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Dat e

o f

Issue :

May

UFg

CYLINDER

198 3

3/4

HOMOGENIZATION

STUDY

-

EXPERIMENTAL

WITH

A

10-TON

CYLINDER

K/PS—449

DE84

RESULT

011589

S. H. Park Systems and Equipment Technology Process Support Division

Union Carbide Corporation, Nuclear Division Oak Ridge Gaseous Diffusion Plant 1 Oak Ri,dge, Tennessee „

DISCLAIMER

This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency thereof, nor any of their

employees, makes any warranty, express or implied, or assumes any legal liability or responsi- ' bility 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. Refer- ence herein to any specific commercial product, process, or service by trade name, trademark,' manufacturer, or otherwise does not necessarily constitute or imply its endorsement, recom- mendation, or favoring by the United States Government or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the

United States Government or any agency thereof.

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5/6

TABLE OF CONTENTS

ABSTRACT

INTRODUCTION

INSTRUMENTATION AND PROCEDURE

General

 

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9

 

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10

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10

Q

Experimenta l .Design

12

Test .

16

RESULTS

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ACKNOWLEDGEMENT

DISTRIBUTION

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27

29

31

7/8

ABSTRACT

The UFg cylinder homogenization process has been investigated experimentally with a 10-ton cylinder. A specially modified cylinder

equipped with sampling probes and temperature sensors was filled with essentially equal amounts of three different assay materials. The cylinder was then heated in an autoclave with saturated steam for

Samples were drawn from each of four sampling ports for

11 hours. Temperature measurements indicated that solid UFg existed in the cylinder for 5 hours, and the assay mixing pattern during this period was fairly localized. Large scale mixing of the different assay materials followed after the complete melt down of the solid UFg due co a large temperature gradient in the liquid. The temperature gradient decreased to less than 1°F/ft after 11 hours of heating; henceforth, the mixing motion by liquid convection practically ceased. The test results indicated that the variance of assay samples, at any given time, were never smaller than the variance of the spectrometer measurements during the entire test period and, hence, it can be concluded that the cylinder never achieved absolute homogeneity. The definition or requirements for homogeneity of a UFg is beyond the scope of this report; however, since the analysis for assay of a cylinder is considered to be accurate to 0.1%, this would seem to be a minimum requirement. The assays at the four ports were within 0.1% of.each other after 8.5 hours of heating and within 0.05% after 11 hours of heating. Two liquid samples were taken at the end of the test through the valve. The average assay value of these was 2.1743% 2 3 U which was 0.02% off from the theoretically calcu­ *

13 hours.

lated value.

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o

9

INTRODUCTION

In the daily operation of tne uranium toll enrichment process, sampling of a cylinder to determine its assay is an important task. This process is also time consuming since it involves heating the cylinder for a sufficient amount of time to ensure that the contents are in a homogeneous state in terms of assay. In the U.S. enrichment pro­ cess, the heating of the cylinder is conducted in an autoclave with saturated steam. The procedure adopted at the Oak' Ridge Gaseous Diffusion Plant (ORGDP) is to place a cylinder in an autoclave in the

afternoon and heat it overnight, followed by sampling the next' morning. The assay value determined by the sample then, represents the assay of

the cylinder. This heating 1 time, 18 hours or

be sufficient to ensure assay homogeneity in the cylinder. All indica­ tions would evidence that it is a sufficient amount of time for a cylinder to reach assay homogeneity; however, there existed strong needs for information on the minimum time requirements for a given size of cylinder to reach assay homogeneity under autoclave operating conditions and how the variation of operating conditions might affect the time of heating. This information is needed to determine the feasibility of preparing a cylinder for sampling within an 8 hour shift and also in helping to establish an international standard for the cylinder sampling procedure. There have been several attempts in the past to answer these questions. One recent study conducted by R. F. Smith* at the Paducah Gaseous Diffusion Plant (PGDP) showed that a 14-ton cylinder reached assay homogeneity in 12 hours. The study was conducted with nine cylin­ ders which were spiked with different assay material of known amounts. The cylinders were then heated and sampled at various time intervals. One major drawback of this method was the sampling technique which involved stopping the heating process and rotating the cylinder. This interrupted the melting and convective, mixing motion of UFg inside the cylinder and created additional large scale mixing by turning the cylinder. The present study was designed to investigate the assay homo­ geneity process with minimum disturbances of 1 the mixing process-in order to obtain unbiased data. The two objectives of the study are:

longer, may or may not

1. Determine the minimum time for a 10-ton cylinder to reach assay homogeneity.

!: 2. Determine a correlation between temperature and assay

i, variations

in the liquid

UF 6 during the heating period.

