Flash Point by Small Scale Closed Cup Tester: Standard Test Methods For

Download as pdf or txt
Download as pdf or txt
You are on page 1of 10

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D3828 − 16a (Reapproved 2021)

Standard Test Methods for


Flash Point by Small Scale Closed Cup Tester1
This standard is issued under the fixed designation D3828; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

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.

1. Scope responsibility of the user of this standard to establish appro-


1.1 These test methods cover procedures for flash point priate safety, health, and environmental practices and deter-
tests, within the range of –30 °C to 300 °C, of petroleum mine the applicability of regulatory limitations prior to use.
products and biodiesel liquid fuels, using a small scale closed Warning statements appear throughout. See also the Material
cup tester. The procedures may be used to determine, whether Safety Data Sheets for the product being tested.
a product will or will not flash at a specified temperature 1.5 This international standard was developed in accor-
(flash/no flash Method A) or the flash point of a sample dance with internationally recognized principles on standard-
(Method B). When used in conjunction with an electronic ization established in the Decision on Principles for the
thermal flash detector, these test methods are also suitable for Development of International Standards, Guides and Recom-
flash point tests on biodiesels such as fatty acid methyl esters mendations issued by the World Trade Organization Technical
(FAME). Barriers to Trade (TBT) Committee.
1.2 The values stated in SI units are to be regarded as the 2. Referenced Documents
standard. The values given in parentheses are for information
only. 2.1 ASTM Standards:2
D3941 Test Method for Flash Point by the Equilibrium
1.3 This standard should be used to measure and describe Method With a Closed-Cup Apparatus
the properties of materials, products, or assemblies in response D4057 Practice for Manual Sampling of Petroleum and
to heat and flame under controlled laboratory conditions and Petroleum Products
should not be used to describe or appraise the fire hazard or D4177 Practice for Automatic Sampling of Petroleum and
fire risk of materials, products, or assemblies under actual fire Petroleum Products
conditions. However, results of this test may be used as D6299 Practice for Applying Statistical Quality Assurance
elements of a fire risk assessment which takes into account all and Control Charting Techniques to Evaluate Analytical
of the factors which are pertinent to an assessment of the fire Measurement System Performance
hazard of a particular end use. D6708 Practice for Statistical Assessment and Improvement
1.4 This standard does not purport to address all of the of Expected Agreement Between Two Test Methods that
safety concerns, if any, associated with its use. It is the Purport to Measure the Same Property of a Material
E300 Practice for Sampling Industrial Chemicals
1
These test methods are under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
2
Subcommittee D02.08 on Volatility. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved July 1, 2021. Published July 2021. Originally approved contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
in 1979. Last previous edition approved in 2016 as D3828 – 16a. DOI: 10.1520/ Standards volume information, refer to the standard’s Document Summary page on
D3828-16AR21. the ASTM website.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG :HG-DQ*07


