INFORMATION CLEARANCE REVIEW AND RELEASE APPROVAL

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Title: Information Category:

Actual 'tJaste testing ;rli th a single D Abstract D Journal Article D Summary disk SpinTek rotary m.icrofilt.er

D Internet ~ Visual Aid D Software

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Document Number: LAB-RPT-}O-OOOO4 1<.0 JDate: 03/02/2010

Author: Huber, Heinz J.

Purpose of Document: Pre,sentation a t - ACS National meeting

Part II: External/Public Presentation Information Conference Name: PICS 239t', Nationa.l [vleeting

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Date of Conference: 03/25/2010 I Conference Location: San Francisco

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Page 1 of2 A-6003-508 (REV 3)

INFORMATION CLEARANCE REVIEW AND RELEASE APPROVAL

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Page 2 of 2 A-6003-508 (REV 3)

LAB-RPT -10-00004 Revision 0

Actual waste testing with a single disk SpinTek rotary microfilter

Prepared for the U.S. Department of Energy Assistant Secretary for Environmental Management Contractor for the U.S. Department of Energy Office of River Protection under Contract DE-AC27-0BRV14BOO

washington river protecti on solutions

P.o. Box 850 Richland, Washington 99352

Approved for Public Release; Further Dissemination Unlimited

LAB-RPT -10-00004 Revision 0

Actual waste testing with a single disk SpinTek rotary microfilter

Dr. Heinz J. Huber Washington River Protection Solutions

Date Published

March 2010

To Be Presented at ACS 239th National Meeting

American Chemical Society San Francisco, CA

March 25, 2010

Prepared for the U.S. Department of Energy Assistant Secretary for Environmental Management Contractor for the U.S. Department of Energy Office of River Protection under Contract DE-AC27-0BRV14BOO

washington river protectionsolutions

P.O. Box 850 Richland, Washington

Copyright License By acceptance of this article, the publisher and/or recipient acknowledges the U.S. Government's right to retain a nonexclusive, royalty-free license in and to any copyright covering this paper.

J.,Et ~~R {Release Approval

Approved for Public J

Further Dissemination Unlimited

LEGAL DISCLAIMER This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency thereof, nor any of their employees, nor any of their contractors, subcontractors or their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or any third party's use or the results of such use of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise, does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or any agency thereof or its contractors or subcontractors. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof.

This report has been reproduced from the best available copy. Available in paper copy.

Printed in the United States of America

LAB-RPT -10-00004 Revision 0

Actual waste testing with a single disk

SpinTek rotary

m icro filter

Dr. Heinz J. Huber, WRPS

Presentation at ACS 239th National meeting

March 25, 2010 LAB-RPT-10-00004

~~,

~ Actual waste testing using SpinTek microfilter wil.qhington river

protection solutions

1IIIII •••••• IIIIIIIIIIIIIIIIIII11111I1111I1 •• IIlIIIlIIIlI •• II,I\l"I!,.¥~;~~~;:iw~~l~lji?(E~:~',,:~,:::,,':':" " ,

Process Diagram of SpinTek microfilter in 1-F hot cell

B

01 101 0

S3~ ~ (p2) A

0 FILTRATE 0

yD2

T SpinTek

I ST-II I II Filter i I Chiller

Rotor Motor

o ~

QD ... Swagelok Quick Disconnect PL ... Pressure Switch Low PH ... Pressure Switch High P ... Pressure Gauge Sl T ... Temperature Gauge

<&> ... Sample Point Y ... Drain Valve iOf ... Ball Valve

QD CONCENTRATE

[Z] -'-

0 yD3

Heat Exchanger OD

// ~ C'') ........ ""':: ........ , ,

; , ~ ;

I ,;

I I 11

I I

II Wash Tank -

QD

VI

Heat Exchanger

Feed Agitator

I Feed Tank

Progressive Cavity Pump

~ Actual waste testing using SpinTek microfilter wA!<hington river

protection solutions

Setup of the SpinTek rotary microfilter in 1-F hot cell - The unit was prepared in a cold test part of 222-S and then transferred to 1-F

- Support unit is mounted on a separate skid and quick-connected to filter unit

- Used two stainless steel filter disks with 0.1 and 0.5-lJm nominal pore size

~ Actual tank waste composition comparison wAM ington river

protectionsc-Iutions

Aluminum Calcium Chromium Iron Potassium Sodium Silicon Uranium Zirconium Fluoride Chloride Nitrite Nitrate Phosphate Sulfate Oxalate Hydroxide TOC TIC

, .'1:+ '~,":,,:ij "";,-,~,\~,-",,,;'i~ ,ill/1r"'~L

19800 0.73 36000 <50.5 3210

176 0.003 17200 <5.05 2550 3640 0.09 n.d.

