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AD-A244 010 


li lu liil! Llli iiiii lilijii 


Rtport No. AIIXTH-TE-Cfi>6801«U^ 

Mm tfp on 




U SATHAM A 

U.S. Aftny Toxic ami Hazarctoua Matartaia Agency 


LABORATORY-SCALE SOIL 
WASHING TEST ON 
ROCKY MOUNTAIN ARSENAL 
BASIN F MATERIAL 

(TASK OflOER NO. 8) 


August 1968 

Contrset No. DAAK11-89-04)008 


Arthur 0. Uttlo, Inc. 

Acom Parte 

CamhrMgs, ltassa«husstts 0214g>2390 


MTA Rsmsdial Rtsourcst, tno. 
Qoldtn, CotoraCo 90401 


U.S. Army Toxic and 
Htzardoua Matorlais Agency 

Procats Dtvak^smsnt Brar^ 
Absfdaan Prov^ Qround, 10} 21010-9481 


DISTRiBUTION UNUiyBiTED 






The views, opink)ns, nx^or flrejtnQS contak^ in th(S report shoutd not b« constrimd 
as an official Dapartmsnt of tn# Amry position, policy, or dsdsion, unlass so dssig- 
naM by other docunwmation. 

The use of trade names in tttis report cfoes not constitute an official endorsement or 
approval of ths use of such corrsnercial prcducts. Thte report may not be citsd for 
purposes of advertisement. 


Final Report to 

United States Army 
Toxic and Hazardous 
Materials Agency 

August 1988 


Laboratory-Scale Soil Washing 
Test on Rocky Mountain Arsenal 
Basin F Material 


(Task Order Number 8) 

Final Report 

A.A. Balasco 
Program Manager 

J.l. Stevens — Task Leader 
J. W. Adams 
D.L. Cerundolo 

S. Rickard (MTA Remedial Resources) 
P.B. Trost (MTA Remedial Resources) 
Principal Investigators 


K « • 


n 










» - 





1 


Distribution Unlimited 


91-18796 

'Mu* iM iMM M. ^ . 


Arthur D. Little, Inc. 

Contract No. DAAK11-85-0-0008 
Reference 54148 

USATHAMA Reference AMXTH-TE-CR-88016 
k/i .J.^ 







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REPORT DOCUMENTA’ilON PAGE 

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4 PERFORMING ORGANIZATION REPORT NUMBERIS) 

Reference: 54148 

S MONITORING ORGANIZATION REPORT NUM8ER(S) 

AM3CrH-TE-CR-88016 

6a NAME OF PERFORMING ORGANIZATION 

Arthur D. Little, Inc. 

66 OFFICE SYMBOL 
{If 

7a. NAME OF MONITORING ORGANIZATION 

U.S. Army Toxic and Hazardous Materials Agency 

6< ADDRESS (Oty, Star*, tnd ZlfCodti 

Acorn Park 


7b ADDRESS (Cty, Sratr and ZIP Code) 

Attn: CETH-TE-D 

Cambridge, Massachusetts 02140-2390 

Aberdeen Proving Ground, Maryland 21010-5401 

3a. NAME OF FUNDING, SPONSORING 

8b OFFICE SYMBOL 

9 PROCUREMENT INSTRUMENT IDENTIFICATION NUMBER 

ORGANIZAT'ON U.S, Army Toxic i 

Ilf ipplkibl*) 

Contract Mo. DAAK11-85-D-0008 

Hazardous Materials Agency 

CETH-TE-D 

Task Order Mo, 8 


ADDRESS (Gfy, Sfjf#, jnd/;RC oO*) 'Q SOURCE OE F 'JNOING NUMBERS 

Attn: CETH-TE-D PROGRAM 

Ab«irdeen Proving Ground. Maryland 21010-5401 


! ' Title (intluot SKunty CUtiitKition) 

Laboratory-Scale Soil Washing Test on Rocky Mountain Arsenal Basin F Material 


PROJECT 

task 

NO 

NO. 


8 


WORK UNIT 


’2 ’ERSONAc aothor(S) a.a. Balaaco, J.I. Stevens, J.W. Adana, D.L. Cerundolo, S. Rickard and 

P.' 


’ 3a type of report 
F inal 


14 DATE OF REPORT {Y«*r, Mwitfi, Diy) tlS PAGE COUNT 

31 August 1988 I 



' T COSATI COOES _ I '9 SUBJECT TERMS (Continue on reverj# if neceoaty *nd identify by b/<xk number) 

GROUP I SUB-GROUP |* Rocky Mountain Arsenal • Basin F • Soil Washing 

• Technology Evaluation • Technology Development/Testing 

• Soil Decontamination • Site Remediation _ _ 


'■■f ABSTRACT (Continue on reverse if neceiwry tnd identify by bi<xk number' The U.S. Amy Toxlc and Hazardous 
Materials Agency (USATErVMA) under its program for Innovative Technology Development for 
Rocky Mountain Arsenal (RMA) issued Task Order Nc. 8 under Contract No. DAAK11-85-D-0008 to 
Arthur D. Little, Inc, to evaluate and rank Innovative technologies for applicability in 
treating Basin F Materials at the Arsenal. As a result of that ranking (Final Report on 
Evaluation/Selection of Innovative Technologies for Testlrg with Basin F materials prepared 
by Arthur D. Little), soil washing was among the technologies chosen for laboratory-scale 
testing and MIA Remedial Resources, Inc. (MTARRI) was awarded a subcontract to perform the 
work. 

To initiate the evaluation of the soil washing process, MTARRI designed and carried out a 
laboratory program to determine; the applicability of the process; and the conditions that 
would remove both the organic and Inorganic contaminants from Che Basin F materials to yield 
a clean soil that could be placed In a fill on-site. The process was Chen proven by a 
demonstration run, at the bench-scale, with Arthur D. Little personnel observing and 


21 ABSTRAa SECURITY CLASSIFICATION 
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CFTH-TE-0 


JO aiSTP'SUT ON / availability of abstract 
□ UMCLASSIFIED/'JNLIMITED □ SAME AS RPT □ ODC USERS 


,:2j name of RESPONSIBLE INDIVIDUAL 
Craig W. MacPhee 


DO FORM 1 473, 94 mar 33 APR edition mty b* U5*d until «»h»uJ1*d 

All oth*f •ditiom *rt ob«>l«l* 


UNCLASSIFIED 





































UNCLASSIFIED 

SECURITY CLASSIFICATIOM Or THIS PAGE _ 

sampling che demonstration run product screams. Using Che laboratory and deii»nstration run ( 
data, a process flowsheet and material balance was produced for a plant to treat approximate!} 
950 tons per day of contaminated Basin F material. 

Laboratory Developiwnt Program - MT^RI had previously shown that the soil washing process I 
coTild remove organics and inorganics from soils; however, no work had been done with a mater¬ 
ial having the particular contaminants contained in Basin F. Therefore, a laboratory develop¬ 
ment program was required to establish the necessary physical and chemical conditions that | 
would remove these contaminants from the Basin F material. 

At the time the scope of work for this program was developed, there were no guidelines avail- , 
able on the degree of contaminant removal that the soil wash should achieve. Therefore, the | 
laboratory program's objectives were to: develop a process to remove as much as possible of 
all the contaminants (both organic and inorganic); establish the technical feasibility of the 
process; and determine the operating parameters within some ranges. Therefore, the labora¬ 
tory's sope of work was limited to process development. 

The results of the laboratory development program established a process that can eliminate ' 
the majority of the aldrin, and presumably the other organic contaminants of concern. To 

accomplish this removal, an organic prewash of an aqueous slurry of Basin F material is needed 

prior to the flotation. 

During the laboratory test work no unusual problems or conditions were evident that would 
cause difficulties when the process is applied on a large scale. Overall, the laboratory pro¬ 
gram was successful in developing a process to clean up Basin F material. It now only remainf 

CO demonstrate this when Che conditions established, from the prior test work, are employed 
in a cesc run continuously from start to finish. The acid wash section that was initially 
I assumed not to need testing is also a part of this complete demonstration run. \ 

As part of MTARRI's task, a laboratory demonstration run of the process developed during the I 
laboratory test program phase was carried out. Arthur D. Little personnel observed the demon¬ 
stration run and were responsible for the collection of samples and their analysis. Data 
generated during the demonstration run were used as the basis for developing the process flow¬ 
sheet and material balance. Sample collection and analysis by Arthur D. Little was to be 
detailed, in that major compounds of concern were to be tracked, as far as practicable, I 

throughout the entire process. Analytical methods used were approved and certified by 
USATHA.MA. 

In addition, the sampling and analytical program was performed to obtain sufficient data to 
confirm certain aspects of the process chat had not been studied extensively during the lab- 
orator;/ development program. For example, the number of stages in Che organic wash section 
and organic flow requirement were to be evaluated from Che demonstration run data; as was Che 
need for a final acid wash of the Basin F material. 

At the time this program was developed, there were no guidelines available on the degree of 
contaminant removal that Che soil washing process should achieve. Therefore, our objective 
was to remove as much as possible of all Che organic and inorganic contaminants. This caused 
us CO use a more extensive process during the demonstration run than was necessary based upon 
the data subsequently obtained from the demonstration run. Therefore, the soil washing pro¬ 
cess for the full-scale treatment of Basin F material has fewer unit operations than were 
employed in the demonstration run. It has been assumed that if the clean washed Basin F 
material meets Che criteria set forth in the EPA's proposed toxic characteristic leaching 
procedure (TCLP), we would have achieved Che required goal of contaminant removal. 

Overall, the demonstration run showed that soil washing of Basin F material can eliminate the 
contaminants, both organic and inorganic,and yield a final clean soil that passes or exceeds 
the proposed TCLP criteria sec by the EPA. 

During Che demonstration run no problems were encountered that were insurmoutable or would 
make this a difficult process to implement on a large scale. The required equipment is 
currently manufactured so no new equipment design or development is required. Reagents used 
„ are, all, available in large quantities.___ (Continued on separate page) _ 


I'NCLASSIFTED 


5CCU«fTY classification OF THIS PAGE 







: UNCLASSIFIED 

CLAssir.CAT.o,, or THIS P*=g OMO rnnMnupH^ _ 

Although some data was not obtained during the demonstration run aad some problems with the 
I calculated material balances were observed, these were resolved by the described assumptions 
and adjusting the mass flow and analysis. These adjustments were necessary so that material 
balances could be developed and equipment sized, but in no way detracts from the conclusion 
that this process will clean up Basin F material. In addition, analysis of the data from the 
demonstration run showed where some process simplifications could be made. These changes 
were incorporated into the full-scale process flowsheet. 

