Thermal Oxidation Stability of Aviation Turbine Fuels: Standard Test Method For

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: D3241 − 23a´1
Designation 323/21
Standard Test Method for

Thermal Oxidation Stability of Aviation Turbine Fuels1,2
This standard is issued under the fixed designation D3241; 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.
ε1 NOTE—Editorially updated A4.11 in January 2024.
1. Scope* mendations issued by the World Trade Organization Technical

1.1 This test method covers the procedure for rating the Barriers to Trade (TBT) Committee.
tendencies of gas turbine fuels to deposit decomposition 2. Referenced Documents
products within the fuel system.
2.1 ASTM Standards:3
1.2 The differential pressure values in mm Hg are defined D1655 Specification for Aviation Turbine Fuels
only in terms of this test method. D4057 Practice for Manual Sampling of Petroleum and
1.3 The deposition values stated in SI units shall be re- Petroleum Products
garded as the referee value. D4306 Practice for Aviation Fuel Sample Containers for
Tests Affected by Trace Contamination
1.4 The pressure values stated in SI units are to be regarded E177 Practice for Use of the Terms Precision and Bias in
as standard. The psi comparison is included for operational ASTM Test Methods
safety with certain older instruments that cannot report pres- E691 Practice for Conducting an Interlaboratory Study to
sure in SI units. Determine the Precision of a Test Method
1.5 No other units of measurement are included in this 2.2 ISO Standards:4
standard. ISO 3274 Geometrical Product Specifications (GPS)—
1.6 This standard does not purport to address all of the Surface texture: Profile method—Nominal characteristics
safety concerns, if any, associated with its use. It is the of contact (stylus) instruments
responsibility of the user of this standard to establish appro- ISO 4288 Geometrical Product Specifications (GPS)—
priate safety, health, and environmental practices and deter- Surface texture: Profile method—Rules and procedures
mine the applicability of regulatory limitations prior to use. for the assessment of surface texture
For specific warning statements, see 6.1.1, 7.1, 7.3, 12.1.1, and 2.3 ASTM Adjuncts:5
Annex A6. Color Standard for Heater Tube Deposit Rating
1.7 This international standard was developed in accor-
3. Terminology
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the 3.1 Definitions of Terms Specific to This Standard:
Development of International Standards, Guides and Recom- 3.1.1 deposits, n—oxidative products laid down on the test
area of the heater tube or caught in the test filter, or both.
3.1.1.1 Discussion—Fuel deposits will tend to predominate
1
at the hottest portion of the heater tube, which is between the
This test method is under the jurisdiction of ASTM International Committee
D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct 30 mm and 50 mm position.
responsibility of Subcommittee D02.J0.03 on Combustion and Thermal Properties.
The technically equivalent standard as referenced is under the jurisdiction of the
3
Energy Institute Subcommittee SC-B-8. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Oct. 1, 2023. Published October 2023. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1973. Last previous edition approved in 2023 as D3241 – 23. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D3241-23AE01. the ASTM website.
2 4
This test method has been developed through the cooperative effort between Available from International Organization for Standardization (ISO), 1, ch. de
ASTM and the Energy Institute, London. ASTM and IP standards were approved by la Voie-Creuse, CP 56, CH-1211 Geneva 20, Switzerland, http://www.iso.org.
5
ASTM and EI technical committees as being technically equivalent but that does not Available from ASTM International Headquarters. Order Adjunct No.
imply both standards are identical. ADJD3241. Original adjunct produced in 1986.
*A Summary of Changes section appears at the end of this standard

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

1
'RZQORDGHGSULQWHGE\
8QLYHUVLGDG,QGXVWULDOGH6DQWDQGHUSXUVXDQWWR/LFHQVH$JUHHPHQW1RIXUWKHUUHSURGXFWLRQVDXWKRUL]HG
D3241 − 23a´1
3.1.2 heater tube, n—an aluminum coupon controlled at 6.1.1 Portions of this test may be automated. Refer to the
elevated temperature, over which the test fuel is pumped. appropriate user manual for the instrument model to be used
3.1.2.1 Discussion—The heater tube is resistively heated for a description of detailed procedure. A manual is provided
and controlled in temperature by a thermocouple positioned with each test rig. (Warning—No attempt should be made to
inside. The critical test area is the thinner portion, 60 mm in operate the instrument without first becoming acquainted with
length, between the shoulders of the heater tube. Fuel inlet to all components and the function of each.)
the heater tube is at the 0 mm position, and fuel exit is at 6.1.2 Certain operational parameters used with the instru-
60 mm. ment are critically important to achieve consistent and correct
3.2 Abbreviations: results. These are listed in Table 2.
3.2.1 ∆P—differential pressure. 6.2 Heater Tube Deposit Rating Apparatus:
6.2.1 Visual Heater Tube Rater (VTR), the tuberator de-
4. Summary of Test Method scribed in Annex A1.
4.1 This test method for measuring the high temperature 6.2.2 Standardization of Metrology Requirements:
stability of gas turbine fuels uses an instrument that subjects 6.2.2.1 Number of Measured Points—1200 in the ratable
the test fuel to conditions that can be related to those occurring area of the heater tube (between 5 mm and 55 mm above the
in gas turbine engine fuel systems. The fuel is pumped at a bottom shoulder of the heater tube).
fixed volumetric flow rate through a heater, after which it (1) Circumferential Resolution—(number of points mea-
enters a precision stainless steel filter where fuel degradation sured on the heater tube circumference), 24 points equally
products may become trapped. spaced.
4.1.1 The apparatus uses 450 mL of test fuel ideally during (2) Longitudinal Resolution—(number of points measured
a 2.5 h test. The essential data derived are the amount of on the 50 mm ratable length of the heater tube), 50 points
deposits on a heater tube, and the rate of plugging of a 17 µm equally spaced.
nominal porosity precision filter located just downstream of the 6.2.2.2 Standard Spot—Thickest average deposit area de-
heater tube. scribed by either a 2×3 or 3×2 (longitudinal × circumferential)
arrangement of adjoining thickness measurement points,
5. Significance and Use amongst the 1200 measured by the metrology techniques.
5.1 The test results are indicative of fuel performance 6.2.3 Interferometric (Heater) Tube Rater (ITR)—the tu-
during gas turbine operation and can be used to assess the level berator described in Annex A2.
of deposits that form when liquid fuel contacts a heated surface 6.2.4 Ellipsometric (Heater) Tube Rater (ETR)—the tubera-
that is at a specified temperature. tor described in Annex A3.
6.2.5 Multi-Wavelength Ellipsometric (Heater) Tube Rater
6. Apparatus (MWETR)—the tuberator described in Annex A4.
6.1 Aviation Fuel Thermal Oxidation Stability Tester6— 6.3 Because jet fuel thermal oxidation stability is defined
Five models of suitable equipment may be used as indicated in only in terms of this test method, which depends upon, and is
Table 1. inseparable from, the specific equipment used, the test method
shall be conducted with the equipment used to develop the test
method or equivalent equipment.
7. Reagents and Materials
6
The following equipment, as described in Table 1 and RR:D02-1309, was used
to develop this test method. The following equipment, as described in Table 1 and 7.1 Use methyl pentane, 2,2,4-trimethylpentane, or
determined as equivalent in testing as detailed in RR:D02-1631, is provided by PAC, n-heptane as a general cleaning solvent. General cleaning
8824 Fallbrook Drive, Houston, TX 77064. The following equipment, as described solvent shall be 95 mol % purity, minimum. This solvent will
in Table 1 and determined as equivalent in testing as detailed in RR:D02-1728, is
provided by Falex Corporation, 1020 Airpark Dr., Sugar Grove, IL, 60554-9585. effectively clean internal metal surfaces of apparatus before a
This is not an endorsement or certification by ASTM International.
TABLE 1 Instrument Models

Instrument Model Pressurize With Principle Differential Pressure by
230A hydraulic syringe Transducer + Printout
240A hydraulic syringe Transducer + Printout
230 Mk IIIB hydraulic dual piston (HPLC Type) Transducer + Printout
F400C hydraulic dual piston (HPLC Type) Transducer + Printout
230 Mk IVD, E hydraulic single piston (HPLC Type) Transducer + Printout
A
See RR:D02-1309.
B
See RR:D02-1631.
C
See RR:D02-1728.
D
See RR:D02-1757.
E
There are two versions of the 230 Mk IV instrument; one with an inline internal non-consumable filter located upstream of the 0.45 µm pre-filter and one without. Only
the 230 Mk IV instruments without the inline internal non-consumable filter were included in RR:D02-1757 and have been determined by ASTM Committee D02 to be
equivalent to the other apparatus listed above in Table 1. There are no external markings on the instruments to indicate which apparatus contains the inline internal
non-consumable filter. Contact the manufacturer for further information on removal of the inline internal non-consumable filter.

2
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
TABLE 2 Critical Operating Characteristics of D3241
Item Definition
Test apparatus Tube-in-shell heat exchanger as illustrated in Fig. 1 and dimen-
sions in Fig. A5.1.
Heater Tube:
Heater tube A, B, C, D, E Specially fabricated heater tube that produces controlled heated
test surface; new one for each test.
Heater Tube identificationE Each heater tube shall be physically identified with a unique serial
number, identifying the manufacturer and providing traceability to
the original material batch.
Heater Tube metallurgy 6061-T6 Aluminum, plus the following criteria

a) The Mg:Si ratio shall not exceed 1.9:1
b) The Mg2Si percentage shall not exceed
1.85 %
Heater Tube surface polish over circumference of center section Rotational cut buffing technique with polishing compound to
achieve mechanical surface finish.
Heater Tube dimensions: Dimension Tolerance

Heater Tube length,F mm 161.925 ±0.254
Center section length, mm 60.325 ±0.051
Outside diameters, mm
Shoulders 4.724 ±0.025
Center section 3.175 ±0.051
Inside diameter, mm 1.651 ±0.051
Total indicator runout, mm, max 0.013
Mechanical surface finish, nm, over circumference in center 50 ± 20
section in accordance with ISO 3274 and ISO 4288 using the
mean of four 1.25–measurements
Test filter 6 nominal 17 µm stainless steel mesh filter element to trap deposits;
new one for each test
Stainless Steel Mesh Twilled Dutch Weave, 304 Stainless Steel, 165 × 1400 Mesh (tol-
erance; 4 % on 1400 and 2 % on 165) with Warp Diameter =
0.0028 in. and Shute Diameter = 0.0016 in.
Instrument parameters:
Sample volume 600 mL of sample is aerated, then 450 mL ± 45 mL of this aerated
fuel shall be pumped during the heating phase for a valid test
Aeration rate 1.5 L ⁄min dry air through sparger
Flow during test 3.0 mL ⁄min ± 10 % (2.7 mL/min minimum to 3.3 mL/min maxi-
mum)
Pump mechanism positive displacement or piston syringe
Cooling bus bars fluid cooled to maintain consistent tube temperature pro-
file
Thermocouple (TC) Type J, Inconel sheathed, or Type K, Inconel sheathed
Operating pressure:
System 3.45 MPa ± 10 % on sample by hydraulically transmitted force
against control valve outlet restriction
At test filter differential pressure (∆P) measured across test filter by electronic
transducer in mm Hg
Operating temperature:
For test as stated in specification for fuel
Uniformity of run maximum deviation of ±2 °C from specified temperature
Calibration Models 230 and 240 – Three point calibration including tin (see
7.5) at 232 °C, lead (see 7.4) at 327 °C for high point and ice +
water for low point reference
All other models – Two point calibration using pure lead at 327 °C
for high point and ice + water for low point reference
A
D3241/IP 323 Thermal Stability is a critical aviation fuel test, the results of which are used to assess the suitability of jet fuel for aviation operational safety and regulatory
compliance. The integrity of D3241/IP 323 testing requires that heater tubes meet the regulations of D3241 Table 2 and give equivalent D3241 results to the heater tubes
supplied by the original equipment manufacturer (OEM).
B
The following equipment, heater tubes, manufactured by PAC, 8824 Fallbrook Drive, Houston, TX 77064, was used in the development of this test method. This is not
an endorsement or certification by ASTM International.
C
A test protocol to establish equivalence of heater tubes is on file at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1550.
D
The following equipment, heater tube and filter kits, manufactured by Falex Corporation, 1020 Airpark Dr., Sugar Grove, IL, 60554-9585, was run through the test
protocol in RR:D02-1550 and determined as equivalent to the equipment used to develop the test method. This test is detailed in RR:D02-1714. This is not an endorsement
or certification by ASTM International.
E
An electronic recording device, such as a radio-frequency identification device (RFID), may be embedded into the heater tube rivet located at the bottom of the heater
tube. Tube identification data may be stored on an electronic recording device, such as a RFID, embedded into the heater tube.
F
Tube length measurements are only applicable to the aluminum portion of the heater tube. Additions, such as an RFID, do not contribute to the length measurement of
the heater tube.