170000 7.39 128000 198 0.004 11100

<0.10 - <0.005 <0.005 - <251

730 0.04 -5440 0.15 -

55900 1.22 -

135000 2.18 -

884 0.01 -

3920 0.04 -

464 0.01 -

35800 2.11 n.d. 847 0.07 10800

6470 0.54 7180

1.33 23000 0.85 181000 6.70 0.08 <50.5 <943 0.33 4490 0.09 14100 0.27 0.05 <5.05 6170 0.11

- 2170 0.06 n.d. 5.57 189000 8.22 15200 0.66 0.22 176 0.003 5010 0.10

- <0.10 - 2410 0.01 - <0.005 - 1920 0.02 - 35.1 0.002 - 7000 0.20 - 68300 1.48 - 169000 2.73 - 2720 0.03 - 3360 0.04 - 266 0.003 - 39900 2.35 n.d.

0.90 1540 0.13 312 0.03 0.60 4300 0.36 382 0.03

~ Actual tank waste solids comparison wA,~hington river

protection sclutions

Mineral Formula AN:'105 (%) SST (%)

Cancrinite Na-Ca-AI-Si-carbonate 25 5

Natroxalate Na2C204 25

Gibbsite AI(OHh 85

Hematite Fe20 3 5

Boehmite AIO(OH) 5

unknown ? 45

Nitratine NaN03 5

:/Sao AN-105 SST 7sno

2000

-ih ... § ~ 8. t~ao f sono '" i 1: :§ - 1000

2561)

E,n!}

0 I I I 'ric.iT Gi."~. 'AICOHi'(SS,Or I

II L II I! ~I III I I I C I M'Goe.r'~·,'me'Feoo'rTI

~,o, .. ,~.?1 .. .'lqfl,,,,.A"'''mU ... _ bllirIiH\i"j'),,.!.~1

I Gl-089-2SZS> "iio"'" -"0"0,(5,0%) I t'o 20 3'0 t • ~b (I 50 I ! eo"" 50 00 10

Two-Thet. (deg)

~j Actual waste testing using SpinTek microfilter wilRhington river

protectionsofutions

Schedule of Slurries and Disks (all runs with 40 psi transmembrane pressure)

Slurry Disk Comments

AN -105 supernate 0.5 Illl -

AN-I05 0.29 wt% 0.5 Illl Actual and duplicate test runs

AN-I05 1.29 wt% 0.5 Illl Actual and duplicate test runs

AN-I05 1.29 wt% O.lllll Actual, partial, and duplicate test runs

SST supernate 0.5 Illl -

SST 0.29 wt% 0.5 Illl Actual and duplicate test runs

SST 1.29 wt% 0.5 Illl Actual and duplicate test runs

SST 1.29 wt% 0.5 Illl Concentrating run

SST sill 1.29 wt% 0.5 Illl Actual test run

AN-I05 sill 1.29 wt% 0.5 Illl Actual and duplicate test runs

AN-I05 1.29 wt% 0.5 Illl Actual and duplicate test runs

~ Actual waste results using SpinTek microfilter wil.qhington river

protectionsclutions

Filtrate Flux of AN-1 05 and SST actual slurries

..... N e E

01.25

01.2

,~

a 0.15 -i!C ,::J ~ 'al' ... ~E 0.1 ;:!: .-I.L

01.05

o

(corr. to 35°C; 40 psi transmembrane pressure)

O.5-pm disk

o 0

.. . .. ..

o °0 o 00 c9

o AN-1D5 01.29 wt.%

AN-105 1.29 wt.%

A SST 01.29

... SST 1.29

~OO~.o 00 °D. OOOO ........ -!At ... tt • • ttA. , ~~ .• A"'·'·

01:001 1:0101 2:00 3:010 4:00 5:00 6:00 1:010 8:001 9:010 Ourntion [h)

