IWNL-13376

Compilation and Integration of K Basin SludgeParticle Size Analysis Data

P.R. BredtJ. M. TingeyA. J. Schmidt

June 2, 1999

Prepared forNumatec Hanford Corporation

Work Supported bythe U.S. Department of Energyunder Contract DE-AC06-76RL0 1830

Pacific Northwest National LaboratoryRichland, Washington 99352

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NOVf f)2000Summary and Conclusions

OSTIAll existing particle size analysis data on the K Basin sludge were compiled and analyzed to develop acomprehensive picture of the particle size distributions (PSDS) for the various sludge types. This analysiswill be used to update the design basis feed compositions for the baseline K East (KE) and K West (KW)Basin sludge process streams expected to be generated during Spent Nuclear Fuel (SNF) Projectactivities.

Particle size will dictate the makeup of most of the K Basin sludge process streams. For example, StreamKE2 will consist of 250 to 6350 pm sludge particles collected from the KE canister removal and fuelwashing operations. Consequently, knowledge of the PSD is necessary to project the inventory of theprocess streams. Furthermore, the PSD of the sludge streams will affect the performance of all physicalunit operations, including sludge retrieval, pumping/transport, and separations (settling, filtration,hydroclones). Particle size, along with uranium metal content of the sludge, largely determines thechemical reactivi~ of the sludge. Chemical reactivity will constrain how the sludge maybe handled,transported, and stored. Additionally, some sludge disposition pathways being considered as alternativeapproaches to baseline chemical treatment include approaches in which the sludge may be segregated onthe basis of particle size.

The PSD analyses were conducted during various sludge characterization efforts (from 1993 through1998) and involved samples of sludge collected from the KE Basin floor, the KE Weasel Pit, the KENorth Loadout Pit, the KE canisters, and the KW canisters. Also analyzed were residual sludge samplesgenerated during the transport of KE and KW fuel elements. In performing the analysis of the data forthis report, it became apparent that comprehensive PSD data (i.e., distribution from 0.12 to 6350 ~m) arelimited, and the existing data are not always fully representative of the individual sludge samples tested.Much of the data was collected from discrete fractions of individual sludge samples. In addition, severaltechniques were used to collect data that span the PSD range of interest. Because these techniques are notwholly compatible, assumptions were made to prepare the PSD curves for this document.

During future characterization efforts, PSD analyses should be performed on a larger fraction of thesamples. The PSD analysis should be performed on representative subsamples of the discrete samplesrather than on discrete sample layers. Alternatively, analyzing representative composite sludge sampleswould generate very useful PSD data.

As a part of the sludge characterization activities, wet and dry sieving with wire mesh screens was used tosegregate and quantifi the particle size distribution of larger particles (250 to 6350 pm). Smaller particles(below 710 pm) were analyzed using optical techniques (Leeds and Northrup Microtrac X1OOParticleSize Analyzer and Brinkmann Model2010 Analyzer). Some samples were analyzed by only one method;some were analyzed by both methods at the same time; and others were analyzed by both methods atdifferent times (in some cases, samples dried out between the analyses). In addition to sludge samples,cold ion exchange resins (Purolite NRW 100 and NRW 400) were analyzed for comparison with sludgesamples. For most of the optical analyses, the Microtrac X100 was used; the Brinkmann Analzer wasused for a set of samples collected in 1993.

Since sieving uses mass and the optical analysis is based on volume, assumptions were used to combinethe data sets. The approach used in this report was to assume the density of the particles was uniformfrom 0.12 to 6350 pm. With that assumption, the volume percent of particles in a given range equaled themass percent in that range. From that key assumption and other minor assumptions, the information fromthe two techniques was combined to prepare PSD curves that span the range of 0.12 to 6350 pm.

...111

Figures S.1 through S.4 are the integrated PDS curves for the following types of sludge: KE floor andWeasel Pit sludge, KE canister sludge, KW canister sludge, and residual sludge from fuel elementtransport. Figure S.5 compares the PSD for the five sludge types in a single plot. The error bars in thesefigures indicate the highest and lowest value for each discrete size range (high-low bars). These curveswere prepared by averaging the PSD results from samples of the same sludge type. The data used for thelower particle size range in these figures (below ’71Opm) were generated using the optical method afterthe sludge samples were sonicated to break up any particle agglomerates. A complete description of howthe existing PSD data were manipulated to produce these comprehensive curves is provided in the mainbody of this report.

Comparing the PSD curves fi-omthe various sludges (Figure S.5) shows the KE canister sludge containsthe greatest distribution of particles above 1000 pm. The PSD of the KE Weasel Pit sludge is comparableto that of the KE floor sludge below -250 pm. The KE floor sludge is finer than both the KE Weasel Pitand the KE canister sludge. The residual sludge exhibits the finest PSD of the sludge types examined.Below 200 ~m, the KW canister sludge is finer than all but the residual sludge. The bulk of the materialabove 200 pm in the KW canister sludge is the friable Grafoil fragments generated from thedisintegration of the Grafoil seal between the canister and canister lids.

Through a series of assumptions and calculations, a diverse set of particle size data was integrated toprovide particle size distribution curves that span a range of K Basin sludge. These curves can be used toupdate the design basis sludge feed compositions, provide input to sludge disposition alternativeselection, and provide data for safety-related calculations. However, as shown in this report, theintegrated curves were developed from limited samples and sample fractions. As new particle size databecome available, these curves should be revised.

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ix

Contents

.

.

Summary and Conclusions.,.

.......................................................................................................................... 111

1.0

2.0

3.0

4.0

5.0

Introduction ..............................................................................................4.................................... 1.1

Sample History mdDesctiptions ..............................................................................""""".""........"""2"12.1 1993 KE Basin Floor and Pit Sludge Sampling .....................................................................2.l2.2 1995 KEBasin Floor and Weasel Pit Sludge Sampling .........................................................2.l2.3 1996 KE Basin Canister Sludge Sampling .............................................................................2.22.4 1996 KWBasin Canister Sludge Sampling ..................................................i.........................2.32.5 1998 K Basin Residual SludgeGenerated fi-omFuel Element Transport ..............................2.3

Particle Size Measurement Methods .............................................................................................3.l3.1 Sieving Methods .....................................................................................................................3.l

3.1.1 Dry Sieving .............................................................................................................3.l3.1.2 Wet Sieving ............................................................................................................3.1

3.2 Optical Analyses ................................................................................+....................................3.33.2.1 Brinlunann Model 2010 halyzer ..........................................................................3.33.2.2 Microtrac X1OOParticle Size Analyzer .................................................................3.3

Results ................................................................'...........................................................................4.l4.14.24.3

4.4

Results fi-omSieving ..............................................................................................................4.lBrinkmann Analyzer Results ..................................................................................................4.2Microtrac Xl 00 Results on Individual Samples Before Sonication(0.12 to 71o ~) .....................................................................................................................4.2Microtrac Xl 00 Results on Individual Samples After Sonication(0.12 to 710 pm) ..........................................~.....................................+....................................4.3

4.5 Microtrac Xl 00 Results for Sludge Types Before and After Sonication(0.12 to 710 ~) .................!..............................................4......................................c.............4.3

4.6 Combined PSD Results from Sieving and Microtrac X1OOData(0.12 to 6350 V) ...................................................................................................................4.4

References .....................................................................................................................................5.l

Appendix Supporting Particle Size Data from Microtrac Xl 00 Analyses

xi

Figures

4.1

4.2

4.3

4.4

4.5

4.6

4.7

4.8

4.9

4.10

4.11

4.12

4.13

4.14

4.15

4.16

Comparison of Sieving Results for KE Basin Canister Sludges ..l................................................4.6

Particle Size Distribution Results for ICEBasin 1993 Sampling(Brinkmann Model 2010,0.5 to 150 ~) ......................................................................................4.7

Particle Size Distribution Data ffom Samples KES-M- 13 (ICEFloor Sludge) andKES-T-20 (KE Weasel Pit) Before Sonication Without Sieving (Microtrac X1OO,0.12to 710 ~) .............................................................................................................................4.8

Particle Size Distribution Data from Sample 96-04 (KE Canister Sludge)Before Sonication Without Sieving (Microtrac X1OO,0.12 to 710 pm) .......................................4.9

Particle Size Distribution Data from Sample 96-06 (KE Canister Sludge)Before Sonication Without Sieving (Microtrac X1OO,0.12 to 710 pm) .....................................4.lO

Particle Size Distribution Data from Sample 96-11 (KE Canister Sludge)Before Sonication Without Sieving (Microtrac X1OO,0.12 to 710 pm) .....................................4.11

Particle Size Distribution Data from KW Canister Sludge SamplesBefore Sonication Without Sieving (Microtrac X1OO,0.12 to 710 pm) .....................................4.l2

Particle Size Distribution Data from Residual Sludge Samples (from Fuel ElementTransport) Before Sonication Without Sieving (Microtrac Xl 00,0.12 to 710 Lm) ...................4. 13

Average Particle Size Distribution Results for Samples KES-M-13 (KE Floor Sludge)and KES-T-20 (KE Weasel Pit) After Sonication (Microtrac X 100, 0.12 to 710 pm) ...............4.14

Average Particle Size Distribution Results for Sample 96-04 (KE Canister Sludge)After Sonication (Microtrac X1OO,0.12 to 710 ~) ...................................................................4.l5

Average Particle Size Distribution Results for Sample 96-06 (KE Canister Sludge)Afler Sonication (Microtrac X1OO,0.12 to 710 pm) ...................................................................4.l6

Average Particle Size Distribution Results for Sample 96-11 (KE Canister Sludge)After Sonication (Microtrac X1OO,0.12 to 710 pm) ...................................................................4.l7

Average Particle Size Distribution Results for KW Canister Sludge SamplesAfter Sonication (Microtrac X1OO,0.12 to 710 pm) ...................................................................4.l8

Average Particle Size Distribution Results for Residual Sludge Samples (from FuelElement Transport) After Sonication (Microtrac X1OO,0.12 to 710 p.m)...................................4.19

Comparison of Average Particle Size Distributions for Sludge Types Before Sonication(Microtrac XIOO,0.12 to 710 pm) ..............................................................................................4.2O

Comparison of Average Particle Size Distributions for Sludge Types After Sonication(Microtrac X1OO,0.12 to 710 pm) ...........................................i..................................................4.2l

xii

8

a

4.17

4.18

4.19

4.20

4.21

4.22

4.23

4.24

4.25

4.26

4.27

Figures (Continued)

Integrated Particle Size Distribution for Samples KES-M- 13 (KE Floor Sludge) andKES-T-20 (KE Weasel Pit) After Sonication (Microtrac X1OOand Sieving,0.12 to 6350 ~) .........................................................................................................................4.22

Integrated Particle Size Distribution for Sample 96-04 (ICECanister Sludge)After Sonication (Microtrac X1OOand Sieving, 0.12 to 6350 pm) .............................................4.23

Integrated Particle Size Distribution for Sample 96-06 (KE Canister Sludge)After Sonication (Microtrac X1OOand Sieving, 0.12 to 6350 pm) .............................................4.24

Integrated Particle Size Distribution for Sample 96-11 (KE Canister Sludge)Afier Sonication (Microtrac X1OOand Sieving, 0.12 to 6350 pm) .............................................4.25

Integrated Particle Size Distribution for KW Canister Sludge SamplesAfter Sonication (Microtrac X1OOand Sieving, 0.12 to 6350 pm) .............................................4.26

Integrated Particle Size Distribution for Residual Sludge Samples (from FuelElement Transport) After Sonication (Microtrac X1OOand Sieving, 0.12 to 6350 ~m) .............4.27

Integrated Particle Size Distribution for K East Floor and Weasel Pit SludgeAfter Sonication (Microtrac X1OOand Sieving, 0.12 to 6350 pm) .............................................4.28

Integrated Particle Size Distribution for K East Canister SludgeAfter Sonication (Microtrac X1OOand Sieving, 0.12 to 6350 pm) .......... ..................................4.29

Integrated Particle Size Distribution for K West Canister SludgeAfter Sonication (Microtrac XIOOand Sieving, 0.12 to 6350 pm) .............................................4.3O

Integrated Particle Size Distribution for Residual Sludge (from Fuel Element Transport)After Sonication (Microtrac X1OOand Sieving, 0.12 to 6350 ~) .............................................4.3l

Comparison of Integrated Particle Size Distributions for Sludge TypesAfter Sonication (Microtrac X1OOand Sieving, 0.12 to 6350 ~) .............................................4.32

..Xlll

Tables

2.1 KE Floor and Weasel Pit Sludge Samples (1995) &alyzed .........................................................2.2

2.2 KE Canister Sludge Layer Samples (1996) ...................................................................................2.3

3.1 KBasin Samples Analyzed for Particle Size Distibution ............................................................3.2

3.2 Sieve Sizes Used for Wet and Dry Sieving. ..................................................................................3.3

3.3 Samples Analyzed Using the Microtrac Xl 00, Including Conditions and AnalysesUsed in Calculations ......................................................................................................................3.4

4.1 Wet and Dry Sieving Results on a Wt% Solids Basis ...................................................................4.2

xiv

1.0 Introduction

Approximately 2100 metric tons of irradiated N Reactor fuel have been stored at two retention basins onthe Hanford Site 100 K Area since the 1970s. During the time the waste has been stored, approximately44 m3 and 6.7 m3of sludge have accumulated in the K East (KE) Basin and K West (KW) Basin,respectively (Baker 1998). For the Spent Nuclear Fuel (SNF) Project, sludge is defined as any material inthe K Basins less than or equal to 6350 pm (%-in.). The sludge has been found within the spent fuelstorage canisters, as well as on the basin floor: and in associated pits. Characterization has shown thesludge is primarily uranium oxide, windblown sand, and aluminum and iron oxides and hydroxides.Minor components include organic and inorganic ion exchange materials, uranium metal particles, paintchips, and polychlorinated biphenyls. The concentrations of primary and minor components vary bylocation and depth.

