ASTM D5600 Test Method for Trace Metals in Petroleum Coke by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
7. Apparatus
7.1 Balance, top loading, with automatic tare, capable of weighing to 0.0001 g, 150 g capacity.

7.2 Ceramic Cooling Plate, desiccator plates have been found effective.

7.3 Crucible Support, nichrome wire triangles.

7.4 Furnaces, electric, capable of regulation of temperature at 700 °C +/- 10 °C and 1000 °C +/- 10 °C, with allowances for exchange of combustion gases and air.

7.5 Inductively Coupled Plasma Atomic Emission Spectrometer - Either sequential or simultaneous spectrometer is suitable.

7.6 Magnetic Stirring Bars, polytetrafluoroethylene (PTFE) coated, approximately 12 mm (1/2 in.) in length.

7.7 Magnetic Stirring Hot Plate.

7.8 Meker-Type Forced Air Burner.

7.9 Nebulizer - A high-solids nebulizer is strongly recommended. This type of nebulizer reduces the possibility of clogging and minimizes aerosol particle effects.

7.10 Peristaltic Pump - A peristaltic pump is strongly recommended to provide a constant flow of solution.

7.11 Platinum Dish, 50 mL to 58 mL capacity.

7.12 Platinum Dish, 100 mL to 200 mL capacity.

7.13 Platinum-tipped Tongs.

7.14 Ring Stand, with crucible support.

7.15 Sieves, 0.250 mm (No. 60) and 0.075 mm (No. 200), conforming to Specification E11.

7.16 Tungsten Carbide Mill, laboratory size.

7.17 Vacuum Filtration Apparatus.

7.18 Filter Paper, sized to fit vacuum filtration apparatus, fine porosity, slow flow rate, 2.5 micron particle retention.

8. Reagents
8.1 Purity of Reagents - Reagent-grade chemicals shall be used in all tests. It is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination.

8.2 Purity of Water - Unless otherwise indicated, references to water shall be understood to mean Type II reagent water as defined in Specification D1193.

8.3 Argon Gas Supply, welding grade.

8.4 Lithium Borate, either, or a blend containing both.
8.4.1 Lithium Metaborate (LiBO2), powder (high purity).

8.4.2 Lithium Tetraborate (Li2B4O7), powder (high purity).

8.5 Solution No. 1, Hydrochloric Acid, 20 % by volume (400 mL of concentrated HCl diluted to 2000 mL with water).

8.6 Solution No. 2, Standard and Sample Solution Additive - Weigh 20.0 g +/- 0.1 g of lithium borate into a 100 mL to 200 mL platinum dish. Place in a furnace at 1000 °C for 5 min to fuse to a liquid. Remove and cool. Place the cooled platinum dish containing the fused recrystallized lithium borate and a magnetic stirring bar into a 2 L glass beaker. Add 1000 mL of Solution No. 1 (20 % HCl). Heat gently and stir the solution on a magnetic stirring hot plate until the lithium borate completely dissolves. After dissolution, remove the platinum dish with a glass rod. Rinse the platinum dish and glass rod with water into the lithium borate solution. Immediately transfer the warm solution quantitatively to a 2 L volumetric flask. Dilute to about 1800 mL with water to avoid crystallization. Mix the solution and cool to room temperature. Dilute to volume with water, mix thoroughly, and vacuum-filter the entire solution through filter paper.

NOTE 1 - Fifty millilitres of Solution No. 2 contains exactly 0.5 g lithium borate and 25 mL Solution No. 1.

8.7 Standard Stock Solutions - Prepare standard stock solutions from high purity (99.9 % or better) metals, oxides, or salts. Stock solutions of 1000 µg/mL (ppm) for each metal are needed for preparation of dilute standards in the range from <1.0 µg/mL to 50 µg/mL (ppm).

NOTE 2 - To minimize the potential of contamination, prepare the platinum ware by boiling in dilute HCl (5 volume % HCl + 95 volume % water) and rinsing thoroughly with water. After this initial cleaning, handle the platinum ware with clean platinum-tipped tongs and protect from all sources of contamination. Similarly acid clean all glassware used in the analyses.

NOTE 3 - Commercially available standards and other reagents solutions may be used in place of laboratory preparations.

8.8 Quality Control Materials - NIST SRM 2718A green petroleum coke or 2719 calcined petroleum coke can be used as QC materials for this analysis.