1
'RZQORDGHGSULQWHGE\
PRKDPDGZDKLGLQ $PVSHF//& SXUVXDQWWR/LFHQVH$JUHHPHQW1RIXUWKHUUHSURGXFWLRQVDXWKRUL]HG
D3828 − 16a (2021)
E1137/E1137M Specification for Industrial Platinum Resis- introduced and tested. This procedure is repeated until the flash
tance Thermometers point is established within 5 °C (9 °F).
2.2 ISO Standards:3 4.2.3 The procedure is then repeated at 1 °C (2 °F) intervals
Guide 34 General requirements for the competence of refer- until the flash point is determined to the nearest 1 °C (2 °F).
ence material producers 4.2.4 If improved accuracy is desired the procedure is
Guide 35 Reference materials—General and statistical prin- repeated at 0.5 °C (1 °F) intervals until the flash point is
ciples for certification determined to the nearest 0.5 °C (1 °F).
EN ISO 3679 Determination of Flash Point—Rapid Equilib- 4.3 Test Time and Specimen Volume:
rium Closed Cup Method 4.3.1 For all products, except biodiesel; for test tempera-
EN ISO 3680 Determination of Flash/No Flash—Rapid tures up to and including 100 °C (212 °F), the test time is
Equilibrium Closed Cup Method 1 min and the specimen volume is 2 mL.
ISO 60751 Industrial Platinum Resistance Thermometers 4.3.2 For all products, except biodiesel; for test tempera-
and Platinum Temperature Sensors tures over 100 °C (212 °F), the test time is 2 min and the
2.3 Energy Institute Standards:4 specimen volume is 4 mL.
IP 523 Determination of Flash Point—Rapid Equilibrium 4.3.3 For biodiesel; for all test temperatures, the test time is
Closed Cup Method 1 min and the specimen volume is 2 mL.
IP 524 Determination of Flash/No Flash—Rapid Equilib-
rium Closed Cup Method 5. Significance and Use
3. Terminology 5.1 Flash point measures the response of the test specimen
3.1 Definitions: to heat and ignition source under controlled laboratory condi-
3.1.1 equilibrium, n—in flash point test methods, the condi- tions. It is only one of a number of properties that must be
tion where the vapor above the test specimen, and the test considered in assessing the overall flammability hazard of a
specimen are at the same temperature at the time the ignition material.
source is applied. 5.2 Flash point is used in shipping and safety regulations to
3.1.1.1 Discussion—This condition may not be fully define flammable and combustible materials and classify them.
achieved in practice, since the temperature may not be uniform Consult the particular regulation involved for precise defini-
throughout the test specimen, and the test cover and shutter on tions of these classes.
the apparatus can be cooler or warmer. 5.3 Flash point can indicate the possible presence of highly
3.1.2 flash point, n—in flash point test methods, the lowest volatile and flammable materials in a relatively nonvolatile or
temperature of the test specimen, adjusted to account for nonflammable material.
variations in atmospheric pressure from 101.3 kPa, at which
5.4 These test methods use a smaller sample (2 mL to 4 mL)
application of an ignition source causes the vapors of the test
and a shorter test time (1 min to 2 min) than traditional test
specimen to ignite under specified conditions of test.
methods.
4. Summary of Test Methods 5.5 Method A, IP 524 and EN ISO 3680 are similar methods
4.1 Method A—Flash/No Flash Test—A test specimen is for flash no-flash tests. Method B, IP 523 and EN ISO 3679 are
introduced, by a syringe, into the test cup of the selected similar methods for flash point determination.
apparatus that is set and maintained at the specified tempera-
ture. After a specific time an ignition source is applied and a 6. Apparatus
determination made as to whether or not a flash occurred. 6.1 Test Cup and Cover Assembly—The essential dimen-
4.2 Method B—Finite (or Actual) Flash Point—This sions and requirements of the apparatus are shown in Fig. A1.1
method essentially repeats Method A a number of times, and by and Table A1.1 of Annex A1. The apparatus and accessories
changing the test temperature and test specimen a number of are described in detail in Annex A1. The temperature range is
times, determines the flash point. from –30 °C to 300 °C. Some versions of the apparatus may
4.2.1 A test specimen is introduced into the test cup of the not cover the full temperature range.
selected apparatus that is maintained at the expected flash 6.2 Barometer, accurate to 0.5 kPa. Barometers that have
point. After a specified time an ignition source is applied and a been pre-corrected for use at weather stations or airports are
determination made whether or not a flash occurred. not suitable.
4.2.2 The test specimen is removed from the test cup; the
6.3 Draft Shield—A shield located at the back and on two
test cup and cover are cleaned, and the test temperature
sides of the instrument, for use in circumstances where
adjusted 5 °C (9 °F) lower or higher depending on whether or
protection from drafts does not exist.
not a flash occurred previously. A fresh test specimen is
7. Reagents and Materials
3
Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
7.1 Cleaning Solvent—Use only non-corrosive solvents ca-
4th Floor, New York, NY 10036, http://www.ansi.org.
4
Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR, pable of cleaning the test cup and cover. Two commonly used
U.K., http://www.energyinst.org.uk. solvents are toluene and acetone. (Warning—Toluene, acetone

