ASTM D56-16a Procedural Outline

Standard Test Method for Flash Point by Tag Closed Cup Tester
The following summarizes the procedural steps required for the determination of the flash point,
by tag manual and automated closed testers, of liquids with a viscosity below 5.5 mm2/s (cSt) at
40 °C (104 °F), or below 9.5 mm2/s (cSt) at 25 °C (77 °F), and a flash point below 93 °C (200 °F).

Reference is made to Sections 6 through 13 of the standard.

The following steps apply for apparatus (manual instrument). (Section 6)

1. Tag Closed Tester
a. The apparatus is shown in Fig. 1 and described in detail in Annex A1. (Section
6.1)

FIG. 1 Tag Closed Flash Tester (Manual)

2. Shield (Section 6.2)

a. 460 mm (18 in.) square and 610 mm (24 in.) high, open in front, is recommended.

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 3. Temperature Measuring Device (Section 6.3)
a. A liquid-in-glass thermometer, as prescribed in Table 1, or an electronic
temperature measuring device such as a resistance device or thermocouple.
b. The device shall exhibit the same temperature response as the liquid-in-glass
thermometer.

TABLE 1 Thermometers

At 4 °C to 49 °C Above 49 °C
For tests Below 4 °C (40 °F) (40 °F to 120 °F) (120 °F)

Use ASTM 57C or (57F) 9C or (9F) 9C or (9F)

ThermometerA 57C or (57F)

A Complete specifications for these thermometers are given in ASTM Specification E1.

Note: Whenever thermometers complying with ASTM requirements

are not available, thermometers complying with the requirements
for The Institute of Petroleum thermometer IP 15C PM-Low can be
used. (Note 2).

The following steps apply for sampling (Section 7)

4. Erroneously high flash points will be obtained when precautions are not taken to avoid
the loss of volatile material. (Section 7.1)
a. Containers should not be opened unnecessarily to prevent loss of volatile
material and possible introduction of moisture.
b. Transfers should not be made unless the sample temperature is at least 10 °C
(18 °F) below the expected flash point
c. When possible, flash point shall be the first test performed on a sample and the
sample must be stored at low temperature.
5. Do not store samples in gas-permeable containers since volatile materials may diffuse
through the walls of the enclosure. (Section 7.2)
a. Samples in leaky containers are suspect and not a source of valid results.
6. At least 50 mL of sample is required for each test. (Section 7.3)
a. Refer to sampling information in ASTM Practice D4057.

The following steps apply for preparation of apparatus (manual). (Section 8)

7. Support the manual apparatus on a level steady surface, such as a table. (Section 8.1)
8. Unless tests are made in a draft-free room or compartment, surround the tester on three
sides by the shield for protection from drafts.
9. Tests are not to be made in a laboratory draft hood or near ventilators.
10. Natural gas and bottled gas flame and electric ignitors have been found acceptable for
use as the ignition source. (Section 8.2)

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 Warning: Gas pressure supplied to the apparatus must not be
allowed to exceed 3 kPa (12 in.) of water pressure.
11. For flash points below 13 °C (55 °F) or above 60 °C (140 °F), use as a bath liquid a 1 + 1
mixture of water and ethylene glycol. (Section 8.3)
Warning: Ethylene Glycol—Poison. Harmful or fatal if swallowed.
Vapor harmful. Avoid contact with skin.
12. For flash points between 13 °C (55 °F) and 60 °C (140 °F), either water or a water-glycol
mixture can be used as bath liquid.
13. The temperature of the liquid in the bath shall be at least 10 °C (18 °F) below the
expected flash point at the time of introduction of the sample into the test cup.
14. Do not cool bath liquid by direct contact with dry ice (solid carbon dioxide).
Note: Due to possible difficulty in maintaining the prescribed rate of
temperature rise and due to the formation of ice on the lid, results
by this test method for samples having flash points below 0 °C
(32 °F) may be unreliable. Trouble due to ice formation on the slide
can be minimized by carefully lubricating the slide shutter with high-
vacuum silicone lubricant. (Note 3)
15. Verify the performance of the manual apparatus (or in Section 11.2.3, the automated
apparatus) at least once per year by determining the flash point of a certified reference
material (CRM), such as those listed in Annex A2, which is reasonably close to the
expected temperature range of the samples to be tested. (Section 8.4)
a. The material shall be tested according to the procedure of this test method and
the observed flash point obtained in Section 9.5 shall be corrected for barometric
pressure, reference Section 13.
b. The flash point obtained shall be within the limits stated in Table A2.1 for the
identified CRM or within the limits calculated for an unlisted CRM,
reference Annex A2.
16. Once the performance of the apparatus has been verified, the flash point of secondary
working standards (SWSs) can be determined along with their control limits. (Section
8.5)
a. These secondary materials can then be utilized for more frequent performance
checks, reference Annex A2.
17. When the flash point obtained is not within the limits stated in Section 8.4 or 8.5, check
the condition and operation of the apparatus to ensure conformity with the details listed
in Annex A1, especially with regard to: (Section 8.6)
a. tightness of the lid, reference A1.1.3,
b. the action of the shutter,
c. the position of the ignition source, reference A1.1.3.3, and
d. the angle and position of the temperature measuring device, reference A1.1.3.4.
18. After any adjustment, repeat the test in Section 8.4 using fresh test specimen, with
special attention to the procedural details prescribed in the test method.

