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5,266,494

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organics, from soils and the like by converting the mate
BENCH SCALE TREATABILITY METHOD FOR rial to a slurry, adding surfactants and/or alkaline
EVALUATION OF SOIL WASHING agents, and concentrating the toxic substance in the
liquid phase preferably with a modi?er in a froth ?ota
FIELD OF THE INVENTION tion cell.
This invention relates to a method and apparatus for Some of the limitations of the currently used pro
cleaning particulate materials such as soils which are cesses are that they are optimized for removing only
contaminated with a variety of contaminants such as one type of contaminant or for cleaning only one type
heavy metals, radioactive compounds and organics, of soil, they are geared to cleaning the larger particles
often in combination, through a combination of leach while concentrating the ?nes in a fraction for later dis
ing, washing, attrition scrubbing, countercurrent ?ow posal, and they often use ?ltration for water removal
size separation and density separation. This invention which is a capital intensive operation with high operat
further relates to the recovery of such contaminates ing costs.
following removal from the soils, for additional pro Once the contaminants have been removed from the
cessing, recycling or disposal. Most particularly this soil or other particulate material they must in turn be
invention relates to a bench scale method of evaluating recovered for further processing, such as mining and/or
soil for contaminants and other conditions in order to smelting in the case of heavy metals, or disposal, for
determine the best approach for washing the soil. example, through mixing with a ?xative material such
BACKGROUND INFORMATION 20 as concrete. The ability to recover contaminants from
Contaminated soil is becoming a more serious envi
the cleaning system is to a large extent dependent upon
ronmental problem every day. The contaminants can the method by which the contaminants were removed
include heavy metals, such as for instance, copper, lead from the soil in the ?rst instance. Mineral extraction in
and mercury; radioactive species such as for example, general and soil washing in particular often require the
radium, uranium and thorium; and organics such as for 25 oxidation of the metals and sometimes the organic frac
example, oils, polychlorinated biphenyls, (PCBs) ?ue tion of the soil for the removal of the metals. Radioac
soot and others. Various techniques have been devel tive metals are also included with heavy metals requir
oped to remove speci?c contaminants from soil. For ing oxidation, since most radioactive materials are also
instance, heavy metals are known to be found predomi heavy metals, such as uranium, thorium or radium.
nantly in the silt, humic or clay fraction of soil. Hence, Some typical oxidants for heavy metal removal in
they can be removed by size separation such as tiltable clude nitric acid, sodium hypochlorite and calcium
tables, concurrent flow in a mineral jig and chemical hypochlorite. However, the use of nitric acid is gener
techniques, such as the use ofleachates. The radioactive ally not practical due to the fact that nitric acid is nonse
compounds when originating as a spill can be removed lective in its action, dissolving the rock matrix as well as
to a large extent by leaching. Since these compounds oxidizing and dissolving the metal of interest, it is ex
are often also present in the finer particles, the most pensive, and results in nitrate-laden waste liquors which
severely contaminated fraction can also be removed by can present environmental hazards unless treated. So
countercurrent flow size separation. Organics can be dium hypochlorite is expensive to use because commer
removed by washing with surfactants, thermal treat cial solutions are supplied as a 15% liquid which in
ment or biological processes. creases the freight costs. Calcium hypochlorite intro
Special problems develop when the different types of duces large amounts of calcium ion into the leachate
contaminants are present in the same soil. Generally, solution when used in quantities sufficient to oxidize the
biological or thermal processes are more effective for metal, and the calcium ions can then precipitate if car
removing organics than washing, in the case of ?ner bonate bleach liquors are used or if the leachate solution
grain soils and clays. However, toxic inorganics such as 45 is left standing in contact with air. This calcium carbon
lead or chromium (+6), if present, tend to deactivate
ate precipitate is dif?cult to handle and can clog pro
biological systems due to their toxicity and aggravate
air pollution problems endemic to thermal destruction cessing equipment. In addition, if common soaps are
used to remove organics, the high calcium ion content
process. In addition, thermal processes may mobilize
contaminants that were otherwise fixed in the treated tends to precipitate some of the soap which requires use
soil. of additional soap.
Radioactive contamination (e.g., uranium, thorium In addition to the above problems, frequently, it is not
radium, etc.) can be removed by soil washing. Soil immediately clear which of the several possible soil
washing provides a means to process soils having multi washing techniques, or combinations thereof, should be
ple contaminants. The washed soil is compatible with used for a soil of particular interest. Even if the precise
subsequent biological or thermal treatment. Inorganic nature of contamination is known (and it may not be)
and radioactive compounds may be separated from the most ef?cient method of removing that contaminant
organics for separate sale or disposal. or contaminants may depend on a host of variables and
Many soil washing processes are presently available. trial-and-error solutions. Attempting to make a determi
Most use mine equipment to provide intimate soil/ex 60 nation of the economics of particular processing meth
tractant contact. US. Pat. No. 4,783,253 discloses a ods and parameters in the ?eld is impractical, and would
process for separating radioactive contaminants from require shifting and replacing relatively large pieces of
soil using a concurrent flow of water to ?oat away equipment, re?tting pumps and piping, etc. until the
lighter uncontaminated particles from heavy contami best soil washing approach is determined for each par
nated particles. The slurry of lighter particles is dewa 65 ticular site. Furthermore, ?eld equipment often requires
tered using a spiral classi?er, centrifuge, ?lter or the large batches of soil to operate effectively, further in
like. US. Pat. No. 4,783,263 is directed to a process for creasing the inef?ciency of determining an optimal
removing toxic or hazardous substances, in particular washing method for the particular soil.