The baseline plans are to remove the sludge, and then chemically treat it to meet Tank Waste RemediationSystems (TWRS) Waste Acceptance Criteria (Westra 1998). A critical component in developing thesludge retrieval and treatment process [led by Numatec Hanford Company (NHC)] is understanding theparticle size distribution (PSD) of the sludge. This understanding is necessary to design the sludgeretrieval and processing system and to address sludge transportation and storage safety issues due to thepotential reactivity of sludge. Furthermore, other sludge disposition pathways are being considered asalternative approaches to chemical treatment. For some of these alternatives, including interim storage,the sludge may be segregated or processed on the basis of particle size. Particle size, along with uraniummetal content of the sludge, largely determines the chemical reactivity of the sludge. Chemical reactivitywill constrain how the sludge may be handled, transported, and stored.

The information provided in this report is a compilation of the particle size distribution data generatedduring the K Basin sludge characterization campaigns (1993 through 1998). The overall goal of thisreport is to consolidate and integrate the data to develop the best possible particle size distribution curvesfor the various sludge types. During the particle size distribution analyses, different measurementtechniques were used to cover the large range of particles sizes in the K Basin sludge (i.e., submicron to6350 ~m). Specifically, sieving with wire mesh screens was used to segregate and quanti~ the particlesize distribution of the larger particles (250 to 6350 pm), and optical techniques were used to analyze theparticle size distribution of the smaller particles (below 710 pm). This report includes a description ofsamples analyzed, a description of the measurement techniques, and a presentation of the analyses thatcombines the two types of data gathered. Additional data tables and plots are included in the appendix.

,The PSD analyses were previously conducted during various sludge characterization efforts and involvedsamples of sludge collected from the KE Basin floor, the KE Weasel Pit, the KE North Loadout Pit, theKE canisters, and the KW canisters. Also analyzed were residual sludge samples generated during thetransport of KE and KW fuel elements. In performing the analysis of the data for this report, it becameapparent that comprehensive PSD data (i.e., distribution from 0.12 to 6350 pm) are limited, and theexisting data are not always fully representative of the individual sludge samples tested. Much of the datawas collected from discrete fractions of individual sludge samples. In addition, several techniques wereused to collect data that span the PSD range of interest. Because these techniques are not whollycompatible, assumptions were made to prepare the PSD curves for this document.

1.1

2.0 Sample History and Descriptions

Beginning in 1993, a systematic effort has been conducted to collect and characterize K Basin sludgesamples. These overall characterization efforts have included particle size determinations on a portion ofthe sludge samples. This section describes the samples and subsamples fi-omthese characterizationcampaigns that were analyzed for particle size data.

2.1 1993 KE Basin Floor and Pit Sludge Sampling

In May 1993, four samples were collected from KE Basin and transferred to the 222-S Laboratory andanalyzed for particle size distribution (Bechtold 1993). These samples consisted of clear water (i.e., nosuspended fine particulate) and up to -60 ml of sludge at the bottom of the sample vessels. The resultsof the initiaI analyses are reported in Bechtold (1993). Information provided by DESH (personalcommunication with Ron Baker, April 1999) indicates that one sample was collected from the west sideof the Weasel Pit (S3-032-01 ), one from the east side of the Weasel Pit (S3-032-02), one from theKE Basin floor (S3-032-03), and one from the North Loadout Pit (S3-032-04).

2.2 1995 KE Basin Floor and Weasel Pit Sludge Sampling

Fifteen samples were collected from the KE Basin floor and five from the Weasel Pit in August andSeptember 1995 (Makenas et al. 1996). Samples were collected by isolating a core of sludge with a metaltube. The isolated sludge cores were then collected in sample bottles by using a vacuum probe with aWin. orifice (specifically designed to exclude particles- greater than %in. in diameter). Next, the sampleswere shipped to the 222-S Laboratory and were resettled using basin water as a suspension media toexamine the settling rates and behavior. One sample fi-omthe KE Basin floor (KES-M- 13) and one fromthe Weasel Pit (KES-T-20) were then split into research layer subsamples (i.e., distinct layers that formedduring settling) for analyses. The four resulting research samples (KES-M- 13 Top, KES-M-13 Bet,KES-T-20 Top, and KES-T-20 Bet) were shipped to the Radiochemical Processing Laboratory (RPL, 325Building) for physical and theological properties analyses, which included particle size distribution.

In 1997, sieving was performed on archived samples KES-H-08, KES-M- 13 Top, KES-S- 19, andKES-T-20 Bot (Makenas 1999). Sample KES-H-08, which consisted mainly of organic and inorganic ionexchange material, was wet. The other samples were dry and consequently were re-wet with K Basinsupematant. Additionally, these samples were sonicated at 40 W for 90 sec to break up agglomeratesbefore wet sieving.

By June 1998, all remaining material from the 1995 sampling of the KE floor and Weasel Pit had beentransferred to the RPL for archiving. With the exception of sample KES-D- 14, all samples were driedprior to storage or they dried naturally during storage. In preparation for compositing sludge for processdevelopment testing, sample KES-D- 14 was vacuum dried at room temperature for approximate] y 5 days.A significant portion of the archived sludge samples was then used to prepare two composites (Schmidtet al. 1999). One composite (KE Floor Comp) was prepared using material collected from the floor, andthe other composite (KE Pit Comp) was prepared using material collected from the Weasel Pit. Thecomposites were then dry sieved to gain information on particle size and the content of organic ionexchange resin.

Table 2.1 shows the KE Basin floor and Weasel Pit sludge samples (and subsamples) for which particlesize analyses have been performed. In addition to the sludge samples, Table 2.1 also shows PuroliteNRW 100 and 400, which are nonradioactive organic ion exchange resins. These samples were analyzedto provide data to compare against sample KES-H-08.

2.1

Table 2.1. KE Floor and Weasel Pit Sludge Samples (1995) Analyzed

SampleI

Fraction of OriginalSample in Layer I

KE Floor SludgeKES-M-13 Top 50V0(estimate)KES-M-13 BottOnl 50’3 ””’k (estimate) I

1

KE Floor Comp l’oo% ‘KE Floor Ion Exchange Material

KES-H-08 100%Purolite NRW 100 NAPurolite NRW 400 NA

KE Weasel Pit SludgeKES-S-19 100%KES-T-20 Top 50% (estimate)KES-T-20 Bottom 50’%0(estimate)

I

KE Pit Comp l’oo% ‘

2.3 1996 KE Basin Canister Sludge Sampling

In April 1996, nine sludge samples were collected from different storage canisters located throughout theKE Basin (Makenas et al. 1997). Each canister sludge sample was collected using,the same method aswas used for the KE floor and Weasel Pit sludge samples in 1995. The samples were then transfemed tothe RPL.

The canister sludge samples were transferred to 2-L graduated cylinders, and settling studies wereconducted. Additional liquid collected with the samples was transfen-ed to 10-L glass carboys. Thecarboys containing the sample liquid were reexamined several weeks after sample transfer. A layer offine solids had settled to the bottom of the carboys containing the liquid from samples 96-06 and 96-15.Particle size analyses were performed on the settled solids collected from the bottom of the 96-06 carboy(96-06 Carboy Solids).

Following settling studies, three samples, designated as research samples, were collected from thegraduated cylinders in distinct layers that had formed during settling (see Table 2.2). The researchsamples were: sample 96-04 from a stainless steel canister; sample 96-06 from an aluminum canister; andsample 96-11 from a canister containing no fuel. Each recovered layer was treated as a unique sample. Ifenough sample (>100 ml) was present in the layer, the layer was collected by vacuum transfer. If thelayer was less than 100 ml, a pipet was used to collect it.

Sample 96-04 was split at the interface between the upper smooth and lower granular layers. The upperlayer (96-04 U) represented approximately 70’%of the sample by volume, while the lower layer (96-04 L)represented approximately 30°/0of the volume. Sample 96-06 was split into three layers: a fluffy upperlayer (96-06 U), a middle layer (96-06 M), and a lower layer (96-06 L). The upper layer representedapproximately 5°/0of the original sample volume; the middle represented 53°/0of the volume; and thelower represented 42% of the volume. Sample 96-11 was split at the interface between the thin lighter-colored fluffi upper layer (96-11 U), and the darker-colored bulk of the sample (96-11 L). The upperlayer represented approximately 7% of the sample volume, while the lower layer representedapproximately 93°/0of the sample volume. To ensure the layers did not mix, the interfaces between themwere collected as separate samples. These sample were then identified by the interface location (e.g., the

,

+

2.2

.

.

sample collected between 96-04 U and 96-04 L was identified as 96-04 U/L). Particle size analyses wereconducted on samples 96-04 U/L, 96-04 L, 96-06 M, 96-06 L, 96-06 Carboy Solids, and 96-11 L.

Table 2.2. KE Canister Sludge Layer Samples (1996)

Sample Fraction of Original I PSD Analyses ISample in Layer Performed?

96-04 U 70% NoI 96-04 U/L

i 1NA Yes

t 96-04 LI 1

30% Yes96-06 U 5% No96-06 U/M NA No96-06 M 53% Yes96-06 M/L NA No96-06 L 42% Yes96-06 Carboy Solids NA Yes96-11 U 7’% No

I

96-11 U/L NA No96-11 L 93% Yes

2.4 1996 KW Basin Canister Sludge Sampling

In December 1996, nine sludge samples were collected fi-omdifferent storage canisters locatedthroughout the KW Basin (Makenas et al. 1998). Each sludge sample was collected in a sample containerusing specially designed sampling equipment similar to that used to collect KE floor and Weasel Pit(1995) and KE canister sludge samples (1996). The sample containers were removed from the basin andtransferred to the RPL. The samples were then transfen-ed to 2-L graduated cylinders, and settling testswere conducted. The volume of settled sludge in each sample was small (-10-30 ml) compared to theanticipated volume of-500 ml.

Following settling studies, three of the samples (96-21, 96-23, and 96-24) were designated as researchsamples. Given the low sample volumes, it was not possible to recover the research samples in layers aswas done for the KE canister samples; therefore, the entire samples were wet sieved.

2.5 1998 K Basin Residual Sludge Generated from Fuel Element Transport

Five fuel elements were sampled in 1998 to recover coatings on the element surfaces and sludge trappedunder the cladding. While this work was primarily focused on the internal sludge and coatings samples,sludge (i.e., residual sludge) was observed in the shipping containers used to transport the fuel elementsfrom the K Basins to the Postirradiation Testing Laboratory (PTL, 327 Building). This residual sludgewas dislodged from the fuel elements during shipment, probably fi-omthe surface of the element, from thecenter coolant passage in the annular fuel slugs and/or from the damaged areas. During fuel elementretrieval, the residual sludge would likely be removed by the fuel washing process and would become apart of the K Basin sludge inventory. Two of the residual sludge samples (Rl and R5) were analyzed atthe RPL for selected physical properties, including particle size distribution. Sample R1 was collectedfrom an element stored in an aluminum canister in KE Basin open to the basin water, while sample R5was collected from an element stored in a sealed stainless steel canister in KW Basin. Therefore, inaddition to being stored in canisters composed of different materials, one fuel element was exposed tointrusion of windblown sand and other basin debris, while the other was not.

2.3

Samples RI and R5 dried prior to delivery to the RPL. The samples were resuspended in K Basin waterand sonicated before the particle size analyses were performed. After the residual sludge samples werewet sieved, optical analyses were performed on certain sieved fractions. Sample numbers were assignedto these samples based on the applicable sieve. For example, the material from sample R1 retained in theTyler 60 sieve was designated as R1-60; material that passed through all sieves and was captured by thebottom pan (also referred to as the receiver pan) was designated RI REC.

.

.

