Flash Point by Small Scale Closed Cup Tester: Standard Test Methods For
Flash Point by Small Scale Closed Cup Tester: Standard Test Methods For
Flash Point by Small Scale Closed Cup Tester: Standard Test Methods For
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
INTRODUCTION
These small scale flash point methods are generally used for testing a sample at a specific
temperature where the specimen being tested and the air–vapor mixture above it are close to thermal
equilibrium. Test Method D3941 covers other flash point equipment operated at a specific temperature.
Flash point values are a function of the apparatus design, the condition of the apparatus used, and
the operational procedure carried out. Flash point can therefore only be defined in terms of a standard
test method, and no general valid correlation can be guaranteed between results obtained by different
test methods, or with test apparatus different from that specified.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
5
Supporting data have been filed at the Energy Institute, 61 New Cavendish 16. Keywords
Street, London W1G 7AR. UK, http://www.energyinst.org and may be obtained by
requesting Research Report IP 523/10. 16.1 combustible; fire risk; flammable; flash point; volatile
TABLE 2 Calculated Repeatability and Reproducibility for Petroleum and Related Products
Temperature, 20 40 60 80 100 120 140 160 180 200 210
°C
Repeatability, 2.0 2.3 2.6 2.9 3.2 3.5 3.8 4.1 4.4 4.7 4.9
°C
Reproducibility, 3.3 3.8 4.4 4.9 5.4 5.9 6.4 6.9 7.4 7.9 8.2
°C
(Mandatory Information)
A1.1 Flash Test Apparatus, see Fig. A1.1 and Table A1.1. of the ignition source shall intersect the plane of the underside
of the cover. The cover is also provided with an orifice
A1.2 Test Cup, consisting of an aluminum alloy or nonrust- extending into the sample well for insertion of the test
ing metal block of suitable conductivity with a cylindrical specimen and also a suitable clamping device for securing the
depression over which is fitted a cover. A temperature measur- cover tightly to the metal block. The three openings in the
ing device is inserted in the block. cover shall be within the diameter of the sample well. When the
A1.2.1 The cover comprises a lid fitted with an opening shutter is in the open position, the two openings in the shutter
shutter and a device capable of inserting an ignition source into shall coincide with the two corresponding openings in the
the test cup when the shutter is open. When inserted, the nozzle cover.
A2.1 Certified Reference Material (CRM)—CRM is a the flash points in Table A2.1 can be found in the research report.5,8
stable, pure (99+ mole % purity) hydrocarbon or other stable NOTE A2.2—Materials, purities, flash point values and limits stated in
Table A2.1 were developed in interlaboratory programs to determine
petroleum product with a method-specific flash point estab- suitability of use for verification fluids in flash point test methods. Other
lished by a method-specific interlaboratory study following materials, purities, flash point values, and limits can be suitable when
ASTM research report guidelines7 or ISO Guides 34 and 35. produced according to the practices of ASTM RR:D02-10077 or ISO
Guides 34 and 35. Certificates of performance of such materials should be
A2.1.1 Typical values of the flash point corrected for consulted before use, as the flash point value will vary dependent on the
barometric pressure for some reference materials and their composition of each CRM batch.
typical limits are given in Table A2.1 (see Note A2.2).
Suppliers of CRMs will provide certificates stating the method- A2.2 Secondary Working Standard (SWS)—SWS is a stable,
specific flash point for each material of the current production pure (99+ mole % purity) hydrocarbon, or other petroleum
batch. Calculation of the limits for these other CRMs can be product whose composition is known to remain appreciably
determined from the reproducibility value of this test method stable.
and then multiplied by 0.7. This value provides a nominal A2.2.1 Establish the mean flash point and the statistical
coverage of at least 90 % with 95 % confidence. control limits (3σ) for the SWS using standard statistical
NOTE A2.1—Supporting data for the interlaboratory studies to generate techniques (see Practice D6299).
7 8
Supporting data have been filed at ASTM International Headquarters and may Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1007. Contact ASTM Customer be obtained by requesting Research Report RR:S15-1010. Contact ASTM Customer
Service at service@astm.org. Service at service@astm.org.
TABLE A2.1 D3828 Typical Flash Point Values and Typical Toler-
ances (Acceptance Limits for a Single Result)
Substance Flash Point, °C Tolerances Limits,
(0.7R)
°C
2-ButanolA 20.7 ±2.3
p-Xylene (1,4- 26.1 ±2.4
dimethylbenzene)A
n-ButanolA 36.5 ±2.6
DecaneB 49.7 ±2.9
UndecaneB 65.9 ±3.2
Diethylene GlycolA 142.2 ±4.5
A
Mean values from interlaboratory test program, see Research Report IP 523/10.
B
Mean values from interlaboratory test program, see Research Report RR:
S15-1010.
A3.1 Background FAME types were used: rapeseed and sunflower seed. Each
A3.1.1 A pan European round robin was conducted using sample type was contaminated with 0 %, 0.05 %, 0.1 %, 0.2 %,
test method EN ISO 3679 in 2001 following a robustness trial. and 0.5 % methanol.
The round robin involved ten laboratories that tested ten blind
duplicate samples (twenty containers for each participant). Two
A4. SUB-AMBIENT TESTING FOR MANUAL APPARATUS WITHOUT INTEGRAL TEST CUP COOLING FACILITIES
A4.1 Apparatus Using a Liquid in Glass Thermometer— target temperature, remove the cooling block and quickly dry
Switch off the power to the test cup heater. the test cup and underside of the cover with a paper tissue to
A4.1.1 If the manual apparatus uses an electronic thermom- remove any moisture. Immediately close the cover and secure.
eter follow the apparatus manufacturer’s instructions for set- (Warning—If a liquid in glass thermometer is being used, do
ting the required sub-ambient test temperature. not cool the sample block below the freezing point of the liquid
in the thermometer.) Prepare to introduce the test specimen into
A4.2 Fill the refrigerant-charged cooling block with a suit- the test cup using the syringe, both of which have been
able material. When the target or specification temperature is precooled to a temperature at least 10 °C (18 °F) below the
not less than 5 °C (40 °F), crushed ice and water can be used required test temperature.
as a charging (cooling) fluid. If below 5 °C (40 °F) a suitable
charging (cooling) fluid is solid carbon dioxide (dry ice) and A4.3 Adjust the test flame and allow the test cup tempera-
acetone. (Warning—Acetone is extremely flammable. Dry ice ture to rise under ambient conditions until the required test
shall not contact the eyes or skin.) If the refrigerant-charged temperature is reached. Immediately apply the test flame.
cooling module is unavailable, refer to the manufacturer’s Watch closely for a flash at the cover openings.
instruction manual for alternative methods of cooling. Raise
the cover, and position the base of the block in the sample cup, A4.4 To determine the flash point of any materials carry out
being careful not to damage or mar the test cup. When the repeat tests, with a new specimen each time, in accordance
thermometer reads approximately 10 °C (18 °F) below the with the steps given in 12.1.
A5.1 General—When in position in the block, the tempera- A5.2.3 Accuracy (after calibration) to meet the require-
ture measuring device shall be fitted to ensure good heat ments of A1.2.2.
transfer between the block and the measuring device. The use
of heat transfer paste between the sensor and the block is NOTE A5.1—Guidelines for digital temperature measuring devices are
given in Specification E1137/E1137M and ISO 60751.
advisable.
A5.2 Digital
A5.2.1 Temperature range, –30 °C to 300 °C.
A5.2.2 Display resolution, better than 0.5 °C.
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