Full-Scale Basin F Soil Washing Process - Using the data collected and numerous flowsheet/ 
material balance studies, a processing plant was designed that will produce clean soil (as 
defined by the EPA's TCLP procedure) chat can be returned to a fill an-site. This plant 
would employ equipment currently available and reagents that are readily available in large 
quantities. 

The largest flow stream in the plant is about 800 gpm (slurry to the organic wash area) and 
the largest piece of equipment, other than tanks, are the four flotation cells at 1500 cu. 
ft. each. 

Overall, a full-scale soil washing plant would be easy to operate, require a minimum of 
maintenance, and would have an above average on-line factor. 

Instrumentation and control loops would be minimal. The major control would be tank levels, j 

I 

The plant would be relatively safe to operate since neither high pressure or high tempera- j 
tures are employed. The plant would be environmentally acceptable since it is temporary and 
all emissions, air, water, and soil would comply with current emission standards. 

If in the final evaluation of Innovative technology to clean up Basin F, soil washing con¬ 
tinues to be a viable technology both from an environmental and cost standpoint, additional 
work is needed to finalize Che process, engineer the plant and finalize the costs for the 
overall project. This additional work would be in three steps: laboratory studies, pilot 
plant demonstration, and engineering design. 

Additional laboratory studies would consist of two parts. First, the process would be 
defined in detail. For e.xample, can toluene be eliminated from the wash solvent, and is 
there a better solvent system that would make the distillation system more effective in 
I eliminating the organic contaminants. Second, data for engineering design needs to be 
I gathered to more accurately size the equipment. Such items needed are size distribution of 
j the feed material to a detailed analysis of flotation variables for scale-up design. 

Pilot/demonstration testing would be required since it would not bs prudent to scale up the 
proposed process from laboratory bench-scale studies to the full-scale plant (950 cons per 
day). Therefore, a pilot/demonstration plant should be built and operated for two to four 
months. This small-scale plant (1000 Ib/hr) would be built based upon additional detailed 
laboratory work which would fi.x the flowsheet so little or no equipment arrangement testing 
will be needed. Therefore, this would be more a demonstration plant with only limited test¬ 
ing on Che effect of process water recirculation, distillation and quality of the clean soil 
produced. All data needed for scaling up to a full-scale plant will be obtained by a month's 
run at steady state conditions. 

During the preceding two steps, the work should be subjected to engineering optimization as 
Che data becomes available. This would require establishing an engineering team to assist 
in program design prior to the start of either phase of work. During the additional data 
collection the engineers could evaluate data and make recommendations for changes, new tests, 
additional data so that upon completion of the pilot/demonstration mn there would be 
sufficient and complete data for the final and detailed engineering of the full-scale soil 
washing process plant. 


UNCLASSIFIED _ 

SeCUSITY CS.»SSIF1C*T10M Of THIS e»GE 





This report was prepared by MTA Remedial Resources, Inc. for 
Arthur D. Little. Inc. in fulfillment of a requirement for 
Task Order Number 3 under Contract DAAK11-85-D-0008. 


SUMMARY 


TABLE OF CONTENTS 


Page No. 

S-1 


1. INTRODUCTION.1 

1.1 Laboratory Development Program...1 

1.2 Demonstration Run.....2 

1.3 Program Analysis and Engineering Design.3 

2. DESCRIPTION OF TEST FACILITIES.4 

2.1 Analytical Support.4 

2.2 Health and Safety. 4 

2.2.1 Worker Protection.4 

2.2.2 Environmental Protection...6 

3. LABORATORY DEVELOPMENT PROGRAM PROCEDURES AMD RESULTS.7 

3.1 Introduction.7 

3.2 Sample (Basin F Material)...8 

3.3 Surfactant Scoping Tests. ...8 

3.3.1 Results of Surfactant Scoping Tests..... 9 

3.4 Flotation/Chemistry Variables Evaluation. 9 

3.4.1 Discussion of Results of Flotation Variables Evaluation.... 9 

3.5 Basic Flotation Process Modification Studies...12 

3.5.1 Discussion of Results for Flotation Process Modification..14 

3.6 Solvent Prewashing Process Evaluation.14 

3.6.1 Solvent Prewash Test Procedure.14 

3.6.2 Discussion of Results of Solvent Washing Evaluation.16 

3.7 Summary and Conclusions of the Laboratory Development Program.... 17 

4. DEMONSTRATION RUN.19 

4.1 Introduction.19 

4.2 Demonstration Run Procedure. 20 

4.2.1 Organic Wash Steps.20 

4.2.2 Flotation Step. 22 

4.2.3 Acid Wash Steps. 23 

4.2.4 Demonstration Run Samples. 23 

4.2.5 Problems During Demonstration Run. 24 

4.3 Demonstration Run Product Analysis and Material Balance...2A 

4.3.1 Analytical Results.24 

4.3.2 Material Balance Calculations.26 

4.3.3 Discussion of Sampling, Analytical and Material 

Balance Results.29 

4.1 Demonstration Run Data Adjustments.29 

4.4.1 Assumptions Used to Adjust Data.29 

4.4.2 Discussion of Adjusted Results.32 

4.5 Process Calculations and Flowsheet Analysis.33 

4.5.1 Acid (Counter-Current Decantation) Wash Section 

(Inorganic Contaminant Removal).33 

4.5.2 Organic Wash Section.33 

4.5.3 Non-Pesticide Organic Contaminant Removal.35 

4.5.4 Heat Balance. 35 

4.6 Summar-y of Demonstration Run. 36 


1 













































5. BASIN F SOIL WASHING PROCESS.37 

5.1 Introduction.37 

5.2 Process Description.39 

5.2.1 Feed Preparation Area.39 

5.2.2 Organic Wash Area.41 

5.2.3 Organic Filtration.41 

5.2.4 Organic Distillation.42 

5.2.5 Flotation Area. 42 

5.2.6 Froth Liquid/Solid Separation.42 

5.2.7 Clean Soil (Tails) Liquid/Solid Separation.43 

5.2.8 Carbon Adsorption.43 

5.2.9 Wastewater Treatment.43 

5.2.10 Volatile Organic Control.44 

5.3 Summary of Basin F Soil Washing Process.44 

6. RECOMMENDATIONS FOR FUTURE WORK.46 

6.1 Additional Laboratory Studies.46 

6.2 Pilot/Demonstration Testing. 46 

6.3 Engineering Optimization.47 

APPENDIX A 

• Soil Wash Plant Flowsheet for Basin F Material 

• Table A - Material Balance Basin F Soil Washing Plant 
























LIST OF TABLES AND FIGURES 

TABLE Page No. 


1 Surfactant Screening Test Results...10 

2 Flotation Process Variable Tests. 11 

3 Organic Addition to the Basic Flotation Process.13 

4 Solvent Washing-Flotation Process Parameter Studies.15 

5 Important Process Parameters for Solvent Prewasli/Flotation 

for the Removal of Pesticides from Basin F Soils.18 

6 Demonstration Run Product Analysis Data.25 

7 Pesticides Material Balance Calculations.27 

8 Inorganic Material Balance Example Calculation........28 

9 Calculated and Estimated Analysis and Material Wts.31 

10 Generalized Material Balance for Basin F Soil Washing Process.40 

FIGURE 

1 Manufacturer' s Drawing of Flotation Cell.5 

2 Demonstration Run Process Steps and Material Flow.21 

3 Generalized Flowsheet for Basin F Soil Wash.38 















SL’WARY 


The U.S. Army Toxic and Hazardous Material Agency (UflATHAMA) under its program 
for Innovative Technology Development for Rocky Mountain Arsenal (RMA) issued 
Task Order No. 8 under Contract flo. DAAK-ll-85-00008 to Arthur 0. Little, Inc. 
to evaluate and rank innovative technologies for applicability in treating 
Basin F Materials at the Arsenal. As a result of that ranking (Final Report on 
Evaluation/Selection of Innovative Technologies frr Testing with Basin F 
Materials prepared by Arthur D. Little) soil washing was among the technologies 
chosen for laboratory-scale testing and MTA Remedial Resources. Inc. (MTARRI) 
was awarded a subcontract to perform the work. 

To initiate the evaluation of the soil washing process. MTARRI designed and 
carried out a laboratory program to detenmne: the applicability of the 
process: and the conditions that would remove both the organic and inorganic 
contaminants from the Basin F materials to yield a clean soil that could be 
placed in a fill on-site. The process was then proven by a demonstration run, 
at the bench-scale, with Arthur 0. Little personnel observing and sampling t!ie 
demonstration run product streams. Using the laboratory and demonstration run 
data a process flowsheet and material balance was produced for a plant to treat 
approximately 950 tons per day of contaminated Basin F material, 

Labcretcrv Teve I comeri'f -rccrem 

MTARRI had previously snown that the soil washing process could remove 
organics and inorganics from soils; however, no work had been done with a 
material having the oarticular contaminants contained in Basin F. 

Therefore, a laboratory development program was required to establish the 
necessary physical and chemical conditions that would remove these 
contaminants from the Basin F material. 


At the time the scope of work for this program was developed, there were no 
guidelines available on the degree of contaminant removal that the soil 
wash should achieve. Therefore, the laboratory program's objectives were 
to; develop a process to ranove as much as possible of all the 


S-1 



contaminants (bovh organic and inorganic); establish the technical 
feasibility of the process; and determine the operating parameters within 
some ranges. Therefore, the laboratory’s scope of work was limited to 
process development. 

The results of fhe laboratory developrent program established a process 
that can eliminate the majority of the aldrin, and presumably the other 
organic contaminants of concern. To accomplish this removal an organic 
pre-wash of an aqueous slurry of 3asln F material is needed, prior to 
the flotation. 

Turino the laboratory test work no unusual problems or conditions were 
evident *hat would cause difficulties when the process is aoplled on a 
large scale, "verall, ti^e laboratory orogram wrss successful in developing 
a process to clean jo Basin ~ material. It now only '“emains to demonstrate 
this when the conditions established, from the prior test work, are 
employed in a *es* run continuously from start to finish. The acid wash 
sec*ion -^hat was ini-^ia!!/ assumed no* to '^eed testing Is also a Dart of 
this ccmplete Semen s-'-at i on r^n. 

Tem<:;nst'~a'*’Icn "“est 

As 030"^ of '.'■'iP^l's Tasn, 3 130003*00'/ demonstration run of the process 
developed dur't-; *ne laccrat'-rv ■"est pregran phase was carried out. 

