多元醇油脂中元素分析检测方案(原子吸收光谱)

Aurora Instruments Ltd.Application Notice #AA-13Cont. on back The Analysis of Al， Cu and Fe in Polyol Ester Oil by GFAAS Introduction： Accurate determination of elements like As， Cu and Fe in polyol ester oils is critical to diagnosingand preventing mechanical failure in compressors. Sample Preparation： All samples were diluted with MIBK to reduce their viscosity， making them easier to inject into thefurnace， and bringing them into the detection range of the instrument. The dissolved sampleswere successfully ashed at relatively low temperatures and showed little background interference.Therefore， aqueous standards were used for calibration. Operating Conditions： Instrumentation：Aurora Instruments Al 1100 GFAASInjection Volume：10 pLModifier Used：NoneSolvent：Analytical grade MIBK Method Name Oil Oil Oil Element Name AI Cu Fe Instrument Mode Absorbance Absorbance Absorbance Display Mode Corrected Corrected Corrected Manual Band Pass 0.2 nm 0.2 nm 0.2 nm Lamp Current 3.0 mA 2.0 mA 5.0 mA Wavelength 309.29 nm 324.75 nm 248.30 nm PMT Voltage 370.0V 350.0V 365.0V Preheat Steps 0 0 0 Cooling Time 30 s 30s 25s Inject Speed 5 5 5 Furnace Profile Steps 7 7 7 Furnace Profile Steps Step Final Temp ((c) Ramp Time (s) Hold Time(s) Gas Flow PlasmaON CollectData Integrate 1 80 1.00 1.00 1.50 Off Off Off 2 110 13.00 2.00 1.50 Off Off Off 3 140 15.00 2.00 1.50 Off Off Off 4 600 5.00 5.00 1.50 Off Off Off 5 600 0.00 2.00 0.50 Off On Off 6 2200* 0.00 1.50 0.50 Off On On 7 30 0.00 2.00 0.50 Off On Off *The atomization temperature was 2200°C for Al， 2500℃ for Cu and 2100℃ for Fe. Aurora Instruments Ltd. Results： For Al Sample ID Description Conc. Peak Height Conc.(PH) %RSD (PH) Al std， ng/ml 0.000 0.0396 -0.3654 NA Al std， ng/ml 10.000 0.2318 10.2435 NA Al std， ng/ml 20.000 0.4216 20.7147 NA Al std， ng/ml 30.000 0.5791 29.4072 NA Blank MIBK 0.0098 -2.0113 33.8345 Oil Sample，ng/ml 2000 times dilution 0.2393 10.6535 2.7853 Sample ID Description Conc. Peak Height Conc.(PH) %RSD (PH) Cu std， ng/ml 0.000 0.0175 -0.1011 NA Cu std， ng/ml 5.000 0.0983 4.7396 NA Cu std， ng/ml 10.000 0.1943 10.4932 NA Cu std， ng/ml 15.000 0.2749 15.3267 NA Cu std， ng/ml 20.000 0.3452 19.5416 NA Blank MIBK 0.0112 -0.4781 16.1594 Oil Sample， ng/ml 100 times dilution 0.2312 12.7046 4.7172 For Fe Sample ID Description Conc. Peak Height Conc.(PH) %RSD(PH) Fe std， ng/ml 0.000 0.0326 0.0494 NA Fe std， ng/ml 5.000 0.1730 4.6118 NA Fe std， ng/ml 10.000 0.3562 10.5659 NA Fe std， ng/ml 15.000 0.4907 14.9361 NA Fe std， ng/ml 20.000 0.6416 19.8368 NA Blank MIBK 0.0408 0.31871 37.5608 Oil Sample， ng/ml 200 times dilution 0.5708 17.5382 1.5511 Discussion： This analysis was performed using manual injection. While the precision was quite adequate， itcould have been improved by using an autosampler with Aurora Instruments’Fast Dry technique.This would have overcome the inherent lack of reproducibility of manual injection and the quickdiffusion of the organic solvent throughout the tube before the furnace temperature was ramped. Due to the relatively large dilution factor used in these analyses， aqueous standards wereusedfor calibration， rather than more expensive organic standards. Thus， the user saves money and isable to work in a much safer and more convenient environment. Introduction:Accurate determination of elements like As, Cu and Fe in polyol ester oils is critical to diagnosingand preventing mechanical failure in compressors.