United States
                     Environmental Protection
                     Agency
Industrial Environmental
Research Laboratory
Cincinnati OH 45268
                     Research and Development
EPA-600/S2-84-091 July 1984
&ER&          Project  Summary
                    Testing  and  Evaluation  of  an
                    Alcohol  Production  Facility
                    Utilizing  Potatoes  as  a  Feedstock

                    William Kuby, Steve Nackord, and Walter Wyss
                       This study presents the sampling and
                     analysis results for the characterization
                     of the liquid effluents and solid residuals
                     from a process in which culled potatoes
                     are used as a feedstock for the produc-
                     tion of ethanol fuel. Gaseous emissions
                     were not studied. The facility, located in
                     eastern  Idaho, produces approximately
                     1 million gallons of ethanol  per year.
                     The effluents were sampled in Decem-
                     ber 1981.
                       Liquid and solid samples were taken
                     from sluice/flume water,  chopper
                     product, makeup water, cooker product,
                     fermenter product, beer tank, stillage,
                     interim  and final product, washwater,
                     fusel oil, acid bath and Sparkle* bath.
                     The  effluents  from the plant were
                     analyzed for ethanol and sugar content,
                     conventional parameters, metals, cya-
                     nide, phenols, nutrients, oil and grease,
                     priority  pollutant organics and selected
                     pesticides. The effluents from this plant
                     in general showed the following signifi-
                     cant characteristics: oxygen demand
                     (TOC, COD, BOD),  solids (TSS, TS,
                     specific conductance), nutrients (nitro-
                     gen and phosphorus) and metals (Al,
                     Cd, Ca, Cr, Fe, Mg. Mn, Hg, Ti, and Zn).
                       This Project Summary was developed
                     by EPA's Industrial Environmental
                     Research Laboratory, Cincinnati, OH,
                     to announce key findings of the research
                     project  that is  fully documented in a
                     separate report of the same title (see
                     Project  Report ordering information at
                     back).
                     •Mention of trade names or commercial products
                     does not constitute endorsement or recommenda-
                     tion for use.
Introduction
  The U.S.  Environmental  Protection
Agency (EPA) conducted a study of the
fuel alcohol industry to determine the
environmental impact of alcohol produc-
tion from grain and waste products. As
part of this study, the Industrial Environ-
mental  Research Laboratory in  Cincin-
nati, Ohio  (lERL-Ci) and the Effluent
Guidelines  Division (EGO)  conducted
sampling and analyses to characterize
the air, water, and solid waste streams
from alcohol facilities and to obtain treat-
ability information.
  Since many of the newer facilities
incorporate feedstocks such as sugar
beets, culled potatoes and fruit, and
sweet sorghum, rather than the grain and
waste products  feedstocks analyzed in
the past, EPA has begun to evaluate the
environmental impacts of these nongrain
feedstock facilities. This report describes
the results  of sampling  and analyses of
the liquid effluents  and solid residuals
from an ethanol facility utilizing one of
these feedstocks - potatoes. The full
report  includes a  description  of the
process at  the  potato  facility and the
environmental impact associated with
the effluents, presents the  techniques
used to acquire the samples for analysis,
outlines the analytical  techniques em-
ployed, and presents the  results. An
appendix contains the quality assurance
and quality control (QA/QC) results.

Process Description
  The alcohol productions facility converts
potatoes and grains  into ethanol. During
the sampling period of December 2, 3,

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and 4, 1981, potatoes were used as the
feedstock. Figures 1 and  2 are  flow
diagrams of the process.

Sampling and Analyses
  The purpose of the sampling was to
characterize solid and liquid discharges
and potential discharge streams through-
out the  process.  Table 1 indicates the
analytical sample matrix and the following
paragraphs discuss the sampling points
and techniques used during the December
1981 sampling period.

Sluice/Flume Water Sample
  The flume  water was sampled at
sampling point 15  as potatoes were
transferred to  the chopper tank. Four 1 -
liter grab samples were taken and
composited. The water  was sampled
twice as it came off the conveyer belt and
twice from the agitated catch basin below
the conveyor. The flume water, which is
reused through three batches, was to be
discharged after the next batch.

Chopper Product
  The chopped potatoes are transferred
as a batch to  a cooker tank. The valve
located at the bottom of the batch tank,
sampling point 1, was used for sampling.

