TECHNICAL BULLETIN

TO: LABORATORY STAFF

SUBJECT: TB-00098 – D2386 STANDARD TEST METHOD FOR

ASTM D2386 – The Proper Apparatus Setup

Following the method specifications is the best way to obtain quality and accurate results. Not
setting up the apparatus or validating the equipment as stated in the methods could lead to
deviations in results.

Please read the full scope of the method prior to evaluating your D2386 apparatus setup. Below
is 1.1 and 1.3 of the scope.

1.1 This test method covers the determination of the temperature below which solid hydrocarbon
crystals may form in aviation turbine fuels and aviation gasoline. If no crystallization point or freezing
point can be measured, this test can be used to report the lowest measurable temperature reached
before the crystallization point.

1.3 This standard does not purport to address all the safety concerns, if any, associated with its use. It
is the responsibility of the user of this standard to establish appropriate safety, health, and
environmental practices and determine the applicability of regulatory limitations prior to use. For
specific warning statements, see 5.4, Section 6, and 8.3.

In the method there are several sections that pertain to the setup of the apparatus, and the
reagents and materials to use. In addition, in the procedure section eight it also addresses the
proper setup and sample size. AmSpec prefers the use of the automatic mechanical stirrer as
stated in section 5 note 2, and verified the cycles as stated in section 8 note 7.

5. Apparatus
5.1 Jacketed Sample Tube—A double-walled, un-silvered vessel, like a Dewar flask, the space between the inner
and outer tube walls being filled at atmospheric pressure with dry nitrogen or air. The mouth of the sample tube
shall be closed with a stopper supporting the thermometer and moisture-proof collar through which the stirrer
passes (Fig. 1). A cork stopper is recommended.

• The technician must inspect the jacketed sample tube for visible cracks.

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5.2 Collars—Moisture-proof collars as shown in Fig. 2 shall be used to prevent condensation of moisture.

5.3 Stirrer—Shall be made of 1.6 mm brass or stainless-steel rod bent into a smooth three-loop spiral at the
bottom.

NOTE 2—The stirrer may be mechanically actuated as described in the apparatus section of Test Method D3117.

5.4 Vacuum Flask—An un-silvered vacuum flask (Warning—Implosion hazard) having the minimum dimensions
shown in Fig. 1 shall be used to hold an adequate volume of cooling liquid and permit the necessary depth of
immersion of the jacketed sample tube. 5.5 Thermometer—A total immersion type, having a range from −80 °C to
+20 °C, designated as ASTM No. 114C/IP No. 14C. (See Specification E1, or Appendix A, IP Standard
Thermometers, Volume 2, IP Standard Methods for Analysis
and Testing of Petroleum and Related Products.)

• The technician must inspect the vacuum flask for visible cracks.

NOTE 3—The accuracy of this thermometer is to be checked in accordance with Test Method E77, at
temperatures of 0 °C, −40 °C, −60 °C, and −75 °C.

6. Reagents and Materials

6.2 Ethanol or Ethyl Alcohol—A commercial or technical grade of dry ethanol is suitable for the cooling bath.
(Warning—Extremely flammable.)

6.3 Isopropyl Alcohol—A commercial or technical grade of dry isopropyl alcohol is suitable. (Warning—Extremely
flammable.)

6.4 Methanol or Methyl Alcohol—A commercial or technical grade of dry methanol is suitable for the cooling bath.
(Warning—Extremely flammable and toxic.)

6.5 Carbon Dioxide (Solid) or Dry Ice—A commercial grade of dry ice is suitable for use in the cooling bath.
(Warning—Extremely cold, −78 °C. Carbon dioxide (solid) liberates gases that can cause suffocation. Contact
with skin causes burns, freezing, or both.)

6.6 Liquid Nitrogen—A commercial or technical grade of liquid nitrogen is suitable for the cooling bath when the
freezing point is lower than −65 °C. (Warning—Extremely cold, −196 °C. Liquid nitrogen liberates gases that can
cause suffocation. Contact with skin causes burns, freezing, or both.)

6.7 Fiberglass—commercial grade, for use in moisture proof collar B.

6.8 Dehydrating Agent—Use one of the following:

6.8.1 Calcium sulfate (CaS04), granulated anhydrous calcium sulfate, for use as a desiccant in moisture-proof
collar B, or to assist in drying the nitrogen gas or air (5.2) used with collar A.

6.8.2 Silica gel, 1.7 mm, for use as a desiccant in moisture proof collar B, or to assist in drying the nitrogen gas or
air (5.2) used with collar A. (Warning—Silica gel dyed with cadmium salts can cause cancer by inhalation.)