■*rThur T. Lit'^ie personnel reserved the demonstration run and were 
responsible ‘cr the ooMec^ion of samples and their analysis. Data 
cenerateJ durin-; rne demens-'ra'^ior. "-un were used as th-e basis for deve I op¬ 
ine ■!'ne process flowsheet a^d '"a'eo’al balance. Sample collection and 
analysis bv J. Li'^tle was to be detailed, in that major compounds 

of concern we^e po fracked, as far as practicable, tnrouchout the 
entire process. Anaivtical methods used were approved and certified by 

In ’dditicn, toe sampling and analytical program was performed to obtain 
sufficient da'fp confirm certain aspects of the process that had not 
been studied ex+ensively during the laboratory development program, "or 






exan’ole, **'e 'iurte'" of staces 'f’f'.e organic was ssctior and organic 
‘icw r^o'j i rereor fo Ce evaluated from the deftcnstrat ion run data; zs 

was t-.e need ^zr a final acid was^ of the Basin F nateriai. 

At the time this program was developed, there were no guidelines available 
on the degree of contaminant removal that the soil washing process should 
achieve. Therefore, our ooiective was to remove as much as possible of all 
the organic and inorganic contaminants. This caused us to use a more 
extensive process during the demonstration run than was necessary based 
upon the data subseguently obtained from the o monstration run. Therefore, 
the SOI' washing orocess for the full-scale t' ?atment of Basin F material 
has fewer unit ocerat’ons than were eniployed ’n the demonstration run. It 
has been assumed that ’f the clean washed Rasm F material meets the 

'-o i~‘'- rr-ocsed ’•’cv I * c‘'arac*eni s*ic ’e-ac"'''g 

jc^'evad -“cuireJ xal ccr^omi-ent 

'•-•meva . 

Ove'^a'', the de'^onstra"'o" '•un showed that so’l washing of Basin F material 
can eliminate the contamiriants, both organic and inorganic and yield a 
final e'ean soil passes O'- mceeds the proposed ’CLP criteria set by 

the F ^ A, 

During the demonstraticn nun no proo'ems were encountered that were 
1 nsurnountao> or wou’d -axe th’s a difficult process to implement on a 
large snx’e, ’f'e negjtred »gu'pmen; is Curnently manufactured so no new 
itdu'oment ies'gn or ieve’ocmem*. is n»quired. Reagents used are all 
avai'ab'e ’n ' juan ’ t ••. 

Althougn some iatJ was ''Ot ob'ained during the demonstration run and Seme 
oroo'iJ-'S wi'.n t’-u :a'cj'at»‘d -atenM’ balances were observed, these were 
*y .'i-sr ■ Oe',' »s , jcip'i ,;ns an.} adjust'ng the mass flow and 

ina’ys’s. sdjustm^n*.-; were necessary so that material balances could 

be de..-ioDed md eouipmer* s'/ed, but m np »ay detracts from the 



conclusic<^ that this process M dean jp rfasin P m3*eri3!. In addition, 
analysis of the data from the dercnstration run showed where sens process 
simplifications could oe made, ''hese changes were incorporated into the 
full“scale process ♦lowsheet. 

Full-Scale oasi^ ~ 'dl iVasni^o ^-ocess 

Using the data collected and numerous flowsheet/matenal balance studies, a 
processing plant was designed that will produce clean soil (as defined by 
the EPA's TCLP procedure) that can be returned to a fill on-site. This 
plant would employ equipment currently available and reagents that are 
readily available in large quant'l'es. 

The largest flow stream in the Dl.jnt. is about BOO gpm (slurry to the 
organic wash area) and t.he largest pi>'ce of equipment, other than tanks, 
are the four f’otat'on cells at 1500 cu. ft. each. 

Overall, a full-sca'e soi' washing plant would be easy to operate, require 
a minimum of maintenanre, and would have an above average on-lme factor, 

.nstrumenta 11 on and control ooos would be minimal. The majo** control 
would be tank levels. 

^he plant would be rwlatwely safe to operate since neither high pressure 
or high tempe'-atures are employed. The plant would be environmenta1ly 
acceptable since it 's temoorary and all emissions, air, water, and soil 
would comply with Current emission standards. 

""‘r: r- ' C sr 

!f in the final evaluation of innovative technology to dean up Basin f, soil 
washing continues to be a viab'e technology both from an environmental and cost 
standpoint, additional work is needed to ^maliie the process, engineer the 
plant and final ue the costs for the overall project. This additional work 
would be in three steps: laboratory studies, pilot plant demonstration, and 
engineering design. 





Addlticnal laboratory studies «ou!d consist of two parts. First, the process 
would be defined in detail, "or example, can toluene be eliminated from the 
wash solvent, and is t'-ere a better solvent system that would make the 
distiNation system "ore effective in eliminating the organic contaminants. 
Second, data for engineering design needs to be gathered to more accurately 
size the equioment. Such items needed are size distribution of the feed 
material to a detailed analysis of flotation variables for scale-uo design. 

Pilot/demonstration *e 5 ming would be required since It would not be brudent 
*0 scale ub tne brcoosed Drqqess ^rcm laborator"/ bench-scale studies co *ne 
‘j!!“SC 3 le bian"*" *cns cer davN ’"hena^cre, a bi iqt/demonstrat iqn slant 

should be bui't and ;bera'*ed ‘or •■w" *c *cur mcntn$. "his s^all-scale blar* 
viSCC ib/hr) would be bui'* based ubcn additional detailed labori*crv work 
wn I :h would *'< “"a <;'ws'-eet ';*r!a or no eculomenr .jrranoemen* *e3*lno 
*N i o.v ■'eeded. t'-.a-a^ore, t-’s would be mcra a ’demonstration oian* wl*'* d-n i 
:;-;*a.d *est'"': “"e ef*'?:* crooess water reo i rcu I at ion, distillation an 

duaiitv o‘ t-a -lean soil qroduced. A|i data "ee^ded for scaling uc *0 a full 
s:.a'e clan* wNi be cb*'a;'ed bv -a ~cnth'j run at 3*eadv s^ate condit!o"s. 

Ounng the preceding two steos, the work should be subjected to engineering 
optimijation as the data becomes available. This would rggmre 
establishing an engineering team to assist in program design prior to the 
start of either phase of work. During the additional data collection the 
engineers couM evaluate data and make recommer.dations for changes, new 
.eSvS. additional data so that uoon completion of the odlot/demonstration 
run there would be sufficient and rnmpleta data for the final and detailed 
engineering of the fuH-sca’e soil washing process plant. 






7. INTRODUCTION 


The U,S. Army Toxic and Hazardous Material Agency (USATHAMA) under its program 
for Innovative Technology Development for Rocky Mountain Arsenal (RMA) issued 
Task Order No. S under Contract "Jo. DAAK-11-85-00008 to Arthur 0. Little, Inc. 
to evaluate and rank innovative technologies for applicability in treating 
Basin F Materials at the Arsenal. As a result of that ranking (Final Report on 
Evaluation/Selection of Innovative Technologies for Testing with Basin F 
Materials prepared by Arthur D. Little) soil washing was among the technologies 
chosen for 1aborato'"y-sca!e testing and MTA Remedial Resources, Inc. (MTARRI) 
was awarded a subcontract to perform the work. 

To initiate the evaluation of the soil washing process, MTARRI designed and 
carried out a laboratory program to determine: the applicability of the 
process: and the conditions that would remove both the organic and inorganic 
contaminants '^rom the Basm F materials to yield a clean soil that could be 
placed in a fill on-site. Tne process was then proven by a demonstration run, 
at the bench-scale, with Arthur D, Little personnel observing and sampling the 
demonstrat ion run product streams. 'Jsmg the laboratory and demonstration run 
data a process flowsheet and material balance was produced for a plant to treat 
approxmately 950 tons per day of contaminated Basin F material. 

"rom the laboratory data, demonstration run results and the flowsheet and 
material balance calculations, capital and operating costs were then 
developed. This cost data is reported m a separate memorandum report for 
incorporation into the Final Firoject Report being prepared by Arthur 0. Little. 
Inc. 


^^ L aborcatpry Development ^n ggram 

"■^TAPRI had previously shown that the soil washing process could remove 
organics and inorganics from soils: however, no work had been done with a 
material having the particular contaminants contained in Bas in F. 
’herefcro. a laboratory development program was required to establish the 
necessary phys’cal and chemical conditions that would remove these 
contaminants from the Basm F material. 




At the time the scope of work for this program was developed, there were no 
guidelines available on the degree of contaminant 'emoval that the soil 
wash should achieve. Therefore, the laboratory program's objectives were 
to: develop a process to remove as much as possible of all the 
contaminants (both organic and inorganic); establish the technical 
feasibility of the process: and determine the opera*”'ng parameters within 
some ranges. Therefore, the laboratory's scope of work was limited to 
process development. 

The data from the laboratory program and demonstration run along with 
engineering judgment were used in the preparation of the preliminary 
process flowsheet and the specification and selection of equipment for a 
full-scale (950 ton per day) treatment plant. The flowsheet and equipment 
specified were then used to estimate the capital and operating costs for 
the full-scale soil washing plant. 

Process conditions established during laboratory development program are 
oresented in Section 3 of this report. The optimum conditions were then 
used in the subsequent demonstration run. 

1 .2 Oemonstraticn 

During the week of April 6, 1987, 'irARPI carried out the demonstration run 
using the techniques and reagents which pruvided the best removal of the 
contaminants from Basm F material based upon the laboratory program. 

During this demonstration period, Arthur 0. Little, Inc. personnel observed 

the run and collected the samples to be analyzed to determine clean up 

effectiveness and to obtain data for materia! balance. These samples were 
analyzed in the Arthur 0. Little. Inc. laboratory which has been certified 

by dSATHAMA for the chemical compounos of concern. The results were 

reported to ‘''TARRI, and are incorporated in the discussion of the 
demonstration run (Section A), 


- 2 - 





1.3 Program Analysis and Enqineering Design 

The scope of the laboratory program did not provide for the collection of 
all the data necessary to design a full-scale plant since this program was 
a preliminary technical assessment of the soil washing process as applied 
to Basin F material. In addition, some data was not obtained during the 
demonstration run. These factors created the need for extensive treatment 
of the data, flowsheet analysis, and engineering estimates to complete the 
process evaluation. The calculations and assumptions used for this data 
treatment are discussed briefly as part of the evaluation of the 
demonstration run. The results of the overall analysis of the program data 
were used to complete the detailed flowsheet and to develop the capital and 
operating costs for a Basin F material washing plant. 


