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EA-6010-14

Dist. Category UC-90C Qqj < 7 1979

MATERIALS RESEARCH FOR CLEAN UTILIZATION OF COAX,

QUARTERLY PROGRESS REPORT

October - December 1977

Samuel J. Schneider

Project Manager

Institute for Materials Research

National Bureau of Standards

Washington, D. C. 20234

PREPARED FOR THE UNITED STATES

DEPARTMENT OF ENERGY

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

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

States Government. Neither the United States nor the United States

Department of Energy, nor any of their employees, nor any of Lheir

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

I .

1 1 .

III.

OBJECTIVE AND SCOPE OF WORK

SUMMARY OF PROGRESS TO DATE

Articles Published end Talks Presented

DETAILED DESCRIPTION OF TECHNICAL PROGRESS

J. Metal Corrosion. .

a. Constant Strain-Rate Test

b. Pre-Cracked Fracture Test

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

3. Chemical Degradation

a. Reactions and Transformations

b. Slag Characterization

c. Vaporization and Chemical Transport

4. Failure Prevention

a. Failure Information Center

b. Materials Properties Data Center

PACE

I

4

4

4

I b

1 /

32

32

33

38

40

40

44

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 longtime 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. A system has been initiated to abstract

and compile all significant operating incidents from coal conversion plants

as well as materials property and performance information important to the

design and operation of these 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 DOE and associated contractors will be provided as requested.

II. SUMMARY OF PROGRESS TO DATE

Brief Summary

1. Metal Corrosion

a. Constant Strain-Rate Test

The testing of specimens of 310 SS , 310s SS, 347 SS , 446 SS , incoloy 800,

and Inconel 671 was completed in a reducing coal gasification environment

(CO-26% ; C02 -14 . 8% ; H 2 -26%; CH 4 -10%; H 2 S-1%; H 2 0-22.2%) at temperatures

of 450°C(840°F) and 600°C(1100°F) at a strain rate of 1 X 10 6 s The

reducing environment did not seem to have a significant effect on the

mechanical properties of any of the alloy specimens tested at 430°C(840°F)

when compared to the mechanical property values of the alloy specimens

tested in the helium environment at 450°C(840°F) . The reducing environment

at 600°C (1100°F) did have a significant effect on 310s SS and Incoloy 800

by reducing the values of the mechanical properties when compared to the

data for the same alloys tested at 600°C(1100°F) in the helium environment.

The effect of the reducing environment at 600°C (1100°F) on the other alloys

did not seem to be significant. A thorough metallographi c examination of

the alloy specimens tested in helium, oxidizing, and reducing environments

at 450°C(840°F) and 600°C(1100°F) is in progress.

During the next quarter, it is planned to complete metal lographic examination of the alloy specimens. Also, it is planned to prepare a summary

of the progress to date of the constant strain rate testing technique.

1
b. Pre-Cracked Fracture Test

The thermal-elastic st ress . int ens it y analysis has been completed lor the

wedge-loaded cantilever beam specimens. These results show that because

the stress-intensity factor decreases significantly with increases in

temperature for alloys of principal interest, such as stainless steels

or Incoloys, this specimen configuration has limited applicability for

reliable testing to determine the susceptibility to environmentally

assisted stress-cracking.

More exact thermal-photo elastic stress analysis tests will be performed

on the three specimen configurations described above as well as on a notched C-shaped specimen configuration.

2. Ceramic Deformation, Fracture and Erosion

A low-alumina refractory concrete has been exposed to a 70% H 2 O

- 30% CO2 environment at temperatures of 510°, 710°, and 910°C and

at pressures of 7.5 and 15.0 MPa. The room temperature flexural

strength, compressive strength and erosion resistance of the concrete

all increased after exposure. Work is continuing on construction and

assembly of the high- temperature , high-pressure mechanical loader. A

pressure balancing unit to regulate the pressure between the inner

containment vessel and the outer pressure vessel is presently being

installed

.

3. Chemical Degradation

a. Reactions and Transformations

Over 60 energy dispersive powder diffraction patterns have been recorded

from a bar of high alumina neat cement while it was being heated in a steam - CO 2 atmosphere. Significant changes were observed, and computerassisted methods are being developed for use in completing the analysis.

During the next quarter x-ray studies of high alumina cement in various

atmospheres containing H 2 O and CO2 will continue, and the results will be

correlated with those obtained under Task 2.

b. Slag Characterization

Construction of the high pressure- temperature viscosity apparatus has

been completed and a synthetic slag has been melted in steam proving the

adequacy of the heating system under pressure conditions.

c. Vaporization and Chemical Transport

A new gas handling system has been constructed and tested. Following

resolution of a suspected reactor alignment problem, the thermodynamic

effects of H 2 O, SO 2 and O2 on Na 2 S 0 it transport will be investigated.

2
4. Failure Prevention

a. Failure Information Center

The Failure Prevention Information Center continued to enlarge its data

collection activity. Seventy-four additional reports of operating

experiences and failure analysis were received, classified, evaluated

and entered into the data base. A detailed review of operating experiences

at the Hygas plant and at the CO 2 acceptor plant was continued and will be

completed during the next quarter.

b. Materials Properties Data Center

The establishment of the work and procedures of the Center continued

with the formation of the library of contractors' reports, study of

the formatting needs for a suitable computer system, investigation of

computer data management systems, study of two series of contract reports,

and preparation and revision of summary reports.

Articles Published and Talks Presented

J. W. Hastie arranged and chaired a session on "Metals in Combustion"

at a Symposium on Metal Halide Vapors at the 152nd Meeting of the

Electrochemical Society (Atlanta, GA, October 1977).

J. W. Hastie participated in a workshop on High Temperature Science and

Solar Thermal Test Facilities (Albuquerque, New Mexico, November 1977).

J. W. Hastie participated in a workshop on High Temperature Chemical

Kinetics: Applications to Combustion Research (NBS, December 1977).

J. H. Smith, "Failure Prevention at NBS," First International Conference

on Materials for Coal Conversion and Utilization, October 11-13, 1977,

National Bureau of Standards, Washington, D. C.

J. H. Smith, "Materials Failure Analysis," 9th Synthetic Pipeline Gas

Symposium, sponsored by the American Gas Association, Chicago, 111.,

October 31 through November 2, 1977.

J. H. Smith, "Materials Failure Analysis," published in the Proceedings

of the 9th Synthetic Pipeline Gas Symposium, American Gas Association.