3
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
9.1.1 Fuel Quantity, 450 mL minimum for test plus about
50 mL for system.
9.1.2 Fuel Pre-Treatment—Filter the fuel through a single
layer of “qualitative” quality, medium-flow, cellulose filter
paper. Filter should be a pleated (folded) circular shape and
fitted into a conical funnel to filter fuel. Filter paper grades 2V,
MN514, or better, are recommended. After filtration, aerate the
fuel for 6 min at 1.5 L ⁄min air flow rate for a maximum of
1000 mL sample using a coarse 12 mm borosilicate glass gas
dispersion tube.
9.1.3 Fuel System Pressure, 3.45 MPa (500 psi) 610 %
gauge.
FIG. 1 Standard Heater Tube Test Section, Essential to All D3241 9.1.4 Thermocouple Position, at 39 mm.
Test Instruments 9.1.5 Fuel System Prefilter Element, filter paper of 0.45 µm
pore size.
test, especially those surfaces (before the heater tube test
9.1.6 Heater Tube Control Temperature, preset as specified
section) that contact fresh sample. (Warning—Extremely
in applicable specification.
flammable. Harmful if inhaled (see Annex A6).)
9.1.7 Fuel Flow Rate, 3.0 mL ⁄min 6 10 %.
7.2 Use a nylon bristle brush and trisolvent to clean internal 9.1.8 Minimum Fuel Pumped During Test, 405 mL.
(working) surface of heater tube test section only. Trisolvent is 9.1.9 Test Duration, 150 min 6 2 min.
an equal mix of acetone (1), toluene (2), and isopropanol (3). 9.1.10 Cooling Fluid Flow, approximately 39 L ⁄h, or center
All three components of trisolvent shall be 95 mol % purity, of green range on cooling fluid meter.
minimum. (Warning—(1) Extremely flammable, vapors may 9.1.11 Power Setting, internally set for computer models.
cause flash fire; (2) and (3) Flammable. Vapors of all three
harmful. Irritating to skin, eyes, and mucous membranes.) Use 10. Preparation of Apparatus
a nylon bristle brush that makes stiff contact with the inner
walls of the heater tube test section. 10.1 Cleaning and Assembly of Heater Tube Test Section:
10.1.1 Clean the inside surface of the heater tube test section
7.3 Use dry calcium sulfate + cobalt chloride granules (97 + using a nylon brush saturated with trisolvent to remove all
3 mix) or other self-indicating drying agent in the aeration deposits. Replace the nylon brush when it shows signs of wear
dryer. This granular material changes gradually from blue to (such as missing bristles) and no longer makes stiff contact
pink color indicating absorption of water. (Warning—Do not with inner walls of heater tube test section.
inhale dust or ingest. May cause stomach disorder.) 10.1.2 Check the heater tube to be used in the test for
7.4 Lead, 99.9 % minimum purity. surface defects and straightness by referring to the procedure in
7.5 Tin, 99.0 % minimum purity. A1.10. Be careful, also, to avoid scratching the heater tube
shoulder during the examination, since the heater tube shoulder
8. Sampling must be smooth to ensure a seal under the flow conditions of
8.1 General Requirements—The choice of construction ma- the test.
terials is an important factor, particularly in the case of aviation 10.1.3 Assemble the heater tube test section using new
turbine fuel, where thermal stability can be degraded by the items: (1) visually checked heater tube, (2) test filter, and (3)
presence of very low concentration of copper. The use of three O-rings. Inspect insulators to be sure they are undam-
copper or copper alloys shall be eliminated wherever possible aged.
by the use of alternative materials such as stainless steel or NOTE 1—Heater tubes must not be reused. Tests indicate that magne-
aluminum. Zinc and cadmium are two other metals that sium migrates to the heater tube surface under normal test conditions.
adversely affect product quality. Copper, copper alloys (such as Surface magnesium may reduce adhesion of deposits to reused heater
brass), zinc-rich (galvanized) coatings, cadmium alloys, and tube.
cadmium plating shall not be used in sampling aviation fuels 10.1.4 During assembly of the heater tube test section,
for evaluation under this test method. handle the heater tube carefully so as not to touch center part
8.1.1 Sampling Containers—Sampling containers shall be of heater tube. IF THE CENTER OF HEATER TUBE IS
in accordance with the requirements for thermal stability TOUCHED, REJECT THE HEATER TUBE SINCE THE
testing described in Practice D4306. CONTAMINATED SURFACE MAY AFFECT THE
8.1.2 Sampling Equipment—Sampling equipment fabricated DEPOSIT-FORMING CHARACTERISTICS OF THE
from copper or its alloys shall not be used for sampling in HEATER TUBE.
accordance with this test method. Sampling equipment shall be 10.2 Cleaning and Assembly of Remainder of Test Compo-
in accordance with the requirements for aviation fuel described nents:
in Practice D4057.
10.2.1 Perform the following steps in the order shown prior
9. Standard Operating Conditions to running a subsequent test.
9.1 Standard conditions of the test method are as follows: NOTE 2—It is assumed that the apparatus has been disassembled from

4
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
previous test (see Annex A5 or appropriate user manual for assembly/ 12.4.2 Some instrument models may do the following steps
disassembly details). automatically, but verify that:
10.2.2 Inspect and clean components that contact test 12.4.2.1 No more than 1 h maximum elapses from aeration
sample and replace any seals that are faulty or suspect. to start of heating.
10.2.3 Install the prepared heater tube test section (as 12.4.2.2 The test filter bypass valve is closed as soon as the
described in 10.1.1 – 10.1.4). heater tube temperature reaches the test level, so fuel flows
10.2.4 Assemble pre-filter with new element and install. through the test filter (see A5.2.6).
10.2.5 Check thermocouple for correct reference position, 12.4.2.3 DP transducer is set to zero once DP stabilizes (see
then lower into standard operating position. A5.2.6).
10.2.6 On Models 230 and 240, make sure the water beaker 12.4.3 Check fuel flow rate against Standard Operating
is empty. Conditions by timing flow or counting the drip rate during first
15 min of test. (See X1.5.)
11. Calibration and Standardization Procedure
NOTE 6—When counting drop rate, the first drop is counted as drop 0,
11.1 Perform checks of key components at the frequency and time is started. As drop 20 falls, total time is noted.
indicated in the following (see Annexes or user manual for
12.5 Test:
details).
11.1.1 Thermocouple—Calibrate a thermocouple when first 12.5.1 Record filter pressure drop every 30 min minimum
installed and then at least every 6 months (see A5.2.8). during the test period.
11.1.2 Differential Pressure Cell—Standardize once a year 12.5.2 If the filter pressure drop begins to rise sharply and it
or when installing a new cell (see A5.2.6). is desired to run a full 150 min test, a bypass valve common to
11.1.3 Aeration Dryer—Check at least monthly and change all models must be opened in order to finish the test. See
if color indicates significant absorption of water (see 7.3). appropriate User Manual for details on operation of the bypass
11.1.4 Metering Pump—Perform two checks of flow rate for system (see A5.2.2).
each test as described in Section 12. 12.5.3 Make another flow check within final 15 min before
shutdown (see 12.4.3 and accompanying note). (See X1.5.)
12. Procedure 12.6 Heater Tube Profile—If a heater tube temperature
12.1 Preparation of Fuel Test Sample: profile is desired, obtain as described in X1.4.
12.1.1 Filter and aerate sample using standard operating 12.7 Shutdown:
conditions (see A5.2.9). (Warning—All jet fuels must be 12.7.1 Shut down the instrument; some models may do this
considered flammable except JP5 and JP7. Vapors are harmful automatically.
(see A6.3, A6.6, and A6.7).) 12.7.1.1 For applicable models after shutdown, turn FLOW
NOTE 3—Before operating, see Warning in 6.1.1. SELECTOR VALVE to VENT to relieve pressure.
NOTE 4—Test method results are known to be sensitive to trace 12.7.1.2 For Models 230 and 240, the piston actuator will
contamination from sampling containers. For recommended containers, retreat automatically.
refer to Practice D4306.
12.7.1.3 Measure the amount of spent fluid pumped during
12.1.2 Maintain temperature of sample between 15 °C and the test.
32 °C during aeration. (1) For the Models 230 and 240, measure effluent water in
12.1.3 Allow no more than 1 h to elapse between the end of drip receiver, then empty.
aeration and the start of the heating of the sample. (2) For other models, measure the fuel in the receipt
12.2 Final Assembly: container.
12.2.1 Check all lines to ensure tightness. 12.7.1.4 If the amount of water or fuel measured is less than
12.2.2 Recheck thermocouple position at 39 mm. 405 mL, the test shall be rejected.
12.2.3 Make sure drip receiver is empty. 12.8 Disassembly:
12.3 Power Up and Pressurization: 12.8.1 Disconnect fuel inlet line to the heater tube test
12.3.1 Turn POWER to ON. section.
12.3.2 Inspect the system for leaks. Depressurize the system 12.8.2 Disconnect the heater tube test section.
as necessary to tighten any leaking fittings. 12.8.2.1 Remove the heater tube from the heater tube test
12.3.3 Set controls to the standard operating conditions. section carefully so as to avoid touching the center part of
12.3.4 Use a heater tube control temperature as specified for heater tube, and discard the test filter.
the fuel being tested. Apply any thermocouple correction from 12.8.2.2 Flush the heater tube with recommended general
the most recent calibration (see A5.2.8). cleaning solvent (see 7.1) from top down. If the heater tube is
NOTE 5—The test can be run to a maximum tube temperature of about grasped from the top, do not wash solvent over gloves or bare
350 °C. The temperature at which the test should be run and the criteria for fingers. Allow to dry, return the heater tube to original
judging results are normally embodied in fuel specifications. container, mark with identification and hold for evaluation.
12.4 Start Up: 12.8.3 Disconnect and remove any containers.
12.4.1 Use procedure for each model as described in the 12.8.3.1 Discard water and fuel to waste disposal.
appropriate User Manual. 12.8.4 Disconnect gas dispersion tube (i.e., sparger).

