METHODS FOR SAMPLING AND
INORGANIC ANALYSIS OF COAL
U.S. Geological Survey
Bulletin 1823
Edited by D.W. Golightly and F.O. Simon
APPENDIX: REFERENCE MATERIALS FOR COAL ANALYSIS
By D.W. Golightly and F.O. Simon
The following tabulations list some of the reference materials available for use in the chemical analysis of coal. Data given in these tables are intended only to illustrate the degree to which the individual materials have been characterized. The analyst should always refer to specific certificates of analysis or other data provided directly by the supplier of the reference materials used.
Several coal standards now are being (or only recently have been) prepared by different laboratories; plans for preparation of these materials and available data are included in this section to alert the reader to these developments. The most significant program underway for the preparation and distribution of new coal standards is the Premium Coal Sample Program at Argonne National Laboratory. This program, described later, has produced eight new coal standards collected, analyzed, processed, and maintained for distribution to the coal research community. Important new coal and coal-ash standard reference materials for trace elements and radioactivity are expected to be available from the International Atomic Energy Agency in 1988. Also, the U.S. Geological Survey is preparing a new trace-element coal standard; preliminary data for this sample are included in this appendix.
SULFUR IN COAL: NBS STANDARDS 2682 THROUGH 2685
Sulfur | Furnace Ash | Higher Heating | ||
SRMa | Coal Type | % | % | Valueb MJ/kg |
2682 | Subbituminous | 0.47 | 6.37 | 27.08 |
2683 | Bituminous | 1.85 | 6.85 | 32.58 |
2684 | Bituminous | 3.00 | 11.09 | 29.21 |
2685 | Bituminous | 4.62 | 16.53 | 27.61 |
aSRM: Standard
Reference Material. bMoisture free. |
These SRMs are intended primarily for use as analytical standards for the determination of total sulfur in coal, ash content, and calorific value. Semiquantitative data for these SRMs are available from NBS on 32 elements, including carbon, hydrogen, and nitrogen.
Source: National Bureau of Standards (NBS) certificate of analysis for standard reference materials 2682, 2683, 2684, and 2685, February 25, 1985.
TRACE MERCURY IN COAL: NBS STANDARD 1630
Mercury concentration = 0.13m g/g |
CONCENTRATIONS OF ELEMENTS IN NBS-SRM COALS AND COAL FLY ASHa
Concentration, m g/gb | |||
Element or Property | 1632b | 1635 | 1633a |
Al(%) | 0.855 | (0.32) | 14.3 |
As | 3.72 | 0.42 | 145 |
Ba | 67.5 | - | (0.15) |
Be | - | - | (12) |
Br | (17) | - | - |
C(total, %) | 78.11 | - | - |
Ca | 0.204 | - | 1.11 |
Cd | 0.0573 | 0.03 | 1.0 |
Ce | (9) | (3.6) | (180) |
Cl | (1260) | - | - |
Co | 2.29 | (0.65) | (46) |
Cr | (11) | 2.5 | 196 |
Cs | (0.44) | - | (11) |
Cu | 6.28 | 3.6 | 118 |
Eu | (0.17) | (0.06) | (4) |
Fe(%) | 0.759 | 0.239 | 9.4 |
Ga | - | (1.05) | (58) |
H(%) | 5.07 | - | - |
Hf | (0.43) | (0.29) | (8) |
Hg | - | - | 0.16 |
K(%) | 0.0748 | - | 1.88 |
La | (5.1) | - | - |
Li | (10) | - | - |
Mg(%) | 0.0383 | - | 0.455 |
Mn | 12.4 | 21.4 | 179 |
Mo | (0.9) | - | (29) |
N(%) | 1.56 | - | - |
Na(%) | 0.0515 | (0.24) | 0.17 |
Ni | 6.10 | 1.74 | 127 |
Pb | 3.67 | 1.9 | 72.4 |
Rb | 5.05 | - | 131 |
S(%) | 1.89 | 0.33 | (0.18) |
Sb | (0.24) | (0.14) | 6.8 |
Sc | (1.9) | (0.63) | (40) |
Se | 1.29 | 0.9 | 10.3 |
