Detection Target
Multielement Determination of Used and Unused Lubricating Oils and Base Oils
Overview
This solution conforms to the ASTM D5185 Standard Test Method for Multielement Determination of Used and Unused Lubricating Oils and Base Oils by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). It covers the determination of additive elements, wear metals, and contaminants in used lubricating oils by inductively coupled plasma atomic emission spectrometry (ICP-AES).
Summary
In the daily work and production process, some special components are often protected, so it is necessary to regularly monitor the accumulation of wear particles on these components, which is often the analysis of metal elements in oil, based on the composition of metal components and the accumulation rate in the oil can accurately determine the failure cycle of the machine components. In addition, lubricating oil also needs to monitor its foreign contamination components (such as metal elements brought in by dust and dirt). Determining the content of wear metal in the lubricant can accurately understand the operating status and performance of the equipment. The metal contained in the oil shows the severity of the wear of the parts, which is very important for the maintenance of the equipment and the evaluation of the working performance. Monitoring methods for the determination of trace metals in lubricating oils as a component of wear are particularly important.
Instrument Usage
The HKL-5185F is an Inductively Coupled Plasma-Atomic Emission Spectrometer (ICP-AES) featuring a vertical observation mode, a CCD detector, and full-spectrum direct-reading capabilities. This instrument is primarily utilized for the determination of trace and minor element concentrations in various substances (specifically those soluble in nitric acid, hydrochloric acid, hydrofluoric acid, etc.). Its scope of application is extensive, encompassing a wide array of fields such as environmental protection, petroleum products, rare earth elements, semiconductors, geology, metallurgy, chemical engineering, clinical medicine, food analysis, biological samples, forensic science, and agricultural research.
Working environment
1 Storage and transportation temperature: 5℃-40℃.
2 Relative humidity for storage and transportation: ≤85
3 Atmospheric pressure: 86-106 kPa
4 Power adaptability: 220±22VAC 50±1Hz
5 Working humidity: ≤70%
6 Working temperature: 15℃～30℃
Instrument Mainframe
1. Optical system1.1 The cross-dispersion structure of the middle-step grating and prism, the use of ultra-pure SiO2 prisms, and the high optical path transmission efficiency ensure elemental measurements in the deep UV region.
1.2 Optimized optical design with aspherical optics improves imaging quality and spectral acquisition efficiency.
1.3 Optical chamber multi-point inflation technology, shorten the optical chamber inflation time, improve the sensitivity and stability of the UV spectrum, can be measured on the power on.
1.4 The gas circuit of the optical chamber is independent and can be filled with nitrogen or argon.
1.5 Optical system: Medium step 2D beam splitter optical system, focal length 400mm
1.6 Spectral range: 165nm-950nm
1.7 Grating specifications: medium step grating, size: 100mm x 50mm
1.8 Prism: Ultra-pure SiO2 material
1.9 Stray light: 10,000 μg/ml Ca solution has an equivalent background concentration of ＜2ug/ml at As189.042nm
1.10 Temperature control: 38±0.1℃, temperature can be set.
2. Detector2.1 Large-area CCD detector, full-spectrum response, high UV quantization efficiency, a single exposure to complete the full spectrum of the spectral signal acquisition and reading, so as to obtain more rapid and accurate analysis results.
2.2 The largest target size in its class, million pixels, single pixel area 24μm X 24μm, three-stage semiconductor cooling, cooling temperature -35 ℃, with very low noise and better stability.
2.3 Detector: Scientific grade CCD detector, anti-saturation overflow
2.4 Number of pixels: 1024x1024, pixel area: 24µm x 24µm
2.5 Operating temperature: ＜-40 degrees Celsius, stabilization time ＜3 minutes
2.6 Quantization efficiency: no coating, quantization efficiency up to 75% or more
3. RF generator3.1 All-solid-state RF generator, small size, high efficiency, fully automatic load matching, fast speed, high precision, can adapt to a variety of complex matrix samples and volatile organic solvents testing, with excellent long-term stability.
3.2 Cold cone elimination of tail flame technology, minimize self-absorption effect and ionization interference, so as to obtain a wider dynamic linear range and lower background, to broaden the detection range of the instrument, to ensure accurate measurement results.
3.3 The vertical torch tube design provides better sample tolerance, reduces cleaning requirements and lowers consumption of spare torch tubes.
3.4 Simple torch tube mounting and positioning design for quick positioning and precise position reproduction.
3.5 With a low power standby mode, the standby reduces the output power, reduces the gas flow, and only maintains the plasma operation, saving the use of costs.
