In the daily work and production process, some special parts are often protected. Therefore, it is necessary to regularly monitor the accumulation of wear particles of these parts, that is, the analysis of metal elements in oil, which are often mentioned, based on the composition of metal components. And the speed of accumulation in the oil can accurately determine the failure period of the machine components. In addition, lubricants need to be monitored for their externally contaminated components (eg, metal elements brought in by dust and dirt). Measuring the content of wear metal in the lubricating oil can accurately understand the operating state and performance of the equipment. The metal contained in the oil shows the severity of the wear of the machine, which is critical for the evaluation of the maintenance and working performance of the equipment. It is particularly important to measure the trace metal in the lubricating oil as a monitoring method for the wear component.
1 instruments and methods
1.1 Instruments and reagents Tianrui Instrument ICP2060T (Petrochemical-specific) Inductively Coupled Plasma Emission Spectrometer
1. The semiconductor refrigeration sample introduction device improves the stability and sensitivity of the injection, and the test is more accurate and reliable.
2. Gasoline special torch to ensure long-term stability of the plasma and reduce the background of the substrate.
3. Increase oxygen assisted injection to maintain plasma stability and prevent carbon deposition.
1.2 Instrument working condition High frequency generator: 27.12MHz, quartz torch with 0.6mm center channel, high frequency power 1100W, reflected power about 50W, plasma gas flow 15L/min, auxiliary gas flow 1.0L/min, carrier gas flow 0.4 L/min, oxygen flow rate 30 ml/min, spray chamber temperature -10 ° C, peristaltic pump speed 3 ml/min.
1.3 Test method After the instrument is automatically ignited and the parameters are set according to the working conditions of the instrument, the diluent directly enters the mist chamber through the atomizer and enters the plasma. After the instrument is stabilized, the blank solution, the standard solution and the diluted sample solution are sequentially measured. The instrument can directly derive the content of each element in the final sample according to the working curve.
1.4 Repeatability test Continuously test 6 parallel samples and calculate the relative standard deviation of 6 test data, which is the repeatability data. The results are shown in the table below.
1.5 Accuracy test This method is used to test the standard content of GBH (E) 130129 and GBW (E) 130132 of the metal content of lubricating oil. The actual measured value and standard value are compared to obtain the recovery rate of the actual test, and the accuracy data is obtained. See the table below
Determination of the results of GBW (E) 130129 - Lubricant metal content spectral analysis of reference materials (mg / kg)
Determination of GBW (E) 130132 - results of spectral analysis of lubricating oil metal content standards (mg / kg)
2. Conclusion Compared with the inorganic digestion of aqueous solution injection ICP method, ICP organic injection method has an absolute advantage in analysis speed. The optimization of the working conditions of the instrument is the key to ensure the accurate analysis results of the ICP organic injection method. The organic injection method has good accuracy and repeatability and can meet the analytical requirements. It is suitable for accurate testing of batch samples. The detection results have good detection limits, accuracy and repeatability, and are suitable for popularization in the petrochemical industry.
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