i,

'

■-■

f.The first objective could be readily achieved by assay sampling of the cylinder. This, however, would not provide information on the effect of changes in cylinder size and autoclave operating conditions on the minimum time requirement to obtain homogeneity. It was decided that this information could best be obtained by developing a numerical mociel

♦Smith, R. F., Steam Bath Cycle Required for Isotopic Homogeneity of c 14-Ton UF 6 Cylinder (U), KY-556, Union Carbide Corp., Nuclear Div. ,

Paducah Gaseous Diffusion Plant, June 17, 1968. UNCLASSIFIED.

 

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of thermal convection currents in the cylinder. The model would be constructed to match known temperature gradients in the cylinder which could be correlated to assay gradients. In order to meet this objec­ tive, it was essential to obtain the variation with space and time of the temperature and assay of the UFg in the cylinder.

It was paramount that these parameters be obtained with minimum interference of the heating and mixing motions which required substan­ tial changes to the sampling techniques that had been employed in the past. , This was accomplished by providing four sampling lines which penetrated the autoclave and the cylinder so that -Samples could be taken at any time without opening the autoclave or rotating the cylinder. The space variation of temperature/assay was obtained from the positioning of the probes in the cylinder/ and the time variation was acquired by sampling at various times during the heating period.

< INSTRUMENTATION AND PROCEDURE

GENERAL

''

As stated above, one of the requirements to accomplish the objec­ tives of the experiment was to obtain data with minimum disturbance to the UF 6 contents. This required two basic changes in the method of" autoclave operation:

1. The test'cylinder, once placed in the autoclave, would not be rotated or tilted. V,, The heating process would not be stopped during the test.

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2. The temperature and assay would be monitored continuously

,J throughout the heating

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The experiment was conducted, with a 10-ton cylinder. The cylinder was modified to accept three temperature/assay probes and one pressure tap. The probes, described in detail in report K/PS-452*, consist h of 1-inch diameter steel pipes, 4 feet in length, which contain five tem­ perature sensors and one assay sample port; one probe contains two sampling ports. The position of these probes, shown in Figure 1, indi­ cates the relative position of the \sample ports. The cylinder contained 15 temperature sensors, four sampling ports, and one (pressure trans­ ducer. With this'-i instrumentation, it was possible to monitor temperature/pressure continuously and draw samples without interfering with the heating process-; The overall scheme of the test was to heat the cylinder with three different assay materials of known amounts and sample until the assay of the samples reached the calculated value of the mixture. Unfortunately, the assay of the samples could not be deter- ; mined instantaneously, so it was necessary to take samples over a suf-

'-• *Branam,

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A., UFg Homogenization Study Sample Probes, (U),

K/PS-452, Union Carbide Corp., Nuciear ; i uiv. , T O be issued at oak Ridge Gaseous Diffusion Plant. UNCLASSIFIED.tt

S1

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S2

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T3()AB

T4()

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DWC . NO . K/G-S3

|U)

S1,S2, S3 -TEMPERATURE/ASSAY

O TEMPERATURE SENSORS

A ASSAY SAMPLE PORT

-

-

PI, P2 - PRESSURE TAP

Figure 1 SCHEMATIC DIAGRAM OF THE TEST CYLINDER

12

ficient time span to ensure that the cylinder reached the homogenous state.

EXPERIMENTAL DESIGN

The cylinder was loaded with three different assay materials of almost equal amounts, as shown in Table 1.

Table 1. Summary of the Feed Materials

J>

Material

No.