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The following steps apply for procedure (manual). (Section 9)
19. Using a graduated cylinder and taking care to avoid wetting the cup above the final liquid
level, measure 50 mL ± 0.5 mL of the sample into the cup, both the sample and
graduated cylinder being precooled, when necessary, so that the specimen temperature
at the time of measurement will be 27 °C ± 5 °C (80 °F ± 10 °F) or at least 10 °C (18 °F)
below the expected flash point, whichever is lower. (Section 9.1)
a. It is essential that the sample temperature be maintained at least 10 °C (18 °F)
below the expected flash point during the transfers from the sample container to
the cylinder and from the cylinder to the test cup.
20. Destroy air bubbles on the surface of the specimens by use of knife point or other
suitable device.
21. Wipe the inside of the cover with a clean cloth or absorbent tissue paper; then attach the
cover, with the temperature measuring device in place, to the bath collar.
22. Light the test flame, when used, adjusting it to the size of the small bead on the
cover. (Section 9.2)
a. Operate the mechanism on the cover in such a manner as to introduce the
ignition source into the vapor space of the cup, and immediately bring it up
again.
b. The time consumed for the full operation should be 1 s, allowing equal time
periods for the introduction and return.
c. Avoid any hesitation in the operation of depressing and raising the ignition
source.
d. When a flash is observed on the initial operation of the mechanism, discontinue
the test and discard the result.
e. In this case, a fresh sample shall be cooled an additional 10 °C (18 °F), below the
original specimen installation temperature
23. Exercise care when using a test flame, if the flame is extinguished it cannot ignite the
specimen and the gas entering the vapor space can influence the result. (Section 9.2.1)
a. When the flame is prematurely extinguished the test shall be discontinued and
any result discarded.
The following steps apply to flash points below 60ºC (140ºF) (Section 9.3)
24. When the flash point of the sample is known to be below 60 °C (140 °F), apply and
adjust the heat so that the temperature of the portion will rise at a rate of 1 °C (2 °F)/min
± 6 s.
25. When the temperature of the specimen in the test cup is 5 °C (10 °F) below its expected
flash point, apply the ignition source in the manner just described in Section 9.2 and
repeat the application of the ignition source after each 0.5 °C (1 °F) rise in temperature of
the specimen.
The following steps apply to flash points at 60ºC (140ºF) or above (Section 9.4)

