measurement of dwpf glass viscosity -final report/67531/metadc701893/m2/1/high... · temperature...

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WSRC-RP-99-01053

Measurement of DWPF Glass Viscosity - Final Report

by

J. R. Harbour

Westinghouse Savannah, River CompanySavannah River Site \

Aiken, South Carolina 29808

T. B. Edwards

R. F. Schumacher

R. J. Workman

DOE Contract No. DE-AC09-96SR18500

This paper was prepared in connection with work done under the above contract number with the U.S.Department of Energy. By acceptance of this paper, the publisher and/or recipient acknowledges the U. S.Government’s right to retain a nonexclusive, royalty-free license in and to any copyright covering this paper, alongwith the right to reproduce and to authorize others to reproduce all or part of the copyrighted paper.

*-.*-. .

WESTINGHOUSE SAVANNAH RIVER COMPANYSavannah River Technology Center

WSRC-RP-99-O1O53-TLRev. O

January 4,2000

M. N. Brosee, ManagerDefense Waste Processing Facility

Attention: W. D. Kerley, 704-S .. .

Task Initiato~ R. E. Edwards, 704-25S

MEASUREMENT OF DWPF GLASS VISCOSITY - FINAL REPORT (U)

The attached report details the results of a scoping study funded by the DWPF for the measurement of meltviscosities for simulated glasses representative of Macrobatch 2 flank 42/51 feed). The driver for this taskwas the fact that Macrobatch 2 glasses had predicted viscosities very close to the upper limit of 100 poise at1150°c.

A significant accomplishment of this work was the establishment of an in-house capability for measuringglass viscosities at 1150°C. This Harrop, high-temperature viscometer measures viscosity as a function oftemperature with a very small amount of glass (-6 grams). This enables SRTC, and consequently DWPF,to obtain viscosity data within a reasonable time for relatively low cost. Several WCP glasses weremeasured and compared with results from previous measurements by Sharp-Shurtz. In addition, CELS(Corning) and PNNL measured viscosities of some of these glasses as part of this study. The resultsrevealed that SRTC’S measurements were - 10% higher than measurements by CELS and Sharp-Shurtz,but close to those of PNNL. With this knowledge, it is now possible to measure glass melt viscosities in-house and obtain useful, approximate values of melt viscosity at 1150°C.

The limited results obtained from this study on simulated Macrobatch 2 glasses (with and without uranium)reveal that uranium may increase melt viscosity in this compositional region. For uranium-bearing glasses,predicted viscosities from the measured compositions appear to be less than the measured viscosity values, .whereas for glasses without uranium, the predicted viscosity tends to be less than measured. PNNL andCELS measurements support SRTC’S results with these glasses (PNNL measured the uranium containingglasses while CELS measured the glasses without uranium). Further work will be required to determinewhether this effect is real.

If you have any questions about the results contact J. R. Harbour at 5-8725 or T. B. Edwards at 5-5148., I

E. W. Holtzsch&terImmobilization Technology Section

..

WSRC-RP-99-O1O53

Revision 0

DISCLAIMER

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This report has been reproduced directly from the best available copy.

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Available electronically at Mp:hww.doe.govlbridgeAvailable for a processing fee to U.S. Department of Energy and its contractcm, in paper, from:U.S. Department of Energy, Office of Scientific and Technical Information, P.O. Box 62, OakRidge, TN 37831-0062,phone: (865) 576-8401fax: (86S) 576-572Sernail: reports@ adonis.osti.gov

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iv

WSRC-RP-99-O1O53Revision O


INTRODUCTIONThis report details the results of a scoping study funded by the Defense WasteProcessing Facility (DWPF) for the measurement of melt viscosities for simulatedglasses representative of Macrobatch 2 (Tank 42/51 feed). The driver for this task

* was the fact that Macrobatch 2 glasses had predicted viscosities very close to theupper Iimit of 100 Poise [1, 2]. Therefore, one objective of this scoping study wasto gain insight into the adequacy of the viscosity model in the compositionalregion of interest for Macrobatch 2. As part of this objective, glasses werefabricated using depleted uranium to determine whether uranium has an effect onglass viscosity at 1150”C. Uranium is not considered in the current viscositymodel.

A second, major objective of this task was to determine the viability ofdeveloping a measurement technique for glass viscosity at SRTC. The benefits ofestablishing this measurement, capability at SRTC are (1) a faster turnaround ofviscosity results (2) lower cost for the data by keeping the work scope withinSRTC, and (3) use of onIy a small amount of glass (-6 grams) for eachmeasurement. The small sample size is important at the bench-scale experimentallevel since it enables SRTC to measure many more glass samples, therebyimproving the quality of the results and conclusions.’

The results of the initial viscosity measurements using the SRTC high-temperature viscometer were included in an Interim Report [3], and these valuesare repeated here for completeness. This Final Report focuses on (1) the qualityof the data generated at SRTC and (2) on the comparison of the SRTC viscosityresults with recent results from Corning (CELS) and the Pacific NorthwestNational Laboratory (Pm) and with previous results from Sharp-Shurtz (SS).The CELS, PNNL, and SRTC results were determined using samples of the samebatch glasses.

RESULTSSRTC Viscometer. The setup and establishment of a Harrop, high-temperatureviscometer at SRTC has been described in an internal report [4]. This unit usesapproximately 6 grams of glass, which is considerably less than the amount usedby CELS and PNNL. CELS required 700 grams per viscosity measurement andPNNL required 200 grams for each viscosity measurement. Two crucible/spindlesets (Set A and Set B) were used for these measurements. This allowed for oneviscosity measurement per day, since it takes - 1 day to clean the crucible andspindle. Set A was calibrated using the NIST 717a borosilicate glass standard.This NIST glass is significantly more viscous than DWPF-type glasses with aviscosity close to 2000 Poise at 1200°C. For comparison, the normal range forDWPF glasses is from 20 to 100 Poise at 1150”C.

1 Smalkr samples are of particular advantage when working with uranium-bearing glasses.

1


Due to the high viscosity of the NIST 717a glass, it was decided to measure theviscosities of the HM, Purex, and Batch 1 WCP glasses. The melt viscosities forthese glasses had been previously measured by SS, thereby providing anindependent measure of glass viscosity for glasses in the range of interest forDWPF.

.Experimental. The melt viscosity was measured according to GTOP-3-1 11,Rev.O. The glass density for each sample was determined since a constantvolume of glass is required in the crucible for each glass sample. The mass ofglass to be added to the crucible is 2.6 cc ● glass density in Q/cc). Viscositymeasurements were made at 5 temperatures starting with a temperature of -1190”C. The temperature was lowered in - 50”C intervals and, after equilibrationat each temperature, another measurement was made.

Volatilization and crystallization can affect the viscosity results. For example,volatilization of a compound that reduces viscosity will lead to an increase inviscosity with time. On the other hand, crystallization in the melt has thepotential to increase the measured viscosity. Starting the viscosity experiment attemperatures above the liquidus temperature minimizes the effeet ofcrystallization on glass viscosity. The impact of volatile species can bedetermined by measuring the viscosity as a function of time or by choosing athermal profile that allows for detection of hysteresis effects.

A detailed determination of the impact of volatilization and crystallization on themeasured viscosity was beyond the scope of this task. Rather, a comparison ofthe results from PNNL, Corning, and SRTC was used to demonstrate thatconsistent results could be obtained. Crystallization does not significantly impactthe Fulcher fit for these data since the viscosity change with temperature isrelatively small in the region of 1150°C. Therefore, even if crystallizationoccurred, its impact on the measured viscosity at 1150°C would be small. PNNLfollowed a sequence of temperatures that allows for hysteresis effects on viscositydue to volatility to be observed. If the PNNL and SRTC results are close, it maybe assumed that no significant volatility occurred with these glasses during theviscosity measurements.

Viscosity Measurements. The viscosities at a series of temperatures werecalculated from the rpm’s of the spindle, the %torque on the spindle, and aconstant, K, measured from the NIST 717a glass. The K constant actually variedslightly with temperature, and for temperatures between 1050 and 1500 “C itfollowed the form: 198.4-(0.063454 x T in “C)? Using this equation, the

viscosity at a given measurement temperature was then calculated by equation

(l):

Viscosity (Poise) q= [% torque/ RPM] o K (1)

2The development of this equation relating K to temperature is documented in notebook WSRC-NB-89-30(E-57157) on pages 91 through 98.

2


All of the viscosity measurements generated by SRTC are provided in Exhibit A.1of the Appendix. The viscosity (in Poise) of each of these glasses at 1150°C is tobe estimated from a Fulcher equation fitted to these measurements. Thefictional form of the (three-parameter) Fulcher equation (expressed in Poise)used to fit these data is given by equation (2):

●

lnti=A+(T~C)(2)

where lnfi represents the natural logarithm of the estimated viscosity (in Poise),

fi, and A, B, and C represent the parameters of the model that were determined

from the available measurements (expressed in Poise) at vaxious temperatures(represented by T, in degrees Celsius). The fitted model was then &ed to predictthe viscosity of the given glass at 1150”C.

Exhibit A.2 in the Appendix provides the results from such a Fulcher fit for eachset of viscosity measurements presented in Exhibit A. 1. Exhibits A.3-A.5 providethe results of the Fulcher fits to the viscosity measurements horn PNNL, CEILS,and SS, respectively.

Repeatability. The Batch 1 glass, with a viscosity close to 50 Poise at 1150°C(see Table 5), was chosen as the secondary standard for this work and forviscosity measurements of glasses produced during the glass studies for saltdisposition. A number of measurements were made at SRTC on the Batch 1 glassas a function of time and the results are presented in Table 1 and Figure 1. Theseresults provide a measure of the reproducibility of the technique.

Table 1. SRTC Batch 1 Viscosities at 1150°C (Poise) from Fulcher EquationsI Crucible/ nllm

ilpl21919i A I 48.6 I 3.8847117199 A 49.7 3.906

Datr 1...-.

+indle IViscosity at 1150”C (Poise) I . In(ql 1s0)

8/19/99 I A I 49.9 I 3.9108131199 B 49.5 3.902

4/30/99” B 46.4 3.8376/8/99 A 48.9 3.8906/9/99 B 47.3 3.857

There is no indication of a statistical difference in the viscosities presented inTable 1 due to the crucible/spindle set used. The relative standard deviation ofthese data (expressed as a percentage) is 2.7%, a (l-sigma) measure of therepeatability of the SRTC measurement process.

Figure 1 also presents the repeatability data by providing a plot of the Fulcher fitsfor all of the SRTC Batch 1 measurements.

.

—.-—.--—


Figure 1. Graphical Comparison of SRTC Batch 1 Vkcosities

Poise

650

600:

550: 90-

500:70-

450:

400:

350:

300:

20- —,,,J[l,,,,,J1,250:

200:

150:

loa :

50:

0 # I 1 I I I 1 I

90+3 950 100a 1050 1100 1150 1200 1250 1300 1350

Temp(DegC)

‘SRTC Bald 1oam)‘SRTC Batch1W7S9B

‘SRTC Bxch 1Sd B (-)

‘SRTC B..h 1(6%59,

‘sRTC B,lch 1SUB (69..?3)

‘SRTC Mch 1(W19.99,

‘SRTCB.ti 1S@B [u31M)

Comparisons. In this section, comparisons are made between the SRTC resultsand those obtained by PNNL, CELS, ador Sharp-Shurtz (SS). Figure 2 providesa plot of the SRTC values for Batch 1 along with a previous measured set of SSresults for this glass.

4


Figure 2. Graphical Comparison of Batch 1 Viscosities (SRTC and SS)

Poise 1UuJ

90-

80- .

70-

60-

50-

~40-

-1

:L1130 1140

Temp I

, , , , 1 * , ,

650

* 600:

550:

500:

450:

400:

350:

300:

250:

200:

150:

100:

50:

!-,,,,,,,,,,,,o I [ I I

50 1160 1170

eg C)

900 950 1000 1050 1ICO 1150 1200 1250 1300 1:

Temp(DegC)

‘SRTC Batch1(219199)‘SRTC Batch1 (2/17199)‘SRTC Batch1SetB (4/30/99)‘SRTC Batch1(6/8/99)‘SRTC Batch1SetB (619199)‘SRTC Batch1(8/19/99)‘SRTC Batch1SetB (8/31/99)‘SS BatchI

At 1150”C, the average SRTC result is 48.6 Poise and the Sharp-Shurtz result is44.2 Poise, a difference of 9.9% for the Batch 1 glass. When compared using a(natural)’logarithm scale, the difference is only 2.5%.

