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The Chemical Analysis of Argonne Premium Coal Samples

Edited by Curtis A. Palmer

1997
U.S. Geological Survey Bulletin 2144


Determination of 62 Elements in 8 Argonne Premium Coal Ash Samples by Automated Semiquantitative Direct-Current Arc Atomic Emission Spectrography

By Carol J. Skeen, B.J. Libby, and W.B. Crandell

Table 1. Photoplate preparation conditions

[Table modified from Dorzapf and others (1989, table 4). A, ampere; ASTM, American Society for Testing and Materials; dc, direct current; L, liter; min, minute; s, second; V, volt]

Electrodes Cathode: ASTM type C-6, 50 mm long. Anode: 6.3-mm diameter, thin-walled graphite (Ultra Carbon no. 3170).
Electrode charge 15 mg sample + 30 mg graphite (type UCP-2, 200 mesh).
Spectrograph 3.4-m Ebert (Jarrell-Ash Mark III).
Power source 325 V, open circuit.
Excitation 15-A dc arc, set with empty graphite electrodes.
Arc gap 4 mm, maintained throughout arcing.
Exposure 20 s at 5 A followed by 130 s at 15 A, continuous arcing.
Atmosphere 70% Ar + 30% O 2 ; 6.6 L/min flow rate, with top of Helz jet nozzle 2 mm below top of electrode.
Wavelength range 230.0-470.0 nm; first order.
Grating 600 grooves/mm; 0.5 nm/mm reciprocal linear dispersion.
Slit 25 m wide and 2 mm high.
Filter 14% transmission neutral-density filter at slit.
Illumination Arc image focused on collimator by 450-mm focal-length cylindrical quartz lens at slit.
Mask at collimator 18 mm.
Emulsion Eastman-Kodak III-0 (102 508 mm plates).
Processing Eastman-Kodak D-19 developer,
3.25 min at 20C stirred by nitrogen bursts; Eastman-Kodak indicator stop bath, 30 s; Eastman-Kodak fixer,
10 min; wash, 20-30 min at 20C; Eastman-Kodak photo-flow, 1 min; and dry with warm air for 30 min.
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