NB/SH/T 0940-2016 Standard test method for analysis of in-service lubricants using a specific four-in-one tester (atomic emission spectrometry, infrared spectrometry, viscosity and laser particle counter)

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NB/SH/T 0940-2016 applies to the quantitative analysis of in-service lubricating oils using an automated four-in-one tester combining atomic emission spectrometry, infrared spectrometry, viscometry and a laser particle counter.

Evidence note: the content of this page was compiled from the original text of this standard held in the Origin Standard library (points marked "[to be verified]" are "[source unclear]" in the original); for individual values and current status, refer to the original pages of the standard and the product certificate.

Scope: Applies to the quantitative analysis of in-service lubricating oils using an automated four-in-one tester (atomic emission spectrometry, infrared spectrometry, viscosity and laser particle counter). 1.2 It applies to the analysis of in-service lubricating oils in the ISO viscosity grade range 10 mm²/s–320 mm²/s; the ranges of oil properties measured are given in Tables 1 and 2. (The unit in the original is [source unclear] as "mm'/s", [to be verified] ([source unclear])). 1.3 It is used for trend analysis of wear and contamination in in-service oils, but the test results may not be consistent with the test results of the corresponding test methods in current national standards, industry standards and international standards. 1.4 It does not apply to the analysis of crude oil. 10 Sampling: in-service lubricating oils in the ISO viscosity grade range 10 mm²/s–320 mm²/s can be analysed, including hydraulic oils, transmission oils and power steering oils.

Principle: Method summary: collect an in-service oil sample from the equipment being monitored into a new, clean 120 mL sample bottle; sampling should be carried out within 30 minutes after the equipment is shut down. To obtain correct evaluation information, the oil type and service information need to be recorded. Prepare the four-in-one tester according to the operating manual and the on-screen prompts. Place the sample in the sample transport system for analysis. The application software guides the whole process and controls sample transport, data storage, on-screen display and printing of results. 5 Significance and use: 5.1 The four-in-one tester is mainly used for on-site analysis of in-service lubricating oils in mining, construction, off-road vehicles, marine transport, power generation, agriculture, industry and manufacturing. 5.2 For proactive and preventive maintenance, timely in-service oil analysis results are essential. On-site oil analysis can extend equipment uptime and equipment life through continuous system monitoring and control of potential contamination.

Apparatus: Four-in-one tester: the specific four-in-one tester shall be composed of two or more of the following sensors: emission spectrometer, infrared device, viscometer and particle counter. 7.2 Emission spectrometer: composed of an excitation source, an excitation stand and an optical system. 7.3 Infrared device: composed of an infrared source, a sample cell and an optical system. 7.4 Dual-temperature viscometer: composed of a temperature-controlled sample reservoir and an electronic control system. 7.5 Particle counter: a precision sensor cell using red laser extinction technology, calibrated in accordance with GB/T 18854 and reporting results in accordance with GB/T 14039. 7.6 Sample bottle: capacity not less than 120 mL; the sample bottle shall not be contaminated and shall be discarded after use. Maximum dimensions of the sample bottle: height 10.8 cm, diameter 8.9 cm. The opening of the sample bottle shall not be less than 1.6 cm. 7.7 Ultrasonic water bath: an ultrasonic bath filled with water, used to agitate the sample to ensure that all contaminants are suspended in the lubricating oil sample. This step is usually carried out when the lubricating oil sample is to be analysed for particle counting. 7.8 Computer application software and operating manual: the computer application software provides the application programmes for the four-in-one tester; an electronic user and simplified reference manual with a help interface provides quick reference, and a tiered equipment database is used to store, analyse, manage and interpret data and to generate reports automatically. A complete operating manual and troubleshooting guide accompany the software application.

Reagents and reference materials: The following materials are used with the four-in-one tester (available from the instrument manufacturer) to ensure accurate operation of the integrated tester. 8.1.1 Electrodes: high-purity silver electrode pair (upper and lower electrodes). 8.1.2 Flush oil: an environmentally friendly mineral or synthetic oil used to flush the internal system of the instrument. In most cases, clean flush oil can be used as the base oil for instrument calibration. The flush oil is a non-flammable white oil. 8.1.3 Test standard oil: used as a calibration standard to calibrate the four-in-one tester. It is a multi-element solution of specific concentration and shall be a certified reference material. The certified concentrations are those of standard solutions prepared according to the assayed concentration of the raw materials and gravimetric procedures. The associated uncertainty of the certified concentration of each element is ±2 mg/kg; to verify these standard values, inductively coupled plasma emission spectrometry (ICP) analysis may be carried out for confirmation. It is recommended to shake the solution thoroughly before use. Note: the manufacturer guarantees the accuracy of the solution within its period of validity, i.e. under normal laboratory conditions provided the cap is kept tight and it is stored in the original bottle. Do not refrigerate or store in direct sunlight, and minimize exposure to humid or high-humidity environments. 8.1.4 High-viscosity fluid: used for the viscometer only. This fluid is a liquid of known viscosity; the viscometer is calibrated or recalibrated by periodically analysing this liquid. It consists of a highly refined mineral oil and an internal combustion engine oil additive package containing detergents and dispersants. 8.1.5 Low-viscosity fluid: used for the viscometer only. This fluid is a liquid of known viscosity; the viscometer is calibrated or recalibrated by periodically analysing this liquid. It consists of a highly refined mineral oil and an internal combustion engine oil additive package containing detergents and dispersants. 8.1.6 Reference oil: verifies the accuracy of the physical property test results of the infrared device. The physical properties of the reference oil are known, and calibration is carried out by comparing these known physical properties with the test results of the infrared device. The reference oil consists of a highly refined mineral oil plus ZDDP (zinc dialkyldithiophosphate). 8.1.7 Clean cotton swabs: used for electrode cleaning. The operator shall use uncontaminated swabs, and the swabs used shall not have been bleached with sodium-containing hypochlorite. Before using cleaning swabs, check the manufacturer's instructions to confirm whether the swabs have been bleached during production.