For this task the melt viscosity for the HM glass was measured by CELS, SRTC,and PNNL w a function of temperature. These results are summarized in Figure 3and Table 2 and include a previous HM viscosity measurement by SS.

5

nPoise

2400

● 2200

2000

1800

1600

1400

1200

1000

800

600

400

200


Figure 3. Graphical Comparison of HM Viscosities

1 I

1130 1140 llfo 1160 1170

n 150

Poise140

130

120

110

100

90. . r

ITemp (Deg c)

.

0 I , , , 8 I , , 8 1 , , r I , , , 1 , , 1 1 I 1 , , , I , # , s I 1 1 t I , , , r

900 950 1000 1050 1100 1150

Temp (Deg C)

t‘PNNL HM

‘SRTC HM SCI A (1/22/99)

‘SRTC HM Set A (1/28/99)

‘SRTC HM Set A (4/7/99)

‘SRTC HM Set B (4/2S/99)

I ‘CELS HM

! ‘SS HM

1200 250 1300 1350


Table 2. HM Viscosities from the Fulcher Fits

Imlso

Organization Viscosityat 1150”C(Poise) In(qllm)

,

CELS 111.5 4.714Pm 121.5 4.800 .

SRTC (Set A, 1/22/99) 121.8 4.802SRTC (Set A, 1/28/99) - 122.6 4.809SRTC (Set A. 41’7199) 121.9 4.803 .SRTC (Set B; 4/28/99) I 120.6 I 4.792

00 ii AA .4 -AnI aa I 114.4 I 4. 14U i

The average SRTC value is 121.7 Poise: 9.1% higher than the CELS value, 0.2%higher than the PNNL value, and 6.4% higher than the Sharp-Shurtz value. Inlog-space, the differences are: SRTC is 1.9% higher than CELS, 0.03% higherthan PNNL, and 1.3% higher than SS.

Figure 4 provides a similar plot of viscosities for the Purex glass, measured bySRTC and SS.

.

7


Figure 4. Graphical Comparison of Purex Viscosities (from Fulcher Fits)

I 1

I I n- 30I

280-Poise

28-.

260-

240-

220-

200-

180-

160-

140-

120-

100-

80-

Ss +

60-

40-

20-

~

oI

, , , I , , , I ,i

, , , 1 , , I I I , t , I , , , , I , , # i , , , , I , , , ,

900 950 1000 1050 1100 1150 1200 1250 1300 1350

Temp (Deg C)

. . . .

‘SRTC Purex (2/2/99)



‘SS Purex

..

The average SRTC value is 22.5 Poise, 12.5% higher than the SS value of 20.0

Poise for Purex. In log-space, SRTC is 0.6% higher than SS.

8

.


Uranium Glasses. The three uranium-containing glasses included in this taskwere sent to PNNL for viscosity measurements. This was done to provideindependent verification of the SRTC results. The CELS would not accept thesedepleted uranium glasses for measurement of viscosity due to the radioactivity.The results are shown in Table 3 and Figures 5,6 and 7.

.

Table 3. Measured Viscosities (from the Fulcher fits)for the Three Uranium-Containing Glasses

mlw

Glass Organization Viscosityat ln(qllm)ID 1150”C(Poise)

1 PNNL 88.8 4.486

1 SRTC (4/12/99) 88.5 4.483

1 SRTC (5/4/99) 87.3 4.469. . .

3 PNNL 95.8 4.562

3 SRTC (3/31/99) 98.4 4.589

3 SRTC (4/19/99) 107.4 4.677 .

3 SRTC (5/1 1/99) 101.6 4.621

5’ PNNL 104.7 4.651 - ““

5 SRTC (4/15/99) 107.4 4.677

5 SRTC (4/27/99) 109.4 4.695

For Glass 1, the average SRTC viscosity at 1150°C is 87.9 Poise, 1.0% lower thanthe PNNL value of 88.1 Poise. For Glass 3, the average SRTC viscosity at1150°C is 102.5 Poise, 7.0% higher than the PNNL value of 95.8 Poise. ForGlass 5, the average SRTC viscosity at 1150°C is 108.4 Poise, 3.5% higher thanthe PNNL value of 104.7 Poise.

In log-space, the differences are: for Glass 1, SRTC is 0.2% lower than PNNL, forGlass 3, SRTC is 1.5% higher than PNNL, and for Glass 5, SRTC is 0.7% higherthan PNNL.

.

9

---- .. . _,-L.T ~ -,. ,.-. , ,“.. , ,., , , m-”mT,..v.”s7....,m,T ,., . . . . . . , ,.m. .. ,. ,,, ,- -r?.T”T... .:-.-.<.-.-.-,..7----- .. -=- , . . . .. .< -., , ., .. -- . - -

— —


c1Poise

1600-

1400-

1200-

1000-

800-

600-

400 “

200-

0-

Figure 5. Graphical Comparison of Glass 1 Viscosities(A Uranium-Bearing Glass)

n 110Poise

105

95

90

1130 1140 11

Temp (D

\

r , , I , I-

160 1170

1~I 4 s I , t I t , , , I , * I 8 ,

900 950 1000 1050 1100 1150 1200 1250 1300 1350

Temp (Deg C)

10

nPoise

*1800

1600

1400

1200

1000

800

600

400

200

0



85+

75%-l--1130 1140 1:

Temp (D

n 135

Poise125

115

~-at,,,,,,,,,,, , , I , , 6 I , I * , , 1 t , , ,

900 950 1000 1050 1100 1150

Ternp (Deg C)

Y) 1160 1170

c)

‘SRTCGkMs3(3/31/99)

‘SRTC Glass 3 (4/1 9/99)

‘SRTC Glass 3 (5/1 1/99)

‘PNNL Gkiss 3

1200 1250 1300 1350

ElPoise

.

1800

1600

1400

1200

1000

800

600

400

200

(



nPoise140

K

130 -

120

110t

1130 1140 11

Temp (D

\

1“ r

I 1160 1170

c)

l———I I I I I 1 , I , , i ,

900 950 1000 1050 1100 1150

Temp (Deg C)

1200 1250 1300 1350

.. E12


Other Glasses. Two other glasses (designated as Glass 2 and Glass 4) wereincluded in this task. These glasses did not contain uranium, and they were sentto CELS for viscosity measurements. This was done to provide independentverification of the SRTC results for these glasses. The results are shown in Table4 and Figures 8, and 9.

●

Table 4. Measured Viscosities (from the Fulcher fits)for GIass 2 and Glass 4

Glass %s0ID Organization Viscosityat ln(qllw)

1150”C(Poise)2 CELS 61.2 4.114

2 SRTC (2/24/99) 65.9 4.188

2 SRTC (3/4/99) 65.3 4.179

4 CELS 92.8 4.530

4 SRTC (3/2/99) 102.3 4.628

4 SRTC (3/9/99) 102.4 4.629

For Glass 2, the average SRTC viscosity at 1150 “C is 65.6 Poise, 7.2% above theCELS value of 61.2 Poise. For Glass 4, the average SRTC viscosity at 1150”C is102.4 Poise, 10.3% higher than the CELS value of 92.8 Poise.

In log-space, the differences are: for Glass 2, SRTC is 1.7% higher than CELSand for Glass 4, SRTC is 2.2% higher than CELS.

I

13

.—.— -=?-. :,’7.-, ,-.,,.--=-,.. . , /.,.,,. . ..-.Y/-.wJY=;;K; :-: sm.m-> —m ,. -7 . . . ,-—,---


Figure 8. Graphical Comparison of Glass 2 Vkcosities

D:Poise

.

1100-

1000:

900:

1130 1140 IL800 z

Temp (De

700- -

600- -

500- -

400 :

300 :

200 ;Er

100 :

I 1160 1170

c)

~~

01 , I , , I I I , ,

900 950 1000 1050 1100 1150 1200 1250 .1300 1350

Temp (Deg C)

..

14

.

rPoise

1800

.

1600

1400

1200

1000

800

600

400

200

0


Figure 9. Graphical Comparison of Glass 4 Viscosities

nPoise

13’ r

> , s I s , * I a 1 I t t ,

J) 1160 1170

c)

-1 , t 1 , , I , , * , I , , , I

900 950 1000 1050 1100 1150 1200 1250 1300 1350

Temp (Deg C)

‘SRTC @iss 4 (3/2/99)

‘SRTC @Ms 4 (3/9/99) .!‘CELS G]ass 4

15

_ .....


Viscosity Model Predictions. Exhibit A.5 in the Appendix provides the viscositypredictions for the glasses considered in this study determined from the DWPFmodel for this property, which relates viscosity at 1150°C to glass composition[5]. Viscosity predictions for the glasses are provided using target (or reference)

* and measured (where available) “compositions. Information from Exhibit A.5 issummarized in Table 5.

Table 5: Summary of Viscosity Measurements and Predictions (in Poise) at li50°C

Based on Target and Measured Compositions of the GlassesI I Predicted Vkcosity

Measured Viscosity2I -lass I 1arget / MeasuredI rl–– I m– . I

ID Composition Composition SRTC PNNL CELS SsGlass 1 (U)’ 82.5 63.1 87.9 88.8 -

Glass 2 82.5 94.0 65.6 - 61.2 -Glass 3 (U) 92.9 82.9 102.5 95.8 -

Glass 4 108.9 119.8 102.4 – 92.6 -Glass 5 (U) 108.9 92.7 108.4 104.7 –

n., . .,- .- . ..-~atcn 1 30.2 45.0 44.2

HIM 137.2 121.7 121.5 111.5 114.4Purex 24.8 22.5 20.0

Uranium Std 33.2 32.3‘ U implies a uranium-bearing glass.2 Values were calculated using the Fulcher fit to the measurement data.

The results for the five glasses, denoted as Glass 1 through Glass 5, representingMacrobatch 2 (with and without uranium) are of primary interest. The PNNL andSRTC data support the idea that DWPF’S current viscosity model (usingmeasured compositions) may underpredict the viscosity for uranium-bearingglasses in this compositional region. Specifically, the viscosity model may tendto overpredict the viscosity measurements for glasses without uranium but maytend to underpredict the viscosity for glasses with uranium in this compositionalregion. These results indicate that uranium may play a significant role indetermining melt viscosity for glass compositions similar to those of DWPF’SMacrobatch 2, as suggested in the interim report [3].

Alternate Salt Studies. A large number of glasses were fabricated for thealternative salt program in FY99 [6, 7]. The two options considered were (1)small tank — involving Precipitate Aqueous Hydrolysis (PHA) and (2)Crystalline Silicotitanate (CST) pretreatment. The glasses fabricated containedPHA from 7 to 13 weight percent (wt%) or CST from 3 to 9 wt%, with both setsof glasses containing approximately 2.0 wt% oxide depleted uranium. The meltviscosities of these glasses were determined by SRTC and the results were:

(1) The measured viscosities were generally higher than the predictedviscosities using both target and measured compositions and

(2) - The measured viscosities of the PHA glasses werepredicted values than was the case with CST glasses.

16

closer to


These results do not appear to show the influence of uranium exhibited for thesludge-only glasses (Glasses 1, 3, and 5). Further work will be required tounderstand the influence of uranium on glass viscosity.

CONCLUSIONS .A Harrop, high-temperature glass viscometer has been installed, calibrated usingthe NIST 717a borosilicate glass standard, and tested at SRTC. This viscometeruses only 6 grams of glass per viscosity measurement. The repeatability of theinstrument was checked over time using Batch 1 glass. The relative standarddeviation of these data (expressed as a percentage) was 2.7%.