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There is a need therefore for an improved process identifying particle size ranges for the contaminated soil
and apparatus for treating particulate materials, such as by passing at least a portion of the representative con
soil and the like, contaminated with a mixture of wastes taminated soil sample through a series of particle size
such as radioactive materials, organics and heavy met classi?ers; identifying contaminants to be removed from
als. the contaminated soil; identifying an effective soil wash
There is a further need for such a process and appara ing extractant by passing at least a portion of the repre
tus which separates organic and inorganic contaminants sentative contaminated soil sample through a bench
thereby allowing for optimum disposal routes or post scale soil washing process adapted to substantially cor
treatment strategies to be used on the concentrated respond to a full-scale soil washing process for the con
contaminated fractions. I taminated soil, the bench scale soil washing process
10
There is also a need for such a process and apparatus being adapted for removing contaminants from contam
which produces a high solids content ?nes stream. inated soils having particle size ranges corresponding to
There is yet another need for such a process and the ranges identi?ed in the previous step, the bench
apparatus which is not capital intensive, is economical scale soil washing process including washing a known
to operate and can be made portable for on-site treat 5 quantity of the representative soil sample with a ?rst
ment. extractant, then repeating the bench scale soil washing
There is a further need for a system that can effec process using at least one additional extractant (which
tively recover the contaminants once they have been may be a different concentration of the ?rst extractant)
removed from the soil, requiring a minimal amount of and recovering and identifying at least one of the con
equipment, chemicals, and being portable to the job site, taminants from the representative contaminated soil
which further allows for the processing of recovered sample, in order to determine those soil washing condi
contaminants, such as metals, through mining and/or tions favoring extraction of the contaminant from the
smelting operations, and allows for effective leach contaminated soil; and identifying a suitable leachate
resistant ?xation of contaminants which are to be dis treatment process for treating at least one contaminant
posed. 25 removed in the previous step from the representative
There is also a need for a scaled-down soil washing contaminated soil sample.
evaluation system which may be run on relatively small In one preferred embodiment of the invention the
batches of contaminated soil and which quickly and particle size classi?ers comprise a set of screens includ
accurately provides optimal soil washing parameters for ing a ?rst screen and at least one additional screen ar
the particular contaminated particulate matter being ranged in order of decreasing screen size relative to the
evaluated, be it soil, sludge or other solids. direction of passing the representative soil sample
through the screens.
OBJECTS OF THE INVENTION
It is an object of the invention to provide a bench or
BRIEF DESCRIPTION OF THE DRAWINGS
small scale process for treating contaminated soils FIG. 1 is a schematic representation of a typical soil
which contain organic and/or inorganic contaminants washing concept.
and is able to remove such contaminants from a few FIG. 2 is a more detailed schematic representation of
pounds or less of soil sample. a typical soil washing ?owsheet.
It is a further object to provide a process which eval FIG. 3 is a graphical representation of contaminant
uates the distribution of contaminants in the soil ofinter 40 concentration versus particle size distribution for a soil
est, sample evaluated according to a preferred embodiment
It is yet another object of the invention to provide a of the present invention.
process which evaluates the extraction efficiency of a
variety of extractants while modeling the soil washing DETAILED DESCRIPTION OF THE
PREFERRED EMBODIMENTS
process of interest. 45
It is still a further object of the invention to provide a Referring to FIG. 1, a simpli?ed schematic ofa typi
process which evaluates the effectiveness of the various cal soil washing concept is illustrated, in which contam~
leachate treatment steps. inated soil, generally 1, is transported through a soil
It is another object of the invention to provide a washing system, generally 2, which may comprise
process which determines the volumes and probable chemical extraction or physical separation or combina
product recoveries and contaminant concentrations in tions thereof, depending on the contaminant being re
those product streams. moved from the soil. The contaminated concentrates or
It is a further object of the invention to determine the effluent removed from the soil washing system 2 can
amount of extractants, acids, flocculent, and other comprise one or two streams, a radioactive/heavy
chemicals needed for operation of any soil washing metal stream 30 andan organics stream 3b. The radioac
system. tive/heavy metal stream 30 is typically concentrated for
These and other objects and advantages of the pres disposal or processing as recovered metal ore feed. The
ent invention will become more readily apparent as the organics are typically rendered more environmentally
following detailed description of the preferred embodi acceptable either through biotreatment or thermal deg
ments proceeds. radation. The clean soil which is recovered 4 is typi
cally returned to the site.
