NBSIR 81-2278

Test Procedures for the

Determination of the Gross

Calorific Value of Refuse and

Refuse- Derived -Fuel By

Conventional Bomb and Large

Bomb Calorimetry

SUMMARY QF THE 1979 FISCAL YEAR RESULTS

D. R. Kirklin, J. Colbert, P. Decker, S. Abramowitz, and E. S. Domalski

Chemical Thermodynamics Division

Center for Chemical Physics

U.S. Department of Commerce

National Bureau of Standards

Washington, DC 20234

June 1 981

Prepared for: U.S. Department of Energy

Assistant Secretary for

Conservation and Renewable Energy

Office of Energy from Municipal Waste

Washington, DC 20585

and

Q(L-

/0O

use.

If *7

C . *2—

'ironmental Protection Agency

I Environmental Research Laboratory

I Hazardous Waste Research Division

ti, OH 45268

NBSIR 81-2278

TEST PROCEDURES FOR THE

DETERMINATION OF THE GROSS

CALORIFIC VALUE OF REFUSE AND

REFUSE-DERIVED-FUEL BY

CONVENTIONAL BOMB AND LARGE

BOMB CALORIMETRY

SUMMARY OF THE 1979 FISCAL YEAR RESULTS

D. R. Kirklin, J. Colbert, P. Decker, S. Abramowitz, and E.

Chemical Thermodynamics Division

Center for Chemical Physics

U.S. Department of Commerce

National Bureau of Standards

Washington, DC 20234

June 1 981

Prepared for: U.S. Department of Energy

Assistant Secretary for

Conservation and Renewable Energy

Office of Energy from Municipal Waste

Washington, DC 20585

and

U.S. Environmental Protection Agency

Municipal Environmental Research Laboratory

Solid and Hazardous Waste Research Division

Cincinnati, OH 45268

S. Domalski

U.S. DEPARTMENT OF COMMERCE, Malcolm 3aldrige, Secretary

NATIONAL BUREAU OF STANDARDS, Ernest Ambler, Director
mm

111
Table of Contents

Abstract

I. Introduction

II. Experimental

A. Materials

1 . Benzoic Acid

2. Oxygen

3. ASTM Round Robin RDF-3 Samples

(a) First Round Robin Sample

(b) Second Round Robin Sample

(c) Third Round Robin Sample

(d) Bituminous Coal Round Robin Sample

4. Teledyne National RDF

(a) RDF Pellets

(b) RDF-3 (Fluff) Sample

5. ECO FUEL-II RDF

6. Americology RDF-3 (Fluff)

7. New Castle County, Delaware MSW

8. Steam Size Reduction RDF

9. NCRR Storage Pit RDF (Charred Storage Sample)

10.

NCRR RDF (Low Ash Sample)

B. Oxygen Bomb Calorimeters

1. 2.5 gram capacity bomb calorimeter

2. 25 gram capacity bomb calorimeter
C. Sample Preparation Apparatus

1. Steelman 450°F Electric Bake Oven

2. W. W. Grinder Corporation Hammer Mill

3. Wiley Model 4 Laboratory Mill

4. Patters on -Kelley Company

Twin Shell Dry Blenders

5. Carver Laboratory Press, Model M

D. Sample Preparation Procedure

1. Sample Drying

2. Particle Size Reduction

3. Sample Homogenization

4. Preparation of Pelletized Analysis Sampl

E. Calorimetric Procedure

III. Results and Discussion

A. Bomb Calorimetric Measurements

1. General Discussion

2. Test Procedures

3. Sample Preparation

4. Bomb Preparation

5. Calorimeter Preparation

6. Temperature Measurements

7. Calorimeter Corrections

3. Calculation of the Calorific Value

B. Calibration of the Calorimeters

1. NBS 2.5 gram Capacity Bomb Calorimeter

2. NBS 25 gram Capacity Bomb Calorimeter
C. Calorimetric Measurements on RDF

1. ASTM Subcommittee E-38.01 Round Robin Testing on RDF-3

a. First Round Robin Sample

b. Second Round Robin Sample

c. Third Round Robin Sample

d. Bituminous Coal Sample

2. Americology RDF Sample

3. Large and Small Calorimeter Comparison Measurements

a. Teledyne National Sample

b. ECO FUEL-I I RDF

c. Americology RDF

4. Bureau of Mines Processing of New Castle County, Delaware MSW

5. Representative or Unique RDF's

a. Teledyne National RDF.

r> b. Steam Size Reduction RDF

c. NCRR Storage Pile RDF

d. NCRR Low Ash RDF

IV. Summary and Conclusions

V. References

Appendix A

Evaluation of Data on Higher Heating Values Determined during ASTM Round

Robin Testing of RDF-3

Appendix B

Large Isoperibol Bomb Calorimeter
Appendix C

Emission Spectrochemi cal Analysis of Bomb Residues

1. Teledyne National RDF

2. ECO FUEL-II RDF

3. Ameri oology RDF

Appendix D

Conversion Table for the Calculation of Data to Different Bases

Appendix E

Calculation of Total Moisture in an RDF Sample

Acknowledgement

v
List of Tables

Table 1

Table 2

Table 3

Table 4

Table 5

• fable 6

Table 7

Table 8

Energy Equivalent Values Determined During FY 1979,

(2.5 Gram Capacity Bomb Calorimeter)

Determination of the Energy Equivalent,

Calibration Experiments on Standard Sample Benzoic Acid,

(2.5 Gram Capacity Bomb Calorimeter, Six Typical Experiments)

Determination of the Energy of Combustion of "Commercial" Benzoic Acid,

(2.5 Gram Capacity Bomb Calorimeter)

Determination of the Energy Equivalent,

Calibration Experiments on "Commercial" Benzoic Acid,

(25 Gram Capacity Bomb Calorimeter)

Determination of Calorific Values, ASTM Round Robin Testing of RDF-3

(Fi rst Round)

,

(2.5 Gram Capacity Bomb Calorimeter)

Determination of Residual Moisture, Ash, and Sulfur Content,

ASTM Round Robin Testing of RDF-3 (First Round),

(2.5 Gram Capacity Bomb Calorimeter),

(Samples Equilibrated at 45% R.H.)

Determination of Residual Moisture, Ash, and Sulfur Content,

ASTM Round Robin Testing of RDF-3 (First Round),

(2.5 Gram Capacity Bomb Calorimeter),

Dried Samples at 105°C

Calorific Values Calculated to Different Bases,

ASTM Round Robin Testing of RDF-3 (First Round),

(2.5 Gram Capacity Bomb Cal orimeter )

,

Samples Equilibrated at 45% R.H.

vi
Table 9 Calorific Values Calculated to Different Bases,

Table 10

Table 11

Table 12

Table 13

Table 14

Table 15

ASTM Round Robin Testing of RDF-3 (First Round),

(2.5 Gram Capacity Bomb Calorimeter)

Dried Samples at 105°C

Determination of Calorific Values,

ASTM Round Robin Testing of RDF-3 (Second Round),

(2.5 Gram Capacity Bomb Calorimeter)

Determination of Residual Moisture, Ash, and Sulfur Content,

ASTM Round Robin Testing of RDF-3 (Second Round),

Interlab Comparison Sample,

(2.5 Gram Capacity Bomb Calorimeter)

Determination of Residual Moisture, Ash, and Sulfur Content,

ASTM Round Robin Testing of RDF-3 (Second Round),

RDF-3 Processed to 0.5mm Powder,

(2.5 Gram Capacity Bomb Calorimeter)

Calorific Values Calculated to Different Bases,

ASTM Round Robin Testing of RDF-3 (Second Round),

Interlab Comparison Sample,

(2.5 Gram Capacity Bomb Calorimeter)

Calorific Values Calculated to Different Bases,

ASTM Round Robin Testing of RDF-3 (Second Round)

RDF-3 Processed to 0.5mm Powder,

(2.5 Gram Capacity Bomb Calorimeter)

Determination of Calorific Values

ASTM Round Robin Testing of RDF-3 (Third Round),

(2.5 Gram Capacity Bomb Calorimeter)

vii
Table 16

Table 17

Table 18

Table 19

Table 20

Table 21

Table 22

Determination of Residual Moisture, Ash, and Sulfur Content,

ASTM Round Robin Testing of RDF-3 (Third Round),

Interlab Comparison Sample,

(2.5 Gram Capacity Bomb Calorimeter)

Determination of Residual Moisture, Ash, and Sulfur Content,

ASTM Round Robin Testing of RDF-3 (Third Round),

RDF-3 Processed to 0.5mm Powder,

(2.5 Gram Capacity Bomb Calorimeter)

Calorific Values Calculated to Different Bases,

ASTM Round Robin Testing of RDF-3 (Third Round),

Interlab Comparison Sample,

(2.5 Gram Capacity Bomb Calorimeter)

Calorific Values Calculated to Different Bases,

ASTM Round Robin Testing of RDF-3 (Third Round)

RDF-3 Processed to 0.5mm Powder,

(2.5 Gram Capacity Bomb Calorimeter)

Determination of Calorific Values,

ASTM Round Robin Testing of RDF-3,

NBS (SRM 1632a) Bituminous Coal Sample,

(2.5 Gram Capacity Bomb Calorimeter)

Determination of Residual Moisture, Ash, and Sulfur Content,

ASTM Round Robin Testing of RDF-3,

NBS (SRM 1632a) Bituminous Coal Sample,

(2.5 Gram Capacity Bomb Calorimeter)

Calorific Values Calculated to Different Bases,

ASTM Round Robin Testing of RDF-3,

NBS (SRM 1632a) Bituminous Coal Sample,

(2.5 Gram Capacity Bomb Calorimeter)
Table 23 Determination of Calorific Values,

Americology RDF, “Grab" Sample,

(2.5 Gram Capacity Bomb Calorimeter)

Table 24 Determination of Residual Moisture, Ash, and Sulfur Content,

Americology RDF “Grab" Sample,

(2.5 Gram Capacity Bomb Calorimeter)

Table 25 Calorific Values Calculated to Different Bases,

Americology RDF “Grab" Sample,

(2.5 Gram Capacity Bomb Calorimeter)

Table 26 Determination of Calorific Values,

Americology RDF, Representative Sample,

(2.5 Gram Capacity Bomb Calorimeter)

Table 27 Determination of Residual Moisture, Ash, and Sulfur Content,

Americology RDF, Representative Sample,

(2.5 Gram Capacity Bomb Calorimeter)

Table 28 Calorific Values Calculated to Different Bases,

Americology RDF, Representative Sample,

(2.5 Gram Capacity Bomb Calorimeter)

Table 29 Determination of Calorific Values,

Calorimeter Comparison Measurements,

Teledyne National RDF,

(2.5 Gram Capacity Bomb Calorimeter)

Table 30 Determination of Calorific Values,

Calorimeter Comparison Measurements,

Teledyne National RDF,

(25 Gram Capacity Bomb Calorimeter)

IX
Calorimeter Comparison Measurements,

Teledyne National RDF,

(2.5 Gram Capacity Bomb Calorimeter)

(25 Gram Capacity Bomb Calorimeter)

Table 32 Calorific Values Calculated to Different Bases,

Calorimeter Comparison Measurements,

Teledyne National RDF,

(2.5 Gram Capacity Bomb Calorimeter)

(25 Gram Capacity Bomb Calorimeter)

Table 33 Determination of Calorific Values,

Calorimeter Comparison Measurements

ECO FUEL-II RDF,

(2.5 Gram Capacity Bomb Calorimeter)

Table 34 Determination of Calorific Values,

Calorimeter Comparison Measurements,

ECO FUEL-II RDF

(25 Gram Capacity Bomb Calorimeter)

Table 35 Determination of Residual Moisture, Ash, and Sulfur Content,

Calorimeter Comparison Measurements,

ECO FUEL-II RDF,

(2.5 Gram Capacity Bomb Calorimeter)

(25 Gram Capacity Bomb Calorimeter)

Table 36 Calorific Values Calculated to Different Bases,

Calorimeter Comparison Measurements,

ECO FUEL-II RDF

(2.5 Gram Capacity Bomb Calorimeter)

,

(25 Gram Capacity Bomb Calorimeter)

Table 37 Determination of Calorific Values

I Calorimeter Comparison Measurements,

| Ameri col ogy RDF,

(2.5 Gram Capacity Bomb Calorimeter)

x
Table 38 Determination of Calorific Values,

Calorimeter Comparison Measurements,

Americology RDF,

(25 Gram Capacity Bomb Calorimeter)

Table 39 Determination of Residual Moisture, Ash, and Sulfur Content,

Calorimeter Comparison Measurements,

Americology RDF,

(2.5 Gram Capacity Bomb Calorimeter)

,

(25 Gram Capacity Bomb Calorimeter)

Table 40 Calorific Values Calculated to Different Bases,

Calorimeter Comparison Measurements,

Americology RDF,

(2.5 Gram Capacity Bomb Calorimeter)

,

(25 Gram Capacity Bomb Calorimeter)

Table 41 Determination of Calorific Values,

New Castle County, Delaware MSW, Processed

Through the Bureau of Mines Facility, College Park, Md.

,

(25 Gram Capacity Bomb Calorimeter)

Table 42 Determination of Calorific Values,

New Castle County, Delaware MSW, Processed

Through the Bureau of Mines Facility, College Park, Md.

,

(25 Gram Capacity Bomb Calorimeter)

Table 43 Determination of Calorific Values,

New Castle County, Delaware MSW, Processed

Through the Bureau of Mines Facility, College Park, Md.

,

(25 Gram Capacity Bomb Calorimeter)

xi
Table 44 Determination of Calorific Values,

New Castle County, Delaware MSW, Processed

Through the Bureau of Mines Facility, College Park. Md.

,

(25 Gram Capacity Bomb Calorimeter)

Table 45 Determination of Air Dry Loss, Residual Moisture, Ash, and Sulfur Content,

New Castle County, Delaware MSW, Processed

Through the Bureau of Mines Facility, College Park., Md.

,

Cyclone No. 1, Secondary Shred, 2 Inch Pieces,

Total Weight of Sample, 3268.3 Grams,

(25 Gram Capacity Bomb Calorimeter)

Table 46 Determination of Air Dry Loss, Residual Moisture, Ash, and Sulfur Content,

New Castle County, Delaware MSW, Processed

Through the Bureau of Mines Facility, College Park, Md.

,

Cyclone No. 1, Trommel Undersize, +14 Mesh,

Total Weight of Sample, 2237.5 Grams,

(25 Gram Capacity Bomb Calorimeter)

Table 47 Determination of Air Dry Loss, Residual Moisture, Ash, and Sulfur Content,

New Castle County, Delaware MSW, Processed

Through the Bureau of Mines Facility, College Park, Md.

,

Cyclone No. 2, Secondary Shred, 2 Inch Pieces,

Total Weight of Sample, 2672.5 Grams,

(25. Gram Capacity Bomb Calorimeter)

Table 48 Determi nation of Air Dry Loss, Residual Moisture, Ash, and Sulfur Content,

New Castle County, Delaware MSW, Processed

Through the Bureau of Mines Facility, College Park, Md.

,

Cyclone No. 2, Trommel Undersize, +14 Mesh,

Total Weight of Sample, 2361.2 Grams,

(25 Gram Capacity Bomb Calorimeter)
Table 49 Determination of Air Dry Loss, Residual Moisture, Ash, and Sulfur Content,

New Castle County, Delaware MSW, Processed

Through the Bureau of Mines Facility, College Park, Md.

,

Secondary Shred, Cyclone No. 3, As-Collected,

Total Weight of Sample, 3540.4 Grams,

(25 Gram Capacity Bomb Calorimeter)

Table 50 Determination of Air Dry Loss, Residual Moisture, Ash, and Sulfur Content,

New Castle County, Delaware MSW, Processed

Through the Bureau of Mines Facility, College Park, Md.,

Heavy Organic Combustibles,

Total Weight of Sample, 3664.8 Grams,

(25 Gram Capacity Bomb Calorimeter)

Table 51 Determination of Air Dry Loss, Residual Moisture, Ash, and Sulfur Content

New Castle County, Delaware MSW, Processed

Through the Bureau of Mines 'Facility, College Park, Md.

,

Organic Wastes, Jig Overflow,

Total Weight of Sample, 3202.1 Grams,

(25 Gram Capacity Bomb Calorimeter)

Table 52 Calorific Values Calculated to Different Bases,

New Castle County, Delaware MSW, Processed

Through the Bureau of Mines Facility, College Park, Md.

,

Cyclone No. 1, Secondary Shred, 2 Inch Pieces,

(25 Gram Capacity Bomb Calorimeter)

Table 53 Calorific Values Calculated to Different Bases,

New Castle County, Delaware MSW, Processed

Through the Bureau of Mines Facility, College Park, Md.

,

Cyclone No. 2, Secondary Shred, 2 Inch Pieces,

(25 Gram Capacity Bomb Calorimeter)

xi i i
I' Table 54 Calorific Values Calculated to Different Bases,

New Castle County, Delaware MSW, Processed

Through the Bureau of Mines Facility, College Park, Md

Secondary Shred, Cyclone No. 3, As-Collected,

(25 Gram Capacity Bomb Calorimeter)

Table 55 Calorific Values Calculated to Different Bases,

New Castle County, Delaware MSW, Processed

Through the Bureau of Mines Facility, College Park, Md

Cyclone No. 1, Trommel Undersize, +14 Mesh,

(25 Gram Capacity Bomb Calorimeter)

Table 56 Calorific Values Calculated to Different Bases,

New Castle County, Delaware MSW, Processed

Through the Bureau of Mines Facility, College Park, Md

Cyclone No. 2, Trommel Undersize, +14 Mesh,

(25. Gram Capacity Bomb Calorimeter)

Table 57 Calorific Values Calculated to Different Bases,

New Castle County, Delaware MSW, Processed

Through the Bureau of Mines Facility, College Park, Md

Heavy Organic Combustibles,

(25 Gram Capacity Bomb Calorimeter)

Table 58 Calorific Values Calculated to Different Bases,

New Castle County, Delaware MSW, Processed

Through the Bureau of Mines Facility, College Park, Md

Organic Wastes, Jig Overflow,

(25 Gram Capacity Bomb Calorimeter)

Table 59 Determination of Calorific Values

Teledyne National RDF, Single Stage Moisture,

(2.5 Gram Capacity Bomb Calorimeter)

xi v
Table 60 Determination of Residual Moisture, Ash, and Sulfur Content,

Table 61

Table 62

Table 63

Table 64

Table 65

Table 66

Table 67

Table 68

Teledyne National RDF, Single Stage Moisture,

(2.5 Gram Capacity Bomb Calorimeter)

Calorific Values Calculated to Different Bases,

Teledyne National RDF, Single Stage Moisture,

(2.5 Gram Capacity Bomb Calorimeter)

Determination of Calorific Values,

Teledyne National RDF, Two Stage Moisture,

(2.5 Gram Capacity Bomb Calorimeter)

Determination of Residual Moisture, Ash, and Sulfur Content,

Teledyne National RDF, Two Stage Moisture,

(2.5 Gram Capacity Bomb Calorimeter)

Calorific Values Calculated to Different Bases,

Teledyne National RDF, Two Stage Moisture

(2.5 Gram Capacity Bomb Calorimeter)

Determination of Calorific Values,

Steam Size Reduction RDF,

(2.5 Gram Capacity Bomb Calorimeter)

Determination of Residual Moisture, Ash, and Sulfur Content

Steam Size Reduction RDF,

(2.5 Gram Capacity Bomb Calorimeter)

Calorific Values Calculated to Different Bases,

Steam Size Reduction RDF,

(2.5 Gram Capacity Bomb Calorimeter)

Determination of Calorific Values,

NCRR Storage Pit RDF, Charred Storage Sample,

(25 Gram Capacity Bomb Calorimeter)

xv
Table 69

Table 70

Table 71

Table 72

Table 73

Table 74

Determination of Residual Moisture, Ash, and Sulfur Content,

NCRR Storage Pit RDF, Charred Storage Sample,

(25 Gram Capacity Bomb Calorimeter)

Calorific Values Calculated to Different Bases,

NCRR Storage Pit RDF, Charred Storage Sample,

(25 Gram Capacity Bomb Calorimeter)

Determination of Calorific Values,

NCRR (Low Ash) RDF Sample,

(2.5 Gram Capacity Bomb Calorimeter)

Determination of Residual Moisture, Ash, and Sulfur Content,

NCRR (Low Ash) RDF Sample,

(2.5 Gram Capacity Bomb Calorimeter)

Calorific Values Calculated to Different Bases,

NCRR (Low Ash) RDF Sample,

(2.5 Gram Capacity Bomb Calorimeter)

Summary of Mean Calorific Values,

Obtained for Measurements,

on RDF i n Btu* 1 b""'
Appendix A

Table 1

Table 2

Table 3

Table 4

Table 5

Table 6

Table 7

Table 8

Table 9

RDF-3 Testing Program

ASTM Round Robin Testing of RDF-3 (First Round),

Statistical Data on Higher Heating Values,

RDF-3 Sample Prepared by NCRR

ASTM Round Robin Testing of RDF-3 (First Round),

Statistical Data on Total Moisture, Residual Moisture, and Ash,

RDF-3 Sample Prepared by NCRR

ASTM Round Robin Testing of RDF-3 (Second Round),

Statistical Data on Higher Heating Values,

RDF-3 Sample Prepared by NCRR

ASTM Round Robin Testing of RDF-3 (second Round),

Statistical Data on Total Moisture, Residual Moisture, and Ash,

RDF-3 Sample Prepared by NCRR

ASTM Round Robin Testing of RDF-3 (Second Round),

Statistical Data on Higher Heating Values,

RDF-3 Interlaboratory Comparison Sample Prepared by Wisconsin Electric

ASTM Round Robin Testing of RDF-3 (Second Round)

Statistical Data on Residual Moisture and Ash,

RDF-3 Interlaboratory Comparison Sample Prepared by Wisconsin Electric

ASTM Round Robin Testing of RDF-3 (Third Round),

Statistical Data on Higher Heating Values,

RDF-3 Sample Prepared by Americology

ASTM Round Robin Testing of RDF-3 (Third Round),

Statistical Data on Total Moisture, Residual Moisture, and Ash

RDF-3 Sample Prepared by Americology

xvi 1
Table 10

Table 11

Table 12

Table 13

Table 14

Table lb

Table 16

Table 17

ASTM Round Robin Testing of RDF-3 (Third Round),

Statistical Data on Higher Heating Values,

RDF-3 Interlaboratory Comparison Sample Prepared by ORNL

ASTM Round Robin Testing of RDF-3 (Third Round)

Statistical Data on Residual Moisture and Ash,

RDF-3 Interlaboratory Comparison Sample Prepared at ORNL

ASTM Round Robin Testing of RDF-3,

Statistical Data on Higher Heating Values,

Coal Sample (SRM 1632a) Distributed by NBS

ASTM Round Robin Testing of RDF-3,

Statistical Data on Residual Moisture and Ash,

Coal Sample (SRM 1632a) Distributed by NBS

Summary of Repeatability and Reproducibility Intervals,

For Higher Heating Value HHV2, Dry Basis,

In ASTM Round Robin Testing of RDF-3

Summary of Repeatability and Reproducibility,

Of Total Moisture in ASTM Round Robin Testing of RDF-3

Summary of Repeatability and Reproducibility,

For Residual Moisture in ASTM Round Robin Testing of RDF-3

Summary of Repeatability and Reproducibility Intervals,

For Ash Content in ASTM Round Robin Testing of RDF-3

Appendix C

Table 1 Emission Spectrochemical Analysis of

Teledyne National RDF Bomb Residue [1]

Table 2 Emission Spectrochemical Analysis of ECO FUEL- 1 1 RDF Bomb Residue

fable 3 Emission Spectrochemical Analysis of ECO FUEL- 1 1 RDF (As-Received)

Table 4 Emission Spectrochemical Analysis of Americology RDF Bomb Residue
Table 5 Emission Spectrochemical Analysis of Ameri oology RDF processed

to 0.5mm Particle Size

Appendix D

Conversion Table for the Calculation of Data to Different Bases

Conversion Formula Table

xi x
List of Figures

Figure 1 U.S. Bureau of Mines, College Park, Md.

Resource Recovery Facility

Overall Flow-Diagram for Processing MSW

Figure 2 U.S. Bureau of Mines, College Park, Md.

Resource Recovery Facility:

MSW is shredded by a primary shredder; the light fraction is

separated by a light air classifier and collected in cyclone

No. 1; the large particles are separated by a trommel and

reshredded by a secondary shredder.

Figure 3 U.S. Bureau of Mines, College Park, Md.

Resource Recovery Facility:

MSW is shredded by a primary shredder; the light fraction is .

.separated by a light air classifier and collected in cyclone

No. 1; the small particles are separated by a trommel with

3/4 inch openings and further separated from fine glass and

dirt by a No. 14 mesh screen.

Figure 4 U.S. Bureau of Mines, College Park, Md.

Resource Recovery Facility:

MSW is shredded by a primary shredder; the heavy fraction is

separated from the light fraction by a light air classifier;

ferrous metals are removed from this heavy fraction by a magnetic

separator; and the light portion of this heavy fraction is separated

by a primary air classifier and collected in cyclone No. 2; the large

particles are separated by a trommel and reshredded by the

secondary shredder.

xx
Figure 5 U.S. Bureau of Mines, College Park, Md.

Resource Recovery Facility:

MSW is shredded by a primary shredder; the heavy fraction is

separated from the light fraction by a light air classifier;

ferrous metals are removed from this heavy fraction by a magnetic

separator and the light portion of this heavy fraction is separated

by a primary air classifier and collected in cyclone No. 2; the

small particles are separated from the large particles by a trommel

with 3/4 inch openings and further separated from fine glass and

dirt by a No. 14 mesh screen.

Figure 6 U.S. Bureau of Mines, College Park, Md

Resource Recovery Facility:

MSW is shredded by the primary shredder; the heavy fraction is

separated from the light fraction by the light air classifier;

ferrous metals are removed from this heavy fraction by a magnetic

separator and the heavy portion of this heavy fraction is separated

by the primary air classifier; the large particles of this heavy

portion are separated by a trommel and reshredded by the secondary

shredder; the lighter portion is then removed by the secondary air

classifier and collected in cyclone No. 3

•

XXI
Figure 7

Figure 8

U.S. Bureau of Mines, College Park, Md.

Resource Recovery Facility:

MSW is shredded by the primary shredder; the heavy fraction is

separated from the light fraction by the light air classifier;

ferrous metals are removed from this heavy fraction by a magnetic

separator; and the heavy portion of this heavy fraction is

separated by the primary air classifier; the large particles

of this heavy portion are separated by a trommel and reshredded

by the secondary shredder; the heavier portion is then separated

from the lighter portion by the secondary air classifier;

aluminum is removed from this heavier portion by an electrostatic

separator leaving only the heavy organic material.

U.S. Bureau of Mines, College Park, Md.

Resource Recovery Facility:

MSW is shredded by the primary shredder; the heavy fraction is

separated from the light fraction by the light air classifier;

ferrous metals are removed from this heavy fraction by a magnetic

separator and the heavier portion of this heavy fraction is

separated by the primary air classifier; the small particles of

this heavy portion are separated by a trommel with 3/^ inch

openings and allowed to fall into a mineral jig filled with

water and the organic wastes are floated off the top of the

mineral jig.

xx i i
Appendix A

Figure 1 RDF-3 Reduced to 0.5

Magn i f i ed 50 Times

,

(Each square is 0.25

Figure 2 RDF-3 Reduced to 0.5

Magn i f i ed 50 Times

,

(Each square is 0.25

Figure 3 SRM 1632a Bituminous

Magn i f i ed 50 Times

,

(Each square is 0.25

mm,

mm on a side)

mm,

mm on a side)

Coal Sample,

mm on a side)

Appendix B

Figure 1 25 Gram Capacity Bomb Calorimeter

Figure 2 Inner Arrangement of Large Combustion Bomb

xx i i i
TEST PROCEDURES FOR THE DETERMINATION OF THE

GROSS CALORIFIC VALUE OF REFUSE-DERIVED-FUEL

BY CONVENTIONAL BOMB AND LARGE BOMB CALORIMETRY

SUMMARY OF THE 1979 FISCAL YEAR RESULTS

D.R. Kirklin, J. Colbert, P. Decker/ S. Abramowitz, and E.S. Domalski

National Bureau of Standards

Washington, D.C. 20234

ABSTRACT

This report provides the results of investigations during fiscal year 1979

to develop test procedures for the determination of the calorific value of refuse

and refuse-derived-fuel (RDF) by means of oxygen bomb calorimetry. The results

of' 138 calorimetric measurements are discussed, along with 32 calorimeter

calibration measurements, for 20 different RDF samples. In addition,

determinations have been carried out on these RDF samples for air dry loss,

residual moisture, furnace ash, bomb ash, and sulfur content to correct the

calorimetric data for their presence; the latter group of measurements amounts

to 283 experiments.

The calorimetric (and related) measurements can be categorized into five

classes: (1) measurements carried out in conjunction with ASTM round robin

testing of RDF-3, (2) measurements on an Americology RDF extracted using both

selective and non-selective sampling methods, (3) measurements required to

compare data obtained from the small (2.5 gram capacity) and large (25 gram

Summer student from the University of Maryland, Baltimore County

Campus during the summer of 1978 and 1979.

1
capacity) bomb calorimeters, (4) measurements carried out in the large

bomb calorimeter on seven processed samples of different particles sizes

obtained from New Castle County, Delaware MSW, and (5) measurements on

some RDF's of special interest.

Five appendices include additional information on: the evaluation

of data on higher heating values obtained during ASTM round robin testing

of RDF-3, the large bomb calorimeter, spectrochemical analysis of bomb

residues, conversion tables, and calculation of total moisture in a RDF

sample.

An evaluation of data on higher heating values determined during the

ASTM round robin testing of RDF-3 showed that the repeatabi 1 i ty (within-lab

agreement) and reproducibility (between-lab agreemtn) are 250 and 750

Btu/lb when values are converted to a dry basis. These variabilities

are 5 and 7.5 times greater, respectively, than the precision levels

accepted in ASTM protocols for determining the higher heating values of

coal or coke on a dry basis (see Appendix A).

Measurements on three RDF samples in both small (2.5 gram-capacity)

and large (25 gram-capacity) bomb calorimeters showed that equivalent

high precision can be obtained in both calorimeters. The large bomb

calorimeter has the advantage that it can accommodate RDF samples whose

particle size is as large as 25 mm (1 inch).

The mean and standard deviation of the calorific values obtained for

20 different RDF samples give 9482 and 553 Btu/lb, respecti vely , on a

moisture-ash free basis using the furnace ash method to determine the

ash content. Thse results support the generally accepted value of

9500 Btu/lb as the higher heating value for RDF on a moisture-ash

free basis.

2
I. Introduction

This report provides the results of an investigation which was

carried out at the National Bureau of Standards during fiscal year 1979

under a research agreement with the U.S. Department of Energy and the U.S.

Environmental Protection Agency on the development of test procedures to

determine the calorific values of refuse and refuse-derived-fuel (RDF) by

means of oxygen bomb calorimetry. This is the third report of studies on

the development of such test procedures. Earlier reports [1,2]

+ should be

consulted to obtain further information on the efforts in fiscal years

1977 and 1973.

This investigation responds to the Resource Conservation and Recovery

Act of 1976 (PL 94-580) in which the National Bureau of Standards has been

mandated to furnish guidelines for the development of specifications for

materials which can be recovered from wastes and have been otherwise destined

for disposal. The specifications refer to the physical and chemical properties

and related characteri sties of such materials.

The results of this report are of interest to the Committee on

Performance Test Codes for Large Incinerators (PTC-33) of the American

Society for Mechanical Engineers (ASME). This committee has indicated the

need to find more accurate test methodology for the determination of calorific

values of refuse samples which will more reliably represent the heterogeneous

array of orignal solid waste. It is the opinion of many engineers that one

cannot accurately sample a multi -ton pile of refuse down to a few grams for bomb

calorimeter measurement. In addition, these engineers suggest that size reduction

to small particle dimensions (i.e., 2 mm or 0.5 mm) could alter the chemical

nature of this heterogenoeous material. The latter assumption is somewhat severe;

+ Number in brackets identify references at the end of this report.

3
however, experimental evidence which would confirm or disprove this idea is needed.

If improved test methodology to determine the calorific value of refuse and RDF could

be found, a better means would be available to evaluate whether or not

large incinerators or refuse-fired boilers are in compliance with their

contract performance specification.

The results of this report are also of interest to Committee E-38

on Resource Recovery of the American Society for Testing and Materials (ASTM).

This committee is involved in the development and publication of test

procedures needed to characterize RDF so that it can be established as an

article of commerce. A laboratory procedure which yields reproducible results

will better equip commercial testing laboratories to certify accurately the

energy content of RDF of various compositions. As an article of commerce

RDF can be bought and sold as a regulated low-sulfur fuel to supplement

1 coal -fired systems.

Project Objectives

The major objectives of this research project are:

(1) to investigate the size reduction and homogenization required to

obtain representati ve samples of refuse and RDF,

(2) to evaluate calorimetric methods for conventional-size (2.5 gram

capacity) combustion bomb calorimeters and an NBS large (25 gram capacity)

combustion bomb cal orimeter; and

(3) to develop test procedures for determining the calorific value of

refuse and RDF samples using bomb calorimetric methods.

4
One of the most significant property of a fuel is its heating value (calorific

value). For the past 100 years, the calorific value of solid fuels has

been determined in a reliable way by the methods of oxygen bomb calorimetry.

Traditionally, small (1-3 gram) samples are burned in an oxygen bomb

calorimeter to estimate the calorific value of gross quantities of a fuel.

Since the techniques of oxygen bomb calorimetry are well understood, the

accuracy of estimating the calorific value of gross quantities of a fuel

is dependent upon making measurements on small (1-3 gram) fuel samples.