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG :HG-DQ*07


2
'RZQORDGHGSULQWHGE\
PRKDPDGZDKLGLQ $PVSHF//& SXUVXDQWWR/LFHQVH$JUHHPHQW1RIXUWKHUUHSURGXFWLRQVDXWKRUL]HG
D3828 − 16a (2021)
and many other solvents are flammable and a health hazard. sides with a draft shield (see 6.3) for protection. Do not rely on
Dispose of solvents and waste material in accordance with tests made in a laboratory draft hood unless the extracted air
local regulations.) and vapors can be withdrawn without causing air currents over
7.2 Butane, Propane and Natural Gas—For use as a pilot the test cup during the ignition source application period.
and ignition source (not required if an electric ignitor is used). 9.2 Read the manufacturer’s instructions on the care and
(Warning—Butane, propane and natural gases are flammable servicing of the instrument and for the correct operation of any
and a health hazard.) controls.
9.3 Prepare the apparatus for operation in accordance with
8. Sampling
the manufacturers’ instructions for calibrating, checking and
8.1 Obtain at least a 50 mL sample from a bulk test site in operating the equipment, especially the operation of the igni-
accordance with Practices D4057, D4177, E300 or other tion source. (Warning—An incorrectly set test flame size or
comparable sampling practices. setting of an electric ignitor can significantly affect the test
8.2 Store samples in clean, tightly sealed containers at result.)
normal room temperature (20 °C to 25 °C) or colder. 9.4 Clean the test cup, cover and its accessories with an
8.3 Do not store samples for an extended period of time in appropriate solvent (7.1) to remove any traces of gum or
gas permeable containers, such as those made of plastic, residue from the previous test. Wipe dry with absorbent paper.
because volatile material can diffuse through the walls of the A stream of dry clean air may be used to remove the last traces
container. Samples in leaky containers are suspect and not a of solvent used. A pipe cleaner may be used to clean the filler
source of valid results. orifice.
8.4 Erroneously high flash points can be obtained when 9.5 Measure and record the barometric pressure (6.2) before
precautions are not taken to avoid loss of volatile materials. Do commencing a test.
not open containers unnecessarily. Do not make a transfer 9.6 Use an electronic thermal flash detector for flash point
unless the sample temperature is at least 10 °C below the tests on biodiesels such as fatty acid methyl esters (FAME) (see
expected flash point. Where possible perform the flash point as A1.7). The flash detector may be used for other test materials.
the first test on the sample.
9.7 For sub-ambient test temperatures see Annex A4, unless
8.5 Samples containing dissolved or free water may be the apparatus has integral test cup cooling facilities.
dehydrated with calcium chloride. (Warning—If the sample is
expected of containing volatile components, the treatment as 10. Verification of Apparatus
described in 8.5 should be omitted.)
10.1 Verify and correct, if necessary, the readings on the
8.6 Cool, or adjust the temperature of the sample and its temperature measuring device at least every 12 months, ac-
container to at least 10 °C below the expected flash point cording to the manufacturer’s instructions and that the tem-
before opening to remove the test specimen. If an aliquot of the perature measuring device is in accordance with A1.2.2 and
original sample is to be stored prior to testing, ensure that the Annex A5.
container is filled to between 85 % and 95 % of its capacity.
NOTE 1—Results of flash point tests can be affected if the sample 10.2 Verify the performance of the apparatus at least once
volume falls below 50 % of the container’s capacity. per year by determining the flash point of a certified reference
8.7 If sufficiently fluid, mix samples by gently shaking by material (CRM) such as those listed in Annex A2, which is
hand prior to removal of the test specimen, taking care to reasonably close to the expected temperature range of the
minimize the loss of volatile components. If the sample is too samples to be tested. The material shall be tested according to
viscous at ambient temperature, gently warm the sample in its Method B, Section 12 and the detected flash point determined
container to a temperature not warmer than 10 °C below the in 12.1.6 and 12.1.6.1 shall be corrected for barometric
test temperature, such that the sample can be mixed by gentle pressure (see Section 13). The flash point obtained shall be
shaking. Ensure that high pressures do not develop in the within the limits stated in Table A2.1 for the identified CRM or
container when warming. within the limits calculated for an unlisted CRM (see Annex
A2).
8.8 If the sample cannot be made sufficiently fluid to be
introduced into the test cup through the orifice by heating in 10.3 Once the performance of the apparatus has been
accordance with 8.7, transfer the test specimen with a solids verified, the flash point of secondary working standards (SWS)
dispenser or spatula while the cover is open. The specimen size can be determined along with their control limits. These
can be the mass equivalent of the required volume and the secondary materials can then be utilized for more frequent
specimen should be spread over the bottom of the test cup as performance checks (see Annex A2).
evenly as possible. Precision has not been determined for solid 10.4 When the flash point obtained is not within the limits
samples. stated in 10.2 or 10.3, check the condition and operation of the
apparatus to ensure conformity with the details listed in Annex
9. Preparation of Apparatus A1, especially with regard to tightness of the cover (A1.2.1),
9.1 Place the apparatus on a level, stable surface. Unless the action of the shutter, the size or intensity of the ignition
tests are made in a draft-free area, surround the tester on three source, the position of the ignition source (A1.3), the operation

