ASTM D7417-10

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D7417 − 10
Standard Test Method for
Analysis of In-Service Lubricants Using Particular Four-Part
Integrated Tester (Atomic Emission Spectroscopy, Infrared
Spectroscopy, Viscosity, and Laser Particle Counter)
This standard is issued under the fixed designation D7417; 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.
1. Scope D2896 TestMethodforBaseNumberofPetroleumProducts
by Potentiometric Perchloric Acid Titration
1.1 This test method covers the quantitative analysis of
D4057 Practice for Manual Sampling of Petroleum and
in-service lubricants using an automatic testing device that
Petroleum Products
integrates these varied technologies: atomic emission
D4739 Test Method for Base Number Determination by
spectroscopy, infrared spectroscopy, viscosity, and particle
Potentiometric Hydrochloric Acid Titration
counting.
D6595 Test Method for Determination of Wear Metals and
1.2 This is suited for in-service lubricating oils having
Contaminants in Used Lubricating Oils or Used Hydraulic
viscosities in the range between ISO 10 and ISO 320 and
Fluids by Rotating Disc ElectrodeAtomic Emission Spec-
properties in the ranges given in Tables 1 and 2.
trometry
1.3 Thistestmethodmaybeusedtoestablishtrendsinwear D7042 Test Method for Dynamic Viscosity and Density of
Liquids by Stabinger Viscometer (and the Calculation of
and contamination of in-service lubricants and may not give
equivalent numerical results to current ASTM test methods. Kinematic Viscosity)
E2412 Practice for Condition Monitoring of In-Service Lu-
1.4 This test method is not intended for use with crude oil.
bricants by Trend Analysis Using Fourier Transform
1.5 The values stated in SI units are to be regarded as
Infrared (FT-IR) Spectrometry
standard. No other units of measurement are included in this
2.2 ISO Standards:
standard.
ISO 4406:99 Hydraulic Fluid Power Solid Contaminations
1.6 This standard does not purport to address all of the Code
safety concerns, if any, associated with its use. It is the ISO 11171 Automatic Particle Counter Calibration Proce-
responsibility of the user of this standard to establish appro- dures
priate safety and health practices and determine the applica-
3. Terminology
bility of regulatory limitations prior to use. (Specific hazard
statements are given in Section 9 and 11.3.) 3.1 Definitions:
3.1.1 electrode, n—in an integrated tester, set of two (upper
2. Referenced Documents
and lower) used in excitation of wear metals during emission
spectroscopic testing.
2.1 ASTM Standards:
D445 Test Method for Kinematic Viscosity of Transparent
3.1.2 emission spectrometer, n—component used to report
and Opaque Liquids (and Calculation of Dynamic Viscos-
elements in parts per million in lubricants. This process
ity)
measures 20 different wear/additive metals that can be present
D2270 Practice for Calculating Viscosity Index from Kine-
in the used lubricant after the oil has been in service for a
matic Viscosity at 40 °C and 100 °C
period of time. Test Method D6595 can be used for reference
or definition.
This test method is under the jurisdiction of ASTM Committee D02 on
3.1.3 infrared spectrometer, n—component used to report
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
condition and contamination of the lubricant (for example,
Subcommittee D02.96.07 on Integrated Testers, Instrumentation Techniques for
water, oxidation, fuel dilution (gasoline and diesel), nitration,
In-Service Lubricants.
glycol, soot, calculated viscosity, and base number). Practice
Current edition approved Oct. 1, 2010. Published November 2010. DOI:
10.1520/D7417-10.
E2412 can be used for reference or definition.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
the ASTM website. 4th Floor, New York, NY 10036, http://www.ansi.org.
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D7417 − 10
TABLE 1 Element Test Parameters Measured, Calculated, and Reported
Element Low Range, mg/kg High Range, mg/kg Element Low Range, mg/kg High Range, mg/kg
Aluminum 5 to 100 NA Molybdenum 10 to 1000 NA
Barium 25 to 150 150 to 2000 Nickel 5 to 100 NA
Boron 5 to 100 100 to 1000 Phosphorous 100 to 600 600 to 4000
Calcium 25 to 500 500 to 9000 Potassium 10 to 1000 1000 to 4000
Chromium 8 to 100 NA Silicon 5 to 150 150 to 3000
Copper 5 to 500 500 to 1000 Sodium 10 to 1000 NA
Iron 6 to 1000 1000 to 3000 Tin 6 to 100 NA
Lead 6 to 150 NA Titanium 8 to 100 NA
Magnesium 5 to 100 100 to 3000 Vanadium 7 to 100 NA
Manganese 5 to 100 NA Zinc 8 to 100 100 to 4000
TABLE 2 Physical Properties Parameters Measured, Calculated, and Reported
NOTE 1—Review Test Method D4739 and D2896 for particular lubricating oil applications.
