ASTM D5600 Test Method for Trace Metals in Petroleum Coke by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
9. Sample Preparation
9.1 Crush and divide the gross sample to obtain a laboratory analysis sample. Crush to pass a 0.250 mm (No. 60) sieve using Practice D346.
9.2 Use a tungsten carbide mill to crush approximately a 30 g representative portion of the minus 0.250 mm (No. 60) sieve analysis sample, as prepared in 9.1, to pass through a 0.075 mm (No. 200) sieve. Dry this sample to constant mass at 110 °C to 115 °C and store in a desiccator until cool and needed for the analysis.
9.2.1 Preparation of the minus 0.075 mm analysis samples, from the minus 0.250 mm analysis samples, shall neither remove metals through loss nor increase metals through contamination. Full dissolution of the ash is required.
10. Preparation of Apparatus
10.1 ICP-AES Instrument - Consult the manufacturer's instructions for operation of the inductively coupled plasma atomic emission spectrometer.
10.2 Peristaltic Pump - When a peristaltic pump is used, inspect the pump tubing and replace it, as necessary, before starting each day. Verify the solution uptake rate and adjust it to the desired rate.
10.3 ICP Excitation Source - Initiate the plasma source at least 30 min before performing the analysis. Some manufacturers recommend even longer warm-up periods.
10.4 Wavelength Profiling - Perform any wavelength profiling that is required in the normal operation of the instrument.
10.5 Operating Parameters - Assign the appropriate operating parameter to the instrument task file so that the desired elements can be determined. Parameters to be included are element, wavelength, background correction points (optional), inter-element correction factors (optional), integration time, and internal standard correction (optional).
10.6 Each analyst shall determine the sensitivity and linear range of calibration of their own equipment and choose concentration ranges for standards compatible with the samples and instrument specific to their own work. Sample dilutions can be required for the determination of some elements (see 11.6).
10.7 The linear response range shall be established for each particular instrument being used. This is accomplished by running intermediate standards between the blank and the calibration standard and by running standards containing higher concentrations than the calibration standard within the linear range of response.