The SRTC viscosity measurements at 1150°C (from the Fulcher fit of the data)for Batch 1, HM, and/or Purex glasses were compared with data from CELS,PNNL, and SS. The SRTC viscosity values were always higher than the CELSand SS values averaging about 9% with a range from 6 to 12 %. On the otherhand the SRTC and PNNL results for the HM glass were different by only 0.2%.Conducting these comparisons in (natural) log-space leads to even smallerdifferences. These results indicate that the SRTC Harrop Viscometer provideshighly repeatable viscosity values at 1150°C and reasonable correspondence withCELS, PNNL, and SS data.

The 5 glasses fabricated to study the influence of uranium on viscosity were sentto PNNL (Glasses 1, 3, and 5) and to CELS (Glasses 2 and 4) for confirmation ofthe SRTC measurements. PNNL measured the three glasses containing uraniumand the results were within 7 % of the SRTC values. CELS measured theremaining two glasses that did not contain uranium. The results revealed that theSRTC viscosity values were - 10% higher than those measured by CELSconsistent with the Batch 1 results.

These five glasses are representative of DWPF’S Macrobatch 2 (with and withouturanium). The PNNL and SRTC data support the idea that DWPF’S currentviscosity model may underpredict the viscosity for uranium-bearing glasses in thiscompositional region. These results indicate that uranium may play a significantrole in determining melt viscosity for glass compositions similar to those ofDWPF’S Macrobatch 2.

. I

I

On the other hand, the results obttined with glasses produced through coupledflowsheets in an independent study for the Salt Alternatives Program do notappear to show the influence of uranium exhibited for the sludge-only glasses.Further work will be required to understand the influence of uranium on glassviscosity. .

17 I

-,-- - .“ , ,7-,. ,-???- . , T’???,. . .. . .-. -.-.-,,w-mm . ., .x.%,--- ,. .-F— . . . . . m’ .-,-, Z’ -.-,- . . —,- . ... -... — I

.-


RECOMMENDMHONInitiate a task to determine the influence of uranium on melt viscosity for sludge-only glasses and, if necessary, incorporate a uranium term into the viscositymodel for DWPF glasses.

.

PATH FORWARD .In suppofi of this recommendation, SRTC will seek finding to initiate a task to(A) develop a procedure for measurement of glass viscosity that identifies andminimizes the impact of volatility and crystallization on measured viscosities, (B)characterize the uncertainties in the measurements through a statistically designedset of experiments, and (C) provide the basis for an in-house capability forviscosity conflation and model revision tasks.

Since this capability will benefit not only DWPF but also TFA, BNFL, and SaltAlternative programs joint funding will be sought.

ReferenCeS

[1]

[2]

[3]

[4]

[5]

[6]

[7]

Cicero-Herman, C. A., M. K. Andrews, and T. B. Edwards, “Results of the Tank 42(Batch lB) Variability Study,” WSRC-TR-98-O0180, June 5,1998.

Fellinger, T. L., et al., “Confirmation Run of the DWPF SME Cycle Using the Sludge-Only Flowsheet with Tank 42 Radioactive Sludge and Frit 200 in the Shielded CellsFacility (U),” WSRC-RP-98-O0351, June 5, 1998.

Schumacher, R. F., et al, “Measurement of DWPF Glass Viscosity—Interim Report (U), .WSRC-RP-99-O0350, Rev. O,May 5, 1999.

Schumacher, R. F. and D. K. Peeler, “Establishment of Harrop, High-TemperatureViscometer (U),” WSRC-RP-98-O0737, Rev. O,September, 1998. .

Brown, K. G. and R. L. Pestles, “SME Acceptability Determination for DWPF ProcessControl (U), “ WSRC-TR-95-0364, Revision 3, February 21, 1996.

Edwards, T. B., J. R. Harbour, R. J. Workman, “Summary of Property Measurementsfrom CST Glass Study (U),” WSRC-TR-99-O0384, Rev. O,October 4, 1999.

Edwards, T. B., J. R. Harbour, R. J. Workman, “Summary of Results for PHA GlassStudy: Composition and Property Measurements (U),” WSRC-TR-99-O0332, Rev. O,September 9, 1999.

..

18


Appendix: Exhibits.

I

.


This page intentionally left blank.

20

.

Appendix: ExhibitsExhibit A.1: SRTC Vkcometer Results in Date Order

DateGlassGoal

Actual amt

TIME. MIL

113511401145122012251230131013151320140014051410144514501455

1128199HM STD

6.6386.628

TIMELEFT0.130.080.030.0130.080.030.080.03.OIH0.080.03.OIH0.110.060.01

SET RATE“c

12001200120011501150115011001100110010501050105010001000Iotxl

Sample RPMTemperature

‘c1188 601134 601081 301028 12976 6

cruc.&glass“crucible

glass

FURNACE“c

12001200 .12001149115011501100110011001049105010509999991000

293.632287.004

~ 6.628

SAMPLE“c

118811881188113511341134108110811081102810281028976976976

SPEEDRPM

606060303030303030121212666


% Torque K ViscosityMeasured

Poise43.4 123.01665 88.98204233.6 126.44316 70.80817253.7 129.80623 232.3531436.3 133.16929 402.837132.6 136.4689 741.481

920

TORQUE43.443.443.433.633.633.653.753.753.736.336.336.332.732.632.5

Appendix: ExhibitsExhibit A. 1: SRTC Viscometer Results in Date Order

DateGlassGoal

Actual amt

TIME. MIL

102510301035I0401045112311281133120512101215125513001305124013451350

1122/99HM STD

6.63896.632

TIMELEFI’0.120.070.02.OIH.OIH0.1

0.05.OIH0.120.070.020.06.OIH.OIH0.1

0.05.OIH

Sample

SET RATE“c

12001200120012001200115011501150110011001100105010501050100010001000

RPMTemperature

“c1187 601131 301079 301027 12974 12

cruc.&glasscrucible

glass

FURNACE“c

12011200 .12001200120011491150115010991100110010491050105099910001000

910Torque

43.733.954.3

36.6565.75

293.668287.036

6.632

SAMPLE“c

11871187118711871187113111311131107910791079102710271027974974974

K

123.0801126.63353129.93313133.23274136.5958

SPEEDRPM

3030306060303030303030121212121212

ViscosityMeasured

Poise89.643341143.09588235.17897406.915

748.43118

WSRC-RP-99-OI053Revision O

TO;QUE21.721.921.943.743.733.933.933.954.454.354.236.736.636.665.965.765.7

A2

Appendix: ExhibitsExhibit A.1: SRTC Viscometer Results in Date Order

Date 2.12J99Glass Purex

Goal=2.6cc=6.876gmsActual amount 6.879 -

TIME* MIL

105010551100113511401145122012251230123513051310131513201355140014051410

LEFT0.150.10.050.150.10.050.150.10.05

00.150.10.05

00.10.05.OIH.OIH

SampleTemperature

‘c1187113410791026974

SET RATE“c

120012001200115011501150110011001100110010501050105010501000100010001000

RPMPX Glass

6060606060

cruc.&glasscrucible

glass

-A~E‘c

12001200120011491149115010991099110011001049104910491050999100010001000

% Torque2/2/99

8.912.719

29.849.7

.

293.888287.009

6.879

SAMPLE“c

118711871187113411341134,10781079107910791026102610261026974974974974

K

123.0801126.44316129.93313133.2962136.5958


SPEEDRPM

606060606060606060606060606060606060

Viscosity

%TORQUE

8.98.98.912.712.712.719.119.019.019.029.929.829.829.849.849.749.749.6

Poise18.25688226.76380341.14549266.203777113.146858

A3

.. .. . .


Date 2/5199Glass Purex

Goal 2.6cc=6.876grnsActual amount 6.879

TIME.

MIL9509559601040104510501122112711321205121012151250125513001305

TIMELEFT0.120.070.020.070.02

O.OIH0.120.070.020.130.080.030.140.090.04

O.OIH

Sample

-“c1187113310791026

SET RATE‘c

1200120012001150115011501100110011001050105010501000100010001000

RPMPX Glass

60606060

974 60

cruc.&glasscrucible

glass

FURNACE“c

1200120012001150115011501099109911001049104910499999999991000

YO Torque2J5199

8.4512.05

1828.3

46.67

293.945287.066

6.879

SAMPLE“c

118711871187113411321133107910791079102610261026974974974974

K

123.0801126.50662129.93313133.2962136.5958

SPEEDRPM

60606060606060606060606060606060

ViscosityMeasured

Poise17.33378125.40674638.97994

62.871372106.24877


%TORQUE

8.458.458.4512

12.112.0518.05

1818

28.428.328.2

47.0546.846.646.6

A4

Appendix: ExhibitsExhibit Al: SRTC Viscometer Results in Date Order

Date 2.19/99Glass Batch 1Goal 2.6cc=6.773grnsActual amount 6.777

TIME, MIL

102510301035111011151120120012051210124512521255133013351340

TIMELEFT0.150.100.050.150.100.050.100.050.000.100.02

0.02H0.120.070.02

SampleTemperature

‘c1187113310801027976

SET RATE‘c

120012001200115011501150110011001100105010501050100010001000

cruc.&gk3sscrucible

glass

-ACE‘c

12001200 ~120011491149115010991100110010491049104999910001000

RPM 7. TorqueBatch 1 Glass

60 17.760 26.660 41.160 66.730 57.45

293.790287.013-6.777

SAMPLE“c

118711871187113211331133108010801080102710271027975976976

K

123.0801126.50662129.86968133.23274136.4689


SPEEDRPM

606060606060606060606060303030

ViscosityMeasured

Poise36.30863

56.08460188.960731148.1104

261.33794

%TORQUE

17.717.717.726.626.626.641.141.141.166.866.666.757.4557.4557.45


Date 117/99Glass Batch 1 cruc.&glassGoal 2.6cc=6.773gms crucibleActual amount 6.774 glass

. MIL104510501055113011351140121512201225130513121322135814031408

TIME SET WTE ~RNACELEFT ‘c ‘c

0.160.110.060.160.110.060.160.110.06

0.22H0.160.060.010.05

O.OIH

Sample RPM

120012001200115011501150110011001100105010501050100010001000

120012001200114911491150109910991100104910491050999

10001000

% TomueTemperature Batch 1 Glass “‘c

1188 60 18.051133 60 27.11080 60 41.91028 60 67.5976 30 58.3

293.795287.021

6.774

SAMPLE“c

118811881188113311331133108010801080102810281028976976976

SPEEDRPM

606060606060606060606060303030


K ViscosityMeasuredPoise

123.01665 37.007508126.50662 57.138822129.86968 90.692327133.16929 149.81545

136.4689 265.20455

TO$QUE18.0518.0518.0527.127.127.1

4241.941.867.767.567.558.558.258.2

A6


Date X24199Glass #2 (96 NoU)God 2.6cc=6.907grnsActual amount 6.907

TIME TIME● MIL LEFT

1030 0.131035 0.081040 0.031115 0.131120 0.081125 0.031205 0.081210 0.031250 0.081253 0.051258 O.OIH1330 0.121335 0.071340 0.02

SampleTemperature

“c1187.5113510791026974

SET RATE“c

12001200120011501150115011001100105010501050100010001000

cruc.&glass

crucibleglass

-ACE .“c

12001200 .1200114911491150110011001049105010509999991000

293.984287.077, 6.907

SAMPLE“c

1187.51187.51187.511351135113510791079102610261026974974974

SPEEDRPM

6060606060606060603030301212

RPM %Torque K ViscosityGkss 2 (96 Nom Measured

Poise60 23.45 123.04838 48.09140760 36.15 126.37971 76.14377560 58.05 129.93313 125.7103130 49.35 133.2962 219.27224.12 36 136.5958 409.78741


%TORQUE

23.4523.4523.4536.2

36.1536.1

58.0558.0598.6

49.3549.3590.13636


DateGlassGoal

Actual amt6.817

● TIMEMIL104210471052112611311136121112161221125613011306134113461351

312/99#4(high)6.81596.817

TIMELEFT0.110.060.010.120.070.020.120.070.020.120.070.020.120.070.02

Sample

SET RATE“c

120012001200115011501150110011001100105010501050100010001000

RPM‘Temperature

“c1187 601136 601081 301028 12976 12

cruc.&glasscrucible

glass

.tiACE‘c

1200 .120012001149115011501099109911001049105010509999991000

% Torque

3655.8

45.5531.457.7

293.848287.031

6.817

SAMPLE“c

118711871187113611361136108110811081102810281028976976976

K

123.0801126.31626129.80623133.16929136.4689


SPEEDRPM

606060606060303030121212121212

ViscosityMeasured

Poise73.848061117.47412197.08912348.45964656.18794

%TORQUE

36.0536

35.9555.955.855.845.6

45.5545.531.531.431.358

57.757.6

As

Appendix: ExhibitsExhibit A. 1: SRTC Vkcometer Results in Date Order

Date 314199Glass #2 (96 NoU)Goal 2.6cc=6.907gms

Actual amt 6.91

TIME TIME● ,MIL LEFT

1035 0.061040 .OIH1045 .OIH1123 0.091128 0.041133 .OIH1205 0.121210 0.071215 0.021252 0.11257 0.051302 01340 0.071345 0.021350 O.OIH

SampleTemperature

“c1186113110781025974

SET RATE‘c

120012001200115011501150110011001100105010501050100010001000

cruc.&glasscrucible

glass

mACE‘c

12001200 .120011501150115010991099110010491050105099910001000

293.938287.028

- 6.91

SAMPLE‘c

118611861186113111311131107810781078102510251025974974974

SPEEDRPM

606060606060606060303030301212


RPM % Torque K ViscosityMeasured

Poise60 23.75 123.14356 48.74432460 36.4 126.63353 76.82433960 58.5 129.99659 126.7466730 49.75 133.35965 221.1547512 36.3 136.5958 413.20231

%TORQUE

23.7523.7523.7536.436.436.458.658.558.449.8549.7549.6590.4536.336.3

A9

..7 - --,T, -,.-.-,-m .., ,... -,-..-r v.- .,,.r,.,-.-—,— —— ---- .—.


