EA-6010-11

(Formerly FE-3800) »* Dist. Category UC-90C

MATERIALS RESEARCH FOR CLEAN UTILIZATION OF COAL

QUARTERLY PROGRESS REPORT

January - March 1977

Samuel J. Schneider

Project Manager

Institute for Materials Research

National Bureau of Standards

Washington, D. C. 20234

PREPARED FOR THE UNITED STATES

ENERGY RESEARCH AND DEVELOPMENT ADMINISTRATION

Under Contract No. EA-77-A-01-6010

(Formerly E(49-l)-3800)

"This report was prepared as an account of work sponsored by the United

States Government. Neither the United States nor the United States

ERDA, nor any of their employees, nor any of their contractors, subcontractors, or their employees, makes any warranty, express or implied,

or assumes any legal liability or responsibility for the accuracy,

completeness, or usefulness of any information, apparatus, product or process disclosed, or represents that its use would not infringe privately

owned rights."

TABLE OF CONTENTS

PAGE

I. OBJECTIVE AND SCOPE OF WORK 1

II. SUMMARY OF PROGRESS TO DATE 1

Articles Published and Talks Presented 4

III. DETAILED DESCRIPTION OF TECHNICAL PROGRESS 5

1. Metal Corrosion 5

a. Constant Strain-Rate Test 5

b. Pre-Cracked Fracture Test 25

2. Ceramic Deformation, Fracture and Erosion .... 28

3. Chemical Degradation 48

a. Reactions and Transformations 48

b. Slag Characterization 58

c. Vaporization and Chemical Transport 63

4. Failure Avoidance Program 54
If
I. OBJECTIVE AND SCOPE OF WORK

Coal Gasification processes require the handling and containment of

corrosive gases and liquids at high temperature and pressures, and also

the handling of flowing coal particles in this environment. These

severe environments cause materials failures which inhibit successful

and long-time operation of the gasification systems. The project

entails investigations on the wear, corrosion, chemical degradation,

fracture, and deformation processes which lead to the breakdown of

metals and ceramics currently being utilized in pilot plants. Studies

will also be carried out on new candidate materials considered for

improved performance. Special emphasis will be devoted to the development of test methods, especially short-time procedures, to evaluate the

durability of materials in the gasification environments. These methods

will focus on wear, impact erosion, stress corrosion, strength, deformation, slow crack growth and chemical degradation of refractories. A

system has been initiated to abstract and compile all significant

operating incidents from coal conversion plants. This program will

provide a central information center where problems of common interest

can be identified and analyzed to avoid unnecessary failures and lead to

the selection of improved materials for coal conversion and utilization.

Active consultation to ERDA and associated contractors will be provided

as requested.

II. SUMMARY OF PROGRESS

Brief Summary

1. Metal Corrosion

a. Constant Strain-Rate Test

The slow strain rate (1 x 10~^s“^) testing of 310, 310S, 347 SS, and

Incoloy 800 at 540°C (1000°F) in H2 S saturated at room temperature with

water vapor was completed. 310 SS specimens were tested in H2 at 8.4 X

10“^s“^. One tested in H2 at 540°C (1000°F) fractured in a brittle type

manner with secondary cracking. While another 310 SS specimen tested in

H2 at 454®C (850°F) fractured in a ductile manner with no secondary

cracking. Incoloy 800 specimens were tested in the same manner as 310

SS where cracking occured (low strain rates), but no loss of ductility

was apparent in the Incoloy 800. All parts and equipment for testing in

coal gasification environments are on hand with the exception of a distilled water reservoir and steam line heating tapes which will be

delivered in two weeks.

1
Brief Summary (continued)

b. Pre-Cracked Fracture Test

The modification of the elastic stress-intensity calibration for the use of the double cantilever beam specimen at elevated temperature

has been completed and limits for the use of the elastic stress

analysis have been established. Sample calculation for grade 310

stainless steel have been completed.

The elastic-stress-intensity calculations will be extended to the

elastic-plastic stress range and applied to other materials of

interest. Experimental verification of these analyses will be

started .

2. Ceramic Deformation, Fracture and Erosion

Studies of creep deformation, fracture and erosion has proceeded in

three major work areas: construction and assembly of a high temperature high pressure mechanical tester; accumulation of strength data

on castable refractories after exposure to hydrothermal environments;

and accumulation of high temperature erosion data on castable

refractories. Work on the high pressure vessel is nearing completion;

the vessel should be operational by this summer. Strength degradation

studies after hydrothermal exposure of a high and low purity aluminum

oxide refractory (calcium aluminate bonded) have been completed to

910°C; strength degradation is observed in the high purity refractory

(at approximately 410°C), but not in the low purity refractory.

Erosion studies as a function of particle velocity, temperature and

impingement angle have been completed on a phosphate bonded refractory.

A model has been developed to explain the angular dependence of the

erosion rate.

3. Chemical Degradation

a. Reactions and Transformations

Construction of major components of the apparatus for x-ray examination

of refractory castables under simulated gasification conditions has

been completed. The system will be assembled during April 1977, and

tested at high temperature. Operation will be limited to one atmosphere of pressure until the flange seals arrive. _In s^tjj x-ray

diffraction measurements are expected to begin in April 1977 as proposed .

2
Brief Summary (continued)

b. Slag Characterization

The main pressure vessel for viscosity determinations has been

constructed and pressure tested. The viscosity of several slag

compositions have been measured at ambient pressure and the

predictive equation of Watt-Fereday checked against the measured

values.

c. Vaporization and Chemical Transport

After several months experience with the prototype platinum tube

reactor a severe gas leak developed, necessitating construction of

a new reactor. Calibration tests have proceeded with this new reaction using Na2S04 with the particular objective of monitoring

the Na2S04 vapor species which was not observed in our earlier tests.

Auxiliary classical Knudsen effusion studies on Na2S04 were

performed to obtain equilibrium data for comparison with the reactor

experimental results. Following this testing and calibration phase

we plan to introduce gases such as H2O, H2, SO2 and HCl into the

system and determine their effect on vapor phase transport, for

Na2S04 and NaCl initially.

4 . Failure Prevention

Continued enlargement of the Failure Prevention Information Center

was carried out. Additional reports of operating experiences were

received, classified, and evaluated. Programs were developed to

conduct failure mode and other statistical analysis of data in the

data base. Future plans are to continue to enlarge the data base

and to begin issuing abstract and summary reports on failure

prevention.

3
Articles Published and Talks Presented

G. Ugiansky, "Constant Strain Rate Testing at Elevated Temperatures,"

at the General Electric Research Laboratory. (Invited Lecture)

J. M. Bukowski, E. R. Fuller, Jr., C. H. Kim, and C. Robbins,

"Microstructural Analysis of Hydrothermally Treated Refractory

Concretes," American Concrete Institute’s Symposium on Refractory

Concretes, March 17, 1977, San Diego, California. (Talk)

S. M. Wiederhorn, "Refractories for Coal Gasification," University

of North Carolina at Raleigh, March 17, 1977, Raleigh, North Carolina.