G. M. Ugiansky presented a talk, "Slow Strain Rate Stress Corrosion

Testing in Coal Gasification Environments," at the First International

Conference on Materials for Coal Conversion and Utilization held at NBS

in October 1977.

J. L. Waring, R. S. Roth, W. S. Brower, and C. A. Harding, "Investigation

of Calcium Aluminate Cement Phases Under High Gaseous Pressure," .Journal

of Research of the National Bureau of Standards, Volume 82, No. 3,

November-December 1977.

3
HI. DETAILED DESCRIPTION OF TECHNICAL PROGRESS

1. Metal Corrosion

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

Progress : Testing of specimens of 310 SS, 310s SS, 347 SS, 446 SS,

Incoloy 800, and Inconel 671 was completed in the reducing coal

gasification environment (C0-26%; C02~14.8%; H2~26%; CH4~10%; H2S-1.0%;

^0-22.2%) at temperatures of 450°C(840°F) and 600°C ( 1 100° F) at a strain rate of 1 X 10“^ s -

-*-. The results of these tests at 450°C(840°F)

and 6Q0°C (1100°F) are shown in Tables 1 and 2 respectively.

It was previously shown (April-June 1977 Quarterly Progress Report and

July-September 1977 Quarterly Progress Report) that an increase in

test temperature from 450°C(840°F) to 600°C (1100° F) in ultra-pure

helium environment and an oxidizing environment caused a significant

change in the values of the mechanical properties* for the alloys tested.

The same was noted for the reducing environment as seen in tables 1 and

2. This effect of increasing test temperature from 450°C(840°F) to

600°C (1100°F) can also be noted in the stress-strain curves in figures

1 , 2 , 3 , 4 , 5 , and 6

.

The effect of environment on the mechanical properties of the specimen

alloys can be noted in tables 3, 4, and 5 and also in figures 1, 2, 3,

4, and 6. The values for the mechanical properties obtained in the

helium environment (Table 3) are used as a base and the values for

the mechanical properties obtained from the oxidizing (Table 4) and

reducing (Table 5) environments are compared to that base. A significant effect caused by the environment is, at this point,

arbitrarily set as a change of + 10% in at least two of the three

mechanical property values measured. The oxidizing environment

(Table 4) had no significant effect on the mechanical properties of

the specimen alloys tested at 450°C(840°F) with the exception of

Inconel 671 which showed an increase in elongation and reduction in area while the tensile strength remained the same. The oxidizing

environment had a significant effect by decreasing the values of the

mechanical properties of specimens of alloys 310 SS, 446 SS, and Incoloy

800 when tested at 600°C (1100°F) . The reducing environment (Table 5)

had no significant effect on the mechanical properties of the alloy

*Mechanical properties — tensile strength, elongation, and reduction

in area.

4
specimens tested at 450°C (840°F) . The reducing environment did have

a significant effect by decreasing the values of the mechanical

properties of alloy specimens of 310s SS and Incoloy 800 when tested

at 600°C (1100°F)

.

Metal lographic examination of the alloy specimens tested in helium,

oxidizing, and reducing environments at 450°C(840°F) and 600°C (1 100° F)

have been completed but not evaluated.

Plans : To further evaluate the results of testing in the oxidizing

and reducing environments and prepare a summary of the results obtained

to date by the constant strain rate test technique.

5
Table 1

Alloy Tests at 450°C(840°F) at a Strain Rate of 1 X 10

b

s

* in the

Reducing Environment*

Alloy Tensile Strength Elongation RA

MPa psi % %

310 SS 598 86,700 35.6 60.2

310s SS 513 74,400 38.8 69.9

347 SS 590 85,500 18.4 59.7

446 SS 574 83,200 21.0 58.0

In 800 551 79,800 34.3 70.5

In 671 676 97,900 38.0 39.3

*CO-26 %, C02 -14.8%, H 2 -26%, CH4 -10%, H 2 S-1.0%, H 2 0-22.2%.

Table 2

Alloy Tests at 600°C (1100°F) at a Strain Rate of 1 X 10~ b s

1 in the Reducing Environment*

Alloy Tensile Strength Elongation RA

MPa psi % %

310 SS 362 52,500 (-39%)**

310s SS 336 48,700 (-35%)

347 SS 426 61,700 (-28%)

446 SS 160 23,200 (-72%)

In 800 353 51,100 (-36%)

In 671 448 64,900 (-34%)

*CO-26%

,

C02 -14 . 8%

,

H2 -26%

,

CH4 -10%,

19.9 (-44%)

30.3 (-22%)

14.8

(-20%)

49.5 (+236%)

32.7 (-5%)

16.3 (-57%)

H 2 S-1.0%, H, 0-22. 2%

23.4

(-61%)

33.8

(-52%)

58.3 (-2%)

83.3 (+144%)

61.7 (-12%)

16.8 (-57%)

**Note : The numbers in parentheses show the percent change in

the mechanical property values with an increase in test temperature

from 450°C(840°F) to 600°C(1100°F)

.

6
Table 3

Alloy Tests in Ultra-Pure Helium Environment at a Strain Rate of 1 X 10“6 s - -*-

Alloy Temp

°C

Tensile

psi

Strength

MPa

Elongation

%

RA

%

310 SS 450 87,300 602 37.9 64 .

6

600 53,400 368 19.9 28.8

310s SS 450 75,100 518 38.9 63.7

600 63,400 437 3] .9 42.8

347 SS 450 82,300 568 18.8 65.2

600 65,300 451 13.4 52.2

446 SS 450 85,000 586 17.3 57.0

600 22,000 152 62.0 86.0

In 800 450 76,200 526 37.3 72.1

600 67,700 467 37.1 60.1

In 671 450 98,600 680 32.8 37.7

600 60,300 416 16.1 lb. 3

7
Table 4

Alloy Tests in Oxidizing Environment* at a Strain Rate

of 1 X 10-6 s _1

Alloy Temp Tensile Strength

°C psi MPa

Elongation

%

RA

%

310 SS 450 84,200 581 (-3%)** 35.4 (-7%) 55.1 (-15%)

600 50,300 347 (-6%) 14.0 (-30%) 21.6 (-25%)

310s SS 450 75,200 519 (0) 38.6 (-1%) 65.1 (+2%)