The accuracy of these measurements is, in turn, dependent upon the representativeness

of the analysis samples which are extracted from gross lots of the

fuel. The traditional fuels, such as coal and coke, are

homogeneous enough so that techniques [3,4] have been developed for obtaining

(1-3 gram) analysis samples which are representative of the gross lot of the

fuel. The heterogeneity of refuse has made it necessary to re-evaluate the

test procedures fo.r determining the calorific value of coal and coke before they

can be applied in a reliable manner to refuse and RDF. This heterogeneity

problem can be attacked by either of two approaches. First, one may choose

a representative gross sample of refuse or RDF and through appropriate

particle size reduction and blending, obtain a representative (1-3

gram) sample. Second, one may construct combustion calorimeters

that can handle larger samples of RDF which are more representati ve of the

gross lot of the RDF fuel. NBS is investigating this problem from both

approaches. One method involves the processing of heterogeneous samples to

obtain a homogeneous sample from which a small (1-3 gram) representative

sample can be selected for use in the NBS conventional-size calorimeter. The

other method involves the design and the construction of large calorimeters

capable of making calorific value measurements on large (kilogram-size)

samples of refuse and RDF. The latter approach impacts upon the advancement

of the state-of-the-art of calorimetry.

5
This report will present calorific values measured in the NBS

conventional size (2.5 gram capacity) oxygen bomb calorimeter on highly

processed "homogeneous" analysis samples of RDF. It also provides

calorific values measured in the (25 gram capacity) oxygen bomb calorimeter

which was built at NBS for less processed RDF samples.

The RDF samples that were studied can be placed in five arbitrary

classes. The first class consists of those RDF's investigated as part

of ASTM E- 38 . 01 (Subcommittee on Energy of the ASTM Committee E-38 on

Resource Recovery) Round Robin testing of RDF-3. The second class deals

with an Americology RDF sample from which sub-samples were extracted for

calorimetric measurements in both a selective and a non-selective manner.

The thi rd class consists of those RDF samples used in comparative studies

e of the same RDF investigated in both the NBS conventional size (2.5 gram

capacity) and the NBS large (25 gram capacity) oxygen bomb calorimeters.

The combustible fractions of a sample of municipal solid waste (MSW)

from New Castle County, Delaware, which had been processed through the

U.S. Bureau of Mines Resource Recovery facility in College Park, Maryland

constitutes still a fourth class of RDF samples. The fifth class of RDF

samples consists of several RDF's from different parts of the USA that

had some unusual characteristics or history which prompted calorific

value measurements to ascertain what variations might be present.

The RDF's investigated provide useful answers to all of the objectives

of this research project. Comparison of the methods and results of

samples which had received various degrees of processing and were investigated

in both the 2.5 gram capacity and the 25 gram capacity bomb calorimeters

provides information on the effects of the size reduction and homogenization.

The variability of the calorimetric data provides some insight into the

extraction of representati ve RDF samples. The comparison study on the same
RDF's investigated in both the small and large bomb calorimeters will help

to evaluate the methods required to measure calorific values in a reliable

manner by the use of either the conventional size or larger bomb calorimeter.

Also, test procedures were developed to be used for the measurement of the

calorific value of RDF samples in both bomb calorimeters. In addition, RDF's

with unusual characteristics provide information on the general properties

of RDF. Thus, this report addresses itself to all of the objectives of this

project and also provides some general information on the properties of refuse

and refuse-derived-fuels (RDF).

7
II. Experimental

A. Material

s

1 . Benzoic Acid

(a) NBS Standard Reference Material 39i with a certified energy

of combustion of 26434 + 3 J*g~^ at standard bomb conditions was used to

calibrate the conventional-size (2.5 gram capacity) bomb calorimeter.

(b) Fisher Scientific Company's certified benzoic acid with a measured

energy of combustion of 26437 +3 J*g~^ was used to calibrate the large

(25 gram capacity) bomb calorimeter.

2. Oxygen

Ultra High Purity (UHP) grade oxygen was supplied by Matheson Gas

Products. This oxygen is certified by the supplier to contain combustible

impurities not exceeding 0.002 percent and total impurities of less than

t 0.05 percent.

3. ASTM Round Robin RDF-3 Samples [5]

Refuse-deri ved-fuel -3 (RDF-3) is defined as a shredded fuel derived

from municipal solid waste (MSW) which has been processed for the removal

of metal, glass, and other entrained inorganic material. Generally, this

material has a particle size such that 95 weight percent passes through

a 2-inch square mesh screen.

The round robin testing of RDF-3 was coordinated through ASTM

Subcommittee E-38.01 on Energy. Each laboratory participating in the

ASTM round robin testing program received five samples of RDF-3 weighing

about 2.5 kg each. Four were used for sieve analysis while the fifth was

processed after air drying to 0.5 mm particle size for physical and chemical

analysis. Gram-size amounts of milled sample were used in the various

analyses

8
Samples of RDF-3 were prepared at the National Center for Resource

Recovery (NCRR), Washington, D.C., and were distributed to various participating

laboratories for two preliminary series or zeroth rounds of round robin

testing. Six laboratories participated in the first and second preliminary

rounds, however, the data obtained appeared to have a wide dispersion. It

was felt that a period of acclimation was required for laboratory analysts

to acquire some experience in processing and analyzing RDF-3 samples.

(a) First Round Robin Sample

The first round robin sample was prepared at NCRR, Washington, D.C.

Eight laboratories participated in the first round robin tests, which took place

in June and July of 1978.

(b) Second Round Robin Sample

The second round robin sample was prepared at NCRR, Washington, D.C.

Twelve laboratories participated in the second round robin tests, which took

place in December 1978 and January 1979. In an effort to ascertain whether

improved prec-ision could be obtained for higher heating values, moisture,

ash, elemental analysis, and volatile matter, an inter-laboratory reference

or comparison sample was also prepared. A sample of RDF-3 from NCRR was

shipped to the Wisconsin Electric Power Co., Milwaukee, WI for milling down

to 0.5 mm particle size. The milled sample was thereafter distributed to

the participating laboratories in quantities of about 200 grams. It was hoped

that the comparison sample would eliminate possible biases which might have

been introduced into the particle size reduction operation at each of the

participating laboratories

(c) Third Round Robin Sample

The third round robin sample was prepared at Americology (Division of

American Can Co.), Milwaukee, WI. As with the second round of testing,

twelve laboratories participated in the third round of testing during May and

June of 1979. Again, an interlaboratory comparison sample was prepared.

9
This time, a sample of RDF-3 was shipped from Americology to the Oak Ridge

National Laboratory, Oak Ridge, TN, for milling to 0.5 mm particle size.

Distribution of the milled sample was made to the participating laboratories

in quantities of about 200 grams.

(d) Bituminous Coal Round Robin Sample

In an effort to assure that the testing laboratories had good quality

control over their test procedures for higher heating value, residual

moisture, and ash content determinations, another series of round robin tests

was carried out using a NBS Standard Reference Material (SRM) bituminous

coal sample (1632a). Quantities of 100 grams were distributed to six

laboratories for test during February and March of 1980. This SRM had a

particle size of about 0.25 mm (-60 mesh).

4 Teledyne National RDF

(a) RDF Pellets

A 20 kilogram sample of extruded RDF pellets was received from the

Baltimore Co.unty Resource Recovery Facility operated by Teledyne National

in Cockeysvi 1 le, MD. The Teledyne National pellets are cylindrical in

shape with a diameter of 2.5 cm (1 inch), and are broken-off into lengths of

about 2.5 to 7.5 cm (1 to 3 inches). A portion of the extruded pellets was

broken up in an arbor press or put through a grinder and run through a micromill

to yield a 0.5 mm. (-10 mesh) powder. The powdered RDF sample was homogenized

in a vee blender to provide an analysis sample.

(b) RD F-3 (Fluff) Sample

Two samples of RDF-3 (fluff) weighing approximately 3 kg each were

obtained from Teledyne National's Resource Recovery facility in Cockeysvi 1 le,

Md. One sample remained at NBS and the other was sent to Gilbert Associates, Inc.

in Reading, PA. The sample was analyzed by both laboratories using proposed

ASTM E-38 test procedures following single step and two step moisture

determinations.

10
5.

ECO FUEL-II RDF

A 20 kilogram sample of ECO FUEL-II RDF was received from the Combustion

Equipment Associates Facility at Bridgeport, CT and had a particle size of

approximately 0.42 mm. (-40 mesh).

6. Americology RDF-3 (Fluff)

The Americology Resource Recovery Facility processes the municipal

solid waste from the city of Milwaukee and supplies the Wisconsin Electric

Power Company with RDF-3 which is co-fired with coal to generate electricity.

A 55 gallon drum of RDF-3 (Fluff) was obtained from Americology.

7. New Castle County, Delaware MSW

A representative sample of municipal solid waste (MSW) from New

Castle County, Delaware was shipped to the Bureau of Mines' College Park, Md.

Resource Recovery Facility in March 1979. The College Park Resource Recovery

Facility has seven sampling points within the processing stream from which

combustible material can be collected. The New Castle County, Delaware, MSW

was processed through the College Park Facility and representati ve samples were

obtained from each of the seven sampling points.

8. S team Size Reduction RDF

This RDF was produced by a novel technique at Burke, Davoud, and

Associates in Richmond, V A. The process is similar to that used to make

puffed cereals. The refuse is pressurized with steam in a closed container.

An instanteous release of the pressure causes the steam and heated refuse

to expand and thus be reduced in particle size to an RDF.

11
9 . NCRR Storage Pit RDF (Charred Sorage Sample )

This is RDF which had charred during storage. The National Center

for Resource Recovery had processed some Washington, D.C. municipal solid

waste into RDF. The RDF was stored in Washington, D.C. for approximately

10 months. When the RDF was being removed for a test burn in an industrial

boiler, portions of the RDF were found to have spontaneously undergone a

chemical reaction to form a partly charred RDF. A grab sample of the RDF

char was obtained for a few calorific value measurements.

10. NCRR RDF (Low Ash Sample)

The National Center for Resource Recovery (NCRR) prepared an RDF

from office waste collected in various government buildings in the Washington,

D.C. area. The RDF was prepared for a test burn in one of the boilers at the

Pentagon in Washington, D.C. A grab sample was obtained from NCRR for

measurement of the gross calorific value of RDF produced from this collection

of office waste.

ALTHOUGH TRADE NAMES, ACTUAL SOURCES FROM WHICH SAMPLES WERE OBTAINED,

SPECIFIC APPARATUS AND/OR ITS MANUFACTURER HAVE BEEN IDENTIFIED, THE NATIONAL

BUREAU OF STANDARDS DISCLAIMS ANY ENDORSEMENT, OR RECOMMENDATION OF USE FOR

THE COMMERCIAL MATERIALS OR APPARATUS USED IN THIS SCIENTIFIC INVESTIGATION.

12
B. Oxygen Bomb Calorimeters

1

2.5 Gram Capacity Bomb Calorimeter

The NBS conventional size (2.5 gram capacity) oxygen bomb calorimeter which was

designed at NBS and built by Precision Scientific Co. is an isoperibol (isothermal jacket

bomb calorimeter. The calorimeter has a history of providing high precision

results with fuels and various materials of high purity.

2.

25 Gram Capacity Bomb Calorimeter

A large (25 gram capacity) oxygen bomb calorimeter was designed and

built at NBS for high precision measurement on large samples. The two

calorimeters are very similar in design except for the sample size capacities.

Details of the large (25 gram capacity) oxygen bomb calorimeter were

presented earlier [2] and are also described briefly in Appendix B.

C. Sample Preparation Apparatus

1 . Steelman 450°F Electric Bake Oven

A model 568ETC A, 300 cubic foot oven was used for air-drying and total moisture

determinations. It was equipped with movable shelves to accommodate drying racks

whose volume was one cubic foot, and had an upper temperature limit of 450°F. The

drying oven was equipped with a Portlow model RFC-15 24 hour chart recorder

and programmer.

2. W. W. Grinder Corporation Hammer Mill

A model F-21-M-18, 5 horsepower hammer mill was used with either

3/4 inch or 1/4 inch screen.

3. Wiley model 4 Laboratory Mill

The Wiley model 4 laboratory mill has a 1/2 horsepower motor and

performed size reduction of RDF samples through either a 2 mm or 0.5 mm

screen. The mill has 6 stationary blades and 4 rotating blades.

13
4. Patterson Kelley Company Twin Shell Dry Blenders

These vee blenders were used with an 8 quart stainless steel twin shell

and a 26 prong rotation mixer-intensifier rod to enhance the homogenization

of RDF samples. Lucite shells of 1 or 3 quart capacity were also used.

5. Carver Laboratory Press, Model M

The Carver Laboratory Press was a hydraulic press capable of exerting

50,000 pounds of force. Dies of 1 3/8 or 5/8 inch diameter bores were

fabricated in the NBS Instrument Shops and used in conjunction with the

press to prepare pelleted RDF samples for various determinations.

D. Sample Preparation Procedure

The processing of an RDF sample involved four basic steps. RDF

samples were: (1) dried, (2) milled to reduce the particle size, (3) blended

to a "homogeneous state" and (4) pelletized into analysis samples.

1 . Sample Drying

As-received RDF samples were dried in either a one step or two step

method. The one step method was performed in the drying oven set at

107 + 3°C for 24 hours. The two step method consisted of air-drying of the

sample in the drying oven at 37 + 3°C until the sample was in equilibrium with

ambient conditions. A residual moisture determination was carried out

subsequently on the analysis samples and combined with the air-dry-loss to

compute the total moisture of the sample (see Appendix E).

2. Particle Size Reduction

Samples were milled to either 2 mm or 0.5 mm particle size for analysis

purposes. RDF samples larger than 3/4 inch were processed through the 5

h.p. hammer mill to obtain particles that could pass through either a 3/4 inch or

1/4 inch metal screen. If more processing was required, the material was then

milled in a 1/2 h.p. Wiley laboratory mill to pass through a 2 mm stainless

steel screen. When further particle size reduction was required, the 2 mm material

was processed through the Wiley laboratory mill again until it passed through a

0.5 mm screen.

14
3. Sample Homogenization

The 0.5 mm RDF was coned and quartered to obtain a laboratory sample

which would fit into the 8 qt. twin-shell dry blender. The laboratory

sample was then blended throughly in the twin shell blender.

4. Preparation of Pelletized Analysis Samples

After stopping the twin shell blender, analysis samples were immediately

drawn from the blended RDF and pressed into pellets with the Carver Laboratory

Press

E. Calorimetric Procedure

Determination of test procedures for measuring the calorific values of

refuse and RDF is one of the objectives of this project. Therefore, a detailed

description of the calorimeteric procedure will be presented in the

Results and Discussion Section of this report. Only a brief description of

the calorimetric procedure will be presented here. A detailed description

of the 25 gram capacity bomb calorimeter is provided in Appendix B.

15
The pelletized RDF sample was weighed into either a platinum, stainless

steel, or quartz crucible. The crucible and sample were then placed in the

crucible support of the bomb, which contained either 1.00 cm (small bomb) or

10.0 cm (large bomb) of water. A 2cm (small bomb) or 7 cm (large bomb)

length of 0.003 inch diameter platinium wire was connected to the bomb electrodes

and placed in contact with the sample. The bomb was sealed and then filled with

30 atm (40 atm-large bomb) of ultra high purity oxygen. The ambient temperature

was recorded during the bomb-filling operation. The loaded bomb was then placed

into the calorimeter vessel, which contained a measured amount of water. The

calorimeter vessel was enclosed in a submarine vessel and immersed in a constant

temperature water bath. The calorimeter fluid was then heated electrically to 24.98°C

and then allowed to rise at a rate of 0.001 °C per 100 seconds. The rate of rise was

related to the stirring energy imparted by the calorimeter stirrer and the

thermal leakage from the calorimeter jacket. Time and temperature measurements

were recorded from a frequency counter connected to a quartz temperature

probe. Integrated frequencies were recorded every 100 seconds. At a frequency

corresponding to 25°C, the sample was ignited by discharging a 32,000 yf capacitor,

which had been previously charged to 23 V, through the platinum wire fuse.

Integrated frequencies were recorded throughout the main reaction period and

also during the after period when thermal eui librium had been obtained.

The calorimeter was opened and the bomb removed. The bomb was opened and

the original liquid contents and the subsequent bomb washings were weighed in

a polyethylene container. Weighed aliquots of the bomb washings were analyzed

for total acid and sulfur content.

16
The final value obtained in a calorimetric measurement is the ratio of the

algebraic sum of the amount of energy released into the calorimeter, corrected for

energy released by accompanying side reactions, and the calorimeter sample mass

corrected for the amount of moisture and ash. Residual moisture and ash determination

were carried out concurrently on pelleted samples with the calorimetric determination.

The residual moisture sample is weighed into a dry, weighed porcelain

crucible and then dried in a moisture oven maintained at 107 + 3°C. The residual

moisture was used to correct the mass of the RDF calorimetric sample to the dry

basis

The amount of ash in the calorimetric sample was determined by two methods.

In one method, the mass of the bomb residue is determined by weighing the dry

crucible and residue upon completion of the calorimetric determination. In the

other method, an ash sample is weighed in a dry weighed porcelain crucible and

placed in a furnace. The temperature of the furnace is allowed to rise

slowly in a 4 hour period to 575 + 25°C and is then maintained at that temperature

for 2 hours. The amount of ash found in the determination is used to correct

the mass of the calorimetric sample to an ash-free basis.

17
III. Results and Discussion

A. Bomb Calorimetric Measurements

1 . General Discussion

Different methods for bomb calorimetric measurement of heat of combustion are available

for various types of materials. Certain modifications exist depending on the

precision desired and the properties of the material investigated. Apparatus

and methods for the precise calorimetric measurement of the heat of combustion are

present in the literature [6,7,8]. The methods followed in this laboratory are

patterned after the precise measurement techniques utilized by Jessup [8].

The NBS isoperibol bomb calorimeters consist essentially of a calorimeter vessel

which contains a measured amount of water. Imnersed in the calorimeter water is

a constant volume bomb in which combustible material are burned completely with the

aid of high purity oxygen under high pressure. Also in the water are a stirring

device for maintaining a uniform and meaningful calorimeter temperature, and a

thermometer for measuring the calorimeter temperature. In order to control the

heat transfer between the calorimeter and the environment, the calorimeter vessel

is enclosed in a submarine vessel which i's immersed in a constant temperature

water jacket. The calorimeter vessel is separated from the submarine vessel,

and hence the thermal environment of the water jacket, by a 1 cm air space.

A measurement of the heat of combustion of a given material is carried out by

comparing the corrected temperature rise of the calorimeter water in an experiment

in which a known amount of energy was supplied to it, with the corrected temperature

rise of the calorimeter water produced in another experiment by combustion of a

weighed sample of the material of interest. The temperature rise in both experiments

should be, as nearly as possible, over the same temperature range from the standard initil

temperature to the standard final temperature. This comparison method eliminates

some of the systematic errors associated with calorimetric measurements and requires

that the procedures be, as nearly as possible, identical in the two experiments

which are compared. Calibration experiments are used to determine the amount

of energy necessary to produce a specific corrected temperature rise. The mean of

18
I

i

i

1

the calibration experiments is called the energy equivalent of the calorimeter.

The product of the energy equivalent and the corrected temperature rise of the

calorimeter in an experiment, in which a material of unknown heat of combustion

is burned, gives the energy liberated in the combustion reaction and includes any

side reactions which may occur.

2. Test Procedures

The procedures outlined here are applicable to both calibration experiments

with benzoic acid, NBS SRM 39i , and RDF combustion experiments. Modifications

necessary for either type of sample will be specified where applicable.

3. Sample Preparation

Benzoic acid (NBS SRM 39i), should be used to calibrate the bomb calorimeter.

The conditions specified on the NBS certificate should be followed as closely as possible.

The nature of the benzoic acid, SRM39i , is such that it can be used directly

from the bottle, with no further processing. A sample size should be chosen to

produce the desired temperature rise of the calorimeter. The NBS small (2.5 gram

capacity) bomb calorimeter is selected to operate from 25°C to 28°C and requires

approximately 1.63 grams of benzoic acid. The NBS large (25 gram capacity) bomb

calorimeter is selected to operate from 25°C to 30°C and requires approximately

16.2 grams of benzoic acid. Benzoic acid was obtained commercially and its

energy of combustion measured for use in calibration of the large calorimeter.

The benzoic acid combustion samples are pressed into pellets and weighed in a preweighed combustion crucible. Platinium crucibles are used in the small calorimeter

and weighings are carried out to the nearest microgram (0.000001 g). Quartz

crucibles are used in the large calorimeter and weighings are carried out to the

nearest ten micrograms (0.00001 g).

19
RDF samples for use in the small calorimeter should be material which

has been milled to pass a 0.5 mm screen and then thoroughly blended. RDF

samples for the large calorimeter have been from 19mm (3/4 in) to 0.5mm

particle size. The choice of RDF samples from large particle size material

must be done carefully and without bias. A sufficient amount of RDF material

must be chosen to produce a three degree temperature rise in the small calorimeter

or a five degree temperature rise in the large calorimeter. Samples are weighed in

pre-weighed quartz crucibles using the appropriate balances described earlier.

The weighed crucible and sample are then placed in the bomb sample holder.

4. Bomb Preparation

A measured length of firing wire is connected to the ignition electrodes

of the bomb. A 3cm and 7cm fuse is used in the small and large bombs,

r

I respecti vely . A single loop is drawn in the center of the fuse and placed in

contact with the combustion sample which had been placed in the sample holder.

Platinum fuse wire is used without weigtiing because it does not undergo

combustion. When iron fuse wire is used, its weight must be determined

because a thermochemical correction for the combustion of the iron fuse

wire must be applied for the quantity of iron wire burned.

A specific amount of water is placed into the bomb: 1.0 ml in the

small bomb and 10.0 ml in the large bomb. The water is necessary to maintain

an atmosphere that is saturated with water vapors such that any water produced

in the combustion reaction will go to the liquid state so that there is no

uncertainty associated with the calorimetric measurement due to the vaporization

of water.

20
The bomb is assembled and charged with ultra high purity oxygen. The small

bomb is filled to 3 MPa (20 atm) and the large bomb is filled to 4 MPa (40 atm).

In the calibration experiments, the oxygen pressure is released slowly through

the exit valve and then refilled with pure oxygen. This step is carried out to

reduce the nitrogen impurity which is present in the one atmosphere of air

initially present in the bomb. This purging step is omitted with RDF combustion

experiments to ensure that there will be sufficient nitrogen for complete

oxidation of the sulfur in the RDF [9].

5. Calorimeter Preparation

The calorimeter jacket temperature is adjusted to approximately 0.1 °C above the

expected final temperature of the calorimeter (28°C and 30°C for the small and

large calorimeters , respecti vely) . The jacket temperature should be maintained

at 0.001 °C of the specified jacket temperature. , ,

The calorimeter vessel is filled with distilled water and adjusted so that

the water temperature is a few tenths of a degree below ‘the desired initial

temperature (25°C) in the experiment. The calorimeter vessel and water are

placed on a balance and filled with distilled water to a constant mass for both

calibration and combustion experiments. In the small calorimeter, the calorimeter

vessel is filled with water to give a final weight of 3765 grams. It is then

suspended and placed into a submergible calorimeter container. The bomb is placed

into the calorimeter water and connections are made on the calorimeter cover

for the fuse circuit and the calorimeter heater. The cover for the submergible

calorimeter container is attached and the calorimeter stirrer is engaged. With

the submarine sealed and all connections made, the calorimeter and submarine

vessel are lowered into the constant temperature jacket bath.

21
The procedure is slightly different for the large calorimeter since the large

calorimeter vessel contains approximately 21 liters of water; hence, it is more

practical to determine the quantity of water in it vol umetrical ly . The calorimeter

vessel is filled with approximately the proper quantity of water while it is

inside of the submarine vessel. The bomb is placed in the calorimeter and the

water temperature is adjusted to 24.5°C. The fuse and heater leads are connected

and the calorimeter vessel cover is assembled. The calorimeter cover contains

a short length of a calibrated pipette. Water is added through the thermometer

opening and water will rise in the pipette by capillary action to a specific level.

The cover for the submarine vessel is attached and the complete system submerged

into the controlled water bath.

The cover of the submarine vessel contains tubes, through which the

thermometer and electrical connections are made to the calorimeter. The calorimeter

stirrer is started to obtain uniform temperature drift readings between the

calorimeter and jacket. Using the calorimeter heater, the desired starting

temperature is reached, after which the calorimeter is ready for initial

temperature measurements. The NBS fuse circuit is connected to a 32,000 microfarad

capacitor which is charged to 23 volts and upon discharge ignites the fuse

wire over the sample.

6. Temperature Measurements

The temperature is measured every 100 seconds with a quartz thermometer, to

determine the variation of the calorimeter temperature with time. The quartz

thermometer generates a frequency that rises linearly with increasing temperature to a

high degree. A frequency counter is used over 100 second intervals and displays

the calorimeter temperature. The display of the counter gives the average temperature

over the 100 second counting intervals, providing an integrated temperature for

a given calorimetric experiment. Both temperature measurement and data-logging

are automatic. A least square fit of these points is performed using an exponential

equation to produce the corrected temperature rise by correcting the observed temperature

rise for the effects of the heat of stirring and thermal leakage.

I

k

k

22
7. Calorimeter Corrections

Corrections for side reactions producing nitric and sulfuric acids

from the nitrogen and sulfur impurities in the RDF must be determined. The pressure is

released from the bomb and it is opened. The crucible and residue are removed to deteriv1 o

the amount of non-combustibles (bomb ash) in the sample. The bomb interior is

carefully washed and the washings saved for analysis of nitric and sufuric acid.

Aliquots of the washings are used for these determinations. The total acid is

determined by titration with a standard alkali. The sulfur content is determined

gravimetri cal ly by the precipitation of barium sulfate. A 57.7 joule correction is

applied for each mill iequivalent of acid and a 5860 joule correction for each

gram of sulfur obtained from a calorimetric experiment.

A correction is applied for the amount of energy that had to be supplied to the

calorimeter in order to ignite the sample. Since the sample is ignited by the

discharge of a 32000 uf capacitor which has been charged to 23 volts, this correction is

calculated from the difference between initial capacitor energy and the final

2 capacitor energy; the energy of a capacitor is 1/2 C V . The measuring circuit

accounts for 33 percent of the energy discharged.

If iron fuse wire is used, the unburned pieces must be weighed and

subtracted from the initial weight of the iron fuse. 7100 joules per gram of

iron burned is applied for the iron fuse correction.

23
8. Calculation of the Calorific Value

The total energy involved in the bomb process is calculated from the

product of the actual energy equivalent (mean of the calibration experiment

corrected for the heat capacities of the bomb contents) and the corrected

temperature rise. The energy corrections described in the last section are

subtracted from the total energy absorbed by the calorimeter to obtain the

energy released by the combustion of RDF. The energy from the RDF combustion

is then divided by the mass of the RDF sample to determine the calorific

value (as-determined higher heating value, HHV-AD).

Appendix D is a conversion table for the calculation of data to different

bases, i.e., as-determined, as-received, dry basis, and dry, ash-free basis.

24
B. Calibration of the Calorimeters

1 . NBS 2.5 Gram Capacity Bomb Calorimeter

The NBS 2.5 gram capacity calorimeter has an energy equivalent of

14543 A record of the energy equivalent is maintained. We have found that

the energy equivalent of this calorimeter system has not changed significantly over the

last three years. Any changes to the calorimeter are recorded and an appropriate

correction based upon the mass and the heat capacity of the material is applied.

These calculated corrections usually amount to less than 0.1 J*K~^ and are

usually beyond the measurement capabilities of the instrument. However, the

energy equivalent is periodically measured to check for any unforeseen changes

which might occur.

During fiscal year 1979, 23 calibration determinations were performed.

The average value of these 23 determinations was 14543.64 + 2.28 The

estimated uncertainty is twice the standard deviation of the mean (2 sdm).

The value which is presently being utilized for this calorimeter is 14543.45 J*K~^

and is based on the most recent set of 6 energy equivalent (calibration)

measurements. Table 1 contains the results of the energy equivalent measurements

during the 1979 fiscal year. The last six energy equivalent measurements

(marked with an asterisk) are the basis of the value presently being used.

Table 2 contains a more detailed presentation of measurements performed

in the last six calibration experiments, numbers 1238-1244. The headings,

in the order in which they appear in the tables, are described as follows:

Expt. No., the number of the experiment, which can easily be traced

back to our records.

AUc° (28° )/J

•g~~'

, the energy evolved by the combustion of benzoic acid

at the selected final temperature in J*g~^.

m-BA/g (vac) , the mass of the benzoic acid sample, in g, reduced to

mass in vacuum.

25
q -BA/ J

,

the energy evolved by the combustion benzoic acid, in J.

q-ign/J, the electrical energy added to the system to ignite the sample, in J.

q-HN03/J , the energy evolved by the formation of nitric acid in the

combustion process, in J.

q-WC/J

,

the Washburn Correction [6,7] applied to correct the combustion

data from bomb conditions to conditions in which the reactants and products

are in their pure standard states at one atmosphere pressure, in J.

g-corr to t

f/J , a correction applied for the deviation of the actual

final temperature from the selected standard final temperature (usually 28°C),

in J.

Q-total/J

,

the total energy added to the calorimeter, in J.

AT-corr/K, the observed temperature rise of the calorimeter corrected for

stirring energy and thermal leakage, in K.

E-cal/J- K~^

,

the energy equivalent of the actual calorimeter system at the

final temperature, in

Ei -cont/J« K~^

,

the heat capacity of the initial bomb contents, including the

sample, crucible, water, and oxygen, in

E,si -empty/J« K~^ , the energy equivalent of the empty calorimeter at 28°C,

in J* K*^ .

E,si -mean/J»

K~~*

, the mean value of the measured energy equivalent, in

Std. Dev./J-K~\ the standard deviation of a measurement, in J-K"'

1 (and

the percent standard deviation).

Std. Dev. Mean/J«K~\ the standard deviation of the mean, in J*K"^ (and

the percent standard deviation of the mean).

26
2. The NBS 25 Gram Capacity Bomb Calorimeter

The 16 gram sample size of benzoic acid that is required to calibrate the

large calorimeter makes the use of the NBS SRM 39i (benzoic acid-calorimetric

standard) impractical. Therefore, benzoic acid was obtained from a commercial

source to calibrate this large calorimeter. Standard benzoic acid

(NBS SRM 39i ) has an energy of combustion under standard bomb conditions of

26,434 +3 J*g’^. This reduced to 26,410.68 J*g"^ under actual bomb conditions

and is used to standardize the commercially obtained benzoic acid. The "commercial"

benzoic acid was found to have an energy of combustion which reduces to 26,411.36

J*g”^ at actual bomb conditions. Table 3 presents the results of measurement

of the energy of combustion of the "commercial" benzoic acid. The headings are

explained under the calibration experiments of the 2.5 gram capacity bomb

calorimeter.

Table 4 presents the results of a set of calibration experiments for the

large calorimeter. The two additions to the headings described previously are

as follows:

q-Fe/J, energy evolved by the combustion of the iron fuse wire, in J.

g-carbon/J

,

the correction applied for unburned carbon in the bomb, in J.

The calibration experiments in the large calorimeter resulted in an energy

equivalent of 86,043.43 +9.13 J*K~\ This value is about six times the

correspondi ng value for the conventional size calorimeter; however, the precision

of calibration is essentially the same. Compare standard deviations of the mean

in Tables 1 and 4, which are about 0.01 percent.

Subsequent tables which present calorimetric data on RDF samples contain

addition correction headings; they are identified as follows:

Q-RDF/J, total energy delivered to the calorimeter after corrections for

ignition energy, fuse energy, formation of nitric and sulfuric acids, and

the like, in J.

27
m-RDF/g, mass of the RDF sample, in g.

HHV-AD/MJ* kg~^

, higher heating value on as-determined basis,

in MJ-Kg

" 1 (or Btu-lb

-1

)-

28
C. Calorimetric Measurements on RDF

Laboratory samples of RDF undergo considerable processing so that a reasonably

homogeneous sample can be prepared for calorimetric measurement. Before milling,

the samples must be air-dried to remove most of the moisture present in them.

The samples are then milled to 2mm or 0.5 mm powder and pressed into pellets weighing

about 2.5 grams, for calorimetric measurement. The raw calorific values which

are calculated from the bomb calorimetric experiments are referred to as higher

heating values on an as-determined basis, HHV-AD.

The HHV-AD values are not consistent with the heating value of the fuel that

is received and which will be burned in power plants or boilers. Combustion

engineers are primarily interested in the higher heating value on an as-received

basis, HHV-AR (also called HHV1 ) . The sample mass which is used in the calculation

of HHV-AD is corrected for its residual moisture content, and the higher heating

value-moisture free, HHV-MF (also called HHV2), is obtained. HHV1 is obtained from

HHV2 by adding the total moisture to the dry sample mass of HHV2. Also of interest

is the higher heating value on a moisture-ash-free basis, HHV-MAF (also called HHV3).

HHV3 is obtained from HHV2 by correcting the dry sample mass of HHV2 for its

ash content. HHV3 is important because these data are used for comparison of

heating values determined in different laboratories, under different conditions,

on the same RDF sample. The precision obtainable on HHV3 is indicative of the

experimental control which prevails during the calorimetric measurements. The

ash content of analysis samples of RDF vary, sometimes to a significant degree.

Since these ash contents are used to correct HHV2 to obtain HHV3, it has been proposed [ 1_

that precisions can be enhanced if the calorimetric sample masses are

corrected for ash content based upon measurement of the bomb residue (i.e. the actual

ash content of the calorimetric sample). Use of the ash content determined from

the bomb residue weighings eliminates the assumption that an equivalent ash content

determined from the ASTM furnace ash protocol is applicable to combustion bomb

29
calorimetric data. This assumption is not completely valid. In the furnace,

combustion takes place in air at atmospheric pressure at about 575 or 725°C; in the

bomb, combustion takes place in pure oxygen under a pressure of 30 atmospheres

at about 1500 to 2000°C. The composition and character of the two ash residues

(i.e., furnace ash vs. bomb ash) are distinctly different.