(Talk)

F. A. Mauer, T. Negas, A. Perloff, E. N. Farabaugh and C. R. Robbins,

"Analysis of MHD Electrodes and Coal Gasification Reactor Liners by

Diffraction Methods," February 23, 1977, Special session on Application of

Diffraction to Fossil Fuel Energy Related Materials at the American

Crystallographic Association Winter Meeting, Asilomar, Pacific Grove,

California. (Talk)

4
III. DETAILED DESCRIPTION OF TECHNICAL PROGRESS

1. Metal Corrosion

a. Constant Strain-Rate Test (G.M. Ugiansky and C.E. Johnson, 312.04)

Progress : To complete the present phase of testing before the alloys

are tested in a coal gasification environment, 310, 310S, 347 stainless steel, and Incoloy 800 specimens were tested at - 1 x 10“^ s~^

at 540°C (1000°F) in H2 S saturated at room temperature with water

vapor. The completed results are tabulated in Table 1 for the range

of strain rates at which the specimens were tested.

Table 1. Properties of Alloys Tested in H2 O/H2 S or Wet H2 S

at 540°C (1000°F)

Alloy 1Strain Rate, s“^ Elongation, % Reduction in Area, % Environment*

310 SS 1.3 X lo-"" 33.8 63.2 H 2O/H2 S 7.8 X 10“5 32.9 55.9 Wet H 2 S

5.5 X 10" 5 33.4 62.8 H 2O/H 2 S

7.2 X 10"® 22.5 33.1 H 2O/H 2 S 3.9 X 10"® 12.9 25.4 Wet H 2 S

3.6 X 10"® 23.7 30.2 H 2O/H2 S

1.1 X 10"® 17.2 18.4 Wet H2 S

8.4 X 10"^ 18.7 17.5 H 2 O/H2 S

1.9 X 10“^ 9.0 14.4 Wet H2 S

310 SS 1.3 X 10"^ 33.6 63.0 Wet H2 S 1.5 X 10"® 34.5 62 .

6

Wet H2 S

7.3 X 10"® 35.9 62.3 Wet H2 S

8.4 X 10"^ 34.8 50.1 Wet H2 S 1.2 X 10" 27.0 36.5 Wet H 2 S

347 SS 1.3 X 10-^ 17.4 62.0 Wet H2 S

3.7 X 10"® 15.5 63.1 Wet H 2 S

7.3 X 10"® 15.1 64.3 Wet H2 S

8.4 X 10"^ 14.5 55.4 Wet H2 S 8.4 X 10"^ 17.1 61.4 H2 O/H2 S

1.2 X 10"^ 8.6 48.8 Wet H2 S

In 800 1.3 X lO""" 32.8 68.8 Wet H2 S

3.7 X 10"® 33.5 65.3 Wet H2 S

7.3 X 10"® 34.2 55.2 Wet H2 S

8.4 X 10"^ 32.0 49.9 Wet H 2 S

1.7 X 10"^ 35.9 55.0 Wet H 2 S

*H20/H2S = H2 S plus steam

Wet H2 S = H2 S saturated at room temperature with water vapor.

Because of the heavy oxide and/or sulfide scale, the reduction in area measurements on the 310S and In 800 specimen tested at = 1 x 10“^ s~^

5
were calculated by determining the amount of metal lost on the

surface of the specimen outside of the reduced area due to the

formation of scale and adding this amount to the diameter of

unreacted metal in the reduced area remaining after the test.

The data tabulated in Table 1 are plotted in Figures 1, 2, 3, and

4 for the respective alloys. The properties of 310 SS show a considerable decrease as the strain rate is decreased (Fig. 1);

whereas, the properties of lower carbon 310 S (Fig. 2) and

stabilized 347 SS (Fig. 3) do not show a significant decrease

except at the very slow strain rate. Even then the decrease in

properties is not as significant as for the 310 SS. The properties

of Incoloy 800 (Fig. 4) are only slightly affected by the decreasing

strain rate.

Table 2 is a compilation of the rest of the data collected on the

alloys 310, 310 S, 347 SS, and Incoloy 800 at various temperatures

and environments during the preliminary testing of these alloys

before testing in coal gasification environments. Here again it

should be noted that the properties for the 310 SS decrease with

decreasing strain rate independent of environment but at temperatures above 454°C (850°F). Some of the final tests were made on 310 SS in H2 to further determine the effect of environment. The

first 310 SS specimen was tested at 540°C (1000®F) at a strain

rate of 8.4 x 10“^s~^. The H2 was passed through hot copper turnings,

two liquid N 2 traps, and P 2 O 5 to trap moisture before entering the

test chamber. The resulting reduction in area was 23.3%. Secondary

cracking was apparent on the reduced area near the fracture as seen

in Figs. 5 and 6 . Fig. 7 is a higher magnification of one of the

intergranular cracks seen in Fig. 6 . Fig. 8 shows the Intergranular

cracking on the edge on the fracture surface of Fig. 5.

The second 310 specimen was first allowed to soak at 540“C (1000*F)

with no load applied for 67.5 hours. This was done to sensitize the

material. The specimen was then tested at 454°C (850°F) at 8.4 x 10“^ s~^ in H2

. This temperature was selected since it was below any

creep temperature for 310 SS but was still in the sensitizing zone (454-870°C) (958-1600°F) for 310 SS. The resulting elongation was

35% and the reduction in area was 49%. This compares to the 18*

elongation and 23% reduction in area when tested at 540“C (1000“F)

in the same environment and strain rate. Figs. 9 and 10 show that

there is no secondary cracking. While Fig. 11 shows that the edge

of the fracture surface is ductile.

The results of testing at 454“C (850°F) have given a strong indication that the cracking problem that has been seen in 310 SS is

due to creep occurring in the sensitized material with fracture

occurring in or near to the weaker precipitated carbide phase in

the grain boundaries.

Some data has been found to partially substantiate the opinion of

reduced ductility due to creep cracking in 310 SS (1).

(1) ASTM STP-124, 1952.

6
Creep-rupture elongations of 310 SS tested at 540°C (1000°F) in air

were listed at 12 and 16%, much the same as our data when tested

at a slow strain rate of 1 x 10“^s~^. Whereas, short time tensile

tests gave elongation of 36.2% at 540®C (1000°F) which is equivalent

to our data when tested at a fast strain rate (1.3 x 10“‘^s“^).

However, no data reported was for tests under the ultra-high vacuum

needed to insure no environmental interaction. Therefore, a mechanism

of failure involving environmental interaction cannot be ruled out.

Since Incoloy 800 is susceptible to sensitization, specimens were

tested at temperatures where creep occurs in order to investigate the

possibility of producing the same cracking problem and loss of

ductility that has been seen in 310 SS. An Incoloy 800 specimen

was tested at - 1 x 10”^ s~^ at 700°C (1300°F) in H2 with resulting

elongation of 32% and reduction in area of 54.5%. The 700®C (1300°F)

temperature was chosen so that the test would be well into the creep

and sensitization region. Some surface cracks appeared (Fig. 12)

but they seemed to be fissures opened by ductile tearing; whereas, the

cracks seen on the surface of the 310 SS specimens were more distinctive with sharp and jagged edges. Fig. 13 does not show any

large cracks propagating from the surface into the bulk of the

specimen but does show large voids or separations within the bulk

of the specimen.