DateGlassGoal

Actual amt

TIME* MIL

101010151020105511001105114011451150131013151320

#4(high)6.8159

6.82

TIMELEFT

0.10.05

00.1

0.050

0.10.05

00.1

0.050

SET RATE“c

120012001200115011501150110011001100low10001000

cruc.&glasscrucible

glass

lj’URNACE“c

12001200 .120011501150115010991100110099910001000

293.887287.067

6.82

SAMPLE‘c

118811881188113211331133108010801080974975975

SPEEDRPM

606060606060303030121212


%TORQUE

36.3536.3536.3556.2556.256.245.9545.9545.95

5857.857.8

Sample RPM % Torque K ViscosityTemperature Measured

“c Poise1188 60 36.35 123.01665 74.5275861133 60 56.2 126.50662 118.494531080 30 45.95 129.86968 198.91706975 12 57.8 136.53235 657.63082

AlO


DateGlassGoal

Actual amt

TIME. MIL

113611401145122012251230130513101315135013551400143514401445

3/31/99#3 (97-Like)

6.8566.86

TIMELEFT0.140.10.050.150.10.050.150.10.050.150.10.050.150.10.05

SET W’Ill‘c

120012001200115011501150110011001100105010501050100010001000

RPM‘Temperature

“c1187 601137 60

1080.5 301026 12974 12

lj’URNACE‘c

12001200 .12001149114911501099109911001049104910499999991000

7. Torque

34.7553.543.229.453.4

SAMPLE“c

1187118711871136113711371080

1080.51080.5102610261026973974974

K

123.0801126.2528129.83795133.2962136.5958


SPEEDRPM

606060606060303030121212121212

ViscosityMeasured

Poise71.283892112.57542186.96665326.57568607.85133

%TORQUE

34.7534.7534.7553.853.553.543.4543.243.229.529.429.354.153.553.3

.

. .

.—..-.


DateGlassGoal

Actual amt

TIME. MIL

103510401045112011251130120512101215125012551300133513401345

4/7/99HM

6.6386.638

TIMELEFT0.120.070.020.120.070.020.120.070.020.120.070.020.120.070.02

Sarrde

SET RATE“c

1200- 1200

1200115011501150110011001100105010501050100010001000

RPM‘Temperature

“c1191 601136 301084 301031 12978 6

cruc.&gkiss

crucibleglass

-ACE‘c

12001200 .12001149114911501099110011001049104910509999991000

% Torque

42.1532.7552.235.231.7

293.638287

6.638

SAMPLE“c

119111911191113611361136108310841084103110311031978978978

K

122.82629126.31626129.61586132.97893136.34199

SPEEDRPM

606060303030303030121212666

ViscosityMeasured

Poise86.285466137.89525225.5316

390.07152720.34017


%TORQUE

42.1542.1542.1532.8

32.7532.7552.4

52.2552.1535.435.235.231.831.731.6

A12

Appendix ExhibitsExhibit A.1: SRTC Viscometer Results in Date Order

DateGlassGoal

Actualamt

TIME* MIL

1208121312181252125713:0213:3713:4213:471427143214:3715:1515:20

4/12/99#1

6.9056.92

TIMELEFT0.150.100.050.150.100.050.150.100.050.100.050.000.070.02

SET RATE‘c

12001200120011501150115011001100110010501050105010001000

Ij’URNACE“c

12001200 .12001149114911491099109911001050105010509991000

SAMPLE“c

118811881188

1133.511341134108010811081102810281028975975

SPEEDRPM

6060606060603030303030301212



“c1188 601134 601081 301028 30975 12

ToTorque K ViscosityMeasured

Poise31.2 123.01665 63.96865748.4 126.44316 101.9974939.3 129.80623 170.0461666.9 133.16929 296.96751

48.95 136.53235 556.93821

%TORQUE

31.231.231.2

48.6548.4548.3539.4539.3539.25

6766.966.849

48.9

A13

c7m>.7ws,..7-+--:~..~.m-.m.. ,. .— . , ..... .r,-e... —=,-., --- ------ . .. .

—---


Date

Glass

Goal

Actual amt

“ TIME

MIL1027

1032

1037

1114

1119

1124

1157

1202

1207

1242

1247

1252

13271332

1337

4/15/99

#5

6.852

6.852

TIME

LEFT0.15

0.1

0.05

0.12

0.07

0.02

0.15

0.1

0.05

0.15

0.1

0.05

0.15

0.1

0.05

Sample

SET RATE“c

12001200120011501150115011001100110010501050105010001000100Q

RPM

Temperature

“c1188 60

1135.5 601080 301027 12975 12

FtJRiNACE‘c

120012001200114911501150109910991100104910491049999999999

%Torque

37.858.747.532.759.4

SAMPLE‘c

“ 118811881188

1135.51135.51135.51079.510801080

1026.510271027974

975.5975

K

123.01665126.34798129.86968133.23274136.53235

RPM60

60

60

60

60

60

30

30

30

12

12

12

12

12

12

Viscosity

MeasuredPoise

77.500488

123.61044

205.62699

363.05922

675.83513


%TORQUE

37.7537.837.858.858.758.647.7547.647.432.832.7532.65

6059.359.1

A14

Appendix: ExhibitsExhibit Al: SRTC Vkcometer Results in Date Order

DateGlassGoal

Actual amt

TIME. MIL

115512001205124012451250132513301335140514101415145014551500

4/19/99#3 (97-Like)

6.8566.858

TIMELEFT0.150.10.050.150.10.050.150.10.050.150.10.050.150.10.05

SET RATE‘c

120012001200115011501150110011001100105010501050100010001000


“c1190 601137 601080 301028 12975 12

-ACE“c

1200‘1200 .12001149,114911501099109910991049104910499999991000

% Torque

37.3557.9547

32.358.75

SAMPLE‘c

1189.511901190

1136.511371137

1078.51080.51079.5102810281028974.5975

975.5

K

122.88974126.2528129.86968133.16929


RPM606060606060303030121212121212

ViscosityMeasured

Poise76.498863121.93916203.4625

358.44733136.53235 668.43963

%TORQUE

37.3537.3537.3558.25

5857.947.34747

32.432.332.2

59.3558.7558.45


DateGlassGoal

Actual amt

TIME. MIL

110711121117115011551200124012451250132013251330140514101415

4127199#5

6.8526.850

TIMELEFT0.080.03.02H0.150.1

0.050.1

0.050

0.150.1

0.050.150.1

0.05

Samvle

SET RATE“c

120012001200115011501150110011001100105010501050100010001000

RPM“Temperature

“c1190.5 601136.3 601081.5 301028 12975.5 12

J’URNACE‘c

12001200 .12001149114911501099109911001049105010509999991000

7. Torque

37.9558.9347.7532.8359.62

SAMPLE“c

1190.51190.51190.51136.51137

1135.51081.51081.51081;5102810281028975

975.5976

K

122.85801126.29722129.7745

133.16929136.50062

RPM606060606060303030121212121212

ViscosityMeasured

Poise77.707693124.04492206.55774364.32898678.1806


%TORQUE

37.9537.9537.9559.1558.8558.847.7547.7547.75

3332.832.759.9559.659.3

..

A16

Appendix: Ex~bitsExhibit A. 1: SRTC Viscorneter Results in Date Order

DateGlassGoal

Actual amt

TIME● MIL

120512101215125012551300134013451350142414291434150515101515

4128/99HM

6.6386.641

TIMELEFT0.05H0.05H0.040.140.090.040.090.04

O.OIH0.10.050

0.150.10.05

Sample

SET RATE‘c

120012001200115011501150110011001100105010501050100010001000

RPM,-Temperature

“c1193 60

1138.5 601083.5 301030.5 30977.5 12

NEW CRUCIBLE AND SPINDLEcruc.&glass

crucibleglass

-ACE“c

12001200 .12001149I 149115010991100llofJ1049105010509999991000

% Torque

41.363.6551.0585.7861.7

... .

291.516284.875

6.641

SAMPLE“c

1193119311931139

1138.51138.51083.51083.51083.51030.51030.51030.5

977977.5977.5

K

122.69938126.15762129.64759133.01065136.37372

SPEEDRPM

606060606060303030303030121212

ViscosityMeasured

Poise84.458072133.83221220.61698380.32179701.18818


%TORQUE

41.2541.2541.3563.863.6563.6551.151.05

5185.9585.785.762.361.861.6

A17

. . . . ..-..— ,C,....=. .-.m.r .--.-–,--- ,-.SI-:-7.?V 7a~ ...;Y7m-.‘“-~,.- ?—— .,.,, ,-— ~-,-: ~


DateGlassGoal

Actual amt

TIME. MIL

103310381043111811231128120312081213124812531258133313381343

4130199Batch 16.7736.778

TIMELEFT0.150.1

0.050.150.1

0.050.150.1

0.050.150.1

0.050.150.1

0.05

Sample

SET RATE“c

120012001200115011501150110011001100105010501050100010001000

RPMTemperature

‘c1194 601139 601086 601032 60979 30

Crucible B and Spindle Bcruc.&glass

crucibleglass

PACE‘c

12001200 .12001149115011501099110011001049104910509999991000

% Torque

16.224

37.260.1551.7

291.683284.905

6.778

SAMPLE‘c

1194.511941194113711381141

1085.510861086

1031.510321032

978.5979979

K

122.63592126.12589129.48896132.91547136.27853

SPEEDRPM

606060606060606060606060303030

ViscosityMeasured

Poise33.11169950.45035880.283153133.24776234.85334


TO~QUE16.216.216.224.22424

37.337.237.2

60.5560.260.152.151.851.6

A18


DateGlassGoal

Actual amt

●

MIL940945950102510301035111011151120115512001205124012451250

514199#1

6.9056.904

TIMELE~0.150.10.050.150.10.050.150.10.050.150.10:050.150.10.05

SET RITE‘c

12001200120Q115011501150110011001100105010501050100010001000


“c1195.5 601139.5 601088 301035 30982.5 12

-ACE‘c

12001200 .12001149115011501099109910991049104910509999991000

SAMPLE“c

11961195.51195.51139.51139.51139.5108710881088103410351035981.5982.5982.5

SPEEDRPM

606060606060303030303030121212



Poise29.25 122.54074 59.73861245.2 126.09417 94.99093936.4 129.36205 156.9592861.5 132.72511 272.0864844.5 136.05645 504.54265

.,

%TORQUE

29.229.2529.345.3545.245.0536.736.4536.3562.1561.6561.3544.9544.5544.45

Appendix: Exhibits WSRC-RP-99-O1O53Exhibit A. 1: SRTC Viscometer Results in Date Order

DateGlassGoal

Actual amt

TIME. MIL

102510301035111011151120115512001205124012451250132513301335

5/7)99Purex6.8766.877

TIMELEFT

0.10.05

00.1

0.050

0.10.05

00.1

0.050

0.10.05

0

Sample

SET RATE“c

120012001200115011501150110011001100105010501050100010001000

RPMTemperature

“c1196.5 601141.5 601088 601035 60982.5 60

Crucible B and Spindle Bcruc.&gk3ss

crucibleglass

mfwE“c

12001200 .12001150115011501099110011001049104910509999991000

% Torque

7.5510.8516.225.2

41.65

291.749284.872

6.877

SAMPLE‘c

1196.51196.51196.51141.51141.51141.5108810881088103510351035

982.5982.5982.5

K

122.47729125.96726129.36205132.72511136.05645

SPEEDRPM

606060606060606060606060606060

ViscosityMeasured

Poise15.41172622.77907934.92775355.74454694.445849

Revision O

%TORQUE

7.557.557.5510.8510.8510.8516.216.216.2

25.2525.225.1541.8541.641.55

A20


DateGlassGoal

Actual amt

TIME.