In summary, HHV3 can be calculated from either the bomb ash, yielding HHV3-B,

or from the furnace ash, yielding HHV3-F. Higher heating values, therefore,

can be calculated on four different bases from HHV-AD, namely: HHV1, HHV2,

HHV3-B , and HHV3-F.

Higher heating value, residual moisture, and ash experiments are performed

concurrently . Since the residual moisture content and the ash content are used

to correct the mass of the calorimetric sample, the three samples must be

prepared under the same conditions. Therefore, a routine laboratory measurement

of the higher heating value requires the preparation of three samples. As part of the

calorimetric measurements, the bomb residue and sulfur content are also measured.

The RDF calorimetric measurements were previously placed into five classes, namely

(1) measurements carried out in conjunction with ASTM E-38.01 round robin

testing; (2) measurements carried out on an Americology RDF sample, from which

sub-samples were extracted in a selective and non-selecti ve manner; (3) measurements

required to compare the characteristics of the small and large bomb calorimeters

;

(4) large bomb calorimeter measurements of the combustible fractions of New

Castle County, Delaware MSW which had been processed at the U.S. Bureau of Mines,

College Park, MD facility; and (5) measurements on some representati ve RDF's

of special interest. Discussion of RDF measurements is according to each

particular class

.

30
A set of results (usually three tables) is provided for each distinct RDF

sample studied. The first table of a set gives detailed calorimetric data

for each experiment which was carried out on a particular RDF sample. Since

RDF's are fuels which have low sulfur contents, additional corrections will

appear in the tables, as follows:

q-FUS0„/J, the energy involved by the formation of sulfuric acid in

the bomb process, in J.

The second table of a set contains the analytical data necessary to calculate

higher heating values from the as-determined base to the four different bases.

The third table of a set will present the calculated higher heating values

for the four different bases. Hence, for each RDF sample studied, three tables

are presented: (a) calorimetric data, (b) analytical data, and (c) calculated

higher heating values for three different bases, HHV2, HHV3-F, and HHV3-B.

1 . ASTM Subcommittee E-38.01 Round Robin Testing on RDF-3

As mentioned earlier, two zeroth rounds of round robin testing were

carried out over the period of 1 October 1977 to 31 January 1978, in order to allow

laboratory analysts an opportunity to become more acclimated with the new

and/or modified testing protocols. The provisional protocols issued by ASTM

Subcommittee E-38.01 on Energy required that duplicate measurements be

performed on consecutive days for all of the following chemical tests: residual

moisture, higher heating value, ash content, volatile matter, elemental

analysis, and ash fusion temperatures . Our interest focused primarily on

the higher heating value, moisture, and ash content determinations. A complete

technical review and evaluation of data have been made at NBS on the results or

31
the ASTM E-38.01 program to develop test procedures for the characterization

of RDF-3. The program was carried out by a large number of testing laboratories over

the period September 1977 through March 1980. This technical review and the

evaluations can be found in Appendix A of this report.

The milled RDF sample (0.5 mm particle size) was coned and quartered;

each quarter was treated as a sub-sample of the total and had higher heating

value, residual moisture, and ash content determinations made on it. Therefore,

the precision associated with a set of measurements is a function of both our

sampling and measurement techniques.

a . First Round Robin Sample

Gross calorific values determined on two sets of samples for the first

round of testing of RDF-3 are shown in Table 5. One set of samples was equilibrated

in a constant humidity atmosphere at 45 percent relative humidity, while the

second set was dried at 105°C and exposed to the moisture in the laboratory

for several days. Both samples yielded different residual moisture and bomb

ash values, as shown in tables 6 and 7. Furnace ash and sulfur content

determinations were carried out on the samples equilibrated at 45 percent

relative humidity, and were assumed to be same for samples which were dried and

subsequently exposed to laboratory moisture conditions. These observations strongly

suggest that the residual moisture content of an RDF sample is related to the

relative humdity present in the testing laboratory. The RDF sample which had

been previously dried and then exposed to laboratory moisture conditions

had a lower residual moisture content, a higher bomb ash content, and a lower

calorific value. It is possible that combustible substances may have vaporized during

the drying at 105°C, thus enriching the sample in inerts (ash) and perhaps also

decreasing its volatile character. Tables 8 and 9 provide calorific values

for the first round robin sample, calculated to different bases. The data are,

32
in general, in good agreement. Comparison of data on HHV2 shows the largest

dispersion, but this is only about 2 percent.

b. Second Round Robin Sample

Calorific values are provided for the second round of testing on RDF-3

samples in table 10 on both an interlaboratory comparison sample and an RDF sample

processed down to 0.5 mm particles at NBS in the usual manner. Both samples

were equilibrated in a constant humidity atmosphere at 45 percent relative

humidity. Although both the interlaboratory comparison sample and the regularly

processed sample were extracted from the same gross laboratory sample, the

higher heating values on an as-determined basis differ by about 3.5 percent. The

overall hetergeneous nature of refuse is probably responsible for this.

The results of determinations of residual moisture, ash content, and

sulfur content are shown for the interlaboratory comparison sample and the RDF

sample processed down to 0.5 mm in tables 11 and 12, respectively . Note that

the residual moisture determinations carried out on pellets which were equilibrated

in a constant 45 percent relative humidity environment are about the same value,

6.1 wt. percent. However, residual moisture determinations performed on loose

powder which was exposed to laboratory moisture conditions are more

variable, 3. 3-3. 5 wt. percent. The differences between the furnace ash determined

on loose and pelleted samples do not appear significant for either interlaboratory

comparison or regularly processed samples. However, when differences between

corresponding bomb ash values are examined, they are significant (compare bomb

ash values of 18.82 and 13.43 wt. percent in tables 11 and 12, respectively).

Calorific values calculated to different bases are reported in tables

13 and 14 for the interlaboratory comparison sample and the RDF sample

processed to 0.5 mm at NBS, respectively. Agreement is good between

higher heating values on a moisture-ash-free basis (HHV3), in general, but systematic

33
differences do exist between values based upon furnace ash and bomb ash.

c. Third Round Robin Sample

In table 15, one finds data on calorific value determinations for the

interlaboratory comparison sample and the RDF sample which was processed

to 0.5 mm powder at NBS for the third round of testing of RDF-3. The as-determined

calorific values (HHV-AD) for the interlaboratory comparison sample are about 2

percent lower than those for the RDF which underwent processing at NBS. This

agreement is good. Data for residual moisture, ash content, and sulfur

content are given in table 16 for the interlaboratory comparison sample and in

table 17 for the regularly processed round robin sample. Pelleted RDF samples were

not kept in a constant humidity atmosphere, but were exposed to ambient laboratory

conditions. A comparison of analytical measurements on the interlaboratory RDF

sample and the in-house processed sample (compare tables 16 and 17) are in good

agreement. Calorific values which have been calculated to different bases

for the interlaboratory comparison sample and the in-house processed sample

are provided in tables 18 and 19, respecti vely . The calorific values for the

interlaboratory RDF sample are all lower when compared with the sample which was

processed at NBS. The differences, however, are not serious; the range is between

2 and 3 percent.

d. Bituminous Coal Sample

In order to provide some reassurance to the RDF-3 round robin testing program

that the participating laboratories could carry out the

determinations for higher heating value, residual moisture, ash, and

sulfur content in a satisfactory manner, an NBS Standard Reference Material

(SRM 1632a) sample of a bituminous coal was distributed for testing. The

round robin on the SRM bituminous coal sample was an important round because

it could provide the comparison in the levels of precision, i.e., repeatabi 1 i ty

34
and reproducibility of test results, between the analysis of coal and RDF-3.

This comparison would not only furnish some quantitative estimate of what

kind of variability one might expect in the results of tests carried

out on a heterogeneous material like RDF-3, but also would provide an indication

of what the current state-of-the-art of the ASTM protocol was in this testing

program.

The results of duplicate calorimetric and analytical measurements which

were performed on the SRM bituminous coal sample are found in tables 20 and 21.

The results are in good agreement. Table 22 gives the calculation of calorific

values to different bases. Here also, agreement appears good.

A statistical analysis of both the NBS data and those of the other participating

laboratories which have been part of the ASTM testing program on RDF-3, can be

found in Appendix A. The repeatability interval (which is an estimate of within

laboratory measurement agreement) and the reproducibility interval (which is an

estimate of between laboratory measurement agreement) have been calculated for

higher heating value, residual moisture and ash content determinations.

Repeatability intervals for HHV2 (dry basis), residual moisture, and ash

content are 250 Btu/lb, 0.75 wt. percent, and 2.5 wt. percent, respectively.

Compare these data above with equivalent values calculated for ASTM protocols for

coal and coke: HHV2 (dry basis) is 50 Btu/lb, residual moisture is 0.3 wt.

percent, and ash content amounts to 0.5 wt. percent.

Reproducibility intervals for HHV2 (dry basis), residual moisture, and

ash content are 750 Btu/lb, 3.00 wt. percent, and 0.5 wt. percent, respectively.

ASTM coal and coke protocols report comparable reproduci bi 1 i ty intervals of

100 Btu/lb, 0.5 wt. percent, and 1.0 wt. percent, respecti vely

.

The heterogeneity of RDF at particle sizes of both 25 mm (1 inch)

and 0.5 mm limits the ability to which a representati ve sample can be

extracted. Before improvements in the levels of precision, i.e., repeatabi 1 i ty

35
and reproducibi 1 i ty can be expected, further development in sampling and/or

separation techniques for 25 mm as well as 0.5 mm particle size samples

should be pursued.

2. Americology RDF Sample

A sample of RDF-3, which was prepared and collected by Americology

(Division of the American Can Company) for Wisconsin Electric Power

Company, was received at NBS in May 1977. The Americology RDF-3 was

sampled in two ways to determine the effect of different sampling techniques

on a 20 kilogram gross sample. The first method was to take a grab sample of

approximately one kilogram directly from the 2 inch particle size material.

The one kilogram sample was processed to 0.5mm particle size in two steps

using a Wiley, Model 4, laboratory mill which is equipped with 2mm and

0.5mm screens. The 0.5mm material was blended thoroughly in a vee blender

and appropriate amounts of analysis samples were drawn. This method should

give useful information on the effects of selective sampling. .

In the other method, the remainder of the Americology RDF-3 was ground

to 6 mm (1/4 inch) particle size in the 5 hp hammer mill. It was coned and

quartered to select a one kilogram laboratory sample. The one kilogram sample

was processed to 0.5mm and blended in a similar manner to that of the grab

sample. This material should be more representati ve of the 20 kilogram gross

sample and also appeared more homogeneous than the grab sample. The only difference

in the sample treatment of the two samples is in their initial selection;

the first sample was selected directly from 2 inch particle size material

in a selective or grab fashion. The second sample was obtained by coning

and quartering the 1/4 inch particle size material and is more representati ve of

the sample as a whole.

Tables 23, 24, and 25 contain the results of measurements on the Americology

grab sample and tables 26, 27, and 28 contain comparable measurements on the

Americology representati ve sample. Comparison of the average calorific

values calculated to different bases in tables 25 and 28 shows that the

36
differences between the mean values for HHV-AD, HHV2, HHV3-F, and HHV3-B

are 201, 364, 133, and 457 Btu/lb, respecti vely . These differences are

significant and reflect the heterogeneity of refuse and RDF over which only

minimal control is possible using present processing methods.

The pelleted samples of the Americology grab sample were equilibrated

in a constant humidity atmosphere at 30 percent relative humidity, while the

pelleted samples of the Americology representati ve sample were equilibrated at

45 percent relative humidity.

These equilibrations are reflected in the residual moisture determinations

reported for these samples in tables 24 and 27; compare mean values of 3.01

wt. percent for the grab sample in table 24 with 30 percent relative humidity

equilibration and 5.19 wt. percent for the representati ve sample in table 27 with

45 percent relative humidity equilibration. Systematic differences in bomb ash

and furnace ash mean values are apparent from an examination of tables 24 and

27. The differences between samples are due to the heterogenei ty of RDF, while the

differences within a sample are due to the difference in ashing conditions in

the bomb and furnace.

3. Large and Small Calorimeter Comparison Measurements

Calorific values were measured in both the large 25.0 gram capacity bomb

calorimeter and the small 2.5 gram capacity bomb calorimeter to evaluate the

performance of the large bomb calorimeter system. Three different RDF's which

had been characteri zed previously at NBS were chosen for this study. These RDF's

were: (1) Teledyne National RDF, (2) EC0-FUEL-II RDF, and (3) Americology RDF.

Although the large bomb calorimeter is capable of making measurements on RDF's

which have received less size reduction and could be as large as 1 inch in

particle size, 0.5mm RDF samples were used in order that two equivalent sets

of samples could be prepared for measurements in both the large and small bomb

calorimeters . Results obtained in the large calorimeter could then be compared

37
to the results obtained in our small calorimeter which had been in service

for many years at NBS and had a history of consistently providing

calorimetric measurements of high precision.

a. Teledyne National RDF

Tables 29, 31, and 32 present results obtained in the small bomb calorimeter

for the Teledyne National RDF sample. Tables 30, 31, and 32 give the Teledyne

National RDF results obtained in the large bomb calorimeter. In table 32, the

mean values in MJ*kg"^ ( Btu- 1 b

_

) for HHV-AD, HHV2, HHV3-F and HHV3-B are:

19.35 (8318), 20.38 (8762), 24.55 (10553), and 24.03 (10331) for the small

bomb calorimeter. Also in table 32, the corresponding values from the

large bomb calorimeter in MJ-kg""' (Btu* lb”"*) are: 19.50 (8385), 20.54 (8832),

24.42 (10499), and 24.31 (10451). Theoretical ly , the two sets of samples are

identical and should reproduce identical results; however, in practice differences do

' < occur because of random errors, systematic errors, and errors introduced due

to the heterogenei ty of RDF.

Since the calorific values which were calculated to different bases for

the Teledyne National RDF differed by approximately one percent in comparison with

values measured in the small and large bomb calorimeters , we sought an

explanation. We felt that the stainless steel crucibles used in the

large calorimeter were being oxidized in the bomb combustion process, and we knew

from many years of experience that the platinium crucibles used in

the small calorimeter were not being oxidized. This was confirmed when the crucibles

were weighed before and after calorimetric experiments, revealing significant mass

changes in the stainless steel crucibles and insignificant changes

in the platinium crucibles. Since the actual bomb ash residues contained

large amounts of silica ( Si 0^ ) , we decided to use quartz

crucibles in both the large and small calorimeters in all subsequent RDF

experiments. Quartz tubing of the required diameter was used to prepare

38
these crucibles for each bomb calorimeter. The quartz crucibles easily withstand

the thermal shock experienced in the combustion of RDF and other samples, and

after the amount of ash residue is measured, they can be easily cleaned by

heating the crucible and ash residue, and then immersing the hot crucible and

residue into cold water. The rapid contraction of the hot residue frees it from the

crucible bottom and walls, and it can then be cleaned out easily. The quartz crucibles an

thus be used several times.

b. ECO FUEL- 1 1 RDF

Tables 33, 35, and 36 and tables 34, 35, and 36 present the results

measured in the small and large calorimeters, respecti vely , for ECO FUEL- I

I

RDF. The mean values in MJ*kg~^ (Btu*lb"'*) for HHV-AD, HHV2, HHV3-F,

and HHV3-B which can be found in table 36 are 18.78 (8072), 19.09 (8206),

21.98 (9451), and 21.64 (9306) for the small calorimeter, and 18.77 (9071), 19.08

(8205), 21.98 (9449), and 21.64 (9302) for the large calorimeter. On comparing

the two sets of mean values, the differences are less than the standard deviation

obtained for one set of measurements. However, ECO FUEL-II RDF has some particles as

small as 250 m (60 mesh) and is probably the most homogeneous RDF which is

available commercial ly . .These calorimetric results clearly indicate that

the new large 25.0 gram capacity bomb calorimeter gives the same results

as the small 2.5 gram capacity bomb calorimeter, and because of its size,

could possibly even provide more precise results.

c. Americology RDF

Americology RDF, although not as homogeneous as ECO FUEL-II RDF, should

theoretically have identical results in the two calorimeters . Tables 37, 39, and

40, and tables 38, 39, and 40 contain the experimental results measured in the

small and large calorimeter, respecti vely . The mean values in MJ-kg" 1 (Btu-lb’

1 '

of HHV-AD, HHV2, HHV3-F and HHV3-B which can be found in table 40 are 15.67 (6736),

39
16.63 (7150), 22.96 (9871), and 22.69 (9756) for the small calorimeter, and

15.70 (6750), 16.66 (7164), 23.01 (9892) and 22.67 (9746) for the large calorimeter.

Again, on comparing the two sets of mean values, the differences are less than the

standard deviation obtainable for one set of measurements. We feel that the impact

of using quartz crucibles in both calorimeters is also present. Clearly, the two

calorimeters have identical results on the same RDF which has received the same

amount of processing (i.e. particle size reduction). Also, the large 25.0 gram capacity

calorimeter has been proven to be very acceptable for measuring calorific values

of heterogeneous materials as precisely as the conventional small 2.5 gram capacity

bomb calorimeter.

4. Bureau of Mines Processing of New Castle County, Delaware MSW

This set of results are for RDF samples obtained in various stages of

processing through the Bureau of Mines Resource Recovery Pilot Plant in College

Park, MD. Some of these samples had received less processing (i.e. contain larger

particle sizes); however, all had calorimetric measurements performed on

them in the large calorimeter.

To evaluate the applicability of the NBS large gram capacity oxygen bomb

calorimeter, 21 kilograms (46.3 lbs) of RDF was obtained from New Castle County,

Delaware, Municipal Solid Waste (MSW), which had been processed through the

U.S. Bureau of Mines Resource Recovery pilot plant located in College Park, MD

[10]. The pilot plant consists of shredders, magnetic separators, trommels,

air classifiers, cyclones, and mineral jigs. Samples from seven collection

points in the pilot plant had been collected and included in this study.

The overall flow-diagram for this pilot plant is shown in figure 1. The

flow-paths through which each of the seven samples had passed are provided

in figures 2 to 8, respecti vely . The seven fractions (or bags) and their

as-received masses were:

40
1. Cyclone No. 1, Secondary shred, minus 2 inches

2. Cyclone No. 2, Secondary shred, minus 2 inches

3. Cyclone No. 3, Secondary shred, as-collected

4. Cyclone No. 1, Trommel Undersize + 14 mesh

5. Cyclone No. 2, Trommel Undersize + 14 mesh

6. Heavy Organic Combustibles

7. Organic Wastes, Jig Overflow

3664.8 g

3203.1 g

20996.7 g

2672.5 g

3268.3 g

2287.5 g

2361 .2 g

3540.3 g

TOTAL MASS

Each of the seven separate laboratory samples received the following

1. air-drying in a convection oven 0 37+3°C

2. milling to reduce particle size,

a. samples 1-5 were mostly paper and plastic, and were milled

in the Wiley Mill to 2mm particle size;

b. samples 6 and 7 were large pieces of wood, rubber and plastic

and were milled in the hammer mill to 6mm (1/4 inch)

3. splitting to obtain a laboratory sample of workable size by successive

coning and quartering;

4. blending of the laboratory sample in the vee-blenders to obtain a

homogeneous sample;

5. selecting analysis specimens of approximately 2.5 or 25 grams

each:

a. 3 specimens for calorific value measurements

b. 2 specimens for residual moisture measurements

c. 2 specimens for furnace ash measurements

6. analysis specimens were pelletized with the exception of those from

samples 6 and 7, which did not pelletize well.

treatment:

41
The format througnout this report of presenting three tables for each RDF

sample is also followed for these samples. In addition, the air-drying

moisture data are included with the analytical results since these samples had

nigh moistures, characterise c of field samples of RDF. Total moistures (T.M.)

used to calculate HHV1 (as received) were calculated using the residual moisture

(R.M.) fraction, and the air day loss (A.D.L.) fraction, according to the

following equation:

T.M. = R.M. (1 - A.D.L.) + A.D.L. ; see also Appendix E.

Tables 41, 45, and 52 present the results of measurements on cyclone 1

secondary shred (-2 inch) RDF. The mean values of HHV1, HHV2, HHV3-F and HHV3-B

in MJ-kg' 1 (Btu-lb" 1

) were 16.72 (7189), 19.32 (8305), 22.08 (9493), and 21.80

(9374), respecti vely . The calorific values were measured with better than

0.4 percent precision.

Tables 42, 47, and 53 present the results of measurements on cyclone 2-secondary

shred (-2 inch) RDF. The mean values in MJ-kg” 1 (Btu-lb" 1

) for HHV1 , HHV2, HHV3-F

and HHV3-B were 17.32 (7444), 20.00 (8598), 21.81 (9379), and 21.59 (9282),

respecti vely . The precision observed for these measurements was. 0.2 percent.

Tables 43, 49, and 54 present the calorimetric and analytical

results of cyclone No. 3 as-collected RDF. The mean values of HHV1 , HHV2,

HHV3-F , and HHV3-B in MJ-kg' 1 (Btu-lb' 1

) were 16.29 (7003), 20.35 (8751 ), 22.38

(9621), and 22.47 (9662); they were measured with a precision of approximately

0.7 percent.

The three RDF's from the cyclones were composed mostly of light paper and

plastics with ash contents from 8 to 13 wt. percent and had HHV3 values of

approximately 22 MJ-kg" 1 (9400 Btu-lb" 1 ). The RDF from cyclones No.s 1 and 2

which did not pass through the trommel but was retained on a 1.4mm (14 mesh)

screen, consisted of heavier organics and contained considerably more ash (22-35 wt.

percent)

These ashes are believed to be fairly representati ve of the recovery process

utilized. The light air-classified fraction from the first air classifier

contains the greatest percentage of ash since the only processing involved

42
was primary shredding, separation into large and small particle sizes by the

trommel, and secondary shredding of the large particles which passed

through the trommel. The large particles which passed through the trommel were

mostly composed of light paper and plastics. They showed a characteristic moisture

of approximately 14 wt. percent and a moderate ash content of approximately 8 wt.

percent. However, the small particle heavies from cyclone No. 1 which were separated

by the trommel sieve openings were concentrated with the majority of the noncombustible

materials, such as fine metal particles, small pieces of glass, and inorganic

particles. The ash content data contain values having the largest magnitude

approximately 34 wt. percent (see table 46) of all samples processed at College

Park, MD. However, the heavy fraction from the first air classifier was composed

of metals, wet paper, and plastics, which could account for their failure to be air

classified. This material was then subjected to a magnetic separation

process to remove ferrous metals before a second air classification

step took place. With most of the metals removed from the heavies of the first

air classifier, the material passed through a second air classifier to cyclone

No. 2 and through the same trommel sizing step that was used on cyclone No. 1

material. The large particles which passed through the trommel had moisture

characteristics of light paper and plastics but show less evidence of ash

(approximately 8.3 wt. percent in table 47), since the magnetic separation had

removed most metallic particles which were attached to the large pieces of

paper. However, the undersize material from the trommel was heavier

because of moisture and not because of metallic content, and we measured an

increase in moisture to 13 wt. percent, and a decrease in ash to 23 wt. percent

(see table 48) over the material from cyclone No. 1. It appeared that the cyclone

No. 1 material contained only the absorbed moisture on paper and plastic particles

but unusually high ash values since no attempt (other than air classification)

had been made to separate metallic particles. Meanwhile the cyclone No. 2 material was

subjected to a magnetic separation step before air classification and the

small particle heavies contain considerable amounts of moisture but less than

the small heavies from cyclone No. 1.

43
Tables 41, 46, and 55 present the results of cyclone No. 1 trommel

undersize but larger than 14 mesh RDF. The calculated mean values in

(Btu-lb" 1

) were 12.20 (5244), 14.19 (6100), 21.53 (9257), and 20.73 (8914).

Tables 42, 48, and 56 contain the results for cyclone No. 2 trommel

-1 -1

undersize, but larger than 14 mesh RDF. The calculated mean values in MJ-kg (Btu*lb )

were 12.46 (5359), 16.34 (7026), 2123 (9127), and 21.20 (9116).

Even though the composition of these last two RDF's was different from

the first three RDF's, the HHV3 was still approximately 21 MJ-kg”^ (9000 Btu-lb"^),

which appears to be characteristic of RDF's in general. However, there was a

decrease in the precision obtainable on these more heterogeneous samples.

Except for HHV3-B, where the ash content was based on the bomb residue, the

precision is between 1.0 and 1.8 wt. percent. However, the actual ash (based on the

bomb residue) gave HHV3-B with a precision of 0.2 to 0.5 wt. percent, which was

as expected since the selection of equivalent or representati ve samples was more

difficult with high ash content samples.

The remaining two RDF fractions contain large pieces of wood, shoes,

plastic, putrescibles and yard waste. The material had components too

large for the Wiley laboratory mill, and therefore was an opportunity to test

the large calorimeter on samples with minimal processing. These last two RDF

fractions were processed through our 5hp hammermill equipped with a 6mm

(1/4 inch) screen. Usually the combustion samples are pelletized to get

controlled burning from the sample surface, however; the composition of these

samples was such that they did not pelletize well and consequently were burned

as loose material in the combustion crucible. The base material burned more

rapidly because of the increased surface area and made it difficult to collect

all of the bomb combustion residue. Therefore, HHV3-B will not be reported

for these samples because quantitative bomb residues could not be determined.

44
Table 44 contains the experimental results for the heavy organic combustibles

(high tension non-conductors) and organic wastes from the jig overflow RDF's.

In tables 57 and 58, the mean values of HHV1 , HHV2, and HHV3-F

for the heavy organic combustibles RDF in MJ*kg”^ (Btu*lb~^) were 20.85 (8965),

21.92 (9422), and 24.61 (10579), while those for the jig overflow RDF were 19.57

(8416), 20.69 (8896), and 23.37 (10006), respectively. The precision of the heavy

organic combustibles RDF measurements was 0.2 percent and that of the jig overflow RDF

was 1.28 percent. The low precision of the jig overflow RDF could be due to an

unexplained large systematic error in the first combustion experiment (Number 1046).

Omission of experiment number 1046 gave mean values of HHV1, HHV2, and HHV3 in

MJ-kg" 1 (Btu-lb" 1

) of 19.72 (8478), 20.84 (8962), and 23.45 (10 080) for the

jig overflow RDF. Also the precision had increased to 0.04 percent.

Since the ash content was approximately 11 percent, selection of identical samples

should not have been difficult and the experimental results should have been more

repeatable.

The heavies from the second air classifier were subjected to another

magnetic separation step and the remaining material was sent through the sizing

trommel similar to that used for the material from cyclones No. 1 and 2.

The small particle material that did not pass through the trommel was composed

of mostly glass and small pieces of wood and plastic. This small-particle

material was sent to a mineral jig for separation of the organic waste (small pieces

of wood and plastic) from the recoverable glass particles. This material did

not contain much absorbed moisture and only a moderate amount of ash, since it had

had metal and inorganic (glass) materials removed. Therefore, we measured

and calculated approximately 5 wt. percent moisture and 11 wt. percent ash.

The large-particle material that passed through the sizing trommel was

secondary shredded and then air classified into two fractions. The heavies

from the third air classifier were passed over an electrostatic separator to

remove the aluminum. The remaining material was very similar to the organic

45
waste from the jig overflow except that it was larger in particle size (i.e. bigger

pieces of wood, plastics, etc.). The residual moisture and ash values were 5 and 11 wt.

percent, respectively , values similar to the those from the jig overflow

organic wastes. The light fraction from the air classifier was processed

through cyclone do. 3 and then collected. This material contained only 9 percent

ash since most of the metals and inorganic materials had been removed, but did

contain the heavier paper and plastics that were not air classified in two

earlier attempts. This material did show a larger moisture content of 20 wt.

percent, similar to the fraction from cyclone No. 2.

The above discussion dealt primarily with the combustible output of New

Castle County, Delaware MSW that was processed through the Bureau of Mines

Resource Recovery facility located in College Park, Maryland. The process

described is used to recover several recoverable fractions from municipal

solid waste (MSW), namely combustible fraction, glass fraction, ferrous

fraction and non-ferrous fraction. The combined results from the seven

combustible fractions from the Bureau of Mines Resource Recovery facility

provided some important information on the combustible portion of MSW.

A composite calorific value can be calculated by addition of the fraction

of the heating value supplied by each component according to the following

equation:

7 HHV(i) = z

j = l HHV(i.j)

However, this assumed that the mass of each sample is selected in the same

relative proportion as compared to the total mass collected at each point.

The calculated composite HHV(i) in MJ-kg

- "* (Btu*lb~^) would be:

HHV1 = 16.91 (7270)

HHV2 = 19.35 (3319)

HHV3-F = 22.56 (9701)

46
Measurements in the large bomb calorimeter were made on samples with

particle size from 6mm (1/4 inch) to 2mm. The precisions observed were of the

order of 1 percent or better. These measurements show that the large bomb

calorimeter is applicable to RDF samples which have experienced less processing

than those measured in the small (conventional-size) bomb calorimeter.

5 . Representative or Unique RDF's

Several RDF's which had some especially interesting characteri sties were

investigated to evaluate the calorimetric procedures used in the small (2.5 gram

capacity) calorimeter. In addition to tne evaluation of our test procedures,

the effect of some special properties on the calorific value of RDF was

studied. The RDF samples used in the small calorimeter were processed to

0.5mm particle size. As usual, tnree tables are presented for each RDF studied:

one on the calorimetric data, one on the analytical data, and one on the

calorific values which have been calculated to different bases.

a. Teledyne National RDF

A Teledyne National RDF sample was obtained to evaluate the effect

of the method used to determine the total moisture content of a given RDF.

Two techniques have been tested. One was identical to that used for coal and

coke samples and is referred to as the dual -step method, in which the RDF

sample was air-dried to obtain a residual moisture content which was in

equilibrium with ambient laboratory conditions. This was followed by a residual

moisture determination on an analysis sample on the same day of the calorimetric

determination. The air-dry loss was combined with the residual moisture to

determine the total moisture of the as-received RDF.

The otner method, which is referred to as the single-step method, determined

the total moisture in one step at 107 + 3°C. Tables 59, 60, and 61 and 62,

63, and 64 provide the experimental data for the Teledyne National RDF, which

had undergone single-stage and dual-stage moisture determinations,

respecci vely

.

47
The NBS portion of the Teledyne National RDF was split into two equivalent

samples, one for the single-step moisture part of the study and the other for the

two-step moisture part of the study. The fraction of the sample which was used in

the single step moisture experiments was placed into two drying pans and treated

at 107 + 3°C until dry. The measured values for total moisture were 21.79 and

21.65 percent, with a mean value of 21.72 percent. The two-step moisture portion

was also placed into two drying pans, but was only heated to 37 + 3°C until the

samples were in equilibrium with ambient laboratory moisture conditions. The

moisture loss at 37°C (air-dry-loss) was found to be 17.67 and 17.57 percent,

with a mean value of 17.62 percent. The mean value of the air-dry-loss was later

combined with residual moistures that were determined on the day that the heating

value measurements were made. Residual moisture values of 6.25, 6.21, 6.10 and 6.12

percent were combined with the mean of the air-dry-loss, 17.62 percent, to yield

total moistures of 22.77, 22.74, 22.65 and 22.66 percent, with a mean of 22.71

percent. The moisture content depends upon the ambient relative humidity and,-

therefore, inherent in the two-step moisture determination was the assumption that

the relative humidity on the day of the air-dry-loss determination was the same

as on the day of the residual moisture determination. Obviously, no such

assumption is necessary for the single-step moisture technique, and for that

reason it is a superior method.

48
Tables 60 and 63, which report residual moisture, ash, and sulfur content

data, show reasonably good agreement between the furnace ash, bomb ash, and sulfur

determinations. Mean calorific values for HHV2, HHV3-F , and HHV3-B are given in

table 61 for the single-stage moisture method; they are, in MJ«kg

_1

(Btu*lb~^),

as follows: 19.28 (8291), 20.75 (8922), and 20.53 (8824), respecti vely

.

Similarly, mean calorific values for HHV-AD, HHV2, HHV3-F, and HHV3-B are

given in table 64 for the two-stage moisture method; they are, in MJ*kg“^

(Btu-lb" 1 ), as follows: 1825 (7846), 19.45 (8362), 20.98 (9021), and 20.79

(8938), respecti vely

.

b. Steam Size Reduction RDF

A novel approach to the processing of MSW to an RDF is under development

at Burke, Davoud and Associates in Richmond, V a. The process consists of

3 introducing compacted MSW (^ 20 lb- ft ) into a cylindrical pressure vessel 1 ft

in diameter and 8 ft in length (wall thickness 1 inch) and filling the vessel ing

with steam until a pressure of 200 psig is reached. The pressure vessel

has been dubbed: The Great Garbage Gun. The pressure of 200 psig is

maintained for about 45 minutes and temperatures of around 380°F

(193°C) are attained. This period is referred to as the "cook time". After

this period, the door at one end of the cylinder is opened instantly and the

steam and hot MSW expand rapidly into the air. Rapid release of steam and hot

MSW is an important feature. The hot MSW undergoes high turbulence and is

sheared into a finely divided material as it is falls onto a sandy land fill

or is caught on a large plastic sheet. A sample of this product was sent to

us by Mr. Donald K. Walter (DOE Office of Energy from Municipal Waste) for

higher heating value determination. The DOE sample appeared to have an average

particle size of about 0.125 inch.
Tables 65, 66, and 67 present the data for the RDF made in the Steam

Size Reduction. This RDF sample had a furnace ash and bomb ash of 16.55 and 16.82

wt. percent, respectively, and is shown in table 66 along with data on residual

moisture and sulfur content. In table 67, the mean values of HHV1 , HHV3-F,

HHV3-F and HHV3-B are reported in MJ*kg~^ (Btu*lb“^) to be: 16.46 (7076),

17.17 (7383), 20.58 (8846), and 20.64 (8875), respecti vely

.