- 3 - 





2 . DESCRIPTION OF TEST FACILITIES 


The laboratory development program and the bench-scale demonstration run were 
carried cut in a 300 square foot laboratory. For health and safety concerns 
this laboratory, with its contained equipment, was totally dedicated to this 
single project. 

Other than the flotation machine, all laboratory procedures were carried out in 
standard glassware and with conventional laboratory equipment, such as pH 
meters and balances. The flotation machine used was a Denver Equipment D-12 
Lab float machine (Figure 1 is the manufacturer's drawing). In all tests, a 
1000 gram tank was used. This machine provides agitation and aeration, to 
separate hydrophobic materials from the bulk of a slurry. 

2.1 Analytical Support 

The laboratory develcoment program was supported by three different levels 
of analysis. Initial analyses used methylene chloride extraction in 
Soxhlet extractors to produce data to determine the degree of removal of 
the gross organics. This was followed with detailed analysis, by an 
indeoendent analytical laboratory, to determine the disposition of aldrin 
in the test products. Also. ’^TAPPI used its own analytical capabilities to 
aid in the laboratory program. 

For the demonstration run, analytical work was performed by Arthur D. 

Little using USATHANA certified procedures. 

2.2 '-lea 1th and Safety 

Handling and containment of 3asin F material was necessary to safeguard 
workers and the environment. Specific procedures followed are summarized 
below. 

2.2,1 .-iorker P>'otection 

When working with, and around 3asin F material, several steps were 
taken to protect the employees. Medical surveillance was established 
for the employees who would be in contact with the material by 


- 4 - 





FIGURE 1 

















TT! 


' “I^rt 

























X 


pre-exposure physical examinations, including extensive blood 
chemistry analysis. Upon completion of the work, they were examined 
once again to make sure they had not been exposed to excessive levels 
of chlorinated organics. 

While working in the dedicated laboratory, complete changes of fresh 
clothing were provided daily. The clothing was covered by Tyvek* 
coveralls and Tyvek*shoe covers. Hands were protected by two gloves, 
both of which were solvent resistant. Respirators approved for 
organic vapor and dust protection were utilized at all times in the 
laboratory, as were safety glasses. 

2 . 2.2 Environmental Protection 

The dedicated laboratory was provided with a negative pressure 
ventilation system to prevent release of any toxic materials outside 
the laboratory. The heating and cooling system was isolated to 
eliminate diffusion. All equipment in the laboratory remaitied in the 
laboratory for the duration of the entire program. Lab wastes and 
cleaning materials were placed in a sealed container in the 
laboratory; when the laboratory is decontaminated all waste will be 
drummed and shipped back to RMA. 


- 6 - 


3. LABORATORY DEVELOPMENT PROGRAM PROCEDURES AND RESULTS 


This section discusses the work completed during the laboratory development 
program to evaluate the soil washing process on Basin F material. 

3.1 Introduction 

MTARRI's prior work on other contaminated soils provided base line 
information on the soil washing process and reagents which had predicable 
pronability ot success on Basin F material. Initially, it was assumed that 
the inorganic contaminants would be easily removed using a counter-current 
acid wash: this assumption was based upon previous work with soils 
contaminated with the same type of inorganic contaminants. Therefore, this 
step was not examined during the laboratory phase of the program but would 
be te'ted during the demonstration run. 

Previous work by MTARRI on other projects indicated that organic 
contaminants could be freed from soil particles and subsequently separated 
using froth flotation by reacting an aqueous slurry of contaminated soil 
with a mixture of caustic, silicate and a surfactant. This served as the 
starting point of this investigation. In order to expedite the program and 
control costs, it was assumed that if the major contaminant (aldrin) could 
be removed from the contaminated material then the other organic 
contaminants could be also. Therefore, during this laboratory program 
aldrin was the only contaminant monitored. 

Since gathering engineering data was not one of the objectives of this 
assignment, we did not, for example, study in detail the settling rates of 
the slurry after flocculation to carefully size thickeners. We only 
determined if the material could be flocculated, and by observation 
determine if settling was within acceptable rates. Consequently, 
engineering judgments were used in the selection and sizing of much of the 
equipment for the preliminary process flowsheet design. 


- 7 - 




To summarize: the objective of the laboratory program was simply to 
determine the physical/chemical conditions that would remove the 
contaminants from Basin F material using equipment that, based upon our 
professional engineering judgments, could be applied on a large scale. 

3.2 Sample (Basin F Material) 

The contaminated Basin F material used in this program was received in two 
5 gallon sealed plastic pails, early in January 1987. from Rocky Mountain 
Arsenal. This sample was a wet mass with the consistency of moist modeling 
clay. The two pails were mi.-'ed together by emptying them onto a plastic 
sheet and combining them into a single pile. This pile was remixed five 
times and then split in half and returned to the original plastic pails. 

The two pails were then stored at room temperature. 

Several observations were made during the mixing operation. First, the 
sample appeared to be homogeneous. Second, there were no coarse rocks or 
sand. Third, there were lumps of a black material (up to 1/2 inch in size) 
which resembled asphalt. 

Four samples of the Basin F material were taken during the mixing process. 
One of these samples was sent to Arthur D. Little. Inc. for analysis. Two 
of the samples were sent to an independent laboratory for aldrin analysis, 
while the fourth was held in reserve. 

3.3 Surfactant Scoping Tests 

Of the numerous surfactants available, three (each of a different type) 
were selected to be tested. The selection of these three was based upon 
past experience with surfactants that have performed well, each for 
differing types of contaminants. These three were: 1) Biosoft EA4*, an 
alkyl ethoxyelated alcohol, nonionic, soluble in water and organic 
solvents, which has seemed to perform well for a wide range of 
contaminating materials, 2) Makon NFS®, an alkyl aryl ethoxyelated 
surfactant, oil soluble, which removes heavy oils, and 3) Stephanflo 20*, 
an anionic olefin sulfonate, which removes light oils. 





In these scoping tests, 700 g of wet feed (heads) was mixed with one liter 
of water to which sodium hydroxide (to pH 9.5), sodium silicate (7 Ib/ton) 
and surfactant (3 Ib/ton) had been added. This slurry was then mixed at 
room temperature for twenty minutes. The slurry was transferred to the 
1000 g float cell, diluted to 2.5 liters and floated for 30 minutes. The 
tails (washed material) from tests 1, 2 and 3 were then submitted for 
aldrin analysis. 

3.3.1 Results of Surfactant Scoping Tests 

Table 1 presents the results of the surfactant scoping tests (tests 1 
through 3). As can be seen, the Biosoft EA4 achieved greater removal 
of aldrin than the other two and was therefore selected to be used 
throughout the remainder of this program. 

3.4 Flotation/Chemistry Variables Evaluation 

The next series of tests was directed at evaluating the process variables 
for flotation removal. Table 2 presents the data for these tests (tests 4 
through 10). 

These tests were similar in nature to the scoping tests, in that a known 
amount of wet feed (heads) and 2.5 liters of water were added to the 1000 g 
flotation cell. This slurry was mixed using the flotation machine, without 
air, during which time reagents were added. After a suitable time of 
mixing (20 to 30 min.), air was introduced and the froth collected. The 
variables tested are shown in Table 2. 

In tests 8 and 9, the Basin F feed material was slurried with water then 
the solids flocculated and the liquid decanted. This was done to see if 
removal of soluble salts would aid in the flotation removal of the 
pesticides (aldrin, etc,). 

3.4.1 Discussion of Results of Flotation Variabli s Evaluation 
Variables examined were not all inclusive, but were the ones that were 
believed to have the greatest effect upon organics removal from Basin 

F material. As can be seen from Table 2, flotation alone was not 
effective in eliminating aldrin to a level of more than a few hundred 


- 9 - 







TABLE 1 


SURFACTANT SCREENING TEST RESULTS 


TEST MO. 

SURFACTANT USED 

TAIL (WASHED FEED MATERIAL) ANALYSIS (pom) 



Aldrin 

Oieldrin 

Isodrin 

1 

BioSoft EA 4 

465 

203 

62 

2 

Makon NF 5 

875 

415 

31 

3 

Stephanflo 20 

711 

277 

6 

Head 

(Contami 

1 nated Feed ’’’aten a 1 ) 

1190 ± 200 

460 ± " 

42 ± 7 


Source: f'H'A Remedial Resources, Inc. 





table 2 


FLOTATION PROCESS VARIABLE TESTS 


TEST 

■JO. variable ’ES’ED 

: SOLIDS 

Pi DRY TAIL 

ppm ALDRPi 
i?J DRY tail 

: DISTRIBUTION 

OF ALDRIN IN TAILS 

4 

Repeat "est 1 

91 

not analyzed 

— 

5 

'•■otation Time 

73 

310 

20.3 

6 

'^lotat'cn "ime 

91 

520 

39.7 


Ong . • f 1 (It- 

37 

570 

41.8 

3 

^'■ewa'ih 

33 

420 

30.9 

9 

P<'ewa$h-Car(;c'i 

92 

660 

51.1 

:0 

Caustic Atjd't'on 

33 

350 

62.8 


' Cantamtrated "eed '^atenial' 

1190 1 200 



'^O'jrce: '"^TA Inc. 


n 




parts per million. None of the process variables studied reduced 
aldrin below a few hundred parts per million so it appeared that 
flotation alone would not effectively dean up Basin f material. 
However, aldrin removal achieved by flotation was greater than the 
solids in the froth: therefore, it was concluded that if aldrin could 
be freed from the substrate it could be selectively removed. During 
these tests, it was observed that some black, asphaltic type particles 
were not removed by flotation, and the assumption was made that these 
black organic lumps were holding the balance of the pesticides. 
Therefore, a technique to cause the removal of this black, asphaltic 
material needed to be developed. This led to the next phase of the 
study, in which organic solvents were used to dissolve these black 
particles and/or to cause them to float, 

3.5 Basic Flotation Process ‘■Modification Studies 

The third senes of tests used organic solvents to determine whether the 
black, asphaltic material, observed in prior tests, could be made to float 
or dissolve so as to release the pesticides (aldrin) and thus imorove the 
degree of decontamination of the Basin F material. Various solvents and 
techniques were tried m tests 11 through 15 to examine this modification 
to the basic soil washing process. Table 3 presents the summary data for 
these tests. 

For tests 11. 12 and H, the Basin F material was combined with water and 
reagents, as before, m the flotation cell during anitation. Organic 
solvent was added to the agitated slurry and mixed for 10 to 30 minutes. 
Once thoroughly mixed, air was introduced and the resultant froth removed. 