~ Actual waste results using SpinTek microfilter wil~ningt()n river

protection.50iulions

Filtrate Flux of AN-1 05 actual slurry (corr. to 35°C; 40 psi transmembrane pressure)

Om1 -pm dis,k AN-tOtS 0.25

eAN-105 1.29 wt% @AN-105 1.29 wI. %

-N C -

0.2

,15 n 1 CL v. ' 5 ,a -:x = I;:

S : 0.1 ,m ~

~

I.L

0.05

o

• o

• • • • • • • • •

0:00 0:30 1:00 1:30 2:00 2:303:00 3:30 4:00 4:30 5:00 Dumtion [h~

2fi Actual waste results using SpinTek microfilter wflRhingtnn river

protectionwlutions

Influence of Solids Loading on Filtrate Flux (corr. to 35°C; 40 psi transmembrane pressure)

0.2

-a: '. -.. 0.1.5 E .Q. CD -:.c .s 0.1 ,(jJ -.n:I! .... := u: 0.05

I)

o

a

A

o

..

0.5 1

A

1.5

OAN-105

&551

...

2

Solids concentration [wt.:%]

The maximum concentration of 2.7 wt.olo was limited by the actual amount of solids present and the minimum amount of liquid necessary to run the system as it was

designed for these experiments (theoretical max. was 4.0 wt.olo). SRNL presented data of an 11.7 wt. °10 actual tank slurry in WSRC-TR-2003-00030.

~~ - Actual waste results using SpinTek microfilter wA.qhingtnn river

protections-c1utions

Comparison of actual and simulant filtrate fluxes "

lAve. stable filtrate flux at O.5~lJm disk ·O.1-lJm disk : O.5-lJm cleaned Solids I

>

35Q ,C [gpml/ft2] , [gpm/ft2] " ,. [gpm/ft2] . [wt.%l l

AN-105 supernate 0.18 0 I

AN-105 0.29 wt. % 0.16 0.29

AN-105 1.29 wt. % 0.12 0.11 0.29 1.29

AN-105 sim 1-F 0.40 1.29

SST supernate 0.083 0 I

SST 0.29 wt. % 0.060 0.29 I

SST 1.29 wt. % 0.055 1.29 I

SST cone 0.044 1.49

SST cone 0.039 2.13 I

SST sim 1-F 0.037 1.29 I

AN-105 sim cold test 0.49 0.29 I

SST sim cold test 0.22 0.22 0.29

AN-105 sim cold test 0.46 0.34 1.29

SST sim cold test 0.14 0.19 1.29

@ij Actual waste testing using SpinTek microfilter WRRhington riller

protectionwlut/ons

Filtrate clarity

All turbidity measurement results were below the required <4 ntu.

4.0 --------------------- - - .

3.0 -:::J ...... C -,.2:' 2.0 l-ii :a -:::J .... 1.0 I- •

I 0.0

•

•

• O.5-lJm disk

e O.1-lJmdisk

• O . .5-lJm disk7>

• •

I

:I;: post nitric acid cleaning

,

~ Actual waste testing ~sing SpinTek microfilter IVilRhington river I

protectionso/uilons :

i I , ,

Disk Fouling due to inactivity After 3 months in water, the disk shows dark streaks and a highly reduced filtrate flux

Left: O.1-JJm disk as retrieved from the filter housing

Right: clean O.5-JJm disk

~ a wilRhington river

protectionSOillt/ons

I

Actual waste testing lising SpinTek microfilter I

Disk Fouling during operation

The O.1-fJm disk showed serious pressure fluctuations ---+ after removal of the disk material flaked off over night.

SEM-EDS analyses showed that the material flaking off the disk was mostly made of <5 fJm Na-AI silicates, AI-rich (+Cr), Ni-rich, ~-rich and Ca3(P04h-particulates.

~ Actual waste testing using SpinTek microfilter wHshington river

protection.SD/utions

Disk Fouling during operation 2

The 0.5-tJm disk also showed serious pressure fluctuations during AN-105 actual waste tests ----+ Cleaning with 1 M nitric acid restored filtrate flux to 90 0/0.