600 54,500 376 (-14%) 32.8 (+3%) 43.9 (+3%)

347 SS 450 85,700 591 (+4%) 17.0 (-9%) 60.2 (-8%)

600 66,600 460 (+2%) 14.5 (+8%) 46.0 (-12%)

446 SS 450 80,000 552 (-6%) 19.3 (+12%) 61 .4 (+8%)

600 15,800 109 (-28%) 34.7 (-44%) 88.3 (+3%)

In 800 450 78,900 544 (+3%) 32.6 (-13%) 65.8 (-9%)

600 53,400 368 (-21%) 29.4 (-21%) 49.4 (-18%)

In 671 450 97,100 670 (-1%) 38.6 (+18%) 45.3 (+20%)

600 57,600 397 (-5%) 17.5 (+9%) 20.7 (+27%)

*00-11.6% ; C0 2 - 15.4%; H 2 - 13.0%; CH4 - 10% ; h 2 s - 1.0%; h 2 o

- 49%

**The numbers in parentheses in table 4 show the percent change in the

mechanical property values caused by the oxidizing environment when

compared to the results obtained for the same alloys tested in the

ultra-pure helium environment (table 3).

8
Table 5

Alloy Tests in Reducing Environment* at a Strain Rate

of 1 X 10-6 s -1

Alloy Temp Tensile Strength Elongation

°C psi MPa %

RA

%

310 SS 450 86,700 598 (-1%)** 35.6 (-6%) 60.2 (-7%)

600 52,500 362 (-2%) 19.9 (0) 23.4 (-19%)

310s SS 450 74,400 513 (-1%) 38.8 (0) 69.9 (+9%)

600 48,700 336 (-23%) 30.3 (-5%) 33.8 (-21%)

347 SS 450 85,500 590 (+4%) 18.4 (-2%) 59.7 (-8%)

600 61,700 426 (-6%) 14.8 (+9%) 58.3 (+12%)

446 SS 450 83,200 574 (-2%) 21.0 (+21%) 58.0 (+2%)

600 23,200 160 (+5%) 49.5 (-20%) 83.3 (-3%)

In 800 450 79,800 551 (+5%) 34.3 (-8%) 70.5 (-2%)

600 51,100 353 (-24%) 32.7 (-12%) 61 .7 (+3%)

In 671 450 97,900 676 (-1%) 38.0 (+16%) 39.3 (+4%)

600 64,900 448 (+8%) 16.3 (+1%) 16.8 (+3%)

*C0-26%

;

co 2 - 14.8%; H 2 - 26%; CH4 - 10%; H 2

S - 1%; H

2 0 - 22.2%

**The numbers in parentheses in table 5 show the percent change in

the mechanical property values caused by the reducing environment

when compared to the results obtained for the same alloys tested in

the ultra-pure helium environment (table 3).

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15
b. Pre-Cracked Fracture Test (J. H. Smith, iiz.Ol)

P rogress : The thermal-elastic stress intensity analysis has been completed

for the wedge-loaded cantilever beam specimens. These results show that

because the stress-intensity factor decreases significantly with increases

in temperature for alloys of principal interest, such as stainless steels

or Incoloys, this specimen configuration has limited applicability for

reliable testing to determine the susceptibility to environmentally assisted

stress-cracking. This configuration should prove to be suitable for assessing

the susceptibility to environmentally assisted stress cracking of non-metals

or metals with a relatively low coefficient of thermal expansion that can

be loaded with a wedge made of stainless steel.

Preliminary photo-elastic stress analysis experiments showed that a compression loaded double-edge notched specimen should prove to be suitable

for use as an elevated temperature test specimen. By compensating for the

decrease in elastic modulus with increase in temperature by differential

thermal expansion of the loading fixture and the test specimen, a constant

stress intensity with temperature should be obtained. However, the limitation of this specimen is that a more limited length of crack growth is

possible than with the wedge loaded double cantilever beam specimens.

Preliminary photo elastic stress analysis tests were also conducted on a curved single edge notch beam specimen loaded as a bimaterial specimen.

This specimen configuration appears to be suitable for elevated temperature

tests and will permit testing for cracks propagating in the through

thickness direction of piping and pressure vessels.

PJ ans : More exact thermal-photo elastic stress analysis tests will be

performed on the three specimen configurations described above as well

as on a notched C-shaped specimen configuration. Based on these tests,

thermal -elastic stress analyses will be conducted to determine the

stress-intensity factor on the optimum specimens. This thermal elastic

stress analysis will then be extended to the elastic-plastic stress

range typical of metals used at elevated temperature.

16
2. Ceramic Deformation, Fracture, and Erosion (E. R. Fuller, Jr.,

S. M. Wiederhorn, J. M.

Bukowski, C. R. Robbins,

and D. E. Roberts, 313.05)

Progress : Exposure studies on a low alumina (56%) refractory concrete

in a 70% H2 O - 30% CO 2 environment were completed this past quarter. In this investigation, pre-f ired*ref ractory concrete specimens were initially

heated to the exposure temperature In an argon environment at atmospheric

pressure. Once temperature equilibrium was reached, H2 O and gaseous CO 2 were metered into the exposure vessel to give the desired gas mixture

and environment pressure. Samples were exposed to the H2 O - CO 2 environment at temperatures of 510°, 710° and 910°C and at pressures of 7.5 and

15.0 MPa. After an exposure period of 90 hours, the specimens were

allowed to cool to 500°C at which point the exposure environment was slowly vented. By venting the exposure environment at 500°C, the formation

on cool-down of low-temperature reaction products and their effects on subsequent room temperature mechanical property measurements were minimized.

The room temperature flexural strength, compressive strength and erosion

resistance for the low-alumina refractory concrete all increased after

exposure to the 70% H 2 O - 30% CO 2 environment (Table 1) . X-ray diffraction

analysis of samples exposed to the 70% H 2 O - 30% CO 2 environment indicated

the formation of CAS 2 ** at the expense of calcium aluminate phases

(Table 2) . It was found that the amount and crystallinity of CAS 2 seemed to increase both as a function of exposure temperature and environment pressure. As in earlier hydrothermal studies on the same lowalumina refractory concrete, it is the formation of the CAS 2 phase on exposure that is responsible for the increased strength and erosion

resistance

.