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG :HG-DQ*07


3
'RZQORDGHGSULQWHGE\
PRKDPDGZDKLGLQ $PVSHF//& SXUVXDQWWR/LFHQVH$JUHHPHQW1RIXUWKHUUHSURGXFWLRQVDXWKRUL]HG
D3828 − 16a (2021)
of the flash detector (if fitted) and correct reading of the ignition source can cause a blue halo or an enlarged flame; this
temperature measuring device. After any adjustment, repeat the is not a flash and should be ignored.
test in 10.2 or 10.3 using a fresh test specimen, with special 11.7 Record the test result as flash (or no flash) and the test
attention to the procedural details prescribed in the test method. temperature.
METHOD A—FLASH/NO FLASH TEST 11.8 Turn off the pilot and test flames (if used). Remove the
test specimen and clean the test cup and cover. It may be
11. Procedure necessary to allow the test cup temperature to fall to a safe
11.1 For specification purposes carry out a flash/no flash test level before cleaning.
at a temperature (actual) that allows for a correction due to the
ambient atmospheric pressure at the time of the test. Use the METHOD B—FLASH POINT DETERMINATION
following equations to convert a specification flash point test
requirement to the actual test temperature required for the test 12. Procedure
and then round to the nearest 0.5 °C (1 °F). 12.1 This procedure repeats the procedures of Method A
Actual test temperature, °C 5 S c 2 0.25~ 101.3 2 A ! (1) (11.3 through 11.8) a number of times. Each test uses a fresh
Actual test temperature, °C 5 S c 2 0.03~ 760 2 B ! (2)
test specimen and a different temperature. The change of
temperature allows the determination of two temperatures 1 °C
Actual test temperature, °F 5 S f 2 0.06~ 760 2 B ! (3) (2 °F) or 0.5 °C (1 °F) apart for which the lower temperature
where: did not result in a flash while the higher temperature resulted in
Sc = specification, or uncorrected target test temperature, °C, a flash (the flash point).
Sf = specification, or uncorrected target test temperature, °F, 12.1.1 Select the expected flash point of the sample as the
B = ambient barometric pressure, mm Hg, and initial test temperature and follow the procedure 11.3 to 11.8.
A = ambient barometric pressure, kPa. 12.1.2 If a flash is detected, repeat the procedure given in
11.2 Inspect the test cup and cover for cleanliness and 11.3 to 11.8 testing a fresh specimen at a temperature 5 °C
correct operation, especially with regard to tightness of the (9 °F) lower each time until no flash is detected.
cover (A1.2.1), the action of the shutter, the size or intensity of 12.1.2.1 Proceed to 12.1.4.
the ignition source and the position of the ignition source 12.1.3 When no flash was detected, repeat the procedure
(A1.3). Clean if necessary (9.3). Put the cover in place and given in 11.3 to 11.8 testing a fresh specimen at a temperature