MIL104510501055113511401145122012251230130513101315135013551400

5/1 1/99#3 (97-Like)

6.8566.858

TIMELE~0.150.10.050.10.05

00.10.050

0.10.050

0.1.0.05

0

SET IViTE‘c

120012001200I 15011501150110011001100105010501050100010001000

mACE“c

12001200 .120011491150115010991100110010491049105099910001000

SAMPLE“c

1196.51196.51196.51140.51140.51140.51088

1087.51088

1034.510341034981

981.5981.5

SPEEDRPM

606060606060303030303030121212



‘c1196.5 601140.5 601088 301034 30981.5 12


Poise34.1 122.47729 69.607926

52.15 126.03071 109.5416941.85 129.36205 180.4600670.65 132.78856 312.71707

51 136.1199 578.50957

TO~QUE34.134.134.1

52.3552.0552.0541.9541.8541.7570.7570.6570.6551.3

51.0550.95

A21

—-r —-..-z-.’m,.,-..?...>7.. . .. -_,, ,., ,___.,..<.... m=’.rm-.,, ... . ....-’ .,.. * ... ........

—

Appendix: ExhibitsExhibit A.1: SRTC Viscometer Results in Date Order .“

Date 618/99Glass Batch 1God 2.6cc=6.773gmsActual amount 6.780

TIME TIMEv

MIL LEFT1209 0.101214 0.051219 0.001254 0.101259 0.051304 0.001339 0.101344 0.051349 0.001424 0.101429 0.051434 0.001509 0.101415 0.051519 0.00

SampleTemperature

‘c1199.51143.51089.51037984

SET RATE‘c

120012001200115011501150110011001100105010501050100010001000

Crucible & Spindle Acrllc.&!#ass - 293.800

glass

FURNACE‘c

1200I200120011491150115010991100110010491049105099910001000

RPM % TorqueBatch 1 Glass

60 16.560 24.5560 37.7560 6130 52.2

287.0206.780

SAMPLE“c

1199.51199.51199.51143.51143.51143.51089.51089.51089.5103710371037

983.5984984

K

122.28693125.84035129.26687132.5982

135.96126

SPEEDRPM

606060606060606060606060303030

ViscosityMeasured

Poise33.62890551.48967781.330404134.80817236.5726


TO~QUE16.516.516.5

24.5524.5524.5537.8

37.7537.7561.161

60.952.3552.252.2

A22

Appendix ExhibitsExhibit Al: SRTC Viscometer Results in Date Order

Date 6/9/99 Crucible &Spindle BGlass Batch 1 cruc.&glass 291.672God 2.6cc=6.773grns crucible 284.900Actual amount 6.772 glass 6.772

TIME* MIL

925930935

101010151020105511001105114011451150122512301235

TIME SET RATELEFT “c

0.10 .’ 12000.05 12000.00 12000,10 11500.05 1150O.OQ 11500.10 11000.05 11000.00 11000.10 10500.05 10500.00 10500.10 10000.05 1000O.@ 1000

FJJRNACE“c

120012001200114911501150109911001100104910501050999999

1000

Sample RPM % TorqueTemperature Batch 1 GIass“c

1198 60 16.31142 60 23.851089 60 36.45

1035.5 60 59.05982.5 30 50.65

SAMPLE‘c

1197.51198

1198.51141.5

11421142

1088.510891089

1035.51035.51035.5982.5982.5982.5


SPEEDRPM

606060606060606060606060303030

K ViscosityMeasuredPoise

122.38211 33.247139125.93553 50.059374129.29859 78.548896132.69338 130.5924136.05645 229.70863

TO#QUE16.316.316.3

23.8523.8523.8536.4536.4536.4559.0559.0559.05

50.750.65

50.6

. .._ _ .


Date 8119199Glass Batch 1Goal 2.6cc=6.773gmsActual amount 6.791

.MIL103010351040111511201125120012051210124512501255133013351340

LEFT0.120.070.020.120.070.020.120.070.020.120.070.020.120.070.02

Sample

SETRATE“c

120012001200115011501150110011001100105010501050100010001000

RPM

Crucible& SpindteACrucxzgks

crucibleglass

FURNACE‘c

12001200 .1200114911501150109911001100104910491050999

10001000

% TorqueTempe~ture

“c1199

1143.510901037984 30 52.95

Batch 1 Glass -

60 16.8560 2560 38.5560 61.9

293.784286.993

6.791

SAMPLE“c

1199119911991143

1143.51144109010901090103710371037984984984

K

122.31865125.84035129.23514132.5982

135.96126

SPEEDRPM

606060606060606060606060303030

VicosityMeasured

Poise34.35115552.43348

83.033577136.79715239.97163


%TORQUE

16.8516.8516.8525.05

2525

38.5538.5538.5561.961.961.953.252.952.8

A24

-—


.

Date 8131199Glass Batch 1God 2.6cc=6.773gmsActualamount6.774

.TIMEMIL110011051110114511501155123012351240131513201325140014051410

TIMELEFI’0.100.050.000.100.050.000.100.050SX30.100.050.000.100.050.00

SampleTemperature

‘c1200114810921040986

SET RATE‘c

1200120012001150115011501100110011001050105010501000

. 10001000

Crucible& SDindleBcruc.&glass

crucibleglass

FURNACE“c

1200 -12001200

- 11491150115010991loa110010491050105099910001000

RPM V. TorqueBatch 1 Glass

60 16.5560 24.360 37.3560 59.430 51.4

A25

“ 291.650~284.876

6.774

SAMPLE“c,

120012001200

1147.511481148109210921092104010401040986986986

K

122.2552125.55481129.10823132.40784135.83436


SPEEDRPM

606060606060606060606060303030

ViscosityMeasured

Poise33.72205950.84969780.369874131.08376232.72953

?40

TORQUE16.5516.5516.5524.3524.324.337.3537.3537.3559.259.459.651.451.451.4

. . . .. ,7..- r ; ..l, ,..p.{, <,7T,. , ..< . , .,,..,, , ~~~,~-y,.;,,.y-,-,-~,. ,,

-:...>: -s. r+%....,. .“

.- . . . ..-v~– .:—.—,— -,-==’<T<.Z7. , ,/. :,... , .. -<

Appendix: ExhibitsExhibit A. 1: SRTC Vkcometer Results in Date Order

DateGlassGoal

Actual amt

TIME.

MIL110011051110114511501155123012351240131513201325140014051410

10/8199Uranium Standard

7.1097

LEFT0.1

0.050

0.10.05

00.1

0.050

0.10.05

00.10.05

0

SET RATE‘c

120012001200115011501150110011001100105010501050100010001000


“c1199.5 601145 601091 60

1038.5 60984.5 30

FURNACE“c

12001200 .120011491150115010991100110010491050105099910001000

SAMPLE‘c

1199.51199.51199.5114511451145109110911091

1038.51038.51038.5984.5984.5984.5

SPEEDRPM606060606060606060606060303030

ToTorque K ViscosityMeasured

Poise10.95 122.28693 22.31736415.95 125.74517 33.42725824.35 129.17169 52.42217639.4 132.50302 87.01031734.4 135.92954 155.86587


%TORQUE

10.9511.0510.915.915.9515.9524.3524.3524.3539.339.439.534.434.434.4

A26

Appendix: ExhibitsExhibit A.2: Results of Fulcher Fits by Glass in Date Order for SRTC Measurements

1/22/99

JMP@ Nonlinear RegressionParameter Estimate o ApproxStdErrABc

‘ -4.62340847 0.6300421510258.573027 1274.4416561.650376873 62.5434012

(kaDh of Fulcher Fit7.0

6.5

6.0

~“g 5.5~

-~ 5.0~

4.5

4.0950 1000 1050 1100 1150 1200

Temp (Deg C)


I Measured [ In Vise I Measured Predicted

..-.

t+%-

,,.”744 s 4.49249 4.495839 89.34143.0959 4.969874 4.963515 144.01235.179 5.460217 5.460347 235.154n6915 6.003387 6.008604 404.80.--, .--. = -- -.--—— —.

974 748.7312 6.620716 6.61838 750.48 ,.1150 ? 4.802398 ? 121.8

A27

.- —... —... -—. ..— .—+.. ..-—.———


1/28/99

.

ParameterJMP@ Nonlinear

ABc

Estimate “-4.58290860610167.71155

67.374106932

RegressionApproxStdErr

0.35512756715.47967135.2822506

Graph of Fulcher Fit

6.5- ‘

6.0-

5.5-

5.0-

4.5-

4.0 I 1 1 1950 1000 1050 1100 1150 1200

Temp (Deg C)


.-, . A

Measured In Vise Measured PredictedTemp Vise. (Fulcher, lnVisc. Vise.

(Deg C) (Poise) Poise) (Poise) (poise)1188 88.98204 4.490335 4.488435 89.151134 141.6163 4.949685 4.953122 141.131081 232.3531 5.448121 5.448258 232.321028 402.8371 6.001557 5.998532 404.06976 741.481 6.607298 6.60865 740.481150 ? 4.808804 ? 122.58

Appendix: Exhibits WSRC-RP-99-O1O53

Exhibit A.2: Results of Fulcher Fits by Glass in Date Order for SRTC Measurements Revision O

Purex2/2/99

●

JMP@ Nonlinear RegressionParameter Estimate o ApproxStdErrABc

-3.605459573 0.304552426349.3945382 523.880195212.03562655 35.2584469

Graph of Fulcher Fit5.0

4.5-

~ 4.0-.3E.g 3.5->~

3.0-

950 1000 1050 1100 1150 1200

Temp (Deg C)

Purex! Measured in Vise I Measured I Predicted I

Temp Vise. (Fulcher, lnVisc. I Vise. I(Deg C) (Poise) Poise) (Poise)

1187 18.2569 2.9069781134 26.738 3.? R135’

1079 41.1455 3.: .“” s,1026 66.2038 4.195121i37A 112 lAAO A 777A(4

1 (poise) ]2.904543 18.30

----- 2 3.286086 26.6171 $UACI 3.717115 41.19

4.192738 66.36

71’-t lJ.J.17u/ 7.,”, .“ G 4.728687 113.01

1150 ? 3.163875 ? 23.66

I I I I I !

A29

.,” --.,..— , ... .N.....?.,Zc=m-?.->....-!-—--~,;, -“---- .-

-.—— .. .

Appendix: Exhibits WSRC-RP-99-O1O53Exhibit A.2: Results of Fulcher Fits by Glass in Date Order for SRTC Measurements Revision O

Purex2/5/99

.

JMP@Parameter

Nonlinear RegressionEstimate - ApproxStdErr

ABc

-3.898484758 0.139872016788.1400585 249.207654181.45202066 16.2567964


4.5

4.0

3.5

3.0

2.5 1 I I I 1

950 1000 1050 1100 1150 1200

Temp(Deg C)

Pm-m- —. ---

Measured In Vise Measured PredictedTemp Vise. (Fulcher, InVisc. Vise.