Si(%) | (1.4) | - | 22.8 |
Sm | (0.87) | - | - |
Sr | (102) | - | 830 |
Th | 1.34 | 0.62 | 24.7 |
Ti(%) | 0.0454 | (0.02) | (0.8) |
Tl | - | - | 5.7 |
U | 0.436 | 0.24 | 10.2 |
V | (14) | 5.2 | 297 |
W | (0.48) | - | - |
Zn | 11.9 | 4.7 | 220 |
Ash(%) | 6.79 | - | - |
Calorific Value | |||
(MJ/kg) | 32.57 | - | - |
|
MINTEK COAL STANDARDS: SOUTH AFRICAN REFERENCE MATERIALSa
Concentration,m g/gb | |||
Element | SARM 18 |
SARM 19 |
SARM 20 |
Al(%) | 1.36 | 4.24 | 5.96 |
As | - | 7 | 4.7 |
B | (30) | (90) | (90) |
Ba | 78 | 304 | 372 |
Be | 4.1 | 2.8 | 2.5 |
Br | (3) | (2) | (2) |
Ca(%) | 0.13 | 0.99 | 1.34 |
Ce | 22 | 56 | 87 |
Cl | - | (32) | - |
Co | 6.7 | 5.6 | 8.3 |
Cr | 16 | 50 | (67) |
Cs | (1) | 1.4 | (2) |
Cu | 5.9 | 13 | 18 |
Eu | (0.3) | (0.7) | (1) |
Fe(%) | 0.20 | 1.22 | 0.82 |
Ga | (8) | 14 | 16 |
Ge | (8) | 13 | - |
Hf | 1.7 | 5.4 | 4.8 |
Hg | (0.04) | (0.2) | (0.25) |
K(%) | 0.12 | 0.20 | 0.12 |
La | 10 | 27 | 43 |
Li | (11) | (37) | (90) |
Mg(%) | 0.066 | 0.12 | 0.26 |
Mn | 22 | 157 | 80 |
Mo | (1) | (2) | - |
Na(%) | 0.0130 | 0.22 | 0.20 |
Nb | (6) | (10) | (16) |
Ni | 10.8 | 16 | 25 |
P | 30 | 130 | 610 |
Pb | (5) | 20 | 26 |
Rb | 8.1 | 9 | 10 |
S(%) | 0.56 | 1.49 | 0.51 |
Sb | (0.3) | (0.3) | (0.4) |
Sc | 4.3 | 7.6 | 10 |
Se | - | (1) | 0.8 |
Si(%) | 2.90 | 7.01 | 8.26 |
Sm | 2.0 | 4.9 | 6.3 |
Sn | (1.0) | (3) | (4) |
Sr | 44 | 126 | 330 |
Ta | (0.3) | (0.8) | 1.2 |
Tb | (0.3) | (0.7) | (0.9) |
Th | 3.4 | 12 | 18 |
Ti(%) | 0.0683 | 0.204 | 0.38 |
U | 1.5 | 5 | 4 |
V | 23 | 35 | 47 |
W | (2) | (2) | (3) |
Y | (12) | (20) | 29 |
Yb | - | (2) | (2) |
Zn | 5.5 | 12 | 17 |
Zr | 67 | 351 | (180) |
L.O.I.(%)c | 90.11 | 71.28 | 64.66 |
|
Property | Certified Value | 95% Conf. Interval |
Ash | 39.1 mg/g | 0.6 mg/g |
Sulfur | 8.3 mg/g | 0.2 mg/g |
Calorific Value | 34.915 kJ/g | 0.070 kJ/g |
Source: Catalogue of BCR Reference Materials, Commission of the European Communities, Community Bureau of Reference, Brussels, 1982. |
CRM 038 Fly Ash from Pulverized Coal
Element | Certified Concentration m g/g | 95 % Confidence Limit, m g/g |
As | 48.0 | 2.3 |
Cd | 4.6 | 0.3 |
Co | 53.8 | 1.9 |
Cu | 176 | 9 |
Fe | 338.10 | 7.10 |
Hg | 2.10 | 0.15 |
Mn | 479 | 16 |
Na | 374.10 | 15.10 |
Pb | 262 | 11 |
Zn | 581 | 29 |
Particle size = 0.5 to 10
m m. Source: Addendum to the Catalogue of BCR Reference Materials . |
PREMIUM COAL SAMPLE PROGRAM, ARGONNE NATIONAL LABORATORY
This program was established to provide a suite of eight different premium coal samples to serve as standards for comparison. Coal samples designated "premium" have been selected, collected, transported, processed, and stored, while the original conditions were closely maintained. The coals selected represent a range of coalification, maceral content, mineral composition, and commercial significance. Each sample is kept in an inert atmosphere during transportation and in all processing steps. Prepared samples are sealed in glass ampoules and carboys. Each coal has been characterized by physical and chemical methods. The analyses planned include proximate, ultimate, calorific value, sulfur forms, Gieseler plasticity, and others. Information is available from the manager of the Premium Coal Sample Program: Dr. Karl S. Vorres, Chemistry Division, Building 211, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, IL 60439, telephone 312-972-7374.