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 26. If the flash point of the sample is known to be 60 °C (140 °F) or higher, apply and adjust
the heat so that the temperature of the specimen will rise at a rate of 3 °C (5 °F)/min ±
6 s.
27. When the temperature of the specimen in the test cup is 5 °C (10 °F) below its expected
flash point, apply the ignition source in the manner just described in Section 9.2 and
repeat the application of the ignition source each 1 °C (2 °F) rise in temperature of the
specimen.
28. When the application of the ignition source causes a distinct flash in the interior of the
cup, as defined in Section 3.1.1, observe and record the temperature of the specimen as
the flash point. (Section 9.5)
a. Do not confuse the true flash with the bluish halo that sometimes surrounds the
ignition source during applications immediately preceding the actual flash.
Warning: For certain mixtures containing halogenated
hydrocarbons, such as, methylene chloride or trichloroethylene, no
distinct flash, as defined, is observed. Instead a significant
enlargement of the test flame (not halo effect) and change in color
of the test flame from blue to yellowish-orange occurs. Continued
heating and testing of these samples above ambient temperature
can result in significant burning of vapors outside the test cup, and
can be a potential fire hazard. See Appendix X1 and Appendix
X2 for more information.
29. Discontinue the test and remove the source of heat. (Section 9.6)
30. Lift the lid and wipe the temperature measuring device bulb.
31. Remove the test cup, empty, and wipe dry.
32. If, at any time between the first introduction of the ignition source and the observation of
the flash point, the rise in temperature of the specimen is not within the specified rate,
discontinue the test, discard the result and repeat the test, adjusting the source of heat
to secure the proper rate of temperature rise, or using a modified "expected flash point,"
or both, as required. (Section 9.7)
33. Never make a repeat test on the same specimen of sample; always take fresh specimen
of sample for each test. (Section 9.8)

The following steps apply for apparatus (automated instrument). (Section 10)
34. An automated flash point instrument is used that is capable of performing the test in
accordance with Section 9. (Section 10.1)
35. The apparatus can use a gas test flame or electric ignitor.
36. The dimensions for the test cup and test cover are shown in Fig. A1.1 and Fig. A1.2.

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 FIG. A1.1 Specimen Cup

Inch-Pound Equivalents
mm In. mm In.
0.03 0.001 10.32 0.406
0.13 0.005 11.92 0.469
4.78 0.188 15.10 0.594
7.15 0.281 18.0 0.71
9.84 0.387 20.6 0.81

Note: Dimensions relating to the size and position of the

temperature measuring device collar are recommended but not
mandatory. (A1 Note 1)

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 FIG. A1.2 Top of Lid Showing Position and Dimensions of Openings

37. Samples with low flash point may require a source of cooling for the heating area.
(Section 10.2)

The following steps apply for preparation of apparatus (automated instrument).

(Section 11)
38. Support the automated apparatus on a level, steady surface, such as a table. (Section
11.1)
39. Unless tests are made in a draft-free compartment, it is a good practice, but not
required, to surround the tester with a shield to prevent draft.
40. The user of the automatic instrument must be sure that all of the manufacturer's
instructions for calibrating, checking, and operating the equipment are followed. (Section
11.2)
41. Adjust the detection system per manufacturer's instructions. (Section 11.2.1)
42. Calibrate the temperature measuring device per manufacturer's instructions. (Section
11.2.2)
43. Verify the performance of the automated apparatus at least once per year by
determining the flash point of a certified reference material (CRM) such as those listed
in Annex A2, which is reasonably close to the expected temperature range of the
samples to be tested. (Section 11.2.3)
a. The material shall be tested according to the procedure of this test method and
the observed flash point obtained in Section 9.5 shall be corrected for barometric
pressure, reference Section 13.
b. The flash point obtained shall be within the limits stated in Table A2.1 for the
identified CRM or within the limits calculated for an unlisted CRM,
reference Annex A2.

TABLE A2.1 D56 Typical Flash Point Values and Typical Limits for CRM

Hydrocarbon Purity Flash Point Tolerance

(mole %) (ºC) Limits
(0.7R)
(ºC)
n-decane 99+ 50.9 3.0
n-undecane 99+ 67.1 4.1

44. Once the performance of the apparatus has been verified, the flash point of secondary
working standards (SWSs) can be determined along with their control limits. (Section
11.2.4)
a. These secondary materials can then be utilized for more frequent performance
checks, reference Annex A2.

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 45. When the flash point obtained is not within the limits stated in Section 11.2.3 or 11.2.4,
check the condition and operation of the apparatus to ensure conformity with the details
listed in Annex A1, especially with regard to: (Section 11.2.5)
a. tightness of the lid, reference A1.1.3,
b. the action of the shutter,
c. the position of the ignition source, reference A1.1.3.3, and
d. the angle and position of the temperature measuring device, reference A1.1.3.4.
46. After any adjustment, repeat the test in Section 11.2.3 using fresh test specimen, with
special attention to the procedural details prescribed in the test method.

