LAB-X5000 AppNote 15 - Lubricating Oils (D6481 and D7751)

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APPLICATION NOTE - 15

LAB-X5000
LAB-X5000 for the rapid
analysis of lubricating oil to
ASTM D6481 and D7751
INTRODUCTION
Lubricating oils are a blend of highly refined base oils and chemical
additives. The additives impart the final product properties to
meet specific requirements, and can be antioxidants, corrosion
inhibitors, anti-foam agents, detergents/dispersants etc. Additive
packages combine several additives that work together to perform
desired tasks.
To ensure product quality, it is necessary to monitor the content of additive
elements such as phosphorus (P), sulfur (S), calcium (Ca) and zinc (Zn) in the
additive packages and in the end lubricating oil at the manufacturing/blending
location.

X-ray fluorescence (XRF) spectrometry is one of the simplest instrumental


techniques for oil analysis because the sample preparation is simple, and the
analysis is fast. For many years, benchtop energy-dispersive XRF (EDXRF)
spectrometers have been used successfully as a quality control tool to analyse the
additives packages as well as the final blended oil. Hitachi High-Tech have a long
and highly respected reputation within the lubricating oil industry with instruments
such as the Lab-X3000 series, Twin-X and X-Supreme providing simple to use,
accurate, cost-eff ective and dependable 24/7 analysis.

MEETING ASTM D6481 AND D7751 REQUIREMENTS


Now Hitachi High-Tech’s LAB-X5000 EDXRF analyser includes the latest detector
technology to deliver the high performance needed for the stringent quality control
of lubricating oils. The pre-loaded calibration parameters have been optimised to
ensure that the LAB-X meets and even surpasses the performance requirements
of standard test method ASTM D6481 (Standard Test Method for Determination
of Phosphorus, Sulfur, Calcium, and Zinc in Lubrication Oils by EDXRF), and also
fully conforms with D7751 (Standard Test Method for Determination of Additive
Elements in Lubricating Oils by EDXRF Analysis).

LUBRICATING OIL ANALYSIS MADE EASY


With the LAB-X5000, the analysis of additives packages and lubricating oils
couldn’t be easier. Routine analysis is carried out by pouring the oil into a
sample cup, placing the cup in the LAB-X’s analysis port, and pressing a button
to start the measurement. Initial results are displayed within seconds on the
large, industrial LCD touch screen, showing the contents for all key elements.
Pass/Fail messages can be setup to quickly identify if a sample does not meet
specifications.

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The LAB-X includes several features that help protect against damage caused by
sample spills or leaks, thus minimising downtime and preventing costly repairs.
Sample cups fit inside a secondary safety window that contains potential leaks
from the cup. These windows are fitted with Poly-4 film. They are re-usable and the
film can be changed in seconds (no need for a tool). The LAB-X also includes an
automated turntable that only places the sample above the X-ray tube and detector
for the duration of the analysis, minimising the risk of damage or contamination to
critical components. An audible alert is generated when the analysis is finished to
remind users that the sample should be removed.

The automatic atmospheric compensation delivers reliable analysis without the need
for helium or vacuum purge, minimising the cost per analysis without compromising Clear results display
results quality. Helium is used only when strictly necessary, for example when
measuring low energy elements such as Mg.

With up to 100,000 results stored on the analyser itself, operators can view new
and old results easily, print them on the integrated printer for a hard-copy record,
download them on a USB memory device, and even upload them to our ExTOPE
Connect cloud service to manage them remotely. With the LAB-X connected to WiFi,
the results are uploaded to your cloud account automatically, so you do not need to
be near the analyser to access your data!

Users can set-up a QC routine with concentration targets and lower and upper limits
for each control element; the displayed control graphs clearly show if the test is in
control.

SAMPLE PREPARATION
The sample preparation is simple: just pour the oil into a sample cup fitted with
Poly-4 film, place it in the safety window (also fitted with Poly-4 film) in the LAB-X’s
analysis port, and press the Start button.