2.4

3.0 Particle Size Measurement Methods

Measurement methods used during sludge sample analyses included wet and dry sieving and opticaltechniques (Leeds and Northrup Microtrac X1OOParticle Size Analyzer and Brinkmann Model 2010Analyzer). Table 3.1 lists the samples analyzed and the particle size analysis methods used. Asillustrated in the table, some samples were analyzed by only one method; some were analyzed by bothmethods at the same time; and others were analyzed by both methods at different times (note: duringstorage between analyses, some samples dried out). Table 3.1 also lists ion exchange resins (PuroliteNRW 100 and NRW 400) tested for comparison with sample KES-H-08, which contained a highconcentration of organic ion exchange resin.

3.1 Sieving Methods

The sieving technique was used to separate and quantifj the larger particles (250 to 6350 pm) of selectedsamples. Stainless steel sieves manufactured by W.S. Tyler in conformance to ASTM El 1, ANSI, andISO 5653310-1 standards were used, with openings between 3350 ~m and 250 ~m. Table 3.2 lists theTyler sieves used and their aperture sizes, The sieve sizes used varied, depending on the anticipated dataneeds for the individual samples at the time of the analysis. As a result, the same size information is notavailable for all samples.

3.1.1 Dry Sieving

Dry sieving was only performed on KE floor and Weasel Pit composite samples. During dry sieving, theTyler 6 was place on top of the Tyler 8, with a bottom pan underneath. The entire mass of the dryKE Floor Comp or KE Pit Comp was measured and placed on top of the Tyler 6 sieve. The stacks wereshaken gently until all the material appeared (by visual inspection) to be retained on the appropriate sieveor to have passed through to the bottom pan. The masses on each sieve and in the bottom pan weremeasured. Material on the sieves was transfemed back to the original composite j ar, and the material inthe bottom pan was transfen-ed to a new stack of finer sieves. This process was repeated until all sieveswere used. The KE Pit Comp contained several large agglomerated chunks that would not pass throughthe Tyler 6 sieve. These chunks were easily broken up by applying light pressure. Laboratory records donot indicate agglomerated chunks were seen on any of the other sieves.

For dry sieving, wtYodry solids was calculated by dividing the mass of the material retained on each sieveby the total mass of material in each of the sieves and bottom pan. The original sample mass was notused in the dry sieving calculation, because some sample was lost as a fine aerosol during the sievingprocess. Approximately 5.2 wt’Yoof the KE Pit Comp was lost during sieving; KE Floor Comp sampleloss could not be calculated, but was estimated to be similar to the KE Pit Comp loss. The loss is likelyassociated with the smallest Iiaction. However, since definitive data are not available, the loss was notapportioned to any specific fraction within the calculations.

3.1.2 Wet Sieving

During wet sieving, the sieve set was stacked with the Tyler 6 on the top, followed by the other sieves inorder of decreasing size (the sieve sizes varied among the various tests). A known amount of settledsolids was sh.u-riedin basin water. In some cases, the slurry was either stirred or sonicated to break upagglomerates (see Table 3.1). The slurry was then poured through the stack of sieves. The same K Basinwater .used to prepare the slurry was used to wash the solids through each sieve. The accumulated slurry

3.1

Table 3.1. K Basin Samples Analyzed for Particle Size Distribution

Sample Analyzed Analyzed Dry Prior to Shearing prior to Agglomerates

by by Optical Analyses Analyses Observed on SievesSieving Technique

KE Samples from 1993 Sampling

S3-032-01 x No No NAS3-032-02 x No No NAS3-032-03 x No No NAS3-032-04 x No No NA ~

KE Floor SludgeKES-M-13Top x No No NAKES-M-13Top x Yes 40W190sec ProbableKES-M-13Bottom x No No NAKE Floor Comp x Yes No No

KE Floor Ion ExchangeMaterialKES-H-08 x No 40W190sec NoPuroliteNRW 100 x Unknown No NAPuroliteNRW 400 x unknown No NA

KE WeaselPit SludgeKES-S-19 x Yes 40W190sec NoKES-T-20Top . x No No NAKES-T-20Bottom x No No NAKES-T-20Bottom x Yes 40W190sec NoKE Pit Comp x Yes No No

KE CanisterSludge96-04UIL x Yes Stirred Yes, so data not used96-04 L x x No Stirred No96-06 Carboy Solids x No Stirred NA96-06 M x x No Stirred Possible96-06 L x x No Stirred Possible96-11 L x x Yes Stirred No

KW CanisterSludge96-21 x x No Stirred No96-23 x x No Stirred No96-24 x .x No Stirred No

ResidualSludge from Fuel ElementTransportR1 x Yes 40W190sec YesR1 REC x x Yes 40W190sec YesRI 60

.x x Yes 40W/90sec Yes

R5 x Yes 40W190sec NoR5 REC x x Yes 40W190sec No .

in the receiver pan was poured into a collection beaker. After the samples were washed through eachsieve, the sieves were air-dried (typically 2 to 6 hr) to remove any fi-eewater retained and then weighed.While these solids were air-dried to remove free water, they were not dried at elevated temperatures orover an extended period to remove interstitial water and waters of hydration. Therefore, the weightsmeasured after air-drying are referred to in this report as wet weights.sieving procedure is given in the test instructions.

A detailed discussion of the wet

3.2

Table 3.2. Sieve Sizes Used for Wet and Dry Sieving

.

.

Tyler Size US Mesh Equivalent Sieve Aperture (mm) Sieve Aperture (in.)

6 6 3.35 0.132

8 8 2.36 0.0937

14 16 1.18 0.0469

24 25 0.710 0.0278

32 35 0.500 0.0197

60 60 0.250 0.0098

For wet sieving, the VVWOwet solids was calculated by dividing the mass of the material retained on eachsieve by the mass of the original sample. The mass and the WtO/Oof the sludge in the receiver pan weredetermined from a mass balance between the initial settled solids sample mass and the sum of the sludgemasses retained on each sieve.

3.2 Optical Analyses

For most of the optical analyses, the Microtrac X1OOwas used; the Brinkrnann Analyzer was used for the1993 KE Basin sludge samples (S3-032-01 through -04).

3.2.1 Brinkmann Model 2010 Analyzer

Particle size analyses were conducted at the 222-S Laboratory cm KE sludge samples collected in 1993

(samples S3-032-01, -02,-03, and -04) using a Brinkmann Model 2010 Analyzer. For these analyses, thesamples were dispersed in their own associated liquid. The Model 2010 uses a laser eclipsing techniqueto measure the size of particles between 0.5 pm and 150 pm. The analyzer has a video camera forobserving the circulating particles and checking for agglomeration or aspect ratio. The data are taken asmaximum crossing diameters (i.e., signals with gradual rise and fall indicative of glancing eclipses arerejected). The volume distributions are derived by assuming spherical particles. The analyzer depends onthe particles being adequately dispersed and stirred so that all sizes get a fair representation in thescanning beam. Large, heavy particles that are not lofted high enough in the cell are not counted. Forvery dense particles, this could occur at sizes below 150 pm.

3.2.2 Microtrac X1OOParticle Size Analyzer

Particles between 0.12 pm and 710 ~m were analyzed at the RPL using a Microtrac Xl 00 instrument,which analyzes light scattered by the particles. For these analyses, a sample was added to a recirculatingfluid so that a stream of well-dispersed particles passed through the sample cell for analysis. TheMicrotrac X1OOinstrument measures the diffraction pattern of the light scattered by the particles with anarray of optical detectors to determine the size distribution. The flow rate of the recirculating fluid can bevaned, and an ultrasonic probe can be used to induce shear forces on the sample to breakupagglomerates. Both of these techniques were applied. During analysis of the KE canister sludge, astandard protocol was adopted, based on the effects of varying flow rate and applying shear forces, inwhich the particle size distributions of the samples were examined at 40 mlisec flow (90 see) before andafter sonication at 40 W. A new sample was then introduced and examined at 70 ml/see flow rate beforeand after sonication. Since this protocol was adopted after the KE floor and Weasel Pit sludge

3.3

characterization campa&ns (Makenas et al. 1996), it was not used for all sludge types. However, allsamples were analyzed before and after application of some level of sonication.

Table 3.3 lists the flow conditions and sonication power applied to each analysis. “As-Received” inTable 3.3. indicates a new subsample was placed in the instrument. Analyses were conducted for eachsample sequentially. For example, sample R5 RIEC, a new sample, was placed in the instrument andanalyzed at a flow rate of 40 ml/see (analysis 1). The sample was then sonicated at 40 W for 90 sec andanalyzed again (analysis 2). Anew sample was then placed in the instrument and analyzed (analysis 3).The resulting data, both tabular and plotted, are presented in the appendix.

As will be discussed in Section 4.0, calculations were performed to determine an average particle sizedistribution for each sample. The average particle size distributions for the samples were then used tocalculate an average particle size distribution for the different sludge types. Table 3.3 also indicateswhich analyses were used in the calculations for average particle size distributions.

Table 3.3. Samples Analyzed Using the Microtrac Xl 00, Including Conditions and Analyses Used inCalculations

~~ Calculations CalculationsKE Floor SludgeKES-M- 1 60 As-Received(a 1,4 2,513Top

2 60 25 W/120 S

3 60 40w/3oos4 60 As-Received5 60 25wi120S6 60 40W1300s

KES-M- 1 60 As-Received 1,4 2,513Bottom

2 60 25wi120S3 60 40 W1300s4 60 As-Received5 60 25wf120S6 60 40 w/3oos

KEWeaselPitSludgeKES-T- 1“ 60 As-Received 1,4 2,520 Tov

& WV LJVV/l,LWS

3 60 40W1300s I I I

4 60 As-Received5 60 25 W/120 S ,

16 I 60 I 40W1300sKES-T- \ I I 60 I As-Received 1,4 I 2,520Bottom I I

III

I II I I

3 60 40W1300s4 60 As-Received5 60 25w/120S6 60 40w/3oos

.

.

3.4

.

.

.

.

Table 3.3. (Continued) Samples Analyzed Using the Microtrac Xl 00, Including Conditions and AnalysesUsed in Calculations

Sample Analysis F1OW Sonication Analyses Analyses CommentsNumber Rate (power/duration) Averaged in Averaged in

(ml/see) Before AfterSonication SonicationCalculations Calculations

KE Canister Sludge96-04 1 60 As-Received 1,4,7 3,6,8 This samplewas not sieved, soU/L 96-04 L sievingresuks were used

for calculations.2 60 25 wJ125 S

3 60 40WI’300s4 60 As-Received5 606 60 25W190S7 40 As-Received8 40 40W190s9 7010 70 40 W190s

96-04L 1 60 As-Received 1,4 2,5 Analysis7 showslargeparticles,probablybubblesgeneratedbysonicationentrainedbythesystem

2 60at thishighflowrate.

25w/120s3 60 40w/3oos4 40 As-Received5 40 40W/90sec6 707 70 40W190sec

96-06 1 60 As-Received NosignificantsizereductionwithCarboy sonication

2 60 25 W/120 S

3 60 40 w/3oos96-06M 1 60 As-Received 1,2 3

2 40 As-Received3 40 40 w/90 s4 705 70 40w/90 s 4

96-06L 1 60 As-Received2 60 25W1120S i

J

3 60 40W1300s96-11L 1 60 As-Received 1,4 2,5

2 60 25Wi120S3 60 40 w/3oos4 40 As-Received5 40 40w/90 s6 707 70 40 W190s

3.5

Table 3.3. (Continued) Samples Analyzed Using the Microtrac Xl 00, Including Conditions and AnalysesUsed in Calculations

Sample Analysis Flow Sonication Analyses Analyses CommentsNumber Rate (power/duration) Averaged in Averaged in

(mUsec) Before AfterSonication Sonication

~ca’’u’ations I ca’culatiOnsIKW CanisterSludge96-21REC

70 As-Received 1,5,8 3,6,9

12 I 70 I 40w/90 s I13 I 40 I I

4 40 40W190s5 70 As-Received6 70 40 W190s

8 40 As-Received9 40 40w/90 s

96-23 1 70 As-Received 1 2REC

2 70 40wi90 s3 404 40 40W190s

96-24 1 As-Received 1 2REc

2 40w/90 s3 ,

14 I 40w/90 sResidualSludgefromFuelElementTransportRI-60 1 40 As-Received

12 I 40 I 40 w/90 s13 I 70 II 1 1

14 I 70 I 40 W190s5 40 As-Received6 40 40 W190s7 70 As-Received, !

]8 I 70 / 40w/90 s

NA(’) NA

I

I

Particlesabove 100 ~m appearto bereal, but not seen in as high ratios inanalysis 5. This could be Grafoilthat should have been removedduring sieving. Analyses 2 and 3recalculated to exclude particlesabove 200 ym, and analyses 6 and 9recalculated to exclude particlesabove 300 ~m. Followingrecalculation, all as-receivedsarrmles have similar PSD.

Dissolution or particle size reductionbelow detection limits was observedfollowing sonication in analysis 4.

High flow rates were required tokeep larger particles suspended.Dissolution or particle size reductionbelow detection limits was observedfollowing sonication m analyses 6and 8.

.

.

.

.

3.6

.

.