The more highly processed RDF samples, such as that from Teledyne National

(HHV2, 8598 Btu«lb”^) and ECO FUEL- 1 1 (HHV2, 8205 BtU’lb"'®) are about 11 and

16 percent higher in calorific value than the Steam Size Reduction RDF sample we

studied; however, the Burke-Davoud process is less complex. The sample we received

may not have been representative of the original batch and looked different from

other RDF samples which have been studied in our laboratory. It had a sweet odor

reminiscent of brown sugar which is obtained from cooling semi cellulose to

glucose.

c. NCRR Storage Pile RDF

Some densified RDF which had been stored at the NCRR Resource Recovery

Facility in Washington, D.C. for approximately 10 months had spontaneously

charred during storage. As part of our RDF test method development

program, we undertook to determine the calorific value of this charred sample.

The extent of charring of the storage pile RDF could be estimated by examining

the difference between the actually determined calorific value and the mean

calorific value of most RDF samples, 2210 MJ*kg

-

^ (9500 Btu*lb"^), on a

moisture-ash-free basis.

The gross calorific value of the NCRR storage pile char RDF was

comparable to that measured for other RDF's. This material was much like coal

and did not pelletize very well. It had been milled down to a particle size of

0.5 mm (32 mesh) and we experienced sample containment
Il

problems during our combustion experiments. To make reliable measurements on

this RDF char, it is probably necessary to follow the coal processing

l| techniques and mill the sample to 0.25mm (60 mesh). In addition, the ashing

technique may not have been correct. The ash remaining after treatment at

ft 575°C was always larger in mass than the bomb residue. The ASTM editorial draft standard

||

for the ashing of an RDF sample suggests 575°C as the ashing temperature.

Established ASTM protocols for ashing coal and coke samples use 750°C.

|

Apparently, a char must be ashed at temperatures higher than 575°C. In general, a

modified set of procedures must be used for RDF char.

* Tables 63, 69, and 70 provide the data determined for the NCRR charred

(

storage pit sample. Table 68 gives the details of three calorimetric

measurements on this sample, while table 69 gives data on residual moisture, ash,

and sulfur content. The furnace ash (31.03 wt. percent) is larger than the

bomb ash (25.85 wt. percent) by about 5 wt. percent. As mentioned earlier, the

conditions of the two ash forming methods are quite different. The ashing

temperature used in the ASTM ashing protocol (furnace ash method) is 575°C,

and a much higher ash content was found here than with the bomb ash method.

ASTM ashing protocols for coal use 750°C for the ashing temperature, while

coke is ashed at 950°C. Temperatures attained in the combustion bomb during

a calorimetric measurement are of the order 1500-2000°C; hence, a more complete

asning of a char sample is obtained. Table 70 shows the calorific values

calculated to different bases. Mean values in MJ*kg~"* (Btu*lb

- ^) for HHV1

,

HHV2 , HHV3-F , and HHV3-B are: 16.06 (6906), 16.41 (7057), 23.81 (10237),

and 22.17 (9530), respecti vely

.

d. NCRR Low Ash RDF

An RDF sample was collected by NCRR and was primarily office wastes

from various government buildings in the Washington, D.C. area. This RDF was

expected to have a low ash content. Heavy inerts, metals, non-conductors, and food
wastes were expected to be present in very low concentrations. The overall

processing of office wastes should be easier because of an expected low ash

content. Correspondingly , the calculated higher heating value on a moistureash-free basis (HHV3) should also be lower than the usual RDF sample.

Tables 71, 72, and 73 provide data determined for the NCRR Low Ash RDF

sample. Table 71 gives the details of three bomb calorimetric experiments

in which the following calorific values were calculated on an as-determined

basis in MJ-kg" 1 (Btu-lb' 1 ): 15.71 (6753), 15.68 (6741), and 15.62 (6715).

Table 72 shows an average residual moisture, furnace ash, bomb ash, and sulfur

content in wt. percent of: 5.27, 11.80, 11.29, and 0.095, respectively.

Calorific values which have been calculated to different bases are found in

table 73; average values for HHV1 , HHV2, HHV3-F, and HHV3- B in MJ*kg"^ (Btu*lb~^)

are: 15.67 (6736), 16.54 (7111), 18.75 (8062), and 18.64 (8015), respectively.

52
IV. Summary and Conclusions

This report provides data on 106 calorimetric measurements for 20 different

RDF samples. In conjunction with the above calorimetric measurements, 32 calibration

measurements were carried out from time to time on both small and large bomb

calorimeters . Along with the calorimetric measurements, experiments were performed

to determine the air dry loss, residual moisture, furnace ash, bomb ash, and sulfur

content so that the calorimetric data could be corrected for their presence in the

various RDF samples. A total of 283 such experiments were conducted. Critical

examination and evaluation of the experimental results allow us to make certain

conclusions with respect to the objectives of this interagency research agreement.

The objectives, which are also stated in the Introduction, are as follows:

(1) to investigate the size reduction and homogenization required to

obtain representative samples of refuse and RDF,

(2) to evaluate calorimetric methods for conventional-size (2.5 gram capacity)

combustion bomb calorimeters, and an NBS large (25 gram capacity) combustion bomb

calorimeter; and

(3) to develop test procedures for determining the calorific value of refuse

and RDF samples using bomb calorimetric methods.

The measurement and the evaluation of data on higher heating values determined

during ASTM round robin testing of RDF-3 respond to the first objective. It was

found that the heterogenei ty of RDF-3 and RDF which has been milled down to 0.5

mm particles causes the extraction of a representati ve sample from a larger sample lot

to be difficult. The results of the statistical study on the ASTM testing of

RDF-3 for three round robins shows that the within laboratory agreement for HHV2

(dry basis) is 250 Btu*lb""'; compare this value with the maximum acceptable

variability for coal and coke which is 50 Btu*lb~"*. Similarly, between laboratory

agreement on processed RDF-3 samples for HHV2 (dry basis) is 750 Btu*lb"^; again,

53
compare this value with the maximum acceptable limit for coal and coke which is

100 Btu-lb""*. These levels of precision identify the current state-of-the-art

with respect to the determination of the calorific value of refuse and RDF samples

using the tentative ASTM procedures. Improvement in the levels of precision will

come forth as progress is attained in separation, size reduction, and, in particular,

in sampling procedures. As has been mentioned already, the heterogeneity of refuse

and RDF samples milled down to 0.5 mm particles makes extraction of a representati ve

sample difficult.

Studies on the grab and representative samples of Americology RDF provide

additional responses to the first objective. The difference in HHV2 for the two

samples amount to about 5.5 percent (364 Btu*lb"^), while the measurement error

(standard deviation) is about one percent (^ 70 Btu*lb~^). Examination of the ash

content data for the two Americology RDF samples shows that the average values

for the furnace ash differ by 2.9 wt. percent, while the average values for the

bomb ash differ by 1.2 wt. percent. These differences are due in part to the

* assumption that furnace ash data can be applied to higher heating values to

calculate HHV3, and in part due to the overall heterogenei ty of RDF. Here also,

improvements in the agreement between a grab and representati ve sample will develop

when better sampling procedures can be found.

Our studies on combustion measurements of three RDF samples (Teledyne National,

ECO FUEL- II, and Americology) in the small (2.5 gram capacity) and large (25 gram

capacity) bomb calorimeters respond to the second objective. The one percent

difference in calculated calorific values between determinations carried out

in the small and large calorimeters on the Teledyne National sample was due to the

reactivity of stainless steel crucibles used in the large bomb, as compared to

platinum crucibles used in the small bomb. A search for a suitable replacement

for stainless steel resulted in the use of quartz crucibles for the small and

54
large bomb calorimeters. Quartz crucibles were used for the subsequent

measurements on ECO FUEL-II and Americology RDF samples. The results showed that

the calorimetric data on ECO FUEL-II agreed to within 0.01 percent and on

Americology RDF to within 0.2 percent. In summation, calorific values of

equivalent high precision could be obtained in the large bomb calorimeter as well

as the small one.

The calorimetric measurements performed on the New Castle County, Delaware

MSW, which had been processed through the U.S. Bureau of Mines Resource Recovery

facility in College Park, MD were all performed in the 25 gram capacity combustion

bomb calorimeter. Samples which were composed of either 6 mm or 2 mm particles

were burned in this calorimeter. The precisions observed were one percent or

better and showed that RDF samples of larger particle size could be accommodated.

The 6mm material was very difficult to pelletize, and therefore, the combustion

of the material was less controlled. However, the calorific values determined on

the 6mm material were measured with the same precision as those from 2mm or 0.5mm

material. Therefore, for large (25 gram) samples, processing to only 6mm produces

an RDF sample homogeneous enough to choose representative samples for bomb

calorimetric measurements at the one percent level. This is an important finding,

since a great deal of time and effort are consumed in the particle size reduction

process. The main advantage of the large bomb calorimeter is in the time saved

by being able to select and burn a sample after only limited processing.

The third objective, to develop test procedures, is realized in the descriptive

content of the sections of this report under: II Experimental and III Results

and Discussion. The step-wise methodology is outlined in detail and is also

accompanied by interpretive and evaluative commentary. Data for the common

measurement statistics (i.e., mean, standard deviation, and percent standard

deviation) are given in all tables in which data on calorific values are calculated

to different bases. A summary of the mean calorific values obtained in calorimetric

measurements on the RDF's studied is provided in Table 74.

55
The present study, which introduces the 25 gram capacity bomb calorimeter

for the combustion of refuse and RDF samples of large particle size, has also

established the foundation for the next phase of research and development in

the combustion calorimetry of larger samples. We have made some progress in the

proper direction, however, there is still a need to develop a combustion calorimeter

which can accommodate a sample several kilograms in size. The system developed

should probably be a flow (constant pressure), rather a bomb (constant volume),

C system. One ton of refuse or RDF is equivalent to about 1,000,000 or 10 grams.

Calorimeters which accommodate gram-size amounts of sample provide calorific

values representing 1 to 25 ppm of a one ton field sample. A combustion

calorimeter which accommodates kilogram-size samples will provide the additional

assurance needed by combustion engineers who seek data on calorific values that

such a sample represents multi -ton quantities of refuse and RDF. Such a system

would provide reliability heretofore not available to the engineering community.

56
V. References

[1] Kirklin, D.R., Mitchell, D.J., Cohen, J., Domalski, E.S., and Abramowitz, S.,

NBSIR 78-1494, "Test Procedures for the Determination of the Gross Calorific

Value of Refuse and Refuse-Derived Fuels by Oxygen Bomb Calorimetry.

Summary of the 1977 Fiscal Year Results." December 1978.

[2] Kirklin, D.R., Domalski, E.S., and Mitchell, D.J., NBSIR 80-1968,

"Determination of the Calorific Value of Refuse-Derived-Fuels by

Large-Bomb Calorimetry. Summary of. the 1978 Fiscal Year Results."

January 1980.

[3] ANSI/ASTM D 346-78, "Standard Method of Collection and Preparation of

Coke Samples for Laboratory Analysis."

[4] ANSI/ASTM D 2234-76, "Standard Method for Collection of a Gross Sample

of Coal .

[5] Domalski, E.S., and Abramowitz, S, Proceedings of the 7th Mineral Waste

Utilization Symposium, M.Van Ness, Jr., Editor, 20-22 October 1980,

Chi cago , 111., pp 70-83.

[6j Sunner, S. , and Mansson, M. , Combustion Calorimetry, Experimental Chemical

Thermodynamics , Volume 1, Pergamon Press 1979.

[7] Rossini, F.D., Experimental Thermochemi stry , Interscience Publishing

Co. , New York, N.Y. 1 956.

[8] Jessup, R.S., "Precise Measurement of the Heat of Combustion with a

Bomb Calorimeter," NBS Monograph 7, 1960.

[9] Register, S.H., "Oxidation of Sulfur Compounds of Coal, and of Nitrogen

in a Bomb Calorimeter and the Correction to be Applied in Determining

the Heating Value of Coal," Ind. Eng. Chem. 6_, 812 (1914).

[10] Sullivan, P.M., Stanczyk, H.M. , and Speedlove, M.J., U. S. Bureau of

Mines Rept. of Investigations, "Resource Recovery from Raw Urban

Refuse" RI 7760, (1973).

57
TABLE 1. ENERGY EQUIVALENT VALUES

DETERMINED DURING FY 1979

(2.5 GRAM CAPACITY BOMB CALORIMETER)

Date Expt. No. E,si -empty/

J

07-31-78 1175 14550.22

08-01-78 1176 14550.44

08-17-78 1191 14550.51

08-18-78 1192 14543.31

08-18-78 1193 14545.06

12-26-78 1201 14552.37

12-27-78 1202 14543.17

01-04-79 1205 14534.19

01-04-79 1206 14539.05

01-05-79 1207 14537.68

01-05-79* 1208 14541.32

01-06-79 1209 14542.14

01-07-79 1217 14544.70

01-17-79 1218 14546.37

01-18-79 1219 14541.72

01-19-79 1220 14542.89

01-19-79 1221* 14537.99

04-02-79 1238* 14535.57

04-05-79 1239* 14539.68

04-06-79 1240* 14554.84

04-09-79 1241* 14545.42

04-10-79 1242* 14546.47

04-11-79 1244 14538.72

E , s

i -mean/ J - K"

^ = 14543.64

Std . Dev./J-K' 1 = 5.46 (0.04%)

Std. Dev. Mean/J-K' 1 = 1.14 (0.01%)

•* (Most recent calibration results, see Table 2 for details)

5$ I
TABLE 2. DETERMINATION OF THE ENERGY EQUIVALENT

CALIBRATION EXPERIMENTS ON STANDARD SAMPLE BENZOIC ACID

(2.5 GRAM CAPACITY BOMB CALORIMETER, SIX TYPICAL EXPERIMENTS)

Expt. No. 1238 1239

AUc(28°C)/J-g

_1

26410.68 26410.68

m-BA/g(vac.

)

1.633500 1 .633078

q-BA/J 43141.83 43130.72

q-ign/J 1.13 1.28

q-HN0

3

/J 55.46 1.37

q-WC/J 34.20 34.58

q-corr to t^/J 0.02 * 0.02

Q-Total/J 43232.64 43167.96

AT-corr/K 2.970405 2.965121

E-cal/J-K" 1 14554.46 14558.59

Ei -cont/J*

K"^

18.89 18.91

E,si -empty/J*

K"^

14535.57 14539.68

E,si -mean/J* K

- "*

Std. Dev./J*K~^

Std. Dev. Mean/J-K'

1240 1241 1242 1244

26410.67 26410.68 26410.68 26410.68

1.629424 1.628883 1.632755 1.632368

43034.17 43019.92 42122.17 43111 .96

1.10 1.09 1.52 1.10

4.92 3.55 3.10 4.04

34.38 34.48 34.55 34.44

0.03 0.04 0.02 0.00

43074.60 43059.07 43161 .38 43151.54

2.955640 2.956477 2.963287 2.964199

14573.70 14564.32 14565.37 14557.57

18.85 18.90 18.90 18.85

14554.84 14545.42 14546.47 14538.72

14543.45

6.96 (0.05%)

2.84 (0.02%)

59
TABLE 3. DETERMINATION OF THE ENERGY OF COMBUSTION OF

"COMMERCIAL" BENZOIC ACID

(2.5 GRAM CAPACITY BOMB CALORIMETER)

Expt. No. 1188 1189 1190

E-cal/J* K”"

1 14564.92 14564.54 14564.54

A T-corr/K 2.977312 2.379834 2.293676

Q-Total/J 43364.31 34661.17 33406.33

q-ign/J 1 ,03 0.94 0.95

q-WC/J 35.38 27.16 26.13

q-HN0

3

/J 3.57 4.16 3.59

q-corr to t^/J -5.61 -3.62 -3.37

q-BA/J 43329.95 34632.53 33379.03

m-BA/g(vac .

)

1 .640286 1.311060 1.263567

AU°(28°C)/J-g' 1 26416.09 26415.66 26416.52

E,si -mean/J*g“^ 26416.09

Std. Dev./J*g“^ 0.00(0.00%)

Std. Dev. Mean/J*g"^ 0.00(0.00%)

60
TABLE 4. DETERMINATION OF THE ENERGY EQUIVALENT

CALIBRATION EXPERIMENTS ON "COMMERCIAL" BENZOIC ACID

(25 GRAM CAPACITY BOMB CALORIMETER)

Expt. No. 2042 2043 2047 2048 2049 2050

A Uc(30°C)/J*g

_1

26411.36 26411.36 26411.36 26411.36 26411.36 26411 .36

m-BA/g(vac.

)

16.277573 16.252797 16.331530 16.228149 16.277317 16.209109

q-BA/J 429912.79 429258.41 431337.89 428607.41 429906.02 428104.55

q-ign/J 2.99 5.21 1.41 1.67 1.88 2.20

q-HN0

3

629.42 140.51 113.81 57.81 128.40 114.36

q-WC/J 500.61 507.93 511.51 507.83 508.65 507.05

q-corr to t^/J -1 .27 -0.89 -1.34 -0.76 ' -1.14 -0.71

q-Fe/J 57.35 60.35 26.50 28.00 25.64 33.24

q-carbon/J -100.62 -52.44 -11.80 -17.70 -13.77 -13.11

Q-Total/J 431001 .28 429919.08 431977.98 429184.26 430555.68 428647.57

AT-corr/K 5.002353 4.987062 5.014116 4.979931 4.995473 4.973686

E-cal/J-K" 1 86159.71 86206.88 86152.37 86182.77 86189.17 86203.19

Ei -cont/J*K~^ 139.40 139.32 138.83 138.60 138.63 138.74

E,si-empty/J*K~^ 86020.31 86067 . 56 86013.54 86044.17 86050.54 86064.45

E,si -mean/J* K~^ 86043.43

Std. Dev./J*K

_1

22.36(0.026%)

Std. Dev. Mean/JI.IC

1 9.13 (O.i011%)

61
TABLE

5.

DETERMINATION

OF

CALORIFIC

VALUES occ

cc

LU OO

cc UJ CoI LL_

DCo

c_> o o to CM CO

p

s • to CO r'* o CO CO CM r— o to to CO r—

r— to LO o o LO p— to 03 CM 03 r— LO ^r • o o o o • I— • to

<3- • LO • • • • LO • to - ' l~ CM CO o o o o CO CM

CT> CO LO to ^r

p

» CO • '53' r>v CM 03 c*-. CO r^. p— o CO r^. o r— o r* LO LO o o LO 1— CO o CO r— LO vj- • o o o o • CM • to

to • LO • • • • LO • to

0) n— CM CO o o o o CO CM I—

r—’ • a. LO E • r—

03 to to CM CO CO O) to •^r to p ' -C

-a C\i • o CM CO r— 1^ 4-> aj CO to O r— o to CM r^- to =3- c •p“ r— LO to 03 o o LO r— CO I— p— 03 aj

s~ i—

LO 'd- • o o o o • CM • to sa o LO • • • • LO • to (T3 1— CM CO o o o o CO CM Q.C

*3* to 3-

03

03 o 03

to3- 03

a>

+-> c

CO LO r— r— o to CO *3- I-"* 03 a> LO '3' to o o LO LO CO CM CO LO LO • o o o o • • to aj

'Cf « LO • • « LO • to

p s_ CM CO o o o o CO CM Q.

LO

0)3

(13 > l~D

ZZ.

4-> Q.X

LU

(13 U

s-S-0u1 o-X

O (13 -X

+-> e "—, o 03 <D

+->1 1 Ll_1 1 O' 1 cr 1 cr

"3-X

rz> -X

cn i—

_u i . jQ

(“3 i

CO O

Oto

CM

-X CD

:rI cr

aCtC I I O' O'

aaci Q

<CI 3

+-> CD

JO

a 03 03 +J QC CD LO to to ^ *s CQ s: 0 • r— cu LO p— p—

L±_ o r^ CO 0 to r— 0 0 to CO CO 0 LO a) o CO r— LO r^. 03 0 0 to r—•

CO CO 0 JZ 1—

LO • 0 0 0 0 • • +-> CO >- <3- • LO • • • • LO • '—

cc t— p— CM CO 0 0 0 0 CO CM r— aj —1

h—1 • 4-> 1— to zz (13 UO < • 03 CO 03 r—

LU Q. DC LO l"- 03

N 3

h- < cn • p— 0 LO to 0 CJ o LO CO 0 03 1— 0 CO to n— 03 C\J LO r—

CC' LO (— LO CM to 0 0 LO r— to CM ^r 0 (13 t—1

2: <3- r— to LO • 0 0 0 0 • CM • u

CD <c 'd' • to • « • to • o DC +-> r— CM CO 0 0 0 0 CO CM r— 0

QC CO (13 4-> a LO T3 -0 ~rw • O) a> ZD CM +-> LO o p (13 LO co 3

ac s_ to CO 03

X *x ZD CO • to r->» p— CO cn (/) s: r— LO CO LO CO r— 0 03 to r— =3- LO (0 1

r— p— LO CO r— 0 0 LO p— r— 03 ^r 0 s

oo • 1“ f— LO =3- • 0 0 0 0 • r— • < 0 <3- • to • • • • to • LO ^ 

p—

cr r— CM CO 0 0 0 0 CO CM r— 1 LU 01r—

LO • a; 3

r— 03 r— <=^“ +J Q. to 0 r— CO ^ CQ E r^. • f— r— CO *3- • LO

(13 LO CO CO to 1

0 0 r-'» co t"» LO CXJ to to p— LO 0 0 to r— CO CO f— 0 CM r— LO LO • 0 0 0 0 • CM CM • I''* • • • • r^. • ^ 

03

r—

CM CO 0 0 0 0 CO CM r— • 1 ^—

03CM

CD

-X IIIIIIVI

RP
iC CO r—

CO r— o CO oo

4— -P OO CO CO CO CO o CM r— C • I r— r—’ p— i—» o CM 3 O -P a • • • • • • H— CO O S o o o o o o CNJ

LjJ Oco

oc2>

OOQ

OCd < ,—.. , s 1— QC •

#» 00 LU zc 5^

JZ o; H— • OO 'd' CM O') OO r^. oo >—t

LU cd JO * CO OO '=0’ LO LO CM O') < LU E -C • • • • • • • • H—( n O co -P 00 OO OO 00 00 O O Cd 1n

co < 3 CVJ CM CM CM CM

LU OO 0 ^r

cd 1 ZD Lu c 1— 1— O 0 < OO Cd H CO Q o Lu 2: LU . - O 0 1—

CO <

_l

O QC . < 2! >- CO

ZD

—t 1— 1—1 Q 1— hTMH _l

i—i

OO 0 1—1

OO LU < =3

LU 1— Q. cr O) Cd <c LU u cHi ST 0 03 5-S '^r O O O') CO O u_ H—1

OO

C -K LT3 CM LO r— O')O o CO LU S- JO • • • • • • • • 0 < _l O 1/1 -P UD OO 00 O 2: cd oc Cu LU < S CM CM CM CM CM 0 CZ3 t—H 0 < f— 2: LO OO < ZD • -

1

Cd

LU

OCd

ooc

C\J

CO

03 -Q

>)

S_ "O • r- 0J 03 LO 03 iC3 Z5 O

LU T3 +J 5? CT) CXD CO r— CO -P

_J •r- </i LO 0 LO CO LO LO

CO CO -I—

O r— CT) CT^ 0 O CO "CD < CD O -P • • • • • • • 0) (— QC 2 3 LO ’.n LO O r— u

=3 -O

0) . s- > 0) • • <u s- 0 > 0 03

ai CO • 03 • "O -P

-P CO CD 0 c • -p 03 Q. 'JO LO LO 03 -0 00 ZD X r— r— r— r— <U -p —

LU 1 1 r— 1— 21 00 =>«

X

63
TABLE

7.

DETERMINATION

OF

RESIDUAL

MOISTURE,

ASH,

AND

SULFUR

CONTENT o

zr

ZD

OOLU

O<

Q_<Co

<c

00

cooDC <c

CCC3

ccQ

Occ

uo

C\J

O0

i- c

O)

4-> c n o +-> oo O 3 occ

h— cc

oo LU

cc 1—

h—t

LU "u_— S 

b—1

0) cc CJ O

CO o- 0 03 1 _l LO C * ^<0

Ljl_ < o S_ sc • a o r— a to 4-> cc

CD I— U- <

ll. S < o oca oo o LU

O) >> SS- C3 O -U> CO ^

S_ -r- CO

lo

to 1— lo UO CO CO _Q * 3« r^. CO r— CO CM LO to E -£= • • • • • • • • O to +-> CO "=3- UO CO =3- o CM CQ< 3 CM CM CM cu CM

>— CU

03 S_ O =3 a +-> CO LO CTi CM oo 3^

•C- to 3^ CO *=3" LO LO LO

to - 1— CO r— CM ~ CM C\J o CO

CD

O -M • • m • • • • QC s: 3 =3- '3* o i

co

03 .Q

>>

S_ -a

03O

+J +J • 1 1 1 i i i -a 2 | 1 1 i i i aiu

C3 -a

0)s_ > CL) • • OJ s- O > a 03 r— (XI CO a> r^ o • 03 • r— r— r— r— -a 4->

+-> r— r— r— i— c • +-> 03 Q. 03 -a oo Q X O) +-> >

LU s: oo 3^5 -X IIIIIiIIIIII

II

64
TABLE 8. CALORIFIC VALUES CALCULATED TO DIFFERENT BASES

A STM ROUND ROBIN TESTING OF RDF-3 (FIRST ROUND)

(2.5 GRAM CAPACITY BOMB CALORIMETER)

i

If

ii

I

I

m SAMPLES EQUILIBRATED AT 45% R.H.

1 HHV-AD HHV2 HHV3 -F HHV3-B

<pt. No. MJ •kg

-1

(Btu-lb

-1

) MJ-kg

-1

(Btu-lb

-1

) MJ • kg

-1

(Btu-lb

-1

) MJ-kg

-1

(Btu-1

1167 16.34 (7026) 17.22 (7401) 23.12 (9940) 22.60 (9717)

1168 16.45 (7073) 17.34 (7454) 22.87 (9833) 22.62 (9723)

1169 16.42 (7060) 17.28 (7429) 22.56 (9699) 22.56 (9701)

1170 16.40 (7051) 17.26 (7420) 22.59 (9711) 22.62 (9724)

lean 16.40 (7052) 17.27 (7426) 22.78 (9796) 22.60 (9716)

td. Dev. 0.05 (20) 0.05 (22) 0.26 (114) 0.02 01)

Std . Dev. 0.28% 0.29% 1.16% 0.11%

J*kg

-1 = 429.9226 Btu-lb

-1 was used to calculate the Btu-lb

-1

values presented

in parenthesis.

65
TABLE 9. CALORIFIC VALUES CALCULATED TO DIFFERENT BASES

ASTM ROUND ROBIN TESTING OF RDF-3 (FIRST ROUND)

(2.5 GRAM CAPACITY BOMB CALORIMETER)

DRIED SAMPLES AT 105°C

HHV-AD HHV2 HHV3-F HHV-B

xpt. No. MJ-kg" 1 (Btu-lb"

1

) MJ-kg" 1 (Btu-lb' 1

) MJ-kg' 1 Btu-lb' 1) MJ-kg" 1 (Btu-lb

1171 16.27 (6994) 16.99 (7305) 22.41 (9635) 22.28 (9578)

1172 16.16 (6947) 16.88 (7256) 22.26 (9570) 2232 (9597)

1173 16.00 (6877) 16.71 (7182) 22.03 (9473) 22.32 (9595)

1174 16.21 (6970) 16.93 (7280) 22.33 (9602) 22.24 (9559)

ean 16.16 (6947) 16.88 (7256) 22.26 (9570) 22'. 29 (9582)

td. Dev. 0.12 (50) 0.12 (53) 0.16 (70) 0.04 (18)

Std. Dev. 0.72% 0.73% 0.73% 0.18%

J » kg

-

^ = 429.9226 Btu-lb' 1 was used to calculate the Btu-lb'

1 values presented

in parenthesis.

66
TABLE

10.

DETERMINATION

OF

CALORIFIC

VALUES I II aoacooUJ

GO

COo

QCo

CS2:

1—1

h—

GO

COoa;oC£

GO<

oc

LU

LU

QCo

_l0

ca2; oca

C_> <

Q_<co

QC

CO

LOCM

VO

00• CM cn f— CM OD

C\J VO CO O'! r—

O 3” CM LO CM r— O O LO

-X r— LO . OO

O e p— • CO • • • E CM CO O O O

LO VO r— • CO O CO • CO LO CM r— OD 1 O CO O CM VO uo LO O O LO 1— r— LO LO • O O 0 • CO . • • Q r— CM CO O O 0 LU

GO

GO

LUO

QC

Q_ CM

CO

O OO • LO r— 1 CM 1— CO CM 1

O CO LU CM VO CO LO O O LO 0 r— LO LO . O O 0

QC *=d" * . « * 1

CM CO

OO 0

r— LO

CO cn

LO • CO OD

CM r—•CO r—

O 1

CM VO LO

OO LO r— LO LO • O O O » • . . 1

CM CO

OOO 1— -—

X

CO

O C\J LO r— CO r— 1— CM p— CO O • CM • r^ » CO • r^v '—^ O CO CM »—

CM3" ^—

cn CM vo O CO CO LO r— LO CM • O • CM r^. r*-. • . CO • r— >«—

<S)

O CO CM •I—GOaj JZ

+j

33

s_ CO 3

CTD ^ Q.

LO vo

O LO CO LO r— CO

C

r— LO CO • CO •r- O • r— « . r— "O O CO CM a>

+-> c

cdLO

<D LO S_

r-» Cl

O LO CVJ

r-'. LO CM CO *xt“ LO r— 3" LO • ^d- <D O • 1— CS . r-'. . p— '>—

r—

O CO CXI 03>I-Q

co r—

CO cn

LO • 0 O CM r— 3" r— (—

O r—

•X CM r— LO 0 O CO

aj r— LO lo • 0 O 0 r— . LO • • • Q. r— CM CO 0 O 0 E

ra LO

GO r^ LO 3" • 1— CO

SC CM r— r— r—

O 0 0 CM LO LO O O CO

LO r— LO • O

O 0 • r— •=d- • LO • . • s_ r— CM CO O O 0 3

Q.

S=OO co O'! -Q CO CO co 3 CM • n— CM r— CM f— CO '3" r—

O LO

s_ LO CM r^.

OO r"~ aj in LO O O 0 +-> • LO . . • c r— CM CO O O 0

CO UOr^

CM • co CO CM p— LO r-. r—

O cr> CM vo CO O O LO r— LO • O O O * LO # • . 1— CM CO O O O r“|" r~D • LZ 2D O • LX 2: S_ — LX '"D i. LX CO • P— O +J c 0 +J 03 u O CT> 0) 2: CL U 1 +-> •p— LU ~r~ X 1 1— | 1 1 1 LU UJ < cr cr cr cr 3

+-> ca r— ^ 

CO LO vo a) LO LO LO CM cn OJ • r— +J CO cn LO r^. -—. 0 . r— '»—

• ai . LO • sc 4J 0 CO CM — 3 1

r—

cn LU 3

r^. p*

—

a

O

CO cn CO CSJ r—

CO CO co LO 0 3

CO CM • r— +j

U 0 • r— LO r^ • LO . r— —

s_

O 0 CO CM 0 +J • 1—

L- •O

a. ai

GO . 3

CM p-

—V

cn cn LO . GO CO f— LO ac 3

(XI CO '-O • i— s

CO LO cn LO 0 * r— r—

—

LO r— • LO • 1 0 CO CM -Q

4-J p—

(3 *3

CM "—S. T3 -U) co LO a; CO CO LO r— +-> p— !

LO • r— 3 LO CO CO CO LO S- CM 0 • r— r— 

0 CXI • LO • r- cn 0 CO CM r— • 1 •p— cn

cn 2 CM

U«£ " V CT '3‘ 2 • p— CU -X O 1 II \ 2> ST JO a» -X cn (— r— p— 0 -—

a • Q. 1 GO u_ LU <c 0 E cn CM a O 1 4-> 3 .X ~2 ac CDC > CQ GO • I 1 1 2~ >—p' ^

2> O' O' — cc X 2
TABLE 11. DETERMINATION OF RESIDUAL MOISTURE, ASH, AND SULFUR CONTENT

ASTM ROUND ROBIN TESTING OF RDF-3 (SECOND ROUND)

INTERLAB COMPARISON SAMPLE

(2.5 GRAM CAPACITY BOMB CALORIMETER)

Ai r DryResidual

Moi sture

Residual

Moi sture

Furnace

Ash*

Furnace

Ash* Bomb Sul futjj

Moi sture (Loose) (Pellets) (Loose) (Pellets) Ash* Contend

Expt. No. wt.% wt.% wt.% wt.% wt.% wt.% wt.% m

1222 18.42 3.271 6.126 19.95 19.84 19.40 0.2606

1223 -- 3.325 6.202 19.43 19.82 18.32 0.266l"

1224 -- 3.352 6.218 20.35 20.11 18.62 0.2858—

1225 3.458 6.167 20.16 20.28 18.96 0.2656

P

Mean 3.352 6.178 19.97 20.01 18.82

1

0.2695

Std. Dev. -- 0.079

‘ 0.0408 0.40 0.22 0.46 0.011

*

% Std. Dev. _ _ 2.34% 0.661% 1 . 99% 1.11% 2 .46% 4 . 13 % a

*(Data are reduced to a dry basis.)

m

m

m

n

fi
TABLE 12. DETERMINATION OF RESIDUAL MOISTURE, ASH, AND SULFUR CONTENT

ASTM ROUND ROBIN TESTING OF RDF-3 (SECOND ROUND)

RDF-3 PROCESSED TO 0.5mm POWDER

(2.5 GRAM CAPACITY BOMB CALORIMETER)

txpt. No.