COAL AND COAL ASH STANDARDS FOR TRACE ELEMENTS AND RADIOACTIVITY, INTERNATIONAL ATOMIC ENERGY AGENCY
Reference materials for trace elements and radioactivity will be available in 1988. Information is available through Dr. R. Schelenz, Head, Chemistry Unit, Analytical Quality Control Services, International Atomic Energy Agency, P.O. Box 100, A-1400 Vienna, Austria.
Concentrationa, m g/g | Methodb | ||||
Element | AR-l800 | AR-1801 | AR-1802 | AR-1803 | |
Ag | 0.3a | 0.3a | 0.3a | 0.3a | C |
As | 5.0 | 6.1 | 52.0 | 4.8 | A |
B | 129 | 118 | 131 | 60 | B |
Be | 3.9 | 3.3 | 3.9 | 0.3 | C |
Cd | 0.2a | 0.2a | 0.2a | 0.2a | C |
Co | 15 | 11 | 7 | 1 | C |
Cr | 25 | 20 | 19 | 4 | C |
Cu | 24 | 18 | 19 | 10 | C |
F | 83 | 68 | 62 | 46 | D |
Ga | 15a | 15a | 15a | 15a | C |
Ge | 15 | 15 | 13 | - | C |
Hg | 0.03 | 0.04 | 0.32 | 0.05 | E |
Li | 32 | 17 | 13 | 4 | C |
Mn | 15 | 14 | 33 | 11 | C |
Mo | 2 | 2 | 3 | la | C |
Ni | 82 | 58 | 22 | 5 | C |
Pb | 8 | 8 | 64 | 4 | C |
Sb | 0.9 | 0.9 | 0.8 | 1.2 | A |
Se | 2.4 | 2.6 | 3.0 | 0.5 | F |
Sr | 92 | 127 | 114 | 558 | G |
Tl | 3a | 3a | 3a | 3a | C |
V | 53 | 28 | 36 | 11 | C |
Zn | 51 | 109 | 23 | 3 | C |
|
U.S. GEOLOGICAL SURVEY COAL STANDARD:
Preliminary Data for Whole Coala
Element | Concentration, m g/gb |
As | 20 |
Ba | <90 |
Br | 61 |
Ce | 8 |
Co | 4.1 |
Cr | 8.2 |
Cs | 0.2 |
Eu | 0.19 |
Fe(%) | 0.73 |
Hf | 0.3 |
Hg | 0.14 |
K(%) | <0.30 |
La | 5 |
Lu | 0.07 |
Na(%) | 0.02 |
Nd | <20 |
Rb | <20 |
Sb | 0.9 |
Sc | 1.5 |
Se | 1.9 |
Sm | 0.7 |
Sr | 38 |
Ta | 0.13 |
Tb | 0.14 |
Th | 1.2 |
U | 0.4 |
W | <2 |
Yb | 0.5 |
Zn | 43 |
aPreliminary
data are from instrumental neutron activation analysis of
whole coal, September 1983; S. Mee, analyst. bConcentration units are percent, that is, centigrams per gram, for the elements Fe, K, and Na. |
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