O.5;-lJm disk p,ost cleaning (tl

8.,6

...... €'~ e 015 :E .

CiIo :a -:!Ie 01.4 := Ij: CI) -. E 0.3 ~

LL

0.2

0.1

o

CtI

m f'L'i L'VI !.<N W -II m tie:

• •

--

@

• • ® •

ill AN-1D5 sim 1.29 ~vt % ~ AN~105 sim 1.29 VIA. % • AN..:105 '1.29 wt %

AN~105t29 !Nt. % - - - - - average AN-105 pre-clealling

- AN-1D5 sim 1.29 M. % Iloll-fad nab

~ 1Wf 13;l >1'l

,- t---.,

• • •

0:0101 01:30 1:00 1:30 2:0101 2:301 3:001 3:30 4:010 4:30 5:0101 Duration [bID

5fij Actual waste testing using SpinTek microfilter wARhilgron tiller

protectionscfutlons

Summary and Outlook

I. Actual tank waste from Hanford tanks show lower filtrate flux by O.3-0.6x.

II. Disk fouling during operation can be approached by running the system with 1 M nitric acid. This restores the filtrate flux to -- O.9x of original flux.

III. O.1-lJm disk has no apparent advantage over O.5-~m disk; same filtrate clarity, but lower flux rates => not recommended for Hanford tank waste

The single disk model of the 5pinTek filtration unit in 1-F of the 222-5 laboratory is ready for any future tests.

(e.g., new filter materials or different feed slurries)

7hAOk !JOU for !Jour Atteotioot .

i:;;$ Actual waste testing using SpinTek microfilter \vH~hington river

protectiOllsc-lulions

Principle of Filtration in the SpinTek system (backup slide)

Promoters, shaped like wagon wheels, induce the turbulence needed to prevent rotational flow ~ reduced filter fouling

Concentrate I

---------

Feed

Filtrate

Feed

Concentrate

t l ---- .... ----1 E

1 Filtrate Feed

1 ... Filter Housing 3 ... Pall Sintered Steel Disks 2 ... Hollow Shaft 4 .. . Turbulence Promoters

*4 Actual waste testing using SpinTek microfilter wil.~hington river

protectionsolulions

11111111111111l1lil1li111111111.l1li111111111111 •••• ·- !:JE~~)F:~f;vt~~&:~;' '

Calculation of temperature adjusted filtrate fluxes (backup slide)

For better comparison between the different test groups, all filtrate fluxes were corrected to 35°C (= 95 OF = 308.15 K). Temperature corrected fluxes were

calculated using the equation:

F _ 2500( 1 - 1 J 35C - ~riginal_flux • e T+273.15 308.15

(see INEEL/EXT -04-01933, Alternative Ultrafiltration Membrane Testing for the SRS Baseline Process.)

iii Actual waste testing using SpinTek microfilter wRRhingron river

protectionsoflltions

0.6

I~ .-. 0.5

1:: -.. E ~ ~ 0.4 ~ .... ~

Q:; 0.3 ~ Q -r.. ~ 0.2 ~ -.::: ~ 0.1

0.0

0:00

:«><

2:00

Results of single disk model at SRNL (backup slide; from SRNL-STI-2009-00330)

>0<>01% X>®lK

x

>00:

. 0.09 wt% Act. Waste + MST 0.11-12002 • 1.29 wt% Act. Waste + MST 0.11.1 2002

... 4.5 wt% Act. Waste + MST 0.11.1 2002 X 4.5 wt% Act. Waste + MST 0.51.1 2002 )!( 4.5 wt% Act. Waste + MST 0.51.1 2003 0.4 I ~ 2002 Test-0.5 micron rotary-actual waste

_ 2003 T est-0.5 micron rotary-actual waste *-- 0.1 micron crossflow-simulan t

- - - - Design Target Q3 7'

~ .................. 11& ............ ............... ... -. ~ ---.. 8

4:00 6:00 8:00

Time (hours)

10:00 12:00 ~ 0.2 ~

.a ~

0.1 I ......... """

o ~f--------,-------~-------r-------.------~ o 3 6 9 12 15

Solids Loading (wt 0/0)