Residual

Moisture

(Loose)

wt.%

Residual

Moisture

(Pellets)

wt.%

Furnace

Ash*

(Loose)

wt.%

Furnace

Ash*

(Pel lets

)

wt.%

Bomb

Ash*

wt.%

Sul fur

Content*

wt.%

1226 2.452 6.068 — 14.40 12.82 0.1464

1227 2.256 6.061 14.00 14.66 13.81 0.1317

1228 2.341 6.086 14.62 14.75 13.22 0.1386

1229 2.378 6.145 — 14.68 13.88 0.1312

Mean 2.357 6.090 14.31 14.62 13.43 0.1370

Std. Dev. 0.081 0.038 0.44 0.15 0.50 0.0071

% Std. Dev. •3.46% 0.626% 3.06% 1.05% • 3.75% 5.21%

*(Data are reduced to a dry basis.)

69
IJQ• ,—, ^—«S 3 in LO r-«. r— CO

CQ -M o LO 03 r— 03 S 1 CO co co OO (—

co '—« 03 03 03 cr> 03 CM > ' - — —» — ^ 

zc r— C3-S zc 1 03 CO lo cr> lo LO CO

cn 03 p-* CO 00 CO o CM • • • • • • • • i— r— r— r— r— o o rs CNJ CM CM CM CM ^—. « r— i/) 1 1—

JQ LO r— <D • p . ^ ,— , v ^—s

SZ 3 CO 0 1— CM I""- LO 4-> Lu +J +J LO =3" LO OO ^—s

S= 1 CQ CD =3" LO LO LO LO CM CD CO 1— 03 03 03 03 03 LO s- > 1— — p "—^ rO zz r- O) CL

zc 1 Q. ZZ 03 >- JD CO CM <=3- 0 p— CM CM r— r— LO

C • • • • • • • • r—

O CM CM CM CM CM

OO

'“O CM CM CM CM CM -O

00 O) LU +-> oo c < ^ a) CO „—_ r— LO Q 1 <D 1—~ ''' -Q S_ zd r— a.

LU 0 • p—

*—* ^—> ,—v

QZ QZ 3 ^3* CM CM

O LO LU Lu -u> -—

r>» 03

O LO CO

y—v

CD Lu CD QC 1 CQ CD =y LO LO LO CO 3 Lt_ LU CO —•* to 03 03 03 03 03 LO r—

i—< O 1

> O ^—p

—-—^ —

'—•- <T3

Q

O LU zz r—

O >

LU LU 2! zz 1 _l ^3" CO CO CM CO P—

O OO _1 1—1

CT3'—-

OO CO CM r— r— LO p—

1— cu QC -U • • • • • • • 1 2: O • CM CM CM CM CM O O JQ O CO < _J CM CM CM CM CM r—

LU 1 00 < 21 • f— Lu O 3

<c

O zz +-> _l CO 0 CQ CQ

ZD 00 21 t> o Lu H—1 O ID _l O QC CQ (— -C < < 1 +-> o O CU >- JQ -—v ^ —

^—v--—

2: l— r— 03 CO LO aj oo 1—1 0 1—1 • co CM CM ^—

+j LU 1— CD O 3 LO LO LO LO LO CZ5 (13 3) OO <C CM 4-> r^. r^. CO 1—

_l LU CQ Q_ > CQ •*. ^ -

^ 

* •—

3 < 1— c < ZZ - u > _! C_) zz yi* 03 :Z3 =3" ^3" O p—

zz QC r— LO r>. 0 ra o t—1

LU 21 1 . > • • a • • u

1—1

CQ h- <c cn r"- r^. r^. r^. 0 O Lu O QC r— r— r— r— r— 0

1—

H

cz 1—< O • JU DC l"Z o Q LO a. -0

_! zz • CD < ZD CM *—

LO

<L3

O r— 3

QZ 1jQ ^ V -

* ,

^ „

^ LO • y _ 03 LO CM LO LO (13 CO H— • r— r'-» r- LO LO 2

r~— 00 (ZZ 3 r— r— r— r— r— LO < < +J r^. P"- CM r—

LU 1 CQ - - --

—-- s ^ 1 _U > JQ

CO ZZ LO ZZ CO LO yf LO LO r— < zc LO LO LO LO LO O CO • H— 1 • • • • • • • 3

03 LO LO LO LO LOO 0 +-> JX 1 1— 1 1— 1— CQ rO LO 2: CM

CM

03

03CM • *3- > • • CD II 0 > O zz <D r—

CM co LO ZZ • I • CM CM CM CM -O 03

+-> CM CM CM CM c • +-> JZ Ol r— r— r— r— <T3 XJ OO • X CD 4-> l_D

LU 2: 03

70
1Ii«>fiiiiIiIIIi

-Q ^ 

^—„ ^ 

,—. „—.. i— LO r— CO CO

CO • cr> r— LO CO CM .. 1 Z3 o r— r— p— CO CO 4-> GN GN GN as OS CM > CO "w** 1—

— 1 zz —p

CHi ZZ LO O r— ^r CO r-. p— i— r— CM CO CM CM o CO 1 • • • • • • • os r—>

r— r— r— r— o o -SC CM C\J C\i CM CM

toD

JD „ s ^—. ,—. /—s ^ 

-C

r— ol CM LO LO <y\ CO +-> Ll, • 4-> LO O CM p— LO c i Z3 CD CM CM CO CXI C\J a) CO 4-> r— Ol OS as G^ GN LO i_ > CQ p— — >—p • ^ >S—

ca

C/1 zz CD Cl

LU zz Q_ t— as CM CM CO

CO r— '— LO =3* co LO p— LO c < 1 • • i • • • • f~ CQ as p— i

ir— p—

O o ..

0£ CM CM CM <XJ CM T3

H- 3 • a) 2: 2: “D +j

LlJ 2) ST c

QC o <D LQ QC LO

Ll. .p-x .

<D u_ Q QC r— S- t—<

LQ 1 CL

Q

O QC h— JQ ^ , ^ 

CO LQ LQ r— LO i— CO i/l

O LQ

a s: u_ • „—sCO r— CM <D I— OO 3 I—1 i Z3 CD r« CO CM CNJ a v—« O QC CO +-> to os as G'l r— i— Q a. o > CQ o ^ 

ia LQ CO —I zz >—p o 1 1 >

1— 1 E < zz _1 1 LO CO 1 LO ON LO <c Ll. E CO r-» CM CO CM CO r—

_la LO t • • • • « | 23 QC • CQ a> r— r— r— LO r— JQ

C_> o s: CM CM CM r— —J

Ll. o • • C O o CQ 3) a

co 1— s: . +j CO >- • CQ

c/i 2: Q 1— - LQ hH LQ 1—i „

CD zo 1— OO o . -C

—I 00 C/1 <c 1 4-> <c LQ LQ Q_ JQ ,—, .—, ^ -s, p-—, > 1— CO c r— CO CO O LO O <D o CO • CM LO LO LO o +J co ac Z3 os CO as CO GN LO n3 1—«

P-H Q_ s: CM •O r-- r^. p—

Ll. CQ < z> CQ ,— ,—

„ / '—

^ a

H-1 o CO cc zz

—

u

QC QC 1 CO zc r^» as G^ r— as i— o Ll. r— CM CNJ CO p— LO 03 _J Q a LO 1 • • • • • • • O < 2! QC • Ol CO CO 00 CO CO o o CO zo CM r— f— r— r— o o ^ • +J QC • s: -a

'3"T a> r— h— to OO p— 

a

LQ < r—

_1 1 LO CQ -Q .—

.—,PV x-—v

C3 < r— r-^ o CO CNJ GN 2

1—

a • •=3- CO CO CO p— ^—

X < a CO <=^’ CO p— i 4-> C- r-'. I > CQ -—

—p ^ -» V, p' ^ JQ

zz p—

zz CM <o sf LO o o • r

CO r— CO r— CM r— CO

a 1 • • • • • • • -M Ol r^ f^ o o CQ .x r— r— r— r— r—

CO

c\j

C\J

O'!

O'! CM • • > n O > a> 3 CD Q p—

CO CO as

Q i • CM CM CM CM • as

4-> CM CM CM CM sz • a -X

Q. p— p— p— p— ca -a +j • X as +j OO ,-0 LQ s: C/1 s:
CO r— LO S' . CM 1— 03 X X cm • LO CO r— o p— o uo CM CM p>. LO CM 03 CO o o o P'S P^. • 03 E C\J LO cr» o o 1— o • LO X X E r— LO CO • • • • • r— • r—

S" • r— o o o o CM

LD 1— CM O o O LO LO 03 • 1—•

p— r— LO 03 P^ 03 LO r— • S' LO 1— o r— p^ CSJ r^. o o •r—

O LO CM p— CO o o o LO LO CM • 03 LO LU CM LO CO o o r— o • LO X X aj OO r— LO CO • • • • • o • r— — X OO S' • o o o o o CM +-> LU r— CM c

C_) 03 o s_ CC s

Cl r— Q. r— CM LO ^—V

oo CM CO p— LO

X

X e 1 O • r— LO p— o 'd- 03 LO CM 03 •i— LU LO CM CM r—> o o o LO CT> • 03 Q CC1 LO 03 r— o o r— o • LO X X -a

CC r— LO CO • • • • • r— • r—

—

CD S' • CSJ o o o o CM +-> r— CM c

a)

LO

O)s_ 03 a.

CO LO p— p-—s , CM CO CO o S' L/3 0*1 » CM CO p— o r— p^ LO r-p CM X a) 00 Q LO CM LO CO o o o LO CSJ S' • 03 DJ LU CM LO S' o o p— o • uo X X r—

ID re LO CO • • • • • r— • r— ^ ' s o S' • r— o o o o CM > < oc ^ -S r— CM > cc r— Q LU 1 C_3 CC 1— X t—4

4-^ LU p—

LU rn s: • 4—1

H- 4—4 o

O' >— CC 03

X o o i

r-» CO '—

X

_1 co _1 CM S- CSJ 03

X r— < i <c r^. • CM LO p— o CO 03 r— LO r^. X aj o LU o LO CM CO o o 03 LO LO c-. • p^. X Q cm LO S' LO o o o o • LO X X X

Lu O' CQ r— LO p". • • • • • o • p— ^ o s; S' • o o o o o CM O) LU o r— CM X

s. o CQ s o 03 1

i—t

CD >- r— r-— pp. •-

—

p o

i—

X t— CM CM o CM

X CM

u < 4—1 1—4 LU LO • 03 CO r— o 03 03 LO 03 r— x 1 o _l LO CM S' CSJ o o 03 LO CSJ CO • X s

i—i

oo c Cl OJ LO S- o o o o • LO

X

X

u

LU Cl s: p— LO CO • • • • • r— • I —

oc h- < < S' • r— o o o o CM o

LU CJ oo r— CM ^r

X

I— s:

LU u-) T

x

X

QX < o <v O QC oo r— LO Q£ CD 1—t

CM CO 'X ^ 

=5 • cc CM r— LO LO X S'

lo

Q LO <c LO • 03 LO p— o CO o CO LO o o LO r— X • CL LO CM CO o o o 03 r-. LO X • 03 ra =0 OJ S' CM LO LO r^ o o o o • uo X X s

LU o ^ o 1— LO CO • • • • r— • r— * X oc CJ S • r— o o o o CM 1

x p— CM 1 < s; CQ X i

i— <c f—

oo • < cc X o

LU LO 03 r- ^ X

(— ClJ r— CO 03

XX

X s- • LO p— o 03 \—> X r-p

X i—i LO CM LO CO o o 03 LO *=d* CM • X CvJ LO LO LO o o o o • X X X CM p— LO CO >» • • • • r— • p— • CM

S' • r— o o o o CM 03 r— CM p—t 03

03 -CM r— UC p— S' 1 S3 • 1 • X X S3 -X S3 X 11 o • — S3 -X —. u r— X S3 S- p— -X -o 03 • r—

S- 03 -X co o \ O 1 • r— o 4-> c o oo LL. Lu < +J 03

+-> 03 o O 03 OJ s CM

Q

Q 1 X

X

Q.

a 1 h- -p— u_ JC DC CC > — • X i 1— 1 1 1 1 1 1 1 X LU LU < O* cr

a* or cr

cr E X

72
I

TABLE 16. DETERMINATION OF RESIDUAL MOISTURE, ASH, AND SULFUR CONTENT

ASTM ROUND ROBIN TESTING OF RDF-3 (THIRD ROUND)

Ii INTERLAB COMPARISON SAMPLE

ft (2.5 GRAM CAPACITY BOMB CALORIMETER)

Expt. No.

Air Dry

Moi sture

wt.%

Residual

Moisture

wt.%

Furnace

Ash*

wt.%

Bomb

Ash*

wt.%

Sulfur

Content*

wt.%

1254

1

26.35 4.522 21 .29 21.25 0.4689

| 1255 — 4.458 22.05 19.74 0.4857

|

1256 — 4.382 22.31 19.97 0.4764

* 1257 — 4.376 22.54 21 .29 0.4804

1 Mean -- 4.435 22.05 20.56 0.4779

1 Std. Dev. — 0.069 0.54 0.82 0.0071

U % Std. Dev. 1.562% 2.46% 4.00% 1.48%

I *(Data are reduced to a dry basis.)

!

73
TABLE 17. DETERMINATION OF RESIDUAL MOISTURE, ASH, AND SULFUR CONTENT

A STM ROUND ROBIN TESTING OF RDF-3 (THIRD ROUND)

RDF-3 PROCESSED TO 0.5mm POWDER

(2.5 GRAM CAPACITY BOMB CALORIMETER)

Residual Furnace Bomb Sulfur

Moisture Ash* Ash* Content*

Expt. No. wt.% wt.% wt.% wt.%

1259 4.773 22.83 20.82 0.4734

1260 4.740 22.08 20.87 0.4813

1261 4.843 22.60 21.45 0.4788

1262 4.826 22.56 20.79 0.4859

Mean 4.796 22.52 20.98 0.4799

Std. 1Dev

.

0.048 0.32 0.31 0.0052

% Std . Dev . 0.991% 1.40% V. 49% 1.09%

*(Data are reduced to a dry basis.)

74
TABLE 18. CALORIFIC VALUES CALCULATED TO DIFFERENT BASES

ASTM ROUND ROBIN TESTING OF RDF-3 (THIRD ROUND)

INTERLAB COMPARISON SAMPLE

(2.5 GRAM CAPACITY BOMB CALORIMETER)

HHV-AD HHV2 HHV3-F HHV3-B

Expt. No. MJ-kg' 1 (Btu-lb' 1

) MJ-kg" 1 (Btu-lb" ]) MJ-kg' 1 (Btu- 1 b' 1) MJ-kg' 1 (Btu-1

b

1254 15.79 (6788) 16.54 (7109) 21.01 (9032) 21 .00 (9028)

1255 16.06 (6904) 16.81 (7226) 21.56 (9270) 20.94 (9003)

1256 15.98 (6872) 16.72 (7187) 21.52 (9251 ) 20.89 (8980)

1257 15.73 (6761) 16.45 (7071) 21.23 (9129) 20.90 (8983)

Mean 15.89 (6831) 16.63 (7148) 21.33(9170) 20.93 (8998)

Std. Dev. 0.16 (68) 0.16 '(71) 0.26 (111) 0.05 (22)

% Std. Dev. 0.99% 0.99% 1.22% 0.246%

_i

MJ-kg" 1 = 429.9226 Btu-lb" 1 was used to calculate the Btu-lb" 1 values presented

in parenthesis.

75
TABLE 19. CALORIFIC VALUES CALCULATED TO DIFFERENT BASES

ASTM ROUND ROBIN TESTING OF RDF-3 (THIRD ROUND)

RDF-3 PROCESSED TO 0.5mm POWDER

(2.5 GRAM CAPACITY BOMB CALORIMETER)

HHV-AD HHV2 HHV3-F HHV3-B

Expt. No. MJ-kg' 1 (Btu-lb' 1

) MJ-kg' 1 (Btu-lb"

' ]

) MJ-kg' 1 (Btu-lb'

1

' ) MJ-kg' 1 (Btu-lb

1259 16.20 (6964) 17.01 (7313) 22.04 (9477) 21.48 (9237)

1260 16.28 (6998) 17.09 (7346) 21.93 (9428) 21.59 (9284)

1261 16.07 (6909) 16.89 (7261) 21.82 (9380) 21.50 (9243)

1262 16.23 (6978) 17.05 (7332) 22.02 (9467) 21.53 (9257)

Mean 16.19 (6962) 17.01 (7313) 21.95 (9438) 21.53 (9255)

Std. Dev. 0.09 (38) 0.09 (37) 0.10 (44) 0.05 (21)

% Std. Dev 0.55% 0.51% 0.47% 0.23%

‘

MJ-kg' 1 = 429.9226 Btu-lb' 1 was used to calculate the Btu-lb~ 1 values presented

in parenthesis.
TABLE 20. DETERMINATION OF CALORIFIC VALUES

ASTM ROUND ROBIN TESTING OF RDF-3

NBS (SRM 1632a) BITUMINOUS COAL SAMPLE

(2.5 GRAM CAPACITY BOMB CALORIMETER)

Expt. No. 1012 1013

E-cal/J-K" 1 14385.21 14385.21

AT-corr/K 1.907333 1.916937

Q-total/kJ 27.437 27.576

q-ign/kJ 0.001 0.001

q-Fe/kJ 0.000 0.000

q-HN0

3

/kJ 0.101 0.100

q-H

2

S0

4

/kJ 0.084 0.096

q-RDF/kJ 27.252 27.377

m-RDF/g 1 .047333 1.052734

HHV-AD/MJ-kg' 1 26.020 26.006

/(Btu-lb" 1 ) (11187) (11181 )

MJ*kg”^ = 429.9226 Btu*lb

-

^ was used to calculate the Btu*lb”^ values

presented in parenthesis.

77
TABLE 21. DETERMINATION OF RESIDUAL MOISTURE, ASH, AND SULFUR CONTENT

ASTM ROUND ROBIN TESTING OF RDF-3

NBS (SRM 1632A) BITUMINOUS COAL SAMPLE

(2.5 GRAM CAPACITY BOMB CALORIMETER)

Expt. No.

Residual

Moisture

wt. %

Furnace

Ash

wt. %

Bomb

Ash

wt. %

Sulfur

Content

wt. %

1012 1.15 22.19 -- 1.38

1013 1.14 22.13 -- 1.58

Mean 1.145 22.15 1.48

78
TABLE 22. CALORIFIC VALUES CALCULATED TO DIFFERENT BASES

ASTM ROUND ROBIN TESTING OF RDF-3

NBS (SRM 1632a) BITUMINOUS COAL SAMPLE

(2.5 GRAM CAPACITY BOMB CALORIMETER)

HHV-AD HHV2 HHV3-F HHV3-B

Expt. No. MJ-kg" 1 (Btu-lb

_1

) MJ-kg" 1 (Btu-lb"

1 ) MJ-kg" 1 (Btu-lb"

1

) MJ-kg" 1 (Btu

•

1012 26.021 26.323 33.829 --

(11187) (11317) (14544)

1013 26.007 26.307 33.783 —

(11181) (11310) (14524)

Mean 26.014 26.315 33.806 —

(11184) (11314) (14534)

MJ»kg

_1 = 429.9226 Btu-lb_1 was used to calculate the Btu-lb"

1 values presented

. in parenthesis.

I

f

I

(l

!l I

II

V

I 79
TABLE

23.

DETERMINATION

OF

CALORIFIC

VALUES o lO o d lO ix • D CXI CD CM -—

CO CO

D

D p— o co CT)

O co o o I— If) lO in o o in CM m r^x CM 1—’ m r— • o o o O • t— • co

•o- • p— • • • • n— • lO r— CM co o o o o on CM i

—1

in r— o • CO r-» in (/) CO • rx. r— m x • r— ro CO rx in r— o ID CD in CO CVJ 1—= in i—

m CO CO o o in CM x CO aj r— in r— • o o o O • r— • CO JG • r— * • • • r— • LO M i— CM CO o o o o CO CM r— —

e

O)i_

raQ.c o in CO •1— CD o i—

CM • CO CO CO CO

X T3

CO CO CM

m r— o in CD

x

D LO LO Cl) r— in o o o o in CM D CO CT> C\J 4-> r— in CM • o o o O • r— • C

*o- • CM • • • • r— • LO CD r— CM CO o o o o CO CM r— X—

in

CD

t_Q.

in - V CD Od CO D H3

LlJ CO inm r—

LlJ h- r— . o CD

D CO S CO

—1

LlJ CO CO in r— o o D in

D o 1— >

Q. 5~ 1— in r— CM o o in CM r— CM r— cn

s: t—«

r— in CM • o o o O • i— • r— c Of •o- • CM . • • • CM • LO LO | oo o CM CO o o o o CO CM i—

r— = <c • CO C_> 13 < +J Of CO CQ

id CT r o CO r—

D <D CO CO CO CO

r\ o • CO ID

D

X ^—X

+-> Ll_ >- CO CO m O 1— o ix o r— D ^r Q t— r— in CM >=d* o o in CO CO CM r— CNJ <D Of 1—1

r—

m CM . o o o o • r— • LO +-> C_) 'O- • CM • • • • CM • LO LO rO >- < p— CM CO o o o O CO CM p— •—

r—

CO Q_

n o < CJ _I C_) r— o ro o s: U 1 cd CO IX O O

UJ CD CO r— Td- •M

7>

D . D CM CO

x ^ X < in CM CO D CD o o "O' CO o r— LO ^r TH • r— in lO in o o in CM in CM CO co <D CM r— in r— • o o o o • r— • co in —«• • r— . . • • r— • LO 13 r— CM CO o o o o CO CM r— -

cn

rOS

r*“ , lO in '-Q CO CO D p—

CO • in CD COD ^—S • CM CO CM ”=d- r— o ix D in CO LO CVI 13 r— m CO O o o m CM D D CO +-> i m r— . o o O o • O • CQ • i

. . . . o • LO r— CM CO o o o o CO CM r— X ^ mCM

CMD I— • 1 D CO ^ X CM r— r— =d- 1 O • 1 • LC LC -X o -X -Q II o • — x^. o x^ O t—

~r.

r-3 S- r— -X o ~—

-XD ^

• r—

S- rO

—

-X CO o x» o 13 I • o -D c X o cn Ll Li- < +->

D 4-> <0 u o o D o CM a nn i CQ LZ

CL

O 1 +J •r* hi HI QC Of > X • X 1 1— 1 1 1 i 1 i 1 nz

LlJ LlJ c O' a* a- cr

G

r o zc
TABLE 24. DETERMINATION OF RESIDUAL MOISTURE, ASH, AND SULFUR CONTENT

AMERICOLOGY RDF "GRAB" SAMPLE

(2.5 GRAM CAPACITY BOMB CALORIMETER)

Residual Furnance Bomb Sul fur

Moisture** Ash* Ash* Content*

Expt. No. wt.% wt.% wt. % wt.%

1128 2.9774 29.53 29.25 0.2410

1129 2.9664 29.22 28.91 0.2357

1130 3.0585 30.43 26.94 0.2445

1131 3.0499 29.40 27.40 0.2391

1132 3.0275 — 28.24 0.2391

1133 3.0069 — 28.88 0.2355

1134 2.9520 — 29.59 0.2382

Mean 3.0055 29.65 28.46 0.2390

Std. Dev. 0.0417 0.54 0.98 0.0031

% Std. Dev 1.39% 1 .82% 3.45% 1.30%

*(Data are reduced to a dry basis.)

**(Sampl

e

equilibrated at 30% R.H. prior to DET'N.)

81
TABLE 25. CALORIFIC VALUES CALCULATED TO DIFFERENT BASES

AMERICOLOGY RDF "GRAB" SAMPLE

(2.5 GRAM CAPACITY BOMB CALORIMETER)

HHV-AD HHV2 HHV3-F HHV3-B

Expt. No. MJ- kg"

1 (Btu-lb~ ]

) MJ-kg" 1 (Btu-lb"

1

) MJ-•kg"

1 (Btu-lb" 1

) MJ-kg" 1 (Btu-lb

1128 14.75 (6342) 15.21 (6539) 21.62 (9294) 21.50 (9242)

1129 14.85 (6384) 1 5.31 (6582) 21.76 (9357) 21.54 (9259)

1130 15.17 (6524) 15.65 (6726) 22.24 (9561) 21.41 (9206)

1131 15.10 (6491) 15.57 (6693) 22.13 (9514) 21 .44 (9219)

1132 14.95 (6426) 15.41 (6626) 21.91 (9418) 21 .48 (9233)

1133

1 14.82 (6371) 15.28 (6568) 21.72 (9336) 21.48 (9235)

1134 14.70 (6320) 15.16 (6516) 21.55 (9263) 21 .53 (9255)

Mean 14.91 (6408) 15.37 (6607) 21.85 (9392) 21 .48 (9236)

Std. Dev. 0.18 (76) 0.18 (78) 0.26 (112) 0.04 (19)

% Std. Dev. 1.19% 1.19% 1.19% 0.20%

Mj-kg' 1 = 429. 9226 Btu-lb" 1 was used to calculate the Btu-lb" 1 values presented

in parenthesis.

PI

PI
III

III II

CO CO CO o o • CO o CO -—>. o CO CO r— o CO <o- CO 05 r— CM CM in CM o o LO CM r—>

p- CO 00 r— in r— • o o o o • 05 • lo • r— • • • • r— • LO co

r—>

C\J CO o o o o CO 1— i

-—

o o o CO CO CO • CO CO r—> CO LO CO r— o o LO CO r— r^ CO

r—»LO "Of CM o o CO CM 1— >^r cu CO • p— LO i—> • o o o o • o • LO LO • r— • • • • r— • LO CO -r— r— CM CO o o o o CO CM r— LO

aj JO

+-> p^ CO 05 c '=3" LO CM <D • CM CM p— r"~ —

S_ cn CO LO r— o '3- CO p>» o ra r—

LO co LO o o CO CM ^r r— CL f— LO i— • o o o o • o • LO • r— • • • • r— « LO '-O c 1— CM CO o o o o CO CM 1 '

•r-

-a

05 o O I"". +-> LO CO 05 e

LO • o P>» P—V

O)

CT> CO 1— "Sf 1— o o O'- LO co LO 05 LO

L/5 r— LO o o o o CO CM 05 LO LO CO aj LU r— LO CM • o o o o • o • CO S- ro =3" • CM • • • • i— • LO CO a.

_i r— CM CO o o o o CO CM p— ' < LU LO > —1 - » 05 Q. a: 3 o s: LU LO CO r-p r—

i—i

=£ h— ^r p- ^r fT3 Lu OO LU • CM LO co s >

h—1

SI CO LO p- 1— o o CO 05 CO ' LO CO 1 DC LU (—!

p— LO r-* CO o o LO CM LO "d- r— o > DC r— LO r— • o o o o • o • CO | _J i—I o '^r • t— • • • • r— • LO CO JO < I— _J r— CM CO o o o o CO CM r— r— o =C < • t— (_5 3

Lu • +-> o LU CD CO =3" 05 CD OO 2 LO P*. , LU O • CO p» r— ^ 

05 o DC CD CO CO o 05 t— o CO r— ^r CO JO

»—

H

Q. r— LO o =3- o o LO CM CO CO +-> I— LU >- p— LO CO • o o o o • r— • CO c DC 1— ^3" • CO • • • • CO • LO CO 05

•£Z i—i i— CM CO o o o o CO CM i— 4-5 h—1

#\ C_5 03 s: LU <c r—

ocQ Q. 3

LjJ DC < cn o O

H— C_> r— r—

LU >- o • 05 co LO 05 p—

03

a CO SI CO CO CO LO 1— o CM CO co r*^ CO

O o < 1

LO *ct- CM o o LO CM i— CM co o

_1 DC r— LO r— • o o o o • o • CO

C • o o • r— • • . . r— • LO CO 4-> CO o r— CM CO o o o o CO CM p— p CM t—4

LO -a DC • 05 LU LU CM LO _! 21 **—

CO LO 05 3

CD <c =3- CO CO =£ CO • r^. CM CO CM ^ -V L0 1

CO CM CO r— o o CO LO o ^r CM 03 r— LO p^ CO o o -O CM LO CO ^r co 2

f— LO • o o o o • o • CO

'd- • r— • • • • r— • LO CO i—

CM CO o o o o CO CM r— i.a• p~. i

^r 3

'd' LO co ^ +-> r^. • CO CO CO r— CO CD r^ CO r-'v p-. r— o LO CO 05 CO CO r— LO CM 05 o o o CM CO CM • LO lO ( LO • o o o o • o LO CO CM • o • • • • o • r— CM 1

CM CO o o o o CO CM 05 i— • | ^—

05

CD 1— CM r— 1 "3- 1 • JD • LZ “3 "05 I— II o • "

r~D • S_ r— ""3 =3" "~3 05 \ C3 r—

S_ 03 ^3 CO o —

\ Q 4-> 1 • r— o 4-> c o LO LU LU <C CD 35

+-> 03 o O 05 aj cr CM CD CD l —

p

QU 1 +-> • f— LU JZ DC C5C > • X 1 (— 1 1 1 1 1 1 J_ zc "“3 LU LU < cr cr cr cr cr

O" sz HZ

83
TABLE 27. DETERMINATION OF RESIDUAL MOISTURE, ASH, AND SULFUR CONTENT

AMERICOLOGY RDF, REPRESENTATIVE SAMPLE

(2.5 GRAM CAPACITY BOMB CALORIMETER)

Expt. No.

Residual

Moisture

Content**

wt.%

Furnace

Ash*

wt.%

Bomb

Ash*

wt.%

Sulfur

Content*

wt.%

1177 5.131 26.727 30.24 0.2012

1178 5.240 26.896 28.98 0.2285

1180 — -- 29.88 0.2317

1184 5.175 27.098 29.26 0.2238

1194 — -- 29.15 0.2276

1195 5.211 26.544 28.66 0.2362

1197 — -- 30.49 0.2309

1198 — 30.26 0.2238

1200 29.64 0.2102

Mean 5.189 26.816 29.62 0.2238

Std. Dev. 0.047 0.237 0.64 0.0112

% Std. Dev. 0.907% 0.882% 2.17% 4.99%

*(Data are reduced to a dry basis.)

**( Sample equilibrated at 45% R.H. prior to DET'N.)

84
TABLE 28. CALORIFIC VALUES CALCULATED TO DIFFERENT BASES

AMERICOLOGY RDF, REPRESENTATIVE SAMPLE

(2.5 GRAM CAPACITY BOMB CALORIMETER)

I

HHV-AD HHV2 HHV3-F HHV3-B

Expt. No. MJ- kg'

1 (Btu-lb" ') MJ-kg" 1 (Btu-lb"

1

) MJ-kg" 1 (Btu-lb”

1

) MJ-kg" 1 (Btu-lb"

1177 15.27 (6566) 16.11 (6925) 22.01 (9462) 22.53 (9708)

1178 15.54 (6682) 16.39 (7048) 22.40 (9630) 22.60 (9718)

1180 15.37 (6606) 16.21 (6968) 22.15 (9521) 22.61 (9722)

1184 15.44 (6638) 16.28 (7001) 22.25 (9566) 22.54 (9689)

1194

f

( 15.46 (6646) 16.31 (7010) 22.28 (9579) 22.53 (9687)

1195 15.56 (6689) 16.41 (7056) 22.42 (9641) 22.53 (9688

119.7 15.14 (6510) 15.97 (6866) 21.82 (9382) 22.47 (9658)

1198 15.27 (6563) 16.10 (6922) 22.00 (9459) 22.58 (9708)

1200 15.31 (6582) 16.15 (6942) 22.06 (9486) 22.46 (9655)

Mean 15.37 (6609) 16.21 (6971) 22.16 (9525) 22.54 (9693)

Std. Dev. 0.14 (60) 0.15 (63) 0.20 (86) 0.06 (24)

% Std. Dev. 0 . 90% 0.91% 0.90% 0.25%

MJ-kg" 1 = 429 .9226 Btu-lb' 1 was used to calculate the Btu-lb" 1 values presented

in parenthesis.

i 85
TABLE 29. DETERMINATION OF CALORIFIC VALUES

CALORIMETER COMPARISON MEASUREMENTS

TELEDYNE NATIONAL RDF

(2.5 GRAM CAPACITY BOMB CALORIMETER)

Expt No. 1233 1234 1235

E-cal/J-K” 1 14561 .54 14561.63 14561 .62

AT-corr/K 2.660558 2.652241 2.634082

Q-total/kJ 38.742 38.621 38.357

q-ign/kJ 0.001 0.001 0.001

q-Fe/kJ 0.000 0.000 0.000

q-HN0

3

/kJ 0.069 0.068 0.067

q-H

2 S04

/kJ 0.16 0.17 0.018

Q-RDF/kJ 38.656 38.535 38 1 271

m-RDF/g 2.001529 1 .986701 1.979255

HHV-AD/MJ kg

-

"

1 19.31 19.40 19.34

/(Btu-lb' 1

) (8303) (8339) (8313)

86
TABLE 30. DETERMINATION OF CALORIFIC VALUES

CALORIMETER COMPARISON MEASUREMENTS

TELEDYNE NATIONAL RDF

(25 GRAM CAPACITY BOMB CALORIMETER)

Expt. No. 2051 2052 2053 2054 2055 2056

E-cal/J*k“^ 86220.02 82218.55 86219.98 86218.54 86182.10 86181 .92

AT-corr/K 4.516466 4.506280 4.509029 4.497590 4.515228 4.495162

Crucible material 316SS 316SS 316SS 316SS Pt 316SS

Q-total/kJ 389.410 388.525 388.768 387.776 389.132 387.402

q-ign/kJ 0.002 0.002 0.002 0.002 0.001 0.001

q-Fe/kJ 0.036 0.037 0.032 0.033 0.027 0.030

q-HN0

3

/kJ 0.643 0.476 0.560 0.585 0.674 0.653

q-H^SO^/kJ 0.161 0.130 0.147 0.150 0.173 0.152

Q-RDF/kJ 388.568 387.880 388.027 387.006 388.257 386.565

m-RDF/g 20.00515 19.94353 19.98236 19.96562 19.78861 19.60786

HHV-AD/MJ-kg" 1 19.42 19.45 19.42 19.38 19.63 19.71

/(Btu-lb" 1

) (8351) (8362) (8348) (8333) (8439) (8476)

87
TABLE 31. DETERMINATION OF RESIDUAL MOISTURE, ASH, AND SULFUR CONTENT

CALORIMETER COMPARISON MEASUREMENTS

TELEDYNE NATIONAL RDF

(2.5 GRAM CAPACITY BOMB CALORIMETER)

(25 GRAM CAPACITY BOMB CALORIMETER)

Residual** Furnace Bcmb Sul fur

Moisture Ash* Ash* Content*

Expt. No. wt.% wt.% wt.% wt.%

1233 5.036 15.843 15.53 0.1462

1234 -- -- 14.61 0.1544

1235 5.052 15.793 15.40 0.1601

2051 5.107 15.996 15.19 0 1 444

2052 - - — 15.40 0.1170

2053 5.067 15.866 15.60 0.1324

2054 -- -- 15.69 0.1348

2055 -- -- 15.38 0.1573

2056 -- -- 15.67 0.1397

Mean 5.065 15.874 15.386 0.1429

Std. Dev. 0.030 0.086 0.332 0.0137

% Std. Dev. 0.592% 0.545% 2.156% 9.598%

*(Data are reduced to a dry basis.)

