Agilent Analysis of Fuel Lubricating Oils by Simultaneous ICP-OES Application Note Manual
Contents
1. T McKenzie Atomic Absorption Spectrophotometry for the analysis of Wear Metals in Oil Samples Varian Australia Pty Ltd Mulgrave Victoria 3170 Australia AA At Work No 10 January 1981 M B Knowles T Nham S J Carter A Charged Coupled Device Detector for Atomic Emission Spectroscopy American Laboratory September 1998 C Webb A T Zander P V Wilson and G Perlis A Fast Automated Spectral Curve Fitting Technique for ICP AES Spectroscopy May 1999 14 5 58 63 For More Information For more information on our products and services visit our Web site at www agilent com chem www agilent com chem Agilent shall not be liable for errors contained herein or for incidental or consequential damages in connection with the furnishing performance or use of this material Information descriptions and specifications in this publication are subject to change without notice Agilent Technologies Inc 1999 Printed in the USA November 1 2010 ICPES 27 j Agilent Technologies2. 3 mg kg 113 9 0 7 115 1 0 5 112 8 0 8 0 19 0 04 lt 0 1 107 4 0 5 IC 5 4 mg kg 3 05 0 05 22 8 0 3 50 9 0 7 2 04 0 05 lt 0 1 0 958 0 009 IC 6 mg kg lt 0 02 0 16 0 03 1 11 0 02 69 9 0 9 21 4 0 4 0 161 0 002 IC 10 mg kg 0 131 0 002 1 32 0 02 6 5 0 1 10 5 0 2 0 46 0 01 0 233 0 003 IC 15 mg kg lt 0 02 0 17 0 01 0 44 0 05 0 310 0 005 lt 0 1 0 006 0 002 N LS T S R M 1084a 96 8 1 3 97 6 1 1 98 8 2 4 97 9 1 5 98 8 1 5 Certified value mg kg 98 3 0 8 100 0 1 9 98 9 1 4 99 5 1 7 100 3 1 4 lt Values expressed as 10 times the standard deviation of background emission Value not certified Table 3 Na 588 995 nm Ni 216 555 nm P 213 618 nm Pb 220 353 nm Si 251 611 nm Ti 334 941 nm IC 1 mg kg 0 436 0 006 5 80 0 03 lt 1 0 98 0 02 6 01 0 08 5 45 0 03 IC 2 mg kg 2 24 0 05 28 3 0 2 lt 1 2540 2 29 4 0 2 29 1 0 2 IC 3 mg kg 2 97 0 06 108 1 lt 1 48 1 0 7 112 7 0 7 112 7 0 7 IC 5 4 mg kg 6 7 0 1 lt 0 1 119 5 0 7 19 1 0 2 7 57 0 09 0 205 0 008 IC 6 mg kg 0 62 0 01 lt 0 1 248 3 lt 03 1 58 0 03 0 011 0 004 IC 10 mg kg 37 1 0 8 3 08 0 03 23745 0 91 0 02 2 78 0 03 0 064 0 004 IC 15 mg kg 4 82 0 05 4 58 0 08 lt 1 lt 03 lt 05 lt 0 01 N LS T S R M 1084a 100 2 1 2 100 0 0 9 96 1 0 9 98 9 1 3 Certified value mg kg 99 7 1 6 TOTE 1 3 103 100 4 3 8 lt Values expressed as 10 times the sta
3. Author Andrew Ryan Multi Element Analysis of Fuel and Lubricating Oils by Simultaneous ICP OES Application Note Inductively Coupled Plasma Optical Emission Spectrometers Introduction The determination of metal levels in both fuel oil and lubricating oils is of prime impor tance to the industrial machinery transport and utility industries In general metal levels are determined to provide early warning of failure of components in physical contact with the oil Oil analysis can also indicate whether oil in a system has been contaminated by another source other than wear For example increases in silicon or aluminum levels may indicate dirt contamination or increased levels of sodium per haps seawater contamination or antifreeze leakage 1 Conversely a decrease in the levels of additive metals for example Ca Mg Zn Pb may indicate a dilution of the oil by one oil not containing these additives Many large fleet operators and mining companies rely on the analysis of used lubricating oil samples to extend the period between oil changes in their equipment and to warn of the beginning of mechanical failure so that preventive maintenance may be scheduled In this study various fuel oils and National Institute of Standards and Technology N I S T standard reference material S R M 1084a Wear Metals in Lubricating Oil were diluted in dekalin decahydronaphthalene and analyzed using a Agilent Vista simultaneous Inductively Coupl
4. ed Plasma Atomic Emission Spectrometer ICP OES with the axially viewed plasma RE Agilent Technologies For the analysis of volatile organic solvents with an axially viewed ICP the Auxiliary Gas Module 1 AGM 1 oxygen accessory is required The AGM 1 adds a small flow of oxygen to the plasma auxiliary gas thus reducing molecular band emissions This gives lower detection limits and prevents the build up of carbon within the torch and on the cooled cone interface The use of a simultaneous ICP OES instrument significantly improves the efficiency of analysis when a large number of ele mental determinations are to be made Typically large laborato ries specializing in used oil analysis test hundreds of samples each day In this study 21 elements were determined at around 105 seconds per sample including sample introduction and rinse time It should be noted that the measurement of more than this number of elements would not add further to the analysis time due to the simultaneous detection of the Vista Instrumental The Vista simultaneous ICP OES with axially viewed plasma was used for the analysis The Vista features a free running air cooled 40 MHz RF generator and cooled cone interface The Vista s optical system is based on an echelle polychroma tor with CCD detector 2 The polychromator is thermostatted to 35 C for stability and the unique CCD detector features 70 000 pixels detectors arranged to exactly match the 2 d