SUMMARY OF THE INVENTION The process illustrated in FIG. 1 reduces the volume
According to the present invention, a method of of contaminants and therefore the cost of remediating
characterizing contaminated soil in order to determine the contaminated site. The soil washing process is based
an effective treatment approach for removing contami upon commonly available mineral treatment processes
nants from the soil is disclosed. The method comprises for handling larger particles. Several of these soil wash
the steps of obtaining a representative contaminated soil ing processes have been successfully employed in Eu
sample from a site containing the contaminated soil; rope for several years for washing contaminated soils.
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Examples include the clean-ups at HWZ Bodemsaner current ?ow mode. We preferably operate the mineral
ing B.V. where 98% of the PNAs were removed. See jig 18 in a countercurrent ?ow mode. For such counter
Extractive Methods for Soil Decontamination; A Gen current ?ow operation, the jig can be operated with a
eral Survey and Review of Operational Treatment In stroke length of i to 2 inch, a pulse frequency of 300 to
stallations, J. W. Assink Contaminated Soil, First Inter 400 per minute, an up?ow rate of contaminant mobiliz
national TNO Conference on Contaminated Soil, Nov. ing solution of l to 8 liters per minute, an under?ow rate
11-15, 1985, UTRECHT, the Netherlands, p. 655, in of 1 to'3 liters per minute, with one layer of balls 3/16
corporated by reference herein. As another example, at inch in diameter or greater to provide a soil under flow
a clean-up in Hamburg, 90% of the heavy metal and of 80 to 95 percent and soil over the top of 20 to 5
organic contents were removed by simple size classi? percent.
cation. See Sand From Dredge SludgeDevelopment The intermediate sized particles between 5 mm and
of Process for the Mechanical Treatment of Dredged 60 microns in diameter, which are discharged from the
Material, J. Werther, et al., First International TNO bottom of the mineral jig 18, are abraded in an attrition
Conference on Contaminated Soil, Nov. 11-15, 1985 scrubber 220 which dislodges mineral slime or ?nes
UTRECHT, the Netherlands, p. 887, incorporated by from them. Another attrition scrubber 22 may precede
reference herein. the mineral jig 10. The intermediate sized particles and
Referring to FIG. 2, a particular embodiment of a soil the dislodged ?nes discharged from the attrition scrub
washing process is illustrated. This process is described ber 220 through line 24 are rinsed in a second counter
in a copending US. patent application Ser. No. 529,092 current ?ow size separator such as the second mineral
now US. Pat. No. 5,128,068, Jul. 7, 1992, commonly 20 jig 26 operated in the manner discussed above in con
owned by the asignee of the present invention. Initially, nection with jig 18. The countercurrent ?ow in the
the excavated soil 1 is processed to remove large rocks second mineral jig 26 is wash water which ?ows up
and debris. This step is not shown in FIG. 2. The soil is wardly at a velocity again selected to separate the dis
then processed in a mechanical size separator 10 such as lodged ?nes, typically of 60 microns in diameter and
for instance a rotating drum or vibrating screen device smaller. The slurry of ?nes and wash water is dis
to sort and prewash the feed soil with a contaminant charged through line 28.
mobilizing solution, provided through line 12. Large The remaining intermediate sized particles dis
pieces of soil, for instance larger than 5 mm are washed charged from the second mineral jig 26 are processed in
with the contaminant mobilizing solution, rinsed with a density separator such as a cross-current ?ow jig 30 to
water supplied through line 14, checked for residual extract higher density heavy metal solid waste particles.
contaminants, and returned to the site as recovered soil. The mineral jig 30, which is similar to the jigs 18 and 26
The contaminant mobilizing solution (or process is operated in the cross-current ?ow mode with a stroke
stream) used to wash the soil will be dependent upon length of Lto 3/ 16 inch, a pulse frequency of 100400/
the contamination to be removed. For soluble contami min, a water up?ow rate of 1 to 8 liters/min, one to
nants, the solution will contain a leaching agent. Many three layers of balls less than 3/16 inch to provide soil
suitable leaching agents are known and common leach over the top of 80 to 95 percent and a soil under?ow of
ing agents suitable for leaching radioactive compounds 20 to 5 percent. The cross-current ?ow carrying the
include for example potassium carbonate, sodium car intermediate sized soil particles is discharged through a
bonate, acetic acid, sodium hypochloride, and others. line 32 into dewatering apparatus such as, for instance,
Leaching agents for contaminants typically found in 40 a clari?er 34 or a hydroclone. Sludge from the clari?er
contaminated soils and the like are well known. For 34 is pumped by a pump 36 onto a drying pad 38. The
dispersible contaminants, the contaminant mobilizing dried particles recovered from the drying pad are
solution contains a suitable surfactant. Again, suitable checked for cleanliness and returned to the site as addi
surfactants for dispersing contaminants such as oil, tional cleaned soil. Water removed by the clari?er 34 is
grease, polychlorinated biphenyls, etc., are also known. 45 circulated by a pump 40 through a line 42 as the coun
The contaminant mobilizing solution may contain vari tercurrent wash water for the second mineral jig 26, and
ous combinations of leaching agents and surfactants, through line 44 as the cross-current ?ow for the density
again, depending on the contaminants in the soil to be separator jig 30.