Table 3.3. (Continued) Samples Analyzed Using the Microtrac X1OO,Including Conditions and Analyses

Sample

RI REC

R5 REC

Used in Calculations -

Analysis Flow Sonication AnalysesNumber Rate (power/duration) Averaged in

(mlkec) BeforeSonicationCalculations

1 40 As-Received 1,5,72 40 40W190s3 70 t I

4 I 70 I 40 w/90 s5 40 As-Received6 40 40W190s7 70 As-Received8 70 40 w/90 s1 40 As-Received 1,3,5,7

2 I 40 I 40w/90 s3 I 70 I As-Received I

I !4 I 70 I 40W190s5 I 40 As-Received6 140. I 40w/90 s I,7 ] 70 As-Received

—--..-18 \ 70 I 40w/90 s(a) As-ReceivedunderSonicationindicatesa newsubsarmlewasdated i

Analyses CommeutsAveraged inAfterSonicationCalculations2,6,8

I

II

1r Dissolution or particle size reductionbelow detection limits was observedfollowing somcat]on m analyses 2,

I

I

I

I I

the instrument for this and subsequent analyses.(b) NA, sampleRI -60 not includedin averages.

3.7

4.0 Results

In the analyses of particle size distribution for K Basin sludge samples, the results from sieving provideda distribution based on the mass of particles in different size ranges, while the results fi-omopticaltechniques provided a distribution based on the volume of particles in different size ranges. Since onetechnique uses mass and the other volume, caution must be used when trying to combine the data sets.The approach employed in this report to integrate the two data types was to assume the density of theparticles was uniform from 0.12 to 6350 pm. With that assumption, the volume percent of particles in agiven range equals the mass percent in that range. The results from individual data sets are given inSections 4.1 through 4.5, then the integrated PSD results are presented in Section 4.6.

4.1 Results from Sieving

The wet and dry sieving results are presented in Table 4.1. Sieving results for KE Basin samples showcomparable results for sludge samples fi-omsimilar areas of the basin. The KE floor samples areprimarily fine particles (below 710 ~m); the Weasel Pit samples have a higher wW. of larger particles;and the canister samples have the largest content of particles above 710 ~m. Theseresults are presentedin Figure 4.1. The KE canister sludges (96-04 L, 96-06 M, and 96-06 L) average 57 WtO/Obelow 710 pm,10 to 20 wtYobetween 710 ~m and 1180 gm, and 6 to 12 wt’Yobetween 2360 pm and 6350 ~m. Sample96-11 L is from a KE canister containing no fuel, and compares well with the KE Floor Comp sample.Samples 96-11 L and KE Comp are composed primarily (99’7’.)of particles below 710 ~m. SampleKES-H-08 does not compare well with the other floor samples due to its high ion exchange materialcontent. The integrity of sample KES-M- 13 Top was compromised due to a high number of agglomeratesthat formed during the drying of the sample that occurred during archiving. The Weasel Pit samples(KES-S-19, KES-T-20 Bet, and KE Pit Comp) all contain 82 to 87 wt% particles below 710 ~m, 8 to12 wtYoparticles between 710 ym and 1180 pm, and 4 to 5 wt’XObetween 1180 pm and 2360 pm.

Results of sieving tests also showed the individual KW canister sludge samples (96-21, 96-23, and 96-24)have very similar particle size distributions. The samples all contained 81 to 89 wt’Yoparticles below710 pm. Visual inspection during the sieving indicated that most of the material above 710 ~m wasGrafoil (a graphite gasketing material) used to seal the lids on the fuel storage canisters.

Sieving results suggest that residual sludge samples (Rl and R5) were the finest material in the basins.The results for sample R5 indicate that all the solid particles or agglomerates were less than 500 pm indiameter, whereas 49 wt% of solids in sample R1 were above 250 pm. The large chunks in R1 could becrushed by applying moderate pressure with a pair of tongs. These observations suggest that the largeparticles were agglomerates most likely generated by partial drying of R1 before the samples werereceived at the RPL. Thus, it is speculated that the R1 and R5 samples may have had similar wet sievingdistributions if they had not dried prior to this testing. Based on these results, all of the particles in theresidual sludge are anticipated to be below 500 pm.

As described above, K Basin water was used as the rinsing fluid during the wet sieving. The as-receivedK Basin water used for sieving the R1 and R5 samples was clear and colorless. Following the rewettingand sieving work, the rinsing fluid was clear and green. The green color suggests that either some of thesolids in the RI and R5 samples have dissolved or some suspended particles are present that are too fineto settle by gravity.

4.1

Table 4.1. Wet and Dry Sieving Results on a Wt% Solids Basis

SampleSieving Tyler 6 Tyler 8 Tyler 14 Tyler 24 Tyler 32 Tyler 42 Tyler 60 Receiver

Method (3350 pm) (2360 pm) (1180 pm) (710 pm) (500 pm) (335 Km) (250 pm) Pan

KE Floor SludgeKES-M-13Top(’)

Wet NA(b) NA

KE Floor c

Comp

.

KEs-H-08(d)KE Weasel Pit

~:rn:.p : : : ‘: : : : : ‘KE Canister Sludge96-04 L Wet o 12 22 9 NA NA NA 5696-06 M Wet 5 6 20 11 NA NA NA 58

96-06 L Wet 3 3 15 22 ~ NA NA NA 58

96-11 L Wet o 0.1 0.7 1 NA NA NA 98KW Canister Sludge

96-21 Wet 1 0 4 6 NA NA NA 89

96-23 Wet 6 3 8 3 NA NA NA 81

96-24 Wet 12 0 3 2 NA NA NA 83Residual Sludge from Fuel Element Transport

R1 Wet 30 5 4 3 NA NA 6 51R5 Wet o 0 0 0 0 NA NA 100

(a) Sample KES-M-I 3 Top contained a large number of agglomerates formed by drying during the archiving process; thereforesieving results are suspect.

(b) NA-Not Applicable, not all sieve sizes used for all sampIes.(c) A Tyler 5 screen (3960 V.) was used in place of the Tyler 6 screen.(d) Sample KES-H-08 is primarily ion exchange material and therefore is not representative of the other floor samples,

4.2 Brinkmann Analyzer Results

The shape of the number distribution histograms suggest a significant number of particles existed below0.5 pm that could not be quantified. one sample (S3-032-02) indicated significant volumes greater than150 pm existed. Results are plotted in Figure 4.2.

4.3 Microtrac X1OOResults on Individual Samples Before Sonication(0.12 to 710 pm)

Sample analyses conducted by laser scattering (Microtrac Xl 00) were averaged to generate an averageparticle size distribution for each sample before sonication. These plots are presented in Figures 4.3through 4.8. The error bars in these figures indicate the highest and lowest value for each range (high-lowbars). A line is used to connect the points, but this line only provides direction to the next point andshould not be used to interpolate values between points.

For samples that were split into research layers (96-04, 96-06,96-11, KES-M- 13, and KES-T-20), theaverage curves for each research layer were combined in proportion to the estimated volume percent ineach layer to calculate the originaI sample average. The data in Tables 2.1 and 2.2 were used in thiscalculation. Because no information was available on the relative volumes of the top and bottom layers of

4.2

KES-M-13 and KES-T-20, it was assumed that these samples were evenly divided. This approach seemsreasonable since there was very little difference between the top and bottom layers.

No particle size distribution data were available for the upper layers of the KE canister research samples;therefore, for sample 96-04, the 96-04 U/L layer was assumed to be representative of the upper layer of96-04. For sample 96-06, the 96-06 Carboy sample was assumed to be representative of the upper layerof 96-06.

4.4 Microtrac X1OOResults on Individual Sludge Samples After Sonication(0.12 to 710 pm)

The calculations described in Section 4.3 were repeated using the laser scattering particle size distributiondata following sonication. These data are presented in Figures 4.9 through 4.14. Comparing figures forthe same samples before and after sonication (for example, Figures 4.4 and 4.10, respectively) shows, ingeneral, sonication shifts the curves to the lefl, (i.e., to smaller particle sizes). In addition, sonicationreduces the error bars. Therefore, sonication both reduces the particle size and produces a more uniformparticle size distribution between duplicate sludge types.

4.5 Microtrac X1OOResults for Sludge Types Before and After Sonication(0.12 to 710 pm)

Average particle sludge distributions were calculated for the different sludge types (KE canister sludge,KW canister sludge, residual sludge, KE floor sludge, and KE Weasel Pit sludge) using the average of theresults from the individual samples (Figures 4.3 through 4.14). Because KES-M- 13 and KES-T-20 werethe only KE floor and Weasel Pit samples analyzed, they were assumed to be representative of the KEfloor and KE Weasel Pit averages, respectively. The particle size distributions for samples 96-04 and96-06 were averaged to generate an average particle size distribution for KE canister sludge fromcanisters containing fuel elements. Sample 96-11 was collected from a KE canister that did not containfuel; thus, its particle size distribution was very different from 96-04 and 96-06 and was not averagedwith 96-04 and 96-06. Data tlom samples 96-21, 96-23, and 96-24 were combined to generate theaverage for KW canister sludge, and sample R1 and R5 data were combined to calculate the average forresidual sludge.

The resulting particle size distributions for the different sludge types before and after sonication areplotted in Figures 4.15 and 4.16 respectively. These figures are complicated by overlap in the error bars.Based on the overlap in the high-low bars in Figure 4.15, there is no significant difference in particle sizedistributions between any of the sludge types below 100 ym prior to sonication. It appears that above100 pm, the KE canister and KW canister sludges have a higher percentage of large particles.

Figure 4.16 shows that after sonication the residual sludge is the finest material, followed by the KWcanister sludge. The KE canister sludge, KE Weasel Pit sludge, and KE floor sludge are all very similar.It appears the KE floor sludge and sludge from KE canister 96-11 (without fuel) maybe slightly finerwith a very tight distribution of particles centered around 10 ~m. It is interesting to note that the particlesize distributions of sample 96-11 and the KE floor sludge are similar. This observation is also valid forthe sieve data. The similarity is likely because the bottom of the KE canister is open to the KE floor.

4.3

4.6 Combined PSD Results from Sieving and Microtrac X1OOData(0.12 to 6350 pm)

The average particle size distribution calculations were repeated factoring the sieving data with the laserscattering data. This calculation was performed by multiplying the volume percent data reported from theMicrotrac X1OOby the mass fraction of material passing through the finest sieve. For example, sample96-06 M contained 58 wtYo(0.58 mass fraction) particles below710 ym, according to the sieve data.Based on the Microtrac Xl 00 data (analysis 1), the sample also contained 4.88 vol% patiicles below0.972 ~m. Therefore, combining the two data sets, the percentage of particles below 0.972 pm is 2.83%(4.88 x 0.58= 2.83). As stated previously, this calculation is only valid by assuming the density of theparticles above 710 pm is the same as the density of the particles below 710 pm. Since wtYoand VOWOare the same for a sample with uniform density, the resulting plots are then both WtO/Oand VOlO/O.

In some cases, sieving data were not available for all the samples analyzed using the Microtrac X1OO,andin some cases sieving data were not valid because the samples had dried. Sample 96-04 U/L was notsieved, so the 96-04 L sieving results were used for calculations involving this sample. SampleKES-M- 13 was sieved, but very little material was observed on the sieves. Large agglomerates that brokeup easily after the material was dried were also observed. As a result, the KE Floor Comp sieving resultswere used for calculations involving KES-M- 13. Use of the KE Floor Comp sieving results should alsoreduce errors in sample inhomogeneity, since the KE Floor Comp represents a much larger material mass(-120 g for KE Floor Comp versus 1.5 g of ICES-M-13 sieved). While sample KES-T-20 was sieved, theresults were very similar to those for the KE Pit Comp. Since the KE Pit Comp represents a much greaterfraction of Weasel Pit material than KES-T-20 a].one (-280 g for KE Pit Comp versus 27 g of KES-T-20sieved), the KE Pit Comp sieving data were used for calculations involving KES-T-20.

The sample RI sieving results suggest that agglomerates were formed during the drying of the sampleprior to delivery to the RPL and that the agglomerates formed in R1 were not broken up during thesieving process. As a result, the R1 sieving results were not used in these calculations. The R5 sievingresults were used for calculations of the R 1 particle size distribution.

*

The results of the calculations combining the sieving and laser scattering (following sonication) data areshown in Figures 4.17 through 4.22. Average particle size distributions were then calculated for thedifferent sludge types (KE floor sludge, KE Weasel Pit sludge, KE canister sludge, KW canister sludge,and residual sludge,) using the average sample plots (Figures 4.17 through 4.22). The resulting averagesludge types are presented in Figures 4.23 through 4.26 and compared in Figure 4.27.

As shown in Figure 4.1, sieving results indicate that the KE canister sludge (96-04 L, 96-06 M, 96-06 L)has the greatest distribution of larger particles in sludges examined from the KE Basin. The Weasel Pitsludge is finer than the canister sludge, and the floor sludge is finer than the Weasel Pit sludge. Figure4.16 shows that using the Microtrac Xl 00 data alone, the KE canister sludge, KE Weasel Pit sludge, and

,

KE floor sludge are all very similar. However, adding the sieving data forces the trend on the newcalculated data set presented in Figure 4.27. .