5. imensional echellogram The detector provides rapid readout and excellent detection limits The instrument was controlled with an IBM computer with an Intel Pentium processor and Agilent s Vista software running under Microsoft Windows NT operating system In this work a Vista with manual gas pressure regulator was used Mass flow control of the nebulizer flow which allows the nebulizer gas flow to be automatically adjusted is available as an option Instrument parameters Power Plasma gas flow Auxiliary gas flow Nebulizer type Torch type Spray chamber type Pump speed Pump tubing Sample uptake rate AGM 1 setting Sample delay Stabilization time Fast pump Replicate time Replicates Background correction 1 3 kW 15 L min 0 75 L min Glass concentric type K Demountable with 1 8 mm quartz injector Sturman Masters 15 rpm Inlet viton black black 0 76 mm id Outlet viton white white 1 02 mm id 0 6 mL min 5 130 mL min 15 seconds 45 seconds On 5 seconds 3 Off peak background correction or fitted back ground correction Fast Automated Curve Fitting Technique FACT was used for Na 588 995 nm Sample Preparation Approximately 2 g of used oil was accurately weighed into a 20 mL volumetric flask and made up to volume with dekalin One gram of N I S T S R M 1084a Wear Metals in Lubricating Oil was accurately weighed into a 50 mL volumetric flask and made up to volume with dekalin Resu
6. lts In this study seven fuel oil samples and one lubricating oil sample were analyzed The lubricating oil was a standard ref erence material obtained from NIST Gaithersburg MD USA and used to validate the method Triplicate analyses were performed and the average result is shown Table 1 Ag 328 068 nm Al 257 509 nm B 249 678 nm Ba 493 408 nm Ca 317 933 nm Cd 226 502 nm IC 1 mg kg 0 011 0 002 5 83 0 03 lt 0 2 lt 0 003 5 35 0 06 lt 0 02 IC 2 mg kg 0 0148 0 0005 28 7 0 1 lt 0 2 lt 0 003 26 5 0 3 lt 0 02 IC 3 mg kg 0 04 0 01 114 6 1 3 0 270 0 01 lt 0 003 109 0 0 6 lt 0 02 IC 5 4 mg kg 0 04 0 01 2 80 0 03 lt 0 2 37 5 0 3 222 1 0 95 0 02 IC 6 mg kg 0 09 0 01 lt 1 1 34 0 1 lt 0 003 640 4 lt 0 02 IC 10 mg kg 0 031 0 002 lt 1 0 53 0 08 16 3 0 2 3210 7 0 117 0 003 IC 15 mg kg lt 0 01 lt 1 lt 0 2 lt 0 003 0 974 002 lt 0 02 N LS T S R M 1084a 100 3 1 2 100 4 0 4 Certified value mg kg 101 4 1 5 104 lt Values expressed as 10 times the standard deviation of background emission Values in parenthesis are not certified but provided for information only Value not certified Table 2 Cr 267 716 nm Cu 324 754 nm Fe 259 940 nm Mg 279 553 nm Mo 284 824 nm Mn 257 610 nm IC 1 mg kg 6 21 0 05 6 41 0 04 5 95 0 05 0 067 0 007 lt 0 1 5 69 0 03 IC 2 mg kg 29 4 0 3 29 3 0 1 28 5 0 4 0 16 0 03 lt 0 1 28 2 0 3 IC
7. ndard deviation of background emission Values in parenthesis are not certified but provided for information only Value not certified Table 4 Discussion M SATO nin a For the NIST SRM 1084a sample measured values are in good IC 1 mg kg 5 68 0 03 5 76 0 05 agreement with the certified values demonstrating the IC 2 mg kg 28 3 0 3 28 2 0 3 suitability of the axial Vista ICP OES for the analysis of used IC 3 mg kg 11242 108 1 0 7 oils IC 5 4 mg kg lt 0 1 32 4 0 5 Ic 6 mg kg soi IYE Background structure the result of using an organic solvent posed some difficulties in the measurement of sodium at 1C 10 mg ka oda 00G PS8 E 588 995 nm Using Vista s Fast Automated Curve fitting IC 15 mg kg 15 3 0 2 0 356 0 007 Technique FACT improved the background measurement at N LS T_ S R M 1084a 96 4 1 3 this line and improved the levels of detection FACT uses Certified value mg kg 95 9 9 4 Gaussian curve modeling techniques to accurately character lt Values expressed as 10 times the standard deviation of background emission Value not certified ize and correct for neighboring spectral background 3 FACT has been proven to provide accurate background correction even when peaks are as close as 0 2 pixels and is ideal for correcting the background observed from organic solvents Acknowledgment The author wishes to thank Stewart Carter for his assistance in preparing this manuscript References
Download Pdf Manuals
Related Search
Agilent Analysis of Fuel Lubricating Oils by Simultaneous ICP OES Application Note Manual