cleaned. The two waste slurry streams in the lines 20 and 28
The effluent of soil particles smaller than 5 mm. and from the ?rst and second mineral jigs 18 and 26, respec
contaminant mobilizing solution discharged from the tively, are discharged into precipitation equipment 46 to
mechanical separator 10 through line 16 is then pro which is added a precipitant to precipitate the dissolved
cessed in a countercurrent flow size separator such as metals. A sul?de or other suitable agent can be used to
the mineral jig 18. In the jig 18, additional contaminant precipitate the dissolved metals present in a particular
mobilizing solution supplied through line 13 flows up contaminated soil. These precipitates and ?ne soil parti
wardly countercurrent to the effluent. The ?nes are cles will be highly contaminated with organics and
carried upwardly with theupward ?ow of contaminant heavy metals. A ?occulant, such as for example Nalco
mobilizing solution to form a slurry which is discharged 7182, an anionic polymer that does not interfere with
through a line 20. These ?nes typically include heavy trace metal absorption and co-precipitation, supplied by
metal particles. The velocity of the upward ?ow of 60 the Nalco Chemical Company, Naperville, H1, is added
contaminant containing solution in the mineral jig 18 is to the precipitates and ?nes conveyed from the precipi
set to separate ?nes of a desired size, for example ?nes tation equipment 46 through a line 48 to dewatering
smaller than 60 microns in diameter. The slurry dis apparatus 50 which may include for instance Bardles
charged in the line 20 includes, in addition to the ?nes, Mozley concentrator 52 which separate micron size
contaminant mobilizing solution which contains particles of high speci?c gravity. Simultaneously, ?ne
leached and dispersed metals and organics. particles are washed by the high shear, orbital shaking
Heretofore, mineral jigs such as that disclosed in US. of the table. Fine soil solution which is washed from the
Pat. No. 4,873,253, have only been operated in a con table is passed through high intensity matrix magnetic
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separators which remove micron sized particles coated The essential steps of the process include ?rst identi
with weakly paramagnetic hydroxides containing inor fying the contaminated particle size ranges contained in
ganic contaminants. Solids from the remaining solution the soil sample, followed by identifying an effective
are then separated from the stream by either ?ltration or extractant for use in connection with the contaminants
?occulation settling and pelletizing in apparatus 54. The contained in that sample, followed by identi?cation of
organically contaminated fractions can be further an effective leachate treatment approach for use with
treated biologically, chemically or thermally and re respect to the particular soil and contaminants of the
turned to the site. sample. Each of these three aspects to the process will
Concentrated solids removed by the Bartles-Mozley now be discussed in greater detail.
concentrator 52 can be disposed of or sold as a concen Before engaging in the process of the present inven
trate. The ?ltrate is passed through the line 55 to an tion, it is necessary to ?rst obtain a representative con
activated carbon bed 56 to remove all organics before taminated soil sample from the site of interest which
being sent through line 58 for recycling. The recycled contains contaminated soil for which cleaning is de
solution is discharged in the one of two contaminant sired. In this regard, it may be preferable to obtain a
containing solution makeup tanks 60 and 62 which is not number of samples from various locations at the site in
currently being used to feed the process. Makeup chem order to establish that soil processing parameters and
icals 61 may be supplied and/or recycled to the makeup needs are consistent throughout the site. Every effort
tanks 60 and 62. The contaminated activated carbon in should be made to obtain a soil sample which fairly
the bed 56 can be thermally or chemically treated or represents the characteristics of the contaminated soil
buried. The recycled contaminant mobilizing solution is contained in the site as a whole, in terms of particle size,
analyzed and an active component such as caustic or contaminant contained in the soil, etc.
emulsi?er are made up on a batch basis in the off-line Once a representative contaminated soil sample is
makeup tank 60 or 62. Contaminant mobilizing solution obtained from the site, according to the present inven
from the active one of the tanks 60 and 62 is pumped by tion it is necessary to evaluate that sample to determine
the pump 64 or 66, respectively, through the line 12 to 25 the various particle size ranges making up the sample
the mechanical size separator 10 and through the line 13 and the weight fraction of each range in that sample.
to the ?rst mineral jig 18. Any suitable particle size classifying apparatus may be
Referring again to FIG. 2, excavated feed soil (repre used for this function, although we have found sieves,
sentative contaminated soil sample) is ?rst processed to preferably USA standard testing sieves meeting ASTM
remove large rocks and debris and yield a pre-washed E-ll speci?cations to perform acceptably.