Figure 4.27 suggests that after sonication, the ICEcanister sludge contains the greatest distribution oflarge particles above 1000 pm. The particle size distribution of the KE Weasel Pit sludge is comparableto that of the floor sludge below -250 pm. The ICEfloor sludge is finer than both the KE Weasel Pitsludge and the KE canister sludge. The residual sludge remains the finest material of those examined.The particle size distribution for the residual sludge is not affected by the addition of sieving data sinceR1 and R5 were calculated using the R5 sieving data, and all material in R5 was below 500 ~m.Comparing the plots for the KW canister sludge in Figures 4.16 and 4.27 shows that below 200 pm this

4.4

sludge is finer than all but the residual sludge. However, adding the sieving data to the KW canister plotresults in a very broad particle size distribution. This wide distribution is the result of friable Grafoilpresent in the samples. Removing the Grafoil would result in a particle size distribution similar to thatfound by laser scattering as shown in Figure 4.16.

4.5

Figure 4.1. Comparison of Sieving Results for KE Basin Sludges

100

95

90

85

80

75

70

65

60

55

50

0

% Floor Sludgr (and 96-llL)

WeaselPlt Sludge

1! 1

Ca.msterSludge

1000 2000 3000 4000 5000 6000 7000

+ KE Floor Comp

+ KE Pit Comp

+ KES-S-19

— KES-T-20 Bottom

+ 96-04 L

+ 96-06 M

+ 96-06 L

+96-11 L

Particle Size (urn)

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-

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1

!\

I

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00

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A

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.

.

.

.

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) \i

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o 0 0m =1-

0 0m N

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0

4

40

4.17

100

90

80

70

60

50

40

30

20

10

0

.—.

I

Average Particle Size Distribution Results for KW Canister Sludge SamplesAfter Sonication (Microtrac X1OO,0.12 to 710 urn)

II_-+...-,-.

d

/

.-

7..—

—

—

/

/.—

7

..

.-

—

,

,

——.

—-

—

z

—.

—

—

—

—

.

.

+96-21

+ 96-23

+ 96-24

10 100

Particle Size (urn)

& *

1000

1I

I

\ I I

I

I

,

I ‘!! I

I I I

1

I ! II

I ,( \

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00

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0 0a

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0 0*.C-4

mim.ra~ aqpm~

4.19

100

90

80

70

60

50

40

30

20

10

0

Figure 4.15. Comparison of Average Particle Size Distributions for Sludge Types Before Sonication(Microtrac X1OO,0.12 to 710 urn)

—.——

1

T

//

k—.——/

L

10

—..-

—

1000

.- .—. .—...——. .-

+ K West Fueled Canister

+ U ‘-~+ ~l~fi- cl~~~geAxLa LALUUAdLuu

+ K East Pit Sludge

+ K East Empty Cansker

+ K East Fueled Canister

--- Res&al Slu&e

Particle Size (urn)

.

.

.

4- +-J

23Wwk4M

H1 , 1 1 , I i

( I I I

1 1I ! ! !

I

I

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4.21

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w Ill- I1 I 1 .,

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00

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4

0

.

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I

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0 0 0 0m w-

0 0P-) ml

A

b.P

100

90

80

70

60

50

40

30

20

10

0

..

.-.

Figure 4.19. Integrated Particle Size Distribution for Sample 96-06 (KE Canister Sludge)After Sonication (Microtrac X1OOand Sieving, 0.12 to 6350 urn)

t“

..

7#

10

.—.

r

—

----

%-06 Carboy sampleusedto ~

{—...-.

.. . . . .

F.-

.-

ive average jut not

lsed to calculate high-low range

I100 1000 10000

Particle Size (urn)

1~96-06 I,.-—––––..... ,

I ,

I ! I I!

I t I

f I I I! I I 1 II I I I I I

II ,

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it +

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I

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00

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.Pw

100

90

80

70

60

50

40

30

20

10

0

Figure 4.26. Integrated Particle Size Distribution for Residual Sludge (from Fuel Element Transport)After Sonication (Microtrac X1OOand Sieving, 0.12 to 6350 urn)

1

/

A

*

/

100

. -+-

1000

-

+ Residual Sludge

.

0000

000

00

0

d

IIII I I ! I

I I I i I

I \I I I \ 1 I

I L I ,+

.

I

0

5.0 References

Baker, R. B., T. L. Welsh, B. J. Makenas, and K. L. Pearce. 1998. “Sampling and Analysis Plan forSludge Located on the Floor and in the Pits of the 105-K Basins.” HNF-3556, Duke Engineering&Services Hanford, Richland, Washington.

Bechtold, D. B. 1993. “Analysis of 105 KE Basin Sludge Samples.” WHC memo 1211O-PCL93-O69 toM. A. Meier dated July 17, 1993. Westinghouse Hanford Company, Richland, Washington.

Makenas, B. J., T. L. Welsh, R. B. Baker, D. R. Hansen, and G. R. Golcar. 1996. “Analysis of Sludgefrom Hanford K East Basin Floor and Weasel Pit.” WHC-SP-1 182, Westinghouse Hanford Company,Richland, Washington.

Makenas, B. J., T. L. Welsh, R. B. Baker, E. W. Hoppe, A. J. Schmidt, J. Abrefah, J. M. Tingey, P. R.Bredt, and G. R. Golcar. 1997. “Analysis of Sludge from Hanford K East Basin Canisters.”HNF-SP- 1201, Duke Engineering& Services Hanford, Richland, Washington.

Makenas, B. J., T. L. Welsh, R. B. Baker, G. R. Golcar, P. R. Bredt, A. J. Schmidt, and J. M. Tingey.1998. “Analysis of Sludge tiom Hanford K West Basin Canisters.” HNF-1 728, Rev. O,Fluor DanielHanford, Inc., Richland, Washington.

Makenas, B. J., Ed. 1999. Supplementary Information on K-Basin Sludges. HNF-2367, Rev. O, FluorDaniel Hanford, Inc., Richland, Washington.

Schmidt, A. J., C. H. Delegard, K. L. Silvers, P. R. Bredt, C. D. Carlson, E. W. Hoppe, J. C. Hayes, D. E.Rinehart, S. R. Gano, and B. M. Thornton. 1999. “Validation Testing of the Nitic Acid Dissolution StepWithin the K Basin Sludge Pretreatment Process,”PNNL-12120, Pacific Northwest National Laboratory,Richland, Washington.

Westra, A. G., T. A. Flament, and L. de Lamartinie. 1998. “K Basin Sludge Treatment ProcessDescription.” HNF-2735, Rev. O,Numatec Hanford Corporation, Richland, Washington.

5.1

*

.

Appendix

Supporting Particle Size Data from Microtrac X1OOAnalyses

RI 60 Volume Dktribution Data

Sample analyzed As-Received 40 mkec (1), then sonicated at 40 W and analyzed at 40 mlkc (2), then flow increasedand analyzed at 70 mlkec (3), then sonicated at 40 W and analyzed at 70 mlkec (4).

Duplicated several days later, As-Received 40 mlkec (5), then sonicated at 40 W and analyzed at 40 ml/see (6), then newsample analyzed at 70 mlkec (7), then sonicated at 40 W and analyzed at 70 mkec (8).

High flow rate required to prevent settling1 2 3 4 5 6 7 8

As-Received 40 W 40W As-Received 40 W As-Receiv 40 W

Particle size 40 ml/see 40 mlkec 70 mlkec 70 ml/see 40 mVsec 40 ml/see 70 ml/see 70 mkecParticle size 1 2 3 4 5 6 7 8

704.000592.000497.800418.600352.000296.000246.900209.300176.000148.000124.500104.70088.00074.00062.23052.33044.00037.00031.11026.16022.00018.500f5.56013.08011.0009.2507.7786.5415.5004.6253.8893.2702.7502.3121.9451.6351.3751.1560.9720.8180.6880.5780.4660.4090.3440.2890.243

0.2040.1720.145

0000000000

1.083.8

6.377.21

6.36.1

4.674.4

4.566.175.76

4.84.934.462.542.984.653.151.531.160.9

0.620.41

0000

0.360.430.51

0.60.680.73

0,80.890.971.071.141.192.08

0000000000000

1.253.5

5.965.043.993.344.09

3.93.5

3.773,451.972.424.083.091.72

1.51.33

10.710.57

0.560.680.931.271.621.932.24

2.63.043.684.364.463.93

2.962.2

3.36

0000000000000

0.43.037.125.813.042.013.444.685.064.8f2.371.522.314,353.262.021.78

1.50.990.740.51

0.50.61.3

1.611.852.011.782.793.694.675.415.374.29

2.50.88

0

0000000000000

0.993.945.373.262.091.813.234.173.88

3.41.981.452.264.142.771.631.611.470.990.690.480.540.761.691.932.012.06

23.364.876.547.577.044.89

2.40.73

0

00

0.631.913.814.453.833.033.033.473.824.184.144.32

4.14.273.333.083.023.672.972.212.242.231.461.872.92

1.90.920.750.650.460.32

0000

0.350.450.560.680.630.991.221.511.721.831.781.773.5

0000000

0.6100

0.471.5

3.123.041.851.641.762.924.02

3.91.911.12

1.52.792.992.932.321.12

0.91.7

2.161.160.490.340.712.146.062.690.770.593.137.75

11.479.885.041.51

0000

000

2.462.041.91

22.332.64

2.72.422.252.092.252.352,742.36

2.32.272.752.281.822.012.121.421.832.972.111.151.040.970.740.520.410.430.570.88

1.31.681.96

2.22.522.943.624.374.453.682s41.863.75

000000000

0.340.691.512.212.07‘1.481.511.672.593.343.291.691.021.372.472.482.622.281.170.9

1.551.891.050.44

00.511.424.412.991.361.083.538.32

12.5911.937.062.590.58

000

I

. . ,

r- u) ‘d- m

●

D

●

●

●

o

0

0-00

a)0 N

05

.

o

.

a)Q

Emu)o

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.

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n

EL

00

0 .v

r-

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o/~WNTIOA

ml o

. . , . . .

8

●

●

●

●

0000

v

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00

00“

0 .7

a)N.-

(Y)

co ml o

ml

.

m

I

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i

I

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0 00 a v ml 0

0 .~0

000

a)0 N.-Ocn

0 .T

0/0 wu’lloA

1-

r

ml 0 co

0/0

(0 d- OI 0

wN’l[oA

00z

0

00

00“

0 .Y

w-

0

.

RI REC Volume Distribution Data

v

.

.

Sample analyzed As-Received 40 mkc (1), then sonicated at 40 W and analyzed at 40 mlkec (2), then flowincreased and analyzed at 70 mkec (3), then sonicated at 40 W and analyzed at 70 mkec (4).

Duplicated several days later, As-Received 40 mlkec (5), then sonicated at 40 W and analyzed at 40 mlkec (6),then new sample analyzed at 70 ml/see (7), then sonicated at 40 W and analyzed at 70 mlkec (8).

1 2 3 4 5 6 7 8As-Received 40 W 40W As-Received 40 W As-Receiv 40 W

Particle size 40 ml/see 40 mksec 70 mlkc 70 mllsec 40 mlkec 40 mlkc 70 mllsec 70 mllsecParticle size

704.000592.000497.800418.600352.000296.000248.900209.300176.000148.000124.500104.70088.00074.00062.23052.33044.00037.00031.11026.16022.00018.50015.56013.08011.0009.2507.7786.5415.5004.6253.8893.2702.7502.3121.9451.6351.3751.1560,9720.8180.6880.5780.4860.4090.3440.2890.2430.2040.1720.145

10

0000000000

0.531.523.064.275.595.235.887.19

10.439.026.295,725.413.574.51

6.63.981.811.260.69

000000

“oo000

0.320.580.931.181.211.010.821.39

2000000000000000

0.631.282.433.946.556.295.075.435.814.175.66

96.053.212.872.351.260.48

0

0000

0.490.771.141.652.32

3.34.42

4.73.72

2.191.2

1.62

3000000000000000

0.571.172.213.596.096.125.175.635.924.11

5.58.896.093.232.822.26

1.20.47

0000

0.310.s2

0.81.17

1.72.383.394.574.883.862.261.261.86

40000000000000000

0.51.15

2.34.685.424.935.42

5.653.985.619.616.833.623.122.511.370.56

000

00.480.761.091.492.042.793.955.335.594.17

2.221.141.69

50000000

0.660.721.01

1.281.582.04

3.24.435.685.035.868.06

11.617.724.024.03

6.045.494.93

3.51.5

1.181.680,72

000000000000

0.822.182.83

1.70.5

00

60000000000000

0.330.460.881.28

2.13.325.695.794.915.275.37

3.64.797.925.643.022.632.211.360.670.35

00.