Another Incoloy 800 specimen was allowed to soak at 700°C (1300°F)

in H2^, for 72 hours under a no load condition and then tested at

-lx 10“^s“^ at 540°C (1000°F) in H2 with resulting elongation of

30% and reduction in area of 58%. No cracking and no loss of

ductility was apparent as seen from Figs. 14 and 15. From the

data collected, we conclude that the Incoloy 800 does not have the

same susceptibility to cracking that the 310 SS has when tested

under sensitizing conditions.

Fig. 16 is a flow diagram of how the coal gasification environment

will be obtained. The completion of the setup for testing in coal

gasification environment has been delayed- awaiting the arrival of

a distilled water reservoir and steam line heating tapes which will

be delivered in two weeks.

Plans ; Test 310, 310S, 347, 446 stainless steels, Incoloy 800, and

Inconel 671 in an oxidizing coal gasification environment containing

CO, CO2, H2, CH4, H2S, and water.

7
Table 2. Properties of Alloys Tested At Various

Temperatures in Various Environments

Alloy Strain Rate Elongation, % Reduction Testing

s~^ in Area, % Temp. °C,(°F’) Environment

310 SS

310 SS

347 SS

In 800

2.0 X 10-^ 39.2 73.4

7.2 X 10"^ 35.9 72.6

7.2 X 10“^ 38.4 66.3

4.2 X 10"^ 32.7 68.4

1.1 X 10"^ 35.5 75.1

8.4 X 10“^ 32.9 61.2

8.4 X 10"^ 34.6 55.9

8.4 X 10 ^ 35.0 48.7

1.3 X

10"‘" 32.8 58.0

1.3 X 10-^ 34.4 55.7

1.3 X lO""* 36.6 60.5

7.2 X 10"^ 31.2 56.9

1.1 X 10"^ 18.7 24.2

1.1 X 10"^ 16.0 19.8

8.4 X 10"^ 15.4 19.0

8.4 X 10"^ 18.0 19.0

8.4 X 10"^ 17.3 25.3

8.4 10"^ 14.2 15.0

8.4 X 10"^ 17.9 23.3

8.4 X 10"^ 11.4 14.5

1.1 X 10-^ 40.6 20.8

8.4 X 10"^ 29.3 00

8.4 X 10“^ 31.7 74.6

5.2 X 10“5 16.3 64.1

7.4 X 10"^ 14.5 63.7

1.1 X 10“^ 14.6 57.5

8.4 X 10“^ 16.1 65.9

8.4 X 10“^ 29.9 58.0

8.4 X 10 ^ 32.3 54.4

23 (73) Wet H2 S

23 (73) Dry He

Dry He ^ ^ 23 (73)

23 (73) Air

23 (73) Wet H. S

370 (700) Dry He

370 (700) Wet HoS

454 (850) H2 (5)

540 (1000) Dry He

Dry He y ^ Dry He

540 (1000)

540 (1000)

540 (1000) Dry He

540 (1000) Tank Argon

540 (1000) Purified Argon

540 (1000) Dry He

540 (1000) Dry He

540 (1000) Ultra Pure He

540 (1000) House Vacuum, 34 Tor r 540 (1000) H, 815 (1500) Air

1038 (1900) Air

540 (1000) House Vacuum, 34 Torr

23 (73) House Vacuum, 34 Tor r 540 (1000) House Vacuum, 34 Torr

540 (1000) House Vacuum, 34 Tor r 540 (1000) House Vacuum, 34 Torr

540 (1000) House Vacuum, 34 Tor r

540 (1000) H,

704 (1300) H.

(1) Wet H 2 S - H 2 S saturated at room temperature with water vapor.

(2) 310 SS specimen was soaked for 72 hours at 540°C (1000“F) in dry Ho under

a no load condition before testing in dry He at 23“C (73“F).

(3) 310 SS specimen was soaked for 67.5 hours at 540“C (1000“F) In H under a no load condition before testing in H 2 at 454“C (850“F).

(4) 310 SS specimen was soaked for 72 hours at 540“C (1000“F) In drv He under

a no load condition before testing in dry He at 540“C (1000®F).

(5) 310 SS specimen was soaked for 72 hours at 540“C (1000"F) In wet H S under

a no load condition before testing in dry He at 540"C (1000*F).

(6) Incoloy 800 specimen soaked for 72 hours at 704“C (1300“F) In H under .1 no load condition before testing in H 2 at 540**C (1000'*F).

8
neT

9-3

9-3

I E t L

I t t t t [ 1 « « a a « a

a S t*' N H

NI NOJi.3n<13 fcl

C-3

A

rl

Iin

V

u

tn

Of

z

H

H

or

1“

m

I

9

Fig.

1.

Curve

of

reduction

in

area

versus

strain

rate

for

310

stainless

steel.

Tests

conducted

in

saturated

H

2

S

(wet

H

2

S)

and

in

steam

and

H2

S

(H

2

O/H2

S)

at

540“C

(1000*F)

.
UCT

H.S

H

<5i3> ni NDJiDn<33J±i

10

BTRPXN

RPTE.

<

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^^3

n

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( p a

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iD «

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I

|(u ;. I> t:

I c

eO Cl (D t

, cO Oil C tt H dh c0

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(II

01

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a

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a

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«

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01 B B

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W

B

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<*> ^a3fcjy Ni NDii.3n<i3a

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ft

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I-

(L

or

z

H

d

or

t“

m

11

Fig.

3.

Curve

of

reduction

in

area

versus

strain

rate

for

347

stainless

steel.

Tests

conducted

in

saturated

H

2

S

(wet

H

2

S)

and

in

steam

and

H

2

S

(H

2

O/H2

S)

at

SAO^C

(1000*F)

.
HET

HiS

6-J

12

5TRPXN

RPTE,

<

s~
Fig. 5

steel

8.4 X

. Scanning electron micrograph of the fracture of a 310

specimen tested at 540°C (1000°F) in at a strain rate

in-7c-l 20 X.

stainless

of

13
Fig. 6. Photomicrograph of the cross-section of the 310 stainless

steel specimen in Fig. 5 tested at 540°C (1000°F) in H. at a strain

rate of 8.4 X lO'^s"!. 20 X

^

14
Fig. 7, Photomicrograph of one of the cracks penetrating into the

310 SS specimen in Fig. 6. 500 X.

15
Fig. 8. Scanning electron micrograph of an area near the edge of

the fracture surface of the 310 SS specimen in Fig. 5, 700 X.

16
Fig. 9. Scanning electron micrograph of the fracture of a 310 SS

specimen tested at 454°C (850°F) in at a strain rate of 8.4 X 10“7s~l.

20 X.

^

17
Fig. 10. Photomicrograph of the cross-section of the 310 SS specimen

in Fig. 9. 20 X.

18
j Fig, 11. Scanning electron micrograph of an area near the edge of

the fracture surface of the 310 SS specimen in Fig. 9. 700 X.