5
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
12.8.4.1 Flush gas dispersion tube (i.e., sparger) with rec- NOTE 7—Either the heater tube rating or the ∆P criteria, or both, are
ommended general cleaning solvent (see 7.1). Allow solvent to used to determine whether a fuel sample passes or fails the test at a
specified test temperature.
fully dry before using the gas dispersion tube (i.e., sparger) for
another test. 14.1.5 Spent fuel at the end of a normal test (see 12.7.1.3).
14.1.6 Heater tube serial number may be reported.
13. Heater Tube Evaluation
13.1 Rate the deposits on heater tube in accordance with 15. Precision and Bias
Annex A1, Annex A2, Annex A3, or Annex A4 as directed by 15.1 An interlaboratory study of oxidative stability testing
the specification referencing this method and record data. was conducted in accordance with Practice E691 by eleven
13.1.1 When a specification allows multiple rating laboratories, using thirteen instruments including two models
techniques, the method providing deposit measurements in SI with five fuels at two temperatures for a total of ten materials.
units is preferred. Each laboratory obtained two results from each material.7
13.1.2 When the rating techniques do not agree, the method 15.1.1 The terms repeatability and reproducibility in this
providing measurements in SI units shall be regarded as the section are used as specified in Practice E177.
referee.
15.2 Precision—It is not possible to specify the precision of
13.2 Return the heater tube to original container and retain this test method because it has been determined that test
as appropriate. method results cannot be analyzed by standard statistical
14. Report methodology.
14.1 Report the following information: 15.3 Bias—This test method has no bias because jet fuel
14.1.1 The heater tube control temperature. This is the test thermal oxidative stability is defined only in terms of this test
temperature of the fuel. method.
14.1.2 Heater tube deposit rating(s).
16. Keywords
14.1.3 Maximum pressure drop across the filter during the
test or the time required to reach a pressure differential of 16.1 differential pressure; fuel decomposition; oxidative
25 mm Hg. deposits; heater tube deposits; thermal stability; turbine fuel
14.1.4 If the normal 150 min test time was not completed,
for example, if the test is terminated because of pressure drop 7
Supporting data have been filed at ASTM International Headquarters and may
failure, also report the test time that corresponds to this heater be obtained by requesting Research Report RR:D02-1309. Contact ASTM Customer
tube deposit rating. Service at service@astm.org.
ANNEXES
(Mandatory Information)
A1. TEST METHOD FOR VISUAL RATING OF HEATER TUBES
A1.1 Scope A1.3 Terminology

A1.1.1 This method covers a procedure for visually rating A1.3.1 abnormal—a heater tube deposit color that is neither
the heater tube produced by Test Method D3241. peacock nor like those of the Color Standard.
A1.3.1.1 Discussion—This refers to deposit colors such as
A1.1.2 The final result from this test method is a heater tube
blues and grays that do not match the Color Standard.
color rating based on an arbitrary scale established for this test
method plus two additional yes/no criteria that indicate the A1.3.2 peacock—A multicolor, rainbow-like heater tube
presence of an apparent large excess of deposit or an unusual deposit.
deposit, or both. A1.3.2.1 Discussion—This type of deposit is caused by
A1.1.3 This international standard was developed in accor- interference phenomena where deposit thickness exceeds the
dance with internationally recognized principles on standard- quarter wave length of visible light.
ization established in the Decision on Principles for the A1.3.3 Heater Tube Rating—A ten-step discrete scale from
Development of International Standards, Guides and Recom- 0 to >4 with intermediate levels for each number starting with
mendations issued by the World Trade Organization Technical 1 described as less than the subsequent number.
Barriers to Trade (TBT) Committee. A1.3.3.1 Discussion—The scale is taken from the five
colors—0, 1, 2, 3, 4—on the ASTM Color Standard. The
A1.2 Referenced Documents
complete scale is: 0, <1, 1, <2, 2, <3, 3,< 4, 4, >4. Each step is
A1.2.1 Adjunct:5 not necessarily of the same absolute magnitude. The higher the
Color Standard for Heater Tube Deposit Rating number, the darker the deposit rating.

6
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
A1.4 Summary of Test Method A1.9.2.4 Ignore spots, axial (that is, longitudinal) streaks, or
A1.4.1 This test method uses a specially constructed light scratches on a heater tube that are considered heater tube
box to view the heater tube. The heater tube is positioned in the defects. These will normally not be present, since the heater
box using a special heater tube holder. Uniformity of the new tube is examined before use to eliminate defective heater tubes.
heater tube surface is judged under the optimum light condi- A1.10 Pretest Rating of Heater Tubes
tions of the box. Color of the heater tube is judged under light
and magnification by comparing to the Color Standard plate A1.10.1 Examine the heater tube without magnification in
slid into optimum position immediately behind the heater tube. laboratory light. If a defect is visible, discard the heater tube.
Then examine the center (thinner area) of the heater tube
A1.5 Significance and Use between 5 mm and 55 mm above the bottom shoulder using the
Tuberator. If a defect is seen, establish its size. If it is larger
A1.5.1 The final heater tube rating is assumed to be an
than 2.5 mm2, discard the heater tube. Fig. A1.1 provides an
estimate of condition of the degraded fuel deposit on the heater
illustration of defect areas equivalent to 2.5 mm2.
tube. This rating is one basis for judging the thermal oxidative
stability of the fuel sample. A1.10.2 Examine the heater tube for straightness by rolling
the heater tube on a flat surface and noting the gap between the
A1.6 Apparatus flat surface and the center section. Reject any bent heater tube.
A1.6.1 Heater Tube Deposit Rating Apparatus—The colors A1.11 Procedure
of deposits on the heater tube are rated by using a tuberator and
the ASTM Color Standard. A1.11.1 Set Up:
A1.11.1.1 Snap the upper end of the heater tube into the
A1.7 Test Samples (Heater Tube) clamp of the holder for the heater tube.
A1.11.1.2 Push the heater tube against the stop of the holder
A1.7.1 Handle the heater tube carefully so as not to touch
for the heater tube.
the center portion at any time.
A1.11.1.3 Slide the holder with the heater tube over the
NOTE A1.1—Touching the center of the heater tube will likely contami- guide rod into the tuberator.
nate or disturb the surface of the heater tube, deposit, or both, which must A1.11.1.4 Rotate the holder and position the heater tube
be evaluated in pristine condition.
such that the side with the darkest deposit is visible.
A1.8 Standard Operating Conditions A1.11.1.5 Insert the ASTM Color Standard into the tubera-
tor.
A1.8.1 Inside of Light Box, opaque black.
A1.11.2 Evaluation:
A1.8.2 Light Source, three 30 W incandescent bulbs, clear, A1.11.2.1 On completion of the test, compare the darkest
reflective type; all shall be working for optimum viewing. heater tube deposit color, between 5 mm and 55 mm above the
A1.8.3 Bulb Positions, one above, two below, each directed bottom shoulder, with the ASTM Color Standard. Only rate a
toward heater tube holder and color standard.
A1.8.4 Magnification, 2×, covering viewing window.
A1.8.5 Evaluators—Use persons who can judge colors, that
is, they should not be color blind.
A1.9 Calibration and Standardization

A1.9.1 No standardization is required for this test apparatus,
but since the Color Standard is known to fade, store it in a dark
place.
NOTE A1.2—The lifetime of the Color Standard is not established when
continuously or intermittently exposed to light. It is good practice to keep
a separate Standard in dark (no light) storage for periodic comparison with
the Standard in regular use. When comparing, the optimum under the light
conditions are those of the heater tube rating box.
A1.9.2 Standardization of Rating Technique:
A1.9.2.1 In rating a heater tube, the darkest deposits are
most important. Estimate grades for the darkest uniform
deposit, not for the overall average color of the deposit area.
A1.9.2.2 When grading, consider only the darkest continu-
ous color that covers an area equal or larger than a circle of size
one-half the diameter of the heater tube.
A1.9.2.3 Ignore an axial (that is, longitudinal) deposit streak
that is less in width than one-quarter the diameter of the heater
tube regardless of the length of the streak. FIG. A1.1 Defect Areas

7
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
deposit if the area is greater than 2.5 mm2 and the width of any A1.12.1.2 If there are only P or A, or both, deposits, report
axial (that is, longitudinal) streak or spot is greater than only these and do not attempt to estimate a numerical grade.
0.8 mm. Fig. A1.1 provides an illustration of spots or axial A1.12.2 Examples:
streaks with an area equivalent to 2.5 mm2. A1.12.2.1 Example 1—A heater tube has a maximum de-
A1.11.2.2 When the darkest heater tube deposit color cor- posit falling between Color Standard Codes 2 and 3 with no
responds to a color standard, that number should be recorded. other colors present. The overall heater tube rating would be
A1.11.2.3 If the darkest heater tube deposit color being less than 3.
rated is in the obvious transition state between any two A1.12.2.2 Example 2—The darkest deposit on a heater tube
adjacent color standards, the rating should be recorded as less matches a Code 3, but there is also a peacock deposit present.
than the darker (that is, higher number) standard. The overall rating of the heater tube would be reported as 3P.
A1.11.2.4 In the event the heater tube has deposits which do A1.12.2.3 Example 3—A heater tube has a deposit that
not match the normal Color Standard colors, use the following matches Color Standard Code 1 and also has an abnormal
rules for rating. With reference to standard terms: deposit. The overall heater tube rating would be reported as
(1) If the heater tube deposit is peacock color, rate this as 1A.
Code P, but also rate any heater tube deposit that shows normal
deposit color; or A1.13 Precision and Bias
(2) If the heater tube deposit contains an abnormal color,
A1.13.1 Precision—The precision of the procedure in Test
rate this as Code A, but also rate any heater tube deposit that
Method D3241 for measuring heater tube deposit rating by this
shows normal deposit color.
method was evaluated by the subcommittee and is reported in
A1.11.3 Remove the rated heater tube and return to its RR:D02-1786.8
original container.
A1.13.2 Bias—The procedure in Test Method D3241 for
A1.12 Report determining heater tube deposit rating has no bias because the
A1.12.1 Report the numerical rating for the heater tube value of heater tube deposit rating is defined only in terms of
deposit plus A or P, or both, with additional description, if the test method.
applicable.
A1.12.1.1 When reporting the overall rating, report the 8
maximum rating, and, if there are colors present that do not be obtained by requesting Research Report RR:D02-1786. Contact ASTM Customer
match the Color Standard, report these also. Service at service@astm.org.
A2. TEST METHOD FOR THICKNESS DEPOSIT RATING OF HEATER TUBES—INTERFEROMETRIC METHOD
A2.1 Scope NOTE A2.2—If this procedure is to be used to rate the heater tube after
the thermal oxidation test, the new heater tube may also be examined by
A2.1.1 This annex describes a procedure for the interfero- the same technique to establish a base line or condition of satisfactory
metric thickness deposit rating in the range of 0 nm to 1200 nm starting quality.
of heater tubes produced by Test Method D3241—Thermal
Oxidation Stability of Aviation Turbine Fuels. A2.2 Terminology
A2.1.2 The final result from this rating procedure is an A2.2.1 Definitions of Terms Specific to This Standard:
absolute measurement of the thickness and volume of deposit A2.2.1.1 deposit—film of oxidized product deposited on the
on the heater tube that provides a basis for judging the thermal test area of the heater tube after D3241 test procedure.
oxidative stability of the fuel sample. For aircraft fuel systems A2.2.1.2 deposit profile—three-dimensional representation
performance, deposit thickness and volume are useful param- of deposit thickness profile along and around the length of the
eters. heater tube test section.
A2.1.3 An interlaboratory study was conducted in October A2.2.1.3 deposit thickness—the thickness of deposit present
2011 (see ASTM Research Report RR:D02-17869 for support- on the heater tube substrate surface expressed in nanometers,
ing data) involving 8 interferometric instruments and 117 nm.
heater tubes tested in duplicate. The interferometric procedure
demonstrated objective rating. A2.2.1.4 deposit volume—the volume of deposit present on
the test section of the heater tube expressed in mm3.
NOTE A2.1—The particular technique used for this test method is called A2.2.1.4.1 Discussion—The deposit volume is derived by
spectral reflectance.
integration of the area under the deposit profile.
9
A2.2.1.5 interferometry—a technique used for measuring
be obtained by requesting Research Report RR:D02-1786. Contact ASTM Customer the optical properties of surfaces (refractive index and absorp-
Service at service@astm.org. tion coefficient) based on studying the pattern of interference