feed soil 3 by processing the feed soil 16 in a rotating The sieves to be used in classifying the particle size
drum or vibrating screen 10 to prewash the feed soil 16 ranges are identi?ed by sieve size for example, Nos. 10,
using extractant 12 and remove larger particles greater 20, 50, 100, 200, and 325. Other sieve sizes may of
than a nominal one-inch in diameter. Large particles, 4, course be used depending on the characteristics of the
generally greater than 48 mesh, which are more likely 35 particular soil sample being tested.
to be uncontaminated, have been washed with a leach Each sieve is ?rst weighed empty and placed on top
solution, rinsed with water and are returned to the site. of a receiver container in order of decreasing size. For
The remaining contaminated soil is then processed in example, in the array of sieves identi?ed above, the No.
one or more attrition scrubbers 22 followed by a min 325 sieve would be on the bottom and the No. 10 sieve
eral jig 18 which provides counter-current contact be would be on the top.
tween soils less than 48 mesh and greater than 44 mi The soil sample to be evaluated is weighed and
crons and the leach solution. The ?nes, generally less placed on top of the uppermost sieve. The soil sample is
than 44 microns, are carried over with the wash solu then sprayed with water until no further ?nes removal
tion which contains leached organics and metals, 20, 28. through the sieve is observed. Next, the top sieve is
The contaminants are precipitated from this stream and 45 removed and the next sieve is sprayed as previously
removed using flocculation, for example by adding until no further ?nes removal is observed. This proce
NaOl-l, and Na2SiO3. The washed soils less than 48 dure is repeated until all of the sieves have been ade
mesh and greater than 44 microns are then abraded in a quately rinsed. The rinsed sieves are then weighed and
second attrition scrubber 22a and rinsed in a second dried in a hood or low temperature oven at about 50 C.
counter-current mineral jig 26, treated for removal of After drying, the dried sieves are again weighed and the
high speci?c gravity metal contaminants in a speci?c weight of dried soil sample contained on each sieve is
gravity separator 30, monitored and returned to the site. determined.
The ?nes and wash water go to the ?occulation and All of the effluent water from the sieving process,
dewatering system 50 for precipitation and removal. that is, water containing solids of smaller particle size
One of the problems associated with remediating a 55 than are held by the smallest mesh sieve, in this case,
contaminated site, regardless of the particular soil wash less than 325 mesh solids, is ?ltered. This is accom
ing technique being used, is how to inexpensively deter plished in known fashion, for example, by weighing the
mine whether or not the particular soil washing process ?lter paper, then weighing the ?lter paper plus the
is both a technically and economically feasible remedia collected wet solids, drying the solids in a hood or low
tion approach. temperature oven, weighing the dry solids and weigh
We have found that it is possible to run a bench scale ing the ?ltrate. Care should be taken that the tempera
or reduced scale process on virtually any soil sample ture of the drying does not drive off the more volatile
using only a few pounds of sample to determine the organic contaminants.
appropriate processing parameters for a full scale soil After all of the dried solids are classi?ed, including
cleaning operation. The bench scale tests can be run in 65 the dried ?ltrate, the solids are examined through analy
a small area, remotely if needed, which makes the in sis for contaminants of interest. In this way, it is possible
vention suitable for use with hazardous or radioactive to determine which contaminants are more heavily
materials which must be- treated with special care. associated with which classi?cation of soil sizes. The
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particular method of evaluating the dry solids for con A known amount of the representative contaminated
taminants of interest is not critical, so long as it is tai soil sample is placed on the largest sieve, which is posi
lored to the particular contaminants of interest and is tioned over a collection container. Preferably, this soil
suitable for analyzing dried solids. Examples of analysis sample is selected from the same sample used to pro
procedures for determining contaminants of interest duce the particle size characteristics in step 1, however,
include, e.g., mass spectrometry, IR spectrometry, gas preferably the soil used in step 1 is not reused in step 2.
chromatography, or any other known analysis method. That is, preferably fresh contaminated soil having the
An example of the type of data generated by this proce same characteristics as the soil used in step 1 is used for
dure is shown in FIG. 3, which illustrates the correla step 2.
tion between particle size ranges and two contaminants The soil sample is sprayed with a known amount of
of interest, mercury and uranium, for one soil sample. an extractant solution while sieving the sample vigor
The second phase of the process of the invention ously. Examples of extractant solutions include, for
involves the identi?cation of an effective extractant for example, leachants, surfactants, water, detergent solu
use in connection with the particular soil of interest. In tions, oxidizing and reducing agents, etc. The type of
this phase of the process, extraction testing is used to extractant used depends upon the contaminants of inter
determine the optimal conditions for removing the con est, which contaminants are identi?ed as set forth in
taminants identi?ed in the ?rst step from the soil or soil step 1. After spraying the uppermost sieve with the
fraction. Speci?cally, extractants testing is preferably known amount of extractant solution, the sieve is then
performed on those size fractions of soil exhibiting lev sprayed with a known amount of rinse water, again,
20 while sieving the sample vigorously. After the sieve is
els of contamination above acceptable levels.