Exposure studies have also been initiated for a high-alumina (94%)

refractory concrete in a simulated coal gasification environment. The

ambient gas mixture being used is 40% H2 O, 25% H2 , 20% CO, and 15% CO 2 which gives a gaseous environment of H2 O, CO, CO 2 , H 2 and CH4 at the

temperature-pressure exposure condition. Room temperature mechanical

and mineralogical properties of exposed refractory concretes is presently in progress. Experimental observations have indicated mass transport of calcium from the refractory concrete being deposited as calcium carbonate (aragonite and vaterite) in cooler regions of the

exposure vessel.

Work has continued on the development and the construction of the high

pressure vessel for the mechanical testing of refractory concretes in

simulated coal gasification environments. The load system has been

*1010°C - 5 hr.

**Cement Notation: C = CaO ; A = AI 2 O 3 ; S = Si 02 J H - II 2 O

17
installed, and the operation of the hydraulic ram, bellows, and load

cell has been checked by breaking castable refractory specimens at

ambient temperature-pressure conditions. The resulting tests showed an excellent correlation in strength between specimens broken in the hightemperature, high-pressure mechanical loader and specimens broken on a commercial universal testing machine. The installation of a pressure

regulating system which will balance the pressure between the inner

containment vessel and the outer pressure vessel has begun. Minor

modifications of the solenoid control valves used in the regulating

system were found to be necessary in order to ensure rapid response to

pressure imbalances. These modifications are presently being made and

should be completed in a short length of time.

In a continuation of earlier work on the erosion of castable refractories,

the erosion rate of a high density, calcined flint clay refractory has been

investigated. Mean particle velocities of 72 m/ s and 93 m/s were used

in this study at temperatures of 25°C and 1000°C, respectively. As in

previous work, erosion studies were conducted with 100 grit (150 pm)

silicon carbide particles. The results of this study, figure 1, are compared with data obtained on a high alumina castable refractory,

figure 2, and a phosphate bonded castable refractory, figure 3. The

erosion rate is expressed in terms of mg of refractory eroded per gram

of particles actually hitting the refractory surface. In all three

cases, the rate of erosion was insensitive to impingement angle for

angles ranging from 30 to 90°. For impingement angles of less Lhan 15°

a sharp decrease of erosion rate is suggested by some of the data. In

absolute terms, the erosion rate measured at each angle of impingement

was comparable for the three refractories studied, factors of less than

two difference in the erosion rate being considered not significant.

The similar appearance of the three sets of curves suggests a common mechanism of erosion for the three refractories.

As discussed in earlier reports, the rate of erosion of castable refractories is controlled mainly by the rate of wear of the cement holding

the harder aggregate particles together. As erosion proceeds, channels

are developed in the cement that bounds the aggregated particles, see figure 4, and when the channels have grown around the particles to a sufficient extent, the aggregate particles fall from the surface of the

refractory. Channel formation in castable refractories occurs because

the aggregate particles are much more erosion resistant than the cement

matrix. The relative influence of cement versus aggregate wear can be

demonstrated by conducting erosion measurements on the aggregate phase

alone. A study of this type was conducted on two grades of high density

aluminum oxide: one grade contained a 3-5 urn grain size; the other

18
contained a 30 urn grain size. Studies were conducted at temperatures of

25°C, 500°C and 1000°C over a velocity range ^ 40 m/s to 120 m/s. The

results shown in figure 5 may be compared with similar results on two

types of castable refractory, figure 6 , both of which contained aluminum

oxide as the aggregate phase. We note that at equivalent velocity, the

erosion rate of the refractories is approximately 1000 times that of the

aggregate particles. It is for this reason that the erosion is due

primarily to wear of the cement phase. It is also worth noting that the

erosion rate of the aggregate is insensitive to temperature. This

behavior differs from that of the castable, where erosion is temperature

sensitive

.

Channel formation in castable refractories accounts for the relative

insensitivity of erosion rate to angle of impingement, since within each

channel, impact occurs normal to the refractory surface, figure 4.

However, when the angle of impingement decreases below a critical value,

the cement phase will be protected by the aggregate from direct particle

impingement and the rate of erosion will decrease. This process has

been termed "shadowing," and because the erosion resistance of the

aggregate particles of a castable is so much greater than that of the

cement phase, the process of "shadowing" should occur commonly in

refractories, and should provide an explanation for the shape of the wear versus impingement angle curves.

A model for "shadowing" was developed during the last quarter of this

project. The model assumes that the surface aggregate particles can be

approximated by spheres (figure 7) that are completely resistant to

erosion, so that only the cement phase between the spheres is eroded by

direct impingement of erosion particles. As the angle of impingement,

a, decreases, the exposed area, S, of cement between particles decreases.

From geometric arguments, figure 8 , it can be shown that S is related to a and the relative aggregate particle radius R by the following formula:

S = 2 (sina-R) , where it is assumed that the mean spacing between particles

is 1 , so that all results are obtained in terms of the unit spacing

between aggregate particles. As the angle of impingement is decreased,

a second geometric factor comes into play: the number of areas, S,

exposed to the erosion beam increases so that the total available area,

A, for erosion is given by the following formula: A = 2(l-R/sina). If

it is now assumed that for any given mean particle velocity, the erosion

rate is proportional to the exposed area of cement, then the erosion

rate, E, is given by the following formula: E/E 90 = 2(l~R/sina), where

Egg is the rate of erosion at an impingement angle of 90°

.

Theoretical curves for the relative erosion rate, E/E 90 , are plotted in

figure 9 as a function of impingement angle for various values of R. It is noted that for small values of R, the predicted curves are similar in

19
shape to the experimental curves. This finding suggests that the angular

dependence of the erosion rate is determined by the size and spacing of

the largest aggregate particles in the refractory. In the present

study, the ratio of the aggregate particle size to aggregate separation

distance would be expected to be about 0.1. This conclusion is qualitatively in agreement with the appearance of eroded surfaces studied in

the present investigation.

Plans : Exposure studies will continue on both the high-alumina and the

low-alumina refractory concretes in simulated coal gasification environments. Room temperature mechanical property measurements will be made

and correlated to microstructural and mineralogical changes occurring in

the concretes on exposure.

Construction of the high pressure vessel for mechanical testing in

simulated coal gasification environments will be continued. The pressure

regulating system will be installed and checked-out. On satisfactory

operation of the regulating unit, the water injector will be installed

and tested. At this point the mechanical loader should be operational,

and systematic studies on refractory concretes can begin.