**(Sample equilibrated at 45% R.H. prior to DET'N.)

88
TABLE 32. CALORIFIC VALUES CALCULATED TO DIFFERENT BASES

CALORIMETER COMPARISON MEASUREMENTS

TELEDYNE NATIONAL RDF

(2.5 GRAM CAPACITY BOMB CALORIMETER)

HHV-AD HHV2 HHV3- F HHV3'-B

Expt. No. MJ* kg"

1 (Btu*lb~]

) MJ* kg"

1 (Btu* 1 b" 1

) MJ* kg'

1 (Btu-lb" 1

) MJ-kg" 1 (Btu* 1 b“

(2.5 GRAM CAPACITY BOMB CALORIMETER)

1233 19.31 (8303) 20.34 (8746) 24.21 (10409) 24.08 (10355)

1234 19.40 (8339) 20.43 (8784) 24.86 (10686) 23.93 (10287)

1235 19.34 (8313) 20.37 (8757) 24.57 (10564) 24.07 (10350)

Mean 19.35 (8318) 20.38 (8762) 24.55 (10553) 24.03 (10331)

Std. Dev. 0.04 (19) 0.05 (20) 0.32 (139) 0.09 (38)

% Std. Dev. 0.22% 0.22% 1.32% 0.37%

(25.0 GRAM CAPACITY BOMB CALORIMETER)

2051 19.42 (8351) 20.46 (8796) 24.32 (10456) 24.13 (10372)

2052 19.45 (8362) 20.49 (8808) 24.35 (10470) 24.22 (10411 )

2053 19.42 (8348) 20.45 (8794) 24.31 (10453) 24.24 (10419)

2054 19.38 (3333) 20.42 (8778) 24.27 (10434) 24.22 (10411

)

2055 19.63 (8439) 20.68 (8890) 24.58 (10567) 24.43 (10505)

2056 19.71 (8476) 20.77 (8928) 24.69 (10613) 24.63 (10587)

Mean 19.50 (8385) 20.54 (8832) 24.42 (10499) 24.31 (10451 )

Std. Dev. 0.14 (58) 0.14 (61) 0.17 (73) 0.19 (80)

% Std. Dev. 0.69% 0.69% 0.70% 0.76%

MJ*kg' ] = 429 .9226 Btu-lb' 1 was used to calculate the Btu-lb' 1 values presented

in parenthesis.
TABLE 33. DETERMINATION OF CALORIFIC VALUES

CALORIMETER COMPARISON MEASUREMENTS

ECO FUEL-II RDF

(2.5 GRAM CAPACITY BOMB CALORIMETER)

Expt. No. 1245 1246 1247

E-cal/J* K”

1 14561.78 14561.99 148562.00

AT-corr/K 2.781353 3.055371 3.055691

Q-total/kJ 40.501 44.492 44.497

q-ign/kJ 0.001 0.001 0.001

q-Fe/kJ 0.000 0.000 0.000

q-HN0

3

/kJ 0.102 0.109 0.108

q-H

2

S0

4

/kJ 0.060 0.067 0.069

Q-RDF/kJ 40.339 44.315 44.319

m-RDF/g 2.147869 2.359926 2.361323

HHV-AD/MJ-kg

-1

18.78 18.79 18.77

/(Btu-lb

-1

) (8074) (8073) (8069)

MJ-kg" 1 = 429.9226 Btu*lb“"' was used to calculate the Btu*lb~"* values presented

in parenthesis.

90
TABLE 34. DETERMINATION OF CALORIFIC VALUES

CALORIMETER COMPARISON MEASUREMENTS

ECO FUEL- I I RDF

(25 GRAM CAPACITY BOMB CALORIMETER)

Expt. No. 2057 2059 2060 2061 2062

E-cal/J-K' 1 86200.33 86206.47 86206.09 86205.58 86205.28

A T-corr/K 5.089892 5.098377 5.103465 5.122380 5.123829

Q-total/kJ 438.750 439.513 439.950 441.578 441 .654

q-ign/kJ 0.001 0.001 0.001 0.001 0.002

q-Fe/kJ 0.000 0.000 0.000 0.000 0.000

q-HN0

3

/kJ 0.980 0.972 0.935 0.966 0.938

q-H

2

S0

4

/kJ 0.554 0.567 0.613 0.683 0.564

Q-RDF/kJ 437.214 437.973 438.401 439.928 440.150

m-RDF/g 23.29107 23.32159 23.35230 23.43669 23.44928

HHV-AD/MJ-kg" 1 18.77 18.78 18.77 18.77 18.77

/(Btu-lb" 1 ) (8070) (8074) (8071

)

(8070) (8070)

MJ*kg~^ = 429.9226 Btu*lb~^ was used to calculate the Btu*lb~"' values presented

in parenthesis.

91
TABLE 3b. DETERMINATION OF RESIDUAL MOISTURE, ASH, AND SULFUR CONTENT

CALORIMETER COMPARISON MEASUREMENTS

ECO FUEL-II RDF

(2.5 GRAM CAPACITY BOMB CALORIMETER)

(25 GRAM CAPACITY BOMB CALORIMETER)

Residual Furnace Bomb Sulfur

Moisture** Ash* Ash* Content*

Expo. No. wt.% wt.% wt.% wt.%

1245 1 .629 13.149 11.70 0.4841

1246 -- -- 11.92 0.4907

1247 CD CM LD 13.199 11.85 0.5093

2057 1 -- 11.83 0.4127

2059 -- -- 11.78 0.4219

2060 -- -- 11.71 0.4551

2061 -- -- 11.87 0.5053

2062 — — 11.79 0.4174

Mean 1 .627 13.714 11.806 0.4621

Std. Dev. 0.002 0.035 0.077 0.0405

% Std. Dev 0 . 1 44% 0.266% 0.648% 8.772%

*(Data are reduced to a dry basis. )

**(Sample equilibrated to 30% R.H. prior to DET'N.

)

92
TABLE 36. CALORIFIC VALUES CALCULATED TO DIFFERENT BASES

CALORIMETER COMPARISON MEASUREMENTS

ECO FUEL- I I RDF

HHV-AD HHV2 HHV3--F HHV3-B

Expt. No. MJ-kg' 1 (Btu-lb" 1

) MJ-kg" 1 (Btu-lb"

1

) MJ-kg" 1 (Btu-lb" 1

) MJ-kg" 1

( Btu •

1

(2.5 GRAM CAPACITY BOMB CALORIMETER)

1245 18.78 (8074) 19.09 (8208) 21.99 (9453) 21 .62 (9295)

1246 18.79 (8073) 19.09 (8207) 21.99 (9452) 21.67 (9317)

1247 18.77 (8069) 19.08 (8203) 21 .97 (9447) 21 .64 (9305)

Mean 18.78 (8072) 19.09 (8206) 21 .98 (9451 ) 21 .64 (9306)

Std. Dev. 0.01 (3) 0.01 (3) 0.01 (3) 0.03 (ID

% Std. Dev . 0.03% 0.03% 0.03% 0.12%

(25 GRAM CAPACITY BOMB CALORIMETER)

2058 18.77 (8070) 19.08 (8204) 21 .98 (9449) 21.64 (9305)

2059 18.78 (8074) 19.09 (8207) 21 .99 (9453) 21.64 (9303)

2060 18.77 (8071) 19.08 (8205) 21.98 (9449) 21.61 (9293)

2061 18.77 (8070) 19.08 (8204) 21 .98 (9448) 21 .65 (9309)

2062 18.77 (8070) 19.08 (8203) 21 .98 (9448) 21.63 (9300)

Mean 18.77 (8071) 19.08 (8205) 21 .98 (9449) 21 .64 (9302)

Std. Dev. 0.004 (2) 0.004 (2) 0.005 (2) 0.01 (6)

% Std. Dev . 0.02% 0.02% 0.02% 0.06%

MJ-kg" 1 = 429.9226 Btu-lb" 1 was used to calculate the Btu- lb"

1 values presented

in parenthesis.

I

fi

1

93
TABLE 37. DETERMINATION OF CALORIFIC VALUES

CALORIMETER COMPARISON MEASUREMENTS

AMERICOLOGY RDF

(2.5 GRAM CAPACITY BOMB CALORIMETER)

Expt. No. 1250 1251 1252

E-cal/J-K" 1 14562.39 14562.39 14562.36

AT-corr/K 2.965378 2.972371 2.944801

Q-total/kJ 43.183 43.285 42.883

q-ign/kJ 0.001 0.001 0.001

q-Fe/kJ 0.000 0.000 0.000

q-HN0

3

/kJ 0.034 0.041 0.033

q-H

2 S04

/kJ 0.037 0.036 0.035

Q-RDF/kJ 43 .-111 43.206 42.814

m-RDF/g 2.761429 2.750133 2.730152

HHV-AD/MJ-kg" 1 15.61 15.71 15.68

/(Btu-lb" 1

) (6712) (6754) (6742)

MJ-kg

_1 = 429.9226 Btu*lb~^ was used to calculate the Btu*lb val ues

presented in parenthesis.
TABLE 38. DETERMINATION OF CALORIFIC VALUES

CALORIMETER COMPARISON MEASUREMENTS

AMERICOLOGY RDF

(25 GRAM CAPACITY BOMB CALORIMETER)

Expt. No. 2064 2065 2066 2067 2068 2069

E-cal/J-K' 1 86211 .66 86204.17 86205.00 86203.11 86204.06 86202.97

AT-corr/K 4.997517 4.963379 4.975904 4.974333 4.975251 4.936259

Q-total/kJ 430.844 427.864 428.948 428.803 428.887 425.520

q-ign/kJ 0.003 0.003 0.002 0.006 0.002 0.003

q-Fe/kJ 0.000 0.000 0.000 0.000 0.000 0.000

q-HN0

3

/kJ 0.672 0.666 0.670 0.697 0.715 0.725

q-H

2

S0

4

/kJ 0.306 0.303 0.295 0.371 0.318 0.320

Q-RDF/kJ 429.863 426.892 427.980 427.730 427.852 424.472

m-RDF/g ' 27.3768 27.1314 27.1988 27.1076 27.2651 27.2717

HHV-AD/MJ-kg" 1 15.70 15.73 15.74 15.79 15.69 15.56

/(Btu-lb" 1

) (6751) (6765) (6765) (6784) (6746) (6692)

MJ*kg“ ] = 429. 9226 Btu* 1 b" was used to calcu late the Btu* lb~^ values presented

in parenthesis.

95
TABLE 39. DETERMINATION OF RESIDUAL MOISTURE, ASH, AND SULFUR CONTENT

CALORIMETER COMPARISON MEASUREMENTS

AMERICOLOGY RDF

Residual Furnace Bomb Sul fur

Moisture Ash* Ash* Content*

Expt. No. wt.% wt.% wt.% wt.%

(2.5 GRAM CAPACITY BOMB CALORIMETER)

1250 5 .764 27.441 27.06 0.2398

1251 -- -- 26.43 0.2404

1252 5.794 27.709 26.66 0.2329

(25 GRAM CAPACITY BOMB CALORIMETER)

2064 . -- -- 26.43 0.2023

2065 -- -- 26.64 0.2023

2066 -- -- 26.55 0.1967

2067 -- -- 26.17 0.2478

2068 -- -- 26.74 0.2115

2069 -- 26.44 0.2126

Mean 5.779 27.575 26.57 0.2207

Std. Dev. 0.021 0.190 0.25 0.0195

% Std. Dev. 0.359% 0.689% 0.940% 8.832%

*(Data are reduced to a dry basis.)

96
TABLE 40. CALORIFIC VALUES CALCULATED TO DIFFERENT BASES

CALORIMETER COMPARISON MEASUREMENTS

AMERICOLOGY RDF

HHV-AD HHV2 HHV3-F HHV3-B

Expt. No. MJ-kg" 1 (Btu-lb"

1

) MJ-kg' 1 (Btu-lb' 1

) MJ-kg' 1 (Btu-lb" 1

) MJ-kg' 1 (Btu-lb

(2.5 GRAM CAPACITY BOMB CALORIMETER)

1250 15.61 (6712) 16.57 (7124) 22.88 (9836) 22.72 (9766)

1251 15.71 (6754) 16.67 (7169) 23.02 (9898) 22.66 (9744)

1252 15.68 (6742) 16.64 (7156) 22.98 (9880) 22.69 (9757)

Mean 15.67 (6736) 16.63 (7150) 22.96 (9871 ) 22.69 (9756)

Std

.

Dev. 0.05 (21.63) 0.05 (23) 0.07 (32) 0.03 (ID

% Std . Dev. 0.32% 0.32% 0.32% 0.11%

(25 GRAM CAPACITY BOMB CALORIMETER)

2064 15.70 (6751) 16.66 (7165) 23.01 (9882) 22.65 (9738)

2065 15.73 (6765) 16.70 (7179) 23.06 (9913) 22.76 (9786)

2066 15.74 (6765) 16.70 (7180) 23.06 (9913) 22.74 (9775)

2067 15.79 (6784) 16.75 (7200) 23.12 (9941

)

22.68 (9753)

2068 15.69 (6746) 16.65 (7160) 23.00 (9886) 22.73 (9773)

2069 15.56 (6692) 16.52 (7102) 22.81 (9806) 22.46 (9654)

Mean 15.70 (6750) 16.66 (7164) 23.01 (9892) 22.67 (9746)

Std. Dev. 0.07 (32) 0.08 (34) 0.11 (46) 0.11 (48)

% Std . Dev. 0.47% 0 . 47% 0.47% 0.50%

MJ-kg" 1 = 429.9226 Btu-lb" 1 was used to calculate the Btu-lb" 1 values presented

in parenthesis.
TABLE 41. DETERMINATION OF CALORIFIC VALUES

NEW CASTLE COUNTY, DELAWARE MSW, PROCESSED

THROUGH THE BUREAU OF MINES FACILITY, COLLEGE PARK, MD.

(25 GRAM CAPACITY BOMB CALORIMETER)

Cyclone No. 1

,

Processing Path Shred

,

2 inch pi

i

Expt. No. 1011 1014

E-cal/J-K" 1 86206.63 86204.13

AT-corr/K 5.038961 4.708003

Q-total/KJ 434.392 405.849

q-ign/kJ 0.003 0.002

q-Fe/kJ 0.000 0.000

q-HN0

3 /kJ 0.669 0.632

q-H

2 S0

4

/kJ 0.181 0.174

Q-RDF/kJ 433.539 405.041

m-RDF/g 23.7834 22.1607

HHV-AD/MJ • kg" 1 18.23 18.28

/(Btu-lb' 1

) (7837) (7858)

MJ-kg' 1 = 429.9226 Btu-lb" 1 was used

in parenthesis.

ondary

es Cyclone No. 1, Trommel

Undersize, +14 mesh

1015 1029 1030 1031

86101.90 85787.94 85787.02 85787.83

4.748646 3.406100 3.427473 3.512099

408.867 292.202 294.033 301.295

0.003 0.003 0.003 0.003

0.000 0.000 0.000 0.000

0.634 0.540 0.565 0.583

0.174 0.267 0.275 0.289

408.056 291.392 293.190 300.420

22.2285 22.1384 22.0979 22.0558

18.36 13.16 13.27 13.62

(7892) (5659) (5704) (5856)

* calculate the Btu-lb" 1 values presented

98
TABLE 42. DETERMINATION OF CALORIFIC VALUES

NEW CASTLE COUNTY, DELAWARE MSW, PROCESSED

THROUGH THE BUREAU OF MINES FACILITY, COLLEGE PARK, MD.

(25 GRAM CAPACITY BOMB CALORIMETER)

Cyclone No. 2, Secondary Cyclone No. 2, Trommel

Processing Path Shred, 2 inch pieces Undersize:, +14 mesh

Expt. No. 1018 1019 1020 1035 1037 1038

E-cal/JK" 1 85788.62 85787.73 85788.33 85793.38 85795.21 85793.81

AT-corr/K 5.046045 5.094753 5.096709 5.107338 5.111198 5.012434

Q-total/kJ 432.893 437.067 437.238 438.176 438.516 430.036

q-ign/kJ 0.002 0.003 0.003 0.002 0.002 0.002

q-Fe/kJ 0.000 0.000 0.000 0.000 0.000 0.000

q-HN0

3

/kJ 0.628 0.671 0.671 0.817 0.840 0.843

q-H^SO^/kJ 0.157 0.157 0.162 0.347 0.337 0.340

Q-RDF/kJ 432.106 436.236 436.402 437.008 437.337 428.851

m-RDF/g 22.8831 23.0440 23.0188 28.4674 28.5886 28.4646

HHV-AD/MJ-kg

-1

18.88 18.93 18.96 15.35 15.30 15.07

/(Btu-lb

-1

) (8118) (8137) (8151 ) (6600) (6577) (6477)

MJ-kg" 1 = 429.9226 Btu-lb

-1 was used to calculate the Btu-lb-1 values presented

in parenthesis.

99
TABLE 43. DETERMINATION OF CALORIFIC VALUES

NEW CASTLE COUNTY, DELAWARE MSW, PROCESSED

THROUGH THE BUREAU OF MINES FACILITY, COLLEGE PARK, MD.

(25 GRAM CAPACITY BOMB CALORIMETER)

Processing Path Secondary Shred, Cyclone No. 3, as collected

Expt. No. 1023 1024 1025

E-cal/J-K' 1 85787.89 85788.16 85789.37

AT-corr/K 5.130192 5.118568 5.047555

Q-total/kJ 440.108 439.113 433.026

q-ign/kJ 0.002 0.003 0.003

q-Fe/kJ 0.000 0.000 0.000

q-HN0

3

/kJ 0.710 0.731 0.686

q-H^SO^/kJ 0.152 0.146 0.152

Q-RDF/kJ 439.245 438.233 432.186

m-RDF/g 22.6636 22.6696 22.5781

HHV-AD/MJ-kg' 1 19.38 19.33 19.14

/(Btu-lb' 1

) (8332) (8311) (8229)

MJ-kg' 1 = 429.9226 Btu-lb' 1 was used to calculate the Btu- lb'

1

values presented in parenthesis.

100
!|

II

ia

a

TABLE 44. DETERMINATION OF CALORIFIC VALUES

NEW CASTLE COUNTY, DELAWARE MSW, PROCESSED

THROUGH THE BUREAU OF MINES FACILITY, COLLEGE PARK, MD.

(25 GRAM CAPACITY BOMB CALORIMETER)

Processing Path Heavy Organic Combustibles Organi

c

Wastes, Jig Over Flov

|Expt. No. 1041 1042 1043 1046 1047 1048

^E-cal/J-K" 1 85772.98 85771.23 85772.43 85770.95 85772.87 85771 .14

JiT-corr/K 1.427986 1 .451410 1.403397 1.320258 1 .426406 1 .222589

Q-total/kJ 122.483 124.489 120.373 113.240 122.347 104.863

[q-ign/kJ 0.001 0.002 0.003 0.002 0.002 0.003

q-Fe/kJ 0.000 0.000 0.000 0.000 0.000 0.000

*q-HN0

3

/kJ 0.227 0.281 0.270 0.144 0.154 0.130

• |q-H

2

S0

4

/kJ

• 0.070 0.065 0.057 0.047 0.050 0.044

Q-RDF/kJ 122.185 124.141 120.042 113.048 122.141 104.686

[m-RDF/g 5.8045 5.9240 5.7158 5.8160 6.1435 5.2689

1

HHV-AD/MJ-kg" 1 21.05 20.96 21 .00 19.44 19.88 19.87

•

/ (Btu- 1 b" 1

) (9050) (9009) (9029) (8357) (8548) (8542)

i

MJ-kg 1 = 429.9226 Btu«lb"'' was used to calculate the Btu*lb~^ values; presented

in parenthesis.

101
TABLE 45. DETERMINATION OF AIR DRY LOSS, RESIDUAL MOISTURE, ASH, AND SULFUR CONTENT

NEW CASTLE COUNTY, DELAWARE MSW, PROCESSED

THROUGH THE BUREAU OF MINES FACILITY, COLLEGE PARK, MD.

CYCLONE NO. 1, SECONDARY SHRED, 2 INCH PIECES

TOTAL WEIGHT OF SAMPLE, 3268.3 GRAMS

(25 GRAM CAPACITY BOMB CALORIMETER)

Air Dry Residual Furnace Bomb Sulfur

Loss Moisture Ash* Ash* Content*

Expt. No. wt.% wt.% wt.% wt.% wt.%

ion 8.761 5.324 12.503 11.824 0.137

1014 8.454 5.338 12.517 11.460 0.142

1015 8.481 . — 10.932 0.141

Mean 8.565 5.331 12.510 11.405 0.140

Std. Dev. 0.170 0.010 0.010 0.449 0.003

% Std. Dev. 1 .985% 0.183% 0.080% 3.932% 1 .890

*(Data are reduced to a dry basis.)

i

I

I

I

I

I

1

«

I

I

i

i

a

a

a

i

t

a

102
TABLE 46. DETERMINATION OF AIR DRY LOSS, RESIDUAL MOISTURE, ASH, AND SULFUR CONTENT

NEW CASTLE COUNTY, DELAWARE MSW, PROCESSED

THROUGH THE BUREAU OF MINES FACILITY, COLLEGE PARK, MD.

CYCLONE NO. 1, TROMMEL UNDERSIZE, +14 MESH

TOTAL WEIGHT OF SAMPLE, 2237.5 GRAMS

(25 GRAM CAPACITY BOMB CALORIMETER)

Ai r Dry Residual Furnace Bomb Sulfur

Loss Moisture Ash* Ash* Content*

Expt. No. wt.% wt.% wt.% wt.% wt.%

1029 8.535 5.966 34.458 32.512 0.219

1030 8.732 5.830 33.766 32.134 0.225

1031 — -- -- 30.079 0.238

Mean 8.634 5.898 34.112 31 .575 0.227

Std. Dev. 0.139 0.096 0.489 1.309 0.010

% Std. Dev. 1 .615% 1 .633% 1 .435% 4.147% 4.272%

*(Data are reduced to a dry basis.)

103
TABLE 47 . DETERMINATION OF AIR DRY LOSS, RESIDUAL MOISTURE, ASH, AND SULFUR CONTENT

NEW CASTLE COUNTY, DELAWARE MSW, PROCESSED

THROUGH THE BUREAU OF MINES FACILITY, COLLEGE PARK, MD.

CYCLONE NO. 2, SECONDARY SHRED, 2 INCH PIECES

TOTAL WEIGHT OF SAMPLE, 2672.5 GRAMS

(25 GRAM CAPACITY BOMB CALORIMETER)

Expt. No.

Ai r Dry

Loss

wt.%

Residual

Moisture

wt.%

Furnace

Ash*

wt.%

Bomb

Ash*

wt.%

Sulfur

Content*

wt.%

1018 8.316 5.429 8.238 7.133 0.124

1019 8.720 5.323 8.387 7.312 0.123

1020 8.471 -- -- 7.637 0.127

Mean 8.502 5.376 8.313 7.361 0.125

Std. Dev. 0.204 0.075 0.106 0.256 0.002

% Std. Dev. 2.40% 1 . 398% 1.269% 3.471% 1.670%

*(Data are reduced to a dry basis.)

104
I

!

i

TABLE 48. DETERMINATION OF AIR DRY LOSS, RESIDUAL MOISTURE, ASH, AND SULFUR CONTENT

NEW CASTLE COUNTY, DELAWARE MSW, PROCESSED

THROUGH THE BUREAU OF MINES FACILITY, COLLEGE PARK, MD.

CYCLONE NO. 2, TROMMEL UNDERSIZE, +14 MESH

TOTAL WEIGHT OF SAMPLE, 2361.2 GRAMS

(25 GRAM CAPACITY BOMB CALORIMETER)

Expt. No.

Air Dry

Loss

wt.%

Residual

Moisture

wt.%

Furnace

Ash*

wt.%

Bomb

Ash*

wt.%

Sul fur

Content*

wt.%

1035 18.207 6.797 22.176 22.359 0.223

1037 -- 6.704 23.867 22.215 0.216

1038 — i -- 24.214 0.219

Mean 18.207 6.750 23.022 '22.929 0.219

Std. Dev. -- 0.066 1.196 1.115 0.004

% Std. Dev. -- 0.977

%

5.193% 4.862% 1.601%

*(Data are reduced to a dry basis.

)

105
TABLE 49. DETERMINATION OF AIR DRY LOSS, RESIDUAL MOISTURE, ASH, AND SULFUR CONTENT

NEW CASTLE COUNTY, DELAWARE MSW, PROCESSED

THROUGH THE BUREAU OF MINES FACILITY, COLLEGE PARK, MD.

SECONDARY SHRED, CYLCONE NO. 3, AS-COLLECTED

TOTAL WEIGHT OF SAMPLE, 3540.4 GRAMS

(25 GRAM CAPACITY BOMB CALORIMETER)

Air Dry Residual Furnace Bomb Sul fur

Loss Moi sture Ash* Ash* Content*

Expt. No. wt.% wt.% wt.% wt.% wt.%

1023 15.766 5.212 9.182 9.516 0.121

1024 15.298 5.308 8.887 10.944 0.116

1025 _ _ — — _ _ 7.751 0.121

Mean 15.532 5.260 9.034 ‘9.404 0.119

Std. Dev. 0.331 0.068 0.208 1.599 0.003

% Std. Dev. 2.131% 1 .288% 2.308% 17.009% 2.419

*(Data are reduced to a dry basis.)

106 I
TABLE 50. DETERMINATION OF AIR DRY LOSS, RESIDUAL MOISTURE, ASH, AND SULFUR CONTENT

NEW CASTLE COUNTY, DELAWARE MSW, PROCESSED

THROUGH THE BUREAU OF MINES FACILITY, COLLEGE PARK, MD.

HEAVY ORGANIC COMBUSTIBLES

TOTAL WEIGHT OF SAMPLE, 3664.8 GRAMS

(25 GRAM CAPACITY BOMB CALORIMETER)

Ai r Dry Residual Furnace Bomb Sul fur

Loss Moisture Ash* Ash* Content

Expt. No. wt.% wt.% wt.% wt.% wt.%

1041 0.718 4.207 11.671 — 0.215

1042 — 4.117 10.192 -- 0.196

1043 _ — _ — 0.178

Mean 0.718 4.162 10.931 0.196

Std. Dev. -- 0.064 1.046 0.019

% Std. Dev. « _ cHi

C\j LO 9.570% 9.424'

*(Data are reduced to a dry basis.)

107
TABLE 51. DETERMINATION OF AIR DRY LOSS, RESIDUAL MOISTURE, ASH, AND SULFUR CONTENT

NEW CASTLE COUNTY, DELAWARE MSW, PROCESSED

THROUGH THE BUREAU OF MINES FACILITY, COLLEGE PARK, MD.

ORGANIC WASTES, JIG OVERFLOW

TOTAL WEIGHT OF SAMPLE, 3202.1 GRAMS

(25 GRAM CAPACITY BOMB CALORIMETER)

Air Dry Residual Furnace Bomb Sul fur

Loss Moisture Ash* Ash* Content*

Expt. No. wt.% wt.% wt.% wt.% wt.%

1046 0.784 4.560 11.415 __ 0.145

1047 -- 4.735 10.774 — 0.145

1048 -- -- -- -- 0.151

Mean 0.784 4.648 ’ll. 094 -- 0.147

Std. Dev. -- 0.123 0.453 -- 0.003

% Std. Dev. -- 2.656% 4.081% -- 2.357%

*(Data are reduced to a dry basi s .

)

108
TABLE 52. CALORIFIC VALUES CALCULATED TO DIFFERENT BASES

NEW CASTLE COUNTY, DELAWARE MSW, PROCESSED

THROUGH THE BUREAU OF MINES FACILITY, COLLEGE PARK, MD.

CYCLONE NO. 1, SECONDARY SHRED, 2 INCH PIECES

(25 GRAM CAPACITY BOMB CALORIMETER)

HHV1 HHV2

Expt. No. MJ*kg"^ (Btu*lb"^) MJ*kg"^ (Btu*lb~^) MJ*kg'^ (Btu*lb“^) MJ*kg

HHV3-F

-1

HHV3-B

-1

(Btu-lb

_1

)

1011

1014

1015

16.67 (7165)

16.71 (7185)

16.79 (7217)

19.25 (8278)

19.31 (8300)

19.39 (8337)

22.01 (9463)

22.07 (9488)

22.17 (9529)

21.84 (9388)

21.81 (9375)

21.77 (9360)

I

Mean 16.72 (7189) 19.32 (8305) 22.08 (9493) 21.80 (9374)

Std. Dev. 0.06 (26) * 0.07 (30) 0.08 (33) 0.03 (14)

% Std. Dev. 0.36% 0.36% 0.35% 0.15%

MJ*kg"^ = 429.9226 Btu-lb""* was used to calculate the Btu-lb""* values presented

in parenthesis.

109
TABLE 53. CALORIFIC VALUES CALCULATED TO DIFFERENT BASES

NEW CASTLE COUNTY, DELAWARE MSW, PROCESSED

THROUGH THE BUREAU OF MINES FACILITY, COLLEGE PARK, MD.

CYCLONE NO. 2, SECONDARY SHRED, 2 INCH PIECES

(25 GRAM CAPACITY BOMB CALORIMETER)

HHV1 HHV2 HHV3-F HHV3-B

Expt. No. MJ-kg” 1 (Btu-lb” 1

) MJ-kg" 1 (Btu-lb

-1

) MJ-kg” 1 (Btu-lb" ! ) MJ-kg” 1 (Btu-ltj

1018 17.28 (7428) 19.96 (8580) 21.77 (9358) 21.49 (9239

j

1019 17.32 (7447) 20.01 (8601) 21.82 (9382) 21.59 (92801

1020 17.35 (7458) 20.04 (8614) 21.85 (9396)

1

21.69 (9326)’

1

Mean 17.32 (7444) 20.00 (8598) 21.81 (9379)

!

21.59 (9282

)j Std. Dev. 0.04 (15) 0.04 (17) 0.04 (19) 0.10 (44)

% Std. Dev . 0 . 20% 0.20% 0.20% 0.47%

|

1 MJ-kg” 1 = 429.9226 Btu-lb” 1 was used to calculate the Btu-lb” 1 values presented

*

in parenthesis
TABLE 54. CALORIFIC VALUES CALCULATED TO DIFFERENT BASES

NEW CASTLE COUNTY, DELAWARE MSW, PROCESSED THROUGH

THE BUREAU OF MINES FACILITY, COLLEGE PARK, MD.

SECONDARY SHRED, CYLCONE NO. 3, AS-COLLECTED

(25 GRAM CAPACITY BOMB CALORIMETER)

HHVl HHV2 HHV3-F HHV3-B

Expt . No. MJ*kg

-1

(Btu-lb"

1

) MJ-kg" 1 (Btu-lb' 1) MJ-kg' 1 (Btu-lb

-1

) MJ-kg" 1 (Btu-lb~

] )

1023 16.37 (7038) 20.46 (8795) 22.49 (9669) 22.61 (9720)

1024 16.33 (7020) 20.40 (8772) 22.43 (9644) 22.91 (9850)

1025 16.17 (6951) 20.20 (8686) 22.21 (9549) 21.90 (9416)

Mean 16.29 (7003) 20.35 (8751 ) 22.38 (9621) 22.47 (9662)

Std. Dev. 0.11 (46) 0.13 (57) 0.15 (63) 0.52 (223)

% Std. Dev. 0.66% 0.66% 0.66% 2.31%

MJ*kg

-

^ = 429.9226 Btu*lb~^ was used to calculate the Btu*lb“^ values presented

in parenthesis.

Ill
TABLE 55. CALORIFIC VALUES CALCULATED TO DIFFERENT BASES

NEW CASTLE COUNTY, DELAWARE MSW, PROCESSED THROUGH

THE BUREAU OF MINES FACILITY, COLLEGE PARK, MD.