Physical Property Range
Water, wt% 0.1to3
Glycol, wt% 0.1to2
Soot, wt% 0.1to4
Fuel Dilution, wt% 0.1 to 15
Oxidation, abs. 0.1 to 50
Nitration, abs. 0.1to35
Calculated Viscosity - IR 4 to 35 (100° cSt)
Viscosity 40°C, cSt (optional) 30 to 320
Viscosity 100°C, cSt (optional) 5 to 25
Viscosity Index 5to150
Base Number, mg KOH/g 1.0 to 17
3.1.4 integrated tester, n—instrument used to analyze in- 3.2.1 electrode gap, n—in an integrated tester, specific
service lubricants for maintenance, preventative maintenance distance between the upper and lower electrodes in the spark
and service recommendations. This instrument utilizes any chamber.
combination of the following: emission spectrometer, infrared
3.2.2 particle counter, n—component in this particular inte-
device, viscometer, and particle counter.
grated tester that is used to count particles using laser and
3.1.5 sample transport system, n—in an integrated tester, high-resolution digital counter reporting in 4 µm(c), 6 µm(c),
computer controlled assembly that directs the oil samples 14 µm(c) or 2 µm, 5 µm, 15 µm, using ISO 11171 calibration
throughout the integrated tester. method and or ISO 4406:99 reporting method.
3.1.6 spark chamber, n—in an integrated tester, area hous- 3.2.3 sanitized cleaning swabs, n—in an integrated tester,
ing the upper and lower electrodes for emission spectrometer. used to clean the electrodes after each sample analysis.
3.1.7 viscometer, n—in an integrated tester, a viscometer
3.3 Abbreviations:
using calibrated measurements similar to a kinematic viscom-
AES = Atomic Emission Spectroscopy
eter capable of reporting viscosity at 40°C or 100°C in
IR = Infrared
centistokes (cSt), and providing a calculated viscosity index.
OEM = Original Equipment Manufacturer
The results are also used to determine fuel dilution in diesel
lubricants. Reference toTest MethodD445, Practice D2270,or
4. Summary of Test Method
Test Method D7042 can be used as a reference for viscosity
4.1 Asampleofin-servicelubricantiscollectedintoaclean,
definition. Although the integrated tester does not print out SI
new 120 mL sample bottle from the equipment being tested,
units for measuring viscosity, reporting in mm /s can be
preferably within 30 min of equipment shutdown. Lubricant
determined.
description and service information should be recorded for
3.2 Definitions of Terms Specific to This Standard:
properevaluation.Theintegratedtesterispreparedforanalysis
according to the operations manual and on-screen prompts.
4 Thelubricantsampleisplacedintothesampletransportsystem
The sole source of supply of the apparatus (OSA Lab Four Part Analyzer and
and is analyzed using available integrated devices. The appli-
accessories) known to the committee at this time is On-Site Analysis, Inc., 7108
Fairway Drive, Suite 130, Palm Beach Gardens, FL 33418 (manufacturing division
cation software guides the entire procedure, controls the
in Marlborough, MA), www.on-siteanalysis.com. If you are aware of alternative
transfer of the sample, stores data, and generates on screen and
suppliers, please provide this information to ASTM International Headquarters.
printed results with a printed generic recommendation of the
Your comments will receive careful consideration at a meeting of the responsible
technical committee, which you may attend. lubricant’s physical condition.
D7417 − 10
5. Significance and Use 8. Reagents and Materials
8.1 The particular integrated tester uses the following sup-
5.1 Theintegratedtesterisprimarilyusedtoperformon-site
plies which are available from the manufacturer to ensure
analysis of in-service lubricants used in the automotive, high-
accurate operation of the integrated tester:
way trucking, mining, construction, off-road “mining,” marine,
8.1.1 Electrodes—A high-purity silver electrode set (upper
industrial, power generation, agriculture, and manufacturing
and lower).
industries.
8.1.2 Cleaning Fluid—An environmentally safe mineral oil,
5.2 The immediate results of analysis of in-service lubri-
to clean the instruments internal flow system. The cleaning
cants are critical when performing proactive and preventative
solution in most cases can also be used as the base oil for the
maintenance. On-site oil analysis, when used in conjunction
calibration of the instrument. This product is a nonflammable
withtheseprograms,allowscontinuoussystemmonitoringand
product consisting of technical grade Semtol White Mineral
contamination control potentially improving equipment “up- 5
Oil.
time” and equipment life.