1

2

3

ip

wt

wt

Assay

Assay

%

%

235

235 o

o

Amount

lbs

2.6098

2.6098

6,752

2.1759

6,750

1.7394

6,767

Each assay material'was fed into the cylinder followed by a minimum of 3 days of cooling to solidify the material. This was to minimize

mixing during the feeding process and to create the desired stratifica­ tion of assays. The choice of three assay materials was made to reduce

the

the previous fill. The 2.6098 wt percent 235 a ma t e rial was fed first, followed "by 2.1759 and 1.7394 wt percent ^S y material, respectively. With this feeding, the,.theoretical assay of the mixture was 2.17471 wt

time of each fill and i minimize the amount of melting and mixing with

percent 235 u%

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The ideal situation would be to monitor the temperatures and sample

for assay continuously, but it was physically impossible to manage at

this

J The temperatures were monitored every 10 minutes while

samples were drawn every hour. The longer sampling time span was dic­ tated by the sampling sequence adopted for this experiment. The sampling system, shown in Figure 2, consisted of a probe with a sample port, copper tubing, and valves to transfer the"sample to the sample tube, and auxiliary systems for dumping UFg and cleaning the lines.

There were four identical systems in the experiment. All the lines were

heated with-, heat utape to prevent solidification of UF g .

The major

sampling operations included flushing lines with liquid UFg to the dump tank before trapping samples. The',»trapped material was then transferred into the sample tube. The amount of UFg taken in each tube was approxi=^

mately 10 grams•

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Figure 3 and Figure 4 picture the test cylinder with its instrumen­ tations and sampling panel.

TO 1423 EVACUATION SS SYSTEM

NITROGEN

PCV

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DWG. NC . K/G-S2-236R1

AUTOCLAVE

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10 TON

FEED

CYLINDER

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XS 3

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GLASS

FEP TEFLON SAMPLE TUBE

£'

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DUMP TANK

- Figure 2

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PHOTO NO. K/PH-BZ-41Z2

Figure 3 TESTCYUNDER IN AUTOCLAVE NUMBER 1 WITH INSTRUMENTATIONS

Figure 4 SAMPLING SYSTEM PANEL

PHOTO NO. K/PH«t2-442f

(u)

<■■

16

TEST

The test was conducted at the K-1423, Toll Enrichment Facility, in a specially modified autoclave. The sample lines and thermocouple wires were installed through flanges. The sampling system assembly was installed on the floor level so that liquid flow would be enhanced by the combination of pressure differential between the cylinder and the dump tank and the gravity force. Besides the 15 thermocouples inside the cylinder/ there were 17 thermocouples on the external surface of the cylinder and the autoclave wall to monitor their temperature variation during the heating period. The test was conducted on December 13, 19S2.

Before closing of the autoclave, the test cylinder was spiked with 473 grams of Cr02F2 and 58 grams of MoFg by Analytical Chemistry Department personnel for investigation of chemical distribution between the phases» These chemicals of known amount were to be used as soluble traces.

The autoclave temperature setting was at 220°F.

RESULTS

Since there were three different assay materialsi in the cylinder/

the position

of each relative to the temperature sensor ( and/ par­

ticularly to the sampling ports at various 'times, was important in interpreting the test results. Figure 5 shows the schematic of the relative positions of these materials in solid and liquid phases ,at the triple point. If the materials were not mixed«during the feeding period/ sample ports A, C, and D would be in the '2.6098 wt percent 235 U regime and port B would be in the 2.1759 wt percent ,.j 235 U regime

when the "UFg melts. All the temperature sensors recorded the solid/liquid UFg temperatures except T1, located 1/2 inches from the internal surface of the cylinder,, which measured the UFg vapor temp­ erature. The probe S3, which was located in the middle of the cylinder, might represent most closely a two-dimensional representation of the phenomena occurring in the cylinder. The temperature profile of this probe, plotted in^cFigure 6, reveals some interesting facts about the behavior of UFg during the heating period. The first noticeable fact was the complete melt down time approximately < 5 hours after steam was admitted to the autoclave. The temperature gradient between the sensors during the solid-liquid phase period^ remained large and decreased rapidly after complete melting^ of the solid. The cross-over of temperature profiles between sensors T4 and T5 after 3 1/2 hours of heating resulted from the solid UFg movement toward the bottom of the cylinder. A rapid liquid mixing period followed the complete melt down of the solid' because of the large temperature gradients and slowed as the temperatures approached uniformity.