Key conditions: Turn on the main power switch of the four-in-one tester and press the reset button to activate the computer and all components. 11.2 During warm-up, the four-in-one tester runs a self-test programme. After the self-test page appears, allow the four-in-one tester to warm up for 10 min. 11.3 Fill the container holding the cleaning liquid with clean flush oil; the flush oil is a non-flammable product. (Warning: in accordance with local law, waste flush oil shall be poured into an approved waste disposal container.) 11.4 If a printer is connected to the computer, ensure that there is printing paper in the printer tray. 11.5 Check the electrode gap: the gap between the upper and lower electrodes shall be checked periodically to ensure normal operation of the emission spectrometer. The proper electrode gap may be set using a gap tool designed specifically for the four-in-one tester; the electrode gap may only be adjusted before element calibration. 11.6 Clean the electrodes: use clean cotton swabs to clean the outer and inner surfaces of the upper and lower electrodes. 11.6.1 Open the cover of the excitation chamber of the four-in-one tester. Wipe the electrodes with a clean dry cotton swab to remove all sample residue. 11.6.2 With another clean dry cotton swab, insert it into the central hole of the brass holder and wipe the inner wall of the upper electrode holder. Note: cleaning liquid shall not be used to clean the electrodes. Always use clean dry cotton swabs when cleaning the electrodes. 11.6.3 There are no special requirements for oil sample preparation when testing viscosity. 11.6.4 When the particle counting test is used, the sample bottle containing the in-service oil shall be placed in an ultrasonic water bath for 1 min (for non-on-site analysis, the ultrasonic time may be appropriately extended); this step is part of sample preparation. 12.1 Baseline check: using the established system cleaning procedure, run a baseline check to verify the cleanliness of the system. This procedure is executed under the "Calibration" button on the main screen of the four-in-one tester. The baseline check ensures that the atomic emission spectrometer is not contaminated and gives a pass or fail prompt on the computer screen so that the operator knows whether the next sample can be analysed. The specific acceptance criterion for the phosphorus baseline check is ±10 mg/kg; for all other wear and additive elements it is ±5 mg/kg. 12.2 If the baseline check does not meet the cleanliness range requirements of the atomic emission spectrometer, flush the system until the baseline check passes. The baseline check procedure shall be run every 24 h. 12.3 Calibration: calibrate the atomic emission spectrometer of the equipment using the atomic emission test standard oil specified in 8.1.3. 12.3.1 If any device in the specific four-in-one tester fails to meet the accuracy range requirements of the calibration test, a complete calibration procedure shall be performed. Note: the standard [source unclear] may be run at any time to confirm whether the four-in-one tester is calibrated and clean. Detailed check procedures are given in the operating manual. ([source unclear] incomplete at this point in the original, [to be verified] ([source unclear])). 12.3.2 When the reference oil test does not [source unclear], the calibration procedure shall be run as described in the operating manual. ([source unclear] incomplete at this point in the original, [to be verified] ([source unclear])). 12.4 Reference oil check: this procedure is recommended to be run every 96 h. This procedure is used to determine whether sample residue, solids or other wear particles in the infrared spectroscopic component of the four-in-one tester have been flushed away. The software of the four-in-one tester determines pass/fail and displays on the computer screen whether the check has been completed successfully. 12.5 Error: if the instrument reports an "error" message, refer to the troubleshooting guide in the operating manual. ([source unclear] incomplete at this point in the original, [to be verified] ([source unclear])). 12.6 Calibration of the particle counter: calibration is carried out by the manufacturer. Calibrate the particle counter after approximately 1000 particle counting samples have been analysed or every two years, whichever comes first.