Makeup Water
  The site used an onsite water well. The
tap located closest to the well pump (near
the batch  tank) was sampled  after
allowing the water to run for 10 minutes.
This is sampling point 2.

Cooker Product
  Four 1-liter samples of the  cooker
product were taken at sampling point 3,
one at the beginning, two in the middle,
and one near the end of the cycle.

Fermenter Product
  The fermenter product was sampled at
the sampling port  on  the side of the
fermenter tank at sampling point 4. The
sample was composited as the batch was
being pumped to  the  beer  tank. Two
composite fermenter product samples
were taken  simultaneously. The first set
(4C) was maintained on ice during and
after sampling. The second set (4W) was
maintained  at ambient temperatures for
36 hours in an attempt to approximate the
beer tank  effluent. The  samples are
                                                                          referred as "cold" and "warm," respec-
                                                                          tively, in this  report. This sampling
                                                                          protocol was  necessary due to the
                                                                          inaccessibility of the  actual beer  tank
                                                                          effluent (beer still feed) stream. Chemical
                                                                          analysis  in the  laboratory revealed few
                                                                          differences between  the "cold" and
                                                                          "warm" fermenter product samples.

                                                                          Beer Tank
                                                                           The beer tank effluent sampling was
                                                                          minimal due to difficulties in reaching the
                                                                          effluent. Two 500-ml grab samples were
                                                                          taken 16 hours apart at sampling point 5.

                                                                          Stillage
                                                                           The three stillage (beer still bottoms)
                                                                          streams were sampled at sampling points
                                                                          6 and 7. The excess stillage, or stillage
                                                                          overflow, (material which the solid-liquid
                                                                          separator [SOMAT] could not process)
                                                                          was sampled by compositing hourly for
                                                                          10  hours.  The  solid  material or thick
                                                                          stillage stream was sampled hourly for 10
                                                                          hours at the SOMAT  outlet. Also, one
                                                                          grab sample of  the thin stillage stream
                                                                          was taken. This  was sampled at the pipe
                                                                          where the SOMAT discharged the liquid
                                                                          to the main waste stream.
Well water   2
                            \ Optional i  .,,  ,      ,   ,_.     ,22
                            ' feedstock \  AIPha-3maylase (Diazyme) o"
                            !  grain   '  Gluco-amaylase (Taka-Therm)
                                                        A'"
                                                       YY
                                                                                          n.
  I Caustic \
 .t  T . J	
Caustic I Water \
 mix
 tank
                                                                                                     Acid. Epsom
                                                                                                       salt, lime
                                                                                                       Cooker
                                                                                                      discharge
                                                                                                       pump
                                  Drain
      O Indicate sample collection points
Figure 1.  Feedstock processing schematic.

                                  2

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                             Beer feed
    Steam
 Thick  O
stillage
                                                                          Condenser
r                                                                        Benzene   ' '
                                                                        storage  f~^  I
                                                                      Benzene pump   \
                                                                       »*ne batch cleaning by taking two 400-ml
grab samples three  times during each
dump. The sample was taken at the drain
pipe sampling point 11. The three sets
were composited, sealed, and placed on
ice.

Fermenter Washout
  The fermenter washout cycle for the
fermenter tank is identical to the cooker
washout cycle. The sampling and compo-
siting methods were the same as those
for the cooker washout sample. Samples
were taken at point 12.

Combined Washout
  After delivery to the laboratory, the two
washout cycles were combined. Initially
performed a na lyses were repeated on the
combined  sample with the exception of
the coliform analysis.

Fusel Oil
  A grab sample of the accumulated fusel
oil was taken at sampling point 23 after
the material was mixed for approximately
8  hours. This sample was broken  in
transit and was replaced with  a sample
from a later process run; results, there-
fore, are only  generic rather than test
specific.

Acid Bath
  A 500-ml grab sample of the agitated
acid bath was taken at sampling point 24
sterilization cycle. The sample batch was
to be dumped the following day.

Sparkle Bath
  A 500-ml grab sample of the agitated
Sparkle bath was taken at sampling point
25 during the sterilization cycle. The
sampled batch  was dumped after a few
days.

Combined Bath
  After delivery to the laboratory; the two
bath samples  were combined. Subse-
quently, all initial analytical tests per-
formed on the  bath  solutions were
repeated on the combination sample.

