by: Digital Copper Corrosion Measurement Vs. Visual Rating _ Incorporating New Technologies To Method Development Aaron Mendez Ph.D. and Juan Ayala Ayalytical Instruments Inc. 2787 W Fulton St, Chicago, IL 60612 USA www.ayalytical.com Galveston, TX October 16 - 17, 2018
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Digital Copper Corrosion Measurement Vs. Visual Rating _ Incorporating New Technologies To Method Development
Aaron Mendez Ph.D. and Juan Ayala Ayalytical Instruments Inc.2787 W Fulton St, Chicago, IL 60612 USAwww.ayalytical.com
ASTM D130• Corrosiveness to Copper from Petroleum Products by Copper Strip Test
A polished copper strip is immersed in a specific volumeof the sample being tested and heated under conditions oftemperature and time that are specific to the class of materialbeing tested. At the end of the heating period, the copper stripis removed, washed and the color and tarnish level assessedagainst the ASTM Copper Strip Corrosion Standard.
*
*Claret Red
Multicolor Lavender or silver or both overlaid on claret red
Multicolor red and green showing peacock, but not gray
Magenta overcast on brassy strip
Moderate Tarnish Dark Tarnish CorrosionSlight Tarnish
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Reasons for Development• One of the last…
• Remove BIAS from Operator to Operator
• Digital Recording of Images
• LIMS Integration
• Standardization on Light Source
• Magnification of Sample Strip
• Strip Size Determination
• Current Chart – NOT REAL
• Fixed corrosion criteria
• Automatic Measurement…Not assessment
• More reliable
• Repeatable and Reproducible
• A better rating…
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THE DESIGN
*Patent Pending
Digital High Resolution CCD Camera
NFX Strip Holder*
Pogo Pin Connectors
Spring LoadedStrip Holder
D130 Copper Test StripCuDDI Analyzer*
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Vision Algorithm
• Define Strip Area – Automatically
• Inspection Area Determination
• 8x8 Pixel scan, ~96,000 points total
• Accumulate Results
• Calculate Percentage of each Rating
• Pass values through Support Vector Machine and Algorithm for Categorizing
• Ability to “Train” and Adopt Model
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• Lighting
• Fingerprints
• Dimensions
• Proper Polishing
• Holes in D1838
• Water Spots – LPG Samples
• 2a to 3a Logic Handling
• 2c to 3b Logic Handling
D130 Critical Points
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WK62219 Revision of D130-18Revision of D130 - 12 Standard Test Method for Corrosiveness to Copper from Petroleum Products by Copper Strip Test
Rationale:D130-18 is the standard method for the determination of the degree of corrosiveness ofpetroleum products with a vapor pressure up to 124kPa (37.8 °C), such as natural,automotive and aviation gasoline, aviation turbine fuel, kerosene, diesel fuel, distillate fueloil, cleaners solvent (Stoddard), lubricant oils and other hydrocarbon fractions fallingwithin the specified vapor pressure limit. A polished copper strip is immersed and heatedfor a determined time in a predetermined volume of the sample under test. Heatingconditions and time of exposure are specific of the class of material being tested. After theheating, the strip is removed washed and the degree of corrosiveness of the sample isassessed by visual comparison of the level of tarnish and color against an appropriateASTM Copper Strip Corrosion Standard. The proposed revision improves the rating processby a Digital Detection Imaging analyzer removing the subjective visual rating of D130,strictly adhering the classification specified in Table 1. Exact levels of corrosion are digitallyand integrally identified in a 4-step automated vision algorithm process using a high-resolution CCD camera with optical intelligence.
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BALLOT ITEM D02.05 (18-04)
WK #62219 Revision of D130-18
Date: 05/07/2018
To: Subcommittee D.02.05 on Properties of Fuels, Petroleum Coke and Carbon Material
D7960-17Unleaded Aviation Gasoline Test Fuels containing non-hydrocarbon components
D8011-17Natural Gasoline as a Blend Stock in Ethanol Fuel Blends or as a Denaturant for Fuel Ethanol
D8076-18 100 RON Test Fuels for Automotive Spark-Ignition Engines
Table X. Product span for D130-18
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D130-18 Precision Statement
Results by this test method are nonnumerical and involve multi-categoric rating classifications therefore conventional D02 statistical techniques, such as Practice D6300, are not suitable for determining precision.Instead, a statistical simulation approach was used to mathematically assess the “degree of disagreement” under “r” and “R” conditions for the ILS data set. Based on the statistical approach followed, no statistically significant difference in disagreement percentages between r and R conditions was determined for rating classifications in category 1, 2, and 3. For rating classification 4 however, samples showed more within-classification disagreement.Based on this information, the statistician determined that in the long run, the precision of the analysis (that is, both “r” and “R”) is that there is nominally a 5% chance that a difference between any two ratings will exceed the criteria in D130 Table 2.
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D130-18 Revision Plan
D6708-16b _ Standard Practice for Statistical Assessment and Improvement of Expected Agreement Between Two Test Methods that Purport to Measure the Same Property of a Material
• The interlaboratory study must be conducted on at least ten materials that span the intersecting scopes (See Table X) of the test methods and results must be obtained from at least six laboratories using each method.
• Similar cases were automatic procedures with its own precision were added to the standard, specifically D1322-18_ Smoke Point and D3241_ Thermal Oxidation Stability of Jet Fuels (JFTOT).
• A common set of representative coupons previously rated according to D130 can be circulated among cooperators to determine the automatic rating. The minimum number of samples and the degrees of freedom involved is something that must be determined with ASTM D02.94 statisticians.
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CONCLUSIONS
• CuDDI possesses a tight controlled analyzer that guarantees high consistency
• High resolution CCD camera provides precise machining and motors to reproducibly rotate the strip
• The novel Pongo Holder eliminates unwanted markings that might affect the measurement
• Ratings proceed by accurately measuring the degree of corrosion eliminatingoperator bias in the visual subjective assessment
• Low data dispersion between tests and operators/instruments
• CuDDI presents unique advantages in avoiding distortions aroundfringing areas and in determining the real copper strip size
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CONCLUSIONS
• In the case of pass/fail data, no generally accepted method for determining precision is currently available, except for gasoline sample types (see D130-18, 14.1.1 and 14.1.2) analyzed using the test tube procedure stated in D130-18 11.3.1.
• Bias has not been determined for this test method.
• A full fledged Round Robin Study covering all types of fuels is being prepared before resubmitting this work item for approval.