CYCLONE NO. 1, TROMMEL UNDERSIZE, +14 MESH

(25 GRAM CAPACITY BOMB CALORIMETER)

HHV

1

HHV2 HHV3-F HHV3-B

Expt. No. MJ*kg’^ (Btu*lb

- ^) MJ*kg~^ (Btu*lb~^) MJ*kg"^ ( Btu • 1 b”"* ) MJ*kg~"* (Btu*lb

1029

1030

1031

Mean

Std. Dev.

% Std. Dev.

-1

12.03 (5171)

12.12 (5212)

12.44 (5350)

12.20 (5244)

0.22 (94)

1.79%

-1

13.99 (6014)

14.10 (6062)

14.47 (6223)

14.19 (6100)

0.25 (109)

1 . 79%

21.23 (9127)

21.40 (9200)

21.97 (9445)

21.53 (9257)

0.-39 (167)

1.80%

-1

20.73 (891 1 ),

20.78 (8932)

20.70

(8900)J|

1

20.73 (8914)

0.04 (16)

0.18%

MJ*kg = 429.9226 Btu*lb was used to calculate the Btu*lb values presented

ft

| ft

in parenthesis.
TABLE 56. CALORIFIC VALUES CALCULATED TO DIFFERENT BASES

NEW CASTLE COUNTY, DELAWARE MSW, PROCESSED

THROUGH THE BUREAU OF MINES FACILITY, COLLEGE PARK, MD.

CYCLONE NO. 2, TROMMEL UNDERSIZE, +14 MESH

(25 GRAM CAPACITY BOMB CALORIMETER)

HHV1 HHV2 HHV3-F HHV3-B

Expt. No. MJ-kg" 1 (Btu-lb" ]

) MJ-kg" 1 (Btu-lb" 1) MJ-kg" 1 (Btu-lb"

1

) MJ-kg” 1 (Btu-lb

1035 12.56 (5399) 16.46 (7078) 21.39 (9195) 21.20 (9116)

1037 12.51 (5379) 16.40 (7053) 21.31 (9162) 21.09 (9067)

1038 12.32 (5298) 16.16 (6946) 20.99 (9024) 21.32 (9165)

Mean 12.46 (5359) 16.34 (7026) 21.23 (9127) 21.20 (9116)

Std. Dev. 0.12 (53) 0.16 (70) 0.21 (91) 0.11 (49)

% Std. Dev 1.00% 1 .00% 0.99% 0.54%

MJ-kg" 1 = 429.9226 Btu-lb' 1 was used to calculate the Btu-lb" 1 values presented

in parenthesis.

113
TABLE 57. CALORIFIC VALUES CALCULATED TO DIFFERENT BASES

NEW CASTLE COUNTY, DELAWARE MSW, PROCESSED

THROUGH THE BUREAU OF MINES FACILITY, COLLEGE PARK, MD.

HEAVY ORGANIC COMBUSTIBLES

(25 GRAM CAPACITY BOMB CALORIMETER)

HHV 1 HHV2 HHV3-F HHV3-B

Expt. No. MJ-kg" 1 (Btu-lb" 1

) MJ-kg" 1 (Btu-lb" 1

) MJ-kg" 1 (Btu-lb" 1

) MJ-kg' 1 (Btu

1041 20.90 (8986) 21.97 (9444) 24.66 (10603) —

1042 20.81 (8945) 21.87 (9401) 24.55 (10556) —

1043 20.85 (8965) 21.92 (9422) 24.61 (10579) —

Mean 20.85 (8965) 21.92 (9422) 24.61 (10579) --

Std. Dev. • 0.05 (20) 0.05 (22) 0.05 (24) --

% Std. Dev 0.23% 0.23% 0.22 %

--

MJ-kg" 1 = 429.9226 Btu-lb" 1 was used to calculate the Btu-lb" 1 values presented

in parenthesis.
TABLE 58. CALORIFIC VALUES CALCULATED TO DIFFERENT BASES

NEW CASTLE COUNTY, DELAWARE MSW, PROCESSED

THROUGH THE BUREAU OF MINES FACILITY, COLLEGE PARK, MD.

ORGANIC WASTES, JIG OVERFLOW

(25 GRAM CAPACITY BOMB CALORIMETER)

HHV1 HHV2 HHV3-F HHV3-B

Expt. No. MJ-kg" 1 (Btu-lb" ]

) MJ-kg" 1 (Btu-lb' 1

) MJ-kg" 1 (Btu-lb'

1

) MJ-kg" 1 (Btu

1046 19.29 (8291) 20.39 (8764) 22.93 (9858) —

1047 19.73 (8480) 20.85 (8964) 23.45 (10083) —

1048 19.71 (8476) 20.84 (8959) 23.44 (10077) —

Mean 19.57 (8416) 20.69 (3896) 23.27 (10006) --

Std . Dev. 0.25 (108) 0.27 (114) 0.30 (128) —

% Std. Dev. 1.28% 1.28% 1 . 28% --

MJ-kg" 1 = 429.9226 Btu-lb' 1 was used to calculate the Btu-lb" 1 values presented

in parenthesis.

115
TABLE 59. DETERMINATION OF CALORIFIC VALUES

TELEDYNE NATIONAL RDF, SINGLE STAGE MOISTURE

(2.5 GRAM CAPACITY BOMB CALORIMETER)

Expt. No. 1272 1273 1274 1275

E-cal/J-K" 1 14561.90 14561.91 14561.99 14562.01

A T-corr/K. 3.026075 3.029582 3.147106 3.172096

Q-total/kJ 44.065 44.116 45.828 46.192

q-ign/kJ 0.001 0.001 0.001 0.002

q-Fe/kJ 0.000 0.000 0.000 0.000

q-HN0

3

/kJ 0.074 0.078 0.083 0.073

q-H

2

S0

4

/kJ 0.025 0.026 0.026 0.025

Q-RDF/kJ 43.965 44.011 45.718 46.092

m-RDF/g 2.28167 2.28249 2.36948 2.38905

HHV-AD/MJ.kg" 1 -- --

/(Btu-lb" 1

)

HHV2/MJ-kg

_1

19.27 19.28 19.29 19.29

/(Btu-lb" 1

) (8284) (8290) (8295) (8295)

MJ-kg" 1 = 429.9226 Btu-lb" 1 was used to calculate the Btu-lb"

1 values presented

in parenthesis.

116
TABLE 60. DETERMINATION OF RESIDUAL MOISTURE, ASH, AND SULFUR CONTENT

TELEDYNE NATIONAL RDF, SINGLE STAGE MOISTURE

(2.5 GRAM CAPACITY BOMB CALORIMETER)

Residual Furnace Bomb Sul fur

Moisture Ash* Ash* Content*

Expt. No. wt.% wt.% wt.% wt.%

1272 -- 7.100 6.137 0.1900

1273 7.080 6.085 0.1933

1274 -- 7.054 6.109 0.1891

1275 7.059 5.845 0.1801

Mean 7.073 6.044 0.1881

Std. Dev. -- 0.021 0.134 0.0056

% Std. Dev. _ _ 0.298% 2.223% 3.001%

*(Data are reduced to a dry basis.)

117
TABLE 61. CALORIFIC VALUES CALCULATED TO DIFFERENT BASES

TELEDYNE NATIONAL RDF, SINGLE STAGE MOISTURE

(2.5 GRAM CAPACITY BOMB CALORIMETER)

HHV-AD HHV2 HHV3-F HHV3-B

Expt. No. MJ-kg" 1 (Btu-lb" 1

) MJ-kg' 1 (Btu-lb' 1

) MJ-kg" 1 (Btu-lb" 1

) MJ-kg' 1 (Btu-lb

1272 -- 19.27 (8284) 20.74 (8917) 20.53 (8826)

1273 -- 19.28 (8290) 20.75 (8921) 20.53 (8827)

1274 -- 19.29 (8295) 20.76 (8925) 20.55 (8835)

1275 — 19.29 (8295) 20.76 (8925) 20.49 (8809)

Mean -- 19.28 (8291) 20.75 (8922) 20.53 (8824)

Std. Dev. -- 0.01 (5) 0.01 (4) 0.03 (11)

% Std. Dev. 0.05% 0.05% 0.12%

MJ-kg" 1 = 429.9226 Btu-lb" 1 was used to calculate the Btu-lb" 1 values presented

in parenthesis.

118
TABLE 62. DETERMINATION OF CALORIFIC VALUES

TELEDYNE NATIONAL RDF, TWO STAGE MOISTURE

(2.5 GRAM CAPACITY BOMB CALORIMETER)

Expt. No. 1268 1269 1270 1271

E-cal/J-K" 1 14562.13 14562.12 14562.00 14562.03

AT-corr/K 3.145622 3.119644 2.988314 3.015041

Q-total/kJ 45.807 45.429 43.516 43.905

q-ign/kJ 0.001 0.001 0.001 0.001

q-Fe/kJ 0.000 0.000 0.000 0.000

q-HN0

3

/kJ 0.082 0.081 0.081 0.083

q-H

2

S0

4

/kJ 0.030 0.032 0.030 0.030

Q-RDF/kJ 45.694 45.314 43.404 43.791

m-RDF/g 2.506865 2.483743 2.374997 2.398991

HHV-AD/MJ-kg" 1 18.23 18.24 18.28 18.25

/ ( Btu * 1 b" 1 ) (7836) (7844) (7857) (7848)

MJ-kg

_1

= 429.9226 Btu*lb“1 was used to calculate the Btu*lb~'' values presented

in parenthesis.

119
TABLE 63. DETERMINATION OF RESIDUAL MOISTURE, ASH, AND SULFUR CONTENT

TELEDYNE NATIONAL RDF, TWO STAGE MOISTURE

(2.5 GRAM CAPACITY BOMB CALORIMETER)

Residual Furnace Bomb Sulfur

Moisture Ash* Ash* Content*

Expt. No. wt.% wt.% wt.% wt.%

1268 6.251 7.288 6.393 0.2170

1269 6.212 7.260 6.599 0.2345

1270 6.102 7.284 6.435 0.2330

1271 6.116 7.371 6.332 0.2282

Mean 6.170 7.301 6.440 0.2282

Std. Dev. 0.073 0.048 0.114 0.0079

% Std. Dev. 1 . 1 79% 0.664% 1.775% 3.471

'

*(Data are reduced to a dry basis.)

120
TABLE 64. CALORIFIC VALUES CALCULATED TO DIFFERENT BASES

TELEDYNE NATIONAL RDF, TWO STAGE MOISTURE

(2.5 GRAM CAPACITY BOMB CALORIMETER)

HHV-AD HHV2 HHV3-F HHV3- B

Expt. No. MJ •kg"

1 (Btu-lb" 1

) MJ-kg' 1 (Btu-lb' 1

) MJ-kg' 1 (Btu-lb' 1;) MJ-kg' 1 (Btu-lb

1268 18.23 (7836) 19.44 (8359) 20.97 (9016) 20.77 (8930)

1269 18.24 (7844) 19.45 (8363) 20.98 (9018) 20.83 (8954)

1270 18.28 (7857) 19.46 (8368) 20.99 (9025) 20.80 (8943)

1271 18.25 (7848) 19.44 (8359) 20.99 (9024) 20.76 (8924)

Mean 18.25 (7846) 19.45 (8362) 20.98 (9021) 20.79 (8938)

Std. Dev. 0.02 (9) 0.01 (4) 0.01 (4) 0.03 (13)

% Std. Dev. 0.11% 0.05%

•>

0.05% 0.15%

MJ-kg' 1 = 429. 9226 Btu-lb' 1 was used to calculate the Btu-lb' 1 values presented

in parenthesis.

121
TABLE 65. DETERMINATION OF CALORIFIC VALUES

STEAM SIZE REDUCTION RDF

(2.5 GRAM CAPACITY BOMB CALORIMETER

Expt. No. 1258 1263 1264

E-cal/J-K' 1 14562.00 14562.27 14562.26

AT-corr/K 2.791100 2.970305 2.991348

Q-total/kJ 40.644 43.254 43.561

q-ign/kJ 0.001 0.001 0.001

q-Fe/kJ 0.000 0.000 0.000

q-HN0

3

/kJ 0.064 0.065 0.070

q-H

2

S0

4

/kJ 0.023 0.028 0.026

Q-RDF/kJ 40.556 43.161 43.464

m-RDF/g 2.457883 2.635031 2.634345

HHV-AD/MJ-kg

-1

16.50 16.38 16.50

/(Btu-lb

-1

) (7094) (7042) (7093)

MJ-kg" 1 = 429.9226 Btu*lb“^ was used to calculate the Btu*lb"^ values presented

in parenthesis.

122
TABLE 66. DETERMINATION OF RESIDUAL MOISTURE, ASH, AND SULFUR CONTENT

STEAM SIZE REDUCTION RDF

(2.5 GRAM CAPACITY BOMB CALORIMETER)

Residual Furnace Bomb Sulfur

Moisture Ash* Ash* Content*

Expt. No. wt.% wt.% wt.% wt.%

1258 4.159 16.64 16.34 0.1673

1263 4.136 16.46 17.39 0.1890

1264 — -- 16.74 0.1752

Mean 4.148 16.55 16.82 0.1772

Std. Dev. 0.016 0.125 0.53 0.011

% Std. Dev. 0.39% 0.758% 3.15% 6.20%

*(Data are reduced to a dry basis.)

123
TABLE 67. CALORIFIC VALUES CALCULATED TO DIFFERENT BASES

STEAM SIZE REDUCTION RDF

(2.5 GRAM CAPACITY BOMB CALORIMETER)

HHV-AD HHV2 HHV3-F HHV3-B

Expt. No. MJ-kg" 1 (Btu-lb" ') MJ-kg' 1 (Btu-lb' 1

) MJ-kg" 1 (Btu-lb" 1 ) MJ-kg' 1 (Btu-lb

1258 16.50 (7094) 17.21 (7401 ) 20.63 (8868) 20.58 (8846)

1263 16.38 (7042) 17.09 (7347) 20.48 (8803) 20.68 (8892)

1264 16.50 (7093) 17.21 (7400) 20.63 (8867) 20.67 (8888)

Mean 16.46 (7076) 17.17 (7383) 20.58 (8846) 20.64 (8875)

Std. Dev. 0.07 (30) 0.07 (31) 0.09 (37) 0.06 (25)

% Std. Dev . 0.42% 0 . 42% 0.42% 0.29%

MJ-kg" 1 = 429.9226 Btu-lb' 1 was used to calculate the Btu •lb"

1 values presented

in parentehsis.
TABLE 68. DETERMINATION OF CALORIFIC VALUES

NCRR STORAGE PIT RDF, CHARRED STORAGE SAMPLE

(25 GRAM CAPACITY BOMB CALORIMETER)

Expt. No. 1003 1004 1006

E-cal/J* K”

1 86208.25 86197.94 86210.35

AT-corr/K 4.657703 2.858432 4.788010

Q-total/kJ 401.532 243.391 412.776

q-ign/kJ 0.002 0.001. 0.002

q-Fe/kJ 0.000 0.000 0.000

q-HN0

3

/kJ 0.433 0.228 0.777

q-H

2

S0

4

/kJ 0.334 0.262 0.317

Q-RDF/kJ 400.764 245.900 411 .680

m-RDF/g 25.0601 15.1636 25.7628

HHV-AD/MJ-kg" 1 15.99 16.22 15.98

/(Btu-lb

-1

) (6875) (6972) (6870)

MJ-kg" 1 = 429.9226 Btu*lb“^ was used to calculate the Btu*lb'^ values presented

in parenthesis.

125
TABLE 69. DETERMINATION OF RESIDUAL MOISTURE, ASH, AND SULFUR CONTENT

NCRR STORAGE PIT RDF, CHARRED STORAGE SAMPLE

(25 GRAM CAPACITY BOMB CALORIMETER)

Residual Furnace Bomb Sulfur

Moisture Ash* Ash* Content*

Expt. No. wt.% wt.% wt.% wt.%

1003 2.618 30.915 24.93 0.232

(pellet)

1004 1.900 31.1383 22.94 0.301

(loose)

1006 — — 29.68 0.216

Mean 2.259 31.027 25.85 0.250

Std. Dev. 0.508 0.158 3.46 0.045

% Std. Dev 22.48% 0.509% 13.40% 18.09%

*(Data are reduced to a dry basis.

)

126
TABLE 70. CALORIFIC VALUES CALCULATED TO DIFFERENT BASES

NCRR STORAGE PIT RDF, CHARRED STORAGE SAMPLE

(25 GRAM CAPACITY BOMB CALORIMETER)

HHV-AD

-1

HHV2

-1 -1

HHV3-F

-1 -1

Expt. No. MJ-kg" (Btu-lb ) MJ-kg (Btu-lb ) MJ-kg" (Btu-lb” ) MJ-kg

HHV3-B

-1

(Btu-lb"

1 )

1003 15.99 (6875) 16.30 (7009) 23.67 (10178) 21.72 (9336)

1004 16.22 (6972) 16.53 (7107) 24.01 (10321 ) 21.45 (9222)

1006 15.98 (6870) 16.41 (7055) 23.75 (10213) 23.33 (10032

Mean 16.06 (6906) 16.41 (7057) 23.81 (10237) 22.17 (9530)

Std. Dev. 0.13 (58) 0.11 (49) 0.17 (75) 1.02 (438)

% Std. Dev. 0 . 83% 0.69% 0.73% 4.60%

MJ-kg' 1 = 429.9226 Btu-lb" 1 was used to calculate the Btu-lb" 1 values presented

in parenthesis.

127
TABLE 71. DETERMINATION OF CALORIFIC VALUES

NCRR (LOW ASH) RDF SAMPLE

(2.5 GRAM CAPACITY BOMB CALORIMETER)

Expt. No. 1265 1266 1267

E-cal/J-K" 1 14562.01 14561.99 14562.04

AT-corr/K 2.574470 2.545666 2.598256

Q-total/kJ 37.489 37.070 37.836

q-ign/kJ 0.001 0.001 0.001

q-Fe/kJ 0.000 0.000 0.000

q-HN0

3

/kJ 0.057 0.054 0.054

q-HgSO^/kJ 0.012 0.013 0.013

Q-RDF/kJ 37.420 37.002 37.768

m-RDF/g 2.382203 2.359875 2.41 7902

HHV-AD/MJ-kg" 1 15.71 15.68 15.62

/ (Btu* 1 b“^

)

(6753) (6741 ) (6715)

MJ-kg' 1 = 429.9226 BtU'lb

-

”

1 was used to calculate the Btu*lb“^ values

presented in parenthesis.

128
TABLE 72. DETERMINATION OF RESIDUAL MOISTURE, ASH, AND SULFUR CONTENT

NCRR (LOW ASH) RDF SAMPLE

(2.5 GRAM CAPACITY BOMB CALORIMETER)

Residual Furnace Bomb Sulfur

Moisture Ash* Ash* Content*

Expt. No. wt.% wt.% wt.% wt.%

1265 5.295 11.781 11.256 0.0881

1266 5.235 11.824 11.454 0.0995

1267 — -- 11.148 0.0961

Mean 5.265 11.803 11.286 0.0946

Std. Dev. 0.042 0.030 0.155 0.0059

% Std. Dev. 0.806% 0.258% 1.375% 6.189%

*(Data are reduced to a dry basis.)
TABLE 73. CALORIFIC VALUES CALCULATED TO DIFFERENT BASES

NCRR (LOW ASH) RDF SAMPLE

(2.5 GRAM CAPACITY BOMB CALORIMETER)

HHV-AD HHV2 HHV3-F HHV3-B

Expt. No. MJ-kg’ 1 (Btu-lb" ') MJ-kg’ 1 (Btu-lb" 1

) MJ-kg’ 1 (Btu-lb" 1) MJ-kg" 1 (Btu-lb

1265 15.71 (6753) 16.58 (7129) 18.30 (8082) 18.68 (8033)

1266 15.68 (6741) 16.55 (7116) 18.77 (8068) 18.69 (8036)

1267 15.62 (6715) 16.49 (7089) 18.69 (8037) 18.56 (7978)

Mean 15.67 (6736) 16.54 (7111) 18.75 (8062) 18.64 (8016)

Std. Dev. 0.05 (19) 0.05 (20) ' 0.05 (23) 0.08 (33)

% Std. Dev 0.29%

_ l

0.029% 0.29% 0.41%

MJ-kg’ 1 = 429.9226 Btu-lb’ 1 was used to calculate the Btu-lb’ 1 values presented

in parenthesis.

130
TABLE 74. SUMMARY OF MEAN CALORIFIC VALUES

OBTAINED FOR MEASUREMENTS

ON RDF IN BTU-LB"

1

RDF HHV-AD HHV2 HHV3-F HHV3-B

ASTM - RR1 7052 7426 9796 9716

6947 7256 9570 9582

ASTM - RR2 7419 7900 9253 9126

7156 7627 9535 9396

ASTM - RR3 6831 7148 9170 8998

6962 7313 9438 9255

Teledyne Nat. 8352 8797 10526 10391

ECO FUEL II 8072 8205 9450 9304

Americology 6743 7157 9882 9751

Bur. Mines -1 7189 8305 9493 9394

Bur. Mines -2 7444 8598 9379 9282

Bur. Mines -3 7003 8751 9621 9662

Bur. Mines -4 5244 6100 9257 8914

Bur. Mines -5 5359 7026 9127 9116

Bur. Mines -6 8965 9422 10579 — Bur. Mines -7 8416 • 8896 10006 — NCRR - Low Ash 6736 '7111 8062 8016

NCRR - Char 6906 7057 10237 9530

Steam Size Red. 7076 7383 8846 8875

Teled. Nat.Sgl. — 8291 8922 8824

Teled. Nat. Dbl

.

7846 8362 9021 8938

Americology Grab 6498 6607 9392 9236

Americology Rep. 6609 6971 9525 9693

Mean 7124 7726 9482 9285

Std. Dev. 876(12.3%) 841(10.9%) 553(5.3%) 474(5.1%)

(% Std. Dev.)
Figure 1 U.S. Bureau of Mines, College Park, Md.,

Resource Recovery Facility

Overall Flow-Diagram for Processing MSW

Unburned Refuse i

KEY:

£> Air to Baghouse ^ Water to Recycle ^

System

Primary Shredder I

Light Air Classifier 3

Very Light Paper and Plastic

f

Magnetic Metal

to Detinning

CO) B(O)

Nonmagnetics

Massive Metals i

Y

(O) sMe±!S fc)7

Glass. Nonferrous Metals, and Heavy Organics

with Paper and Plastics

Heavy

Iron

Heavy

Nonferrous

Metal i

L- Alternate

3/4” 3/4” Aluminum and Trommel SooS __ Heavy Organics

with Paper and Secondary

Shredder Trommel °°°° 9000

O O O o

1 Plastics * *

Fine Glass and Dirt

Glass, Nonferrous Metals, Heavy Food, and Other Organics

Aluminum

iE®@ ©©

Secondary Air Classifier

Aluminum and Heavy Organics

I +

X Electrostatic x

j Separator y

Paper and Plastic

Heavy

Organics

©

I ©

Compactor

T

Paper and Plastics

(Circled numbers indicate sample collection points)

132
Figure 2 U.S. Bureau of Mines, College Park, Md.

Resource Recovery Facility

nburned Refuse

MSW is shredded by a primary shredder; the

light fraction is separated by a light air

classifier and collected in cyclone No. 1; the

large particles are separated by a trommel

and reshredded by a secondary shredder.

Bag 1 Light Paper

and

Plastic

133
Figure 3 U.S. Bureau of Mines, College Park, Md.

Resource Recovery Facility

Unburned Refuse

/Light Air Classifier

Very Light Paper

and Plastic

MSW is shredded by a primary shredder; the

light fraction is separated by a light air

classifier and collected in cyclone No. 1; the small particles are separated by a trommel with 3/4 inch openings and further

separated from fine glass and dirt by a No. 14

mesh screen.

3/4”

Trommel 9000

9 0 0 0

No. 14 Mesh

Screen

Fine Glass

and Dirt

Bag 2 Light Paper

and

Plastic

134
Figure 4 U.S. Bureau of Mines, College Park, Md.

Resource Recovery Facility

Unburned Refuse

Light Air Classifier T~

(o) ass (Q)

Nonmagnetics

MSW is shredded by a primary shredder; the

heavy fraction is separated from the light

fraction by a light air classifier; ferrous

metals are removed from this heavy fraction

by a magnetic separator and the light portion

of this heavy fraction is separated by a primary air classifier and collected in cyclone No. 2; the large particles are separated by a trommel and reshredded by

the secondary shredder.

135
Figure 5 U.S. Bureau of Mines, College Park, Md.

Resource Recovery Facility

Unburned Refuse

|

Primary

Shredder

Light Air Classifier

Magnetic

Separator

Nonmagnetics

MSW is shredded by a primary shredder; the

heavy fraction is separated from the light

fraction by a light air classifier; ferrous

metals are removed from this heavy fraction

by a magnetic separator; and the light

portion of this heavy fraction is separated

by a primary air classifier and collected in cyclone No. 2; the small particles by a trommel with 3/4 inch openings and further

separated from fine glass and dirt by a No. 14

mesh screen.

Fine Glass

and Dirt

136
Figure 6 U.S. Bureau of Mines, College Park, Md.

Resource Recovery Facility

Unburned Refuse

Glass, Nonferrous Metals,

and Heavy Organics

with Paper and Plastics

MSW is shredded by the primary shredder;

the heavy fraction is separated from the light

fraction by the light air classifier; ferrous

metals are removed from this heavy fraction

by a magnetic separator; and the heavy

portion of this heavy fraction is separated

by the primary air classifier; the large

particles of this heavy portion are separated

by a trommel and reshredded by the

secondary shredder; the lighter portion is then removed by the secondary air classifier

and collected in cyclone No. 3

i 3/ 4

”

oooo - oo oo

Aluminum and

Heavy Organics

with Paper and

Plastics
Figure 7 U.S. Bureau of Mines, College Park, Md.

Resource Recovery Facility

Unburned Refuse

Nonmagnetics

I

Primary

Air Classifier L LI * Glass, Nonferrous Metals,

and Heavy Organics

with Paper and Plastics i

3/ 4

”

T rommel oooo

OOOO

oo oo QOoci

Aluminum and

Heavy Organics

.

with Paper and

Plastics

MSW is shredded by the primary shredder;

the heavy fraction is separated from the light

fraction by the light air classifier; ferrous

metals are removed from this heavy fraction

by a magnetic separator; and the heavy

portion of this heavy fraction is separated

by the primary air classifier; the large

particles of this heavy portion are separated

by a trommel; and reshredded by the

secondary shredder; the heavier portion is then separated from the lighter portion by

the secondary air classifier; aluminum is removed from this heavier portion by an

electrostatic separator leaving only the

heavy organic material.

Secondary

Shredder

* *

A

I

Secondary Air' Classifier

1 Aluminum and

Heavy Organics

i

r

o:':=::0_

i X Electrostatic T Separator

Aluminum

Bag 6 Heavy

Organics

138
Figure 8 U.S. Bureau of Mines, College Park, Md.

Resource Recovery Facility

Unburned Refuse

Glass, Nonferrous Metals,

and Heavy Organics

with Paper and Plastics

i 3/ 4

" ooo

O O O O Trommel 5S00

Glass, Nonferrous Metals,

Heavy Food, and Other Organics

MSW is shredded by the primary shredder;

the heavy fraction is separated from the light

fraction by the light air classifier; ferrous

metals are removed from this heavy fraction

by a magnetic separator and the heavier

portion of this heavy fraction is separated

by the primary air classifier; the small

particles of this heavy portion are separated

by a trommel with 3/4 inch openings and

allowed to fall into a mineral jig filled with

water and the organic wastes are floated off

the top of the mineral jig.

139
'
APPENDIX A

EVALUATION OF

DURING

EUGENE

DATA ON HIGHER HEATING VALUES DETERMINED

ASTM ROUND ROBIN TESTING OF RDF3

S. DOMALSKI and STANLEY ABRAMOWITZ

CHEMICAL THERMODYNAMICS DIVISION

CENTER FOR CHEMICAL PHYSICS

A PAPER PRESENTED AT THE

SEVENTH MINERAL WASTE UTILIZATION

SYMPOSIUM, OCTOBER 20-21, 1980,

CHICAGO, ILLINOIS

A-l
Evaluation of Data on Higher Heating Values Determined

During ASTM Round Robin Testing of RDF -3

E. S. Domalski and S. Abramowitz

ABSTRACT

The potential application of RDF-3 as an alternative or

supplemental fuel is dependent upon its acceptance as an

article of commerce. ASTM Committee E-38 on Resource Recovery

and its Subcommittee on Energy E-38. 01 have been actively

engaged in the development of consensus standards for this

purpose since April 1974. Standard procedures for the

characterization of RDF-3 are being developed. These procedures

are based on those ASTM methods used in coal analysis. The

procedures developed will insure a meaningful purchase -

sales relationship between the buyer and seller. A variety

of chemical and physical test procedures were studied by as

many as 12 laboratories. Currently 20 editorial draft

standards have been prepared and are being studied by the

committee membership.

The National Bureau of Standards in cooperation with

ASTM subcommittee E38.01 has undertaken a technical review

of a selected group of test procedures to determine selected

chemical properties of RDF-3. The property of principal interest

in this evaluation is the higher heating value. In

order to properly characterize this property, critical evaluation

of methods to determine total moisture, residual moisture,
and ash is also necessary. Intralab and interlab variations in

these properties are discussed. A comparison of these

results with those on round robin data for coal are also

made. The results of this study identify the levels of

precision for intralab and interlab agreement.
Introduction

The National Bureau of Standards has been a participant

in the development of standard test methods for refusederived fuel-three (RDF-3) * with ASTM committee E-38 (Resource

Recovery) and its Subcommittee E-38. 01 (Energy) since the

beginning of the testing program in the summer of 1977.

Since that time, two preliminary and three definitive series

of round robin RDF-3 samples have been distributed and

examined by various testing laboratories. At present, some

twenty test protocols are in the form of editorial draft

standards. These standards are undergoing evaluation and

are under vote for acceptance at either Subcommittee or main

Committee levels.

In addition to its role as a participating test laboratory,

WBS has also studied the RDF-3 test protocols for the purpose

of simplifying procedures, attempting to clarify ambiguities,

modifying procedures to improve the precision and accuracy

of test data, providing reasons for the apparent dispersion

of data, developing new procedures when there appeared to be

such a need, and suggesting levels of precision for tests.

Refuse-derived fuel-three (RDF-3) is defined as a shredded

fuel derived from municipal solid waste (MSW) which has

been processed for the removal of metal, glass, and other

entrained inorganic materials. Generally, this material

has a particle size such that 95 weight percent passes

through a 2-inch square mesh screen.
Studies at NBS and elsewhere suggest that the heterogeneity

of RDF still poses a serious problem to the extraction of a

representative sample of RDF for analysis. Sampling techniques

which will provide representative samples need further development. Poor agreement found for data within and between laboratories will not improve until advances in the sampling of RDF

have occurred.

The focus of this paper is directed toward the evaluation

of data on the higher heating values (HHV) of RDF-3 determined

during the round robin testing program. As part of this

evaluation of HHV data, procedures for moisture and ash

content determinations were also studied because of the need

to calculate higher heating values on an as-received basis

(HHV1) , dry basis (HHV2) , and moisture-ash-free basis (HHV3)

.

The initial path taken by Subcommittee E-33.01 toward

the development of standard test methods for RDF-3 was to

examine the ASTM procedures already established for coal and

coke, and to see what kind of changes were necessary to accommodate

the testing of RDF-3. Modifications were introduced as they

appeared necessary.

Definitive Round Robin Testing

Arrangements were made to begin a series of round robin

tests on RDF-3. Samples were prepared at the National

Center for Resource Recovery (NCRR) , Washington, D.C., and

were distributed to the various participating laboratories

A-5
for the first two preliminary and first two definitive

series of round robin tests. The samples for the third

definitive series of testing were prepared and distributed

by Americology , Milwaukee, Wisconsin. The RDF-3 laboratory

sample was composed of one inch or smaller material. Each laboratory

was provided with about 2 kg of sample for chemical analysis.

Prior to processing the sample down to 0.5 mm particles for HHV,

residual moisture, ash, and other determinations, the sample

was air dried in the temperature range from 30 to 40 ‘C so

that its moisture content could be brought near to equilibrium

with the atmosphere in the test laboratory. We used 2.5 gram

pellets which were prepared from 0.5mm RDF for the HHV,

residual moisture, and ash content determinations.

The chronology of the round robin tests is outlined in

table 1. Six laboratories participated in the first and

t tl second preliminary (zero 1

) rounds of testing. The precision

of the data die not seem satisfactory from these rounds. It

was felt that a period of acclimation was required for

laboratory analysts to acquire some experience in processing

ana analyzing RDF- 3 samples.

Eight laboratories participated in the first definitive

series of round robin tests which took place in June and

July of 1978. The mean and standard deviation of measurements

on higher heating values (HHV) as calculated for three

different bases are shown in table 2; as-received basis

(HHV1) , dry basis (HHV2) and moisture-ash-free basis (HHV3)

.

Corresponding data for total moisture, residual moisture,

and ash content determinations are given in table 3.
Each mean value, x, listed in tables 2 through 11 is the

average of four determinations; two runs carried out on day one

and two runs carried out on day two, each being performed in

the same laboratory, by the same analyst, using the same apparatus. The standard deviation, s, of the four replicates is provided in tables 2 through 11. The classification of days and

within-days was ignored in calculating s; however, this statistic is still a rough estimate of the variability within labs.

Also provided in tables 2 through 11 are averages of the means

for the first round robin sample for the participating laboratories, the corresponding standard deviations, and the average

value of the laboratory standard deviations.

Examination of the data on HHV1, HHV2, and HHV3 in table

2 showed that the dispersion of the data between each laboratory

appeared higher than what one might expect and, in most

cases, was considerably higher than what ASTM protocols for coal

and coke (D2015) would allow. The standard deviations of

the average of the means for HHV1 , HHV2, and HHV3 were five

to seven times the dispersion expected. The total moisture,

residual moisture, and ash content data tabulated in table 3

also appeared to be disproportionately high.