I

I

i

i 19
Fig. 12. Scanning electron micrograph of the fracture of an Incoloy

800 specimen tested in H_ at 700°C (1300°F) at a strain rate of

1 X 10-6s-l. 20 X.

^

20
Fig. 13. Photomicrograph of the cross-section of the Incoloy 800

specimen in Fig. 12. 20 X.

21
J

Fig. 14. Scanning electron micrograph of the fracture of an Incoloy

800 specimen tested in at 540°C (1000°F) at a strain rate of

1 X 10-6s"l. 20 X.

^

22
i

i

I

Fig, 15. Photomicrograph of the cross-section of the Incoloy 800

specimen in Fig. 14. 20 X.

I

23
24

Fig.

16.

Flow

diagram

of

the

generation

of

the

coal

gasification

environments
b. Pre-Cracked Fracture Test (J. H. Smith, 312.01)

Progress : The elastic stress- intensity calculation for the wedge loaded

cantilever beam specimen has been modified to account for the effect of

temperature on the elastic modulus and thermal expansion. This calculation

equation is:

K

o o

h a w w

h

w

h a

(T - T ) ] n o

o

where

:

- modulus of elasticity of specimens at test temperature, T

E - modulus of elasticity of specimens at loading temperature

o - stress- intensity at test temperature

- stress-intensity at loading (reference) temperature

h - height of wedge at loading point w

h - height of slot in specimen

- coefficient of thermal expansion of wedge

- coefficient of thermal expansion of specimen

T - test temperature

T^ - loading temperature

Sample calculations using this calibration were done for 310 stainless steel

1. Wedge loaded DCB specimen.

2. Specimen thickness, B = 0.25 in.

3. = a^, loading wedge made of same material as specimen.

A. h =0.1xl0^m o

5. h =0.8xl0^m w

The results of these calculations are shown in Table A.

These results show that when the DCB specimen is loaded at room temperature

and subsequently heated to elevated temperature substantial drop in the

applied stress intensity at the crack tip occurs due to thermal expansion

and due to the change in modulus of the material. Corrections to the

stress intensity due to enlargement of the plastic zone at the crack tip were less than 5 percent up to a temperature of 600 °C.

25
Plans : The best available data for the strength, elastic modulus, and

thermal coefficient of expansion as a function of temperature will be

obtained for all materials of interest in this test program. This data

will be used to calculate the effect of temperature on the elastic stressintensity factor as a function of temperature ‘and to determine the limit

of applicability of the elastic analysis.

Suitable programs are now available to do elastic-plastic stress analyses

by finite element calculation procedures. These analyses will be done for

the double cantilever beam and three point bend specimens at a range of

temperatures and for a range of crack lengths. These analyses must be

repeated for each test material and the complete stress-strain curve must be used in the calculations at each temperature. The load versus

load point displacement (compliance) curve and versus load point

displacement curve will be obtained from these analyses. The results

of these analyses will be verified experimentally by determining the

compliance of the DCB test specimen at a range of temperatures.

26
Table A

Effect of Temperature on Stress Intensity

Temperature (°F)

K

o

0 1.00

400 0.95

800 0.88

1200 0.81

1600 0.66
2. Ceramic Deformation, Fracture and Erosion (E. R. Fuller, Jr.,

S. M. Wiederhorn, J. M.

Bukowski, D. E. Roberts,

and C. R. Robbins, 313.05)

Progress : Work on this project during the past quarter has proceeded in

three major areas; Construction and assembly of a high temperature high

pressure mechanical tester; accumulation of strength data on castables

after exposure to hydrqthermal environments; and accumulation of high

temperature erosion data on castable refractories.

Pressure Vessel

The shop work on the pressure vessel is nearing completion; the remaining shop work consists of machining several minor components and of

correcting any errors in design that might appear as the apparatus is

tested. A schematic diagram of the equipment is shown in figure 1. As can be seen in this figure, the equipment consists of three essential

parts: an environmental chamber to contain the corrosive gases; an external pressure vessel to maintain the structural integrity of the

environmental chamber during operation; and a load application system to

measure the fracture strength of the castable refractories at pressure

and temperature. The environmental chamber and the loading fixtures

that fit into the chamber are constructed of 310 stainless steel to

resist the corrosive effect of the test environment. Cooler parts of

the environment chamber and parts external to the chamber are made of

304 stainless steel. Load application is applied to the specimens by

means of a hydraulic system that is operated by a hand pump on the

control panel. To obtain near frictionless transfer of force and to

maintain the atmosphere of the environmental chamber, a set of bellows

(347 stainless steel) is attached to the rams that penetrate into the

environment chamber. To obtain high temperatures, heating elements

capable of 8 KW power are Installed around the environment chamber.

When completed, this equipment should be capable of operating at a temperature of 1000°C and a pressure of 1000 psi.

The high pressure vessel used to contain the environment chamber is

shown in Figure 2. The vessel was constructed of a 16 inch schedule 80

steam pipe and has an overall length of approximately 65 inches. The

pipe is capped by two 900 pound rated flat end flanges which contains

pipe fittings for electrical and pressure lines to the test equipment

(contained within the pressure vessel) . The vessel was designed in

accordance with the boiler codes and should be capable of 1500 psi at

room temperature. Because of the massive size of the vessel, a sturdy

test stand was constructed to support the vessel. The stand also

provides a convenient work surface to facilitate loading of the vessel

during its operation. An exhaust system was constructed as an integral

part of the test stand to remove any noxious gas that might be vented

into the atmosphere as a result of a leak in the vessel. To date the

28
pressure vessel has been assembled and hydrostatically tested to a pressure of 1500 psl for a period of 30 minutes. As there was no indication of water leakage during this period the seals on the system

seemed to operate adequately.

The internal parts of the test facilities, the environment chamber and

the loading ram are shown in figure 3. This part of the test equipment

has an overall height of approximately 62" and so will completely fill

the pressure vessel. The pressure chamber is mounted on a stainless

steel stand in order to locate the chamber in a central position in the

pressure vessel and to provide an adequate working distance for the

loading system. The hydraulic ram and the push rods can be seen at the

bottom of the figure, and the push rods that attach to the load cell can

be seen at the upper part of the figure. The bellows assembly are shown

in greater detail in figure 4. The interior of the vessel contains

loading fixtures that will be capable of testing castable ceramic bars

in three point bending. To accelerate the rate of testing the loading

fixture will be capable of consecutively testing four specimens. This

is accomplished by using the fixture shown in figure 5. The loading

bars on the fixture are unevenly spaced so that the specimens are broken

in sequence, each broken specimen falling to the bottom of the test

chamber after breakage. A test fixture of similar design has been

successfully used previously at NBS to study the fracture of ceramics.

Hydrothermal Exposure Tests

This part of the program is an extension of earlier work to determine

the effect of coal gasification environments on the strength of castable

refractories. Two types of castable ceramics were studied. Table 1:

One was a high purity aluminum oxide ceramic containing approximately 94

percent alumina; the other was a calcined flint clay ceramic containing

approximately 37 percent silica.