close securely. 5 °C (9 °F) higher each time until a flash is detected.
11.3 Follow the manufacturer’s instructions to set the test 12.1.4 Having established a flash within two temperatures
temperature and the test time, and select the test specimen 5 °C (9 °F) apart, repeat the procedure at 1 °C (2 °F) intervals
volume in accordance with Table 1. from the lower of the two temperatures until a flash is detected.
12.1.5 Record the temperature of the test when this flash
11.4 When the test cup is at the test temperature, fill the occurs as the flash point, allowing for any known thermometer
appropriate syringe (A1.5, A1.6) with the sample to be tested; correction.
transfer the syringe to the filling orifice, taking care not to lose 12.1.6 The flash point determined in 12.1.4 will be to the
any sample; discharge the test specimen into the test cup by nearest 1 °C (2 °F).
fully depressing the syringe plunger; remove the syringe.
12.1.6.1 If improved accuracy is desired (that is, to the
11.5 Start the test timer; light the pilot light and adjust the nearest 0.5 °C (1 °F)) test a fresh test specimen at a tempera-
test flame (if used) to conform to the 4 mm (5⁄32 in.) gauge. ture 0.5 °C (1 °F) below that at which the flash was detected in
11.6 When the end of the test time is indicated, apply the 12.1.4. If no flash is detected, the temperature recorded in
ignition source by slowly and uniformly opening the shutter 12.1.4 is the flash point to the nearest 0.5 °C (1 °F). If a flash
and closing it completely over a period of 21⁄2 s. Watch closely is detected at the lower temperature (12.1.6), record this latter
for a flash at the test cup openings if a flash detector is not used. temperature as the flash point.
11.6.1 The test specimen is deemed to have flashed when a 12.1.7 Turn off the pilot and test flames, if used. When the
large flame appears and instantaneously propagates itself over cup temperature falls to a safe level, remove the test specimen
the surface of the test specimen (see 3.1.2). Occasionally, and clean the cup and cover.
particularly near the actual flash point, application of a gas
13. Calculation
TABLE 1 Test Conditions 13.1 Method A—No further calculations are required as the
Test Specimen Test
effects of barometric pressure were corrected for in Eq 1-3 in
Sample 11.1.
Temperatures Volume Time
All except # 100 °C 2 mL 1 min 13.1.1 If the effects of barometric pressure were not cor-
biodiesel (212 °F) rected before the flash/no flash test, Eq 4-6 shall be used to
All except > 100 °C 4 mL 2 min
biodiesel (212 °F) calculate the corrected test temperature.
Biodiesel # 300 °C 2 mL 1 min
Corrected ~ specification! test temperature ~ °C ! 5 C10.25~ 101.3 2 A !
(572 °F)
(4)

