Astm D7843 - 21
Astm D7843 - 21
Astm D7843 - 21
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D7843 − 21
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D7843 − 21
wiping with a clean, dry, soft, lint-free wiping material and is Analytical Reagents of the American Chemical Society3 where
resistant to saturated solvents. Its color may vary, but it usually such specifications are available. Other grades may be used,
appears in gray, brown, or amber hues. provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
4. Summary of Test Method the determination.
4.1 Insoluble deposits are extracted from an in-service 8. Sampling, Test Specimens, and Test Units
turbine oil sample using a 47 mm, 0.45 µm membrane nitro-
cellulose patch. The color of the patch is then analyzed using 8.1 Using either Practice D4057 (manual sampling) or
a spectrophotometer and the results are reported as a ∆E value Practice D4177 (automatic sampling), obtain a representative
in the CIELAB scale. sample of at least 60 mL of the material to be tested.
NOTE 1—The sample container used shall preclude exposure to UV
light as oil is known to be sensitive to both indoor and outdoor sources.
5. Significance and Use Fluorescent light is known to contain UV components and has been shown
5.1 This test can be a guide to end-users on the formation of to increase deposit levels. This exposure can occur upon drawing of the
sample as well as during incubation period. Wide-mouth laboratory
lubricant-generated, insoluble deposits. quality amber high-density polyethylene (HDPE) bottles have been shown
5.2 The results from this test are intended to be used as a to protect the oil sample from UV light exposure. Other translucent or
clear sample bottles are acceptable for use provided that the sample bottle,
condition monitoring trending tool as part of a comprehensive
upon drawing of the sample and throughout the heating/incubation
program, as outlined in standards such as Practice D4378. process, is immediately placed and stored into packaging or a storage unit
that blocks light. Cylindrical cardboard packaging containers meet this
6. Apparatus intent.
6.1 Variations of apparatus, particularly with respect to filter 8.2 The sample shall be heated to 60 °C to 65 °C for 23 h to
membranes and vacuum pump setting, can affect the test 25 h then stored between 15 °C to 25 °C, away from UV light
results significantly. for an incubation period of 68 h to 76 h. Samples that are
analyzed prior to this aging period may produce fewer color
6.2 When the user of this test method uses an alternate bodies on the patch; thus, producing a lower ∆E value, and
membrane filter, it is incumbent upon them to establish that the may lower the value of trend analysis.
alternate filter will give equal results. NOTE 2—Samples can be analyzed in longer or shorter intervals with
6.3 Required Apparatus: agreement of the end-user. The level of deposit and as a consequence, the
test results may be affected by time duration chosen. It is sometimes
6.3.1 Membrane Filter, 47 mm nitro-cellulose, 0.45 µm. suggested to additionally analyze the sample at multiple incubation
6.3.2 Forceps, smooth-tip. periods to fully understand the operating system.
6.3.3 Borosilicate Filter Holder.
6.3.4 Borosilicate Filtering Flask. 9. Procedure
6.3.5 Wash Bottle equipped with 0.22 µm membranes. 9.1 Preparation of Sample and Materials:
6.3.6 Vacuum Source, capable of maintaining a vacuum of 9.1.1 Document the date and time at the beginning of the
71 kPa 6 5 kPa. test.
6.3.7 Graduated cylinder, 150 mL to 200 mL. 9.1.2 Vigorously mix the sample for 15 s minimum to
6.3.8 Beaker, 100 mL to 250 mL. resuspend insolubles uniformly. Visually inspect the inside of
6.3.9 Petri dish. the bottle for evidence of material adherent to the surface of the
6.3.10 Spectrophotometer, with capabilities of analyzing a bottle before sampling.
standard 15 mm target with a 0°/45° measuring geometry, 10° NOTE 3—If adherent material cannot be removed from bottle after
observer, 10 nm spectral intervals minimum resolution, the repeated attempts to vigorously mix, include as comment in the reporting
visible spectral range of 400 nm to 700 nm and CIELAB documentation.
measuring indices. 9.1.3 Transfer 50 mL 6 1 mL of sample into clean beaker or
Erlenmeyer flask.