A30 .

Appendix: ExhibitsExhibit A.2: Results of Fulcher Fits by Glkss in Date Order for SRTC Measurements

Batch 12/9/99

JMP@ Nonlinear RegressionParameter Estimate - ApproxStdErrA -4.494750139 0.61567372B 8724.7982887 1188.84714c’ 108.53429464 65.4570676


5.5

3.5950 1000 1050 1100 1150 1200

Temp (Deg C)


Batch 1Measured In Vise Measured Predicted

Temp Vise. (Fulcher, lnVisc. Vise.(Deg C) (Poise) Poise) (Poise) (poise) ‘

1187 36.30863 3.59526 3.592055 36.431133 56.0846 4.021687 4.026861 55.801080 88.96073 4.486317 4.488195 88.791027 148.1104 5.004568 .4.997958 149.09976 261.3379 5.563052 5.565814 260.621150 ? 3.882672 ? 48.55

A31

. A

ppendix: ExhibitsExhibit A.2: Results of Fulcher Fits by Glass in Date Order for SRTC Measurements

Batch 12/17/99

JMP@ Nonlinear RegressionParameter Estimate - ApproxStdErrABc

6.0

-4.368131388 0.240079858555.4053557 460.183922115.94617024 25.6476823

5.5

4.0


3.5950 1000 1050 1100 1150 1200

Temp (Deg C)


Batch 1Measured in Vise Measured Predicted

Temp Vise. (Fulcher, lnVisc. Vise.(Deg C) (Poise) Poise) (Poise) (poise)

1188 37.00751 3.612256 3.611121 37.051133 57.13882 4.043818 4.045484 57.041080 90.69233 4.506275 4.507473 90.581028 149.8155 5.012242 5.009404 150.24976 265.2045 5.579392 5.580501 264.911150 ? 3.905524 ? 49.68

A32

Appendix ExhibitsExhibit A.2 Results of Fulcher fits by Glass in Date Order for SRTC Measurements

Glass 22/24/99

*

JMIW Nonlinear RegressionParameter Estimate “ ApproxStdErrA -4.189857342 1.03450359B 8245.3057008 1876.67085c 165.8200733 102.631977


GraDh of Fulcher Fit6.5

6.0-

5.5-

~‘“~ 5.0-~

“~ 4.5-~

4.0-

3.5 ~950 1000 1050 1100 1150 1200

Temp (Deg C)

Glass 2—---- —


(Deg C) (Poise) Poise) (Poise) (poise)1187.5 48.09141 3.880484 3.873104 48.45

1135 76.14377 4.31765 4.332623 75.011079 125.7103 4.839366 4.83398 126.391026 219.2722 5.395702 5.390314 220.46

974 409.7874 6.012457 6.015639 408.49

1150 ? 4.187986 ? 65.89

A33

-.


Glass 43/2/99

.

M@ Nonlinear RegressionParameter Estimate “ ApproxStdErrABc

. .-5.021262968 1.0061808210407.799087 2018.7096271.368094278 96.8389453

Graph of Fulcher Fit–,

950 1000 1050 1100 1150 1200

Temp (Deg C)

Glass 4I I Measured In Vise I Measured Predicted

Temp Vise. (Fulcher, hiVisc. Vise.(Deg C) (Poise) Poise) (Poise) (poise)

1187 73.84806 4.307799 4.30201 74.281136 117.4741 4.754697 4.766218 116.131081 197.0891 5.287246 5.283656 197.801028 348.4596 5.858365 5.853522 350.15976 656.1879 6.483747 6.486447 654.421150 ? 4.627811 ? 102.29

A34

Appendix; ExhibitsExhibit A.2: Results of Fulcher Fits by Glass in Date Order for SRTC Measurements

Glass 23/4/99

,. JMP@ Nonlinear Regression

Parameter Estimate - ApproxStdErrA -3.425115457 0.24581215

B 6856.6345785 404.535923

c- 248.27043953 24.1101762

Graph of Fulcher Fit,


,,

950 1000 1050 1100 1150 1200

Temp (Deg C)

Glass 2Measured In Vise Measured Predicted

Temp Vise. (Fulcher, lnVisc. Vise.m.. m (Pnic~) Pnise) (Poise) (poise)

19 48.76

.

Appendix: ExhibitsExhibit A.2 Results of Fulcher Fits by Glass in Date Order for SRTC Measurements

Glass 43/9/99

.JMP@

ParameterNonlinearEstimate .

ABc

-4.0842273678668.993743155.1141533

RegressionApproxWErr

0.680128291244.7388765.2453892

Gra~h of Fulcher Fit6.5

6.0

5.5

5.0

4.5

950 1000 1050 1100 1150 1200

Temp (Deg C)

Class A


----- .

Measured In Vise Measured PredictedTemp Vise. (Fulcher, lnVisc. Visco

(Deg C) (Poise) Poise) (Poise) (poise)1188 74.52759 4.308756 4.311169 74.351133 118.4945 4.780809 4.774867 119.201080 198.9171 5.288814 5.292888 198.11975 657.6308 6.489188 6.488644 657.991150 ? 4.629329 ? 102.45

●

Appendix Exhibits WSRC-RP-99-O1O53

Exhibit A.2: Results of Fulcher Fits by Glass in Date Order for SRTC Measurements Revision O

Glass 33/31/99

,JMP@ Nonlinear Regression

Parameter Estimate o ApproxStdErrA -5.203487644 2.01681083

B 11025.282625 4234.6444

c 24.135611033 200.696009


6.0-

~ 5.5-.=E.g 5.0->~

4.5-

4.0 I I 1 I950 1000 1050 1100 1150 1200

Temp (Deg C)

Glass 3! Measured in Vise I Measured Predicted

Temp Visc.- (Fulcher, lnVisc. Vise.

(Deg C) (Poise) Poise) “(Poise) (poise)1187 71.28389 4.277655- 4.26667 19 nl

1137 112.5754 4.703631 -- -—- 1 --. .—

1080.5 186.9667 5.233519 5.23093 187.45

1026 326.5757 5.801278 5.788662

974 607.8513 6.40373 6.40993 604.09

1150 ? 4.589239 ? 98.42

‘4 I 4.723623

z

I I I I

A37

.... .. , ... —T.- —--em -,----- .77’,.-, .. ... . .. - _, .,,,.-T7-~ , ,.Z- Z7..TS . . .>- .,... . . .. , . ., .. .. .-.7.,- ., -.. —. -.. --.... . . . . . .

Appendix: Exhibits WSRC-RP-99-O1O53Exhibit A.2: Results of Fulcher Fhs by Glass in Date Order for SRTC Measurements Revision O

4/7/99

JW@ NonIinear RegressionParameter Estimate “ ApproxStdErrABc

7.0

6.5

6.0

~-~ 5.5g

-5 5-0_=

4.5

4.0

.--5.043143248 0.1717515111083.92262 361.695094

24.344662735 17.1110281


I I I I

950 1000 1050 1100 1150 1200

Temp (Deg C)

Measured In Vise Measured PredictedTemp Vise. ” (Fulcher, lnVisc. Vise.


A38

Appendix: ExhibitsExhibit A.2 Results of Fulcher Fits by Glass in Date Order for SRTC Measurements

Glass 14/12/99

●

JMP@ Nonlinear RegressionParameter Estimate “ ApproxStdErrA -5.251703083 0.25159913B 10720.570572 516.056657c 48.707616219 24.5749404



6.0

5.5

5.0

4.5

4.0 ~950 1000 1050 1100 1150 1200

Temp (Deg C)

----- -

Measured in Vkc Measured PredictedTemp Vise. (Fulcher, lnVisc. Vise.

(Deg C) (Poise) Poise) (Poise) (poise)1188 63.96866 4.158147 4.158393 63.951134 101.9975 4.626345 4.624948 102.141081 170.0462 5.133504 ~ 5.13607 169.611028 296.9675 5.695559 5.693623 297.54975 556.9382 6.321933 6.322454 556.65

1150 ? 4.482833 ? 88.49

A39

I

,,.

,,


GIass S4/15/99

*

H@ Nonlinear RegressionParameter Estimate . APProxStdErrABc

. .-4.513995046 0.955752789651.1515193 1862.3280499.882043264 93.5353944


6.5

6.0

;: 5.5.~

> 5.0

4.5

4.0 I I I I

950 1000 1050 1100 1150 1200

Temp (Deg C)

Glass 1Measured in Vise Measured Predicted

Temp Vise. (I?ulcher, lnVisc. Visco(Deg C) (Poise) Poise) (Poise) (poise)

1188 77.50049 4.355587 4.350284 77.911135.5 123.6104 4.805225 4.817135 122.151080 205.627 5.332934 5.326064 207.041027 363.0592 5.895847 5.894566 363.52975 675.8351 6.514406 6.515949 674.79

1150 ? 4.676545 ? 107.40

A40


Glass 34/19/99

●

JMP@ Nonlinear RegressionParameter Estimate “ ApproxStdErrA -4.275829886 1.16787639B 9234.5665897 2234.14731c 118.44944286 115.103158



950 1000 1050 1100 1150 1200

Temp (Deg C)

Glass 3Measured InVise Measured Predicted

Temp Visco (Fulcher, lnVisc. Vise.(DegC) (Poise) Poise) (Poise) (poise)

1190 76.49886 4.342118 4.337276 76.871137 121.9392 4.79055 4.803522 120.37

A41

..-. 2.7 ,7r- -------- -- =,77... .... .. . ,. ...-., ..\... _ ,, ,,, .,7 ,... .--. —y . ~.. —

-. —.


Glass 54/27/99

ParameterJMP@ Nonlinear

ABc

7.C

6.5

6.0

4.5

Estimate o-4.47062997

9636.086810398.661509029


0.38089472744.06878337.5229028

Granh of Fulcher Fit1. —..

I I 1 I4.0950 1000 1050 1100 1150 1200

Temp (Deg C)


Glass 5Measured in Vise Measured Predicted

Temp Vise. (Fulcher, lnVisc.(Deg C)

Vise.(Poise) Poise) (Poise) (poise)

1190.5 77.70769 4.354931 4.352954 77.861136.3 124.0449 4.815925 4.820644 123.461081.5 206.5577 5.333714 5.33058 207.211028 364.329 5.898129 5.898057 364.36

975.5 678.1806 6.51895 6.519414 677.871150 ? 4.694912 ? 109.39

I .. I I

A42

.



HM (Crucible and SpindIe Set B)4/28/99 ~

JMP@ Nonlinear RegressionParameter Estimate “ ApproxStdErrA -4.320142575 0.41438758B 9711.6078471 823.40395c’ 84.219234228 41.9154646

Gra~h of Fulcher Fit

6.5-

6.0-

5.5-

5.0-

4.5-

950 1000 1050 1100 1150 1200

Temp (Deg C)

-—. —


(Deg C) (Poise) Poise) (Poise) (poise)1193 84.45807 4.438674 4.436255 84.66

1138.5 133.8322 4.891453 4.896587 133.151083.5 220.617 5.398455 5.396428 221.061030.5 380.3218 5.942782 5.941018 380.99977.5 701.1882 6.5517 6.552776 700.431150 ? 4.792058 ? 120.55

A43

.

. . .... .


Batch 1 (Crucible and SpindIe Set B)4/30/99

J~@ Nonlinear RegressionParameterABc

5.5

Estimate “ ApproxStdErr-4.874851565 0.51595029491.1788828 1051.0231960.500972194 56.1382161


5.0

3.5

3.0950 1000 1050 1100 1150 1200

Temp (Deg C) I


Batch 1Measured InVise Measured Predicted

Temp Vise. (Fulcher, InVisc. Vise.(Deg C) (Poise) Poise) (Poise) (poise)

1194 33.1117 3.498494 3.499887 33.071139 50.45036 3.925508 3.92099 50.681086 80.28315 4.380329 4.38556 79.861032 133.2478 4.894771 4.89221 133.59979 234.8533 5.458506 5.458961 234.751150 ? 3.836656 ? 46.37

A44

.