The following steps apply for procedure. (Section 12)

47. Adjust the external cooling system, if required, to a temperature necessary to cool the
heating area 10 °C below the expected flash point. (Section 12.1)
48. Place the test cup in position in the instrument. (Section 12.2)
49. Enter the Expected Flash Point; this will allow the heating area to be cooled to the
required minimum starting temperature. (Section 12.3)
Note: To avoid an abnormal heating rate when the specimen is at
a low temperature, it is recommended to precool the test cup and
cover. This may be accomplished by placing the assembly into
position in the instrument while it is cooling to 10 °C (18 °F) below
the programmed Expected Flash Point. (Note 4)
Note: Flash Point results determined in an "unknown Expected
Flash Point mode" should be considered approximate. This value
can be used as the Expected Flash Point when a fresh specimen is
tested in the standard mode of operation. (Note 5)
50. Using a graduated cylinder and taking care to avoid wetting the cup above the final liquid
level, measure 50 mL ± 0.5 mL of the sample into the cup, both the sample and the
graduated cylinder being precooled, when necessary, so that the specimen temperature
at the time of the measurement is 27 °C ± 5 °C (80 °F ± 10 °F) or at least 10 °C (18 °F)
below the expected flash point, whichever is lower. (Section 12.4)
a. It is essential that the sample temperature be maintained at least 10 °C (18 °F)
below the expected flash point during the transfers from the sample container to
the cylinder and from the cylinder to the test cup.
51. Destroy air bubbles on the surface of the specimen by use of knife point or other suitable
device.
52. Wipe the inside of the cover with a clean cloth or absorbent tissue paper; then attach the
cover, with the temperature measuring device in place, to the bath collar.
53. Connect the shutter and ignition source activator, if so equipped, into the lid housing.
54. When using a gas test flame, light the pilot flame and adjust the test flame to 4 mm
(5/32 in.) in diameter.
55. If the instrument is equipped with an electrical ignition device, adjust according to the
manufacturer's instructions.

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 56. Test the ignition source dipping action, if so equipped, and observe if the apparatus
functions correctly.
57. Press the start key.
58. If a flash is observed upon initial operation, discontinue the test and discard the result.
a. In this case a fresh specimen shall be cooled to an additional 10 °C (18 °F) below
the original specimen installation temperature.
Note: Care should be taken when cleaning and positioning the lid
assembly so as not to damage or dislocate the flash detection
system or temperature measuring device. See manufacturer's
instructions for proper care and maintenance. (Note 6)
59. The apparatus shall automatically control the test procedure as described in this test
method. (Section 12.5)
60. When the flash point is detected, the apparatus will record the temperature and
automatically discontinue the test.
a. If a flash is detected on the first application, the test should be discontinued, the
result shall be discarded and the test repeated with a fresh specimen.
Warning: For certain mixtures containing halogenated
hydrocarbons, such as, methylene chloride or trichloroethylene, no
distinct flash, as defined, is observed. Instead a significant
enlargement of the test flame (not halo effect) and change in color
of the test flame from blue to yellowish-orange occurs. Continued
heating and testing of these samples above ambient temperature
can result in significant burning of vapors outside the test cup, and
can be a potential fire hazard. See Appendix X1 and Appendix
X2 for more information.
61. When the apparatus has cooled down to a safe handling temperature (less than 55 °C
(130 °F)) remove the cover and the test cup and clean the apparatus as recommended
by the manufacturer. (Section 12.6)

The following steps apply for report. (Section 13)

62. Correction for barometric pressure. (Section 13.1)
63. Observe and record the ambient barometric pressure at the time and place of the test.
64. When the pressure differs from 101.3 kPa (760 mm Hg), correct the flash point as
follows:
Corrected flash point = 𝐶𝐶 + 0.25 (101.3 − 𝑝𝑝) (1)

Corrected flash point = 𝐹𝐹 + 0.06 (760 − 𝑃𝑃) (2)

Corrected flash point = 𝐶𝐶 + 0.033 (760 − 𝑃𝑃) (3)

where:

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 C = observed flash point, ºC
F = observed flash point, ºF
p = ambient barometric pressure, kPa
P = ambient barometric pressure, mm Hg

65. The barometric pressure used in this calculation shall be the ambient pressure for the
laboratory at the time of test. (Section 13.2)
a. Many aneroid barometers, such as those used at weather stations and airports,
are precorrected to give sea level readings; these shall not be used.
66. Report the corrected flash point to the nearest 0.5 °C (or 1 °F).

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