In tests 13 and 15 the Basin F material, water, and the reagents used in 
the flotation chemistry studies were mixed together. After approximately 
30 minutes of mixing, the organic solvent was added and agitation continued 
for an additional 30 minutes. The agitation was then stopped, the mixer 
removed and the slurry allowed to settle during which time the organic 
phase floated to the top and was removed by decantation. The residual 
slurry was transferred to the flotation machine and floated as in all 
previous tests. 


1 ? 


__SSJ3(W<I NOIlVldlj_ 

Oisva 3H1 01 NOIIIOQV DINVOW 


z — 
o < 

H* 






CO « 


<—• 


cr 

m 

•■4 

• 

• 




0£. SS 


CO 

o 

c^ 

CM 

1—• 

C/^ QC 


00 

CM 

4q> 



< 

u. 

O 



8 


CM 

♦4 

O 

(Tv 

ftm 



13 


Source: MTA fteraedidl Resources, Inc 








3.5.1 Discussion of Results For Flotation Process Modification 
Data from tests 11, 12 and 14 indicate that the addition of organic 
solvent and the recovery of the solvent by flotation, was not an 
effective way to reduce the aldrin concentration in the tail solids. 
However, addition of the organic solvent with removal prior to 
flotation (tests 13 and 15) produced better removal of aldrin from the 
soil (tails) tnan all previous tests. (Mote also that with the pre- 
organic wash followed by flotation, the amount of solids reporting to 
the tails was greater than when flotation was used alone.) 

These five tests suggested that pre-treatment of Basin F feed material 
with an organic solvent prior to flotation would improve the 
effectiveness of the process: that is, a greater degree of aldrin 
removal was achieved. The next series of tests were performed to 
gather data on organic solvent washing in combination with flotation. 

3.6 Solvent Prewashmq Process Evaluation 

Twelve additional tests (16 through 27) were conducted to define the 

process operating conditions pnior to the scheduled demonstration run. 

These tests centered mainly upon the organic solvent pre-wash section. 

Table 4 presents the data from these tests. 

3.6.1 Solvent Pre-wash Test Procedures 

Organic solvent pre-wash was accomplished by mixing varying amounts 
and types of organic solvents with an aqueous slurry of Basin F feed 
material. Subsequent to mixing, the bu’k of the solvent was removed 
by settling and decanting of the floating solvent/emulsion. In the 
staged tests, this step was repeated two or more times. Following the 
last decantation, the required flotation reagents (caustic, silicate 
and surfactants) were added to the slurry and this slurry subjected to 
flotation to remove any trace of the added organic solvents and 
additional Basin F contaminant. In one test (test 12), flotation was 
employed between each stage of solvent washing to enhance solvent 
remova1. 


- 14 - 









Total including intorstage 



3.6.2 Discussion of Results of Solvgnt Washing EvaTuation 
Tests 16 through 27 were scoping in nature and as such have certain 
limitations in determining the extent of removal of aldrin that can be 
achieved using the solvent pre-wash; however, even with this 
limitation, several important conclusions and observations could be 
made. The major conclusion is that organic solvent prewashing does 
effect a good removal of aldrin. 

Test 16 was run to compare the kerosene-toluene mixture with the 
kerosene-octanoI mixture used in test 15 (Table 3). The results 
appeared to be the same but better than diesel (kerosene) alone (test 
13. Table 3). Remaining unanswered was the question "Did these two 
mixtures remove aldrin attached to different constituents in the Basin 
F material'i'" 

Therefore, a toluene, kerosene, octanol-1 (TKO) solvent was tried in 
test 18. The three component solvent removed more aldrin, therefore 
in all subsequent tests this TKO mixture was used. No other solvent 
mixtures were tried but it is very likely that other combinations 
could be found that work as well or better. 

Test 17 was carried out with a very small amount of organic solvent 
mixture, with flotation to recover it between mixing stages. The 
results show that this technique yields the same results as decanting, 
but uses less solvent and fewer stages. This may be the preferred 
method to be employed in a full-scale plant. This method was not 
employed in the laboratory because of testing difficulties at this 
small scale. 

Test 19 was run to see if staging could be eliminated using a larger 
volume of solvent. It seemed this was true. However, a repeat of 
single stage test (test 27) indicated poorer results, which could have 
also been the result of a shorter flotation time used in this test. 


- 16 - 



Tests 18 and 22 were comparable tests but the level of agitation used 
in test 22 was higher than test 18. This indicated that mixing speed 
was an important variable. However, time of mixing, at least beyond 
20 minutes, does not appear to offer any advantage. 

By comparing data from tests 19, 20, 22, 26 and 27 it appears that the 
total flotation time was an important process parameter. To achieve 
good removal of pesticides flotation times in excess of 60 minutes or 
more will be required. This data also indicates that heating during 
the solvent washing is not necessary to achieve good pesticide 
(aldrin) removal. 

This series of tests did elicit the major important process variables 
for treating Basin F material via a soil washing process. Table 5 
presents these variables in an order of importance over the ranges 
tested. 

3.7 Summary and Conclusion of the Laboratory Development Program 
The results of the laboratory development program established a process 
that can eliminate the majority of the aldrin, and presumably the other 
organic contaminants of concern. To accomplish this removal an organic pre¬ 
wash of an aqueous slurry of Basin r material is needed, prior to the 
flotation. 

During the laboratory test work no unusual 
evident that would cause difficulties when 
large scale. 

Overall, the laboratory program was successful in developing a process to 
clean up Basin F material. It now only remains to demonstrate this when 
the conditions established, from the prior test work, are employed in a 
test run continuously from start to finish. The acid wash section that was 
initially assumed not to need testing is also a part of this complete 
demonstration run. 


problems or conditions were 
the process is applied on a 


- 17 - 




TABLE 5 


IMPORTANT PROCESS PARAMETERS FOR 
SOLVENT PREWASH/FLOTATION FOR THE 
REMOVAL OF PESTICIDES FROM BASIN F SOILS 
(in apparent order of importance) 


PARAMETER 

COMMENT 

RANGE STUDIED 

PROBABLE MINIMUM 
REQUIRED 

Flotation Time 

Needed after solvent wash 
to achieve removal of all 
orgamcs. 

30-130 min 

> 60 min 

Stage Addition 

Will reduce amount of 
solvent required 
(counter current). 

1-7 stages 

2 to 4 

Amount of Solvent 

With better interstage 
removal can reduce amount 
used. 

30 ml-400 ml 
per 2 liter 
slurry 

< 30 ml 
per 2 liter 
slurry 

Interstage 

Separation 

Can be achieved by long 
settling time or flotation. 

1-48 hrs. 

use flotation 

Mixing 

Greater mixing energy will 
improve removal of 
contaminants. 

very low to 
low 

unknown 

Mixing Time 

Mixing energy input and 
mixing time must go hand 
in hand. 

20-130 min 

unknown 

Solvent Mixture 

Mixture used probably un¬ 
necessary. Maybe, with what 
is now known, use kerosene 
alone or with 1-2% Octanol-1. 

up to 40% 
other than 
kerosene 

kerosene alone or 
or 1-2% octanol 

Temperature 

Unimportant in solvent wash, 
but needed in flotation. 

Room to 75’C 

none in solvent 
wash, approx. 

50°C 

in flotation. 


Source: MTA Remedial Resources. Inc. 


- 18 - 



4. DEMONSTRATION RUN 


This section describes the demonstration run procedures, presents and discusses 
the results and how they were used to develop the process flowsheet and 
material balance for the "Soil Wash Decontamination Process for Basin F 
Materials." 

4.1 Introduction 

As part of MTARRI's task, a laboratory demonstration run of the process 
developed during the laboratory test program phase was carried out, Arthur 
D. Little personnel observed the demonstration run and were responsible for 
the collection of samples and their analysis. Data generated during the 
demonstration run were used as the basis for developing the process 
flowsheet and material balance. This data In turn led to the development 
of the capital and operating cost estimates (presented in a separate 
memorandum report). Sample collection and analysis by Arthur D. Little was 
to be detailed, in that major compounds of concern were to be tracked, as 
far as practicable, throughout the enti-e process. Analytical methods used 
were approved and certified by USATHAMA. 

In addition, the sampling and analytical program was performed *o ootain 
sufficient data to confirm certain aspects of the process that had not 
hoen studied ey+onsively during the laboratory development program. P'or 
example, 'I’he number of stages in the organic -ash sec+ion and organic 
flow reauirement were to be evaluated frcm demonstration run data; as was 
the need for a final acid wash of the Basin F material. 

At the time this program was developed, there were no guidelines available 
on the degree of contaminant removal that the soil washing process should 
achieve. Therefore, our objective was to remove as much as possible of all 
the organic and inorganic contaminants. This caused us to use a more 
extensive process during the demonstration run than was necessary based 
upon the data subsequently obtained from the demonstration run. Therefore, 
the soil washing process for the full-scale treatment of Basin F material 
has fewer unit operations than were employed in the demonstration run. It 
has been assumed that if the clean washed Basin F material meets the 


- 19 - 



criteria set forth in the EPA's proposed toxic characteristic leaching 
procedure (TCLP), we would have achieved the required goal of contaminant 
removal. 

4.2 Demonstration Run Procedure 

Figure 2 shows the demonstration run steps used and the material flows. 

4.2.1 Organic Wash Steps 

In step 1, 686.2 grams of mixed wet feed sample was taken from the 
5-gallon storage container and put into the round bottom mixing tank. 

To this 2 liters of tap water from Golden, Colorado municipal water 
•system was added. Mixing was begun using a 2 1/2" diameter three 
blade marine type propeller turning at 900 rpm. When the solids had 
been dispersed the organic solvent mixture (TKO) was added. This 
organic mixture consisted of 69. kerosene, 20.0* toluene and 10.6% 
octanol on a weight basis. The slurry was heated, and the temperature 
reached ^1*C. (Due to the ^act that there were tight time constraints, 
not all of the data obtained during the Iaborator/ deveiopment phase 
of the program was comolately analyzed prior to the demonstration 
phase testing, this is true with respect to the data indicating that 
heating during solvent washing is not a necessity *o achieve good 
aldrin r-emovaI. As a result, heating was used during the demonstration 
phase testing.) Mixing was continued for 60 minutes. Mixing was 
stopped and the agitator removed from the slurry and the slurry 
settled for 60 minutes, 'i’he organic layer on taop was then carefully 
decanted (158 ml) from the aqueous slurry. 