20
Impingement Angle

Figure 1. Effect of impingement angle on erosion rate: calcined flint

clay castable* particle velocity = 72 m/s (2b°C) and 93 m/s

(1000°C)

.

21
UJ>

CO<

ocCQ<

Li. o

s:

UJH

&

o

ooO

C£

LlJ

Impingement Angle

Figure 2. Effect of impingement angle on erosion rate: high purity

alumina castable refractory; particle velocity = 72 m/s (25°C)

and 93 m/s (1000°C).

22
Impingement Angle Impingement Angle

Figure 3. Effect of impingement angle on erosion rate: phosphate

bonded castable refractory; particle velocity = 72 m/s (25°C)

and 93 m/s (1000°C).

23
Figure 4. Schematic diagram of channel formation in castable refractories,

a = original, b = eroded surface; “ = angle of impingement.

24
Figure 5. Erosion rate of high-density aluminum oxide ceramics as

a function of temperature and particle velocity.

25
Erosion

Rate

(mg/gm

of

Abrasive)

Particle Velocity (M/s)

Figure 6. Erosion rate of two different castable refractories containing

aluminum oxides as an aggregate phase.

26
Figure 7. Model of the process of "shadowing," in which the aggregate

particle protects the underlying cement.

27
Figure 8. Geometric details of the model used to estimate the role of

shadowing on the erosion process.

28
Figure 9. Theoretical prediction of relative erosion rate as a function of impingement angle.

29
Table

1.

Room

Temperature

Mechanical

Properties

ofa

Low-Alumina

(56%)

Refractory

Concrete

after

Exposure

toa

70% H20-

30%

C02

Environment.

(Specimens

prefired

to

1000°C - 5

hr.)

<D CU O > C -H

cd CO u co CO Cl •H ,0

to cd cu pi Huo GO

too

Cl w 600B

00C

0)Cl

4-1 . co nj

<U> ' •H

CO

to

<U

ClCU6oo

uf ro

CO +|

CO ec2o

LTl

CO PC2

inOm

LO o

vOm

oo

oo cn m m

o> CSI cn +|

CM

•<r mo m

»-H CM **1

vO -0"

crs co, uo +|

mm

cnm ^ +1

vO 00 m +1 &

00c

CU

Cl o

uo

m vo -j oo oo co

r~- O'* in <r eg o

co o

+1

O

>H +|

OO

nj +|

toCi3X

CU

r-H

£-• £ O H,

>H + |

CTl CM

CT> i—I CM O- CO

O

I''.

h cn <r co co o •- + I r~* + 1

i-i + I oCGO

CJ

cu CU

Ci c G 3

CO CO o CO cu CU X Cl w PC

CU

cu Ci Ci 3 3 Cl

CO cO o Ci a a) X cu w B

cu H

CJ oOm

CJ CJ o o O O

rH rH

On

30

mg/gm -

mg

of

specimen

eroded

per

gm

of

abrasive

hitting

the

specimen

surface.
Table

2.

X-Ray

Diffraction

Analysis

ofa

Low-Alumina

Refractory

Concrete

after

Exposure

to

70% H2O30%

CO2

Environment

(Phases

Listed

in

Apparent

Order

of

Abundance) .

CO

u

#> ~ u

(U <u QJ s-j'

4-J CM 4-J r~\ 4-J CN ->.

ol •H <3 •H 3-4 *H <3 34 Pm rH O rH 4-J rH CJ 4-J § CM 03 0) 03 s—

cp 43 - -O r. -O 0 < O <3 O C id) O <3 d) • cj 4-J 1 4-> 1 r—s 4-J 4-J 1 4-J m CO a CO a 3-1 -H co a -h

rH * •H •H 4-10 •h

a

CM 3-1 > 3-1 PH 34 1 x

<3 CJ CM CJ CM T3 CJ CM "O

CJ CP CP CM -H CP -H

QJ - <3 •> <; <2

m 1 <3 >4

M CM CJ (MU CJ

H CM CJ

H 3 <2 CP CP CP

co 1 CO CO CO

co

a < <3 <3

a)w

Pm <u

4-1

(1) •H u rH - 1 34 3 03 CM CM 4-J CO X> <3 CP CP 0 O 1 <2 <3 QJ a 4-J a CJ CJ 4-J X CO •H w •H - #N 1 E

3-1 CU QJ / s d) >1 O 4-1 4-J 1 34 4-J TJ

•H -rH r-v 4-1 •H -H

n iH

H 34^ rH 34 CM 0) 0) 4-J 03 H

C/3 -O CM P ^ dJ -n

CO

O <2

O CM 4J

O 1

03 <3 4-J CJ 4-1 <J -H 4-J p_, CO co cj a CO 34 •H i •H £ •H 4-J

3-i CM 3-i 1 XJ 34

m CJ CP CJ <2 -rH CJ CM • <2 1 34 < - CJ -an 1 CJ

CM CM CM CP CP CP

CO co co < <3 <3

QJ

3-4 CP CP CP 3 QJ pH P4 Pi

co

a |~r! as as 0 -H 1 CL H O 0 0 X on 03 ON w

a)

343 tH

4-1

O

03 3-1 0 0 0

>-i CJ 4-1 rH 1—1

rH

d) 0 3 m

CL

O

B

O

a) H
3. Chemical Degradation of Ceramics

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

Progress: A bar of high alumina neat cement has been heated for 20 days

in an H2 0-C0 2 atmosphere at temperatures and pressures up to 1000°C and

1000 psi. The composition of the atmosphere was approximately 80% H2 0

- 20% C0 2 but varied considerably. In all, over 60 energy dispersive

powder diffraction patterns were recorded. They indicate that significant reactions between the test specimen and the atmosphere occur. The

hydration of CA2 , CA, and A to form compounds in the series C 3 AH5 , AH 3 , AH, and C4 A 3 H 3 , as well as the subsequent dissociation of these hydrates were observed. Because of the inherent low resolution of the energy

dispersive powder diffraction patterns, changes are not as obvious as they would be in conventional powder patterns and individual reactions

cannot be followed by visual inspection of the recorder charts. Fifty

of the patterns have been recorded in digital form on punched paper tape

so that computer assisted methods of interpretation can be used. We are now engaged in developing the software needed to process the digital

data. At present it takes approximately 12 hours to read the 50 tapes

into the computer for storage in a disc file and many problems arise

because of flaws in the tapes. A method for transmitting the patterns

directly to the computer is being sought so that the punched paper tape can be eliminated. Available plotting routines obtained are capable of

plotting only 500 points. These are being modified so that the 1024

points recorded in each of our patterns can be plotted. Programs will

then be written to subtract from each ordinate of a pattern the corresponding ordinate of the previous pattern and to plot the difference.