0.320.45

0.60.791.041.442.043.024.274.944.513,242.223.51

7000000000

0.640.520.560.721.212.03

3.43.8

4.645.999.18

8.46.175.996.064.124.966.754.072.191.961.290.38

0000

00000

0.430.941.782.813.252.621.460.750.91

80000000000000

0.310.42

0.70,981.572.544.55

.

4.934.444.965.173,514.768.045.78

3.12.682.181.29

0.6000

0.370.610.911.241.622.132.81 43.865.14

5.64.743.11

23.35

I

—

m

o cc’ co w o

o“o“o

o0

a)

o .Y

.

r-

% GUHI1OA

.

<

a)EE(uCn

w

of

r

r

000T-

:

0 .-Oco

a)

0 .Y

0/0 ewnloA

1.

,

L

I

L

L

0000

0 .8

00

0 .Y

v

0

*

.

n

EA

a)Nzc1)

.

m co d- Cw 0

0/0alu’lloA

ml=F-

EA

a)0 N.-0(0

Emu)

DC

w

1=

ml

-t

I

0“0“o

n

E3-

a)0 N.-0

0 .Y

u)

R5 REC Volume Distribution Data

Sample analyzed As-Received 40 ml/see(1), then sonicated at 40 W and analyzed at 40 mkec (2), then flowincreased possibly new sample and analyzed at 70 mlkec (3), then sonicated at 40 W and analyzed at 70 mVsec (4).

Duplicated several days later, As-Received 40 ml/see (5), then sonicated at 40 W and analyzed at 40 mlkec (6), then

new sample introduced and analyzed at 70 mkec (7), then sonicated at 40 W and analyzed at 70 mlkec (8).

‘1 2 3 4 5 6 7 8

As-Received 40 W As-Received 40 W As-Received 40 W As-Receiv 40 W

Particle size 40 mllsec 40 mkec 70 mlkiec 70 ml/see 40 ml/see 40 mlk.ec 70 mkec 70 mlkec

704.000

592.000

497.800

418.600

352.000296.000

248.900

209.300176.000

148.000

124.500

104.700

88.00074.000

62.230

52.33044.000

37.000

31.11026.160

22.00018.500

15.560

13.080

11.000

9.2507.7786.541

5.5004.625

3.8893.270

2.750

2.312

1.9451.635

1.3751.156

0.9720.818

0.6880.578

0.4860.409

0.344

0.2890.243

0:204

0.172

0.145

000000000000000000

0.471.47

2.59

3.48

5.13

6.264.65

6.7412.15

9.46

5.495.064.282.42

0.97

0.37

00

00

0.370.56

0.89

1.44

2.26

3.48

4.89

5.364.33

2.551.34

1.54

00000000000000000000

1.343.12

3.452.44

1.914.22

10.98

8.894.514.19

5.124.22

1.78

0.69

0.641.23

2.821.29

0.490.42

1.554,22

7.85

9.72

7.82

3.931.16

0

0

0

00000001

4.22

8.387.09

3.581.44

0.760.51

0.50.42

0.430.470.71

0.81

0.93

1.462.06

1.792.91

5.694.71

2.642.73

2.6

1.93

1.2

0.77

0.590.57

0.650.79

0.941.13

1.42

1.87

2.5

3.4

4.414.83

4.43

3.412.62

4.5

00000000000000000000

0.85

1.9

2.69

2.48

1.9

3.54

8.497.43

4.684.58

4.94

3.691.86

1.15

1.382.27

3.491.01

0.390.55

3.147.16

10.42

9.88

6.432.87

0.83

00

0

0000000000000

0.41

0.410.53

0.590.641.29

2.432.97

3.2

4.3f

5.19

3.87

5.579.967.75

4.514.18

3.672.3

1.1

0.53

0.320

00.37

0.490.66

0.951.42

2.11

3.19

4.52

5.244.86

3.572.53

4.16

000000000000000

0.40

0.360.641.59

2.32

2.38

2.73

3.07

3.15

5.7410

6.43

3.934.91

5.563.361.37

0.73

0.941.65

2.490.77

0

0.311.514.1

7.51

9.23

7.55

3.991.28

0

0

0

00000000000000

0.310.41

0.45

0.620.941.76

2.23

2.59

3.84.89

3.18

5.59.9

7.75

4.574.29

3.812.43

1.2

0.60,380.34

0.390.51

0.67

0.91,251.79

2.553.67

55.655.13

3.72.51

3.73

000000000000000

0.530

00.421.13

1.85

2.07

2.39

2.48

2.284.27

8.78

6.613.984.56

5.14

3.581.71

1.01

1.24

2.08

3.321.03

0.4

0.492.56

6.189.61

9.78

6.65

‘3.010.86

00

0

g

QEmu)

g’

mlI

r

●

●

B

●

o

CNa)EE03u)

,

.

!--

0

t

)

0 a) CD w N 0

T-

a)0 N

OU5

0 .v-

o/~wJnloA

mr

●

●

.

0

.

d-

.

a

r—

I

IL

tr

1 mr -

L1

c

1-

t

0000

0

00

a)N

z

CD *

0/0 wJn[oA

ml o

.

,

96-21 REC Volume Distribution Data

Sample tested at 70 ml/see (1) then solicated and measured at 70 ml/see (2) then slowed flow to 40 mlkec (3) Then sonicated at40W for 90 seconds and Measured at 40 mksec (4).

Duplicate tested at 70 ml/see (5) then solicated and measured at 70 ml/see (6) then slowed flow to 40 mlkec (7) system perturbedpossibly sample changed and analyzed at 40 ml/see (8) Then sonicated at 40W for 90 seconds and Measured at 40 mlkec (9).

1 2 3 4 5 6 7 8 9

First DuplicateAs-Received 40 W 40W As-Received 40 W 40W

Particle size 70 mlkec 70 ml/see 40 mlkec 40 mlk.ec 70 ml/see 70 mkec 40 mkec 40 mlkec 40 mkec704.000592.000497.800418.600352.000

296.000248,900209,300176.000148.000124.500104.700

88.00074.00062.23052.33044.00037.00031.11026.16022.00018.50015.56013.08011.000

9.2507.7786.5415.5004.6253.8893.2702.7502.3121.9451,6351.3751.1560.9720.8180.6880.5780.4860.409

0.3440.2890.243

0.2040.1720.145

11.434.390.830.350.656.23

24.4821.54.270.64

00

0.681.461.661.250.590.410.440.740.860.830.981.060.730.961.571,090.58

0.50.440.32

000000

0.320.390.48

0.50.520.57

0.650.760.850.840.771.25

26.770.91

000

2.2929.4611.01

00000

1.652.731.11

000

0.721.371.521.471.160.630.851.71

1.61

0.820.580.33

00000

0.420.60.8

0.960.990.890.84

0.931.061.040.740.44

0.6

27.610.44

000

1.3425.4114.04

00000

0.972.341.330.4

00.441.021.27

1.11.161.210.831.081.841.480.920.840.650.38

00000

0,430.6

0.770.910.991.011.12

1.381.6

1.460.88

0.40.35

000000000000000000000000

1.198.62

24.1317s48.677.486.85

5.23.48

2.41.9

1.771.85

1.91.751.411.020.720.52

0.40.33

0000

0.87

0000000000000

0.361.32

3.24.1

4.745.016.345.484.474.935.173.414.29

6.74.642.542.362.181.530.880.53

0.40.40.5

0.640.780.911.051.261.57

2.092.753,092.892.251.813.43

000000000000000

0.751.853.364.556.175.143.984.314.63

3.24.156.514.452.422.262.091.420.760.430.320.350.510.771.081.391,712.172.84

3.95.135.37

4.32.7

1.783.25

000000000000000

0.671.723.244.516.175.143.954.284.613.194.156.524.462.45

2.32.131.440.780.440.330.370.53

0.81.121.421.742.192.863.955.215.484.372.721.733.01

000000

0.353.03

10.3211.66

5.72.361.33

1.41.922.822.51

2.22.052.752.762.512.752.661.642.093.492.561.39

1.21.020.670.38

0000

0.380.560.781.041.371.782.373.043.292.932.171.642.93

1.51.040.43

00

0.642.5

7.1810.066.76

2.81.280.8

0.841.071.521.491.571.772.622.682,422.66

2.61.622.083.542.631.421.211.020.710.43

000

0.310.43

0.60.821.091.441,872.5

3.243.633.482.862.394.45

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96-23 REC Volume Distribution Data

Sample tested at 70 mlkec (1) then soiicated and measured at 70mlksec (2) then slowed flow to 40 mlkec (3) Then sonicated at40W for 90 seconds and Measured at 40 mlhec (4).

No Duplicate

1 2 3 4FirstAs-Received 40 W 40W

Particle size 70 mkec 70 mkec 40 ml/see 40 mlk.ec704.000592.000497.800418.600352.000296.000246.900209.300176.000148.000124.500104.70088.00074,00062.23052.33044.00037.00031.11026.16022.00018.50015.56013.08011.0009.2507.7786.5415.5004.6253.8893.2702.7502.3121.945

1.6351.3751.1560.9720.8180.6880.5780.4860.4090.3440.2890.2430.204

0.1720.145

2.634.075.717.92

11.0114.8416.9415.2810.28

5.42.421.220.680.490.360.32

000000000000000000000000000000000

0.43

00000000000000

0.380.570.330.491.815.915.623.29

4.127.878.76

10.449.833.411.080.830.981.211.241.030.810.760.921.261.67

22.162.16

2.12.262.763.353.492.631.441.03

00000000000000000

0.682.264.182.952.234.3110.4

11.9213.1111.083.53

1.10.871,071.36

1.51.381.171.071,161.421.782.122.252.111.781.541.461.46

1.51.421.342.49

000000000000000.0000000000

3.624.3730.43

13.98.486.515.474.01

2.10.72

00000000000000

0.43

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96-24 REC Volume Distribution Data

Sample tested at 70 mlkec (1 ) then solicated and measured at 70

mlkec (2) then slowed flow to 40 mlkec (3) Then sonicated at’40W for 90 seconds and Measured at 40 mlkiec (4).

No Duplicate

1 2 3 4

First

As-Received 40W 40W

Particle size 70 mllsec 70 mlk+ec 40 ml/see 40 mkec

704.000

592.000497.800

418.600

352.000

296.000

248.900

209.300

176.000148.000

124.500104.700

88.00074.000

62.23052.33044.00037.000

31.11026.16022.00018.500

15.560

13.080

11.000

9.250

7.778

6.541

5.5004.625

3.889

3.2702.750

2.3121.945

1.6351.375

1.1560.972

0.8180.688

0.5780.486

0.409

0.344

0.289

0.243

0.204

0.172

0.145

00000000000

0.97

0.4

0

00.521.314.05

5.061.84

0.863.18

9.164.22

5.94

2.61

2.582.984.45

4.991.19

0.30.36

1.052.08

1.1

3.47

0.50

0.423.21

5.755.81

4.34

4.48

5.64

3.881.3

0

0

00000000000

0.641.481.15

0.520.42

0.652.084,42

4.42.26

1.99

3.4

5.17

5.64.54

3.652.01

2.13.362.57

0.90.39

0.360.7

1.52

2.73

1.240.59

0.582.06

5.038.51

9.95

7.82

3.981.23

0

0

0

00000000

‘oo000

1.39

0.320

0.321.49

4.7

5.742.511.53

2.364.83

7.54

5.83

3.021.041.31

3.453.59

1.06

0.33

0

0.711.94

3.31.04

0.40.422.18

5.62

9.47

10.46

7.6

3.52

0.98

0

0

0

0000000000000

1.39

0.350

0.341.584.885.552.19

1.26

2.05

4.72

7.94

5.76

2.68

0.891.17

3.493.89

1.08

0.32

00.7

1.953.53

0.990.32

0.332.09

5.73

9.94

10.92

7.68

3.39

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96-04 U/L Volume DistributionData

This sample was used to study the effects of circulationtime, flow rate and circulationtime on PSD results

Sample analyzed at 60 mlkac (l), then eoniceted at 25 W for 125 seconds and analyzed at 60 mkec (2), then sonicatedat 40 W for300 secondsand analyzed at 60 mlk.ec (3).

New sample was installedand analyzed at 60 mlkec after 2 minutes (4) and then after 25 minutes (5), then sonicated at 25 W for 90sec and analyzed at 60ml/sec (6).

New sample was installedand analyzed at 40 mlkec after 2 minutes (7), then sonicetedat 40 W for 90 sec and analyzed at 40ml/sec(8), then flow increased and analyzed at 70 mlkec (9), then sonicetedat 40W for 90 sec and anlayzed at 70 ml/sec(lO).