In step 2, 200 ml of fresh TKO mixture was added to tne mixing tank 
containing the aqueous slurry from the previous wash step, the 
agitator replaced, heaters turned on and mixed for 60 minutes. During 
this second period of mixing the temperature reached As before, 

the mixer was stopped, removed and the slurry settled for 60 minutes 
and the organic layer (90 ml) carefully decanted off. In this step 
the recovery of organic solvent was poor. 




- 20 - 








cess Steps 
w 


0 0 


0 0 


)(«■ 




lartt 

Floccufcr} 

Wol»f 

Wcler 

lUttic 


Acid 

Acid 

rfoclonl 


Roc oj lord 

riocojlcnl 


Wcter 

nocojlor.) 






fixi(h 
Skrrj 
850 ml 
rma kko 



1*1 Acid 
Wosh 

zceomi 

RMA lOAl 


2 nd Aod 

Woih 
2000 fH 

Rma ICM2 


3rd Acid 
Wosh Fillrcle 
2600 rrJ 
RMA ICK3 



Toll 

(Cleon Soil) 
Not Meosured 
RMA 1038 


FTotoliofi 
Sect' 


Toil Wash Section 






Step 3 was started similar to step 2 but it was observed that the 
system was flocculated. Therefore, 2.7 g D grade sodium silicate was 
added which broke up the flocculants. Mixing was continued for 60 
minutes and in this step the temperature rose to 44‘’C. Again the 
mixer was stopped and the agitator removed and the slurry allowed to 
separate for 60 minutes. After settling, the organic layer was 
decanted off and 356 ml of organic solvent were recovered. 

Step 4 was run the same as step 2 and no additional silicate was 
required. In this step, the temperature reached 68°Cduring mixing; 
205 ml of organic solvent was decanted. 

In step 5. 200 ml of TKO mixture was again added to the aqueous slurry 
from the prior step and mixed for 60 minutes as in the previous steps; 
in this step the temperature rose to 69°C. After the mixing the mixer 
was stopped and removed; the slurry was allowed to settle overnight 
before the organic solvent (218 ml) was decanted. 

4,2.2 riotation Step 

After as much organic solvent as possible was removed, the entire 
volume of aqueous slurry was transferred into the 1000 g flotation 
cell and placed in the laboratory flotation machine. About 1 liter of 
water was added to this mixture and the flotation machine agitator was 
started and the slurry heated with immersion heaters. Then the 
following reagents were added: 

3.50 g Caustic (^JaOH) 

2.00 g 0 grade Sodium Silicate 

0.19 g Biosoft EA4* 

The slurry was mixed and heated for 15 minutes prior to the start of 
flotation. After mixing, the slurry was at 49°C and had a pH of 11. 

Flotation was started by the injection of air with the machine rpm at 
1200. The froth was continuously removed for 30 minutes at which time 
additional surfactant (0.16 g Biosoft EA4*) was added and the rpm 
increased to 1500. Flotation and froth removal was continued for a 
total of 60 minutes. The froth volume was measured at 350 ml, and the 
tail (clean soil) slurry at 2200 ml. 


- 22 - 





The tail slurry was transferred to a 4 liter beaker where flocculants 
were added so the solids could settle and dear water recovered. The 
flocculants used in this step consisted of both organic and inorganic 

compounds: 100 ml of 0.1 g/1 Superfloe 84* solution and magnesium 
chloride. Recovered water was 850 ml after settling for 1 hour and 22 
minutes. 

4.2.3 Acid Wash Steps 

The settled solids remaining were then acid washed in three stages 
using hydrochloric acid (steps 8 through 11). 

In the same beaker used to initially decant off tail water, tap water 
was added to bring the total slurry volume to 3600 ml. HCl was then 
added during mixing to bring the pH down to 5.0; this required 7.3 ml 
of reagent grade acid (37!t HCl), The solids were flocculated again 
using Super-^loc 84* and allowed to settle for 30 minutes. After 
settling. 2.05 1 of clear solution was recovered. 

For the second wash (step 8) tap water was added in the same beaker to 

bring the slurry volume back to 3600 ml. Again HCl was added to pH 

4.3 (1.3 ml reagent grade acid, 37^ HCl) during mixing. The slurry 

was flocculated using the same reagents and allowed to settle; 2.0 1 
of clear solution were recovered. 

The last wash (step 9) was carried out as before, except no acid was 
added: the volume was brought up to 3600 ml with tap water and mixed 
briefly. The pH was 4.9. Flocculant was added and allowed to 
settle. In this step, the clear liquid was decanted off and the 
settled solids were transferred to two Buchner filters to remove 
additional solution. The filtrate and decanted solution were combined 
for a total volume of 2300 ml. The wet filter cake was transferred to 
sample jars. 

4,2.4 Demonstration Run Samples 

During tms demonstration run samples of the products were collected 
by the Arthur D. Little observer. The Arthur 0. Little laboratory 
numbers assigned to these samples are shown in Figure 2. 








The organic solvent material and tails (washed Basin f material) were 
taken m their entirety as samples. In the case of the tails, the 
sample was nlaced in two containers. Only a portion of the other 
streams wc'“f taken for a sample and the remainder discarded; this 
includes the froth slurry, 1st, 2nd, and 3rd acid wash solutions. The 
tail dec*.-’* liquid was not sampled. 

4.2.5 *y~.blems During Demonstration Run 

One process problem which arose during the demonstration run was 
flocculation that occurred during the organic wash (step 3) and 
prevented complete recovery of the TKO (organic wash solution). This 
pr-^'-'. was resolved by adding sodium silicate which improved TKO 
so .* on recovery in the last three wash steps. 

Several problems arose 'n data acquisition for the demons*r’it!cn run 
that created gaos ’n the data, first, the failure to sample the tail 
decant ' iquid. Second, failure to measure the volume and weight of 
tail slurry. Third, failure to analyze all the products for all 
the contvfm-nants of concern, especially the washed Basin F material 
vtail). f.urth. the failure to determine the solids in the test 
product samples. *0 comp sate for these data gaps, some assumptions 
and calculations were m- to fill in the missing data. This is 
discussed more m the following sections. 

4,3 Demonstration hun Product Analysis and 'iaterial Balance 
Analysis of the products and the material balances arising from the 
demonstration run data are presented in this section. 

4.3.1 Anal yt i cal >?esu Its 

Samples of the various output strears from the demonstration run were 
analyzed by Arthur 0. Little using USATHAMA-approved and certified 

ire r'"“sentad |n 'able 6. Also, Included 
"ao'e r ir.^ **■0 anal/s‘s ~f **“« freer "*'0 organic ■"Uture and tap 
wa*er ijced. l- -ao’e t: ♦'■e of a 'TL= laacrahe ‘est ryn cn 'ha 


- 24 - 




m 






tails (washed Basin r material) are given in the column labelled 
Leachate. The blanks in this table are where no analyses were 
performed. 

4.3.2 Material Balance Calculations 

A measure of how carefully laboratory tests were run and analyses were 
performed is how well the amount of material in the feed can be 
accounted for in the test products, that is. a material balance. 

Using the analytical data in Table 6 and the volumes of outflowing 
streams given in Figure 2, material balance calculations were made. 

Material balance calculation for the pesticides is shown m Table 7. 
For all the pesticides there is excess (15 to 2311) material, when the 
five organic wash solutions are compared to the feed. The cause for 
this discrepancy is unknown; possible sources contributing to this 
excess include imprecise measurement of volumes and/or weights or lack 
of precision and accuracy of the chemical analyses. 

'Material balance calculations for some of the inorganic materials are 
shown in Table 3. In these calculations, the concentration of 
material in the solution from the tail decant (step 7) and the 2nd 
Acid Wash solutions had to be estimated as part of the material 
balance calculations. 

‘lotice that with the exception of fluorine, the material balances for 
inorganics are poor. In these cases, the discrepancies in the 
material palance are considerable such that neither errors in sample 
volume measurements or analytical results could explain them; the 
unaccounted for material is either in the froth, or tail slurry which 
were not analy7''d for these inorganic compounds. 






I 


WA Raat«iia| fe*. 






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« 3t(Vl 


1 


$,P;§g5SSgSSS3S3S 

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p'* «N rsj ^ ^ ^ 


jiNcNiN 


c 3 ? a s? ^ 

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- ci- :1^ ^ J 2 ^ ^ i' 


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Souicei WA Fd-idi,i Siij^rcts 





In the case of fluorine, the material balance approaches 90^ when the 
amount that could have been contained in froth slurry liquid is added 
to the total. 

4.3.3 Discussion of Sampling, Analytical 
and Material Balance Results 

As in most research programs where considerable amounts of data are 
collected, some data is overlooked and some does not fit because of 
inaccuracies made in measurements or in analysis. When this occurs, 
the data that has been obtained must be normalized for use in 
developing overall material balance. 

The data obtained was adjusted using assumptions in order that a 
process material balance could be developed. This normalization and 
the assumptions used are discussed in the following section. 

4.4 Demonstration Pun Data Adjustments 

In the preceding section specific data gaps were identified in the data to 
be used for material balance calculations. Therefore, adjustments were 
made to the data collected so as to compile a consistent data set for 
subsequent material balance calculation and process equipment sizing. 

4.4.1 Assumptions Used to Ad.iust Data 

The data gap of most concern involved the lack of information 
regarding the distribution of solids in the froth and tails. To 
resolve this issue, several assumptions were made based upon previous 
test data. These assumptions included: 

1) the feed sample was 75% solids: 

2) the specific gravity of the froth slurry was 1.02: 

3) the tail slurry was 1 liter in volume and contained 36% solids. 

The first assumption was based uoon the percent solids determined in 
the preliminary laboratory program. The specific gravity if the froth 
slurry estimate was based upon a measurement made by Arthur D. Little 
which was measured in the laboratory and found to be about C.98. It 


- 29 - 






was assumed that the technique used had an error of about ±0.04 points 
and so 1.02 was used since the slurry density had to be greater than 
water. Using a solids density of 2.65, the weight of solids in the 
froth slurry was then calculated. It was necessary for the last 
assumption to be made since the tail slurry was collected in two 
containers and was not remixed (homogenized). Consequently, 
measurements on a single container alone (as was done) was not 
sufficient to accurately determine the percent solids. However, a 
measuremen*' on one of the containers (believed to ha*e the lowest 
percent solids) determined the percent solids to be 32%: so the 
assumption of 36% solids seems reasonable. 

The results of these calculations and assumptions are presented in 
Table 9. 