3.6 * Upgraded solid-state power supply technology with solid-state RF power supply output protection device, with small size, high output efficiency, stable output power, with water, gas and overload and other safety protection functions, which greatly improves the safety of the instrument and reduces the failure rate of the instrument. (Provide supporting materials issued by provincial or above authoritative institutions, the purchaser has the right to verify the original when supplying)
3.7 Output power: 500W-1600W continuous 1W adjustable
3.8 Power stability: ≤0.1%
3.9 Oscillation frequency: 27.12MHz
3.10 Frequency stability: ≤0.01%
3.11 Matching method: automatic matching
3.12 EMF leakage radiation intensity: ＜0.5V/m
4.Sample introduction system4.1 The instrument is equipped with a series of optimized injection systems for the testing of organic solvents, high salt/complex matrix samples, and samples containing hydrofluoric acid.
4.2 Easy to maintain with one-piece torch tube, quick changeover and low cost of ownership.
4.3 Using mass flow controller to control the flow of cooling gas, auxiliary gas and carrier gas, the flow rate is continuously adjustable to ensure long-term stability of test performance.
4.4 *With two into six out of the water integrated feedback shunt system, to ensure that the whole instrument water system control. Easy to assemble, smooth and beautiful appearance, easy to use with the instrument. Extend the life of the instrument water system. (Provide supporting materials issued by provincial or above authority, the purchaser has the right to verify the original when supplying)
4.5 4-channel 12-roller peristaltic pump, pump speed continuously adjustable to ensure the stability of sample introduction, with a rapid cleaning function.
4.6 Torch tube orientation: vertical
4.7 Torch coil: 3 turns
4.8 Torch tube: tri-concentric quartz torch tube: OD 20mm; various models are available according to the size of the center channel. (Need to provide color pages and physical drawings to support)
4.9 Atomizer: Concentric atomizer or parallel channel atomizer, outer diameter 6mm, optional standard atomizer, high salt atomizer, hydrofluoric acid atomizer.
4.10 Fog chamber: Cyclone fog chamber, optional double cylinder type fog chamber and HF resistant fog chamber.
4.11 Peristaltic pump: 4-channel 12-roller, continuously adjustable speed.
4.12 Argon consumption: 8L/min~18L/min
4.13 Cooling gas: 0.00L/min~20.00L/min, accuracy 0.01L/min
4.14 Auxiliary gas: 0.00L/min~2.00L/min, accuracy 0.01L/min
4.15 Carrier gas: 0.00L/min~2.00L/min, accuracy 0.01L/min
5. Control system5.1 Humanized interface design, smooth and easy to understand, easy to use, optimized software system for analytical applications, without the need for complex method development, you can quickly carry out analytical operations.
5.2 Multi-window, multi-method analysis program for simultaneous measurement, editing, and viewing of different method data.
5.3 The software spectral line library has more than 70,000 spectral lines library, intelligent prompts potential interference elements, to help users rationally choose to analyze the spectral lines.
5.4 Provides a variety of standard series editing modes, supports a variety of curve calibration modes, such as test first and then set the standard, sandwich method of testing samples, and so on.
5.5 The software supports standard curve method, standard addition method and other analytical methods, with deduction of blank, internal standard correction, interference correction and other data processing methods.
5.6 Easy observation mode setting, intuitive test results display, with a variety of report output format.
6. Technical index of the whole machine
6.1 *Observation mode: classical vertical observation mode
6.2 Liquid content: 0.01ppm~thousands of ppm
6.3 Solid content: 0.001%~70%
6.4 Repeatability: (i.e., short-term stability) relative standard deviation RSD＜ 1%
6.5 Stability: Relative standard deviation RSD＜1.5% @2 hours
6.6 Elemental detection limit (μg/L): 1ppb~10ppb for most elements
Test Part
1.1 Abrasion Elements in Lube Oils
1.1.1 CONOSTAN Dedicated Diluent for ICP
1.1.2 Pipette，0-5ml
1.1.3 Electronic balance, 0.0001
1.2 Test method
After the apparatus is automatically ignited and the parameters are set according to the working conditions of the apparatus, the diluent is directly sucked into the mist chamber through the nebulizer and enters the plasma. After the apparatus is stable, measure the blank solution, standard solution and diluted sample solution at one time. The content of each element in the final sample can be directly obtained. The linear relationship of the elements was determined according to the testing method. At the same time, the blank solution was measured 10 times for each element. The standard deviation of the measured value was divided by the slope of the curve as the method detection limit. As can be seen from the table below, the fitting coefficient of the elemental working curve is higher than 0.999, indicating that the linear relationship is good within the linear range of the working curve. Because the working parameters of the apparatus are optimized, the test conditions of the elements are optimized to improve the accuracy of the test results.