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 8. Procedure
8.1 Collar—Assemble the collar (5.2), thermometer (5.5) and stirrer (5.3) into the cork. To prevent the ingress of
water into the test portion, it is important that an effective moisture proof collar as prepared in accordance with
8.1.1 or 8.1.2 is used.

8.1.1 Collar type A, flush with nitrogen or dry air before fitting to the jacketed sample tube, and throughout the
entire determination.

NOTE 4—The air can be effectively dried by passing through absorbent tubes filled with dehydrating agents
(6.8.1 and 6.8.2). 8.1.2 Collar type B, fill with fiberglass (6.7) and a suitable dehydrating agent (6.8.1 and 6.8.2) as
shown in Fig. 2. The fiberglass shall be replaced every fourth test. The dehydrating agent should be renewed at
intervals of not more than 3 months or when a color change shows it to be ineffective 8.2 Measure out 25 mL 6 1
mL of the fuel and transfer it to the clean, dry, jacketed sample tube. Close the tube tightly with the cork holding
the stirrer, thermometer, and moisture proof collar and adjust the thermometer position so that its bulb does
not touch the walls of the tube flask and is approximately in the center. The bulb of the thermometer should be 10
mm to 15 mm from the bottom of the sample tube. (Warning—Do not add solid carbon dioxide to liquid nitrogen.)

NOTE 5—Performance of this test method can be difficult, since the specimen tube is immersed in a coolant
medium that evolves gas bubbles during the test. This can interfere with visual observations. In addition, the
crystals that are formed in the specimen can be difficult to recognize, and they can appear in a variety of
manifestations. It is strongly suggested that operators seek guidance from experienced operators of this test
method to assist them in the correct recognition of these crystals.

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NOTE 6—This test method should be performed under laboratory conditions where there is an ample supply of
light. Some crystals can be very faint in appearance and difficult to observe under inadequate lighting conditions.
8.3 Clamp the jacketed sample tube so that it extends as far as possible into the vacuum flask (Warning—
Implosion hazard) containing the cooling medium (Note 7). The surface of the sample should be approximately 15
mm to 20 mm below the level of the coolant. Unless the medium is cooled by mechanical refrigeration, add solid
carbon dioxide as necessary throughout the test to maintain the coolant level in the vacuum flask.

NOTE 7—Acetone and either methyl, ethyl, or isopropyl alcohols are suitable. All of these require cautious
handling. Liquid nitrogen may also be used as a coolant instead of liquids cooled with solid carbon dioxide for
fuel samples which have a freezing point below −65 °C. Mechanical refrigeration is permitted. Where used the
refrigerant temperature should be −70 °C to 80 °C. 8.4 Stir the fuel continuously, moving the stirrer up and
down at the rate of 1 cycle ⁄s to 1.5 cycles ⁄s, taking care that the stirrer loops approach the bottom of the flask on
the downstroke and remain below the specimen surface on the upstroke. It is permissible for momentary
interruption of stirring while performing some operations of the procedure (see Note 8). Observe the specimen
continuously for the appearance of hydrocarbon crystals. Disregard any cloud that appears at approximately −10
°C and does not increase in intensity as the temperature decreases, because this cloud is due to water. Record
the temperature at which hydrocarbon crystals appear. This is the crystallization point. Remove the jacketed
sample tube from the coolant and allow the specimen to warm by ambient air, stirring it continuously at 1 cycle ⁄s
to 1.5 cycles ⁄s. Continue to observe the specimen continuously for the disappearance of hydrocarbon crystals.
Record the temperature at which the hydrocarbon crystals completely disappear. This is the observed freezing
point. If the crystallization point cannot be reached by continuously cooling the fuel to the lowest temperature
achievable by the apparatus (between –65 °C and –70 °C) when using solid CO2 and alcohol as
coolant, record the lowest measurable temperature that the fuel reaches.

NOTE 8—Because the gases released by the coolant can obscure observations, the sample tube can be
removed from the coolant for observations. The tube can be removed for periods no longer than 10 s. If
crystals are observed to have already formed, the specimen temperature should be noted, and the specimen
allowed to be warmed by ambient air, with continued stirring, to at least 5 °C above the temperature at which the
crystals disappear. The specimen should then be re-immersed in the coolant and allowed to cool. Remove the
specimen from the coolant slightly above the noted temperature and observe the appearance of the crystals.

NOTE 9—It is recommended to compare the crystal appearance temperature with the crystal disappearance
temperature. The appearance temperature should be colder than the disappearance temperature. If this is
not the case, this is an indication that the crystals were not correctly recognized. Also, the difference between
these temperatures should typically be no greater than 6 °C.

This Technical Bulletin should be reviewed and documented by appropriate personnel using the attached
Training attendee form (also available on SharePoint) within 30 days of bulletin issue date.

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