7. Reagents and Materials 9.1.4 Add approximately 50 mL 6 1 mL of petroleum ether
7.1 Petroleum Spirit (also known as petroleum ether or IP to beaker containing sample.
Petroleum Spirit 40/60) (Warning—Extremely flammable. 9.1.5 Stir sample for approximately 30 s to ensure that a
Harmful if inhaled. Vapors are easily ignited by electrostatic complete solution (and complete mixing) is attained.
discharges, causing flash fire.), having boiling range from 9.1.6 Pour sample into filter funnel within 1 min to 2 min of
35 °C to 60 °C. initial mixing.
7.2 Coleman Camp Fuel—Coleman Fuel is a complex 9.2 Filtration Process:
mixture of light hydrocarbons (primarily aliphatic) produced
by distillation of petroleum. Carbon number range is C5 to C9, 3
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
and contains less than 0.001 % benzene. Standard-Grade Reference Materials, American Chemical Society, Washington,
DC. For suggestions on the testing of reagents not listed by the American Chemical
7.3 Purity of Reagents—Reagent grade chemicals shall be
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
used in all tests. Unless otherwise indicated, it is intended that U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
all reagents conform to the specifications of the Committee of copeial Convention, Inc. (USPC), Rockville, MD.
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TABLE 1 72 h (3 day)
Repeatability Reproducibility
Repeatability Reproducibility
Material Average Standard Standard
Limit Limit
Deviation Deviation
x̄ sr sR r R
Sample 1 15.332 0.861 3.169 2.410 8.874
Sample 2 7.409 0.910 2.830 2.547 7.925
Sample 3 6.970 0.839 3.085 2.349 8.637
Sample 4 3.472 0.468 2.047 1.309 5.732
Sample 5 6.993 0.852 2.968 2.386 8.309
Sample 6 34.258 3.656 11.556 10.236 32.357
Sample 7 3.475 0.176 1.647 0.494 4.611
9.2.1 Using forceps, mount the filter on the center of the b* 5 200@ ~ Y ⁄ Y n ! 1⁄3 2 ~ Z ⁄ Z n ! 1⁄3 # (3)
filter holder. X⁄X n ; Y⁄Y n ; Z⁄Z n .0.01 (4)
9.2.2 Mount and securely clamp the filter funnel to the filter.
9.2.3 Apply a vacuum and ensure a vacuum of less than The tristimulus values Xn, Yn, Zn define the color of the
76 kPa is attained and held. normally white object-color stimulus, in this case the new
9.2.4 Rinse the beaker twice with a minimum of 35 mL of membrane patch. Under these conditions, Xn, Yn, and Zn are the
petroleum ether and pour the rinsing into the filter funnel. tristimulus values of the standard 10° observer, D65 illuminant.
9.2.5 Permit the filtrate to completely flow through. 10.1.1 The total difference ∆E*ab between two colors each
9.2.6 Carefully, remove the clamp and funnel. Wash any given in terms of L*, a*, b* is calculated as follows:
adhering insolubles from the funnel onto the membrane with ∆E* ab 5 @ ~ ∆ L * ! 2 1 ~ ∆ a * ! 2 1 ~ ∆ b * ! 2 # 1⁄2 (5)
petroleum ether. Wash the membrane gently, particularly the 10.2 Reporting:
edges, with petroleum ether from the wash bottle. 10.2.1 Report the spectrophotometer CIELAB ∆E values to
NOTE 4—If any of the deposits fails to remain on (or falls off) the dry one decimal place.
membrane the test must be repeated. 10.2.2 The incubation after heating shall be reported with
9.2.7 Carefully release the vacuum. the ∆E value.
9.2.8 Remove the clamp and filter holder. 10.2.3 Note in the reporting documentation any deviation
9.2.9 Using forceps carefully remove the filter from the from this Standard’s methodology.
filter holder and place into a clean dry petri-dish. To facilitate
handling, the membrane filters might be rested on clean glass 11. Precision and Bias4
rods in the petri-dish. 11.1 The precision of this test method is based on an
9.2.10 Dry the membrane by placing it in a low-level heat interlaboratory study conducted in 2011. Twelve laboratories
source free of ignition sources for flammable vapors, or air dry participated in the study, testing seven different turbine oils,
(typically, 3 h) in a dust-free location. Dryness can be esti- over three and five day periods. Every analyst was instructed to
mated by comparing the white color of the outer edge of the report duplicate test results in this study. Practice E691 was
test membrane with a new membrane. followed for the study design; the details are given in ASTM