The difference plot will be a sensitive indicator of changes in the

intensities of diffraction lines. Plots will also be prepared to show

the trend in intensity in selected channels corresponding to the diffraction peaks in the patterns prepared previously using pure reference

standards. The number of counts in each of 5 diffraction peaks will be

plotted for all of the 50 patterns in succession, and this will be

repeated for each of the phases of interest. The plots will be useful

for estimating the relative rates of transformation under various conditions. Other modes of analysis, as well as improved methods for presentation of data for reports are under consideration.

Additional components for recording process variables during x-ray

studies have been received and will be installed during the next quarter.

Plans : Development of computer programs and improvements in the data

logging equipment should be completed during the next quarter. Installation of additional equipment for controlling temperature and recording

process variables is also expected to be completed. X-ray studies of

high-alumina cement in various atmospheres containing H2 0 and C02 will

continue, and the results will be correlated with recent work done under

Task 2.

32
b. Slag Characterization (W.S. Brower, J.L. Waring, C.A. Harding,

313.03 and D.H. Blackburn, 313.02)

Progress : The first prototype of the high pressure-temperature

viscometer has been completed. Since the last reporting period

the following have been added to the apparatus: new, platinum

heater for melting slag, crucible for holding slag, pedestal to

support crucible, shaft to rotate pedestal, suspension to be

deflected, a sight port for viewing at ambient pressure.

After solving some difficult contact resistance problems, a synthetic slag was melted in high pressure steam, proving the

adequacy of the heating system under pressure conditions.

—

Platinum Heater

The platinum heater (Figure 1) was fabricated from sheet .040"

thick. It consists of a hollow right cylinder 2" I.D. and 4"

long. To this cylinder at 180° were welded two large platinum

tabs approximately .120" thick, 3 1/2" long x 4" high. These

tabs are clamped into the electrodes. Another cylinder of alumina

was cast around the platinum cylinder. The combination was fired

at 1200°C for 24 hours. The outside circumference of the alumina

cylinder was reinforced with platinum wire. This assembly was encased in refractory bricks which were shaped to accommodate

the platinum-alumina cylinder. This additional brick insulation

serves to insulate the heater and to minimize convective cooling

by the steam on the thermocouple. This cooling effect was found

to cause a temperature measurement problem in early experiments.

Crucible and Spindle

The platinum crucible used to contain the molten slag is 1 1/2"

O.D. x 2 1/2" long with a 1/32" wall thickness. On the bottom

of the crucible were welded tabs which form a cross pattern.

These tabs are embedded into notches at the top of the alumina

spindle. The alumina spindle is in turn clamped at the opposite

end into the stainless steel rotating shaft. These precautions

are necessary to prevent accidentally contacting the crucible with

the heater. As an extra precaution a thin alumina liner is inserted

between the rotating platinum crucible and the platinum heater.

Motor Driven Shaft

The stainless steel rotating shaft which supports the alumina spindle

passes through the bottom flange. This shaft is sealed with two

ethylene propylene 0-rings. Outside the vessel the shaft is cooled

33
to prevent degradation of the O-rings. This cooling is accomplished

by passing water through a jacket surrounding the shaft. The shaft

is attached to the motor drive transmission by a universal coupling.

Sight Port and Suspension

Viscosity is to be measured in the following manner. The slag is

placed in a crucible and melted, the bob is then immersed in the

melt and the steam pressure is increased while the temperature

is held constant until an appropriate temperature-pressure

equilibrium is achieved. At this point the crucible is rotated

and the angular deflection of a calibrated torsion member is

observed. This deflection is proportional to the viscosity.

To make this type of measurement two modifications to the viscometer

were made. The first was the introduction of a sight port so that

the bob can be seen when immersed in the molten slag. The second

modification is a method to lower the torsion suspension-bob to

the desired height. To accomplish this a reciprocating shaft was introduced through a blank flange in the top of the vessel. The

seal between the shaft and the flange is a viton-O-ring.

Problems

After assembling the various components and making preliminary

heating experiments, some problems became apparent. When the system

was operating at 1055°C and 130 psi steam, the platinum heater was

using 18.48 KVA or approximately 4600 amps. With high currents

and low voltages the various interfaces along the current path

became extremely important. Originally the adjacent copper buses were made approximately flat and parallel and each mating surface

was tinned. Voltage losses in the leads were noted as much as

60%. Some of this excessive loss was due to copper heating along

the resistance path. The resistance of copper increases approximately

35% as the temperature increases from 20°C to 80°C. To reduce the

effect of poor contacts, tin foil was sandwiched between all butting

copper surfaces. The losses were measured and found to be approximately 15%. Additional water cooling was added at the junctions

along the power leads. This cooling should keep the leads at

approximately room temperature as the pressure vessel is heated.

Results

A synthetic slag with the composition SiO 42 wt%, Fe 0., 25 wt%,

Na

20 15 wt%, K 0 5 wt%, MgO 5 wt% , A1 C> 3 3 wt% and CaO 5 wt% was melted at I045°C and 135 psi of steam. After quenching the

molten material under steam pressure and removing the crucible

34
from the pressure vessel the melted material was found to have

formed a smooth concave meniscus. A significant weight gain of

8 mol % of H 9 0 was detected in the glass melt. This fused

material was^then reheated in air at 1000°C for approximately

30 min and found to foam (Figure 2) . This is a clear indication

that water was indeed present in the material. In this experiment

no attempt was made to determine the maximum amount of water the

molten slag can accommodate. However, it is clear that, in con- junction with viscosity measurements, data should be obtained

concerning the maximum amount of H..0 incorporated in the molten

slag versus time and temperature, viscosity among other properties

should be a function of the amount of water in the melt.

Plans : During the next quarter the viscosity of the previously

melted synthetic slag composition will be measured in steam over

a modest pressure range, from 15 to 100 psi. It will also be

necessary to determine the time necessary to saturate the melt

with respect to steam, this will be accomplished by making a series of viscosity measurements as a function of time at constant

temperature and pressure until the viscosity becomes constant.