This second step examines the effects of extractant rinsed, it is removed from above the container, dried as
chemistry, extractant concentration, extractant solu
previously described and weighed. The dried product
remaining on the screen is then analyzed for the con
tion-to-soil-weight ratio, and contact time on the ef?
taminant of interest. '
ciency of contaminant removal from the soil. In this
The contents of the receiver container are placed into
regard, once contaminants of interest have been identi
the blender or bench scale attrition mill/scrubber and
?ed, it is possible to determine what extractants or com
processed for a predetermined amount of time, gener
bination of extractants could be used for extracting each ally several minutes.
contaminant. Ideally, the extractants are themselves The next largest sieve is then placed on top of a re
relatively non-toxic, since in most cases they will reen ceiver container, in this case, the 48 mesh sieve. The
ter the site. For metals, the objective is generally to contents of the blender or bench scale scrubber are then
solubilize the metal with the extractant. For organics, poured over the 48 mesh screen which is sprayed with
the goal may also be to solubilize, e.g. with surfactants. a known amount of rinse water while sieving vigor
In either case, the objective is to determine the lowest ously. After the sieve is sufficiently rinsed, it is re
effective concentration of active extractant possible, to 35 moved, dried as previously described and weighed to
minimize the cost of the soil cleaning process. Thus, this determine the amount of dried soil sample contained on
second step may involve running a bench scale soil the screen. This dried product is then analyzed for the
washing process on the same soil using the same extract contaminant of interest.
ant, but in different concentrations to determine the best The contents of the receiver container are once again
economies of the soil washing system. placed into the blender or bench scale scrubber and
This step is carried out using equipment which mim processed for a predetermined amount of time, gener~
ics the soil washing process to be used on the full scale ally several minutes. The next largest sieve, in this case
site. In the description immediately following, the spe the 325 mesh sieve, is then placed on the top of a re
ci?c procedures in this second step have been selected ceiver container and the contents of the blender or
to mimic the soil washing process presented in FIG. 2. 45 bench scale scrubber are poured onto this sieve. The
Of course, any soil washing process could bene?t from effluent running through the screen is collected in the
the invention, and the scope of this invention should in receiver container and placed into a storage container.
no way be construed to be limited to a bench scale soil The contents of this screen are then emptied into a
washing process that mimics the process of FIG. 2. blender or bench scale scrubber along with a known
The equipment used in this step includes sieves such amount of extractant and processed for a predetermined
as those used in the ?rst phase of the process just de amount of time, again, generally several minutes. The
scribed, a balance such as a Fisher Scienti?c XT-3000 contents of the blender or scrubber or then poured once
DR, and a food blender or bench attrition mill. again onto the 325 mesh sieve which is sprayed with a
In initiating the second step, the appropriate sieves to known amount of rinse water while sieving vigorously.
be used are identi?ed once again. As previously de 55 After the sieve has been rinsed, it is removed, dried and
scribed, typical sieve sizes may include but are not lim weighed as previously described and the dried product
ited to numbers 10, 20, 50, 100, 200 and 325. The partic is analyzed for the contaminant of interest.
ular sieves used will, of course, depend upon the actual The above procedure is preferably repeated using at
soil being tested, the results of the wet screen contami least one additional extractant to determine which ex
nant identi?cation described above in step 1 and the tractants extract the greatest amount of contaminant of
process being modeled. Each sieve size should be interest from the particular soil being studied. Also,
chosen to represent a point in the soil washing process different concentrations of the same extractants may be
where a major stream of material is to be removed from used to determine the lowest effective concentration for
the process. Preferably, these points correlate to a range extraction of the contaminants of interest.
of particle sizes identi?ed in the ?rst step as bearing the 65 The third phase of the soil sample bench scale evalua
most signi?cant share of the contaminants of interest. In tion process involves the identi?cation of an effective
this particular embodiment, screens used include 1 inch, leachate treatment approach for the soil of interest.
48 mesh (297 micron) and 325 mesh (44 micron). Removing contaminants from the soil requires that
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these liberated contaminants be treated, either for recy was substantially the same as that illustrated in FIG. 2.
cle or disposal. For example, heavy metal contaminants The results of the soil fraction/contaminant screening
may be removed by ?oculation and ?ltration. Organics process are illustrated in FIG. 3. This information was
may be pyrolized. As used herein, the term leachate used to develop the leachate system. Typical product
treatment refers to all methods whereby contaminants, results for the bench scale tests are shown in Table 1.
after removal from soils and as contained in leach solu Based on the success of the bench scale tests, a pilot test
tions, ?nes and wash solutions, are rendered more envi was carried out with about 50 pounds of soil using an
ronmentally acceptable, e.g., by ?xing, e.g., in a con actual attrition scrubber and a mineral jig. These results
crete matrix, or smelting, in the case of metals, or pyrol are shown in Table 2. There exists as illustrated a very
izing, in the case of organics. 10 good agreement in performance between the two'tests
In this third phase, all wash solution, leachate and shown in Tables 1 and 2.
?nes are tested to de?ne a suitable treatment process.
