This note describes the use of the agilent 5100 svdv

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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). Instrumentation All 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. Parameters Settings Read time (s) 10 Replicates 3 Sample uptake delay (s) 20 Stabilization time (s) 10 Rinse time (s) 30 Fast pump (rpm) 80 RF power (kW) 1.20 Aux flow (L/min) 1.0 Plasma flow (L/min) 12.0 Nebulizer flow (L/min) 0.7 Viewing height (mm) 6
52 AGILENT TECHNOLOGIES Speciality chemicals Food & Agriculture Applications Experimental Standard and sample preparation To 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 HNO 3 and 1 mL of 30% H 2 O 2 . 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 HNO 3 . A series of standards (1, 5, 10, 100, 250, 500 ppm) were prepared from multi-element standards in 1% HNO 3 and 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. Element Wavelength (nm) Background Correction Calibration Fit Correlation Coefficient K 766.491 Fitted Linear 0.99966 Na 589.592 Fitted Linear 0.99978 Fe 238.204 Fitted Linear 0.99999 Cu 327.395 Fitted Linear 1.00000 Zn 213.857 Fitted Linear 1.00000 Mn 257.610 Fitted Linear 0.99998 Se 196.026 Fitted Linear 1.00000 Pb 220.353 Fitted Linear 0.99999 Cd 228.802 Fitted Linear 1.00000 As 188.980 Fitted Linear 1.00000 Ca 396.847 Fitted Linear 0.99997 Co 238.892 Fitted Linear 0.99999 Mg 279.078 Fitted Linear 0.99968 Mo 202.032 Fitted Linear 1.00000 Ag 328.068 Fitted Linear 1.00000 TI 190.794 Fitted Linear 1.00000 Results and discussion The 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.

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