METHODS FOR SAMPLING AND INORGANIC ANALYSIS OF COAL
U.S. Geological Survey Bulletin 1823

Edited by D.W. Golightly and F.O. Simon

This manual presents a collection of detailed procedures used in geochemical laboratories of the U.S. Geological Survey for the chemical characterization of coal.

CONTENTS

Methods for Sampling and Inorganic Analysis of Coal - Introduction
By D.W. Golightly and F.O. Simon

Abstract
Introduction
References

Sampling of Coal Beds for Analysis
By R.W. Stanton

Abstract
Purposes of sampling a coal bed
Historical perspective of sampling
Sampling for rank classification
Sampling for chemical analysis
Sampling for other purposes
Procedure for channel sampling
Procedure for sampling drill core
Coal bed descriptions
Identification of carbonaceous shale layers
Sampling thick coal beds
Summary
References

Preparation of Coal for Analysis
By F.G. Walthall and S.L. Fleming, II

Abstract
Introduction
Equipment and procedures
     Sample preparation (grinding) laboratory - equipment
     Safety equipment and provisions
     Safety procedures
     Maintenance of equipment
     Sample preparation (grinding) laboratory - facilities
     Crushing and grinding
     Description of procedure
     Ashing procedure
     Cleaning of work area and equipment
References

Automated Semiquantitative Direct-Current Arc Spectrographic Determination of 64 Elements in Coal Ash

By A.F. Dorrzapf, Jr., C.J. Skeen, and W.B. Crandell

Abstract
Introduction
The method
Exposure procedure
The scanning microphotometer system
The minicomputer configuration
Data handling
Wavelength calibration
Concentration calibration
Spectral-interference corrections
Plate emulsion calibration
Quality control
Conclusions
References

The Determination of 4l Elements in Whole Coal by Instrumental Neutron Activation Analysis
By C.A. Palmer and P.A. Baedecker

Abstract
Introduction
Activation analysis
Experimental methods and procedures
     Sample preparation
     Standards
     Counting facilities
     Data reduction
     Quality control
Discussion
References

The Determination of Major and Minor Elements in Coal Ash and of Chlorine and Phosphorus in Whole Coal by X-Ray Fluorescence Spectrometry
By R.G. Johnson, G.A. Sellers, and S.L. Fleming, II

Abstract
Introduction
Experimental methods and procedures
     Equipment and supplies
     Coal ash
     Whole coal
Conclusions
References

Analysis of Coal Ash by Atomic Absorption Spectrometric and Spectrophotometric Methods
By F.W. Brown and Hezekiah Smith

Abstract
Introduction
Spectrophotometric procedures
Atomic absorption spectrometric methods
Precision of analysis
Preparation of sample solution
     Reagents and supplies
     Procedure
Determination of silicon (as SiO₂)
     Reagents and equipment
     Procedure
Determination of aluminum (as Al₂0₃)
     Reagents, supplies, and equipment
     Procedure
Determination of phosphorus (as P₂0₅)
     Reagents and equipment
     Procedure
Determination of titanium (as TiO₂)
     Reagents and equipment
     Procedure
Determination of calcium, iron, magnesium, manganese, potassium, and sodium
     Reagents and equipment
     Procedure for calcium, iron, magnesium, and manganese
     Procedure for potassium and sodium
Conclusions
References

The Determination of Selected Elements in Coal Ash by Atomic Absorption Spectrometry
By J .S. Kane

Abstract
Introduction
Experimental methods and procedures
     Dissolution of samples
     Cadmium extraction
     Calibration solutions
Instrumentation
Discussion of results
     Manganese
     Lead
     Zinc
     Copper
     Lithium
     Sodium
     Magnesium
     Cadmium
References

The Determination of Mercury in Whole Coal by Cold-Vapor Atomic Absorption Spectrometry
By P.J. Aruscavage and Roosevelt Moore

Abstract
Introduction
Experimental equipment and methods
     Equipment
     Reagents
     Calibration standards
     Coal standards
Procedures
     Dissolution of samples
     Determination of mercury
Discussion
References

The Determination of Fluoride in Coal by Ion-Selective Electrode
By Herbert Kirschenbaum

Abstract
Introduction
Experimental methods and procedures
     Equipment
     Reagents
     Procedure
Accuracy, precision, and detectability
References