8
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
created by their superposition. In the presence of a thin measuring light interferences, heater tube handling assembly,
transparent layer called film, interferometry can also be used to heater tube rotating system, optical probe displacement system
provide film thickness information. and computer-driven software for analyzing the interferometric
A2.2.1.6 standard spot—the mean thickness of the six data.
thickest points in a 2.5 mm2 area, as shown in Fig. A2.6, A2.6.1.2 The instrument must be capable to precisely and
defined in section A1.11.2.1 of this test method. automatically displace the optical probe with the resolution
defined in section A2.8.2.3.
A2.3 Summary of Test Method A2.6.1.3 The instrument must be able to automatically
A2.3.1 An interferometric apparatus, as shown in Fig. A2.1, rotate the heater tube with the resolution defined in section
is used to rate the deposit on the heater tube. The computer- A2.8.2.4.
driven software analyzes the interferometric data. The deposit A2.6.1.4 The instrument, with its optical probe, must be
thickness and deposit volume are derived and displayed. able to automatically detect the edge of one of the two
shoulders of the heater tube; the distance between these two
A2.4 Significance and Use shoulders is 60 mm.
A2.4.1 The final heater tube rating is a direct thickness and A2.6.1.5 The instrument can measure the thickness over the
volume measurement of the degraded fuel deposited on the whole length of the heater tube. However, this test method
heater tube. This rating is one basis for judging the thermal describes a procedure to measure the deposit thickness between
oxidative stability of the fuel sample. the 5 mm and the 55 mm points located between the two
shoulders of the heater tube, as defined in Test Method D3241
A2.5 Reagents and Materials (Fig. A2.7).
A2.5.1 Reference Heater Tube10—with two reference de- A2.6.1.6 For the calculation of the film deposit thickness,
posits of known and traceable thickness made with silicon the computer driven software must be able to automatically
dioxide on silicon (Si + SiO2). See Fig. A2.2. select against wavelength the appropriate refractive index
value (n) and absorption coefficient value (k) for the substrate
A2.6 Apparatus and the deposit film. These values are indicated in the graphs
A2.6.1 Deposit Rater:11 in sections A2.8.2.1 and A2.8.2.2.
A2.6.1.1 Comprising of a suitable UVVIS light source
A2.7 Test Samples (Heater Tube)
(200 nm to 1100 nm), reflected light probe capable to generate
a spot light of 200 µm diameter, detector of reflected light for A2.7.1 Handle the heater tube carefully so as not to touch
the center portion at any time.
10
The sole source of supply of the reference heater tube known to the committee NOTE A2.3—Touching the center (thinner area) of the heater tube will
at this time is AD systems (www.adsystems-sa.com), available from AD systems, likely contaminate or disturb the surface of the heater tube, deposit, or
P.A. Portes de la Suisse Normande, Allée de Cindais, 14320 Saint André sur Orne, both, which must be evaluated in pristine condition.
France. If you are aware of alternative suppliers, please provide this information to
ASTM International Headquarters. Your comments will receive careful consider- A2.8 Apparatus Preparation
ation at a meeting of the responsible technical committee,1 which you may attend
11
The sole source of supply of the deposit rater apparatus known to the A2.8.1 Install the apparatus in accordance with the manu-
committee at this time is AD systems (www.adsystems-sa.com), model DR 10 – facturer’s instructions. If any malfunction is indicated refer to
Deposit Rater, available from AD systems, P.A. Portes de la Suisse Normande, Allée
de Cindais, 14320 Saint André sur Orne, France. If you are aware of alternative the manufacturer’s instructions.
suppliers, please provide this information to ASTM International Headquarters. NOTE A2.4—Malfunctions are checked automatically when switching
Your comments will receive careful consideration at a meeting of the responsible on the instrument and during the operation. Any malfunction will be
technical committee,1 which you may attend. automatically indicated.
FIG. A2.1 Interferometric Apparatus—General Principle

9
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
FIG. A2.2 Reference Heater Tube
FIG. A2.3 n and k Values of the Heater Tube
A2.8.2 Standard Operating Conditions: be used for instrument verification. Behenate films are anisotropic and do
A2.8.2.1 Heater Tube (Substrate)—refractive index (n) and not relate to deposits. They are sub-layered with metals separated by fatty
chains which creates multiple reflection for each sub layer. In other words,
absorption coefficient (k) values are automatically selected by
the Lanmuir-Blodgett films of cadmium behenate do not create any
the computer software using the relationship shown in the interference with spectral reflectance technique when the emitted light is
graph below (Fig. A2.3). normal to the deposit surface which is the case with the DR 10.
NOTE A2.5—The value of n and k index are dependent on the A2.8.2.3 Circumferential Resolution—(number of points
metallurgy and surface roughness of the heater tube under examination.
measured on the heater tube circumference), 24 points (Fig.
The values on the graphs here above are appropriate for heater tubes used
in D3241. A2.5).
A2.8.2.2 Deposit Film—refractive index (n) and absorption A2.8.2.4 Longitudinal Resolution—(number of points mea-
coefficient (k) values are automatically calculated by the sured on a length of 50 mm), 50 points (Fig. A2.6).
computer software using the relationship shown in the graph A2.8.2.5 Heater Tube Scanned Surface—the instrument
below (Fig. A2.4). shall be set up to measure the thickness between the 5 mm and
the 55 mm points. See Fig. A2.7.
NOTE A2.6—This represents the average value of refractive index of
heater tube deposit after D3241 test procedure. A2.9 Apparatus Verification
NOTE A2.7—It is assumed that the film is optically transparent to the
wavelength of UVVIS light used in the DR 10, currently 200 nm to A2.9.1 On a regular basis, a minimum of once per week,
1100 nm.
NOTE A2.8—This method is not applicable to heater tubes coated with
verify the operation of the apparatus by measuring a reference
Langmuir-Blodgett films of cadmium behenate. Consequently, heater heater tube (A2.5.1). To do so, refer to the operation manual
tubes coated with Langmuir-Blodgett films of cadmium behenate cannot delivered with the instrument. The results shall be within 65 %

10
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
FIG. A2.4 n and K Values of the Deposit Film
FIG. A2.5 Circumferential Resolution
FIG. A2.6 Standard Spot
of the known thickness. If the determined values are not within

the acceptable limits, return the apparatus to the manufacturer
for recalibration.

11
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
FIG. A2.7 Description of Heater Tube Scanned Surface
A2.10 Heater Tube Inspection NOTE A2.9—The rotation and the positioning of the heater tube has two
functions. The first one for traceability of the test, the instrument
A2.10.1 Handle the heater tube carefully and do not touch magnifies the serial number and takes a picture of the heater tube serial
the center section at any time. number. Second, it positions the heater tube on the same point of the
circumference to ensure that the sequence of thickness measurements is
A2.10.2 Visually examine the heater tube for straightness by started from the same point on the circumference. Consequently, for
rolling the heater tube on a flat dust-free surface and noting the verification, when the test is repeated on the same heater tube, it facilitates
gap between the flat surface and the center section. Heater the comparison of the deposit profiles.
tubes with a bent center section are not suitable for rating by A2.11.4 At the end of the measurement, the reported values
the DR 10. are displayed and recorded, as shown in Fig. A2.8.
A2.10.3 Examine the heater tube, without magnification, in A2.11.5 Remove the rated heater tube and return it to its
laboratory light for visible mechanical scratches on the centre original container.
section of the heater tube. If such defects are visible, discard
the heater tube. A2.12 Reporting
A2.11 Procedure A2.12.1 Report the following:
A2.12.1.1 Standard spot deposit thickness to the nearest
A2.11.1 To start a test, refer to the operation manual 1 nm.
delivered with the instrument.
A2.12.1.2 Deposit volume to the nearest 0.00001 mm3 or
A2.11.2 For an instrument with software version older than “N/A” when the volume is not reported.
1.2.8.6 perform a baseline calibration prior to initial use and
NOTE A2.10—In some cases, the apparatus is unable to precisely
whenever there is a change in heater tube brand. It is determine the thickness at one or several of the 1200 measured points.
recommended to run the instrument with the latest version of When this situation occurs, because safety is involved with D3241 test, the
the software. Contact the manufacturer for the upgrade. apparatus does not extrapolate the thickness from the surrounding points.
It simply reports “N/A” (Non Applicable) for the point in question. If the
A2.11.3 Once the jet fuel sample details in addition with the number of reported “N/A” points exceeds 10, then the Deposit Volume of
heater tube details are entered, the thickness measurement is is reported as “N/A”. However, the apparatus still reports the standard spot
automatically initiated. thickness which is based on the average of the thickest points in a 2.5 mm2
FIG. A2.8 Reporting Example

