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. The special torch for gasoline ensures long-term stability of the plasma and reduces the background of the substrate. 3. Increase oxygen assisted injection to maintain plasma stability and prevent carbon deposits. 1.2 Instrument working conditions High frequency generator: 27.12MHz , the center channel is 0.6mm Quartz torch, high frequency power 1100W , the reflection power is about 50W Plasma gas flow 15L/min Auxiliary gas flow 1.0L/min Carrier gas flow 0.4L/min Oxygen flow rate 30ml/min , spray chamber temperature -10 °C, peristaltic pump speed 3ml/min . 1.3 experiment 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, and the instrument is operated according to the work. The curve gives the amount of each element in the final sample directly. 1.4 Repeatability test Continuous test 6 Parallel sample, calculation 6 The relative standard deviation of the test data is the repeatability data. The results are shown in the table below. 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% 1.5 Accuracy test Using this method to test the standard content of the metal content spectrum of lubricating oil GBW(E)130129 , GBW(E)130132 Compare the actual measured value with the standard value to obtain the recovery rate of the actual test, and obtain the accuracy data. The results are shown in the table below. Determination GBW(E)130129- Lubricating oil metal content spectral analysis of the results of the reference material ( Mg/kg ) element standard value measured value Recovery rate element standard value measured value Recovery rate vanadium( V ) 10 9.58 95.8% cadmium( Cd ) 10 8.82 88.2% copper( Cu ) 10 10.16 101.6% nickel( Ni ) 10 9.70 97.0% silver( Ag ) 10 9.50 95.0% iron( Fe ) 10 9.97 99.7% titanium( Ti ) 10 9.97 99.7% silicon( Si ) 10 8.25 82.5% barium( Ba ) 10 10.73 107.3% manganese( Mn ) 10 9.61 96.1% calcium( Ca ) 10 10.05 100.5% chromium( Cr ) 10 9.41 94.1% Zinc ( Zn ) 10 10.20 102.0% magnesium( Mg ) 10 8.33 83.3% lead( Pb ) 10 10.35 103.5% phosphorus( P ) 10 10.99 109.9% Determination GBW(E)130132- Lubricating oil metal content spectral analysis of the results of the reference material ( Mg/kg ) element standard value measured value Recovery rate element standard value measured value 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% barium( Ba ) 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% in conclusion Injection with inorganic digestion solution ICP Compared with the law, ICP The organic injection method has an absolute advantage in analysis speed. The optimization of the working conditions of the instrument is guaranteed ICP The key to accurate analysis of organic injection methods. Organic injection method with good accuracy and repeatability , Can meet the analysis 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. Mining Rig,Mining Machine,Mining Rig 2021,Crypto Mining Machine Easy Electronic Technology Co.,Ltd , https://www.yxpcelectronicgroups.com
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