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ICP Repeatability of 16 Elements in Lubricants |
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|
Element |
Repeatability (RSD) |
Element |
Repeatability (RSD) |
|
Vanadium (V) |
1.45% |
Cadmium (Cd) |
2.58% |
|
Copper (Cu) |
0.76% |
Nickel (Ni) |
2.78% |
|
Silver (Ag) |
0.91% |
Iron (Fe) |
1.46% |
|
Titanium (Ti) |
1.35% |
Silicon (Si) |
1.70% |
|
Barium (Ba) |
1.48% |
Manganese (Mn) |
1.22% |
|
Calcium (Ca) |
1.31% |
Chromium (Cr) |
1.10% |
|
Zinc (Zn) |
1.65% |
Magnesium (Mg) |
1.93% |
|
Lead (Pb) |
2.46% |
Phosphorus (P) |
2.36% |
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ICP Repeatability of 16 Elements in Lubricants |
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|
Element |
Repeatability (RSD) |
Element |
Repeatability (RSD) |
|
Vanadium (V) |
1.45% |
Cadmium (Cd) |
2.58% |
|
Copper (Cu) |
0.76% |
Nickel (Ni) |
2.78% |
|
Silver (Ag) |
0.91% |
Iron (Fe) |
1.46% |
|
Titanium (Ti) |
1.35% |
Silicon (Si) |
1.70% |
|
Barium (Ba) |
1.48% |
Manganese (Mn) |
1.22% |
|
Calcium (Ca) |
1.31% |
Chromium (Cr) |
1.10% |
|
Zinc (Zn) |
1.65% |
Magnesium (Mg) |
1.93% |
|
Lead (Pb) |
2.46% |
Phosphorus (P) |
2.36% |
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Results of GBW (E) 130132-Lubricant Metal Content Spectral Analysis Reference Material (mg / kg) |
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|
Element |
Standard Value |
Result |
Recovery Rate |
Element |
Standard Value |
Result |
Recovery Rate |
|
Vanadium (V) |
100 |
98.04 |
98.00% |
Cadmium (Cd) |
100 |
104.91 |
104.90% |
|
Copper (Cu) |
100 |
112.57 |
112.60% |
Nickel (Ni) |
100 |
106.5 |
106.50% |
|
Silver (Ag) |
100 |
102.21 |
102.20% |
Iron (Fe) |
100 |
104.84 |
104.80% |
|
Titanium (Ti) |
100 |
102.11 |
102.10% |
Silicon (Si) |
100 |
91.78 |
91.80% |
|
Aluminum (Al)* |
100 |
118.62 |
118.60% |
Manganese (Mn) |
100 |
106.09 |
106.10% |
|
Calcium (Ca) |
100 |
88.54 |
88.50% |
Chromium (Cr) |
100 |
99.31 |
99.30% |
|
Zinc (Zn) |
100 |
110.57 |
110.60% |
Magnesium (Mg) |
100 |
112.43 |
112.40% |
|
Lead (Pb) |
100 |
108.39 |
108.40% |
Phosphorus (P) |
100 |
97.81 |
97.80% |
Applicable Standard: ASTM D5185 Standard Test Method for Multielement Determination of Used and Unused Lubricating Oils and Base Oils by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
Conclusion
The ICP method is used to directly determine the 16 kinds of wear elements in lubricating oil. The relative digestion method has higher accuracy and better reproducibility. HKL-5185F has the characteristics of low cost, fast speed and high accuracy. The determination of 16 types of wear elements in lubricating oil can fully meet the demands in the petrochemical industry.
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Test Report Comparison |
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Sample Name |
Diesel Engine Oil |
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Receiving Date |
JAN,2ND,2020 |
Test Period |
JAN,8TH,2020 |
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Description |
Viscous Oil Sample |
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Test Requirement |
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Test component |
Ca, Mg, P, Zn |
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Reference |
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Standard |
ASTM D5185 |
Standard Sample |
S-21 Mixed Sample |
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Humidity |
≤70% |
Temperature |
25℃ |
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Test Process |
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Weigh a certain amount of sample into a 100ml volumetric flask, add the internal standard solution, dilute to the mark with blank oil, shake well, and wait for measurement |
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HKL-5185F Full-Spectrum Direct-Reading ICP-OES |
Perkin Elmer Optima 3300 ICP-OES |
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Test Item |
Unit |
Result |
Test Item |
Unit |
Result |
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|
Ca |
mg/kg |
4179.1 |
Ca |
mg/kg |
4225.7 |
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|
Mg |
mg/kg |
22.06 |
Mg |
mg/kg |
21.501 |
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P |
mg/kg |
1064.3 |
P |
mg/kg |
1026.2 |
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|
Zn |
mg/kg |
1133.1 |
Zn |
mg/kg |
1133.1 |
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Configuration
|
Serial |
Name |
Quantity |
Remarks |
|
1 |
HKL-5185F Full-Spectrum Direct-Reading ICP-OES |
1 unit |
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|
2 |
Spectrometer analysis software |
1 set |
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3 |
Quartz rectangles |
2 pieces |
|
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4 |
Imported nebulizer |
1 piece |
|
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5 |
Double-cylinder fog chamber |
2 pieces |
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6 |
Cooling circulating water |
1 unit |
Cooling capacity 2000W |
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7 |
Branded computer |
Coolray dual-core 1.6G PC with no less than 4G RAM, 320G hard disk, 19 LCD monitor. |
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8 |
Brand Printer |
Laser Printer |
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9 |
Voltage stabilized power supply |
1 unit |