The temperatures of the liquid approached a uniform value approxi­ mately 9 hours after heating began and the temperature gradient between sensors was less than 1°F/ft. This indicated that thermal mixing of the fluid had ceased for all practical purposes.

,

17

ASSAY LEVEL OF FEED MATERIAL

O TEMPERATURE SENSOR POSITION

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A ASSAY SAMPLE PORT

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^TJ

T2

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DWG. NO. K/G-83-110S

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SOLID AT

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RELATIVE POSITIONSOF FEED MATERIAL AT DIFFERENT PHASE

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TIME OF HEATING, hr

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Figure 6 TEMPERATURE PROFILE OF PROBE S3

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DWG. NO. K/G-B3-1B07

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Figure 7 shows the temperature profiles of S1 and S3 in order to examine horizontal as well as vertical variations of the temperature in the cylinder. The temperature profile of the probe S1 agreed well with that of S3 even though S1 was located at the end of the cylinder. The only measurable differences occurred in the liquid/solid regime. The cylinder surface measurements showed that the average temperature of the end plates were relatively lower than the side wall during this period. This is reflected in Figure 7 where a lower solid UFg temperature was measured at S1 than S3. > Overall, it might be concluded that the three- dimension effact on the temperature profile during the heating period was minimized.

^

The relative shape and position of solid at the planes S1 and S3 is shown in Figure 8 as n function of time. The one-di.Tiensional represen­ tation can be pictured in two dimensions as disks with no thickness at planes S1 and S3. The disks maintain a constant diameter for 1 hour and 20 minutes until the solid starts to melt and the diameter begins to diminish at plane S3. The melting at plane S1 begins 10 minutes later, but occurs at a slower rate as indicated by the larger diameter disk S1 compared to S3. The slower melting rate at S1 is caused by the lower temperature and heat input at the end of the cylinder which is a < con­

sequence of the location of the steam lines that extend along the length of the cylinder. The uneven melting fashions a contoured dumbbell shaped solid in the cylinder which is held in position by the convex ends until

the center at plane S3 breaks^ after 3 1/2 hours. The discontinuity

of

these curves between 3 1/2 hours and 4 1/2 hours of heating could

be

explained due to the fact that the solid piece remained between the tem­ perature sensors of T4 and T5. t .

It was concluded prior to the test that samples should be obtained

in the early time period of heating to provide information on the mixing motion, with large temperature gradients. Consequently, it was planned to obtain samples after the complete melt down of solid which was

assumed'> to be 2 to 3 hours after - the steam was admitted to

autoclave. However, it was found that the time required for melting was much 'longer- than expected. Therefore, it was determined during the test to initiate >sampling at 2 1/2 hours after the steam was applied, even though solid UFg still existed in•the system. Because of the existing solid phase, only two samples could be obtained from the four sample ports in the first sampling period. The next sample period yielded four samples, as did the following nine sample periods. In all, 42 samples were analyzed by mass spectrometry according to an experimental design* which assured a fair comparison of the four ports within each time period. There were 3 to 6 determinations per each sample which resulted in an average of 4.57 determinations per sample. The statistical results of the sample, as analyzed by K. L. McCormick*, are listed in

the

*K. L. McCormick, Union Carbide Corp., Nuclear Div., Oak Ridge

Gaseous Diffusion Plant, letter '

UNCLASSIFIED.

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Park, March

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1983.

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2

3

4

TIME OF HEATING, hr

5

Figure 7 TEMPERATURE PROFILES OF PROBES S1 AND S3

OWG. NO. K/G-83-1506

(U)

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3

TIME OF HEATING, hr

DWG.

NO.K/G-83-2010

(U)

Figure 8 SOLID UF 6 SIZE AND POSITION DURING THE HEATING PERIOD

22

11

Table 2. The results are also plotted in Figure 9, and can be cate­ gorized into three different regimes of mixing. The first regime covered the first 5 hours of heating when the cylinder contained both solid and liquid UFg. In this regime, the assays of each sample ports were dictated by the movement of solid UF 6 , and liquid mixing. The second regime of mixing occurred from 5 to 9 hours after heat was

applied when large scale mixing motions existed in the liquid UFg. The

last' '-regime prevailed after 9 hours and

was characterized by very little

mixing motion. This last regime coincided with the period when the tem­ perature gradient throughout the cylinder was small.