1 2 3 4 5 6 7 8 9 10As-received 25 W 40 W As-received 25 W As-receive 40 W 40W

Particle size 60 ml/see 60 mlkiec 60 mlkec 60 ml/see 60 mlk.ec 60 ml/see 40 mlk.ec 40 ml/see 70 mlkec 70 ml/see

704.000592;000497.800418.600352.000296.000248.900209.300176.000148.000124.500104.70088.00074.00062.23052.33044.00037.00031.11026.16022.00018.50015.56013.08011.0009.2507.7786S415.5004.6253.8893.2702.7502.3t21.9451.6351.3751.1560.9720,8180.6860.5760.4860.4090.3440.2890.2430.2040.1720.145

00000000000

1.341.3

1.341.551.962.563.27

44.745.335.7

5.896.216.827.477.596.865.674.573.722.992.311.741.34

1.10.930.750.560.39

0000000000

0000000000000

1.81.471.421.531.782.192.873.794.725.335.726.196.667.44

7.57

6.225.334.343.332.542.091.911.821.581.190.8

0.530.4

0.310000000

000000000000000

2.382.1

2.051.931.962.353.25

4.45.2

5.445.616.076.667.036.876.235.193.993.032,572.582.772.672.061.350.860.620.530.510.550.610.56

000

0000000

0.310.360.490.721.151.852.894.195.526.597.367.628.047.726.996.115.485.174.92

4.43.542.621.881.360.960.690.490.36

000000000000000

0000000000

0.330.520.641.352.11

3.24.656.357.888.768.517.636.726.296,296.27

5.74.583.362.461,831,37

10.720.530.410.32

0000!3o0000000

00000000000

0.680.78

11.4

2.093.184.666.187.237.457.08

6.66.4

6,536.676.395.564.483.532.792.211.721.341.060.880.730.590.450.34

0000000000

1.021.8

3.155.016.426.435.384.273.523.183.093.133.17

3.23.223.333.56

44.565.095.054.323.282.461.991.711.441.120.8

0.560.410.31

000000000000000000

000000

0.360.44

0.60.941.592.754.345.876.576.395.83

5.65.95

6.87.356.815.474.333.773.583.3

2.722.031.491.150.930.760.620.520.440.380.32

000000000000

00000

0.320.370.420.560.891.532.694.295.846.536.325.775.565.976.647.416.815.444.313.773.593.312.732.041.511.170.940.770.620.520.440.380.32

000000000000

0000000

0.560.690.921.32

23.014.275.416.025.975.775.666.426.986.865.934.934.334.093.833.272.54

1.91.471.190.990.840.710.610.520.440.35

00000000000

o

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96-04 U/L Sample 3

“r”~”-— ““-1– I II IITI T

1

–T Ililll

_ As-Received, 40 mlkec (7’)

m 40 W for 90 see, 40 mkec (8)

_ 70 ml/see (9)

W 40 W for 90 see, 70 mllsec (10)

I I I I 1

0.1 1.0 10.0 100.0

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96-04 L Volume Distribution Data

The sample was analyzed at 60 mkec (1), then sonicated at 25W for 120 seconds and analyzed at 60mi/sec (2), Then sonicated at 40 W for 300 seconds and analyzed at 60 mllsec (3).

New sample was installed and analyzed at 40 mlkec (4), then sonicated at 40 W for 90 seconds andanalyzed at 40 mlkc (5), then flow increased to 70 ml/second and analyzed (6), then sonicated at 40W for 90 seconds and analyzed at 70 mlkec (7).

1 2 3 4 5 6 7

As-received 25 W 40 W As-received 40 W 40W

Particle size 60 ml/see 60 ml/see 60 mkec 40 ml/aec 40 mkec 70 mkec 70 mlk.ec704.000592.000497.800418.600352.000

296.000248.900209.300176.000148.000124.500104.700

88.00074.00062.23052.33044.00037.00031.11026.16022.00018.50015.56013.08011.000

9.2507.7786.5415.5004,6253.8893.2702.7502.3121.9451.6351.3751.1560.9720.8180.6880.5780.4860.4090.3440.2890.2430.2040.1720,145

11.17.482.010.560.410.933.187.368.27

5.43.172.492.914.366.226.715.073.182.141.851.972.192.151.851.51

1.31.2

1.110.910.640.39

00000000000

00000000

00000

0.991.412.833.31.

2.!31.2

1.061.874.91

10.4711.97.063.482.432.984.746.486.134.433.192.812.943.032.541.670.97

0.590.450.410.420.430.410.35

000000000000

000000

0.772.283.47

2.61.410.981.232.635.868.687.264.392.962.923.865.266.085.93

5.44.964.573.963.072.111.370.930.720.650.660.670,640.560.460.380.32

000000000

3.475.968.198.937.956.254.753.823.262.882.552.322.222.252.312.32

2.32.342.47

2.62.562.291.941.671.521.441.361.241.090.950.83

0.720.630s5

0.50.460.420.370.32

00000000000

000

3.773.04

2.562.352.412.673.033.413.874.455,025.16

4.73.943.433.283.393.373.032.512.121.961.992.052.051.971.911.871.81‘1.691.561.481.49

1.51.41

1.20.93

0.70.52

0.40000000

000

3.391.41

1.071.281.842.442.792.872.973.27

3.84.254.344.023.773.783.983.953.512.892.482.392.512.632.582.442.332.282.212.081.941.881.931.971.851.531.150.83

0.60.440.33

000000

18.4911.152.24

0.40

0.37

1.223.274.533.452.05

1.41.331.672.232.582.422.071.811.721.671.591.481.451.54

1.71.831.85

1.81.761.741.721.661.611.641.741.821.73t .431.080.8

0.610.5

0.450.4

00000

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96-06 Carboy Volume Distribution Data

sample was analyzed at 60 ml/min (1), then sonicatedat 25 W for 120 seconds and analyzed at 60 mlkec (2),then sonicated at 40 W for 300 sec and analyzed at 60ml/see (3).

No duplicate

1 2 3

As-Received 25W 40W

Particle Size 60 ml/see 60mi/sec 60ml/sec704.000592.000497.800418.600352.000296.000246.900209.300176.000148.000

124.500104.70088.00074.00062.23052.330

44.00037.00031.11026.16022.00018.50015.56013.08011.0009.2507.7786.5415.5004.6253.8893.2702.7502.3121.9451.6351.3751.1560.9720.8180.6680.5780.4860.4090.3440.2890.2430.2040.1720.145

000000000

0.60.6

0.680.831.081.522.253.385.157.6610.5

12.0811.268.886.524.753.442.421.691.241.030.960.940.940.961.011.11

1.21.21

1.10.930.730.560.440.35

000000

00000000000

2.171.87

1.51.371.612.283.495.438.24

11.0912.1710.59

8.015.874.333.092.081.421.09

11

0.980.890.780.710.69

0.70.70.7

0.680.640.580.530.54

0.60.58

000

00000000000

3.242.932.392.132.242.593.073.734.946.989.57

11.0810.17

7.65.093.33

2.271.661.341.231.211,191.110.970.640.760.72

0.70.690.670.630.590.560.570.620.59

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96-06 M Volume Distribution Data

Sample was installed and analyzed at 60 mlkec (l).

New sample was installed and analyzed at 40 ml/see (2), then sonicated at 40W for 90 sec and analyzed at 40 ml/see (3). Flow rate was increased andsample analyzed at 70 mlkec (4), then sample sonicated at 40 W for 90 secand analyzed at 70 ml/see(5).

1 2 3 4 5

As-receive As-received 40 W 40WParticle size 60 mkec 40 mk.ec 40 ml/see 70 mkec 70 mlkec

704.000592.000497.800418.600352.000296.000246.900209.300176.000146.000124.500104.70088.00074.00062.23052.33044.00037.00031.11026.16022.00018.50015.56013.08011.0009.2507.7786.5415.5004.6253.8893.2702,7502.3121.9451.6351.3751.1560.9720.8180.6880.5780.4860.4090.3440.2890.2430.2040.1720.145

00000

0.86

000

0.631.561.711.010.71

1.13.097.23

7.93.89

1.50.951.332.855.27

6.35.414,434.094.16

4.34.354.253.883.272.682.312.131.971.68

1.30.910.610.38

0000000

000

1.213.214.59’4.173.443.213.443.824.164.384.594.774.914.934.84

4.74.554.283.853.342.942.732.632.472.f61.741.341.020.790.610.480.380.32

00000000000000

00000

0.460.550.67

0.91.362.072.984.03

5.26.226.75

6.45.62

4.94.554.394.19

3,83,413.213.213.243.142.882.562.261.981.711.471.291.161.040.870.670.490.37

000000000

00000

0.640.720.790.991.412.06

2.93.844.855.746.25

6.15.52

4.94.544.364.183.85

3.53.3

3.253.263.182.962.692.422.151.881.631.431.261.090,880.660.470.35

000000000

00000

0.70.760.85

11.291.722.21

2.73.314.11

4.95.194.994.634.474.434.324.013.663.473.463.533.563.453.212.882.522.171.891.7!

1.61.511.351.110.870.670.530.450.420.39

00000

u)(1)QECGcoua)>.—a)0a)CK

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.

96-06 L Volume Distribution Data

sample was analyzed at 60 ml/min (1), then sonicatedat 25 W for 120 seconds and analyzed at 60 mlkec.(2), then sonicated at 40 W for 300 sec and analyzed at60 ml/see (3).No duplicate

1 2 3As-Received 25 W 40 W

Particle Size 60 mlkec 60ml/sec 60ml/sec704.000592,000497,800418.600352.000296.000248.900

209,300176,000148.000124.500104.70088.00074.00062.23052.33044.00037.00031.11026.16022.00018.50015.56013.08011.000

9.2507.7786.5415.5004.6253.8893.2702.7502.3121.9451.8351.3751.1560.9720.8180.6860.5780.4860.4090.3440.2890,2430.2040.1720.145

21.9718.486.51

21.23

1.83.43

4.42.861.180.530.430.661.362.442.952.421.741.441.551.882.111.961.641.44

1.41.441.391.220.99

0.80.670.580.520.490.480.470.430.380.33

0000000000

00000

2.91.48

1.571.721.451.030.881.212.44

4.76.034.843.312.73

33.6

3.833.41

2.92.712.822.972.932.762.69

2.82.92.8

2.542.382.482.642.612.221.671.230.95

0.80.730.710.65

0000

00000

1.670.770.93

1.41.621.351.091.232.063.916.026.284.713.17

2.42.252.45

2.72.782.752.762.832.842.772.772.953.173.162.892.662.682.892.932.561.951.43

1.10.930.850.820.82

0.7000

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96-11 L Volume Distribution Data

Sample was analyzed at 60 mlk+ec (1), then sonicated at 25W for 120 seconds and analyzed at 60mlkec (2), then sonicated at 40 W for 300 sec and analyzed at 60 mlk+ec (3).

New sample was installed and analyzed at 40 mkec (4), then sonicated at 40W for 90 sec andanalyzed at 40 mlkec (5), then flow rate was increased and analyzed at 70 mkec (6), then sonicatedat 40 W for 90 sec and analyzed at 70 mlkec (7).

1 2 3 4 5’6 7

As-received 25W 40W As-received 40W 40W

Particle size 60ml/sec 60ml/sec 60ml/sec 40ml/sec 40ml/sec 70ml/sec 70ml/sec704.000592.000497.800418.600352.000296030248,900209.300176.000148.000124.500104.70088.00074.00062.23052.33044.00037.00031.11026.16022.00018.50015.56013.08011.000

9.2507.7786.5415.5004.6253.8893.2702.7502.3121.9451.6351.3751.1560.9720.8180.6880.5780.486

0.4090.3440.2890.2430.2040.1720.145

0000

00.810.640.710.780.770.740.79

11.452.183.083.884.464.96

5.66.296.786.79

6.56.195.915.484.783.91

3.1

2.461.961.581.281.080.930.810.680.550.430.350.31

00000000

00000000000

0.630.751.051.542.172.763.253.764.495.47

6.57.197,427.236.826.17

5.34.4

3.62

2.982.441.981.621.37

1.21.080.940.780.640.530.470.45

0.480.540.640.690.65

00

0000000000000

0.831.141.581.942.152.352.833.795.256.757.727.867.576.835,925.024.25

3.63.012.492.091.84

1.71.581.411.180.96

0.80.710.68

0.70.79

0.90.940.84

00

00000

1.051.031.111.251.481.782.22

2.83.584.465.295.896.296.S26.61

6.45.875.154.S2

4.13.813.493.052.532.031.611.281.020.830.690.590.520.450.380.32

0000000000

0000

000

0.620.650.760.951.291.862.773.925.045.786.156.346.536.536.245.645,054.654.414.133.663.072.48

21.61

1.31.060.890,770.680.590.490.410.350.320.310.340.36

00000

00000

0.480.460.490.570.710.921.261.822.683.794.945.746,176.396.566.54

6.25.585.014.654.444.17

3.73.09

2.52.011,621.311.070.9

0.780.690.590.490.410.350.310.31

0.3000000

000000000

0.960.991.121.391.942.823.944.955.646.036.326.446.235.765.295,024.884.654.163.492.84

2.31.871.541.281.090.970.860,750.640.530.460.41

0.40.420.48

0.570.57

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KES-M-I 3 top Volume Distribution Data

Sample was analyzed at 60 mlk.ec (1), then sonicated at 25W for 120 seconds and analyzedat 60 mlkec (2), then sonicated at 40 W for 300 sec and analyzed at 60 mksec (3).