12
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
area. This reported standard spot is calculated with all the points for which TABLE A2.1 Precision of Deposit Thickness Measurement by
the thickness was determined. Interferometric (Heater) Tube Rating (ITR) (nm)
In some cases, when the apparatus reports a “N/A Deposit Volume”, the Measurement Range Repeatability (r) Reproducibility (R)
heater tube in question is visually rated (VTR) as an abnormal deposit. No
7.2 to 1189.6 0.0009857 (x+2000) 0.001996 (x+2000)
correlation can be established between “N/A Deposit Volume” reporting
and abnormal visual rating. It was observed with the results of the ILS
conducted in 2011 (Research Report RR:D02-1786) that when a “N/A
Deposit Volume” was reported, it was associated with thick deposits and same heater tube, would in the long run, in the normal and
it is expected to be typical. correct operation of Annex A2, exceed the values in Table A2.1
only in one case in twenty, where x is the average of the two
A2.13 Test Report deposit measurements.
A2.13.1 The test report shall contain at least the following A2.14.1.2 Deposit Volume:
information: (1) Repeatability Limit (r)—The difference between suc-
A2.13.1.1 Sufficient details for complete identification of cessive deposit measurements, obtained by the same operator
the fuel and the heater tube tested; with the same apparatus under constant operating conditions on
A2.13.1.2 A reference to this standard; the same heater tube, would in the long run, in the normal and
A2.13.1.3 The result of the test (see A2.11); correct operation of Annex A2, exceed the values in Table A2.2
A2.13.1.4 Any deviation, by agreement or otherwise, from only in one case in twenty, where x is the average of the two
the procedure specified; deposit measurements.
A2.13.1.5 The date of the test. (2) Reproducibility Limit (R)—The difference between two
single and independent deposit measurements, obtained by
A2.14 Precision and Bias different operators working in different laboratories on the
A2.14.1 Precision—The following criteria provides infor- same heater tube, would in the long run, in the normal and
mation on the accuracy of the deposit measurements using this correct operation of Annex A2, exceed the values in Table A2.2
technique:12 only in one case in twenty, where x is the average of the two
A2.14.1.1 Deposit Thickness: deposit measurements.
(1) Repeatability Limit (r)—The difference between suc- A2.14.2 Bias—Since there are no accepted reference mate-
cessive deposit measurements, obtained by the same operator rials suitable for determining the bias for this procedure, bias of
with the same apparatus under constant operating conditions on deposit thickness and deposit volume measurements between
the same heater tube, would in the long run, in the normal and Annex A2, Annex A3, and Annex A4 of this test method have
correct operation of Annex A2, exceed the values in Table A2.1 not yet been determined.
only in one case in twenty, where x is the average of the two A2.14.3 The precision statements were derived from a 2011
deposit measurements. intralaboratory study of deposit thickness and volume measure-
(2) Reproducibility Limit (R)—The difference between two ments.12 One laboratory using 8 instruments tested 117 heater
single and independent deposit measurements, obtained by tubes in duplicate for deposit thickness and deposit volume.
different operators working in different laboratories on the Information on the heater tubes and their average deposit
measurements are in the research report.12
12
Supporting data have been filed at ASTM International Headquarters and may TABLE A2.2 Precision of Deposit Volume Measurement by
be obtained by requesting Research Report RR:D02-1786. Data supporting auto- Interferometric (Heater) Tube Rating (ITR) (mm3)
mated baseline calibration of the ITR in effect since software version 1.2.8.6 has
been filed at ASTM International Headquarters and may be obtained by requesting Measurement Range Repeatability (r) Reproducibility (R)
Research Report RR:D02-2051. Contact ASTM Customer Service at 0.0004 to 0.1934 0.002274 (x+0.2) 0.006447 (x+0.2)
service@astm.org.
A3. RATING OF HEATER TUBES—ELLIPSOMETRIC METHOD
A3.1 Scope NOTE A3.1—If this procedure is to be used to rate the heater tube after
the D3241 test, the new heater tube may be examined in an Ellipsometeric
A3.1.1 This annex describes a procedure for the ellipsomet- (Heater) Tube Rater (ETR) to establish a base line or condition of
ric rating of heater tubes produced by Test Method D3241— satisfactory starting quality.
Thermal Oxidation Stability of Aviation Turbine Fuels.
A3.2 Terminology
A3.1.2 The final result from this rating procedure is an
absolute measurement of the deposit thickness on the heater A3.2.1 Definitions of Terms Specific to This Standard:
tube that can provide a basis for judging the thermal oxidative A3.2.1.1 deposit profile—three-dimensional representation
stability of the fuel sample. For aircraft fuel systems of the deposit thickness along and around the length of the
performance, deposit thickness is a useful parameter. heater tube test area.

13
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
A3.2.1.2 deposit thickness—the thickness of deposit present A3.6 Apparatus
on the heater tube substrate surface expressed in nanometers A3.6.1 Ellipsometric (Heater) Tube Rater (ETR)15 is com-
(nm). prised of a suitable laser light source, optical detector for
A3.2.1.3 ellipsometry—a technique used for measuring the measuring the ellipsometric parameters, heater tube handling
optical properties of surfaces (refractive index and absorption assembly and computer-driven software for analyzing the
coefficient) based on changes in the polarized state of light ellipsometric data. It is designed to combine the ellipsometric
upon reflection from the surface. principles with specific heater tube handling.
A3.2.1.3.1 Discussion—In the presence of a thin transparent
A3.6.2 The thickness measurement is performed over the
layer, with a known refractive index and absorption coefficient,
length of the heater tube, from 5 mm to 55 mm of the total
ellipsometry can also be used to provide film thickness
60 mm length, as designed by Test Method D3241.
information.
A3.2.1.4 maximum deposit thickness—the maximum thick- A3.7 Apparatus Preparation
ness of an average 2.5 mm2 deposit present on the heater tube A3.7.1 Install the apparatus in accordance with the manu-
surface, expressed in nanometers, nm. facturer’s instructions. Ensure satisfactory function of the
ellipsometric device in terms of alignment and optical diag-
A3.3 Summary of Test Method
nostics. If any malfunction is indicated refer to the manufac-
A3.3.1 An ellipsometric apparatus13 is used to rate the turer’s instructions.
deposits on the heater tube. The computer-driven software
A3.7.2 Standard operating conditions.
analyses the ellipsometric data and the maximum deposit
A3.7.2.1 Substrate refractive index setting 2.65.
thickness of an average 2.5 mm2 is derived and displayed.
NOTE A3.2—The value of refractive index selected is dependent on the
A3.4 Significance and Use metallurgy and surface roughness of the D3241 heater tube under
examination. The value 2.65 is appropriate for heater tubes used in D3241.
A3.4.1 The final heater tube rating is a direct measure of the See the ETR operating instructions for detailed requirements for other
thickness of the degraded fuel deposited on the heater tube. metallurgies.
This rating is a basis for judging the thermal oxidative stability
A3.7.2.2 Substrate absorption coefficient setting (k) – 9.40.
of the fuel sample.
NOTE A3.3—The value of absorption coefficient is dependent on the
A3.5 Reagents and Materials metallurgy of the D3241 heater tube under examination. The value of
minus 9.40 is appropriate for heater tubes used in D3241. See ETR
A3.5.1 Ellipsometer NIST Traceable Reference Tube, a operating instructions for detailed requirements for other metallurgies.
special tube designed for holding two wafer pieces with known
NIST Traceable deposits of SiO2 on Si in the ranges of 60 nm A3.7.2.3 Deposit film refractive index setting 1.45.
and 100 nm. Additional areas on the tube to align wafer pieces NOTE A3.4—This represents the average value of refractive index based
to laser beam (refer to Fig. A3.1). Each tube includes a on many organic films.
certification of thickness of the spots for the user to compare in A3.7.2.4 Deposit film absorption coefficient 0.00.
the verification process.14
NOTE A3.5—It is assumed that the film is optically transparent to the
13
15
be obtained by requesting Research Report RR:D02-1774. Contact ASTM Customer The sole source of supply of the ETR ellipsometric rater apparatus known to
Service at service@astm.org. the committee at this time is Falex Corporation, Model Falex 430 Ellipsometer
14
The sole source of supply of the apparatus (reference tube kits) known to the available from Falex Corporation, 1020 Airpark Dr., Sugar Grove, Ill 60554. A
committee at this time is Falex Corporation, 1020 Airpark Dr., Sugar Grove, Ill Falex 430 Mk I/Mk II correlation report is available as RR:D02-1912. If you are
60554. If you are aware of alternative suppliers, please provide this information to aware of alternative suppliers, please provide this information to ASTM Interna-
ASTM International Headquarters. Your comments will receive careful consider- tional Headquarters. Your comments will receive careful consideration at a meeting
ation at a meeting of the responsible technical committee,1 which you may attend. of the responsible technical committee,1 which you may attend.
FIG. A3.1 Ellipsometer NIST Traceable Reference Tube

14
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
wavelength of the laser light used in the ETR, currently 1550 nm. A3.11.1.3 The deposit volume in mm3;
A3.7.2.5 Resolution (number of circumferential points), 24 A3.11.1.4 Sufficient details for complete identification of
points. the fuel and the heater tube tested;
A3.7.2.6 Resolution (number of longitudinal points), 50 A3.11.1.5 A reference to this standard;
points. A3.11.1.6 Any deviation, by agreement or otherwise, from
the procedure specified; and
NOTE A3.6—The ETR has the capability to measure up to a maximum
of 100 points along the length of the heater tube and up to 360 equally
A3.11.1.7 The date of the test.
spaced points around the circumference of the heater tube.
A3.12 Precision and Bias
A3.7.2.7 The ETR records the maximum average 2.5 mm2
A3.12.1 Precision—The following criteria provides infor-
deposit thickness in nanometers, nm. When using the test
mation on the accuracy of the deposit measurements using this
resolution of 24 × 50 points, the 2.5 mm2 area is defined 6
technique:16
points in a row or any set of 3 consecutive pairs of points. The
A3.12.1.1 Deposit Thickness:
manufacturer includes an algorithm that automatically identi-
(1) Repeatability Limit (r)—The difference between suc-
fies all 6 point combinations, calculates the average thickness
cessive deposit measurements, obtained by the same operator
of each of these combinations, selects the maximum average 6
with the same apparatus under constant operating conditions on
point combination, displays the maximum average and shows
the same heater tube, would in the long run, in the normal and
the location of the maximum on the deposit graph.
correct operation of Annex A3, exceed the values in Table A3.1
A3.8 Apparatus Verification only in one case in twenty, where x is the average of the two
deposit measurements.
A3.8.1 Verify the operation of the ellipsometric apparatus
(2) Reproducibility Limit (R)—The difference between two
by measuring Ellipsometer reference tubes (A3.5.1). The
single and independent deposit measurements, obtained by
results shall be within the 65 % of the known thickness and
different operators working in different laboratories on the
61 mm of the known position. If the determined values are not
same heater tube, would in the long run, in the normal and
within the acceptable limits contact the manufacturer for
correct operation of Annex A3, exceed the values in Table A3.1
re-calibration service.
A3.9 Heater Tube Inspection deposit measurements.
A3.12.1.2 Deposit Volume:
A3.9.1 Handle the heater tube carefully and do not to touch (1) Repeatability Limit (r)—The repeatability of heater
the center portion at any time. tube deposit volume measurements by Ellipsometric (Heater)
A3.9.2 Visually examine the heater tube for straightness by Tube Rating has not yet been determined.
rolling the heater tube on a flat surface and noting the gap (2) Reproducibility Limit (R)—The reproducibility of
between the flat surface and the center section. Heater tubes heater tube deposit volume measurements by Ellipsometric
with a bent center section are not suitable for rating by the (Heater) Tube Rating has not yet been determined.
ETR. A3.12.2 Bias—Since there are no accepted reference mate-
A3.10 Procedure rials suitable for determining the bias for this procedure, bias of
deposit thickness and deposit volume measurements between
A3.10.1 Run the instrument in accordance with the manu- Annex A2, Annex A3, and Annex A4 of this test method have
facturer’s operating instructions. not yet been determined.
A3.10.2 At the end of the measurement procedure, record A3.12.3 The precision statements were derived from a 2013
the maximum average 2.5 mm2 deposit thickness in intralaboratory study of deposit thickness measurements.16
nanometers, nm. When using the test resolution of 24 × 50 One laboratory using 6 instruments tested 10 heater tubes in
points, the 2.5 mm2 area is defined 6 points in a row or any set duplicate for deposit thickness. Information on the heater tubes
of 3 consecutive pairs of points. The manufacturer includes an and their average deposit measurements are in the research
algorithm that automatically identifies all 6 point report.16
combinations, calculates the average thickness of each of these
combinations, selects the maximum average 6 point
16
combination, displays the maximum average and shows the Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1774. Contact ASTM Customer
location of the maximum on the deposit graph. Service at service@astm.org.
A3.11 Reporting
TABLE A3.1 Precision of Deposit Thickness Measurement by
A3.11.1 Report the: Ellipsometric (Heater) Tube Rating (ETR) (nm)
A3.11.1.1 The heater tube reference number; Measurement Range Repeatability (r) Reproducibility (R)
A3.11.1.2 The maximum average 2.5 mm2 deposit thick- 6 to 112 0.00981 (x+73.12) 0.0261 (x+73.12)
ness in nm;