9.3 Color Determination of the Membrane Patch: Research Report RR:D02-1752.
9.3.1 Standardize the instrument using a patch developed 11.1.1 Repeatability limit (r)—Two test results obtained
from clean solvent application of the method to establish the within one laboratory shall be judged not equivalent if they
background color white. differ by more than the “r” value for that material; “r” is the
9.3.2 Follow the standardization procedure defined by the interval representing the critical difference between two test
instrument manufacturer. results for the same point, obtained by the same operator using
9.3.3 Analyze the patch as recommended by the instrument the same equipment on the same day in the same laboratory.
manufacturer. 11.1.1.1 Repeatability limits are listed in Tables 1 and 2.
9.3.4 Analyze the color of the patch in accordance with the 11.1.2 Reproducibility limit (R)—Two test results shall be
equipment manufacturer’s instructions to produce a CIELAB judged not equivalent if they differ by more than the “R” value
value. for that material; “R” is the interval representing the critical
difference between two test results for the same point, obtained
10. Calculation of Results by different operators using different equipment in different
laboratories.
10.1 CIE 1976 L* a* b* Uniform Color Space and Color-
11.1.2.1 Reproducibility limits are listed in Tables 1 and 2.
Difference Equation—This is an approximately uniform color
11.1.3 The above terms (repeatability limit and reproduc-
space System defined by Practice E308. It is produced by
ibility limit) are used as specified in Practice E177.
plotting in rectangular coordinates the quantities L*, a*, b*,
calculated as follows:
4
L* 5 116* ~ Y ⁄ Y n ! 1⁄3 2 16 (1) Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1752. Contact ASTM Customer
a* 5 500@ ~ X ⁄ X n ! 1⁄3 2 ~ Y ⁄ Y n ! 1⁄3 # (2) Service at [email protected].
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TABLE 2 120 h (5 day)
Repeatability Reproducibility
Repeatability Reproducibility
Material Average Standard Standard
Limit Limit
Deviation Deviation
x̄ sr sR r R
Sample 1 17.125 1.530 4.287 4.284 12.004
Sample 2 7.618 0.715 2.919 2.003 8.174
Sample 3 7.473 0.710 3.000 1.989 8.401
Sample 4 3.584 0.519 1.872 1.452 5.242
Sample 5 7.883 0.620 3.132 1.736 8.770
Sample 6 38.615 4.889 12.300 13.690 34.439
Sample 7 3.867 0.437 1.568 1.223 4.392
11.1.4 Any judgment in accordance with statements 9.1.1 Sample 3: 2011Sept-3, 3 day heating experiment – for the 3 day wait
and 9.1.2 would have an approximate 95 % probability of after heating + 2011Sept-3, 5 day heating experiment – for the 5 day
wait after heating
being correct.
11.2 Bias—At the time of the study, there was no accepted Sample 4: 2011Sept-4, 3 day heating experiment – for the 3 day wait
after heating + 2011Sept-4, 5 day heating experiment – for the 5 day
reference material suitable for determining the bias for this test wait after heating
method, therefore no statement on bias is being made.
Sample 5: 2011Sept-5, 3 day heating experiment – for the 3 day wait
11.3 The precision statement was determined through sta- after heating + 2011Sept-5, 5 day heating experiment – for the 5 day
tistical examination of 312 test results, from a total of twelve wait after heating
laboratories, on seven turbine oils. The seven materials were Sample 6: 2011Sept-6, 3 day heating experiment – for the 3 day wait
described as: after heating + 2011Sept-6, 5 day heating experiment – for the 5 day
wait after heating
Sample 1: 2011Sept-1, 3 day heating experiment – for the 3 day wait
after heating + 2011Sept-1, 5 day heating experiment – for the 5 day
Sample 7: 2011Sept-7, 3 day heating experiment – for the 3 day wait
wait after heating
after heating + 2011Sept-7, 5 day heating experiment – for the 5 day
wait after heating
Sample 2: 2011Sept-2, 3 day heating experiment – for the 3 day wait
after heating + 2011Sept-2, 5 day heating experiment – for the 5 day
wait after heating
12. Keywords
12.1 membrane patch colorimetry; turbine oil; varnish
APPENDIXES
(Nonmandatory Information)
X1.1 In turbine lube oils, thermo-oxidative degradation is not black soot. These parameters, sometimes combined as
the predominant breakdown pathway and often yields amber- MPC (a*+b*), can therefore be used to distinguish amber-
brown color bodies indicative of an increased potential for brown patches which have a high ∆E value as a result of
varnish-formation. In phosphate esters, amber-brown varnish varnish from black patches which have a high ∆E value due to
can be formed by thermo-oxidative breakdown or hydrolysis, soot or other high-temperature breakdown products.