New sample was installed and analyzed at 60 ml/see (4), then sonicated at 25W for 120seconds and analyzed at 60 mlkc (5), then sonicated at 40 W for 300 sec and analyzed at60 ml/see (6).

1 2 3 4 5 6As-received 25W 40W As-received 25W 40W

Paticle size 60 ml/see 60ml/sec 60ml/sec 60ml/sec 60ml/sec 60ml/sec704.000592.000497.800418.600352.000296.000248.900

209.300176.000148.000124.500104.700

88.00074.00062.23052.33044.00037.00031.11026.16022.00018.50015.56013.08011.0009.2507.7786.5415.5004.6253.8893.2702.7502.3121.9451.6351.3751.1560.9720.8180.6880.578

0.4860.4090.3440.2890.2430.2040.1720.145

000000000

0.580.660.831.131.622.363.354.475.676.757.537.667.176.355.695.325.074.664.013.292.672.211.851.55

1.31.120.980.870.750.62

0.50.420.360.33

0.30

00000

00000000000

0.650.750.971.341.942.813.955.216.316.836.666.175.795.715.735.534,95

4.23.52

32.582.211.921.711.581.461.291.070.850.690.560.52

0.50.52

0.50

000

00000000000

0.520.6

0.761.021.472.133.074.175.25

5.95.975.735.525.565.695.615.154.493.873.392.992.622.32

2.152.092.031.861.561.230.980.820.73

0.70.710.720.62

000

00000

0.130.130.150.180.790.961.251.712.383.234.215.176.056.787.247.196.645.855.214.834.564.193.643.022.472.051.721.441.211.040.91

0.80.680.570.470.390.340.22

0.2000000

00000000000

0.60.720.961.351.982.874.025.286.366.846.64

6.15.735.685.745.544,954,173.492.972.562.211.921.711.591.47

1.31.070.850.680,580.520.510.530.51

0

000

00000000000

0.460.550.731.041.552.273.244.355.395.985.975.625.385.445.635.595.124.43

3.83.322.95

2.62.322.16

2.12.061.881.561.230.970.810.73

0.70.720.730.62

000

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co

o00

0

00

00

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KES-M-I 3 Bottom Volume Distribution Data

Sample was analyzed at 60 ml/see (1), then sonicated at 25W for 120 seconds andanalyzed at 60 mlkec (2), then sonicated at 40 W for 300 sec and analyzed at 60

ml/see (3).

New sample was installed and analyzed at 60 ml/see (4), then sonicated at 25W for

120 seconds and analyzed at 60 mlkec (5), then sonicated at 40 W for 300 sec and

analyzed at 60 mlkec (6).

1 2 3 4 5 6

As-received 25 W 40 w As-receive 25 W 40 w

Particle size 60 mlkiec 60 ml/see 60 mkec 60 ml/see 60 ml/see 60 mlkec

704.000

592.000497.800

418.600

352.000

296.000

248.900

209.300

176.000148.000

124.500

104.700

88.00074.000

62.23052.33044.000

37.000

31.11026.160

22.00018.500

15.56013.080

11.000

9.2507.778

6.541

5.5004.625

3.889

3.2702.750

2.3121.9451.635

1.3751.156

0.972

0.818

0.688

0.578

0.486

0.409

0.344

0.2890.243

0.204

0.1720.145

00000

1.5

1.53

1.61

1.782.08

2.52

3.07

3.664.22

4.654.94

5.065.11

5.044.94

4.724.43

4.1

3.85

3.663.553.35

3.05

2.7

2.342.02

1.731.47

1.251.080.940.82

0.70.59

0.49

0.42

0.36

0.34

0.310

0

0

0

00

0000

“oo0

0.82

0.850.99

1.261.752.47

3.39

4.345.12

5.555.67

5.625.47

5.184.824.454.214.13

4.09

3.93

3.58

3.14

2.732.39

2.09

1.811.571.391.261.14

10.64

0.68

0.56

0.48

0.43

0.41

0.39

0

00

00

0000000

0.65

0.670.77

0.971.35

1.922.71

3.584.41

55.33

5.445.39

5.184.86

4.524.33

4.34.324.19

3.64

3.392.972.63

2.332.04

1.61.631.53

1.431.28

1.07

0.86

0.70.59

0.53

0.50.51

0.48

0

000

00000

2.11

2.09

2.12

2.232.47

2.64

3.313.794.21

4.494.65

4.664.66

4.62

4.58

4.444.24

3.983.76

3.6

3.47

3.26

3.01

2.662.32

2

1.711.451.241.06

0.930.81

0.690.59

0.490.42

0.37

0.34

0.31

0

0

00

00

0000000

1.121.14

1.3

1.62.1

2.83.64

4.424.99

5.25

5.32

5.245.16

4.974.7

4.384.154.05

4

3.85

3.55

3.14

2.732.37

2.061.79

1.561.391.26

1.13

0.990.64

0.690.57

0.49

0.44

0.42

0.4

00

00

0

00000

0.2

0.22

0.23

0.261.22

1.431.6

2.32.88

3.474

4.414.75

4.96

5.1

4.994.74

4.434.264.23

4.264.17

3.87

3.45

3.042.68

2.372.1

1.871.71

1.6

1.5

1.341.14

0.940.77

0.66

0.59

0.560.56

0.560.36

0

00

.,

.

0

g)QEmu)

n

Es

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o000r-

000

0.Y

KES-T-20 top Volume Distribution Data

Sample was analyzed at 60 mkec (1 ), then sonicated at 25W for 120 seconds andanalyzed at 60 ml/see (2), then sonicated at 40 W for 300 sec and analyzed at 60 ml/see

(3).

New sample was installed and analyzed at 60 ml/see (4), then sonicated at 25W for 120

seconds and analyzed at 60 ml/see (5), then sonicated at 40 W for 300 sec and analyzed at

60 ml/see (6).

1 2 3 4 5 6

As-received 25 W 40 w As-received 25 W 40 wParticle size 60 mllsec 60 mlk.ec 60 ml/see 60 ml/see 60 mlkec 60 ml/see

704.000

592.000497.800

418.600

352.000

296.000

248.900

209.300

176.000148.000

124.500104.700

88.00074.000

62.230

52.33044.000

37.000

31.110

26.16022.000

18.50015.560

13.08011.000

9.2507.7786.541

5.5004.625

3.889

3.270

2.7502.312

1.9451.635

1.3751.156

0.972

0.8180.688

0.578

0.486

0.409

0.344

0.289

0.2430.204

0.172

0.145

000

2.26

1.82

1.47

1.24

1.14

1.16

1.271.45

1.722.07

2.533.06

3.654.21

4.73

5.16

5.45.354.98

4.46

4.043.79

3.65

3.473.472.79

2.42

2.11

1.83

1.591.39

1.251.15

1.050.94

0.82

0.70.62

0.57

0.55

0.57

0.610.67

0.680.44

00

00000

1.73

1.25

0.97

0.86

0.891.021.24

1.561.98

2.46

3.03

3.844.34

5.03

5.585.71

5.434.914.494.29

4.22

4.06

3.713.27

2.84

2.48

2.17

1.88

1.651.5

1.41

1.331.211.04

0.89

0.77

0.7

0.68

0.7

0.750.8

0.80.73

00

00000

1.46

0.82

0.57

0.510.56

0.70.93

1.241.652.12

2.66

3.22

3.854.52

5.14

5.41

5.254.81

4.464.36

4.38

4.283.93

3.48

3.04

2.712.41

2.131.9

1.791.77

1.761.65

1.431.21

1.04

0.96

0.94

0.98

1.041.09

1.02

0.84

0

0

1.49

1.781.18

2.88

1.17

0.78

0.79

0.97

1.21

1.451.68

1.932.21

2.593.05

3.554.06

4.6

5.1

5.45.244.68

4.03

3.613.48

3.48

3.393.072.65

2.25

1.95

1.69

1.48

1.31.181.11

1.04

0.95

0.810.69

0.59

0.54

0.53

0.55

0.590.65

0.60

00

3.05

3.762.58

2.481.14

0.79

0.76

0.89

1.07

1.241.4

1.581.81

2.122.51

2.97

3.48

4.074.66

5.11

5.064.614.02

3.613.46

3.463.393.12

2.722.32

21.74

1.511.33

1.221.15

1.080.98

0.85

0.72

0.620.56

0.55

0.57

0.610.66

0.610

00

000

1.15

0.32

1.49

0.71

0.55

0.570.7

0.931.22

1.551.912.31

2.75

3.23

3.814.43

5

5.265.054.61

4.244.08

4.07

4.02

3.83.41

2.99

2.62

2.31

2.051.87

1.771.74

1.71.58

1.391.18

1.03

0.94

0.92

0.93

0.991.02

0.970.83

00

a)EEm0’)Qo1-0ql

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KES-T-20 Bottom Volume Distribution Data

Sample was analyzed at 60 ml/see (1), then sonicated at 25W for 120 seconds and

analyzed at 60 ml/see (2).

New sample was installed and analyzed at 60 ml/see (3), then sonicated at 25W

for 120 seconds and analyzed at 60 ml/see (4).

1 2 3 4 6

As-received 25 W As-received 25 W 40 w

Particle size 60 ml/see 60 mlkec 60 ml/see 60 mkec 60 mlkec

704.000

592.000497.800

418.600

352.000296.000

248.900

209.300

176.000148.000

124.500104.700

88.00074.000

62.230

52.33044.000

37.000

31.11026.160

22.00018.500

15.560

13.08011.000

9.2507.778

6.5415.500

4.625

3.889

3.270

2.750

2.3121.9451.635

1.3751.156

0.972

0.8180.688

0.578

0.486

0.409

0.344

0.289

0.2430.204

0.172

0.145

00000

1.04

0.49

0.38

0.362.13

1.47

1.49

1.81

2.4

3.194

4.524.76

4.83

4.9

4.824.63

4.39

4.274.3

4.334.18

3.8

3.36

2.99

2.69

2.4

2.441.861.69

1.61.5

1.35

1.17

0.99

0.850.73

0.63

0.56

0.530.5

00

0

0

00000

0.93

0.42

0.310.29

1.81

1.22

1.26

1.532

2.68

3.464.084.45

4.674.64

4.894.74

4.51

4.434.52

4.634.5

4.09

3.59

3.192.89

2.61

2.312.031.85

1.741.641.48

1.27

1.08

0.920.79

0.68

0.590.56

0.52

00

00

4.59

5.6

3.73

3.771.77

1.34

1.49

1.99

2.482.67

2.54

2.37

2.352.52

2.81

3.13.323.49

3.613.66

3.533.26

2.96

2.762.68

2.672.612.41

2.15

1,88

1.66

1.48

1.321.49

1.11.03

0.960.85

0.73

0.620.53

0.48

0.46

0.47

0.51

0.50

0

0

0

000

4.69

1.32

0.7

0.67

0.941.42

1.91

2.23

2.41

2.62.9

3.25

3.563.76

3.944.11

4.27

4.264.07

3.77

3.54

3.44

3.413.353.14

2.64

2.52

2.24

2

1.811.661.58

1.531.461.32

1.13

0.95

0.820.75

0.72

0.730.77

0.81

0.70

0

0

000

3.8

0.96

0.49

0.47

0.660.98

1.34

1.64

1.89

2.14

2.432.74

3.03

3.263.49

3.744.01

4.74

4.14

3.98

3.643.8

3.833.8

3.613.29

2.932.62

2.36

2.162.01

1.941.911.841.66

1.42

1.191.02

0.93

0.89

0.9

0.940.96

0.820

00

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QEC6v)

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NRW 100

Volume Distribution Data

1

As-received

Particle size 60 mkec

704.000 94.58

592.000 5.42

497.800 0418.600 0352.000 0296.000 0248.900 0209.300 0176.000 0148.000 0124.500 0104.700 088.000 074.000 062.230 052.330 044.000 037.000 031.110 026.160 022.000 018.500 015.560 013.080 011.000 09.250 07.778 06.541 05.500 04.625 03.889 03.270 02.750 02.312 01.945 01.635 01.375 01.156 00.972 00.818 00.688 00.578 00.486 00.409 00.344 00.289 00.243 00.204 00.172 00.145 0

NRW 400

Volume Distribution Data

1

As-received

Particle size 60 mlkec

704.000592.000497.800418.600

352.000

296.000

248.900

209.300

176.000

148.000

124.500

104.700

88.00074.000

62.23052.33044.00037.00031.11026.?6022.00018.50015.56013.08011.0009.2507.7786.541

5.5004.6253.8893.2702.7502.3121.9451.6351.3751.156

0.9720.8180.6880.5780.486

0.4090.344

0.2890.2430.2040.1720.145

93.586.42

000000000000000000000000000000000000000000000000