Table 1. Partial chemical compositions of castable refractories

(weight percent)

A94

High Alumina

Composition castable

Alumina (AI 2 O 3 ) 94.4

Lime (CaO) 4.5

Silica (Si02 ) 0.1

Iron Oxide (Fe203 ) 0.1

Soda (Na20 ) 0.2

A56

Calcined Flint

clay castable

55.6

4.5

37.0

0.8

0.2

29
Previous exposure tests were conducted in fixed volume vessels (Morrey

Bombs) which had a temperature capability of approximately 500°C. The

vessels were charged with water and ceramic and then heated to various

temperatures in the range 22-510°C. Strength measurements (by fourpoint bending) after exposure indicated a considerable contrast between

the two refractories. The strength of calcined flint clay refractory

(figure 6) was relatively Insensitive to hydrothermal exposure over the

range of temperatures studied. By contrast, severe strength degradation

(figure 7) was observed in the high alumina refractory at temperatures

in excess of 310°C.

Changes in strength of the castable refractories were correlated with

microstructural changes in the refractories resulting from chemical

interactions between the refractory and the high pressure steam. The

high purity aluminum oxide refractory forms a compound, C4A3H3 (cement

density notation in which: CaO = C; AI2O3 = A; H2O = H; Si02 = S)

which has little structural integrity. The formation of the C4A3H3

compound along with the disappearance of Boehmite (AH), which acts as

a binding phase, accounts for the strength loss. By contrast, the

calcined flint clay refractory forms anorthite (CAS2) when exposed to

steam. This reaction, which is similar to that occurring in earth as a result of geothermal reactions, forms a densely knit network of platelike grains. This network remains its integrity as the refractory is

cooled to low temperatures, thus accounting for the high strength of

the calcined flint-clay refractory.

Because of the inability to control both temperature and pressure in a fixed volume hydrothermal apparatus, the data described above has only

limited applicability to coal gasification situations. Therefore, two

systems were obtained that allow the temperature and pressure to be

controlled independently (figure 8) . One system contains two vessels

that can be used at 960°C and 1000 psi; the other system contains one vessel which can be used at 610°C and 5000 psi. These apparatus have

now been used to obtain hydrothermal exposure data at temperatures and

pressures that more accurately reflect conditions in coal gasifiers.

Hydrothermal experiments were conducted using two modes of operation

(figure 9). In one mode of operation the vessel was heated to the final

temperature before injecting steam to bring the vessel to the operating

pressure. In the other mode, water was injected first so that the

pressure and temperature followed the saturated vapor curve during heatup. Once the final operating pressure was achieved, steam was vented

from the vessel as required to maintain the operating pressure as the

temperature was increased to the final operating temperature. This

procedure was followed to evaluate the effect of heat-up procedure on

the strength.

30
The effect of hydrotheraal treatment on strength for Mode I operation is

shown in figure 10. The pressure for all of these studies was 1000 psi.

We note that in Mode I operation neither of the refractories studied in

this project gives any indication of strength reduction as a result of

exposure. In fact, a slight strength increase was registered for both

refractories. Similar conclusions were reached for the calcined flint

clay refractory in Mode II operation (figure 11). By contrast, the high

purity aluminum oxide refractory shows strength degradation at approximately 410°C. However, as the temperature is increased to higher

temperatures the strength is regained, and at 910°C the strength is the same as the specimens tested in Mode I operation. X-ray diffraction and

scanning electron microscopy studies indicate that the strength loss at

410°C can be accounted for by the same reaction (the formation of the

C4A3H3 compound) as occurred in earlier studies. No firm conclusion has

yet been reached on the reason for the high strengths at elevated

temperatures. However, X-ray diffraction studies indicate that temperatures

of 610®C and higher, the refractory dehydrates to form CA2 and CA, and it

is possible that a dehydration reaction is responsible for the increase

in strength at high temperatures. Thus, it appears that for the high

purity alxomina refractory, there may be a danger zone ranging from about

310 to 610°C in which strength degradation can occur in the presence of

high pressure water.

One of the reasons for using silica free castable refractories is to

prevent the transfer of silica resulting from a water hydration reaction.

In some applications this transfer results in a decrease in the efficiency

of heat transfer units as a result of silica coat formation. While it

is not certain that this reaction will be important in coal gasification

applications, it is worth reporting that hydrothermal transfer of silica

has been observed in the present set of experiments. Silica in the form

of cristobalite has been found on the cool parts of the pressure vessel;

the operating conditions (mode II) of the vessel at the time were 910°C,

1000 psi steam for 42 hours. The transfer had no apparent effect on the

strength of the refractory.

Erosion Studies

During the past quarter studies to investigate the effect of angle of

impingement on the erosion rate were continued. Measurements were

conducted on a phosphate bonded refractory using 100 mesh silicon carbide

particles. The results of this study, figure 12 can be compared with a study conducted earlier on a high purity castable alumina, figure 13.

The erosion rate measured in these figures give the weight loss from the

refractory, divided by the weight of particle hitting the specimen.

The particle velocity for these studies was kept constant at a value of

72 m/s for the 25 °C data and a value of 90-95 m/ s for 1000 °C data.

Generally, the appearance of the two sets of curves is similar suggesting

that the mechanism of erosion is the same for both types of refractories.

We note that for impingement angles ranging from 30° to 90°, there is

only a small change in erosion rate. At 15° impingement the erosion

rate appears to drop more rapidly for 3 of the 4 graphs shown in these

figures (room temperature erosion of the high alumina refractory shows

only a slight decrease in rate of 15°).

31
The rate of erosion of these castable refractories is controlled mainly

by the rate of wear of the cement phase holding the agregate particles

together. Thus, as erosion proceeds channels develop in the refractories

and when the channeling is sufficiently developed, the aggregate particles

fall from the refractory surface. The formation of channels accounts

for the relative insensitivity of these refractories to angle of impingement, because within each channel impact occurs noirmal to the cement

surface. However, when the angle of impingement decreased below a critical value, shadowing of the surface by the exposed aggregate particles

will occur resulting in a net decrease in the erosion rate. For three

of the four examples given in figure 12 and 13 shadowing appears to

become effective at angles ranging from between 15° and 30°. We have no ready explanation for the behavior of the fourth example. However, it

should be noted that channels did not form on this refractory, suggesting

that the erosion resistance of the cement phase was nearly as great as the aggregate phase.

Erosion measurements have also been made on castable refractories that

have been exposed to hydrothermal environments. This study is an extension of an earlier one, in which the erosion rate was found to bf

related to the strength of the castable after exposure to steam. For

each set of specimens prepared for strength measurements, a second set was prepared for erosion studies. Both sets were made from the same batch and given the same hydrothermal exposure. Erosion studies to date

were conducted only on specimens that exhibited high strength after

exposure. These specimens also were observed to have a relatively high

resistance to erosion in agreement with earlier studies on the same refractory. A summary of the data collected on the specimens studied is

given in table 2.