15
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
A4. RATING OF HEATER TUBES—MULTI-WAVELENGTH ELLIPSOMETRIC METHOD
A4.1 Scope reported, known as a standard spot. The deposit volume is also
A4.1.1 This annex describes a procedure for the multi- calculated and reported.
wavelength ellipsometric rating of the heater tubes in Test A4.4 Significance and Use
Method D3241—Thermal Oxidation Stability of Aviation Tur-
bine Fuels. A4.4.1 The final heater tube rating is a measure of the
thickness and volume of the degraded fuel deposited on the
A4.1.2 This procedure covers fuel deposit thickness mea- heater tube. This rating is a basis for judging the thermal
surement in the range of 2 nm to 252 nm, and the precision has oxidative stability of the fuel sample.
been estimated for fuel deposit thickness in the range of 2.8 nm
to 234 nm. A4.4.2 For aircraft fuel systems performance, deposit thick-
ness and volume is a useful parameter.
A4.1.3 The multi-wavelength ellipsometer is capable of
deposit thickness measurement above 252 nm, however, pre- A4.5 Reagents and Materials
cision has not been estimated. A4.5.1 Ellipsometer reference tubes, on which layers of
A4.2 Terminology deposits of known thickness of 30 nm, 50 nm, 80 nm, 130 nm,
and 250 nm have been generated using atomic layer deposition
A4.2.1 Definitions of Terms Specific to This Standard: of silicon dioxide upon aluminum.
A4.2.1.1 deposit, n—film of oxidized product deposited on NOTE A4.1—Reference tubes with deposits of known thickness are
available from the manufacturer of the multi-wavelength ellipsometer.
the test area of the heater tube after D3241 test procedure.
A4.2.1.2 deposit profile, n—three-dimensional representa- A4.6 Apparatus
tion in terms of deposit thickness along and around the length A4.6.1 Multi-Wavelength Ellipsometric (Heater) Tube
of the heater tube test section. Rater (MWETR)17,18 as shown in Fig. A4.1 is comprised of
A4.2.1.3 deposit thickness, n—the thickness of deposit pres- suitable LED light source(s), optical detector(s) for measuring
ent on the heater tube substrate surface expressed in nanome- the ellipsometric parameters, precise heater tube handling
ters (nm). assembly and computer-driven software for analyzing the
A4.2.1.4 deposit volume, n—the volume of deposit present ellipsometric data. It is designed to combine the ellipsometric
on the test section of the heater tube expressed in mm3. principles with specific heater tube handling.
A4.2.1.4.1 Discussion—The deposit volume is derived by A4.6.2 The thickness and volume measurement is per-
integration of the area under the deposit profile. formed over the length of the heater tube, from 5 mm to 55 mm
A4.2.1.5 ellipsometry, n—a technique used for measuring of the total 60 mm length, as defined by Test Method D3241.
the optical properties of surfaces (refractive index and absorp- A4.6.3 The rater shall sequentially acquire ellipsometric
tion coefficient) based on changes in the polarized state of light data across four discrete wavelength bands centered at 466 nm,
upon reflection from the surface. 525 nm, 596 nm, and 638 nm.
A4.2.1.5.1 Discussion—In the presence of film deposits, A4.6.4 The rater shall sequentially pass each LED wave-
with presumed refractive index and absorption coefficient, length on a point on the heater tube surface of approximately
ellipsometry can also be used to provide film thickness 0.41 mm by 1.1 mm with the Brewster Angle set nominally at
information. 69.8 degrees.
A4.2.1.6 maximum deposit thickness, n—the maximum A4.6.5 The rater analytical system shall be capable of
thickness of an average 2.5 mm2 deposit present on the heater selecting against wavelength the appropriate refractive index
tube surface, expressed in nanometers, nm. value (n) and absorption coefficient value (k) for the substrate,
A4.2.1.7 standard spot, n—the mean thickness of the six oxide layer, and the deposit film. These values are indicated in
thickest points in a 2.5 mm2 area, as defined in section section A4.7.
A1.11.2.1 of this test method. A4.6.6 The rater shall be capable of precisely displacing the
A4.2.2 Abbreviations: heater tube longitudinally and rotationally, in relation to the
optical bench, with the resolution defined in A4.7.
A4.2.2.1 MWETR, n—multi-wavelength ellipsometric
(heater) tube rater
17
A4.2.2.2 VTR, n—visual heater tube rater The sole source of supply of the multi-wavelength ellipsometric (heater) tube
rater known to the committee at this time is PAC LP (www.paclp.com.com), model
A4.3 Summary of Test Method Opitireader™, available from PAC LP, 8824 Fallbrook, Houston, Texas, USA
77064. If you are aware of alternative suppliers, please provide this information to
A4.3.1 A multi-wavelength ellipsometric apparatus is used ASTM International Headquarters. Your comments will receive careful consider-
ation at a meeting of the responsible technical committee,1 which you may attend.
to rate the deposits on the heater tube. The computer-driven 18
software analyzes the ellipsometric data and the maximum be obtained by requesting Research Report RR:D02-1872. Contact ASTM Customer
deposit thickness of an average 2.5 mm2 is derived and Service at service@astm.org.

16
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
FIG. A4.1 Multi-Wavelength Ellipsometer Apparatus—General Principle
A4.6.7 The rater shall be capable of calculating and record- A4.7.2.3 Aluminum Oxide refractive index setting (n)
ing the thickness in nanometers and the volume in cubic n(466 nm) = 1.778
millimeters over the 24 by 50 points. n(525 nm) = 1.772
A4.6.8 The rater shall be capable of calculating the mean n(596 nm) = 1.768
thickness amongst all 24 points in each of the 50 rows. Subtract n(638 nm) = 1.766
the minimum row mean value from each of the 1200 overall NOTE A4.4—The value of aluminum oxide refractive indices selected
points, and generate the final thickness report. were obtained from well-known reference literature.19
A4.6.9 The rater shall be capable of searching for any A4.7.2.4 Aluminum Oxide absorption coefficient (k)
cluster of six neighboring points with an average thickness of k(466 nm) = 0
greater than 85 nm or more and reporting status. k(525 nm) = 0
k(596 nm) = 0
A4.6.10 The rater shall be capable of calculating and
k(638 nm) = 0
reporting the total deposit volume, in cubic millimeters, of the
thickness and surface area scanned. NOTE A4.5—The value of aluminum oxide absorption coefficients
selected were obtained from well-known reference literature.19
A4.7 Apparatus Preparation A4.7.2.5 Deposit film refractive index setting (n)
A4.7.1 Install the apparatus in accordance with the manu- n(466 nm) = 1.478
facturer’s instructions. Ensure satisfactory function of the n(525 nm) = 1.471
ellipsometric device in terms of alignment and optical diag- n(596 nm) = 1.466
nostics. If any malfunction is indicated refer to the manufac- n(638 nm) = 1.464
turer’s instructions. NOTE A4.6—The average value of deposit film refractive indices
A4.7.2 Standard operating conditions. selected were derived from many representative organic films measured
A4.7.2.1 Substrate refractive index setting (n) on multiple multi-wavelength instruments which had the substrate con-
stants and aluminum oxide constants set to the stated literature values.
n(466 nm) = 0.662
n(525 nm) = 0.856 A4.7.2.6 Deposit film absorption coefficient (k)
n(596 nm) = 1.177 k(466 nm) = 0.107
n(638 nm) = 1.400 k(525 nm) = 0.082
k(596 nm) = 0.064
NOTE A4.2—The value of refractive indices selected were obtained k(638 nm) = 0.057
from well-known reference literature.19
A4.7.2.2 Substrate absorption coefficient setting (k) NOTE A4.7—The average value of deposit film absorption coefficients
selected were derived from many representative organic films measured
k(466 nm) = 5.659 on multiple multi-wavelength instruments which had the substrate con-
k(525 nm) = 6.382 stants and aluminum oxide constants set to the stated literature values.
k(596 nm) = 7.21
A4.7.2.7 Resolution (number of circumferential points), 24
k(638 nm) = 7.668
points.
NOTE A4.3—The value of absorption coefficients selected were ob- A4.7.2.8 Resolution (number of longitudinal points), 50
tained from well-known reference literature.19 points.
NOTE A4.8—The rater has the capability to measure up to a maximum
19
Palik, Edward D., Handbook of Optical Constants of Solids, Handbook of of 5000 points along the length of the heater tube and up to 384 equally
Optics, 3rd edition, Vol. 4, 2009, McGraw-Hill. spaced points around the circumference of the heater tube.