The next assumptions made were that the solution in the tail slurry 
had the same concentration as the 3rd Acid Wasn solution and that the 
TCLP leaching process removed all of the compounds of interest 
remaining adsorbed on the solids. The first assumption is reasonable: 
the second is questionable. Using the volumes of filtrate and volumes 
of leach solution, the total amount of the compounds of interest were 
then calculated and the excess over that in solution was assumed to be 
associated with the solids. 

The solids may have more of the compounds of interest than calculated 
by this method: however, this does not affect the material balance 
used for flowsheet development. 

Results of this calculation of the tail slurry, tail (clean soil) and 
tail solution analysis are presented in Table 9 in the columns headed 
Tail Slurry (Total, Solids and Soln). 

The balance of the adjustments were made based upon volume of solution 
added and removed, and the assumption that no inorganic salts were 
contained in the organic wash solutions. The final normalized data is 


- 30 - 





31 









shown in Table 9. Where ND occurs, zero values were assumed rather 
than detection limit values in performing the material balance 
calculations. 

4.4,2 Discussion of Adjusted Results 

Comparison of Table 9 with Table 5 indicates that even though 
assumptions and estimates had to be made, there is considerable 
agreement between the data. Consequently, the assumptions and 
subsequent calculaticrs oased on these assumptions did not result in 
any major disagreement with the actual data that was obtained. During 
the course of these calculations, no cases were encountered where the 
assumptions were shown to be invalid. 

Assumptions used and subsequent calculations do imply, however, that a 
considerable quantity of inorganic material went with the froth 
solids. Flotation was carried out at a pH of 11, where even magnesium 
would form a solid hydroxide: consequently, the assumption and 
resulting material balance calculation may not be too far from what 
actually happened. Hydroxides are known to gather organics from 
solution and it is postulated that this is what occurred. 

The actual distribution of solids between all the products from the 
test is unknown since no accurate determination of the percent solids 
was made at the time of analysis of the demonstration run samples by 
Arthur D. Little. If the real distribution is considerably different 
than that developed using the assumption then there may be some impact 
upon the oper=i'’ing costs of the process. 

Overall, the adjustments made to the data do not detract from the 
results and conclusion of the demonstration run. The washed soil was 
shown to meet the criteria of EPA's TCLP test. The material balance 
and flowsheet developed using these data are reasonable and no major 
changes will occur even if some changes in analytical or mass 
distribution were made. This is due to the fact that all of the 
assumptions and calculations were reasonable and conservative. 


- 32 - 


4.5 Process Calculations and Flowsheet Analysis 

The analysis of the compounds of concern indicated that some process 
simplifications could be made from those tested in the demonstration run 
and would not effect the final results. These changes reduced the capital 
and operating costs (including the cost of ancillary functions such as 
organic distillation and wastewater treatment) for a full-scale treatment 
system. 

4.5.1 Acid (Counter-Current Decantation) Wash Section 
(Inorganic Contaminant Removal) 

Material balance calculations indicated that the majority of the 
inorganic contaminants were eliminated in the flotation section and 
any additional elimination of heavy metals accomplished by acid 
washing was insignificant, for example, only 1.9% additional arsenic 
was eliminated by acid washing. Flowsheet/material balance studies 
indicated that this same reduction could be achieved by a single 
filtration step of the tail slurry with adequate water wash on the 
filter. This change reduced the number of equipment items as well as 
reduced the volume of wastewater that eventually had to be treated. 
Therefore the acid, counter-current decantation section was 
eliminated. 

4.5.2 Organic Wash Section 

The laboratory development program had not defined either the minimum 
number of stages or the organic to slurry ratio required in the soil 
washing process. The analytical results from the demonstration run of 
the contaminant organics in the organic wash operation produced data 
that defined this area of the process. 

Using the unadjusted data for the pesticides it can be seen that the 
distribution coefficient of the pesticides between the TKO organic 
phase and the aqueous slurry is very large. For example, for the 
first step there was 200 ml of TKO with a concentration of 3100 ug/ml 
aldrin, which accounts for all the aldrin in the feed (620,000 ug in 
TKO vs, 570,000 in the feed). This suggests that aldrin may be 
completely absorbed into the TKO mixture. The other pesticides show 








similar results. Therefore, the removal of pesticides, at least 
theoretically, can be accomplished in a single stage if the organic 
phase can be completely separated from the aqueous slurry provided the 
solubility of the pesticides in the TKO mixture is not exceeded. 

Since the separation of the organic phase from the aqueous slurry will 
not be complete due to the solubility of the TKO and very fine 
droplets in the slurry, three stages of counter-current organic wash 
have been provided. To achieve the maximum organic removal, 
coalescing type oil/water separators would be employed. These units 
typically reduce the level of entrained organics to 10 mg/1; which for 
the flows in this process amounts to a 99.9% removal per stage. 

No data was obtaineo from the laboratory tests or demonstration run to 
determine the minimum organic to slurry flow ratio. Solubility of the 
feed organics in the organic solvent was at least 3100 ug/ml for 
aldrin, as determined in the demonstration run. However, thiu did not 
appear to be the maximum based upon published data of solubilities in 
organic solvents. Therefore, a value of 15,000 ug/ml was used as the 
solubility of the feed organics in the TKO organic solvent to set the 
organic (TKO) to aqueous slurry flow ratio at 0.023. 

One other point about the organic wash section that should be 
discussed is the fate of the organic contaminants other than 
pesticides. The TKO solvent loaded with pesticides and other organic 
contaminants is to be distilled to recover the TKO. Analysis of the 
distillation unit operation by Arthur 0. Little personnel pointed out 
the fact that the majority of the organic contaminants, other than the 
pesticides, would report in the returned organic solvent. The 
demonstration run data shows that the distribution coefficient between 
the TKO solvent and the aqueous slurry is low for these compounds, so 
that they would be washed out of the TKO solvent into the aqueous 
phase and would have to be removed by the following processing steps. 


- 34 - 






4.5.3 Non-Pesticide Organic Contaminant Removal 

The developed flowsheet, based upon the preceding information, 
required that all of the dithiane, sulfoxide, sulfone, and OMMP would 
have to be removed either in the flotation area or by other means. 

The adjip'^ted Hata presented in Table 9 suggests that about two thirds 
of these other organic contaminants would be removed by flotation: the 
balance remain in solution. Therefore, an activated carbon adsorption 
system was added to the process to treat a bleed stream of water to 
eliminate the balance of these other organic contaminants. The loaded 
carbon would be disposed of with the flotation froth solids and 
distillation bottoms. 

4.5.4 Heat Balance 

Data from the laboratory development program indicated that heat was 
not required during solvent washing and it appeared that heat was not 
an important variable during flotation. However, no studies were done 
to establish the effect of heat in the reactor prior to flotation. In 
addition, heat was used in every step in the demonstration run. A 
compromise was used to estimate the heat required for the soil washing 
plant. It was assumed that a temperature of 180°F would be required 
in the pre-flotation reactor only. 

Therefore, in the process flowsheet provisions were included to heat 
the pre-flotation reactor to 130°F and to recover heat from the slurry 
exiting the tank in a single pass heat exchanger to heat the incoming 
slurry. In addition, heating panels are incorporated in the reactor 
to add the additional heat. Overall, the heat balance calculation 
showed that 30 x 10^ BTU's per hour would be required during very cold 
periods. This heat load allows for heat losses, boiler efficiency and 
will be used throughout the year to calculate the operating costs. 

The flotation feed slurry will be maintained at 78°F. 


- 35 - 







4.6 Summary of Demonstration Run 

Overall, the demonstration run showed that soil washing of Basin F material 
can eliminate the contaminants, both organic and inorganic and yield a 
final clean soil that passes or exceeds the proposed TCLP criteria set by 
the EPA. 

During the demonstration run no problems were encountered that were 
insurmountable or would make this a difficult process to implement on a 
large scale. The required equipment is currently manufactured so no new 
equipment design or development is required. Reagents used are all 
available in large quantities. 

Although some data was not obtained during the demonstration run and some 
problems with the calculated material balances were observed, these were 
resolved by the described assumptions and adjusting the mass flow and 
analysis. These adjustments were necessary so that material balances could 
be developed and equipment sized, but in no way detracts from the 
conclusion that this process will clean up Basin F material. 

Analysis of the data, from the demonstration run, showed where some process 
simplifications could be made. These changes were incorporated into the 
process flowsheet presented in the following section. 


- 36 - 


5. BASIN F SOIL WASHING PROCESS 


From the information obtained during the laboratory program, a soil washing 
proces-s was developed. This process was further refined based on the 
analytical results and flowsheet analysis using the demonstration run data. 

5.1 Intrcduction 

Soil washing of Basin F contaminated material was studied in the laboratory 
with the emphasis on pesticide removal. It was initially assumed that: 

1) the other organic contaminants would follow the pesticides; and 2 ) the 
inorganics would have to oe eliminated by an acid wash of the organic free 
soil. The data from the demonstration run showed both of these 
pre-conceived ideas to be incorrect. The other organic contaminants could 
not be eliminated along with the pesticides: therefore an activated carbon 
adsorption unit was added to the process for the elimination of these other 
organic contaminants. The inorganics, principally the heavy metals were 
found to be concentrated and removed with the froth solids, probably as 
metal hydroxides. Since the anions and the cations such as chloride and 
sodium can not be eliminated by this method, a water bleed stream will be 
needed to control these contaminants. 

With all these factors considered, a process flowsheet was developed along 
with a material balance for soil, water, pesticides, other organic, and 
inorganic contaminants. 

The generalized process flow diagram is illustrated m Figure 3. This 
diagram shows the individual operational process areas and how they are 
interconnected by the material flows, the inputs (feed, reagents.water, 
etc.; and outputs of the process. The process has five output streams 
containing various contaminants that currently are anticipated to be 
disposed of by incineration. One aqueous output, free of organics, must be 
treated to eliminate the dissolved salts. It is anticipated that a portion 
of this aqueous output stream can be used, as required, as process water in 
the incinerator and the balance evaporated with the recovered water being 
returned to the soil washing plant. 


- 37 - 






xjurce! wifi ffe-TEdial , hiC. 















Table 10 summarizes the material balarce for the various constituents for 
the generalized flow diagram (Figure 3). 

The generalized flowsheet and material balance resulted from a more 
detailed flowsheet which was completed to size the various pieces of 
equipment. While these details are not pertinent to the understanding of 
this reoort. the detailed flowsheet and material balance are included in 
Appendix A. 

5.? Process Description 

The following is a brief discussion of what is to be accomplished in each 
process areas, shown m the generalized flowsheet, and how it is to be 
accomplished, and with what equipment. 