32
Table II. Erosive Wear of Hydrothermally Treated Castable Refractories

Hydrothermal

Temperature (°C)

untreated

110

310

410

610

710

910

110

310

410

610

710

910

Calcined Flint Clay

Strength

(MPa)

10.1

13.9

10.9

15.2

15.5

15.2

14.8

17.4

23.4

24.1

27.1

24.8

25.1

28.0

Erosion Rate

(mg/gm of abrasive)

20.3

13.3

13.3

16.0

14.0

16.0

13.6

18.2

9.6

14.6

15.2

9.2

10.2

11.6

High Purity Alumina Refractory

untreated

Plans ; Construction of the high pressure vessel for mechanical testing

in simulated gasification environments will be continued. First the

heating elements will be attached to the equipment and the heat zone

will be characterized as a function of temperature and pressure. Then

the pressure regulating system will be installed and checked to determine

its characteristics. Once the heating and pressure system have been

demonstrated, the load system will be installed and the operation of the

hydraulic ram, bellows and load cell will be checked using castable

refractory specimens at ambient j high and low temperatures but at pressure.

Finally the water injector will be installed and the system will be

operated with steam in the enviornmental chamber. When this check-out

scheme has been completed, the system will be operational and systematic

studies on castable refractories will be started. The system is expected

to be operational at the end of the coming quarter.

33
Exposure studies will continue on both the high purity alumina and the

calcined flint clay castable refractories. The environments to be used

will be H2O-CO2 mixtures and H20-C0-C02-CH4-H2 mixtures. With the

exception of H2S and NH3, the latter mixture will fully simulate the

coal gasification environment. As in the previous studies, a range of

temperature, pressure and exposure time will be investigated. The

dependence of strength on heat-up procedure will also be studied. X-ray

diffraction and scanning electron microscopy will be used to identify

important phase changes that occur during exposure.

In the erosion studies, work on the effect of temperatures and impingement angle on the wear rate will be completed. A study will then be

initiated to determine the effect of particle size and particle type on

the erosion rate. The particles to be used in these studies will include silicon carbide, sand and glass spheres ranging in size from

approximately 70 micrometers to approximately 1 millimeter. The size

range and the types of particles should approximate the erosion characteristics of particles found in gasifiers. Erosion studies will also be

conducted on castable refractories that have been exposed to hydrothermal

environments.

34
APPARATUS

FOR

In

Shn

TESTING

'Figure

1.

Schematic

diagram

of

high

preaaure

vessel

for

in

situ

testing.
oi

bx.e»*fn»c

agwssj

%,o
Figure

2.

External

view

of

high

pressure

vessel

and

associated

attachments.

-Figure 3* Environmental chamber assembly

^Figure

4.

Bellows

.ngsembly

u*ed

to

Igolate

the

environmental

chamber

from

the

preggure

veggel.
jTOMS

rtteapn

to

T*o7*PS

ppe

saAitouBeuffi

cp*ap«i.

«w

bi^»tms

*®»»s
'Figure

5.

Loading

fixture

for

three-point

bend

tests.
i
CALCINED

FLINT

CLAY

CASTABLE

(psi)

u) 2-

UJ

OC3

I-<

IOCUJ

Q.S

UJ

UJsK<

UJ

OC<

OCUJX

»-o

OCo

>-X c

0)e

•u

0) CO

I-I 0) XI >-l CO 4-* u

CO rH

CO CO CJ Bu

QJ cO X X 4-t O O

4-J X) c

•H

X

1—i

U-l 4-1o X

QJd

•Ha

t-HCOo

U-lO CO X CO U CO

t)0 d >.

(Dd

4-1 CO

V4O

4-J o

cOd

d M-i

QJ QJ PQ >-i X

QJd3

bO

•H

40
I
ROOM

TEMPERATURE

BEND

STRENGTH

(MPa)

HIGH-PURITY, CALCIUM-ALUMINATE CASTABLE

50 230 410 590 770 950

2,000

1,500

1,000

800

600

500

400

300

250

HYDROTHERMAL TREATMENT TEMPERATURE

Figure 7. Bend strength of high alumina castable

refractory as a function of hydrothermal

treatment

.

41

(psi)
o

42

Figure

8.

Schematic

diagram

of

hydrothermal

exposure

equipment.
TWO

EXPERIMENTAL

MOPES

Figure

9.

Schematic

diagram

demonstrating

the

two

modes

of

operation

of

the

hydrothermal

experiment.
flODE I I o•-H Ooo•-H CO

<z> O

ODor—uno•-H 4TOr—i o

CNI

c;0

•H

4-1

<TJ

V-i 01ao

(U T)OO

•o

JZ

U-tou

(D

LU

0)uD

00

44

Hydrothermal

Treatment

Temperature,
Mode

11

vdW 'HiDNaais ivanxaij aaruvaadwax wooy

M

M

<U 'ao

rC

4-1 00c

(Uuu

COco

4-i c

a)B

u

cO(U

>-l -u

COB

u

Q)

4-1 o

>-( T3 42

<4-1 C

o o

•H

4J 4J O CO

a) )>4

<4-1 0) <4-1 Cl. w o

<u

)-l 3

00

•H

[i.

45
46

Figure

12.

Effect

of

impingement

angle

on

erosion

rate:

calcined

flint

clay

refractory.
il

!

I

i

i

I

I

(3Msvaev dO w0/dw) 3ivy Noisoa]

CO

c

o

•H

cno

}-i <uc ^

o u

o

(U -u rH CJ 60 cO C t-i CO 4-1(U •w }-l c

(U CO e c

OJ -H 60 e

C 3

•H iH a CO e

•H >,

4-1 -H O U

3 U Cu

(3Aisvag\/ dO W9/0W) divy Noisoa]

44w

m

(UVj3

60 •H

Pm

-C

60

47
3. Chemical Degradation of Ceramics

a. Reactions and Transformations (F. Mauer and C. R. Robbins, 313.06)

Progress : During the past quarter, work was continued on construction

of the apparatus for x-ray examination of refractory castables under

simulated gasification conditions. The pressure vessel and goniometer

(for mounting and aligning the vessel) were completed by the MBS Instrument Shops. The specimen holder and internal heater were fabricated and

installed in the pressure vessel. All components (with one exception) are now on hand and the system is ready for assembly and calibration

runs. It was decided to use a new type of flange seal in the pressure

vessel instead of solid copper gaskets as originally planned. Delivery

of the new gaskets is expected in April.

A technician has been trained to assist in the operation of the system

and in the processing of the x-ray data. A high- temperature furnace has

been ordered to facilitate preparation and study of reference standards,

refractories and refractory components.

The elemental analysis capability of the system was used to screen reference materials by the detection of impurities. A calculator program has been written for use in converting d-spacings and intensities

of conventional powder diffraction patterns to channel numbers and

counts (peaks and backgrounds) for energy dispersive diffraction (ED)CD)

patterns. This program was used in the interpretation of the energy

dispersive patterns of reference standards shown in Figures 1-8.