or both. Because of the stresses inherent to hydraulic control
fluid applications, phosphate esters also tend to form black X1.3 The total difference ∆(a*+b*) between the obtained a*
insoluble color bodies (soot) as a consequence of microdiesel- and b* values of the isolated insoluble color bodies and the
ing or other high-temperature breakdown pathways. The pres- blank filter membrane is calculated as follows:
ence of soot is not necessarily indicative of an elevated
∆ ~ a * 1 b * ! 5 @ ~ a * final 2 a * blank! # 1 @ ~ b * final 2 b * blank! #
potential for varnish formation; however, these insolubles may
(X1.1)
lead to other operational concerns.
X1.2 Both amber-brown varnish and black soot will lead to X1.4 The mass of the color bodies (varnish, soot, etc.)
elevated ∆E measurements indicative of poor EHC fluid captured by a membrane filter patch, colloquially referred to as
condition; however, the latter does not necessarily indicate that “patch weight,” can also provide a useful tool for their
an EHC fluid possesses a high potential for varnishing. Caution quantification in in-service turbine control oils. Although this
is therefore advised when evaluating an EHC fluid’s “varnish standard does not provide guidance relating to patch weight
potential” based solely on its ∆E value. Most spectrophotom- measurement, this information can be found in other standards
eters used to measure MPC ∆E also measure and report MPC including, but not limited to: Test Methods D4898, D5452, and
a* and b*. Colorimetrically, positive MPC a* (red) and b* D7317. Users who wish to evaluate MPC “patch weight” are
(yellow) values are characteristic of amber-brown varnish but advised to consult these standards for guidance.
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X1.5 Since the identity and quantity of the insoluble color test provider report patch weight and ∆(a*+b*) in addition to
bodies that have been captured on an MPC filter patch has ∆E. It is best lab practice to record MPC patch weight,
important implications on equipment performance, reliability, ∆(a*+b*) and ∆E for trending purposes regardless of whether
and maintenance, end users may wish to request that their MPC or not this information has been requested by an end user.
X2.1 Several examples of the deposits observed on mem- “patch weights” are reflective of higher insoluble color body
brane filter patches obtained from in-service EHC fluids in levels in the relevant test fluid.
addition to recommended interpretations are shown in Table
X2.1. For all of the membrane filter patches shown, higher
TABLE X2.1 Types of Deposits on Membrane Filters obtained from In-service EHC Fluids
NOTE 1—The images within Table X2.1 show general examples only. Complete oil analysis must be performed to determine the cause of membrane
patch color and to characterize fluid degradation products.
Black patch indicates the presence of soot. Brown patch indicates the presence of thermal degradation
Characterized by high ∆E value with little ∆(a*+b*) contribution. products associated with varnish.
Characterized by high ∆E value with a significant ∆(a*+b*) contribution.
RELATED MATERIAL
Sasaki, A., et al., “Investigation of Oil Contamination by Colorimetric ASTM International Paper ID: JAI100465, January 2007.
Analysis” STLE/ASM Tribology Conference, San Francisco, CA, June Hobbs, M. and Dufresne, P., “Improved Phosphate Ester Condition
2001. Monitoring using Membrane Patch Colorimetry” Symposium High-
Livingstone, G., Thompson, B., and Okazaki, M., “Physical, Performance lighting Standard Guides and Practices that Support the Lubricant
and Chemical Changes in Turbine Oils from Oxidation,” Journal of Condition Monitoring Industry, December 2020.
SUMMARY OF CHANGES
Subcommittee D02.C0 has identified the location of selected changes to this standard since the last issue
(D7843 – 18) that may impact the use of this standard. (Approved April 1, 2021.)
(1) Addition of Test Methods D4898, D5452, and D7317 to (3) Addition of Appendix X1 and Appendix X2.
Section 2 Referenced Documents. (4) Addition of Hobbs reference to Related Material.
(2) Addition of “soot” to Section 3 Terminology.
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