Glass 15/4/99f

JMP@ Nonlinear RegressionParameter Estimate “ - ApproxStdErrA - -4.699833614 0.76175876Bc

9562.1367256 1483.96856107.18914576 75.2170732

Gra~h of Fulcher Fit -6.5

6.0

~ 5.5.22.g 5.0>~

4.5

4.0950 1000 1050 1100 1150 1200

Temp (Deg C)

Glass 1I Measured in Vise I Measured Predicted

I TemP I Vise. I (Fulcher, I lnVisc. I Vise. I(Deg ~) (Poise) Poise) (Poise) (poise)

1195.5 59.73861 4.086385 4.089979 59.52

1139.5 94.99094 4.563013 4.553782 95.87

1088 156.9593 5.049382 5.055986 155.93

1035 272.0865 5.606294 5.60612 272.13

982.5 504.5407 6.224442 6.223648 504.94

1150 ? 4.469746 ? 87.33

A45

.+ —.“..,,...-,....e=~.- ..—=~...—.,—.. --.x ., .7= -..-.. .. . . . . .. . . . . . . . . . . . , . . . .- . .1=-s.. % . . . . . .7, .. . .7 --7= ,., .,. ... ., —————— ---,


Purex517/99

.

JMP@ Nonlinear. RegressionParameter Estimate - ApproxStdErrABc

5.0

4.5

4.0

3.5

3.0

2.5

-4.372307534 0.156297997485.1219273 293.275854143.34920218 18.2825477

GraDh of FuIcher Fit.

I I I I

950 1000 1050 1100 1150 1200

Temp (Deg C)

Purex— —. ---


(Deg C) (Poise) Poise) (Poise) (poise)1196.5 15.41173 2.735053 2.735129 15.411141.5 22.77908 3.126682 3.125843 22.801088 34.92775 3.551384 3.553282 34.861035 55.74455 4.022371 4.02078 55.83 i982.5 94.44585 4.547569 4.548027 94.401150 ? 3.063361 ? 21.40

1- 1 I I


Appendix ExhibitsExhibit A.2: Results of Fulcher Fits by Glass in Date Order for SRTC Measurements


Glass 35/11/99

JMP@ NonIinear RegressionParameter Estimate s ApproxStdErrABc“

-3.949730409 0.613956498562.9111795 1141.73437”150.96686754 61.6522803

“Granh of Fulcher Fit

I I I I

950 1000 1050 1100 1150 1200

Temp (Deg C)

----- .

I Measured In Vise / Measured I Predicted I

I Temp I Vise. I (Fulcher, I lnVisc. I Vise. I(Deg C) (Poise) Poise) (Poise) (poise)

1196.5 69.60793 4.240265 4.242878 69.431140.5 109.5417 4.703756 4.696305 110.361088 180.4601 5.188592 5.195509 179.221034 312.7171 5.747427 5.745299 313.38

981.5 578.5096 6.360408 6.360455 578:48

1150 ? 4.621468 ? 101.64

,.

A47

——


Batch 16/8/99

J~@ NonlinearParameter Estimate .ABc

5.5

5.0

~“g 4.50

.=>~

4.0

-4.1634176668160.6533445136.65295042


0.26297363498.12462428.7540657


3.5 -J-

950 1000 1050 1100 1150 1200

Temp (Deg C)


-- .”.. A

Measured In Vise Measured PredictedTemp Vise. (Fulcher, lnVisco Vise.

(Deg C) (Poise) Poise) (Poise) (poise)1199.5 33.6289 3.514689 3.515386 33.611143.5 51.48968 3.941739 3.941381 51.511089.5 81.3304 4.401077 4.39852 81.541037 134.8082 4.90048 4.903853 134.35984 236.5726 5.46741 5.466255 236.851150 ‘? 3.88975 ? 48.90

A48

Appendix ExhibitsExhibit A.2: Results of Fulcher Fits by Glass in Date Order for SRTC Measurements

Batch 1 (Crucible and SpindIe Set B)6/9/99

JIWIWParameterABc

5.5

5.0

‘Zj-“~ 4.50

.3>~

4.0

3.5

Nonlinear RegressionEstimate . ApproxStdErr

-3.478220023 0.37284869


6922.5011794 652.766354206.14511702 41.019357


950 1000 1050 1100 1150 1200

Temp (Deg C)

I I

Batch 1Measured InVise Measured Predicted

Temp Vise. (Fulcher, lnVisc. Vise.(DegC) (Poise) Poise) (Poise) (poise)

1198 33.24714 3.501129 3.503969 33.151142 50.05937 3.918761 3.91321 50.341089 78.5489 4.362821 4.363721 78.48

1035.5 130.5924 4.86863 4.872081 130.14982.5 229.7086 5.438451 5.436812 230.091150 ? 3.856065 ? 47.28

A49

—.- .Y-..7--n7- -T---T,7r777m7m ,,,. . ,,,.. >T.-.>r,>,?w:;:y,:;:y, .,..=-:WX77. . ,.,. , , . ., . < “t . . . . . . . . . . . , . ,-, . . . ,. , . . ..?0 --.,—f -, ’-.: , . , ~, -..- .- .-m- ..— .. ---- . ..-

_ . . ..——

Appendix Exhibits WSRC-RP-99-O1O53Exhibit A.2: Results of Fulcher Fits by Glass in Date Order for SRTC Measurements Revision O

Batch 18/19/99

.tJMP@Nonlinear Regression

Parameter Estimate “ ApproxStdErrABc

—-4.546871487 0.209160118960.434251 415.591051

90.405311289 22.929557


5.0

4.5

4.0

3.5950 1000 1050 1100 1150 1200

Temp(DegC)

-- . . . . A

Measured in Vise Measured PredictedTemp Vise. (Fulcher, lnVisc. Visco

(Deg C) (Poise) Poise) (Poise) (poise)1199 34.35115 3.535825 3.536636 34.32

1143.5 52.43348 3.961798 3.959545 52.551090 83.03358 4.417196 4.419245 82.861037 136.7972 4.919096 4.918499 136.88984 239.9716 5.480532 5.480521 239.97

1150 ? 3.909602 ? 49.88

A50



Batch 1 (Crucible and Spindle Set B)8/31/99

JMP@ Nonlinear RegressionParameter Estimate - ApproxStdErr “A.Bc

-4.429398801 0.829988788734.1932506 1633.32405101.72050786 91.5526932

Granh of Fulcher Fit5.5

5.0

~“g 4.50.

.=>~

4.0

3.5950 1000 1050 1100 1150 1200

Temp (Deg C)

Batch 1Measured in Vise Measured Predicted

Temp .: Vise. (Fulcher, lnVisc. Vise.(Deg C) (Poise) Poise) (Poise) (poise)

1200 33.72206 3.523216 3.518152 33.891148 50.84697 3.91846 3.928821 50.321092 80.36987 4.390529 4.386639 80.681040 131.0838 4.879334 4.875837 131.54986 232.7295 5.447787 5.449877 232.241150 ? 3.902533 ‘? J 49.53

.

A51

.—.



Uranium Standard Glass10/8/99

J~@ Nonlinear RegressionParameter Estimate - ApproxStdErrABc

-3.565831384 0.243483896350.8231927 406.90651247.41179886 26.5893295

Granh of Fulcher Fit5.5

5.0

4.5

4.0

3.5

3.0 1 1 I I

950 1000 1050 1100 1150 1200

Temp (Deg C)

UraniMeasured

m Standard Glass

Temp(Deg C)

1199.511451091

1038.5984.51150

in Vise(FuIcher,

Poise)3.1045833.5095993.9625144.4621275.0502653.470404

PredictedVise.

(poise)22.3033.4352.5986.67156.0632.15

MeasuredlnVisc.Vise.

(Poise)22.31736418

(Poise)3.1053653.5093723.95933

4.4660275.048996

?

33.4272576952.422175987.01031712155.8658691

?

..

Appendix: ExhibitsExhibit A.3: Results of Fulcher Fits by Glass for PNNL Measurements

PNNL

JMP@ Nonlinear Regression. Parameter Estimate ApproxStdErr

ABc

——-2.193010134 0.323227255907.120649 “ 556.112826

305.22809368 40.17480


5.5 l\

. \

3.5I ,,,\

1000 1100 1200 1300

Temp (Deg C)


HM Measured by PNNLMeasured In Vise Measured Predicted


1235 65.13 4.160291 4.176385 64.091187 89.54 4.506138 4.494685 90.571137 136.34 4.908841 4.915152 135.481186 90.46 4.513744 4.504908 91.261235 64.48 4.160291 4.166355 64.091284 46.52 3.842227 3.839882 46.631333 34.75 3.554491 3.54818 34.971236 63.93 4.153465 4.157789 63.651088 209.51 5.353404 5.344771 211.33

.1039 351.47 5.85734 5.862124 349.791150 -? 4.799553 ? 121.46 ““

A53

I

,,I

Appendix: ExhibitsExhibit A.3: Results of Fulcher Fits by Glass for PNNL Measurements

PNNLGlass 1

JMP@ Nonlinear RegressionParameter Estimate ApproxStdErrABc

6.5

6.0

5.5

G 5.0.=

5 4.5.a>~ 40

3.5

3.0

-6.454877277 1.4307806813955.979894 “ 3567.35447-125.5193544 158.757186


1 I 1 1 I I

950 1000 1100 1200” 1300

Temp (Deg C)

Glass 1 Measured bv PNNLMeasured In Vise Measured

Temp Vise. (Fulcher, lnVisc.

1 ,— -.--,

4.219214(Deg C) (Poise) Poise) I (Poise)

1186 67.98 4.1862011138 98.011088 156.05 :2::+1137 98.38 4.599195 -1--H%H1187 66.42 4.1780931235 44.58 3.802955 3.7972851283 31.21 3.453386 3.4407391187 64.76 4.178093 4.1706881039 243.78 5.529449 5.496266990 434.83 6.055869 6.0749551150 -? 4.486532 ?


PredictedVise.

(poise)

65.7798.54155.3399.4065.24.44.8331.6165.24

252.01426.6188.81

A54

Appendix: ExhibitsExhibit A.3: Results of Fulcher Fits by Glass for PNNL Measurements “

PNNLGlass 3

JMP@ NonIinear Regression● Parameter Estimate ApproxStdErr

ABc

——-4.806614893 0.7676723810310.952765 “ 1640.1553849.452807306 84.5435612


6.0

5.5

‘lJ--~ 5.0

4.0

3.5950 1000 1100 1200 1300

Temp (Deg C)

Glass 3 Measured by PNNL


Measured In Vise .Measured PredictedTemp Vise. ‘ (I?ulcher, lnVisc. Vise.

(Deg C) (Poise) Poise) (Poise) (poise)1184 73.32 4.281551 4.294833 72.351136 107.22 4.683035 4.674883 108.101087 170.23 5.131201 5.13715 169.221135 107.59 4.691777 4.678328 109.051184 , 72.96 4.281551 4.289911 72.351233 50.2 3.905292 3.916015 49.66

A55

.

Appendix: ExhibitsExhibit A.3: Results of Fulcher Fits by Glass for PNNL Measurements “

PNNLGlass 5


kTemp

(De C)11841136

I-H+

=

12331282118410389891150

-4.194028723 0.466124129166.6082047 “ 935.617028113.63583061 50.9315169

GraDh of Fulcher Fit

6.0

5.5

5.0

4.5

4.0

3.5950 1000 1100 1200 1300

Temp (Deg C)

Glass 5 Measured bv PNNL


Measured In Vise Measured PredictedVise. (Fulcher, lnVisc. Vise.

(Poise) Poise) (Poise) (poise)80.23 4.36998 4.384898 79.04117.17 4.77206 4.763626 118.16185.34 5.223421 5.222192 185.57117.91 4.780839 4.769922 119.2079.5 4.36998 4.375757 79.04

54.35 3.995092 3.995445 54.3338.14 3.651649 3.641264 38.5479.96 4.36998 4.381527 79.04

303.13 5.722635 5.714162 305.71536.24 6.277737 6.284582 532.58

? 4.65094 ? 104.68I

A56

Appendix: ExhibitsExhibit A.4: Results of Fulcher Fits by Glass for CELS Measurements “

CELS


—-2.483958723 0.118348956343.3354217 . 133.842921268.78934915 5.59577481

Grauh of Fulcher Fit

600 700 800 900 1000 1100 1200

Temp (Deg C)

HM Measured by CELS


Measured In Vise NJeasured PredictedTemp Vise. (Fulcher, InVisc. Vise.