8.1.3 Test Standard—This solution is intended for use as a
calibration standard for the integrated tester. It is a multi-
6. Interferences 6
element solution of Primol N352 that was prepared with
neutral oil as a functional antioxidant for specific concentra-
6.1 Sample Size—Using less than the required 130 mL of
tions. The certified concentrations are based upon the assayed
sample for the analysis may result in erroneous numbers.
concentrations of the raw materials and the gravimetric proce-
6.2 High Concentration—Of a contaminant such as water
dures used to prepare the final standard. The uncertainty
and or soot in the IR device might cause other parameters to be
associatedwitheachcertifiedconcentrationis 62mg/kg(parts
blocked out in the IR band resulting in a default returned value
per million). In order to verify these certified values, the final
of not applicable or “n/a” for these other parameters.
solution was analyzed by plasma emission spectroscopy (ICP).
NOTE 1—The manufacturer guarantees the accuracy of this solution
7. Apparatus
until the expiration date shown, provided it is kept tightly capped and
7.1 Integrated Tester—The particular integrated tester will stored in original bottle under normal laboratory conditions. Do not
refrigerate or store in direct sunlight. Minimize exposure to moisture or
incorporate two or more of the following sensors: an emission
high humidity. It is recommended that the solution be thoroughly mixed,
spectrometer, an infrared device, a viscometer, or a particle
by shaking the bottle, prior to use.
counter.
8.1.4 High Viscosity Fluid—For use with viscometer only.
7.2 Emission Spectrometer—Consists of an excitation
This fluid is blended with known viscosities and is periodically
source, spark stand, and optical system.
analyzedtoconfirmcalibrationortorecalibratetheviscometer.
It consists of a highly refined mineral oil and a detergent/
7.3 Infrared Device—Consists of an infrared source, sample
dispersant engine oil additive package.
cell, and optical system.
8.1.5 Low Viscosity Fluid—For use with viscometer only.
7.4 Dual Temperature Viscometer—Consists of a tempera-
This fluid is blended with known viscosities and is periodically
ture controlled sample reservoir and electronic control system.
analyzedtoconfirmcalibrationortorecalibratetheviscometer.
It consists of a highly refined mineral oil and a detergent/
7.5 Particle Counter—Consists of a sophisticated sensor
dispersant engine oil additive package.
cellusingredlaserlightextinctiontechnologyutilizingtheISO
8.1.6 Reference Oil—Used to verify accuracy of physical
11171 calibration and ISO 4406:99 reporting.
property test results reported by infrared device. The reference
7.6 Sample Container—Sample container of no less than
oil has known physical properties which are tested against the
118 mL that is free of contaminants shall be used for the
infrared device using the software to determine standardiza-
in-service oil samples and shall be discarded after use. The
tion. It consists of a highly refined mineral oil combined with
maximumdimensionsof10.8cmhigh,8.9cmindiameter,and
zinc alkyl dithiophosphate.
an opening of no less than 1.6 cm shall be used.
8.1.7 Sanitary Cleaning Swabs—Used to clean the elec-
trodes after each sample analysis. Operator shall use contami-
7.7 Sonic Bath—Water-filled, vibrating tool used to be sure
nant free cotton swabs that are not treated with sodium from
that all of the contamination is in suspension in the lubricant
the hypochlorite bleaching process. Check the manufacturer’s
sample.This is mostly used when preparing a lubricant sample
for a particle count analysis procedure.
7.8 Computer Application Software and Operations 5
The sole source of supply of the apparatus known to the committee at this time
is Sonneborn, Inc., 771 Old Saw Mill River Rd.,Tarrytown, NY10591-6716. If you
Manual—The computer application software provides the
are aware of alternative suppliers, please provide this information to ASTM
functionality for the particular integrated tester; an electronic
International Headquarters. Your comments will receive careful consideration at a
user with help screens and a condensed reference manual for 1
meeting of the responsible technical committee, which you may attend.
quick reference, interface, hierarchical equipment database to
The sole source of supply of the apparatus known to the committee at this time
is ExxonMobil (Corporate Headquarters), 5959 Las Colinas Blvd., Irving, TX
store, analyze and manage data, embedded logic for data
75039-2298. If you are aware of alternative suppliers, please provide this informa-
interpretation; and automatic reporting tools. A complete op-
tion to ASTM International Headquarters. Your comments will receive careful
erations manual and troubleshooting guide accompany the
consideration at a meeting of the responsible technical committee, which you may
software application. at
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