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG :HG-DQ*07


4
'RZQORDGHGSULQWHGE\
PRKDPDGZDKLGLQ $PVSHF//& SXUVXDQWWR/LFHQVH$JUHHPHQW1RIXUWKHUUHSURGXFWLRQVDXWKRUL]HG
D3828 − 16a (2021)
Corrected ~ specification! test temperature ~ °F ! 5 F10.06~ 760 2 B ! under constant operating conditions on identical test material,
(5) would, in the long run, in the normal and correct operation of
Corrected ~ specification! test temperature ~ °C ! 5 C10.03~ 760 2 B ! this test method, exceed the following values only in 1 case in
20. For examples of precision, see Table 2; valid range 20 °C
(6)
to 210 °C.
where: r 5 0.01520~ x 1 110! °C (10)
C = actual test temperature, °C,
F = actual test temperature, °F, where:
A = ambient barometric pressure, kPa, and x = the mean of two results.
B = ambient barometric pressure, mm Hg.
15.1.2 Reproducibility—The difference between two single
13.2 Method B—If the ambient barometric pressure (9.5) and independent results obtained by different operators work-
differs from 101.3 kPa (760 mm Hg) correct the flash point as ing in different laboratories using different apparatus on iden-
follows: tical test material, would, in the long run, in the normal and
Corrected flash point ~ °C ! 5 C10.25~ 101.3 2 A ! (7) correct operation of this test method, exceed the following
Corrected flash point ~ °F ! 5 F10.06~ 760 2 B ! (8) values only in 1 case in 20. For examples of precision, see
Table 2; valid range 20 °C to 210 °C.
Corrected flash point ~ °C ! 5 C10.03~ 760 2 B ! (9)
R 5 0.02561~ x 1 110! °C (11)
where:
C = detected flash point, °C, where:
F = detected flash point, °F, x = the mean of two results.
A = ambient barometric pressure, kPa, and
B = ambient barometric pressure, mm Hg. 15.2 Bias—The procedure in this test method has no bias
because flash point can be defined only in terms of a test
14. Report method.
14.1 Method A (flash/no flash), report flash (or no flash) at 15.2.1 Relative Bias—A relative bias assessment5 was car-
the specification (corrected) temperature (report temperature) ried out in accordance with Practice D6708 methodology
rounded to the nearest 0.5 °C (1 °F), and that Method A was between instruments using gas or electric ignitors. The statis-
used. tical evaluation outcome did show a relative bias. The preci-
sion as reported in 15.1.1 and 15.1.2 represents a combination
14.2 Method B (flash point determination), report the cor-
of gas and electric ignitors. In any case of dispute, the use of
rected flash point rounded to the nearest 0.5 °C (1 °F), and that
gas ignition shall be considered the referee.
Method B was used.
14.3 Report the identification of the material tested, the test 15.3 Precision ILS—The precision data as shown in 15.1.1
date and any deviation, by agreement or not, from the and 15.1.2 were developed from a 2010 joint Energy Institute
procedures specified. and ASTM interlaboratory study. Nineteen (19) laboratories
(11 gas and 8 electric ignitors) tested 15 samples in duplicate
15. Precision and Bias5 covering a wide range of petroleum and related products with
15.1 Precision—The precision for Procedure B of this test a flash point temperature range of 20 °C to 210 °C. Full details
method for petroleum and related products as determined by of the study are given in the research report.5
statistical examination of interlaboratory results is given in NOTE 2—The three technical bodies, ASTM D02.08.B0 TG D3828
15.1.1, 15.1.2, and Table 2. See Annex A3 for precision of fatty Revision, EI SC-B-4 Flammability, and ISO TC28 WG9 JWG Flash Point
acid methyl esters (FAME). Test Methods, involved in the revision of D3828, IP 523, and EN ISO
15.1.1 Repeatability—The difference between the two test 3679, respectively, were all presented with the ILS Research Report and
results, obtained by the same operator with the same apparatus results of the ILS, and all three bodies agreed that a combination of gas
and electric data should be used for the precision used in the test methods.

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

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG :HG-DQ*07


5
'RZQORDGHGSULQWHGE\
PRKDPDGZDKLGLQ $PVSHF//& SXUVXDQWWR/LFHQVH$JUHHPHQW1RIXUWKHUUHSURGXFWLRQVDXWKRUL]HG
D3828 − 16a (2021)
ANNEXES

(Mandatory Information)

A1. FLASH TEST APPARATUS

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.

NOTE 1—All dimensions are in millimetres.