(Deg C) (Poise) Poise) (Poise) (poise)1136.1 123.2 4.82984 4.813809 125.191115.2 146.6 5.010436 4.987708 149.97 “1075 216.2 5.384128 5.376204 217.92

1029.3 349.9 5.856931 5.857647 349.65984.8 601.2 6.375317 6.398928 587.17940.3 1096 6.962407 6.999422 1056.17899.3 1993 7.576673 7.597396 1952.12859.3 3863 8.25816 8.259199 3858.99809.9 10310 9.238848 9.24087 10289.18762.2 31360 10.37214 10.35329 31956.75713.6 125900 11.7768 11.74324 130195.9669 622900 13.36603 13.34214 637961.2

643.2 ..1975000 14.45823 14.49608 19016431150 ? 4.714474 ? 111.55

A57

t

. —-—. ..rFro.,,,,,,,..,,-.m . . . . . . . . .,7./~,m--:.:w ~. ! -.?.?ZI. , ,.. ...s ,.A . . “ ......—-%?l?z?m: .<.,.,,...,. ,..,. -,~~ .-.;r, . .. .,- . . . .,.<.,.,,.. ., . . ~.,,.. . . . . . . .~,.,.,1 .,, ”. ., ,.. - ,., ..... .:, .,’.-- I

—.

Appendix: ExhibitsExhibit A.4: Results of Fulcher Fits by Glass for CELS Measurements

CELSGIass 2

JMP@ NonlinearParameter EstimateABc

-2.7534920445804.0133568304.83858554 -


0.0597287662.611818

2.63956508


12.5

~ 10.0.$220

.= 7.5>~

5.0

2.5 I I 1 I 1

600 700 800 900 1000 1100 1200

Temp (Deg C)

WSRC-RP-99-01053Revision O

Glass 2 Measured by CELSI I Measured In Vise I Measured Predicted

I Temp I “Vise. . I (Fulcher, I InVisco I Vise.(Deg C) (Poise) Poise) (Poise) (poise)

1131.5 71.7 4.267536 4.272491 71.351115 80.79 4.410529 4.391853 82.31

1071.5 122.8 4.817012 4.810557 123.601028.4 196 5.26796 5.278115 194.02982.7 331 5.80875 5.802118 333.20935.7 646.5 6.446648 6.471573 630.59893.2 1244 7.111216 7.126087 1225.64851.1 2590 7.871482 7.859413 2621.45809.5 6336 8.747315 8.754003 6293.76766.2 18060 9.826696 9.801455 18521.66723.2 67880 11.11971 11.1255 67488.48679.8 335000 12.72547 12.72189 336202.7640.5 2070000 14.53778 14.54306 ~1150 “. ? 4.113851 ? 61.18

A58

Appendix: ExhibitsExhibit A.4: Results of Fulcher Fits by Glass for CELS Measurements “

CELSGlass 4


-2.662146769 0.119061616132.528355 128.209885

297.45020649 “ 5.28653656


12.5

10.0

7.5

5.0

2.5600 700 800 900 1000 1100 1200

Temp (Deg C)


Glass 4 Measured by CELSMeasured InVise Measured Predicted


1137.7 103.7 4.636312 4.641502 103.161115.6 122.8 4.833459 4.810557 125.641074.4 182.1 5.230935 5.204556 186.971030.1 296.3 5.708194 5.691372 301.33985.2 531.6 6.254655 6.275891 520.43943 975.9 6.837552 6.88336 932.20

898.8 1955 7.535792 7.578145 1873.93858.3 3906 8.272204 8.270269 3913.56823.2 8076 9.002201 8.996652 8120.94781 21910 10.02016 9.994698 22475.10

737.2 78140 11.28335 11.26626 79486.92690.2 411600 12.95219 12.92781 421760.2647.6 2893000 14.85187 14.8778 28189281150 -? 4.531015 ? 92.85

A59

I

! I

-.

Appendix: ExhibitsExhibit A.4: Results of Fulcher Fit to Historical Sharp-Schurtz Measurements ‘

Sharp-Schurtz (SS)

~@ Nonlinear RegressionParameterABc

Estimate-2.801823619

6904.78796234.43663463

ApproxStdErr0.36173537575.945501.32.7818745


4~900 950 1000 1050 1100 1150 1200

Temp (Deg C)

I


HM Measured by SSI I Measured in Vise I Measured I Predicted

I Temp I Vise. I (Fulcher, I lnVisc. I Vise.(Deg C) (Poise) Poise) (Poise) (poise)1192.53 81.33 4.404977 4.398515 81.861136.36 128.57 4.853802 4.856474 128.23

I 1079.07 I 21~

960.08 816.11 6.7901.78 1900.55 7.5448561150 ? 4.739749 I . I AA-r.-rA

5.37307 5.387061 215.521021.47 389.61 5.97136 5.965146 392.04

713578 6.704549 823.517.549899 1890.99

? llAA1

A60


Appendix: ExhibitsExhibit A.4: Results of Fulcher Fit to Historical Sharp-Schurtz Measurements ‘

Sharp-Schurtz (SS)Batch 1

JNUW Nonlinear RegressionParameter Estimate ApproxStdErrABc

-3.032985109 0.281075466242.3592243 459.435771235.02116276 “ 29.5718562

Granh of Fulcher Fit ~ _7

6

5

4

3800 900 1000 1100 1200 1300

Temp (Deg C)

Batch 1 Measured by SSI I Measured in Vise I Measured I Predicted I

Temp Vise. (Fulcher, lnVisc. Vise.(Deg C) (Poise) Poise) (Poise) (poise)1264.72 20.85 3.02933 3.037354 20.681207.85 29.4 3.383724 3.380995 29.481153.8 42.85 . 3.761206 3.757706 43.00

1094.46 67.25 4.230312 4.208417 68.741050.26 103.01 4.624107 4.634826 101.91999.91 171.95 5.128147 5.147204 168.70945.56 312.32 5.752403 5.744028 314.95 -892.53 638.85 6.46097 6.45967 639.681150 ? 3.789423 ? 44.23

A61

— ..

Appendix: ExhibitsExhibit A.4: Results of Fulcher Fit to Historical Sharp-Schurtz Measurements “

Sharp-Schurtz (SS)Purex

JMP@ParameterABc

NonlinearEstimate

-3.1584338575390.4148385274.39604438 .


0.0252220835.28581112,24902056


6-

5-

4-

3-

2 I I I800 900 1000 1100 1200

Temp (Deg C)

WSRC-RP-99-01053Revision O

Purex Measured by SSI I Measured In Vise I Measured Predicted

Temp Visce (Fulcher, lnVisco Vise.(Deg C) (Poise) Poise) (Poise) (poise)1155.32 19.331097.62 29.61

I 2.960613 2.961658 19.31.389499 3.388112 29.65

1051.16 43.85 3.781145 3.780775 43.87---- # ,998.24 72.85 4.288496 4.288403 72.86 —

946.17 129.97 4.865716 4.867304 129.76

893 258.42 5.555404~ -- .--/ -----

t

8383.>3438b 238.b3

605.34 6.40575; 6.40579 605.32

1

1150 ? 2.997791 ? 20.04

L I I I I

A62

Appendix ExhibitsExhibit A.5: Viscosities Predicted by the DWPF Viscosity Model


Target & Measured Compositions and Predicted& Average Measured Viscosities at 1150 ‘CI ,----

SKIL

Glass ID TargetCompositionsas WeightFractionsA1203 B203 CaO Cr203 CUO

Glass 1 0.0623 0.0850 0.0148 0.0010 0.0003Glass2 0.0623 0.0850 0.0230 0.0013 0.0009Glass3 0.0605 0.0865 0.0139 0.0009 0.0003Glass4 0.0664 0.0853 0.0178 0.0010 0.0003Glass5 0.0664 0.0853 0,0140 0.0010 0.0003Batch 1 0.0488 0.0777 0.0122 0.0011 0,0040

HM 0.0715 0.0703 0.0101 0,0009 0.0025Purex 0.0299 0.1033 0,0109 0.0015 0.0042

UraniumStd 0.0410 0.0921 0,0130 0.0030 0.0000

Fe2030.12910.12910.11150.11150.11150.12840.07780.13250.1320

K20 Li20 MgO MnO0.0000 0,0342 0.0219 0.01590.0000 0.0342 0.0280 0.01850.0000 0.0355 0.0209 0.01430.0000 0.0333 0.0275 0.01880.0000 0.0333 0.0200 0,01500.0327 0,0443 0,0142 0,01730.0221 0.0462 0.0149 0,01760.0341 0.0322 0.0141 0.01690.0300 0,0306 0.0121 0,0289

Na200.10970.10970.10960.10950.10950.09000.08560.12620.1180

N1O Si02 Ti020.0022 0.5040 0.00100.0020 0.5040 0.00200.0020 0.5177 0.00200.0020 0.5257 0.00100.0020 0.5257 0.0010000075 0.5022 0.00670.0041 0,5579 0.00560.0119 0.4654 0.00680.0112 0,4535 0.0105

U3080.01600.00000.01600.00000.01500.00000.00000.00000.0241

PredictedVise.Poise SRTC82,51 87.982,51 65.6

92.884 102.5108.895 102.4108.895 108.456.167 48.6137.244 121.724.832 22.533.2 32.2

SRTC PredictedGlass ID Measured Compositions as Weight Fractions Vise.

A1203 B203 CaO Cr203 CUO Fe203 K20 Li20 MgO MnO Na20 NiO Si02 Ti02 U308 Poise SRT.CGlass 1 0.0683 0,0892 0.0174 0.0008 0,0003 0.1320 0.0000 0.0343 0.0207 0.0160 0.1190 0.0022 0.4820 0,0014 0.0131 63,14Glass 2

87.90.0648 0,0864 0.0232 0.0012 0,0009 0.1160 0,0000 0.0290 0.0241 0.0158 0.1060 0.0019 0.4790 0.0022 0.0000 94.003 65,6

Glass 3 0,0651 0,0880 0,0158 0,0007 0,0004 0,1030 0,0000 0.0373 0,0195 0.0139 0,1140 0.0019 0.5050 0,0022 0,0146 82.875 102,5Glass 4 0.0685 0,0896 0,0195 0.0010 0,0003 0,0988 0.0000 0.0275 0.0242 0,0153 0,1130 0.0020 0.5120 0,0133 0,0000 119.752. 102.4Glass 5 0.0665 0.0867 0.0144 0.0008 0.0003 0.1010 0.0000 0.0343 0.01770.014’? (2.11xl 001119 0 5f10fs 0O(I17 n 01A? c)?6<A 1(-RA

CELS PNNL SS88.8

61.295.8

92.6104.7

44.2111.5 121.5 114.4

20

CELS PNNL SS88.8

61.295.8

92.6104.7

?...,,; ,1

.!‘.

,.-./,,,,.]

...,.,..,.1,,.~~I.,..:

A63

---- .. .


D.WPF Distribution

M. N. Brosee, 704-SR. E. Edwards, 704-25SH. H. Elder, 704-SD. C. Iverson, 704-30SW. D. Kerley, 704-SJ. E. Occhipinti, 704-27SJ. F. Ortaldo, 704-SJ. W. Ray, 704-35S

SRTC Distribution

D. F. Bickford, 773-43AK. G. Brown, 704-lTA. D. Cozzi, 773-43AD.A. Crowley, 773-43AT. B. Edwards, 773-42AC. R. Goetzman, 773-AJ. R. Harbour, 773-43AE. W. Holtzscheiter, 773-AC. M. Jantzen, 773-AJ. C. Marra, 773-43AS. L. Marra, 704-TL. M. Papouchado, 773-AD. K. Peeler, 773-43AR. F. Schumacher, 773-43AM. E. Smith, 773-43AR. H. Spires, 773-AR. C. Tuckfield, 773-42AJ. R. Workman, 773-A

measurement of dwpf glass viscosity -final report/67531/metadc701893/m2/1/high... · temperature...

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