//

The mixing process of the solid/liquid regime, which lasted for 5 ,hours, was the most difficult process to understand. The assay results from the initial samples indicated that mixing had already occurred because they differed from the assays of any of the feed materials. However, the assay at C was still the highest, which indi­ cated that most of each material fed into the cylinder remained in its relative position. The decreasing assays of A, B, and C in the next 3 to 4 hours could be explained by a chunk of solid UFg, which consisted of low and medium assay material, slowly sinking to the bottom of the cylinder, and mixing with the higher assay materials that existed in that location. The lower assay existing at A compared to C during this

period, could have resulted from excessive mixing when the materials were fed into the cylinders and more melting and mixing occurred at the end than the middle of the cylinder because of the close proximity to the

valve. The mixing in the 4 hours following completion of solid

melt down was produced soley by the convective motion of the 'liquid UFg which developed from the temperature gradient. This large scale or rapid mixing was enhanced by comparatively large density differences in the liquid. As the temperature gradient decreased with time, the degree of mixing motion subsided in direct proportion. The three different mixing regimes are depicted again in Figure 10 by the maximum difference in assay between samples at each sample time which is normalized to the mean value and plotted as a function of time. The plot shows three dif­ ferent patterns; increasing differences followed by fast decreasing values before reaching an almost flat pattern of small differences in sample assays. The increasing portion of regime coincided with the solid/liquid regime where localized melting and mixing of UFg created large assay differences between^ports. The peak of this regime coin­ cided with the complete melt down time of the solid UFg. The fast decreasing regime in the next 4 hours corresponds to the liquid mixing regime which was followed by a regime of greatly reduced mixing. The external variance of assays between ports was never smaller, than the internal variance during the test and absolute homogeneity of the con- . tents was never achieved. Obtaining complete homogeneity in a cylinder would require an infinite time and is not feasible, but a degree of homdgenization is needed. The current methods'for determining the assay of cylinders is not considered to be more accurate than 0.1%. If this amount of variation in cylinder assay is considered to be adequate for homogenization, then it was achieved in the test after 8.5 hours and a variation of less than 0.05% was achieved after 11 hours of heating.

feed

23

Table 2. Summary Statistics of the Experimental Data

Hours

Port

2.5 B

C

3.5 A

B

C

D

-,

4.5 A

B

C

D

5.5 A

B

c

D

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6.5 A

B

C

D"

7.5 A

B

C

D

8.5 A

9,5

B

C

D

A

B

C

D. m ' : v .

 

Standard

 

Average

Deviation

2.2063

0.000075

2.2612

0.000072

2.1735

0.000111

2.1918

v 0.000132

2.2706

0.000284

2.1831

0.000164

 

0

 

2.1988

0.000161

2.1374

0.000080

2.2246

0.000017

2.1829

0.000167

2.0871

0.000079

2.0936

0.000043

2.1999

0.000081

2.2121 rj

0.000176

2.1784

0.000106

2.1776

0.000104

2.1717

0.000075

2.1817

0.000076

2.1799

,0.000039 "

2.1757

0.000076

2.1698

0.000102

2.1766

0.000147

2.1765

0.000055

2.1754

0.000102

2.1749

0.0 00025

2.1744

0.0 00063

 

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,

 

2.1758

* 0.000077

't

2.1755

0.000121

2.1748

0.0 00022

2.1754

'■ 0.000173

•24

Table 2. Summary Statistics of the Experimental Data (continued)

Hours

Port

Average

10.5

A

2.

1759

B

2.

1757

C

2.

1746

D

2.1758

11.5

A

2.

1756

B

2.1754

C

2.

1748

D

2.

1750

12.5

A '

2.

1756

B

2.

1755

C

2.

1749

D

2.

1757

Standard

Deviation

0.,000177

0.,000156

0.000167

0.000104

0.,000119

0.,000090

0.,000162

0.,000094

1

0.,000083

0.,000105

0.,000133

0.,000089

 

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2.30

 

C

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2.20

A.