Other Samples
  Other samples were taken at various
points for possible analysis should  the
mainstream analyses have shown poten-

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7a6/e 1.    Analytical Sample Maxtrix
                                                                       Parameter
                                                                          tfl
                                                                          
                                                                *

ID No.
1
2
3
4C
4W
5i
5
5T
6
7
7G
8
9

11
12
13
15
23
24
25
27
30
Stream
Chopper product
Makeup water
Cooker product
Fermenter product (cold)
Fermenter product (warm)
1st beer tank effluent
2nd beer tank effluent
Beer tank tops
Excess stillage
Thick stillage
Thin stillage
Distillation product
200-proof dehydration
product
Washout cooker
Washout fermenter
Washout combination
Sluice water
Fusel oil
Acid bath
Sparkle bath
Bath combination
Field/lab blank
m
8
03
X
X
X
X
X
X
X

X
X
X



X
X
X
X

X
X
X
X
§
X
X
X
X
X



X
X
X





X
X



X
X
o
X
X
X
X
X



X
X
X





X




X
X
to
£5

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X
X
X

X

X

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X
X



X
X
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X
X
X
X
X
X
X
X
X
X
X



X
X
X
X

X
X
X
X
4
X
X
X
X
X
X
X
X
X
X
X



X
X
X
X

X
X
X

C S
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X X

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S> £ 6 ^ *
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^ 5 "5 -c x
Q- O O O. Cj

X X X X X






X X X X X





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X X X X X
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— O Q:
«j 
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Table 2.    General Chemical Analysis

    Parameter
                     Method
BODs
COD

TOO
Total suspended solids
Total solids
Phenols (total)
Cyanides (total)
Ammonia
Nitrate
Sulfate
Phosphorus (total)
Specific conductance
Metals*
pH
Total Kjeldahl nitrogen

Oil and grease
Total and fecal coliform
Sugars, reducing
5-day incubation, sample analyzed for oxygen depletion
Acid dichromate reflux, back titrate with ferrous ammoni-
um sulfate
Conversion to COz, infrared quantitation
Gravimetric,  W5°C, weigh residue on filters
Gravimetric,  105°C, weight of residue
Distill, aminoantipyrine color, CHCIs extraction
Distill, barbituric acid colorimetry
Distill, followed by nesslerization
Brucine colorimetric
Turbid/metric
Nitric/suHuric acid digest, ascorbic acid colorimetry
Wheatstone bridge conductivity
Atomic adsorption spectrophotometry following acid di-
  gestion. Analysis by cold-vapor flame/ess AA (Hg), flame
  and graphite furnace analyses as appropriate for others
Electrometric
SuHuric acid mercuric oxide digestion, distillation, ness-
  lerization
Partition/gravimetric, freon extraction
Multiple tube fermentation (gas producers)
Condense with orthotoluidine in acetic acid followed by
  spectrophotometry on liquid portion of samples
"Metals: At, Sb, As, Ba, Be, Bi, Ca. Cd, Cr. Cu. Fe. Pb, Mg, Mn, Hg, Ni, Se. Ag. Tl. Ti, and In.
on  the relation  of  their acidity  to  the
buffering  capacity of the receiving
environment. A pH drop of any magnitud ?
could result  in aquatic population shifts
and destruction, corrosion of metallic
systems, and agricultural crop damage.
  The results of the metals analyses
indicate that the wastes have significant
levels of several metals including alumi-
num,  cadmium, calcium,  chromium,
copper,  iron, magnesium,  manganese,
mercury, titanium  and  zinc.  Without
further testing  the source of metals
cannot be definitively isolated; however,
most can be attributed to the materials
added (e.g., Epsom salt) and to leaching
from the process equipment (primarily
stainless steel and aluminum). The levels
of these metals ranged  from  180 to
67,000 //g/liter in the makeup water and
7 to 176,000  /ug/liter in  the excess
stillage.
  No priority pollutant organics were
detected in the samples. One unknown
sulfur compound was detected at 12/ug/L
Table3.    Values for Conventional Parameters (mg/L, Unless Noted Otherwise)
                                                                             Parameter


ID No.
1
2
3
4C
4W
Si
5
5T
6
7
7G
11
12
13
15
24

25

27

30


Stream
Chopper product
Makeup water
Cooker product
Fermenter product (cold)
Fermenter product (warm)
1st beer tank effluent
2nd beer tank effluent
Beer tank tops
Excess stillage
Thick stillage
Thin stillage
Washout cooker
Washout fermenter
Washout combination
Sluice water
Acid bath

