This note describes the use of the Agilent 5100 SVDV ICP-OES for the trace elemental analysis of a bovine liver standard reference material (SRM). InstrumentationAll measurements were performed using an Agilent 5100 SVDV ICP-OES with unique Dichroic Spectral Combiner (DSC) technology and vertical plasma that enables axial and radial view analysis at the same time. The sample introduction system consisted of a SeaSpray nebulizer, double-pass glass cyclonic spray chamber and a standard 5100 Dual View torch (demountable, quartz, 1.8 mm injector). The instrument uses a solid-state RF (SSRF) system operating at 27 MHz to deliver a robust plasma capable of excellent long term analytical stability. The instrument operating conditions used are listed in Table 1 and the wavelengths and calibration parameters selected for the analysis are given in Table 2.Table 1.The Agilent 5100 SVDV ICP-OES operating parameters used.ParametersSettingsRead time (s)10 Replicates3Sample uptake delay (s)20Stabilization time (s)10Rinse time (s)30Fast pump (rpm)80RF power (kW)1.20 Aux flow (L/min)1.0 Plasma flow (L/min)12.0Nebulizer flow (L/min)0.7Viewing height (mm)6
52AGILENT TECHNOLOGIES Speciality chemicalsFood & Agriculture ApplicationsExperimentalStandard and sample preparationTo validate the method, the National Institute of Standards and Technology (NIST) Standard Reference Material (SRM) 1577 Bovine Liver was prepared for analysis. The SRM was digested using a Milestone Ethos microwave digestion system, with approximately 0.5 g of samples being accurately weighed into the digestion vessel. This was followed by the addition of 7 mL of concentrated HNO3and 1 mL of 30% H2O2. Samples were digested using the pre-loaded digestion methods, allowed to cool, then made up to 50 mL with DI water. The final acid concentration was approximately 12% v/v HNO3.A series of standards (1, 5, 10, 100, 250, 500 ppm) were prepared from multi-element standards in 1% HNO3and a multi-element spike of the bovine liver digest was prepared at 100 ppb.Table 2.The wavelengths and calibration parameters selected for the analysis. ElementWavelength (nm)Background CorrectionCalibration FitCorrelation Coefficient K766.491FittedLinear0.99966Na589.592FittedLinear0.99978Fe238.204FittedLinear0.99999Cu327.395FittedLinear1.00000Zn213.857FittedLinear1.00000Mn257.610FittedLinear0.99998Se196.026FittedLinear1.00000Pb220.353FittedLinear0.99999Cd228.802FittedLinear1.00000As188.980FittedLinear1.00000Ca396.847FittedLinear0.99997Co238.892FittedLinear0.99999Mg279.078FittedLinear0.99968Mo202.032FittedLinear1.00000Ag328.068FittedLinear1.00000TI190.794FittedLinear1.00000Results and discussionThe linear dynamic range (LDR) for Na and K on the 5100 SVDV ICP-OES shows good linearity (Figures 1 and 2). Both elements can be calibrated up to 500 ppm with a correlation coefficient greater than 0.999 and less that 10% calibration error on each calibration point. This highlights the excellent LDR for Na and K in a single reading using the 5100 SVDV ICP-OES. On a conventional Dual View instrument, multiple readings of the sample would be required to achieve a comparable LDR.