17
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
A4.7.2.9 The rater records the maximum average 2.5 mm2 A4.11.1.5 Reference to this standard, and annex;
deposit thickness in nanometers (nm). The manufacturer in- A4.11.1.6 Reference to the Optics Model “PAC Thick4
cludes an algorithm that automatically identifies all 6 point Fast”;
combinations, calculates the average thickness of each of these A4.11.1.7 Any deviation, by agreement or otherwise, from
combinations, selects the maximum average 6 point the procedure specified;
combination, displays the maximum average and total deposit A4.11.1.8 Date of the test.
volume, and shows the location of the maximum on the deposit NOTE A4.10—A typical report is shown in Fig. A4.2.
graph.
A4.12 Precision and Bias
A4.8 Apparatus Verification
A4.12.1 Precision—The following criteria provides infor-
A4.8.1 Verify the operation of the multi-wavelength ellip- mation on the accuracy of the deposit measurements using this
sometric apparatus periodically by measuring ellipsometer technique:20
reference tubes (A4.5.1). The results shall be within the 65 % A4.12.1.1 Deposit Thickness:
of the known thickness. If the determined values are not within (1) Repeatability Limit (r)—The difference between suc-
the acceptable limits contact the manufacturer for re- cessive deposit measurements, obtained by the same operator
calibration service. with the same apparatus under constant operating conditions on
NOTE A4.9—A recommended interval for verification is at least once
per week, or at any time that re-calibration or changes in condition are
the same heater tube, would in the long run, in the normal and
apparent. correct operation of Annex A4, exceed the values in Table A4.1
A4.9 Heater Tube Inspection deposit measurements.
A4.9.1 Handle the heater tube carefully and do not touch the (2) Reproducibility Limit (R)—The difference between two
center portion at any time. single and independent deposit measurements, obtained by
A4.9.2 Visually examine the heater tube for straightness by same heater tube, would in the long run, in the normal and
rolling the heater tube on a flat surface and noting the gap correct operation of Annex A4, exceed the values in Table A4.1
between the flat surface and the center section. Heater tubes only in one case in twenty, where x is the average of the two
with a bent center section are not suitable for rating by the deposit measurements.
MWETR. A4.12.1.2 Deposit Volume:
A4.10 Procedure (1) Repeatability Limit (r)—The difference between suc-
cessive test deposit measurements, obtained by the same
A4.10.1 Operate the instrument in accordance with the operator with the same apparatus under constant operating
manufacturer’s operating instructions. conditions on the same heater tube, would in the long run, in
A4.10.2 Insert the heater tube into the measuring system the normal and correct operation of Annex A4, exceed the
with the serial number on bottom and opposing the operator (6 values in Table A4.2 only in one case in twenty, where x is the
o’clock position). average of the two deposit measurements.
A4.10.3 Enter the heater tube details in the user interface (2) Reproducibility Limit (R)—The difference between two
and initiate the deposit thickness and volume measurements. single and independent deposit measurements, obtained by
A4.10.4 At the end of the measurement procedure, record same heater tube, would in the long run, in the normal and
the maximum average 2.5 mm2 deposit thickness in nanome- correct operation of Annex A4, exceed the values in Table A4.2
ters (nm) as provided by the apparatus. The manufacturer only in one case in twenty, where x is the average of the two
includes an algorithm that automatically identifies all 6 point deposit measurements.
combinations, calculates the average thickness of each of these
combinations, selects the maximum average 6 point A4.12.2 Bias—Since there are no accepted reference mate-
combination, displays the maximum average and shows the rials suitable for determining the bias for this procedure, bias of
location of the maximum on the deposit graph. deposit thickness and deposit volume measurements between
Annex A2, Annex A3, and Annex A4 of this test method have
A4.10.5 Record the deposit volume in cubic millimeters not yet been determined.
(mm3) as provided by the apparatus.
A4.12.3 The precision statements were derived from a 2016
A4.11 Reporting intralaboratory study of deposit thickness and deposit volume
measurements.20 One laboratory using 6 instruments tested 45
A4.11.1 Report:
heater tubes in duplicate for deposit thickness and deposit
A4.11.1.1 The heater tube reference number;
volume. Information on the tubes and their average deposit
A4.11.1.2 The maximum average 2.5 mm2 deposit thick-
measurements are in the research report.20
ness to the nearest 1 nm;
A4.11.1.3 The volume deposit to the nearest 0.00001 mm3; 20
A4.11.1.4 Sufficient details for complete identification of be obtained by requesting Research Report RR:D02-1872. Contact ASTM Customer
the fuel and the heater tube tested; Service at service@astm.org.

18
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
FIG. A4.2 Multi-Wavelength Ellipsometer Apparatus Typical Reports 3D and 2D Color Maps (VTR 3)
TABLE A4.1 Precision of Deposit Thickness Measurement by

Multi-Wavelength Ellipsometric (Heater) Tube Rating (MWETR)
Measurement Range Repeatability (r) Reproducibility (R)
2.8 to 234 1.0627 (x0.2) 1.5251 (x0.2)
TABLE A4.2 Precision of Deposit Volume Measurement by Multi-

Wavelength Ellipsometric (Heater) Tube Rating (MWETR) (mm3)
Measurement Range Repeatability (r) Reproducibility (R)
0.00024 to 0.04827 0.001386 (x0.5) 0.005254 (x0.5)

19
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
A5. EQUIPMENT
A5.1 Test Instrument (5) Flow of fuel in all models can be monitored by visually
A5.1.1 The instrument described in this annex is the Avia- counting drops of flow. Also allow volumetric measure of flow
tion Fuel Thermal Oxidation Stability Tester that is used to test with time, which is considered the most accurate flow measure.
the thermal oxidation stability of turbine fuel. There are five A5.2.3 Heating/Temperature Control System—The heater
instrument models which will be described. All provide a tube is resistively heated by the conductance of high amperage,
means to pump the sample once through the test system across low voltage current from a transformer through the heater tube.
the heater tube and through a test filter. There are means to The heater tube is clamped to relatively heavy, water cooled
control and measure heater tube temperature, system pressure, current conducting bus bars, which increase in temperature
and pressure drop across the filter, and methods of control and relatively little.
measurement vary with each instrument model. Mechanism for A5.2.3.1 The temperature controller in all instrument mod-
pumping is positive displacement using a gear pump or piston els serves as indicator and controller. In automatic mode, the
pump. controller provides a source of steady heat during the test,
varying the power as necessary to maintain the target (setpoint)
A5.2 Test Details temperature. Temperature range of operation is from 180 °C to
A5.2.1 General Description—This instrument uses a fixed 350 °C.
volume of jet fuel that has been filtered, then aerated to provide A5.2.3.2 Critical to temperature control is the thermocouple
a sample saturated with air. During the test, fuel is pumped at and its position. The thermocouple itself must be calibrated to
a steady rate across a heater tube which is maintained at a ensure acceptable accuracy. The position of the tip must be
relatively high temperature, typically 260 °C, but higher under carefully placed so the temperature reading during automatic
some specifications. The fuel, saturated with oxygen from the control is the maximum (the hottest spot) for the heater tube. A
aeration, may degrade on the hot heater tube to form deposits simple mechanical positioning system allows easy and accurate
as a visible film. Also, the degraded materials of the fuel may placement of the thermocouple.
flow downstream and be caught by the test filter. Both the A5.2.3.3 A diagram of the basic heating system is shown in
increase in differential pressure across the test filter and the Fig. A5.4.
final heater tube rating are used to determine the oxidative
A5.2.4 Cooling System—In the normal operation of the
stability of the fuel.
instrument, some cooling is necessary to remove heat going
A5.2.2 Fuel System—Freshly filtered and aerated fuel is into the bus bars by conduction from the hot heater tube.
initially placed in a container, then circulated once through the Cooling water is circulated through each bus bar using an
apparatus to a spent sample container. Motive force for the internally circulated and radiator cooled liquid system. The
sample is a positive displacement pump that will maintain flow only precautions with these systems is to monitor them to be
at 3.0 mL ⁄min and overcome any tendency of initial filter sure they are working and to avoid use of coolants that contain
blockage from affecting the flow rate. Deviation of 10 % in contaminants or salts that may eventually foul the system.
flow rate is permitted. If filter blockage becomes severe, the
A5.2.5 Pressurization—At the temperature of a normal test,
bypass valve located before the test filter can be opened in
jet fuel would typically boil at the temperature of the heater
order to finish the test. Then, any deposit on the heater tube can
tube. This would prevent accurate temperature control and
be evaluated based on a complete test.
interfere with natural deposit formation. Therefore, the system
A5.2.2.1 The heart of the test system is the tube-in-shell
must be operated under a total pressure of about 3.45 MPa
heat exchanger, or heater tube test section Fig. A5.1, which
(500 psi). This pressure level is accomplished by a hydraulic
holds the heater tube and directs flow of fuel over it. It is
piston pump (Models 230 and 240) to produce the high
important for the heater tube to be aligned correctly in the
pressure needed.
heater tube test section as shown in Fig. A5.2. This component
A5.2.5.1 A pressure transducer is used to measure and allow
is critical to consistent results and is a common component in
monitoring of the total system pressure. The hydraulically
all models.
pressurized systems have a relief valve through which the fluid
A5.2.2.2 There are some other points regarding the fuel
passes in a constant leak throughout the test. For the relief
system that deserve mention:
valve control to operate uniformly for any fuel, a displacement
(1) Fresh fuel is filtered immediately out of the container
cell is used where the spent fuel enters the top displacing water
containing the aerated fuel through 0.45 µm membrane filter
out the bottom and through the relief valve (for Models 230
paper before entering the heater tube test section;
and 240 only). Since the valve sees only water, the valve works
(2) The heater tube is sealed in the heater tube test section
consistently.
by elastomer O-rings (Fig. A5.3);
(3) The test filter is of stainless steel of 17 µm rated A5.2.6 Differential Pressure Measure—All instruments use
porosity. Bypass of the filter occurs automatically when differ- an electronic ∆P transducer.
ential pressure reaches 250 mm Hg; A5.2.6.1 Proper use of this differential measuring device
(4) All models use two containers, one for fresh fuel and requires two special actions: bypass and air bleeding. The first
one for spent; allows the fuel flow to bypass the filter whenever that action

20
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
FIG. A5.1 Test Section Dimensions
becomes necessary. The second is used to remove air that at 6 % higher than true occurs. A transducer is not subject to this
times may become trapped in the cell chambers. error, so in order to have manometer and transducer models
A5.2.6.2 The original manometer system, by nature, in- read the correctly a 6 % bias is added to the transducer so it
cluded a bias due to the presence of fuel instead of the usual air gives the same value as would a manometer.
over the mercury. This changed the value of pressure expressed A5.2.6.3 When operated, the ∆P measuring device em-
in terms of column height of mercury such that a result about ployed must be zeroed under actual flow conditions at the start

21
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
FIG. A5.4 Heater Tube and Temperature Control Schematic
FIG. A5.2 Alignment of Heater Tube

checked by a technique of reading the pressure created by a
column of known density fluid on each side of the ∆P cell. The
details for doing this are included as part of each operating
manual for the particular model instrument. This standardiza-
tion is really a verification that the ∆P cell is operating
correctly and is not meant to be a true calibration of the cell.
Calibration must be done by the manufacturers of the cell if
such action is suggested based on the results of the standard-
ization.
A5.2.8 Thermocouple Calibration—It is important for the
thermocouple to be accurate. To ensure this value, a method of
calibration against known melting points is used and is
described in detail in the appropriate User Manual for each
instrument. Models 230 and 240 use two metals, tin (see 7.5)
at 232 °C and lead (see 7.4) at 327 °C, to define two points
surrounding the normal range used with the instrument. Also,
an ice-water mixture is used to establish a 0 °C low reference
point. Other models only use lead and an ice-water mixture.
A5.2.8.1 The principle used with melting point of metals is
to centrally immerse the thermocouple tip in the melted metal,
then allow the metal to cool. As the metal goes through its
freeze point, the temperature reading will hesitate momentarily
indicating the known point for the metal.
A5.2.8.2 The difference between the known metal freezing
value and the displayed temperature becomes a correction for
setting test temperatures. For example, using tin with a known
freeze temperature of 232 °C (see Fig. A5.5), if the temperature
FIG. A5.3 Assembly Drawing of Heater Tube Test Section
of the test. This is because a small pressure drop is created

across the system when fuel is flowing. Zeroing the transducer
at the beginning of the test compensates for the flow.
A5.2.7 Differential Pressure Measurement
Standardization—The ∆P measurement accuracy can be FIG. A5.5 Freezing Characteristics of Tin