Doubts about the homogeneity of the milled (particle

size, 0.5 mm) RDF-3 sample were being raised at the ASTM E-38

meeting following the first round of testing. Some analysts

suggested that sub-division was difficult because segregation

of light and heavy particles was sometimes observed in

either riffling or coning and quartering of the sample in

preparation for analysis. The accountability of non-millable
portions of the RDF- 3 sample was not easy and required the personal

and professional judgment of the analyst. It more than likely varied

from one laboratory to another. Unequal distribution of non-millable

material in the laboratory samples also contributed to this variation.

Interlaboratory Comparison Samples

In an effort to ascertain whether improved precision

could be obtained for higher heating values, moisture, ash

content determinations, and other important properties, an

interlaboratory reference or comparison sample was prepared

for round robin testing in addition to the usual sample of

RDF-3 for the second and third rounds. The interlaboratory

comparison sample was milled down to 0.5 mm particle size by

a single laboratory prior to distribution to all of the

participating labs. The comparison sample would eliminate

possible, biases which might have been introduced into -the

particle size reduction operation at each of the participating

laboratories. Differences of opinion as to how: (1) the

RDF-3 sample should be milled, split, blended, (2) nonmillable material should be identified and extracted, and

(3) sampling should be performed, suggested that the decisions

by analysts at the various laboratories were not always equivalent.

It was hoped that an interlaboratory comparison sample would remove

such biases

.

Tables 4 and 5 provide data on the higher heating values,

moisture, and ash content for the RDF-3 sample prepared and

A-8
I

^distributed by Americology to twelve participating laboratories

m

in the second round of testing. A significant improvement

Jin precision was observed except for the results on residual

moisture. The standard deviation of the average of the means

Bfor the residual moisture had doubled while the actual average

| of the means itself had decreased from 4.110 to 2.715 wt. percent.

An examination of the standard deviations of the average of the

J

means for HHV2 in tables 2 and 4 shows a decrease from 287 Btu/lb

to 159 Btu/lb. A more modest improvement is found in

I tables 3 and 5 for total moisture and ash data when the standard

|

deviations of these averages are inspected. Perhaps the laboratory analysts were becoming more accustomed to handling RDF-3.

|

Results in general were still far from the precisions found for

coal and coke.

I Tables 6 and 7 show the statistical data for the inter-

| laboratory comparison sample for the second round. The

improvement in precision was very encouraging. The standard

| deviation of the average of the means for HHV2 was 60 Btu/lb; this

represents about a 60 percent improvement over the corresponding

^ data for HHV2 which was determined after each lab carried

| out its own milling of their laboratory samples. Similarly,

the standard deviation of the average of the means for the ash

, content data for the interlaboratory comparison sample in

table 7 was about half (0.73 wt. percent) of that found for

the corresponding laboratory sample data shown in table 5

(1.46 wt . percent). The standard deviation of the average of the

means for the residual moisture of the interlab sample decreased

A-9
by half in comparison to the regularly processed second

round sample. This improvement suggested that fewer biases

were interacting.

A third round of testing was carried out during the late

Spring of 1979. The statistical data calculated from the

results of testing on both the regular RDF-3 laboratory

sample and another interlaboratory comparison sample are

presented in tables 8 through 11. These results are somewhat

disappointing in that they resemble the first round in their

level of precision more than the second round. Comparison of

HHV1 , HHV2 , and HHV3 in table 8 with table 2 shows the standard

deviation of the average of the means 10 to 20 percent lower

in the third round than in the first round for the regular RDF-3

laboratory sample. Comparison of this same statistic in tables

3 and 9 shows that the precision for total moisture, residual

moisture, and ash content determination had decreased significantly: from 1.23 to 1.75 wt

.

percent for the total moisture,

from 0.497 to 1.54 wt. percent for residual moisture, and from

1.64 to 2.61 wt. percent for ash, respectively. Precisions

were also lower when the standard deviation of the average of

the means is examined for the results of the third inter laboratory

comparison sample and compared to the corresponding data in

the second round of testing. For example, this statistic is

154 Btu/lb for HHV2 for the third round (table 10) as compared

with 60 Btu/lb for the second round (table 6). Similarly, the

standard deviation of the average of the means for the ash data

for the third round is over three times (2.50 wt

.

percent,

table 11) that found for the interlaboratory sample studied
in the second round (0.73 wt. percent, table 7). The

residual moisture, however, is not too much different in the two

interlab rounds of testing; compare this statistic in table 11

(0.643 wt . percent) with the corresponding value in table 7

(0.518 wt. percent).

Bituminous Coal Round Robin

The data obtained for HHV, moisture, and ash content

determinations for the three rounds of testing were significantly

more variable than had been expected. In order to establish

some reassurance that a non-RDF reference sample could be

analyzed satisfactorily, a standard bituminous coal sample

(SRM-1632a) was distributed to six laboratories by NBS for

HHV, residual moisture, and ash determinations. The results

of this series of tests is shown in tables 12 and 13. In

table 12 one finds that the standard deviations of the average of

the means, for the coal sample are about the same for HHV1

,

HHV2 , and HHV3 , i.e., % 50 Btu(lb)

- ^. This value is considerably

lower than comparable values of the standard deviation of the

average of the means found for higher heating values in any of

the three rounds of testing. Similarly, values of this statistic

for residual moisture and ash content for the coal sample are

much lower than comparable values found in earlier rounds of

RDF-3 testing; for the residual moisture, the standard deviation

of the average of the means is 0.207 wt

.

percent and for ash is

0.15 wt

.

percent (table 13).

Hence, this series of tests on bituminous coal showed

that the participating laboratories could analyze a coal

A-H
sample to suitable levels of precision.

Repeatability and Reproducibility

In order to provide some quantitative estimate of where

the current state-of-the-art stood with respect to the

analysis of RDF-3 samples in contrast to the analysis of

coal, we carried out a statistical study of the data accummulated

in the first three rounds of testing using a program based upon

the theory of nested (hierarchical) designs (see "Statistical

Methods in Research and Production" by O.T. Davies, Third

Edition, published for Imperial Chemical Industries Ltd.,

Oliver and Boyd, London and Edinburgh; Hafner Publishing Co.,

New York). In this case, days were nested within labs and

replicates within days. There were two days of testing for

each lab and on each day two replicates were carried out.

The data obtained on the NBS bituminous coal sample

(SRM 1632a) were analyzed using methods described in ANSI/ASTM

E691-79, "Standard Practice for Conducting an Interlaboratory

Test Program to Determine the Precision of Test Methods."

In this case, each laboratory carried out two replicate

determinations, but only on one day.

Two statistics were particularly sought, namely, the

repeatability interval, I(r), which is a measure of within

laboratory agreement, and the reproducibility interval,

I(R) , which is a measure of between laboratory agreement.

These statistics could easily be compared to existing values

listed in documented ASTM Standard Methods of Test for Coal

and Coke for HHV, residual moisture and ash. For example,

in ASTM D2015 (Standard Test Method for Gross Calorific
Value of Solid Fuel by the Adiabatic Bomb Calorimeter) the

precision criteria for judging the acceptability of results

at the 95 percent probability level are:

Repeatability - duplicate results by the same laboratory

on different days, using the same operator and equipment

should not be considered suspect unless they differ by more

than 50 Btu/lb, dry basis.

Reproducibility - results submitted by two or more

laboratories (different equipment, operators, date of test,

and different portions of the same gross sample) should not

be considered suspect unless two results differ by more than

100 Btu/lb, dry basis.

Equations required to calculate the repeatability interval,

I (r)

,

are

:

I (r) = 2.83 s (r)

;

where s(r) is the pooled within- laboratory standard deviation

and 2.83 is a factor which converts the repeatability standard

deviation to a 95 percent repeatability interval.

s (r) = [s^(repl) + (days) ^ where s(repl) is the standard deviation of replicate measurements and s(days) is the standard deviation due to variations

in measurements observed between days.

Similarly, equations needed to calculate the reproducibility

interval, I(R), are:

I (R) = 2.83 s (R)

A-l 3
where s(R) is the between- laboratory estimate of precision

and 2.33 is defined as above.

s(R) = [(s^(repl) + s^(days) + s^ (labs)

where s(labs) is the standard deviation due to variations in

measurements observed between laboratories and s(repl)

and s(days) are as defined above.

Tables 14 through 17 summarize the repeatability and

reproducibility intervals calculated for HHV2, total moisture,

residual moisture, and ash, respectively. Data on all three

RDF-3 rounds of testing are tabulated, including the results

from testing of the bituminous coal sample, SRM 1632a. The

first row of tables 14, 16, and 17 gives the acceptability

limits according -to the appropriate ASTM protocol for coal and coke,

residual moisture, and ash content, respectively. No acceptability

limits are available for total moisture in coal and coke protocols.

Examination of the HHV2 data in table 14 shows that the

repeatability interval for the SRM coal round of testing, 69

Btu/lb, is close to the acceptable limit of 50 Btu/lb. The

reproducibility interval obtained for the SRM coal is 159

Btu/lb; this departs somewhat from the acceptable limit of

100 Btu/lb, yielding a ratio of I(R) to I(r) of 2.30 rather

than 2.00.

A- 1

4
The repeatability interval for the first three rounds

of testing of RDF-3 are between 3 and 6 times the 50 Btu/lb

limit; this includes the interlab comparison samples tested

in rounds two and three. The values of I(r) for the three

rounds of testing give an average value of 226 Btu/lb. The

corresponding average value for I(R) is 694 Btu/lb. It may be

observed that the I(R)/I(r) ratio for HHV2 for coal and coke

is approximately 2.00, and for RDF-3 is close to 3.00. For

practical purposes, one may adopt for RDF-3 repeatability

and reproducibility intervals for HHV2 of 250 and 750 Btu/lb

respectively. The latter values are much larger than those given

for coal and coke, but we feel that they represent the current

state-of-the-art in the repeatability and reproducibility

of HHV2 for RDF- 3.

*• Heterogeneity of RDF3

The heterogeneity of RDF-3 is still present at 0.5 mm

particle size.

Figures 1 and 2 show analysis samples of 0.5 mm RDF-3

magnified 50 times under a microscope. The particles are

heterogeneous even at this level of sub-division. Some are

spherical, some are elongated rods while others are irregularly

shaped. Differences in density are suggested by the black

and white contrast shown in the photos.

A-l 5
Figure 3 is the bituminous coal sample (SRM 1632a)

magnified 50 times under a microscope. The particles are

0.25 mm (-60 mesh) and have a generally homogeneous appearance

in comparison to the RDF-3 at the same magnification.

Differences in the densities of 0.5 mm plastic, cellulose,

iron, aluminum, sand, etc. help to defy the blending process

and extraction of representative samples for various tests.

The values of I(r) and I (R) for the interlaboratory

comparison samples of rounds two and three show that the

second round sample gave better results than the third

round. The reason for this is not immediately clear, but

the I(R)/I(r) ratio does illustrate the benefits of having

only one laboratory perform the processing of one inch

nominal RDF-3 down to 0.5 mm. Biases in the reduction of

tne size of RDF-3 are an inherent part of the reproducibility

interval values and cause I (R) to be so much larger than

I(r) for the three regular rounds of testing.

Summary of Results

The summary of I(r) and I(R) data for total moisture is

given in table 15. A trend is observed between the average of the

means and the repeatability interval I(r). Samples increased

in total moisture as testing went from the first, to the

second round, and to the third rounds; compare 13.82, 18.91,

and 30.09 wt . percent with I(r) values of 0.37, 0.57, and

0,76 wt . percent, respectively. Within-lab repeatability

lies between 0.4 and 0.8 wt . percent while between- lab

reproducibility lies between 3 and 5 wt . percent. The ratio

of X(R)/I(r) is poorest for the first round, 9.21.

A- 16
In table 16, we find I(r) and I(R) values for residual

moisture. The limits imposed on coal and coke samples (ASTM

D3173) are related to the moisture content of the samples

ana are given in the table. For example, if less than 5 wt

.

percent moisture is present in the coal or coke sample, then

I(r) and I(R) values are not considered suspect unless they

are above 0.2 and 0.3 wt . percent, respectively. The data

obtained by the six participating laboratories for the SRM

1632a sample fall within the above acceptability limits

since the sample contained 1.43 wt. percent residual moisture.

There appears to be a trend in the I(r) values for the three

rounds of testing similar to that observed in table 15,

related to the average of the means of the total moisture. Whether

there is a relationship or whether this is merely chance is

not clear. The averages of the means of the residual moisture do not

parallel the I(r) trend. The ratio of I(R)/I(r) ranges from

3.5 to 4.5. Again, for practical consideration, we have adopted

the ratio 4.00 with 0.75 and 3.00 wt. percent as values for

I(r) and I(r), respectively. No limits on the amount of residual

moisture in tne sample have been set as with coal and coke.

In table 17, we find the summary of values for I(r) and

I(R) for the ash content data. The limits for acceptable

data with regard to coal and coke samples (ASTM D31.74)

which contain (or do not contain) carbonates or more than 12

wt . percent moisture are given in the first three rows of

table 17. The results of testing the SRM 1632a coal sample

A-l 7
show that the participating laboratories have determined the

ash content well witnin the levels of acceptability. Values

of 0.08 and 0.16 wt. percent for I(r) and I(R), respectively,

are quite satisfactory. The repeatability and reproducibility

intervals for the first three rounds are quite high in

comparison to the coal and coke acceptability limits. The

same is true for the I(r) ana I(R) values obtained for the

interlab comparison sample. Although the second round data

for I(r) and I(R) are better for both the regular and interlab

samples, the absolute value of the average of the means is

significantly different; compare 14.17 wt. percent for the regular

RDF-3 sample with 19.76 wt . percent for the inter lab sample.

This difference may be due to the overall heterogeneity of

RDF-3. Other biases may be involved but are not apparent.

The suggested values for I(r) and I(R) are 2.5 and 7.5 wt

.

percent, respectively. These values are based on an adopted I(R)/I(r)

ratio of 3.00, and are much higher than expected, but this

is what is observed.

Final Summary and Conclusions

(1) The data from higher heating value, total moisture,

residual moisture, and ash content determinations were

examined and evaluated for three rounds of RDF- 3 sample

testing

.

(2) Repeatability and reproducibility intervals were calculated

as a result of carrying out a statistical analysis of

the data as described in ArJSI/ASTM E691-79 for the bituminous

coal round robin, and in "Statistical Methods in Research and

Production" by 0. T. Davies (loc. cit.) for the RDF-3

round robin tests.

A- 1

8
(3) Repeatability intervals for HHV2 (dry basis) , residual

moisture, and ash content are 250 Btu/lb, 0.75 wt

.

percent, and 2.5 wt. percent, respectively. These

adopted values are significantly higher than the

acceptable limits for coal and coke. Compare the above

with 50 Btu/lb, 0.3 wt. percent, and 0.5 wt . percent,

respectively, which are the acceptable limits for coal and coke.

(4) Reproducibility intervals for HHV2 (dry basis) , residual

moisture, and ash content are 750 Btu/lb, 3.00 wt

.

percent and 7.5 wt . percent, respectively. As with the

repeatability intervals, these adopted values are

significantly higher by six to eight times the acceptable

limits for coal and coke. Compare the above with 100

Btu/lb, 0.5 wt. percent and 1.0 wt . percent, respectively,

which are the acceptable limits for coal and coke.

(5) The heterogeneity of RDF-3 and RDF milled to 0.5 mm

particles makes extraction of a representative sample

difficult. Further development of sampling techniques

for RDF-3 and size reduction to smaller particles must

be pursued before improvement in the levels of precision

of round robin tests can be expected.

Acknowledgements

Funding for this work was provided by the NBS Office of

Recycled Materials and the DOE Office of Energy from

Municipal Waste.

A- 19
Table

1
Table

2

ASTM

Round

Robin

Testing

of

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(First

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Statistical

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on

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6

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Robin

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of

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(Second

Round)

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Data

on

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Values

RDF-3

Interlaboratory

Comparison

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A-28
Table

10

ASTM

Round

Robin

Testing

of

RDF-3

(Third

Round)

Statistical

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RDF-3

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Adopted

Values
Figure 1 RDF-3 Reduced to

Magn i f i ed 50 T i mes

(Each square is 0.25 mm on a

0.5 mm

side)

A-37
Figure 2 RDF-3 Reduced to 0.5 mm

Magnified 50 Times

(Each square is 0.25 mm on a side)

A- 38
Figure 3 SRM 1 632a Bituminous Coal Sample

Magnified 50 T i mes

(Each square is 0.25 mm on a side)

A-39

APPENDIX B

1. Large Isoperibol Bomb Calorimeter

The design of the large isoperibol (isothermal-jacket) calorimeter

which will accommodate the large combustion bomb, described in the following

section, is similar to that of Coops, van Nes, Kentee and Dienske, R.ec. Trav.

Chim. 66_, 113-130 (1947), Coops and van Nes, Rec. Trav. Chim. 66, 131-141 (1947),

and Gundry, Harrop, dead, and Lewis, J. Chon. Thermodynam. 1, 321-332 (1969) and

is shown in Figure 1 of this appendix. The calorimeter is constructed entirely of

stainless steel. It consists of a cylindrical calorimeter vessel 25.4 cm diam. , 45.

an height (10 inch diam. , 18 inch height) in which three rods support a

concentric cylindrical shield 20.3 cm diam., 30.5 cm height (8 inch diam. ,

12 inch height) . The calorimeter lid supports a stirrer assembly and a shield

cover. The shield, shield cover, and stirrer assembly facilitate the flow

of water in the calorimeter so that water is moving downward in the space

between the bomb and shield, and upward between the shield and wall of the

calorimeter vessel. The combustion bomb is supported by a foot which has been

welded to the bottom of the vessel to insure that the bomb will be positioned

in the same tanner in the calorimeter for each experiment. The calorimeter

vessel contains 19 liters of water for each calorimetric measurement and is

housed in a submarine vessel which has a cover. The submarine cover is fastened

to the vessel with six bolts and has four vertical ports for: (1) fuse circuit

leads, (2) a calorimeter heater, (3) a central stirrer assembly and, (4) quartz

thermometer leads. The frequency of oscillation of a temperature- sensitive

quartz crystal is used to determine the calorimeter temperature. The NBS

standard frequencies of 10 and 100 kHz are utilized. The entire

calorimeter system (bomb, calorimeter vessel, and submarine compartment) is

immersed in a constant temperature water bath maintained at 30 + 0.03 3 C. The

overall volume of the bath is 280 liters and holds 235 liters of water with the

calorimeter system immersed in it.
2. narge Corpustion Bornb

The combustion bomb which accommodates a 25 gram sample of RDF was purchased

frail the Parr Instrument Company ana is shown schematically in Figure 2 of this

appenaix. The bait) has an overall height of 35 cm (13.75 in) and has a mass of

13.3 kg (30.5 lb) when assembled; the internal and external volumes of the bcmb are

l.b5 ana 3.62 liters, respectively. A platinum crucible (%50 cm^) was used in

the calibration experiments with benzoic acid and a stainless steel crucible

3 (v50 cm ) was usea in the cambustion experiments with RDF. The bomb body has a

wall thickness of 0.953 cm (0.375 in) ana an outer diameter of 11.4 cm (4.5 in).

3 . Calorimetric Procedures

Stoichicoietrically, 2 grams of oxygen are requirea for the combustion of

1 gram of benzoic acid. Normally, 10 grams of oxygen are used for each gram

of benzoic acid to insure complete cambustion in the conventional- size bomb.

It has been found in practice that 6.5 g of oxygen per gram of benzoic acid

is the minimum requirement for camplete combustion in the present design of

bamb calorimeters . Tne large bomb utilizes a 16 . 3 gram benzoic acid sample

and contains about 100 grams of oxygen under a pressure of 4.1 HPa (40 atm).

This is on the boraerline of the minimum amount of oxygen necessary for complete

combustion in bomb calorimetry. Due to the limited quantity of oxygen in the

large bamb, combustion is incomplete ana a few tenths of a milligram of carbon

residue is found in the combustion crucible. The energy of combustion of benzoic

acid assumes complete cambustion ana therefore a small correction for unbumed

carbon, q-carbon, is included in the energy summation. In our experiments, the

total correction for unbumed carbon is usually less than 40 joules for a 400 000

joule experiment (1 part/ 10 000; hence, even without this correction, the

error introduced would be below the 1 part in 10 000 level, and acceptable for

precision combustion calorimetry of benzoic acid.

B-2
The correctea temperature rise of the calorimeter, AT-corr, is calculated

ana aividea into the total energy supplied to the calorimeter, Q- total, to yield

the energy equivalent, E-cal, of the calorimeter. The mass of water introduced

into the bomb, the crucible, and the sample may change from experiment to experiment

.

The product of the mass of these materials and their specific heats is subtracted

from the energy equivalent of the calorimeter, and the energy equivalent of the

"empty" calorimeter, E-si, is obtained.

The important parameters to compare between the two calorimeters are the

energy equivalents and the total energy capacities. The energy equivalent

of the small calorimeter is 14 555 joules per Kelvin while that of

the large calorimeter is 86 162 joules per Kelvin. The product of the

energy equivalent and the specified temperature rise gives the total energy

capacity . The large calorimeter has a total energy capacity of 430 310 j oules

,

as compared to 43 665 joules of the small calorimeter. Therefore, a sample which has

a mass ten times larger and less particle .size reduction can be used in the

large calorimeter. This is extremely important since the calorific value of an

RDF sample can now be determined with only minimal processing, and the possibility

of chemical changes imposed upon the RDF sample as a result of size

reduction can now be investigated quantitatively.

B-3

25-gram-capacity Bomb Calorimeter

A, pulley to stirrer motor; B,one of four stacks attached to the submarine lid to

accommodate (1) fuse circuit, (2) heater, (3) temperature sensor, and (4) stirrer,

C, submarine lid; D, submarine flange with “O” ring-, E, calorimeter vessel lid; stirrer

shaft; G,shield cover; H, stirrer, I, calorimeter vessel supports; J, shield; K, combustion

bomb; L, submarine vessel-, M, calorimeter vessel; N,bomb foot.

FIGURE 1

B-4
A

B

C

D

E

F

G

H

I

J

K

LM

N

0

PQ

Inner Arrangement of Large Combustion Bomb

A Grounded Electrode

B Valve

C Split Ring

D Compression Ring

E Drop Band

F Buna-N 0-Ring

G Bomb Head

H Bomb Body

I Handle

J Gas Inlet Tube

K Ungrounded Electrode

L Fuse

M Fuse Attachment Hook

N Ring Holder

0 Ring Support

P Sample Pellet

Q Crucible

FIGURE 2

B-5
Appendix C

Emission Spectrochemical Analyses of Bomb Residues

1. Teledyne National

2. ECO FUEL-II

3. Ameri oology

Emission spectrochemical analyses were performed on bomb residues which

were collected after bomb calorimetric measurements were performed on RDF sampl

The RDF samples for which emission spectrochemical analyses are available

are: Teledyne National, ECO FUEL-II, and Americology. Semi -quantitative

results which were obtained for the RDF residues are provided in tables 1, 2,

and 4 of this appendix. The elements are listed in order of decreasing

abundance in the residue with the approximate percentages adjacent to the

elemental symbol in parenthesis. In addition, similar data are given for ECO

FUEL-II and the Americology RDF samples prior to their combustion in a bomb

calorimeter. The latter data are shown in tables 3 and 5 of this appendix.
Table 1. tmission Spectrochemi cal Analysis of

Teledyne National RDF Bomb Residue [1]

c/ . I

to > 1 1 >

c6 > .1 .1 > % > .01 .01 > °/> >

Si (50) Mn (.• 5) Li (.05) Ag (.002)

Ca (15) Ba (• 2) Cu (.04) Be (.001)

Na (10) Sr (.• 2) Cd (.02)

A1 ( 5) Cr (..1) Ni (.02)

Fe ( 2) Pb ( 1) V (.02)

Zn ( 2) Sn (• 1) Zr ( .02)

K ( 2) B (.01)

Mg ( 1) Mo (.01)

Ti (-1) Rb (.01)

C-2
Table 2. Emission Spectrochemical Analysis of ECO FUEL-II RDF Bomb Residue

% > 1 1 > % > . 1

Si (»1 5) Ti (.5)

A1 (5) Mn (.3)

Ca (3) Ba (.2)

Fe (2.5) Sr (.1)

IMa (.2)

Mg (1.5)

K (1)

.1

i A |

A o — .01 > % .001

Cr (.05) Ag (.001)

Cu (.05)

Ni (.02)

Su (< -02)

V (< -02)

B (.01)

C-3
Table 3. Emission Spectrochemical Analysis of ECO FUEL-II RDF (as-received)

% > 1 1 >%_>.! .!>%> .01 .01 > S> .001

Si (2) A1 (.5) Mn (.05) Ag (< .001)

Fe (.5) Ti (.05)

Ba (-.5) Ba (.02)

Ca (.2) Cu (.02)

K (.2) Cr (< .02)

Mg (.2) Ni (< .02)

, ( Su (< .02)

Sr (< .02)

§

C-4
Table 4. Emission Spectrochemical Analysis of Ameri oology RDF Bomb Residue

1o > 1 i > i > ,i .1 > % > .01 .01 > % >

Si (>>15) Ti (.5) Cr (.05) Ag (.002)

Na (10) Ba (.2) Cu (.05)

Ca (5) Mn (.2) Sr (.05)

Mg (5) Pb (.2) Ni (.02)

A1 (2.5) Sn (.02)

Fe (1.5) V (< .02)

K (1) B (.01)

C-5
Table 5. Emission Spectrochemical Analysis of Americology RDF processed

to 0.5mm Particle Size

% > 1 1 > % >_ . 1 .1 > % > .01 .01 > % > .001

Si (5) A1 (.5) Mn (.05) Ag (< .001

)

Na (1) Ca (.5) Ti (.05)

Mg (1

)

Fe (.3) Ba (.02)

K (.2) Cu (.01)

Pb (.2) Ni (< .02)

Sn (< .02)

Sr (< .02)

V (< .02)

Cr (< .02)

B (< .01

C-6
APPENDIX D

Conversion Table for the Calculation of Data to Different Bases

Conversion Formula Table

Given

Wanted

As Determined (ad) As Received (ar) Dry (d) Dry Ash-Free (daf)

As Determined (ad)

100 - Mar

100 - M

ad

100 100

100 - M

ad

100 - H

ad

- A

ad

As Received (ar) 100 - M

ad

100 - Mar

100

100

100 - M 100 - M - A

ar ar ar

Dry (d)

100 - M

ad

100

100 - M

•ar 100

100

100 - A

Dry, Ash-Free (daf)

^ ~ M

ad

" A

ad

100 - M - A ar ar

100 - A

100 100 100

To convert any of the analysis values for the parameters listed above from one basis

to another, multiply the given value by the value shown in the appropriate wanted

column; M is the as-received or total moisture, M . is the as-determined or

a i dU

residual moisture, A

ad

is the as-determined ash content, and A^ is the ash content

on a dry basis. Moisture and ash content data should be in units of wt. percent.

D-l
I
APPENDIX E

Calculation of Total Moisture in an RDF Sample

A. Definitions

1 . Total Moisture

A determination of the water contained in a sample in the as- received state.

This determination is made by drying the sample in an atmosphere under rigidly

controlled conditions of temperature, time, and air flow. This determination

may consist of a single-step or a two-step drying process.

2. Air Drying

A process of partially drying RDF to bring its moisture content to near

equilibrium with the ambient atmosphere in which further reduction, division,

and characterization of the sample are to take place. In order to bring about

this equilibrium, the RDF is usually subjected to drying under controlled

temperature conditions ranging from 30 to 40°C.

3. Air Dry Loss (A.D.L.

)

The decrease in mass due to air drying. This decrease is presumed to be

moisture in the sample.

4. Residual Moisture

The moisture content remaining in an RDF sample after it has been milled to

small particle sizes such as 2 mm or 0.5 mm. A certain amount of the

residual moisture may be lost or picked up by the sample during the equilibration

with the ambient atmosphere. Prior to milling, the RDF sample should have

been subjected to either a total moisture determination (single-step), or an

air drying procedure.

B. Calculation of Total Moisture

M (total) = M (residual) x (100-A.D.L. ) / 1 00 + A.D.L. where M (total) is the

total moisture in the sample, M (residual) is the residual moisture, and A.D.L.

is the air dry loss; units should be expressed in wt. percent.

E-l
m
Acknowledgement

We wish to acknowledge the assistance of Mr. David J. Mitchell from the

NBS Thermal Processes Division in the preparation of some of the RDF samples

for calorimetric measurement, and in some of the determinations of moisture and

ash content.

F-l

NBS-114A [rev. 2-80

U.S. DEPT. OF COMM. 1 . BIBLIOGRAPHIC DATA

SHEET (Seem structions)

PUBLICATION OR 2 REPORT NO.

. Performing Organ. Report NoJ 3 Pu NBSIR 81-2278

blication Date June 1981

4. TITLE AND SUBTITLE

Test Procedures for the Determination of the Gross Calorific Value of Refuse and

Refuse-Derived Fuel by Conventional and Large Bomb Calorimetry. Summary of 1979 Fiscal

Year Results

5. AUTHOR(S)

D.R. Kirklin, J. Colbert, P. Decker, S. Abramowitz, and E.S. Domalski

6. PERFORMING ORGANIZATION (If joint or other than NBS. see in struction s) 7. Contract/Grant No. NATIONAL BUREAU OF STANDARDS

DEPARTMENT OF COMMERCE

WASHINGTON, D.C. 20234

543-3405 DOE 543-3406 EPA

S, Type of Report & Period Covered

Interim

1 Oct 1978 - 30 Sent 197$

9,

SPONSORING ORGANIZATION NAME AND COMPLETE ADDRESS (Street. City. State, ZIP)

U.S. Department of Energy, Office of Energy from Municipal Waste, Forrestal Bldg., 100

Independence Ave. S.W., Wash. D.C. 20585; U.S. Environmental Protection Agency, Solid

and Hazardous Waste Research Division, 26 W. St. Clair Str. Cincinnati, OH 45268

10.

SUPPLEMENTARY notes

Funding shared equally by Sponsors. DOE contract No. EA-77-A-01 -6101 , Task Order No.

A926-BCS, PR #80CS20459.001 EPA Contract No. EPA- I GA-D7-01 1 18

| Document describes a computer program; SF-185, FlPS Software Summary, is attached.

11.

ABSTRACT (A 200-word or less factual summary of most si gnificant information. I f document includes a significant

bi bliography or literature survey, mention it here) . ,

. . . . , , - . , . . . This report provides the results of investigations

during fiscal year 1979 to develop test procedures for the determination of the calorific value of refuse and refuse-derived-fuel (RDF) by means of oxygen bomb calorimetry.

The results of 138 calorimetric measurements are discussed, along with 32 calorimeter

calibration measurements, for 20 different RDF samples. In addition, determinations have

been carried out on these RDF samples for air dry loss, residual moisture, furnace ash,

bomb ash, and sulfur content to correct the calorimetric data for their presence; the

latter group of measurements amounts to 283 experiments. The calorimetric (and related)

measurements can be categorized into five classes: (1) measurements carried out in con- junction with ASTM round robin testing of RDF-3, (2) measurements on an Americology RDF

extracted using both selective and non-selective sampling methods, (3) measurements re- quired to compare data obtained from the small (2.5 gram capacity) and large (25 gram

capacity) bomb calorimeters , (4) measurements carried out in the large bomb calorimeter

on seven processed samples of different particle size obtained from New Castle County

Delaware MSW, and (5) measurements on some RDF's of special interest. Five appendixes

include additional information on: the evaluation of data on higher heating values obtained during ASTM round robin testing of RDF-3, the large bomb calorimeter, spectrochemical analysis of bomb residues, conversion tables, and calculation of total moisture in an RDF sample.

12.

KEY WORDS (Six to twelve entries; alphabetical order; capitalize only proper names; and separate key words by semicolon sj ASTM round robin testing; bomb calorimetry; 2.5 and 25 gram capacity bomb calorimeters

;

higher heating value; refused-deri ved-fuel ; sample characterization; sample processing

effects

13. AVAILABILITY 14. NO. OF

PRINTED PAG ES

Uni imited

1

| For Official Distribution, Do Not Release to NTIS 216

j 1 Order From Suoerintendent of Documents, U.S. Government Printing Office, Washington, D.C. 20402. 15. Price

33] Order From National Technical Information Service (NTIS), Springfield, VA. 22161 $17.00

l USCOMM-DC 6043-P90
An evaluation of data on higher heating values determined during the

ASTM round robin testing of RDF-3 showed that the repea tabi 1 i ty (within-lab

agreement) and reproducibility (between-lab agreemtn) are 250 and 750

Btu/lb when values are converted to a dry basis. These variabilities

are 5 and 7.5 times greater, respecti vely , than the precision levels

accepted in ASTM protocols for determining the higher heating values of

coal or coke on a dry basis (see Appendix A).

Measurements on three RDF samples in both small (2.5 gram-capacity

)

and large (25 gram-capaci ty ) bomb calorimeters showed that equivalent

high precision can be obtained in both calorimeters. The large bomb

calorimeter has the advantage that it can accorranodate RDF samples whose

particle size is as large as 25 mm (1 inch).

The mean and standard deviation of the calorific values obtained for

20 different RDF samples give 9482 and 553 Btu/lb, respecti vely , on a moisture-ash free basis using the furnace ash method to determine the

ash content. Thse results support the generally accepted value of

9500 Btu/lb as the higher heating value for RDF on a moisture-ash

free basis.
OOA 204- 1

3 ANO TITLE Of THAVfLtniS) 4 ORGANIZATIONAL UNIT lOfwuon etc I

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