A.

A.

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B

B

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TIME OF HEATING, hr

Figure 9 VARIATION OF ASSAYS DURING THE HEATING PROCESS

MEAN VALUE

SPREADASSAY

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VARIATION OF ASSAY DEVIATION IN THE CYLINDER WITH TIME

27

The measured cylinder pressure was plotted in Figure 11 wi-th calcu­ lated pressures based on liquid and vapor- temperatures. The measured values were higher throughout the experiment which indicates the existence of the light gases in the system.

CONCLUSION

This report contains the experimental results of the study with a 10-ton' cylinder. The complete melt down time of the UFg in the cylinder with 220°F autoclave control temperature was about 5 hours. The largest^-;, temperature gradient existed af the end. of complete melt down of solid UF 6 and the temperature gradient decreased to less than 1°F/ft in ^ 9 hours of heating time. The assay mixing process was strongly dependent on the tenperature gradient in the cylinder. During the first " 5 hours of heating, the mixing process was fairly localized with the existence of solid UFg in the liquid." In the next 4 hours, however, the mixing process became most active as a result of the convective motion in the liquid which was induced by large temperature gradients in the liquid UFg. The temperature gradient decreased to less than 1°F/ft after 9 hours of heating. The main mechanism of any further mixing from this point was probably diffusion which is about two orders of magnitude smaller than achieved from the convective motion of liquid UFg. " The

,

<,

i) spread of>'i- /; assay values between ports was reduced

to

0.1% after

8 1/2 hours of heating and,,to 0.05% after 11 hours. The accuracy of the

Jl assay values determined was _+ 0.055%. Hence, it was assumed that the ->" :

'J>J UFg reached its assay homogeneity at 11 hours of heating even though the external variance was never smaller than the internal variance during the entire test period. The relationship between the assay and the tem­ perature of UFg obtained during this experiment will be used as a basis in constructing a numerical model with which the effect of the variations of physical and operational conditions on the' minimum time ,., scale of homogeneity can be investigated. t

MEASURED

DWG. NO.

K/O-83-IB04

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BY SATURATED LIQUID TEMPERATURE

=8=8=8=© =

=8

BY SATURATED VAPOR TEMPERATURE

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MEASURED

 

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CALCULATED BY VAPOR TEMPERATURE

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CALCULATED BY LIQUID TEMPERATURE

10

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5

6

10

11

Figure 1 i

-

COMPARISON OF CYLINDER PRESSURES - MEASURED AND CALCULATED VALUES

29/30

ACKNOWLEDGMENT

> '

The author wishes to acknowledge the many who contributed to the successful completion of this test. Special recognition should be given to J. O. Dodson and the entire Toll Enrichment personnel where the test was 1 performed. The experience of the Analytical Chemistry personnel, who handled the UFg samples, was crucial to the success of the project as well as the safety aspect. The author would also like to express his gratitude to D. L. Gray and J. L. Patton who participated in the sampling r as well as J. H. Vance for his continuous involvement in the project.

31

Administrative Offices Thomas, W. F.

DISTRIBUTION

Separation Systems Division Riepe, R. C.

Capacity Expansion Program Dykstra, J. Gamble/ J. F. Sternberg, E. o.

Computing Technology Division Beard, B. Kirkpatrick, J. R.

Engineering Division Kellogg, D. R. Parsons, J. A. Trotter, T. C.

Health, Safety and Environmental Affairs Division Golliher, W. R.

Operations Analysis and Planning Division Bradbury, J. T. Davis, W. Younkin, J. M.

Operations Division Dodson, J. 0. Forbes, R. J. Legeay, A. J./Peterson, C. H. Shoemaker, J. E., Jr.

Y-12 Plant Whitehead, H. D.

Goodyear Atomic Corporation Linville, W. E. Manning, R. E. Mentges, C. A. ,,Neely,R. S. Sandman, R. R. Woltz, F. E.

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Paducah Plant Breidert, E. C. Burnett, W. A. Lille, C. D. Loveland, C. w. Smith, R. F. Walter, C. W. ^ Zerby, CD . ^\

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