Referring again to FIG. 3 it is clear that the 250 mi
Various methods for treatment include pH adjustment, cron particle size represented a logical cut point for this
precipitation, ?occulation and/or absorption. Precipita particular soil sample since most of the uranium con
tion methods include hydroxide or sul?de precipitation
or water glass co-precipitation in the case of metal con
tamination occurred in particle sizes less than 250 mi
crons while most of the mercury contamination oc
taminants, and calcium chloride precipitation for or
ganic contaminants. curred in the particle size fractions greater than 250
Flocculation includes chemical or electrolytic ?occu microns.
lation and removal using mechanically aided devices or 20 TABLE 1
settling tanks. Results of Bench Scale Treatability Test
Absorption media include ion exchange resins, zeo Particle Size Residual Soil Contaminant Levels
lites, activated carbon and treated clays, for example. Fraction Treatment Uranium Mercury
The choice of speci?c treatment techniques selected <25O micron Segregation 890 ppm 4500 ppm
depends on the type and level of the contaminants. In 25 by Sieving
this example, it is assumed that the ?nes are contami 250 < < 200 micron Batch Contact 30-45 ppm 90-150 ppm
nated and must be removed and dewatered. This is the with l8g/l
situation facing the typical contaminated soil site. The NaOCl, pH 6
extractant will be assumed to contain the solubilized
contaminant which is a metal and which is removable
on an ion exchange column. The equipment used in this TABLE 2
phase includes a 500 ml. beaker, a 1 inch diameter by 18 Results of Pilot Scale Treatability Test
inch high glass column, a pH meter, a pipette for adding Residual Soil Contaminant Levels
reagents, and a variable speed laboratory stirrer. Product
In this phase of the process, a sample of ?nes slurry 35 Treatment Stream Uranium Mercury
from the above step 2 is obtained and placed in the 500 Attrition scrub a) 250 micron 735 ppm 2000 ppm
ml. beaker. In this example, a 400 ml. sample of fines with ZOg/l b) +250 micron 2050 ppm 100-135 ppm
NaOCl. pH 6
slurry was obtained. The pH of the ?nes slurry was followed by
adjusted to about 6.7 using I-lCl in order to precipitate mineral jig
humic materials. The amount of l-ICl added to achieve 40
the desired pH is recorded. This pH adjusted solution is
then analyzed for the concentration of the contaminant EXAMPLE 2
of interest.
While gently stirring with the laboratory stirrer, floc In this example, soil contaminated with a mixture of
culent solution is then added to the 40 ml. sample until 45 gasoline, diesel oil and lead will be evaluated. The ex
?ocs form and material settles from the solution. The tractant to be used for this example is a commercial
amount of ?oc solution added to obtain this settling is detergent, comprising a solution of NP90 (Henkel Cor
recorded. Additionally, the volume of settled iloc poration, Ambler, Pa. 19002) and Asee 799 (Witco Cor
formed is recorded. The settled slurry is then ?ltered. poration, Houston, Tex. 77245) in water. The detergent
Next, the ?ltrate is carefully poured onto the resin 50 solution is pH adjusted to about 12 with NaOH. A ?rst
bed which has been ?lled with water to the top of the detergent solution will include 1% of both NP90 and
resin, and the resin bed is drained from the bottom until Asee 799. A second detergent will include 0.5% of both
all of the ?ltrate has been processed. NP90 and Asee 799.
The amount of resin required to absorb all of the Use a sample splitter to remove a SOO-gram aliquot of
metal contaminantis estimated. This estimated amount soil. This aliquot is wet-sieved into three fractions,>2
of resin is removed from the top of the column. Next, mm, 50 micron< <2 mm, and <50 micron.
the resin which has been removed from the column is The fractions larger than 2 mm are rinsed with water
stripped with a known volume of regenerating solution and the washed solids assayed for organics and lead.
and the concentration of the contaminant of interest in Next, the 50 micron < <2 mm fraction is contacted
the regenerating solution is measured. The recovery of 60 with the ?rst detergent solution in an attrition scrubber
the contaminant by the regenerating solution compared for about 20 seconds. The solids are then rinsed with
to the amount of contaminant poured into the column water and resieved to the same three size fractions to
from the ?ltrate is the removal ef?ciency for the resin estimate the extent of particle attrition. These solids are
column. then assayed for the presence of organics and lead.