PERFORMANCE AND RESULTS


The data shown in this section highlights the typical performance that the LAB-X
delivers. A simple empirical calibration was created for each method by measuring
a series of standard reference materials to establish the relationship between the
elements’ contents and their X-ray signal. The calibrations used the pre-defined
parameters included in the LAB-X5000 Lube Oil packages (pre-loaded in the
analyser). The limits of detection were calculated from the results of 10 repeat
measurements of a blank oil standard.

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Table 1: Typical calibration performance for lubricating oil analysis (air path)

Standard Limit of Limit of Precision


Calibration range detection quantification (95% confidence) Total analysis
Analyte error of calibration
(% m/m) (3σ) (% m/m) (10σ) (% m/m) (% m/m) time (seconds)
(% m/m)
P 0 – 0.25 0.004 0.0008 0.0027 0.0024
S 0 – 0.60 0.010 0.0003 0.0011 0.0021
100
Ca 0 – 0.60 0.005 0.0001 0.0003 0.0006
Zn 0 – 0.25 0.004 0.0005 0.0018 0.0014

Note: The precision was calculated from the results of 10 repeat measurements of a standard containing 0.15% P, 0.30% S, 0.40% Ca and
0.18% Zn.

Table 2: Typical calibration performance for the rapid analysis of lubricating oil (helium path)

Standard Limit of Limit of Precision


Calibration range detection quantification (95% confidence) Total analysis
Analyte error of calibration
(% m/m) (3σ) (% m/m) (10σ) (% m/m) (% m/m) time (seconds)
(% m/m)
P 0 – 0.25 0.003 0.0007 0.0023 0.0021
S 0 – 0.60 0.003 0.0002 0.0005 0.0010
100
Ca 0 – 0.60 0.004 0.0002 0.0007 0.0009
Zn 0 – 0.25 0.003 0.0003 0.0010 0.0006

Note: the precision was calculated from the results of 10 repeat measurements of a standard containing 0.15% P, 0.30% S, 0.40% Ca
and 0.18% Zn.

Table 3: Typical calibration performance for the rapid analysis of lubricating oil to ASTM D7751

Standard Limit of Limit of Precision


Calibration range detection quantification (95% confidence) Total analysis
Analyte error of calibration
(% m/m) (3σ) (% m/m) (10σ) (% m/m) (% m/m) time (seconds)
(% m/m)
Mg 0 – 0.40 0.01 0.007 0.023 0.018
P 0 – 0.25 0.01 0.001 0.003 0.001
S 0 – 1.55 0.03 0.001 0.004 0.002

Cl 0 – 0.40 0.007 0.0003 0.001 0.003 320

Ca 0–1 0.02 0.0001 0.0004 0.003


Zn 0 – 0.25 0.007 0.0002 0.0006 0.001
Mo 0 – 0.05 0.003 0.001 0.004 0.0005

Note: the precision was calculated from the results of 10 repeat measurements of a standard containing 0.1% Mg, 0.013% P, 0.65%
S, 0.36% Cl, 0.52% Ca, 0.19% Zn and 0.027% Mo.

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SUMMARY
Once calibrated, Hitachi High-Tech’s LAB-X5000 provides reliable lubricating
oil analysis, enabling operators to make process decisions fast. Its ease of
use and ruggedness make it an ideal tool at the blending plant, delivering
results within minutes for maximum productivity.

Visit www.hitachi-hightech.com/hha for more information.

ORDERING INFORMATION
The minimum needed for this application is:

| LAB-X5000 Lube Oil package, which


includes: the analyser, user manual (on
USB memory device), pre-loaded method
parameters and method sheet (calibration
instructions), setting up samples, and a
liquids accessories pack.

| LAB-X5000 Lube Oil Maxi package;


includes all the above, plus a helium purge
for enhanced performance, and pre-loaded
method parameters and method sheets for
the analysis of lubricating to ASTM D7751.

| A set of calibration standards can be ordered


as an option (Part Number 10003360 for
D6481, and 10022254 for D7751).

This publication is the copyright of Hitachi High-Tech Analytical Science and provides outline information only, which (unless agreed by the company in writing) may not be used,
applied or reproduced for any purpose or form part of any order or contract or regarded as the representation relating to the products or services concerned. Hitachi High-Tech
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product or service.

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© Hitachi High-Tech Analytical Science, 2019. All rights reserved.

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