The Determination of Forms of Sulfur in Coal
By Norma Rait and P.J. Aruscavage

Abstract
Introduction
Experimental equipment and methods
     Sample requirements
     Laboratory, supplies, and equipment
     Methods
          Total sulfur
          Laboratory setup for the separation of forms of sulfur
          Monosulfide sulfur separation and determination
          Sulfate sulfur separation and determination
          Pyritic sulfur separation and determination
          Calculation of organically bound sulfur
Discussion
References

Appendix: Reference Materials for Coal Analysis
By D.W. Golightly and F.O. Simon

Sulfur in coal: NBS standards 2682 through 2685
Trace mercury in coal: NBS standard 1630
Concentrations of elements in NBS-SRM coals and coal fly ash
MINTEK coal standards: South African reference materials
BCR reference materials
     CRM 065 coal
     CRM 038 fly ash from pulverized coal
Premium coal sample program, Argonne National Laboratory
Coal and coal-ash standards for trace elements and radioactivity, International Atomic Energy Agency
Trace metals in coal
Alpha Resources, Inc.
U.S. Geological Survey coal standard:
Preliminary data for whole coal

FIGURES

1. Flowchart for samples and analyses of coals
2. Correlation of facies of a single coal bed
3. Natural gamma and high-resolution density logs of a coal bed showing log responses of coal and impure coal or parting
4. Container for collection of core samples
5. Example of description of generalized stratigraphic section of the Upper Freeport coal bed
6. Ash yields of 134 facies samples of the Upper Freeport coal bed
7. X-ray radiograph of an undisturbed coal core showing mineral impurities and coal lithotype layers
8. Sample preparation laboratories
9. Sample preparation procedure for coals
10. Splitting procedure
11. Spectrum of NBS coal standard 1632 collected 5 days after irradiation
12. Lead absorbance as a function of iron concentration in the sample matrix
13. Zinc correlation plot
14. Diagram of arrangement of instrumentation for the measurement of mercury in coal
15. Two typical calibration curves
16. Flowchart for the separation of the forms of sulfur
17. Photograph of setup
18. Diagrams of apparatus

TABLES

1. Lower determination limits for elements in coal or coal ash, listed by method of analysis
2. Selected ASTM standard methods
3. Types of samples and purposes for which samples are commonly collected
4. Instrumentation and operating conditions
5. Spectral lines used in spectrographic analysis, listed in order of decreasing intensity
6. Direct current arc spectrographic analyses of NBS standard reference material coal fly ash
7. Long-lived (>10 h) radionuclides
8. Short-lived indicator radionuclides
9. Concentrations of 40 elements in multiple-element standards used for the analysis of coal
10. Interferences in INAA due to neutron-induced fission of (235)U
11. Instrumental operating conditions for XRF analysis of coal ash
12. Concentration ranges provided by rock standards for the XRF analysis of coal ash
13. XRF calibration of iron in coal ash: simple linear regression analysis results
14. Operating conditions for XRF analysis of whole coal
15. XRF calibration of P205 in whole coal: simple linear regression analysis results
16. Operating conditions for atomic absorption spectrometry
17. Estimated precision of analysis
18. Compositions of coal ashes determined by methods based on atomic absorption spectrometry (AAS) or spectrophotometry and on X-ray fluorescence (XRF) spectrometry
19. Operating parameters: flame and graphite-furnace atomization
20. Detection limits, sensitivities, and calibration ranges for flame and graphite-furnace atomic absorption spectrometry
21. Alternate operating parameters for flame atomic absorption spectrometry and calibration ranges
22. Concentrations of eight elements in the NBS 1633 coal fly ash determined by atomic absorption spectrometric methods
23. Concentrations of analytes determined for NBS standard reference material 1633a and for quality-control samples
24. Some typical concentration ranges of analytes in coal ashes originating from different regions of the United States
25. Concentrations of mercury determined by cold-vapor atomic absorption spectrometry for selected coal and fly-ash standards
26. Dilutions for preparation of individual calibration standards
27. Total sulfur in coal
28. Monosulfide sulfur in coal
29. Sulfate sulfur in coal
30. Pyritic sulfur in coal
31. Pyritic sulfur in coal by direct method
32. Organically bound sulfur in coal by direct method
33. Organically bound sulfur in coal by indirect method

ACRONYMS

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