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3. Terminology 4.1.1.1 Test Methods have been developed for Fourier-
3.1 For definitions of terms relating to infrared spectroscopy transform infrared (FTIR) devices using absorbance spectra
used in this test method, refer to Terminology E131. For obtained using Practice D7418. Particular Test Methods devel-
definition of terms related to infrared-based in-service fluid oped for in-service monitoring of hydrocarbon type (API
condition monitoring, refer to Practice D7418. Group I-IV) fluids include those established for Oxidation
(Test Method D7414, Procedure A), Antiwear Additive (Test
3.2 Definitions of Terms Specific to This Standard: Method D7412, Procedure A), Sulfation (Test Method D7415,
3.2.1 absorbance units (AU), n—units of measurement of Procedure A), Nitration (Test Method D7624, Procedure A),
the raw absorbance spectrum which is obtained using the and Soot (Test Method D7844, Procedure A). These test
definition described in Section 8 (Theory for a Single Com- methods have served to establish the signature infrared spec-
pound Analysis) of Practice E168, which is not normalized for troscopic behavior associated with key in-service monitoring
pathlength. properties. This test method provides property values based on
3.2.2 cell background, n—a single-beam spectrum that is the examination of each property’s signature infrared spectro-
obtained on a clean, empty wipe-clean transmission cell. scopic behavior. The essence of this test method is to capture
3.2.3 mid-infrared grating spectrometer, n—a spectrometer the underlying chemical trends associated with each property
which operates in the mid-infrared spectral range, between at for in-service fluid analysis using a self-contained field appa-
least 960 cm-1 and 3040 cm-1 and creates an infrared spectrum ratus and coupled wipe-clean transmission cell.
by means of a reflective diffraction grating. 4.1.2 From the infrared absorbance spectrum obtained with
3.2.3.1 Discussion—Such a grating spectrometer may be of the self-contained field apparatus, properties of the in-service
any of a variety of designs and optical configurations. Example fluid are calculated. In particular, those properties in Table 1
designs include monochrometer-type systems wherein the are calculated by the device and presented to the user on the
grating is rotated to a single point infrared detector, or display. Additional properties using infrared calibration meth-
array-type systems which utilize an infrared detector array at ods may be calculated and displayed depending on the particu-
the output and a fixed grating. Example optical configurations lar fluid being analyzed and availability of calibrations for that
include Rowland-Circle and Czerny-Turner systems. Typical fluid.
infrared detectors are uncooled thermal detectors such as 4.1.2.1 Infrared spectra generated by the described instru-
thermopile or pyroelectric-based sensors. ment type can be used to provide a further set of properties of
interest to in-service fluid analysis of hydrocarbon type (API
3.2.4 reporting units, n—specifies the reporting units of the Group I-IV) fluids. Such properties must be calibrated to the
fluid analysis property. particular fluid blend, and may be generated using ASTM
3.2.5 self-contained field apparatus, n—a mid-infrared grat- guidelines which govern the creation of such calibrations. Such
ing spectrometer which is of the form factor to allow it to calibrations may be built from either standard regression
operate as an independent device suitable for field use. methods as described in Practice E168 or as described in
3.2.6 wipe-clean transmission cell, n—an infrared transmis- Practice E2412. Further, they may also be multivariate
sion cell which is specifically tailored for field use. calibrations, described in Practice E1655 and Practice E2617.
3.2.6.1 Discussion—In particular, the cell may be utilized Example properties include Acid Number (AN), Base Number
and cleaned with a towel or rag and without the use of reagents (BN), water contamination, ethylene glycol, fluid mixture
or chemicals of any sort, making it convenient for use as a field content, and antioxidant depletion. It should be noted that, due
device. Such transmission cells may accomplish this using to the fact that these calibrations are sample-specific, this test
mechanisms for quick open/close of the cell such as by means method does not provide a prescription for calculating such
of a mechanical lever, demountable screw or press fit, or properties.