Calculation and results: Based on the information entered previously [source unclear] the test results are obtained by analysing the sample. All necessary calculations are performed by the software programme and a data report is generated. [source unclear] diagnostic report and result interpretation report can be produced. ([source unclear] incomplete at this point in the original, [to be verified] ([source unclear])). 15.2 The test results may include a wear rating for the equipment (for example: normal, abnormal or severe) and maintenance recommendations. 16.1 Report the test results as follows: 16.1.1 Wear elements, contamination [source unclear] and additive elements: report as an integer in mg/kg. 16.1.2 Water, ethylene [source unclear] and fuel dilution: report as a mass percentage or in simplified form as "present" or "absent". ([source unclear] incomplete at this point in the original, [to be verified] ([source unclear])). 16.1.3 Base number: report in mgKOH/g. The definition of base number may refer to SH/T 0688. 16.1.4 Oxidation value and nitration value: report in absorbance units (Abs/mm). 16.1.5 Viscosity: report the viscosity at 100 °C or 40 °C, or the viscosities at 100 °C and 40 °C, in mm²/s. If the viscosity is measured at both temperatures, report the viscosity index. 16.1.6 Particle count: report the particle sizes and numbers found. 16.2 The computer software can display the test results on screen. The results can be printed automatically in one of several print formats.

Quality control: Used oil [source unclear] repeatability ([source unclear] incomplete at this point in the original, [to be verified] ([source unclear])). 17.2 The precision is based on statistical analysis of results from 4 laboratories and 5 samples (5 instruments, 5 operators). [source unclear] in-service oils under different service conditions were used. The statistical analysis results reflect differences in spectrometers and instruments. This variability is taken into account [source unclear] using different instruments. Under the same test conditions (95% confidence level), the difference between two consecutive test results on the same sample shall not exceed the values listed in Tables 3 and 4. Table 3 Repeatability of element analysis (low range/high range and corresponding repeatability; the table in the original is severely [source unclear] and misaligned; the following is the legible content, [to be verified] ([source unclear])): Low range (mg/kg): 5–100, 25–150, 5–[source unclear], 100–500, 6–1000, 150–[source unclear], 5–100, 10–1000, 6–100, 8–100, 7–100, 8–100, etc. Low range repeatability (mg/kg): 5, 25, 5, 25, 8, 5, 6, 10, [source unclear], 10, 8, etc. High range (mg/kg): NA, 150–2000, 100–1000, 500–9000, NA, 500–1000, 1000–3000, NA, 100–3000, NA, NA, 600–4000, 1000–4000, 150–8000, NA, NA, NA, NA, 100–4000, etc. High range repeatability: ±20%, NA, NA, ±20%, ±20%, ±15%, NA, NA, NA, NA, ±20%, etc. Table 4 Repeatability of physical property analysis: | Physical property | Range | Repeatability | |---|---|---| | Water (mass fraction)/% | 0.1–3 | 0.2 | | Ethylene glycol (mass fraction)/% | 0.1–2 | 0.2 | | Soot (mass fraction)/% | 0.1–4 | 0.2 | | Fuel dilution (mass fraction)/% | 0.1–15 | 0.4 | | Oxidation value/(Abs/mm) | 0.1–50 | 0.2 | | Nitration value/(Abs/mm) | 0.1–35 | 0.2 | | Calculated viscosity (IR) (100 °C)/(mm²/s) | 4–35 | 2 | | Viscosity at 40 °C/(mm²/s) (optional) | 30–320 | 2 | | Viscosity at 100 °C/(mm²/s) (optional) | 5–25 | [source unclear] ([source unclear]) | | Viscosity index | 5–150 | 5 | | Base number/(mgKOH/g) | 1.0–17 | 1 | 17.3 Reproducibility R: the reproducibility of this method has not yet been established. 17.4 Bias: the bias of this method could not be established.

Normative references: GB/T 265 Petroleum products — Determination of kinematic viscosity and calculation of dynamic viscosity GB/T 1995 Petroleum products — Calculation of viscosity index GB/T 4756 Petroleum liquids — Manual sampling GB/T 11137 Dark petroleum products — Determination of kinematic viscosity (reverse-flow method) and calculation of dynamic viscosity GB/T 14039 Hydraulic fluid power — Fluid contamination — Method for coding the level of contamination by solid particles GB/T 17476 Used lubricating oils — Determination of additive elements, wear metals, contaminants and selected elements in base oils (inductively coupled plasma emission spectrometry) GB/T 18854 Hydraulic fluid power — Calibration of automatic particle counters for liquids SH/T 0251 Petroleum products — Determination of base number (perchloric acid potentiometric titration method) SH/T 0688 Petroleum products and lubricants — Determination of base number (potentiometric titration method) NB/SH/T 0853 Condition monitoring of in-service lubricating oils — Fourier transform infrared (FT-IR) trend analysis NB/SH/T 0865 Used lubricating oils and hydraulic oils — Determination of wear metals and contaminants — Rotating disc electrode atomic emission spectrometry NB/SH/T 0870 Petroleum products — Determination of dynamic viscosity and density and calculation of kinematic viscosity — Stabinger viscometer method GB/T 1.1—2009 (mentioned in the foreword; this standard was drafted in accordance with its provisions)

Evidence note: [to be verified] and [source unclear] mark specific points that still require checking against the original text of the standard and do not indicate that they have been verified. Do not use these values or steps directly as a basis for work.

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