WSRC-TR-99-O01

Preparation

16, Rev. O

of Simulated Waste Solutions

by
D. D. Walker
Westinghouse Savannah River Company
Savannah River Site
Aiken, South Carolina 29808

DOE Contract No.

DE-AC09-96SR18500

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WSRC-TR-99-O0116,
Keywords: Saltprocessing,
waste
Retention

PREPARATION

Rev.O
Highlevel

Permanent

OF SIMULATED WASTE SOLUTIONS

D. D. Walker

Publication Date April 15,1999

qONsl B1l/rp

*.

Westinghouse Savannah River Company

Savannah River Technology Center
A iken, SC 29808

.
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SAVANNAH

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RIVER

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SITE

WSRC-TR-99-O0116 Rev.O
Page 2 of 9
Preparation

of Simulated Waste Solutions

Author

D&

D.mdwt

4/lLl~7

D. D. Walker, Waste Processing Technology

Date

Technical Review

D. T. Hobbs, Waste Processing Technology

Date

Approvals

ld~

gd

S. D. Fink, bvel 4 Manager

Waste Processing Technology

/6- ?~
Date

-.

,$

WSRC-TR-99-O0116 Rev.O
Page 3 of 9

PREPARATION

OF SIMULATED WASTE SOLUTIONS

By D. D. Walker

SUMMARY
Waste Processing Technology personnel routinely prepare 0.5 to 10 L batches of salt
solutions simulating Savannah River Site (SRS) soluble waste. This report describes the

compositions and preparation methods.

DISCUSSION

The simulant compositions vary by waste type (e.g., average, high hydroxide, and high
nitrate) and by total sodium ion concentration (typically 3 to 7 molar Na+). The waste
types represent the average and extreme compositions expected in the feed stream sent to
the salt decontamination process.- As such, they do not represent the extremes in
composition of liquid waste currently in the SRS tank farms. Some blendlng is expected
prior to transfer to the salt decontamination process. The two extreme compositions are
called high hydroxide and high nitrate solutions. The high hydroxide solution
represents tank supemate and the high nitrate solution represents dissolved saft cake. The
average solution represents a blend of all soluble waste in the tank farm. For any of the
three waste compositions (i.e., anion distribution), the total sodium ion concenmation can
be varied up to 7 molar. The nominal sodium ion concentration is 5.6 molar for the feed
to the ion exchange option for salt disposition.
Table I lists the concentrations of 15 major components in the three waste types.
Numerous minor components, particularly hazardous metals such as chromium, are not
routinely included in simuknrts.
Appendix A lists the amounts and identities of chemicals used to prepare 1-L batches of

each waste type at 5.6 M Na+. Small batches of simulants are prepared from reagent or
similar purity chemicals.
When high purity chemicals are used in the preparation, typically less than 0.5 grams of
solids fail to dissolve per liter of solution. Larger amounts of insoluble solids could be
obtained if lower purity chemicals are used in the preparation. For most applications, the
solutions are filtered if solids remain after final dilution. The solutions should be cooled
to room temperature and aged for at least 24 hours before filtering.
Aluminum nitrate [Al(N0,),-9~0] is the usual source of aluminate ion. Use of
aluminum nitrate requires addition of extra sodium hydroxide and less sodium nitrate
based on the following stoichiometry.
Al(NO,), + 4 NaOH = NaAIO1 + 3 NaNO, + 2~0

,.

WSRC-TR-99-O0116 Rev.O
Page 4 of 9
TABLE I. Composition

of Simulated Waste Solutions

Concentration (molar)
High OH
High N03
5.6
5.6

Comuonent
Na+

M
5.6

K+
Cs+
OHN03NO~
A1O;
co32so42clF
Po43Cx042
SiO~2MoOi2

0.015
0.00014
1.91
2.14
0.52
0.31
0.16
0.15
0.025
0.032
0.010
0.008
0.004
0.0002

0.030
0.00037
3.05
1.10
0.74
0.27
0.17
0.030
0.010
0.010
0.008
0.008
0.004
0.0002

0.0041
0.00014
1.17
2.84
0.37
0.32
0.16
0.22
0.040
0.050
0.010
0.008
0.004
0.0002

Aluminum nitrate yields an acidic solution in water and can react with sodium nitrite to
form NO, gas. Thus, the preferred order of addition is to dissolve sodium hydroxide first,
followed by aluminum nitrate. Sodium nitrite is added only after the aluminum nitrate is
completely dissolved in excess sodium hydroxide.

