm D 611-04 Punto Anilina
Astm D 611-04 Punto Anilina
Designation: D 611 – 04
Designation: 2/98
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This standard has been approved for use by agencies of the Department of Defense.
ANNEXES
(Mandatory Information)
A1.1 Apparatus (8.1) into the test tube fitted with stirrer and thermometer. If the
A1.1.1 The apparatus shown in Fig. A1.1 shall consist of the material is too viscous for volumetric transfer, weigh to the
following: nearest 0.01 g a quantity of the sample corresponding to 10 mL
A1.1.1.1 Test Tube, approximately 25 mm in diameter and at room temperature. Center the thermometer in the test tube so
that the immersion mark is at the liquid level, making sure that
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150 mm in length, made of heat-resistant glass.
A1.1.1.2 Jacket, approximately 37 to 42 mm in diameter the thermometer bulb does not touch the side of the tube.
and 175 mm in length, made of heat-resistant glass. Center the test tube in the jacket tube. Stir the mixture rapidly
A1.1.1.3 Stirrer, manually operated, metal, approximately 2 using a 50-mm (2-in.) stroke, avoiding the introduction of air
mm in diameter (14 B&S gage) metal wire as shown in Fig. bubbles.
A1.1. A concentric ring shall be at the bottom, having a A1.2.2 If the aniline-sample mixture is not miscible at room
diameter of approximately 19 mm. The length of the stirrer to temperature, apply heat directly to the jacket tube so that the
a right-angle bend shall be approximately 200 mm. The temperature rises at a rate of 1 to 3°C (2 to 5°F)/min by
right-angle bend shall be approximately 55 mm long. A glass removing or reducing the heat source until complete miscibility
sleeve approximately 65 mm in length of 3-mm inside diameter is obtained. Continue stirring and allow the mixture to cool at
shall be used as a guide for the stirrer. Any suitable mechanical a rate of 0.5 to 1.0°C (1.0 to 1.8°F)/min. Continue cooling to
device for operating the stirrer as specified is an approved a temperature of 1 to 2°C (2.0 to 3.5°F) below the first
alternative for the manual operation. appearance of turbidity, and record as the aniline point the
temperature at which the mixture suddenly becomes cloudy
A1.2 Procedure throughout (Note A1.1). This temperature, and not the tem-
A1.2.1 Clean and dry the apparatus. Deliver 10 mL of perature of separation of small amounts of material, is the
aniline (Warning—See 7.1) and 10 mL of the dried sample minimum equilibrium solution temperature.
NOTE A1.1—The true aniline point is characterized by a turbidity that A1.2.4 Repeat the observation of aniline point temperature
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is so cloudy as to obscure the thermometer bulb in reflected light. by heating and cooling repeatedly until a report as directed in
A1.2.3 If the aniline-sample mixture is completely miscible Section 11 can be made.
at room temperature, substitute a non-aqueous cooling bath for
the heating source, allow to cool at the rate specified in A1.2.2
and determine the aniline point as described.
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FIG. A2.2 Assembly of Thin-Film Apparatus (Test Method B)
A3.1 Apparatus sufficient light transformer oil to cover the bulb of the
A3.1.1 Aniline-Point Tube, of heat-resistant glass, of the thermometer. The inner tube is held in the top of the aniline-
shape and dimensions shown in Fig. A3.1, and fitted internally point tube by a tightly fitting stopper, and a clamp is provided
with a thin-walled glass thermometer tube, sealed at the lower to hold the stopper in position to prevent loss of vapor from the
end. The latter tube accommodates a tight-fitting cork stopper sample.
carrying the thermometer, the bulb of which rests on a cork NOTE A3.1—Any other suitable arrangement, such as a screwed plastic
ring or disk placed at the bottom of the tube; the tube contains gland carrying the thermometer, that will prevent the loss of vapor from
the apparatus, may be used. In such cases it may be possible to omit the
thermometer tube and immerse the thermometer bulb in the aniline-
sample mixture.
A3.1.2 Guard, of stout metal gauze and surrounding the
aniline point tube. It should preferably be combined with the
clamp for holding the thermometer tube in place.
A3.2 Procedure
A3.2.1 Clean and dry the apparatus. Deliver 5 mL of aniline
(Warning—Put on goggles of safety glass and plastic gloves
impervious to aniline. Also see 7.1) and 5 mL of the dried
sample (8.1), both cooled to a temperature at which the sample
may be measured without loss of vapor. Close the tube by
means of the stopper and fit the thermometer tube centrally so
that the bottom is 5 mm from the bottom of the aniline point
tube. Clamp the stopper in position and attach the guard.
A3.2.2 Follow the procedure described in A1.2.2 and A1.2.3
but mix the sample and aniline by shaking the tube. If the rate
of change of temperature is greater than 1°C (2°F)/min when
the aniline point is being approached, place the tube in a jacket
that has previously been warmed or cooled to an appropriate
temperature.
A3.2.3 Repeat the observation of aniline point by heating
and cooling repeatedly until a report as directed in Section 11
FIG. A3.1 Apparatus for Volatile Samples (Test Method C) can be made.
A4.1 Apparatus rapidly draw out and seal the open end of the bulb at about 10
A4.1.1 Bulb, 1.5 to 2.0-mL capacity, blown from heat- mm from the center of the bulb. (Warning—Put on goggles of
resistant glass tubing, 5 mm in external diameter and 3 mm in safety glass and plastic gloves impervious to aniline.)
internal diameter. A4.2.2 Attach the bulb to the thermometer by rubber bands
A4.1.2 Guard, as for Test Method C. so that the bulb is adjacent to the thermometer bulb. Attach the
mesh guard and follow the procedure described in A1.2.2 and
A4.2 Procedure
A1.2.3 but mix the sample and aniline by shaking.
A4.2.1 Dry the bulb thoroughly in an oven at 105 6 5°C, A4.2.3 Repeat the observation of aniline point temperature
allow it to cool to room temperature, and charge it by means of
by heating and cooling repeatedly until a report as directed in
the pipets with 0.5 mL of aniline (Warning—See 7.1) and 0.5
Section 11 can be made.
mL of the dried sample (8.1). Cool the mixture thoroughly and
SUMMARY OF CHANGES
Subcommittee D02.04 has identified the location of selected changes to this standard since the last issue
(D 611–01b) that may impact the use of this standard.
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