FIG. A1.1 Test Cup and Cover Assembly

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG :HG-DQ*07


6
'RZQORDGHGSULQWHGE\
PRKDPDGZDKLGLQ $PVSHF//& SXUVXDQWWR/LFHQVH$JUHHPHQW1RIXUWKHUUHSURGXFWLRQVDXWKRUL]HG
D3828 − 16a (2021)
TABLE A1.1 Essential Dimensions of Flash Test ApparatusA,B These flames may be fueled from an external butane or propane
mm supply6 or from a self-contained or attached tank of butane or
Specimen Block: propane. (Warning—Never recharge or change the self-
Block diameter 61.5–62.5
Specimen well diameter 49.40–49.70
contained gas tank at elevated temperatures, or with the pilot or
Specimen well depth 9.70–10.00 test flames lighted, nor in the vicinity of other flames.) A gauge
Top of block to center of thermometer hole 16.00–17.00 ring 4 mm (5⁄32 in.) in diameter, engraved on the cover near the
Diameter of thermometer hole 7.00 approx
Cover:
test flame, aids uniformity in the size of the test flame. An
Large opening length 12.42–12.47 electric ignitor together with a suitable dipping mechanism and
Large opening width 10.13–10.18 cover (A1.10) is also permitted, however the precision and
Small opening length 5.05–5.10
Small opening width 7.60–7.65
degree of agreement with the gas flame ignitor have not yet
Distance between extreme edges of small openings 48.37–48.42 been determined. The electric ignitor shall be of the electric
Filling orifice diameter 4.00–4.50 resistance (hot wire) type and shall position the heated section
Bore of filler tube 1.80–1.85
Maximum distance of filler tube from base of well with 0.75 max
horizontally and intersect the underside of the cover. Follow
cover closed the manufacturer’s instructions for ensuring the correct opera-
Shutter: tion of the ignitor. In the event of a dispute the gas ignition
Large opening length 12.42–12.47
Large opening width 10.13–10.18 source is the referee.
Small opening length 5.05–5.10
Small opening width 7.60–7.65 A1.4 Audible Signal, indicates for the operator to dip the
Near edge of large opening to end of shutter 12.80–12.85 ignition source into the cup.
Extremes of large and small openings 30.40–30.45
Jet:
Length of jet 18.30–18.40
A1.5 Syringe, equipped with a nozzle suitable for use with
External diameter of end of jet 2.20–2.60 the apparatus, adjusted to deliver 2.00 mL 6 0.05 mL. It is
Bore of jet 1.60–1.65 permissible to use this syringe twice to enable a 4 mL specimen
Height of jet center above top surface of cover 11.00–11.20
Jet pivot to center of block with cover closed 12.68–12.72
to be used.
A
The O-ring seal or gasket, which provides a seal when the cover is shut, must be A1.6 Syringe, equipped with a nozzle suitable for use with
made of a heat-resistant material capable of withstanding the test temperatures
and the materials being tested. the apparatus, adjusted to deliver 4.0 mL 6 0.1 mL.
B
When in position the temperature measuring device must be in good thermal
contact with the test cup block. A1.7 Flash Detector (optional), a low mass thermocouple
device for the detection of the flash point. A flash is indicated
if a temperature rise of 6.0 °C (10.0 °F) is detected within
A1.2.2 Electrical heaters are attached to the test cup in a 100 ms.
manner that provides efficient transfer of heat. The heater
control shall be capable of controlling the test cup temperature, A1.8 Timing Device—An electronic timer.
as measured by the temperature measuring device and in a
A1.9 Temperature Measuring Device—A liquid in glass
draft-free area, to within 60.5 °C (61.0 °F) for test tempera-
thermometer or an electronic temperature measuring device
tures up to 100 °C, and 62.0 °C (64.0 °F) for test tempera-
with an accuracy of better than 0.5 °C (1 °F) up to 100.0 °C,
tures above 100 °C during the test, Cooling of the test cup may
and 2.0 °C (4 °F) at higher temperatures respectively.
use Peltier effect devices, an external cryostat or a cooling
insert (see Annex A4). A1.10 Electric Ignitor Screen—A metal screen to optically
screen the ignitor from the operator. Only required when an
A1.3 Test Flame and Pilot Flame, for dipping into the test
electric ignitor is used.
cup to test for a flash, and a pilot flame, to maintain the test
flame, are required. When inserted, the nozzle of the ignition
source shall intersect the plane of the underside of the cover. 6
External fuel adapters are available from instrument sources.