If disodium hydrogen phosphate is used instead of tnsodium phosphate, additional

sodium hydroxide should be added to neutralize the acidic hydrogen.
Appendix B contains an example of instructions for the preparation of a 1-L batch of salt
solution. Salt solutions in volumes S2 L are usually prepared in volumetric glmswme so
that the amount of water required need not be measured. However, the densities of tie
three types of saft solution have been measured and the required mass of water can be
calculated. The density (g/mL) at 22 C is calculated from the total sodium ion
concentration (molar) by the following equations.3
Average:

d = 1.009 + 0.04454 [Na+]

High hydroxide

d = 1.003 + 0.04302[Na+]

High nitrate

d = 1.006 + 0.04725 [Na+]

!,

WSRC-TR-99-O0116 Rev.O
Page 5 of 9
W.FERENCES

1. P. L. Rutland et al., Bases, Assumptions,

for the Initial Eighteen Salt Disposition
1998.
-

and Results of the Flowsheet Calculations

Alternatives, WSRC-RP-98-O0166, 25 June

2. D. D. Walker, Modeling of Crystalline Silicotitanate Ion Exchange Columns,

WSRC-TR-98-O0343, Rev.0, October 2, 1998.
3. D. D. Walker and G. K. Georgeton, Viscosity and Density of Simulated Salt
Solutions, WSRC-RP-89-1088, October 19, 1989.

WSRC-TR-99-O0116 Rev.O
Page 6 of 9
Appendix A
Chemicals Required for Salt Solutions
Average Salt Solution (l-L batch)

Component

K+
Cs+
OH

N03
NOi
A102co32so42
cl~.
Po43c2042SiO~2
Mo042
Water

KN03
CSN03
NaOH
NaN03
NaNOz
A1(N03)s9Hz0
Na2COqH20
Na2SOd
NaCl
N@
Na2HPOdo7H20
NajCzOd
Na2Si03-9H20
Na2M0042H20

Target
Molecular
Weight
Concentration
M
m
0.015
101.1
194.92
0.00014
1.91
40.00
2.14
84.99
69.00
0.52
0.31
375.14
0.16
124.01
0.15
142.04
58.44
0.025
0.032
41.99
O.plo
268.09
0.008
134.00
284.2
0.004
241.95
0.0002

Amount
Required
m
1.517
0.027
126.40
101.55
35.88
116.29
19.84
21.31
1.461
1.344
2.681
1.072
1.137
0.048
827.9
Total weight: 1258.

High Hydroxide Salt Solution (l-L batch)

Comuonent

K+
Cs+
OHNO~
NO;
AIO~
co32S04Z

clF
Po43CZ042SiOg2
Mo042Water

KNog

CSN03
NaOH
NaN03
NaNOZ
A1(N03)39Hz0
Na2C03H20
NajSOd
NaCl
NaF
Na2HPOA-7H20
Na2CzOd
NazSi039Hz0
Na2MoOA2H20

Molecular
Target
Concentration
Weight
[~mole)
m
101.1
0.030
194.92
0.00037
40.00
3.05
1.08
84.99
69.00
0.74
375.14
0.27
124.01
0.17
142.04
0.030
0.010
58.44
41.99
0.010
268.09
0.008
134.00
0.008
284.2
0.004
0.0002
241.95

Amount
Required
3.033
0.072
165.52
20.37
51.06
101.29
21.08
4.26
0.584
0.420
2.145
1.072
1.137
0.048
871.9
Total weighc 1244,
_

;.

WSRC-TR-99-O0116 Rev.O
Page 7 of 9
High Nitrate Salt Solution (l-L batch)
Com~onent

K+
Cs+
OHNO;
NO~
A1O;
C032
so42Cl
F
P04
c2042-

SiO~2
MoOd2

KN03

CSN03
NaOH
NaN03
NaNOZ
A](NOJ)S9HZ0
NazCOsHzO
Na2S04
NaCl
NaF
NazHPO~-7Hz0
NazCz04
NazSiOs9Hz0
NazMo04-2Hz0

Molecular
Weight
M
101.1
194.92
40.00
84.99
69.00
375.14
124.01
142.04
58.44
41.99
268.09
134.00
284.2
241.95

Target
Concentration
0.0041
0.00014
1.17
2.84
0.37
0.32
0.16
0.22
0.040
0.050
0.010
0.008
0.004
0.0002

Water
Total weight:

Amount
Required
w
0.415
0.027
98.40
159.42
25.53
120.04
19.84
31.25
2.338
2.100
2.681
1.072
1.137
0.048
806.3
1271.

WSRC-TR-99-O0116 Rev.O
Page 8 of 9
Instructions

Appendix B
for Preparation of Salt Solution

Note: The instructions are accompanied by a data sheet listing the chemicals required

with spaces for the exact amounts used. Spaces are also provided for other quality
assurance information (i.e., operator name, date, balance identification, manufacturers
and lot numbers for each chemical).
1. Locate and label a clean, dry, 1-L volumetric flask. Weigh it empty and dry.

the NaOH into the flask. Add_

continuing.

2. Weigh

Caution:

g of water and dissolve the NaOH before

Dissolving NaOH will heat the solution. If the solution becomes too
hot to handle safely, cool it before proceeding.