65 Next, the <50 micron ?nes are ?ltered from the
EXAMPLE 1 combined wash (detergent) and rinse solutions col
A soil contaminated with a mixture of mercury and lected from the previous steps. The solutions are treated
uranium was tested. The soil washing process tested with sodium oxalate followed by electrocoagulation,
5,266,494
13 14
both with and without precipitation using CaCl2, and 3. The method of claim 1 wherein said particle size
the effluent is assayed for organics and lead. classifying means comprise a set of screens including a
The above procedures are then repeated using the ?rst screen and at least one additional screen, arranged
second detergent solution. in order of decreasing screen size relative to the direc
During the bench scale treatment process of this tion of passing said representative contaminated soil
example, the following samples are collected for assay sample through said screens.
for contaminants: 4. The method of claim 3 wherein said screens com
1. One sample from each of the three dry sieve sizes prise a range of sizes from No. 10 to No. 325.
(before washing). (Total three samples.) 5. The method of claim 3 wherein a known quantity
2. Two samples from each of the three wet sieve sizes of said representative contaminated soil sample is
for each wash solution used. (Total 12 samples.) placed on said ?rst screen and said ?rst screen is rinsed
3. Three liquid samples, one before and one after treat with water to wash ?nes through said screen until no
ment, without CaClg and with CaClg precipitation for further ?nes removal is observed, and each successive
each leachate. (Total 6 samples.) said screen is rinsed with additional water until no fur
I claim: ther ?nes removal is observed, and step (b) further
15 comprises the steps of:
1. A method of characterizing contaminated soil and
determining an effective treatment approach for remov (a) drying any solids collected on said screens;
ing contaminants from said soil, said method comprising (b) weighing said dried solids;
the steps of: (c) ?ltering all said rinse water to recover said ?nes;
(a) obtaining a representative contaminated soil sam (d) drying said ?nes; and
ple from a site containing said contaminated soil; (e) analyzing said dried solids and ?nes for contami
nants of interest.
(b) (i) identifying particle size ranges from said con 6. The method of claim 1, wherein said bench scale
taminated soil by passing at least a portion of said
representative contaminated soil sample through a soil washing process of step (0) comprises the steps of:
series of particle size classifying means and (ii)
(a) selecting a ?rst particle classifying means capable
of isolating a particle size from said representative
analyzing each size range of particles for contami 25 contaminated soil sample corresponding to a size
nants of interest in order to correlate the levels of identi?ed in step (b);
said contaminants of interest with said size ranges (b) placing said particle classifying means in commu
to determine which of said size ranges has a greater nication with a receiver means;
proportion of said contaminants than other particle (0) placing a known quantity of said representative
size ranges; 30
contaminated soil sample on said ?rst particle clas
(c) utilizing the information with respect to particle sifying means and spraying said sample with a
size ranges and contaminants from step (b)(ii), iden known quantity of extractant solution;
tifying a ?rst extractant to be used to remove said (d) rinsing said sample with a known amount of rinse
contaminants of interest from said contaminated solution comprising water or extractant solution
soil by passing at least a portion of said representa while collecting a mixture of rinse solution and
tive contaminated soil sample containing size ?nes in said receiver means and collecting a ?rst
ranges determined to have a greater proportion of product sample in said ?rst particle classifying
said contaminants through a ?rst bench scale soil means;
washing process adapted to substantially corre (e) drying and weighing said collected ?rst product
spond to a full-scale soil washing process for said sample;
contaminated soil, said ?rst bench scale soil wash (f) analyzing said dried ?rst product sample for a
ing process adapted for removing said contami contaminant of interest;
nants from contaminated soils having particle size (g) processing said mixture of rinse solution and ?nes
ranges corresponding to said ranges determined in to extract at least one contaminant of interest from
step (b)(ii), said ?rst bench scale soil washing pro said ?nes;
cess including washing a known quantity of said (h) passing said ?nes through a second particle classi
representative soil sample with said ?rst extractant, fying means while rinsing said ?nes with a known
analyzing said washed sample for the quantity of quantity of rinse solution and collecting a second
said contaminants of interest remaining on said mixture comprising ?nes and rinse solution, said
washed sample and second particle classifying means classifying a
(d) repeating step (c) with a second bench scale soil smaller size of ?nes than said ?rst particle classify
washing process on at least one additional repre ing means;
sentative contaminated soil sample obtained from (i) collecting a second product sample in said second
said site with a second extractant, comparing the particle classifying means and drying and weighing
quantity of said contaminants remaining on said 55 said second product sample;
washed soil following said second bench scale soil (j) analyzing said dried second product sample for a
contaminant of interest.
washing process with the quantity of said contami 7. The process of claim 1 wherein the treatment pro
nants remaining on said washed soil following said cess of step (d) is performed on contaminant-bearing
?rst bench scale soil washing process in order to media selected from the group wash liquor, leachate,
determine which of said ?rst or second bench scale 60 ?nes and mixtures thereof.
soil washing processes favors extraction of said 8. The process of claim 1 wherein the treatment pro
contaminant from said contaminated soil; and cess of step (d) is selected from the group pH adjust
(e) identifying a suitable leachate treatment process ment, precipitation, flocculation, ?ltration, settling,
for treating contaminants removed in step (c) from absorption and combinations thereof.
said representative contaminated soil sample. 65 9. The process of claim 6 wherein said ?rst and sec
2. The method of claim 1 wherein said contaminants ond particle classifying means comprise screens for
in said contaminated soil comprise heavy metals, radio sieving said representative contaminated soil sample.
active compounds, organics, or a combination thereof. i t 1 1

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