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG :HG-DQ*07


7
'RZQORDGHGSULQWHGE\
PRKDPDGZDKLGLQ $PVSHF//& SXUVXDQWWR/LFHQVH$JUHHPHQW1RIXUWKHUUHSURGXFWLRQVDXWKRUL]HG
D3828 − 16a (2021)

A2. VERIFICATION OF APPARATUS PERFORMANCE

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. PRECISION FOR FATTY ACID METHYL ESTERS (FAME)

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

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG :HG-DQ*07


8
'RZQORDGHGSULQWHGE\
PRKDPDGZDKLGLQ $PVSHF//& SXUVXDQWWR/LFHQVH$JUHHPHQW1RIXUWKHUUHSURGXFWLRQVDXWKRUL]HG
D3828 − 16a (2021)
A3.2 Equivalence apparatus under constant operating conditions on identical test
A3.2.1 EN ISO 3679 (IP 523) and the associated flash material, would, in the long run, in the normal and correct
no-flash method EN ISO 3680 (IP 524) are technically equiva- operation of this test method, exceed the values shown in Table
lent to Test Methods D3828 and use the same procedure, 2 only in one case in twenty.
apparatus, and precision. Repeatability = 1.9 °C
A3.3.1.2 Reproducibility—The difference between two
A3.3 Precision and Bias9 single and independent results obtained by different operators
A3.3.1 Precision—The precision of this test method, as working in different laboratories on identical test material,
determined by statistical examination of interlaboratory results would, in the long run, in the normal and correct operation of
is as follows: this test method, exceed the values shown in Table 2 only in
A3.3.1.1 Repeatability—The difference between the two one case in twenty.
test results, obtained by the same operator with the same Reproducibility = 15 °C
A3.3.2 Bias—The procedure in this test method has no bias,
9
Supporting data available from CEN as CEN/TR 15160. European Committee because flash point can be defined only in terms of a test
for Standardization (CEN), 36 Rue de Stassart, B1050, Brussels, Belgium. method.

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. TEMPERATURE MEASURING DEVICE SPECIFICATION

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.

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG :HG-DQ*07


9
'RZQORDGHGSULQWHGE\
PRKDPDGZDKLGLQ $PVSHF//& SXUVXDQWWR/LFHQVH$JUHHPHQW1RIXUWKHUUHSURGXFWLRQVDXWKRUL]HG
D3828 − 16a (2021)
A5.3 Liquid-in-Glass Thermometers
A5.3.1 See Table A5.1.

TABLE A5.1 Liquid-in-Glass Thermometer Specification


Type Sub-Zero Low Range High Range
Temperature range, °C -30 to 100 0 to 110 100 to 300
Immersion, mm 44 44 44
Scale marks, °C
Subdivisions 1 1 2
Long lines at each 5 5 10
Numbers at each 10 10 10
Maximum line width, mm 0.15 0.15 0.15
Scale error, °C, max 0.5 0.5 2.0
Expansion chamber Required Required Required
Total length, mm 195 to 200 195 to 200 195 to 200
Stem outer diameter, mm 6 to 7 6 to 7 6 to 7
Bulb length, mm 10 to 14 10 to 14 10 to 14
Bulb outer diameter, mm 4 to 6 4 to 6 4 to 6
Scale Location:
Bottom of bulb to line at, °C -30 0 100
Distance, mm 57 to 61 48 to 52 48 to 52
Length of scale range, mm 115 to 135 115 to 135 115 to 135

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG :HG-DQ*07


10
'RZQORDGHGSULQWHGE\
PRKDPDGZDKLGLQ $PVSHF//& SXUVXDQWWR/LFHQVH$JUHHPHQW1RIXUWKHUUHSURGXFWLRQVDXWKRUL]HG

You might also like

pFad - Phonifier reborn

Pfad - The Proxy pFad of © 2024 Garber Painting. All rights reserved.

Note: This service is not intended for secure transactions such as banking, social media, email, or purchasing. Use at your own risk. We assume no liability whatsoever for broken pages.


Alternative Proxies:

Alternative Proxy

pFad Proxy

pFad v3 Proxy

pFad v4 Proxy