All energy dispersive patterns were recorded under the following

experimental conditions:

X-ray source Target

Tube Voltage

Tube current

Tungsten

40 kVp

15 mA

Diffractometer Diffraction angle

Slits

24°(20)

1°, MR, .2“

Detector Type

Size

Bias

Resolution

Si(LO

80mm'

lOOOV

225eV

Amplifier Time constant

Gain

Baseline

Polarity

8m s 8/6. 0/1

0.04

Positive

Multichannel

Analyzer

Conversion gain

Offset

Time

1024

0

300 sec(Live)

Strip chart Vertical scale

Horizontal scale

5K/10K

1000 chan/ in.

48
The system was calibrated using the x-ray fluorescence lines of Ce, Zr,

and Ag, in addition to the W lines of the tube spectrum. The constants a and b in the equation

E = a + bx

were obtained by linear regression for use in computing the energy,

E(keV), from the channel number, x. The values obtained were a = 0.77

keV and b = 0.0354 keV per channel.

Plans ; Construction of major components, and installation of specimen

holder and Internal heater have been completed. The system can be assembled

during April and tested at high temperature. Operation will be limited

to one atmosphere of pressure until the flange seals arrive. In situ x- ray diffraction measurements (Subtask 3a-3) are expected to begin in

April 1977 as proposed initially.
CHANNEL NUMBER

Figure 1. EDXD pattern of a-Quartz (Si02).

50

J
Figure 2. EDXD pattern of CA.

51
52
I

i

I Figure 4. EDXD pattern of a-Cristobalite (Si02).

53
%

Figure 5 . EDXD pattern of A3S2 (Mullite).

54

J
I

55
%

Figure 7. EX)XD pattern of a-Al 203 ,

56
ft

Figure 8. EDXD pattern of AH (Boehmite)

I

I

i 57
b. Slag Characterization (W. S. Brower, J. L. Waring, 313.03 and I D. H. Blackburn, 313.02)

Progress : Watt and Fereday (1) measured the viscosity temperature relations ' of the ashes of a large number of British coals. From these measurements

an equation was developed to calculate viscosity at any temperature and com- position within specified limits. The important oxides in their viscosity | calculations are Si02 , Al^O^, Fe^O^, and CaO. All other oxides were grouped wi(|

MgO and ignored. ^

The Watt-Fereday equation is

7 log n = 10 M + C

2 (T-150)

where n is viscosity in poises

M = 0.00835 (SiO^) + 0.00601 (AI

2 O3

) “ 0.0109 >

C = 0.0415 (SiO^) + 0.0192 (Al^O^) + 0.0276 ^

(equivalent ^ 0.0160 (CaO) - 3.92

T is temperature in degrees Celsius. '

Tne oxides in parentheses are the concentrations of these oxides

in the melt expressed in weight precents.

To determine if this equation would be useful in describing the viscositytemperature relations for slags derived from American coals at ambient

pressures a series of synthetic slags were prepared and the viscosities

deteirmined over a range of temperature. The compositions of these slaq.s

were varied about the composition of a model Montana Rosebud Ash. The : compositions are given in Tcible 1. |

Table 1. Slag Compositions wt

.

Rosebud No. 384 No. 352 No. 360 No. 389 ! SiO^ 42.10 40.0 45.0 50 30

19.50 20.0 20.0 25 30

7.11 15.0 15.0 12 20

CaO 24.48 17.0 15.0 8 14

Na^O 0.21

K

2 O 0 . 10

MgO 5.50 8.0 5.0 5 6

Ti02 0.90

The viscosity of Rosebud coal ash is given in Fig. 1 to<^eth<T with t fi. viscosity calculated using the Watt-Fereday equatif^n. Th<- m<-.» .ur<- i in<i calculated viscosities for the other compositions in T.iiqe 1 ar- giv. 1, n. Fig. 2 and Fig. 3. The predicted viscosities seem to agr- •• re.i .ii-h 1 . well with the measured values at ambient pressure. Moasur*-meni of . i . i» will be made later on these compositions as a function of pn-ssurr '1 -t- ir..

58
We feel that fairly satisfactory predictability is possible at ambient

pressures, at least for this series of compositions, it is also reasonable

that the Watt-Fereday equation can be used as a base for predicting viscosity

relations as a function of steam pressure.

The pressure vessel to contain the viscosity apparatus has been constructed

and pressure tested and has been delivered to the Bureau.

Plans : The torsion suspension, cup rotator, heater, and angular displacement

sensor will be installed in the pressure vessel. When the internal parts of

the pressure vessel have been installed, the slag compositions in Table 1 will be used for preliminary viscosity measurements at modest steam pressures.

References

1. J. D. Watt and F. Fereday, J. Inst, of Fuel, 338 , 99 (1969).

59
o

o

60

Figure

1

VISCOSITY-TE>TERATURE

RELATIONSHIPS

OF

COAL

SLAGS

Solid

lines

are

Watt-Fereday

calculated

curves.
o

o

o

o

vO

O

o

in

o

o

o

o

cn

(sas^od O^SOT) A:jjsoDSfA 3 ot[

61

Temperature

(C)

Figure

2

VISCOSITY-TEMPERATURE

RELATIONSHIPS

OF

COAL

SLAGS

Solid

lines

are

Watt-Fereday

calculated

curves.
360

/

/

<

/

II I I II I I I

I I I I I

(sas-pod ^^8ox) /\ 8ot

62

Figure

3

VISCOSITY-TEMPERATURE

RELATIONSHIPS

OF

COAL

SLAGS

Solid

lines

are

Watt-Fereday

calculated

curves.
c. Vaporization and Chemical Transport (J. Hastie and D. Bonnell, 313.01)

Progress: A new reactor was constructed to allow for a new skimmer

design and for water cooling at a platinum-stainless steel junction

which previously failed at elevated temperatures ('^^1200°C). A new

series of calibrations are in progress with this reactor using

Na 2 S04 as a test case. Results for this salt reported on in the

previous quarterly report (Oct. 1-Dec. 31, 1976) seemed to indicate

satisfactory reactor performance for the dissociative process:

Na 2 S04 (£) = 2Na + S0 2 + O 2 However, no Na 2 S04 (g) species were observed and this is contrary to

a very recent report by Kohl et al. (1975) from Knudsen effusion

experiments. As the work of Kohl et al*^ differed from the results

of several other investigators, where Na 2 S04 (g) was not observed, we

repeated the Kohl et al.^ experiments using our Knudsen effusion

mass spectrometer system. Our results showed the presence of

Na 2 S04 together with Na, SO 2 , and O 2 , under what are believed to

be thermodynamic equilibrium conditions. Hence the presence of

Na2 S04 in the high pressure transpiration-type reactor should be

a good indication of gas saturation and overall thermodynamic

equilibrium in the reactor. A preliminary test with the newly

constructed reactor has verified the presence of Na 2 S 04 (g), as expected

for an equilibrium system, over liquid Na 2 S 04 at temperatures and total

pressures of 1300-1700 K and 290-620 Torr respectively.

Plans: Following completion of the first phase of calibrations and tests

for the new reactor, using the simple salts Na2 S 04 and NaCl , a second

phase of tests will be made. This will Involve more complex chemical

systems where reactive coal gas components such as H2 O, H2 , SO2 , and

HCl will be allowed to interact with Na2 S04 (initially). As the

thermodynamics of above mentioned species are known, then the reaction

products can be predicted and an assessment made of whether equilibrium

occurs under our reaction conditions. A new gas handling system will

be constructed for these studies. We plan to present a paper on our new mass spectrometric technique at the next annual meeting of the

American Society for Mass Spectrometry (Washington, D.C., May 1977).