22
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
noted at the time the metal froze was higher than 232°, then A5.2.10 Elapsed Time Measurement—There are various
this would indicate the thermocouple was reading high by the methods of timing the test depending on the model. The
difference indicated and the applied correction would be to elapsed time indicator is normally the basis used, but in some
lower any test temperature by this same amount. Where two models, the timing of the ∆P data collection is done with a
metals and ice water (low point) are used, the principle is the different timer. Since these two timers may not be exactly the
same but the correction is calculated and applied automatically same, the last data point may be lost if the test stops before the
by the internal computer. last timed data point. The user manuals for the various
A5.2.9 Fuel Aeration System—All models have means to instrument models cover techniques for avoiding loss of data
aerate the sample prior to testing. Without the presence of points.
oxygen in the sample, a proper test is not achieved. Filtered,
dry air is metered through the sample at about 1.5 L ⁄min rate
for 6 min. This 9 L of air ensures 97 % saturation of the
sample.
A6. WARNING STATEMENTS
A6.1 Acetone A6.4 n-Heptane

A6.1.1 Keep away from heat, sparks, and open flame. A6.4.1 Keep away from heat, sparks, and open flame.
A6.1.2 Keep container closed. Use with adequate ventila- A6.4.2 Keep container closed.
tion. A6.4.3 Use with adequate ventilation.
A6.1.3 Avoid buildup of vapors and eliminate all sources of A6.4.4 Avoid prolonged breathing of vapor or spray mist.
ignition, especially nonexplosion-proof electrical apparatus
and heaters. A6.4.5 Avoid prolonged or repeated skin contact.
A6.2 Toluene A6.5 Compressed Gases (Nitrogen)

A6.2.1 Avoid prolonged or repeated breathing of vapor or A6.5.1 Keep cylinder valve closed when not in use.
spray mist. A6.5.2 Do not enter storage areas unless adequately venti-
A6.2.2 Use only with adequate ventilation. lated.
A6.2.3 Eye irritation and dizziness are indications of over- A6.5.3 Always use a pressure regulator.
exposure. A6.5.4 Release regulator tension before opening cylinder.
A6.2.4 Do not take internally. A6.5.5 Do not transfer to cylinder other than one in which
A6.2.5 Swallowing may cause injury, illness, or death. gas is received.
A6.5.6 Do not mix gases in cylinders.
A6.2.6 Avoid prolonged or repeated contact with skin.
A6.5.7 Never drop cylinder.
A6.2.7 Do not get in eyes.
A6.5.8 Make sure cylinder is supported at all times.
A6.2.8 Can produce toxic vapors on contact with flames,
hot glowing surfaces, or electric arcs. A6.5.9 Stand away from cylinder outlet when opening
cylinder valve.
A6.3 Iso-propanol (2-propanol)
A6.5.10 Keep cylinder out of sun and away from heat.
A6.3.1 Keep away from heat, sparks, and open flame.
A6.5.11 Keep cylinder from corrosive environment.
A6.3.2 Keep container away from heat, sparks, and open
A6.5.12 Do not use cylinder without label.
flame.
A6.5.13 Do not use dented or damaged cylinders.
A6.3.3 Keep container closed.
A6.5.14 For technical use only.
A6.3.4 Use with adequate ventilation.
A6.5.15 Do not use for inhalation purposes.
A6.3.5 Avoid buildup of vapors and eliminate all sources of
ignition, especially nonexplosion-proof electrical apparatus A6.6 Aviation Turbine Fuel (Jet B, See Specification
and heaters. D1655)
A6.3.6 Avoid prolonged breathing of vapor or spray mist. A6.6.1 Keep away from heat, sparks, and open flames.
A6.3.7 Avoid prolonged or repeated skin contact. A6.6.2 Keep container closed.

23
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
A6.6.3 Use with adequate ventilation. A6.7.3 Use with adequate ventilation.
A6.6.4 Avoid breathing vapor or spray mist. A6.7.4 Avoid buildup of vapors and eliminate all sources of
A6.6.5 Avoid prolonged or repeated contact with skin. ignition, especially nonexplosion-proof electrical apparatus
and heaters.
A6.7 Aviation Turbine Fuel (Jet A or A-1, See Specification
D1655) A6.7.5 Avoid breathing vapor or spray mist.
A6.7.1 Keep away from heat, sparks, and open flame. A6.7.6 Avoid prolonged or repeated contact with skin.
A6.7.2 Keep container closed.
APPENDIXES
(Nonmandatory Information)
X1. INSTALLATION, MAINTENANCE, SPECIAL CHECKS
X1.1 Laboratory Installation Requirements X1.3.2 Install a new thermocouple reversing the steps used
X1.1.1 The tester should be placed on a level laboratory to remove old thermocouple. Replace and tighten screws as
bench, allowing a 200 mm to 300 mm wide bench area in front required. The tip of the thermocouple must be flush with top of
of the tester. Ready access to the rear of the tester should be upper fixed bus when position indicator is set at the reference
provided for routine maintenance and service requirements. mark.
Ensure any vents in the instrument cabinet are not obstructed X1.3.3 Check for proper thermocouple indexing under ac-
during installation or use. Adequate ventilation should be tual test operating conditions.
provided, and proper procedures for handling solvents and
X1.4 Heater Tube Temperature Profile (for Models 230
hydrocarbons should be used.
and 240 Only)
X1.2 AutoCal Calibrator Metal Replacement X1.4.1 If it is desired to measure the heater tube temperature
profile, do so after the first hour of the test or before significant
X1.2.1 The tin and lead in the well of the AutoCal Calibra-
∆P occurs. Follow the procedure in the user manual for the
tor must be replaced whenever the quantity is below minimum
particular model.
or when contaminated.
X1.2.2 To remove the metal, install the AutoCal Calibrator X1.5 Flow Rate Check
inverted between the upper fixed bus and the lower floating X1.5.1 Drip Rate Method—Check the flow by observing the
bus. drip from the drip assembly and measuring the time for 20
drops. Models 230 and 240, the time should be 19 s 6 1 s for
X1.2.3 Place a damp paper tissue, cloth rag, or aluminum
20 water drops. Models 230 Mk III, F400, and 230 Mk IV, the
foil under the well to catch the molten metal.
time should be 9 s 6 1 s for 20 fuel drops.
X1.2.4 Apply power to the AutoCal Calibrator as during
X1.5.2 Volumetric Method—Check the flow by measuring
normal calibration, and at same time gently tap the well until
the time it takes to collect 15 mL of fuel in a graduated
all molten metal has dropped out.
cylinder. That time should be between 4 min, 33 s and 5 min,
X1.2.5 Remove and install the AutoCal Calibrator in up- 33 s.
right position and refill with new metal. The proper amount of
X1.5.3 The volumetric method is the referee.
tin for one filling is about 1.5 g to 1.9 g, and for lead about
3.3 g to 4.7 g, or within 1 mm of the top of the cup. NOTE X1.1—Drip rate counts start with zero (drop 0, drop 1, drop 2…
drop 20) to get an accurate measure of the time required for 20 drops.
X1.3 Thermocouple Replacement and Position Adjust- X1.6 Maintenance Manual
ment X1.6.1 A maintenance manual is available that provides
X1.3.1 The thermocouple used for measuring and control- additional maintenance information, such as the electrical
ling the temperature of the heater tube may have to be replaced schematic. Complete details for operating the instrument mod-
at intervals due to damage or failure. els are contained in the user manuals for each instrument.

24
'RZQORDGHGSULQWHGE\
D3241 − 23a´1
X2. DETERMINATION OF BREAKPOINT
X2.1 Definition X2.2 Determination of Breakpoint

X2.1.1 Breakpoint—In Test Method D3241, breakpoint is X2.2.1 The breakpoint can be derived by conducting a
the highest control temperature at which the fuel meets heater series of tests of different control temperatures to arrive at the
tube rating and ∆P specification requirements. temperature, x °C, at which the fuel meets both heater tube
X2.1.1.1 Discussion—This definition of breakpoint de- rating and ∆P specification requirements, and where a test at a
scribes the highest pass temperature for a fuel. Note that some control temperature of (x + 5) °C would result in a fail (that is,
published papers have used the term breakpoint to describe the failure to meet heater tube rating or ∆P requirements). The
lowest fail temperature, which is the (x + 5) °C temperature temperature x °C would then be reported as the Test Method
referred to below. D3241 breakpoint.
SUMMARY OF CHANGES
Subcommittee D02.J0 has identified the location of selected changes to this standard since the last issue
(D3241 – 23) that may impact the use of this standard. (Approved Oct. 1, 2023.)
(1) Revised Table 1 and Table 2. (3) Revised subsection A5.2.8.

(2) Added subsections 7.4 and 7.5.
Subcommittee D02.J0 has identified the location of selected changes to this standard since the last issue
(D3241 – 20c) that may impact the use of this standard. (Approved May 1, 2023.)
(1) Deleted former subsection A2.9 and renumbered subse- (3) Revised Footnote 12 to include new Research Report
quent. RR:D02-2051.
(2) Added subsection A2.11.2.
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/

25
'RZQORDGHGSULQWHGE\

Thermal Oxidation Stability of Aviation Turbine Fuels: Standard Test Method For

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Thermal Oxidation Stability of Aviation Turbine Fuels: Standard Test Method For

Uploaded by

Copyright:

Available Formats

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

Designation: D3241 − 23a´1

Standard Test Method for

ε1 NOTE—Editorially updated A4.11 in January 2024.

1. Scope* mendations issued by the World Trade Organization Technical

*A Summary of Changes section appears at the end of this standard

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

TABLE 1 Instrument Models

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

Heater Tube metallurgy 6061-T6 Aluminum, plus the following criteria

Heater Tube dimensions: Dimension Tolerance

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

A1. TEST METHOD FOR VISUAL RATING OF HEATER TUBES

A1.1 Scope A1.3 Terminology

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

A1.9 Calibration and Standardization

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

FIG. A2.1 Interferometric Apparatus—General Principle

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

FIG. A2.2 Reference Heater Tube

FIG. A2.3 n and k Values of the Heater Tube

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

FIG. A2.4 n and K Values of the Deposit Film

FIG. A2.5 Circumferential Resolution

FIG. A2.6 Standard Spot

of the known thickness. If the determined values are not within

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

FIG. A2.7 Description of Heater Tube Scanned Surface

FIG. A2.8 Reporting Example

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

A3. RATING OF HEATER TUBES—ELLIPSOMETRIC METHOD

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

FIG. A3.1 Ellipsometer NIST Traceable Reference Tube

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

A4. RATING OF HEATER TUBES—MULTI-WAVELENGTH ELLIPSOMETRIC METHOD

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

FIG. A4.1 Multi-Wavelength Ellipsometer Apparatus—General Principle

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

TABLE A4.1 Precision of Deposit Thickness Measurement by

TABLE A4.2 Precision of Deposit Volume Measurement by Multi-

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

FIG. A5.1 Test Section Dimensions

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

FIG. A5.4 Heater Tube and Temperature Control Schematic

FIG. A5.2 Alignment of Heater Tube

FIG. A5.3 Assembly Drawing of Heater Tube Test Section

of the test. This is because a small pressure drop is created

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

A6. WARNING STATEMENTS

A6.1 Acetone A6.4 n-Heptane

A6.2 Toluene A6.5 Compressed Gases (Nitrogen)

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

X1. INSTALLATION, MAINTENANCE, SPECIAL CHECKS

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

X2. DETERMINATION OF BREAKPOINT

X2.1 Definition X2.2 Determination of Breakpoint

(1) Revised Table 1 and Table 2. (3) Revised subsection A5.2.8.

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG 6XQ-DQ*07