When some insight is gained on the kinetics of steam solubility

in the molten slag, then the viscosity measurements will be ex- tended to the design pressure of the vessel (y 300 psi)

.

35
Platinum Heater

TOP VIEW

SIDE VIEW

Figure 1. Platinum resistance element for heating slag container

in steam.

36

SCALE: 5/8 IN =1 IN
37
c. Vaporization and Chemical Transport (J. Hastie and D. Bonnell,

313.01)

Progress : A new gas handling system, incorporating three mass flow was

constructed, calibrated and tested using H 2 O, O2 and SO 2 gases. Two of

the flow controllers are of stainless steel construction and the third

of monel. Gas flows between 0.4 - 5000 cc/min can be generated through

these meters. This system is capable of handling any gaseous component

(including corrosives) present in a coal gasification process and the

composition of four of the constituent gases can be varied independently.

Gas ratios varying from 0.5 to 100% are possible to a precision of better

than 1% in the absolute concentration of any of the component gases. The

system also enables rapid changes in mixture composition to be made during

a series of experiments. Hence data can be obtained over a wide range of

coal gas compositions for each substrate sample studied.

As a test of the gas handling system and the reactor's capability to

faithfully sample a simple heterogeneous reaction system pertinent to

corrosion in coal gasifiers, we initiated a study of the interaction of

H2 O vapor with Na 2 SC>4 liquid at temperatures of 800 - 1400°C and an H2 O

partial pressure of 150 torr in an atmosphere of argon carrier gas.

Under these conditions we expect, from the JANAF Thermochemical Tables,

the following reactions to occur:

Na2 S04 (£) = Na2 S04 (g)

Na2 S04 (£) + H2 0 = 2NaOH + S02 + \ 02

and 2NaOH = (Na0H) 2.

However no mass spectra characteristic of the presence of NaOH, (Na0H)2

or Na2S04 (g) in the sample beam were found. As material deposits were

noted in cooler regions of the reactor at the end of each experimental

run, we know that some vaporization occurred. The inability to detect

any vapor species by the molecular beam sampling process suggested a sudden breakdown in the reactor performance. To check the reactor's

ability to handle and identify NaOH we introduced a pure sample of

NaOH(Jl) to the reactor. Mass spectra were obtained for the NaOH and

(NaOH) 2 species at a temperature of 835°C. However the beam intensities were about a factor of 200 lower than expected, based on the known vapor

pressure of NaOH and the calibrated sensitivity of the reactor-mass

spectrometer system. That is, the NaOH pressure observed equals 1.3 x

10 5 atm as compared with the expected equilibrium pressure of 8.1 x

10 4 atm. Also, several attempts to monitor the vaporization of Nacontaining species from a complex alkali-silicate mixture (components:

Na20 /Si02 /Na2 S 04 /Na2 C03 /H2 0 ) at temperatures in the region of 1000°C were unsuccessful. We believe that the sampler was defective during

all of these experiments. The apparent drastic reduction in sample

beam intensities could be due either to a change in the sampling cone- skimmer alignment during heating or to a change in the orifice geometry

due to corrosion or deposition of nonvolatile material around the orifice.

These possibilities are currently under investigation.

38
Plans: The possible misalignment of the high temperature reactor with

the mass spectrometer will be investigated. if alignment changes during

the experiment are observed the skimmer oritice will be enlarged to

reduce the criticality of skimmer - sampling cone alignment. Also the mass spectrometer will be repositioned during experimental runs to

optimize the ion source - skimmer alignment.

Due to the reactor performance problems encountered during the last

quarter we still need to establish that the system is capable of

faithfully sampling relatively simple heterogeneous systems. Of

particular concern here is whether the sampling process disturbs the

equilibrium composition that is expected for the simple systems using

our operating conditions. If we can demonstrate that the sampling

process does not appreciably alter the composition of the vapor

sample, then any non-equilibrium phenomena found in subsequent studies

of complex coal-gas-ceramic-slag-ash systems can be confidently

attributed to the intrinsic properties of the particular chemical system

under investigation. As was mentioned in our original proposal, a decision on whether the pressure range for study should be extended beyond

the present 1-2 atm capability will be based on whether or not the coal

gas-substrate reactions are intrinsically kinetically controlled. The

modeling phase of our research program cannot readily be extended to actual

coal gasifier pressures if kinetic phenomena are significant at the experimental conditions and if the experimental pressures differ from those In

the gasifier. On the other hand if the reactions attain equilibrium at

atmospheric pressure then they can be assumed to be at equilibrium at the

higher pressures of coal gasifiers and thermodynamic models can be used.

Tests will therefore be resumed on the effect of HO, SO, and 0 on alkali - metal transport. Reactions such as:

Na 2 S 04 ( 2.) - 2Na + S02 + 0? and

Na2 S04 (£) + H2 0 = 2NaOH + S02 + | 02

will be monitored at constant temperature and variable partial pressures

of H2 0, S02 and 02

. If the systems and the sampling process are at equilibrium then the equilibrium constants should be independent of

partial pressure.

39
4. Failure Prevention

a. Failure Information Center (J. H. Smith, R. C. Dobbyn and W. A. Willard,

312,01) (W. S. Brower, 313.03)

Progress : During the quarter the Failure Prevention Information Center

received 74 reports of operational experiences and components and materials

failures in coal conversion pilot plants and process development units.

This number includes several diagnostic failure analyses from Argonne

National Laboratories and Oak Ridge National Laboratories. To date, the

percent contribution of information items received from different coal

conversion processes is shown in Table 1.

These reports have been classified and evaluated for technical completeness

and accuracy and discrepancies have been resolved. Detailed abstracts of

this information have been entered into the Center's computerized data

bank. A recent update of the frequency of failure modes, which analyzes

all information in the system, is shown in Table 2.

The Information Center continued to aid Battelle-Columbus in their

preparation of the DOE Materials and Components Newsletter feature on failure experiences. Weekly updates of all abstracts are furnished to

Battelle together with complete hard copy of certain reports when requested.

During the quarter, the Center furnished 22 updated summaries and 38

complete reports.

The Information Center also handled 23 other requests for information

during the quarter. In response to these inquiries, copies of 1,476

abstracts and several draft reports were transmitted. In addition, nine

visitors to the Center were briefed on its scope, operation and future

plans

.