magnetic coupling. To correct for any cell fringing effects, the 4.2 The results of the test method can be compared against
cell utilizes a wedged design both on the interior faces and pre-defined or user-defined limits so as to judge the condition
exterior faces of the cell windows: The cell windows them- of the in-service lubricant. Warning and alarm limits ex-
selves are wedged at an angle of less than 0.5 degrees. The ceedences which may be pre-defined or set by the user are
spacing between the two windows is wedged at an angle of indicated by the property and associated value being high-
approximately 0.013 degrees. The cell is designed to be lighted using coding established in Guide D7720, with either
nominally 100 µm in pathlength, with ZnSe windows. green (favorable alarm level designation showing acceptable
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condition), yellow (intermediate level alarm designation warn- TABLE 2 Specification for Calculation of Each In-Service Fluid
ing a fault condition is present and will likely need attention in Property
the future), or red (high level alarm designation showing Property Measurement, Baseline(s), Reporting
(cm-1) (cm-1) Units
significant deterioration) indicated by the self-contained field Oxidation Average Average Abs/0.1 mm
apparatus. 1800–1670 1815 to 1805
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11.1.2.2 This check is performed before any cell back- 15. Calculation or Interpretation of Results
ground to be used in the calculation of fluid properties is
15.1 Calculation of in-service fluid properties proceeds
obtained, and the user is warned if the check fails.
according to the spectral analysis detailed in Table 2. These
11.1.3 A cell loading check (as described in Practice D7418) analyses proceed using the signature infrared absorption bands
is performed on each loaded sample to ensure that the cell is gleaned from the obtained infrared absorbance spectrum of the
fully loaded. Such a check is performed according to manu- fluid.
facturer’s recommendations.
15.1.1 Properties are obtained from the absorbance spec-
11.1.3.1 If the cell is determined to not be fully loaded, a trum using the measurement and baseline regions listed in
message that the cell is not fully loaded is displayed alongside Table 2. Properties are presented to the user in the reporting
the results of the analysis. It should be noted that due to the units specified.
nature of the design for field use, the wipe clean transmission
15.1.1.1 Oxidation is obtained from calculating the average
cell has no need for fringe correction.
absorbance (Abs/0.1 mm) in the measurement region between
11.2 Ensure that wipe-clean transmission cell is clean by 1800 cm-1 and 1670 cm-1 Abs,av(1800 to 1670) and performing
visual inspection. a weighted subtraction from the average baseline absorbance
11.3 Gather approximately two drops of sample (on the (Abs/0.1 mm) in the region between 1815 cm-1 and 1805 cm-1
order of 50 µL). Abs,av(1815 to 1805). The resulting units of measurement are
11.3.1 This may be accomplished using a dropper, syringe, Abs/0.1 mm:
or simply by using drops from a fluid dipstick, for example. Oxidation=130 · Abs,av~ 1800 to 1670!
2 38.5 · Abs,av~ 1815 to 1805! @ Abs/0.1 mm# (2)
12. Calibration and Standardization
15.1.1.2 Antiwear additive is obtained from calculating the
12.1 A check fluid is supplied with the apparatus as a average absorbance (Abs/0.1 mm) in the measurement region
qualification test. This fluid should be run after each set of 100 between 1025 cm-1 and 960 cm-1 Abs,av(1025 to 960) and
samples to ensure that the unit remains within calibration. performing a weighted subtraction from the average baseline
12.2 If this qualification test fails, the user should follow absorbance (Abs/0.1 mm) in the region between 1060 cm-1 and
manufacturer’s recommendations regarding calibration and 1030 cm-1 Abs,av(1060 to 1030) as well as the region between
standardization. 1812 cm-1 and 1803 cm-1 Abs,av(1812 to 1803). The resulting
units of measurement are Abs/0.1 mm:
13. Conditioning Antiwear Additive 5 65 · Abs,av~ 1025 to 960!
13.1 The field apparatus does not require conditioning nor 2 8.4 · Abs,av~ 1060 to 1030!
does the sample being analyzed. 2 10.8 · Abs,av~ 1812 to 1803! @ Abs/0.1 mm# (3)
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2 0.11 · Abs,av~ 1847 to 1837!! @ Abs/ cm# for the low and high frequency baselines, respectively. This
(5) yields a sulfation value of 11.5 Abs/0.1 mm:
15.1.1.5 Soot is calculated by measuring the absorbance of Sulfation 5 60 · ~ 0.258! 2 11 · ~ 0.285! 2 5 · ~ 0.168!
the sample at 2000 cm-1 (Abs/0.1 mm) and multiplying the 5 11.5 @ Abs/0.1 mm# (8)
result by 100, yielding a result in units of Abs/cm. This allows 15.1.2.4 Nitration Example—Fig. 4 presents a schematic
for numerical results in a typical range of 0-100 Abs/cm. illustration of the calculation for the nitration property. In this
15.1.2 In the following we provide examples for each of the case, the absorbance at 1630 cm-1 is 0.246 Abs/0.1 mm, and the
five (5) properties detailed in 15.1.1: baseline averages are 0.22 Abs/0.1 mm and 0.004 Abs/0.1 mm
15.1.2.1 Oxidation Example—Fig. 1 presents a schematic for the low and high frequency baselines, respectively. This
illustration of the calculation for the oxidation property. In this yields a nitration value of 5 Abs/cm:
case, the average value of absorbance in the oxidation mea-
surement region is approximately 0.1216 Abs/0.1 mm, and the Nitration 5 100 · ~ 0.246 2 0.89 · ~ 0.22! 2 0.11 · ~ 0.004!!
baseline average is -0.005 Abs/0.1 mm. This yields an oxida- 5 5 @ Abs/cm# (9)
tion value of 16 Abs/0.1 mm: 15.1.2.5 Soot Example—Fig. 5 presents a schematic illus-
Oxidation = 130 · ~ 0.1216! 2 38.5 · ~ 2 0.005! 5 16 @ Abs/0.1 mm# tration of the calculation of soot. In this case, the absorbance at
(6) 2000 cm-1 is 0.31 Abs/0.1 mm. Multiplying this value by 100
we obtain a soot value of 31 Abs/cm:
15.1.2.2 Antiwear Additive Example—Fig. 2 presents a
schematic illustration of the calculation for the antiwear Soot 5 100 · ~ 0.31! 5 31 @ Abs/cm# (10)
additive property. In this case, the average value of absorbance 15.1.3 These methods are chosen so as to give the user a
in the antiwear additive measurement region is approximately reported value which does not rely on any spectral reference.
0.385 Abs/0.1 mm, and the baseline averages are 0.298 Abs/0.1 This is in keeping with the apparatus being used as a field tool.
mm and 0.165 Abs/0.1 mm for the low and high frequency 15.1.4 Limits for each particular fluid of interest may be
baselines, respectively. This yields an antiwear additive value tailored considering the typical range of that particular fluid.
of 20.7 Abs/0.1 mm:
Antiwear Additive 5 65 · ~ 0.385! 2 8.4 · ~ 0.298! 2 10.8 · ~ 0.165! 16. Report
5 20.7 @ Abs/0.1 mm# (7) 16.1 Properties are calculated as described in Section 15 and
15.1.2.3 Sulfation Example—Fig. 3 presents a schematic reported in units as described in Table 2.
illustration of the calculation for the sulfation property. In this 16.2 Trending and Alarm Limits—As defined by the user,
case, the average value of absorbance in the sulfation measure- the apparatus will acquire, report, and log the fluid measured
ment region is approximately 0.258 Abs/0.1 mm, and the properties on a periodic basis. The user may monitor this
baseline averages are 0.168 Abs/0.1 mm and 0.285 Abs/0.1 mm trending behavior and as well set alarm limits in the apparatus
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D7889 − 13
for each particular fluid being analyzed. Guidance on perform- 17. Precision and Bias
ing trending analysis and setting alarm limits on in-service
17.1 A temporary precision statement including repeatabil-
lubricants is provided in Guide D7669 and Guide D7720.
ity is reported in Table 3 based on analyzing five samples tested
16.3 Effects of Fluid Formulation—For each measured thirty times each in the same laboratory. Full precision and bias
property, the reported values as well as the trending tendencies statements based on interlaboratory round robin testing will be
are in general different for each fluid type. The apparatus may determined within five years of adoption of this standard
be designed so that each fluid type may be tracked separately method.
with trend histories being viewed and alarm limits set on the
apparatus per these fluid types.
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18. Keywords
18.1 antiwear additives; condition monitoring; direct trend-
ing; field-based devices; grating spectrometers; handheld de-
vices; infrared spectroscopy; in-service fluid analysis; multi-
variate analysis; nitration; oxidation; soot; sulfation
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