Note: If the solution is not prepared in a volumetric flask (e.g., if the water is
added by weight rather than by filling to the line on the flask), keep the
container closed as much as possible when the solution is hot to

avoid evaporation of water. If using volumetric glassware, reserve a

portion of the water for the final addition in step 6.
3. Add the aluminum nitrate to the flask and mix to dissolve,
Caution:

Do not add sodium nitrite prior to dissolving the aluminum nitrate in

excess NaOH. Poisonous red fumes of NOj could form.

4, Add the remaining chemicals,

5. Mix to dissolve (l-2 hours).
6. Allow the solution to cool to room temperature.
Note If using volumetric glassware, fill to the line with water after cooling.
7. Reweigh the solution and compare to the expwted weight. If the weights differ
significantly, investigate for a missing component or error in weighing.
8. Allow the solution to age at least 24 hours.
Note: The solution should equilibrate long enough after preparation to avoid
concerns from slow precipitation. For volumes as large as 10 L, 24 hours
generally provides adequate equilibration time. The best practice will
include a second hold period and a second filtration.
9. Filter the solution through any convenient filter (medium frit sintered glass is
acceptable).

WSRC-TR-99-O0116 Rev.O
Page 9 of 9

CC:

M.. A. Baich, 704-T

M. J. Barnes, 773-A
J. T. Carter, 704-25S

C. L. Crawford, 773-41A
L. O. Dworjanyn, 779-2A
R. E. Eibling, 704-T
H. H. Elder, 704-S
S. D. Fink, 773-A
F. F. Fondeur, 773-62A
J. R. Fowler, 704-3N
D. T. Hobbs, 773-A
E. W. Holtzscheiter, 773-A
R. A. Jacobs, 704-3N
R. T. Jones, 704-3N
P. S. Kirkland, 703-46A
L. F. Landon, 704-T
D. P. Lambert, 704-1T

D. J. McCabe, 773-42A
C. A. Nash, 773-42A
L. M. Nelson, 773-43A
R. A. Peterson, 773-A
S. F. PICCO]O,
704-3N
M. R. Poirier, 676-T
K. J. Rueter, 706-S
P. L. Rutland, 704-196N
P. C. Suggs, 704-3N
RF. Swingle, 773-A
W. L. Tamosaitis, 773-A
G. A. Taylor, 704-196N
W B. VanPelt, 773-43A
D. D. Walker, 773-A
W. R. Wllmarth, 773-42A
TIM, 703-43A
WPTS Files, 773-A, CIOC.C.Canada, 773-A
ITP files, c/o Cathy Smalls, 241-147H
D. D. Lee, ORNL

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PREPARATION

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<. DESCRIPTIOfVABeTRACT
simulating
Waste Processing Technology personnel routinely prepare O.5to 10 Lbatches ofsaltsolutions
River Site (SRS) soluble waste. This reporl describes the compositions and preparation methods.

Savannah

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2. OpenNet (use OpenNet guidance

to U.S. and non.U.S. public)

for below):

a. If additional source ofher than mating it available through NTIS:

e. OpenNet Document Type

f. OpenNet Document Keywords

(1) Accession Number

(2) Document Location
b, Field Ofice Acronym
c. Decl%sification date (mtrdddlyy~)

,,.,..,

d. Declassification Status
_
Declassified
Sanitized
3. U.S. Dissemination Only
4. Copyrighted

,....,

. . ..
,,,,,,.

material;

g. OpenNet Addressee

/_/_
_

Never classified

Are there any restrictions based on copytight?

5. Small Business

Innovation

6. Small Susiness

Technology

7. Proprietary~rade

Secret

S. Patent Pending
9. Protected data

Research
Transfer

CRADA

(SBIRI Release date

(mmfddl~)

(ST7FfI Release date

(mmfddl~)

_Other

yes

(specify)

no. If yes, list the restrictions

Release date (mm/dd/~)

10. Official Use Only (OUO)

11. Program-Oirected

Special Handling

(speci~

12. Export ControlATARfEAR

13. Unclassified

Controlled

Nuclear Information

(UCNO

14. Classif led Classification Leve!fCateaorv of

a. TMs form . .......................................................................
15. Other information
I. oTHER

ffnfofmation

b. The STI Product

UnClaSajfiRd

............................................

relevant to access (specify; for OSTI internal use only))

useful to include in published

announcement

record which is not suited for any other field on this fortn)

C. CONTACT AND RELEASING OFFICIAL

1.Contact(if appropriate, the organization or sire mntac! to include i. published Cbations wfM would receive any etiemai questions about the content of the
ST! Product or lhe research in fonnaOon contained therein)
K.J. Schmidt,
Manager
STI Program & Site Supporf
Name andor Position
Phone ~-2321
E.mall
organization Westinghouse
Savannah
River Company
;e;~~~~~l~~
E.Mail

~.

I vetify that all necessa~ reviewshave been completed(e.g. Patent,Copyright,ECI, UCN1,etc.)

Schmidt
Date)h~~dWfi
,.,,............................

(S03) 725-7373