*Kohl, J.F., Stearns, A. C. Fryburg, C. G. , "Sodium Sulfate:

Vaporization Thermodynamics and Role in Corrosive Flames," NASA

TM X-71641 (1975).

63
4. Failure Prevention (J. H. Smith and W. A. Willard, 312.01)

Progress ; During this quarter the Failure Prevention Information Center

received approximately 40 reports of operational malfunctions and

component failures in coal conversion pilot plants and process development units. These reports included several diagnostic failure analysis

reports from Argonne National Laboratories and Oak Ridge National

Laboratories.

These reports have been classified and evaluated for technical completeness

and accuracy. Detailed abstracts of this information have been entered

into the CCA Model 204 computerized data base management system for ease

of future retrieval and data dissemination. An update of the frequency

of failure modes which analyzes the information contained in the system

is shown in Table 1.

The Information Center has collaborated closely with Battelle-Columbus

in the preparation of the ERDA Materials and Components Newsletter.

Weekly updates of all abstracts are furnished to Battelle along with

complete copies of all significant information. During this quarter,

21 separate requests for information have been received by the Information

Center. In response to these inquiries, copies of 400 abstracts, 26

complete information items, and 48 print-outs of statistical programs

were sent out.

Five visitors who were interested in the Center's operation were briefed

on the method of operation and types of output the computerized system

is able to produce.

Five draft reports to be used for efficiently disseminating Information

from the Failure Prevention Information Center were prepared. These

reports cover operating discrepancies and component failures from the

HYGAS, SRC and Synthane Pilot Plants. The other report covers the use

of Incoloy 800 in several components and the various failure modes to

which this alloy is susceptible.

Various statistical programs have been developed for use with the data

base management system. These programs are now complete and in use. They enable the Center to perform statistical analyses on failure mode,

type of component, materials of construction, and coal conversion

processes. See Tables 2 and 3 for examples of these programs.

Plans : The information collecting phase of this task will (.>ntlnui- as more information is received on a continuing basis from the pilot pl.ints.

Visits to operating pilot plants and failure analysis laboratories an- planned to significantly augment the information collection aitiviti<s

and to get additional information on operating discrepancies and

component failures. The abstract reports that have be«-n preparod will

be thoroughly reviewed, corrections made and Issued.

64
Table 1

3/30/77

FREQUENCY OF FAILURE MODE

Cause of

Incident

No . of

Items

CO

2 HYGAS SRC Synthane Others

Corrosion

Carburization

129

12 7 3 0 0 2 General 62 3 7 8 12 32

Metal Dusting 5 3 0 0 0 2 Oxidation 8 4 3 0 0 1 Pitting 12 3 2 2 1 4 Sulfidation 30 14 10 0 6 0

Design Defect

General

48

43 6 3 12 5 17

Thermal Stresses 5 0 2 1 0 2

Erosion 64 8 6 10 16 24

Fabrication 15 4 4 0 4 3

Welding 10 2 3 0 2 3

Quality Control 18 4 3 0 6 5

see- CL 31 4 4 2 4 17

Undetermined 32 2 11 0 13 6

65
Table 2

COAL CONVERSION PROCESSES

OF ITEMS PERCENT PROCESS

7 1.96 ALL

1 0.28 BIGAS

14 3.93 BMT

10 2.80 CARBONATE

13 3.65 CLEAN COKE

1 0.28 COED

70 19.66 C02

1 0.28 CPC

64 17.97 HYGAS

1 0.28 LERC

24 6.74 LIGNITE

2 0.56 MERC

26 7.30 MISC.

2 0.56 PERC

1 0.28 RANN

2 0.56 SEVERAL

30 8.42 SRC

1 0.28 SRC-W

69 19.38 SYNTHANE

2 0.56 SYNTHOIL

1 0.28 UNKNOWN

14 3.93 WESTINGHOUSE

356 = TOTAL NUMBER OF ITEMS IN FILE

66
Table 3

COMPONENT FAILURES-ALL PROCESSES

NO OF ITEMS COMPONENT

44

742

166

32

15

23

554

27

6

22

0

38

AUXILIARY PROCESS EQUIPMENT

INSTRUMENTATION

MATERIAL EVALUATION

PIPING

BELLOWS

THERMOWELLS

PRESSURE VESSEL

GASIFIER

REGENERATOR

BOILER

PUMPS

ROTATING EQUIPMENT

THERMOCOUPLE

UNKNOWN

VALVES

67

/iBLiOGR^A^PHIC DATA FE-^800-ll >

i. TiTLli ANDSliimiLH

’’MATERIALS RESEARCH FOR CLEAN UTILIZATION OF COAL"

Quarterly Progress Report, January 1 - March 31, 1977

5. Publication Date April 1977

6. Perlorming Organization C

7. AUTHOR(S)

Samuel J. Schneider, Jr.

8. Performing Organ. Report

\ performing organization NAME AND ADDRESS

HATIONAL BUREAU OF STANDARDS

DEPARTMENT OF COMMERCE

10. Project/Task/Work Unit ^

11. Contract/Grant No.

Ev4v—x^-jSOu

12. Sponsoring Organization Name and Complete Address (Streei, ^ity. z/Py

1 Energy Research and Development Administration

i 20 Massachusetts Avenue

1 Washington, D. C. 20545

13* A ype of Htporc 2c I^crioJ Covered Quarterly

Progress Report

14. Sponsoring Agency Code

Dist. Cat. UC-90(

15. SUPPLEMENTARY NOTES

16. ABSTRACT {A 200-word or less {actual summary of mr<st si^ificant information. If document includes a significant

bibliography or literature survey, mention it here.)

This progrBss irsport covers work on inetal corrosion, metnX erosion, ceramic

defoiuiation, fracture, eroeisn, and chemical dcgra4a£ir'_n.^^ related to coal

gasification systems. This report also covers the failure avoidance program

for ERDA coal conversion pilot plants.

1'/. KtV WORDS (six to twelve entries; alphabetical order; capitalize only the first letter of the first key word unless a props name; separaipd hy semiroions) Cerataic corrosioii, cermaic erosion, ceramic fracture, che

degradation, coal gasification material, failure avoidance, metal corrosion, met;

erosion, vaporization processes

18. AVAILABILITY Qj Unlimited

19. SECURITY CLASS

(THIS REPORT)

21. NO. OF f

?C5C‘ For Official Distribution. Do Not Release to NTIS NBS will not

submit to NTIS; ERDA-FE will submit after approval.

1

1 Order From Sup. of Doc., U.S. Government Printing Office

Washington. D.C. 20402. SD Cat. No. CM

II\CL.\SS1F1ED 69

20. SECURITY CLASS

(THIS PAGE)

22. Price

1

1 Order From National Technical Information Service (NTIS)

Springfield, Virginia 221*51 UNCLASSIFIED
iliv^ -