5.2.1 Feed Preparati o n Area 

In this area the feed is received by dump trucks at a rate of 
approximately 20 tons every 30 minutes and dumped onto a 3" opening 
fixed bar grizzly to remove large rock to protect the log washer 
downstream. The sticky material is washed through the grizzly using 
return process water. Material passing through the grizzly drops into 
a log washer to break up the material. The log washer levels out the 
feed surges. The pulp discharged from the log washer is passed over a 
screen to remove the coarse material. Screen and grizzle oversized 
material is crushed m a jaw crusher that will accept 6" rocks. The 
crushed material is returned to the feed end of the log washer. 

Screen undersized material goes to a large holding tank where it Is 
adjusted to the correct slurry density in preparation for the organic 
wash section, ’he combined holding capacity of the log washer and 
feed surge tank is about 34 tons of solids or a little over 2 hours 
operating time. 

Because of the nature of the material, sticky and plastic. It was 
deemed necessary to store slurry r.itner than excavated feed material. 


- 39 - 



SS33IHd ONIlISm 1IOS i PUSVH MU IMV WH NIHllVW WHWO 




Sources PITA Remedial Resources 


Although no coarse material (+ 1/4") was seen in the Basin F material 
sample received, MTARRI has provided this oversize protection and size 
reduction as an insurance against large material being present. The 
downstream process, especially the flotation section will operate 
better on a sized feed. 

5.2.2 Organic Wash Area 

The feed slurry at 20% solids is pumped to the first mix tank in the 
organic wash area at 596 gpm where it is mixed with 12,7 gpm of TKO 
(organic solvent) moving counter-current to the slurry from the second 
stage of organic wash. The organic/aqueous slurry mix is then pumped 
to a settling tank to allow the majority of the solids to settle out. 
From this tank the top portion of the slurry consisting of water, TKO 
and fine solids is pumped at 300 gpm through an oil/water coalescing 
separator. Leaving the separator are two streams: 1) the pesticide 
bearing TKO solvent; and 2) the aqueous slurry, which contains about 
10 mg/1 TKO. The aqueous slurry is combined with the unde'‘f1ow solids 
being pumped from the settling tank and becomes the feed for the 
second organic wash. The organic phase containing the pesticides is 
pumped to the organic filtration area. 

The second organic wash tank receives the combined aqueous slurry from 
the first wash stage and TKO solvent from the third organic wash stage 
and is processed as in the first stage of organic wash. 

Third and last organic wasJi stage r-coives the cembinsd aqueous slurry 
from the second wash step and TKO solvent which has had the pesticides 
removed by distillation (plus make-up). This step operates the same 
as the first two. The TKO is advanced to the second stage of organic 
wash and the aqueous phase slurry is sent to the flotation section for 
additional cleanup. 

5.2.3 Orqanic Filtration 

From the first step of organic wash the pesticide containing TKO 
organic solvent, which contains some entrapped solids, is filtered 
with a recessed plate and frame f;Iter to eliminate these solids. 


- 41 





This is necessary to prevent problems in the organic distillation 
unit. The TKO is then sent to distillation while the solids removed 
from the press would be and comingled with other contaminated streams 
from the soil washing plant and incinerated. 

5.2.4 Organic Distillation 

Solid free TKO organic solvent is distilled to recover the majority of 
the TKO organic solvent and to concentrate the pesticide in a 
distillation column bottoms stream. The pesticide free organic stream 
is returned to the soil washing plant where fresh organic reagents are 
added to make up for distillation losses. This TKO organic solvent is 
used in the third organic wash stage. The bottoms consisting of 
pesticides, tars, and kerosene (about 13,000 Ib/day) is sent to the 
incinerator for destruction. 

5.2.5 Flotation Area 

The pesticide free slurry from the organic wash area is heated and 
sent to a mix tank reactor where reagents are added to free additional 
organic contaminants to be recovered by flotation. In this reactor, 
sodium silicate, caustic, and a surfactant are added and held for 30 
minutes at ISO^F, with high agitation. 

The reacted slurry is pumped through a heat exchanger to recover heat 
and sent to the flotation cells. In these cells air is blown th’-ough 
the pulp and the hydrophobic material (organics) is collected in a 
froth which floats to the top and is mechanically removed. The bulk 
of the slurry (tails) passes through the cells and is now free of most 
of the organic and inorganic contaminants. 

5.2.6 Froth Liquid/Solid Separation 

Froth from the flotation section contains about 3% solids so water is 

* 

recovered and returned to the process. Also water removal reduces the 
heat load in the incinerator. Water removal is accomplished by adding 
a non-ionic polyacrylamide flocculant reagents to increase the 
settling and filtering rate of the solids. Flocculated slurry is 
settled in a high efficiency thickener; the overflow water being 


returned to the process. The underflow solids still contain a lot of 
water (± 80%) so this stream is filtered on a small belt press 
filter. The filtrate water is returned to the wash process and the 
solid cake (50% solids) sent to incineration. 

5.2.7 Clean Soil (Tails) Liquid/Solid Separation 

The slurry containing the clean soil (tails) must also be separated to 
recover water and produce a solid cake with no apparent free 
moisture. Flocculant was added to the slurry which aided in settling 
the solids in the thickener, and the thickener underflow was 
filtered. The thickener overflow and filtrate water are recycled back 
into the process. The clean soil filter cake is washed with fresh 
water to eliminate the final contaminants remaining dissolved in 
solution in the cake. Finally, the clean soil, containing about 65% 
solids is placed in a fill on-s’te. 

5.2.8 Carbon Adsorption 

Several of the organic contaminants are not completely removed by the 
preceding process steps. Therefore, these remaining organic 
contaminants are eliminated by activated carbon adsorption of a bleed 
stream of water from the plant, A two stage fully automated counter 
flow carbon adsorption system is proposed to accomplish this final 
removal. The water leaving this unit will be free of organics and is 
sent to a wastewater treatment system because of the inorganic salts 
still remaining in it. The carbon, when fully loaded, is sent to 
incineration along with the other contaminated streams from the 
washing plant. 

5.2.9 Wastewater Treatment 

Arthur D. Little is developing the wastewater treatment process. At 
present, about half of the water in the bleed stream will be treated 
to eliminate dissolved salts and returned to the soil washing plant as 
fresh water with the balance of the bleed stream water being used in 
the incineration unit. 


- 43 - 


5.2.10 Volatile Organic Control 

To control emissions of volatile organics from the plant,' several 
designs were incorporated in the process flowsheet to reduce the 
amount of air to be scrubbed. Where possible, process equipment will 
be sealed so no volatile organic will escape. Emission from equipment 
that cannot be sealed will be enclosed in a building which will be air 
swept. 

Areas where v-'latile organic control will be required are principally 
in the truck unloading, screening, and filter presses. Truck 
unloading and screening operations will be in a building with air 
sweep. The organic filter press and the froth belt press will be 
housed in another enclosure with an air sweep. The flotation cell 
will need to be covered with a hood. It is reported that the 
flotation cells will leak at 0.1 SCFM per barrel of material 
processed, or in this case about 2.4 SCFM. 

Overall, the volatile organic control would be small, about 100 SCFM. 
This assumes 5 air exchanges per hour of two buildings having a total 
volume of 10.000 cu. ft. plus that from the flotation cell, 70 SCFM. 

5.3 Summary of Basin F Soil Washing Process 

Using the data collected and numerous flowsheet/material balance studies, a 
processing plant was designed that will produce clean soil (as defined by 
the era's TCLP procedure) that can be returned to a fill on-site. This 
plant would employ equipment currently available and reagents that are 
readily available in large quantities. 

The largest flow stream in the plant is about 800 gpm (slurry to the 
organic wash area) and the largest piece of equipment, other than tanks, 
are the four flotation cells at 1500 cu. ft. each. 

t 

Overall, a full-scale soil washing plant would be easy to operate, require 
a minimum of maintenance, and would have an above average on-line factor. 


- 44 - 







Instrumentation and control loops would be minimal, 
would be tank levels. 

The pl«nt would be relatively safe to operate since 
or high temperatures are employed. The plant would 
acceptable since it is temporary and all emissions, 
would comply with current emission standards. 


The major control 

neither high pressure 
be environmentally 
air, water, and soil 


- 45 - 


6. RECOMMENDATIONS FOR FUTURE WORK 


If in the final evaluation of innovative technology to clean up Basin F, soil 
washing continues to be a viable technology both from an environmental and cost 
standpoint, additional work is needed to finalize the process, engineer the 
plant and finalize the costs for the overall project. This additional work 
would be in three steps: laboratory studies, pilot plant demonstration, and 
engineering design. 

6.1 Additional Laboratory Studies 

These studies would consist of two parts. First, the process would be 
defined in detail. For example, can toluene be eliminated from the wash 
solvent, and is there a better solvent system that would make the 
distillation system more effective in eliminating the organic 
contaminants. Second, data for engineering design needs to be gathered to 
more accurately size the equipment. Such items needed are size 
distribution of the feed material to a detailed analysis of flotation 
variables for scale-up design. 

This program could be completed within three to six months. The 
controlling factor for completing this program will be analytical data 
requirements. Analytical requirements will also be the major cost to 
complete the work. 

6 .2 Pilot/Demcnstration Testing 

It would not be prudent to scale up the proposed process from laboratory 
bench-scale studies to the full-scale plant (950 tons per day) even with 
additional laboratory data. Therefore, a pilot/demonstration plant should 
be built and operated for two to four months. This small scale plant (1000 
Ib/hr) would be built based upon additional detailed laboratory work which 
would fix the flowsheet so little or no equipment arrangement testing will 
te needed. Th’erefore, this would be more a demonstration plant with only 
limited testing on the effect of process water recirculation, distillation 
and quality of the clean soil produced. All data needed for scaling up to 
a full-scale plant will be obtained by a months run at steady state 
conditions. 









6.3 Engineering Optimization 

During the preceding two steps, the work should be subjected to engineering 
optimization as the data becomes available. This would reguire 
establishing an engineering team to assist in program design prior to the 
start of either phase of work. During the additional data collection the 
engineers could evaluate data and make recommendations for changes, new 
tests, additional data so that upon completion of the pilot/demonstration 
run there would be sufficient and complete data for the final and detailed 
engineering of the full-scale soil washing process plant. 


- 47 - 



/ 




APPENDIX A 

• Soil Wash Plant Flowsheet for Basin F Material 
• Material Balance Basin F Soil Wash Plant 


























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