Additional reports required to complete the history of operating experiences

at the Hygas plant have been obtained. This operation experience history

will identify all components failures and operating events that caused

disruption of the planned runs, and significant repairs or modifications.

This review is being constructed from the available operating reports.

Direct contact with operating pilot plants, process development units and

failure analysis laboratories continued. The BCR-Bigas plant submitted

their first 16 failure reports and the Synthane, Hygas and Westinghouse

processes continued their interaction with the Center.

Two presentations were made and one paper was published by J. H. Smith

describing the operation of the Failure Prevention Information Center.

R. C. Dobbyn participated in workshop discussions on recommended practices

for evaluation of metals in high temperature, carburization environments.

40
Plans : The information gathering phase of this project will continue as more information is obtained from operating plants, process development

units and failure analysis laboratories. Expanded interaction with

other pilot plants and coal conversion technology centers is planned and

will be completed as time permits. The operating experience history of

the Hygas plant being constructed from the available operating reports

will be completed.
Table 1

COAL CONVERSION PROCESSES

NO. OF ITEMS PERCENT PROCESS

7 1.44 ALL

1 0.20 BIGAS

1 0.20 BIOMASS

38 7.83 BMI

10 2.06 CARBONATE

19 3.91 CLEAN COKE

1 0.20 COED

73 15.05 CO 2

2 0.41 CPC

2 0.41 EXXON

3 0. 61 GFERC

67 13.81 HYGAS

1 0.20 LERC

23 4.74 LIGNITE

19 3.91 MERC

31 6.39 MISC.

1 0.20 ORNL

3 0.61 PERC

1 0.20 RANN

2 0.41 SEVERAL

34 7.01 SRC

4 0.82 SRC-W

106 21.85 SYNTHANE

4 0.82 SYNTHOIL

1 0.20 UNKNOWN

31 6.39 WESTINGHOUSE

485 + Total number of items in file

42
Table 2

NUMBER OF REPORTED INCIDENTS OF FAILURES

IN COAL CONVERSION PLANTS *,**

FAILURE MODE ANALYSIS

FAILURE MODE co

2 HYGAS

PROCESS

SRC SYNTHANE OTHER TOTAL

Corrosion 48 32 11 25 63 179

Aqueous 0 2 0 0 3 5 Carbur izat ion 10 2 0 0 5 1

7

Metal Dusting 4 0 0 0 3 7 Oxidation 4 3 0 0 5 12

Pitting 3 5 3 6 9 26

Sulfidation 16 11 0 7 4 38

General 11 9 8 12 34 74

Stress-Corrosion 6 5 5 5 32 53

Chloride 4 5 2 4 17 32

Other 2 0 3 1 15 21

Manufacturing Defect 14 10 13 22 37 96

Design 6 4 13 12 27 62

Fabrication 4 3 0 4 3 14

Quality Control 4 3 0 6 7 20

Equipment Malfunction 6 10 3 7 13 39

Overheat 6 10 3 4 11 34

Overstress 0 0 0 3 2 5

Erosion 7 7 11 21 38 84

Stress/Temp Failure 1 6 1 7 15 30

Creep 0 1 0 0 3 4 Fatique 0 2 0 4 10 16

Thermal Stress/Shock 1 3 1 3 2 10

Unknown 4 11 0 22 16 53

* Incidents reported to NBS Failure Prevention 1 nf ormation Center

- Sponsored by DOE

** Operating times and levels of reporting vary with each plant

DATE: January 3, 1978

43
b. Materials Properties Data Center (H. M. Ondik, T. A. Hahn, 313.06,

and I. J. Feinberg, 312.01)

Progress : The newly-established Materials Properties Data Center has

the responsibility for designing and maintaining a data bank containing

properties of materials for use in fossil energy applications. The

program of the Center should provide for more rapid transfer of evaluated

laboratory data and technological information, obtained by DOE-supported

materials research, to designers of systems, materials researchers, and

operating plants. The initial sources of information to be entered in

the data bank are DOE contractors' reports of test data. Data from

other sources will be added as appropriate. The data in the contractors'

reports will be evaluated and summarized so as to provide the users with

as much hard data in as brief a form as is possible. The data management

system is being designed to be compatible with the Failure Prevention

Information System, and to provide for appropriate search capabilities

which will yield complementary information from both data banks. The

information in the materials properties data bank will be made available

to DOE and the fossil energy community in a variety of ways —reports,

handbooks, and by direct query of the Data Center. Designing suitable

means of distributing the information is listed among the duties of the

Center

.

During this first quarter the effort of the Center has been concentrated on establishing the basic operations of the Center. A library of

the contractors' reports has been set up and will be expanded as more reports are written by and received from the contractors. The investigators have been studying the backlog of reports (which were catalogued

earlier) to identify the type of information contained in them. The

nature of the work requires a computer data management system which is

open-ended in order to provide for the addition of new types of information as well as possible multiple entries from different sources for

similar information. The system must have a matrix-type storage to

provide for combination searches on varying sets of items so as to be

responsive to users' needs and answer a variety of questions. There are package programs available with the necessary capabilities offered by

various commercial groups. These groups are highly competitive and care

must be taken to choose the best system. The system must be capable of

handling numerical and textual information. Possibilities for storing

and retrieving information in graphical form have been investigated and

the flexibility available in terms of software and equipment is very

encouraging. Enough of the data are in graphical form to make this

feature desirable, even necessary.

The investigators have worked on specific sets of contractors'

reports (one for refractories, one for alloys), studying and preparing

evaluated summary tables and information statements. These first sets.

44
chosen somewhat randomly as test situations, have been valuable in

providing necessary learning experience, indicating areas of activity in

which our evaluation effort needs more detailed definition, and providing

test examples of the format to be used in summarizing the reports. The

summaries have been revised and new ideas and opinions have been formed

by the investigators. Upon approval by DOE they will form a pattern for

the summarizing of the rest of the reports. A catalogue file of the

materials studied by the contractors is being prepared. Preliminary

checks of the Oak Ridge Technical Information Center data bank have been

made and differences found in comparing the list of reports in the DOE

office files with the references cited in the TIC files.

Plans ; Upon approval by DOE of the format and content of the first

summary reports, further similar summaries of other contract work will

be prepared and a means of distribution suggested to DOE. Catalogueing

of the various materials being studied by the contractors and the designing of the computer file to contain the materials property data will

continue. A full check of the ORNL TIC data base will be made.

45
.