Sparkle bath

Bath combination

Field/ lab blank


in
§
QQ
47,000
<2
107,000
102,000
102,000
59,000
54,000
—
20.0OO
25,000"
18,000
17,100
4,200
9,900
1.980
780

2,700

2,200

<2


a
o
0
160,000
<5
209.000
216.000
201.000
—
—
—
59.8OO
74,700"
54.800
—
—
22,000
7,500
—

—

4,600

<5


0
33,000
3.3
57,500
36,000
34,000
— •
—
—
22.000
29,000"
21,000
—
—
7,700
—
—

—

1.600

1.9
I
a
o
—
<5
18.000
35,000
32,000
—
24,800
—
22,000
—
24,700
—
—
3,080
11,200
—

—

880

NA
CJ
o
§
o
o
76% wt
308
18% wt
6.3% wt
6.1% wt
5.8% wt
6.2% wt
10.7%wt
5.5% wt
8.1% wt
54,000
29.100
4,700
10,100
12,200
1,750

5,600

3,100

<10
©
Q)
I
V.
3: 1
Q^ Ql
5.50
7.39
4.97
4.88
4.88
4.58
4.78
5.16
4.74
4.65
4.67
551
2.76
4.45"
6.90
6.64
4.99s
6.14
4.46°
5.43"
4.63"
—
conductivit]
:m @ 25°C
.u \
•C 24,000
460
—
>24,000
—

—

—

<2
|
a
1
—
<2
—
—
—
—
—
—
<20
—
—
9,200
20
—
270
—

—

—

<2
 "Most of the BOD determinations were performed a second time to bring results in a qua/ifiable
 range.
 "Total solids method was 24 hr at 103°-J05°C.
 cFirst pH determinations were performed on 12/5/81,
 "Combinations were measured on 12/9/81.
 'Rechecks were measured on 2/22/81.
 Units are MPN/100ml (most probable no. per 100ml).
 3mg/kg.

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in the flume water. With the exception of
alcohols, no compounds of significance
were detected in the samples, including
in the fusel oil.
  Bacteriological quality  is of concern
from  the flume  water  and washout
waters. Coliform analyses are performed
as  indicated  tests for  possible health-
related organisms such as fecal strepto-
coccus. More test ing would be required to
preclude bacterial sources other than the
feedstock itself.

Conclusions and
Recommendations
  The preliminary results of this sampling
and analysis are consistent with those of
other fuel alcohol plants using a variety of
other  feedstocks. Thus, the problems  to
be addressed and methods of addressing
them may be similar.
  The effluents from this plant contain
the following water quality variables and
pollutants that could degrade receiving
waters:
  • Oxygen demand (TOC, COD, BOD)
  • Solids  (TSS,  TS,  specific conduc-
    tance)
  • Nutrients (nitrogen and phosphorus)
  • Metals  (Al, Cd, Ca, Cr, Cu, Fe, Mg,
    Mn, Hg, Ti and Zn)
  • Bacteria (total and fecal coliform)
  • Corrosivity, low pH
  Although primary concern for environ-
mental  impacts  should be with those
normal discharges from the process, one
must additionally be concerned with the
"dumping"  of poor batches  and the
disposal of the solid materials other than
by byproducts use (i.e., as a feedstock).
  The  low  pH of the  liquid stream
potentially has two effects:
  • adverse effect on crops if used in land
    farming
  • corrosion of process equipment
It would appear that these  streams
should be neutralized to a  pH of 6 to 8 as
early as possible. Since the acidic level is
required  for the fermentation process,
a realistic point for neutralization would
be downstream of the fermentation tank
in the beer tank. The chemical (a buffer
salt) used for neutralization at this point
must  be benign  with respect to the
byproduct use.
William Kuby, Steve Nackord. and Walter Wyss are  with Acurex Corporation,
  Mountain View. CA 94042.
Mary Ann Curran is the EPA Project Officer (see below}.
The complete report, entitled "Testing and Evaluation of an Alcohol Production
  Facility Utilizing Potatoes as a Feedstock," (Order No. PB 84-187 962; Cost:
  $ 10.00, subject to change) will be available only from:
        National Technical Information Service
        5285 Port Royal Road
        Springfield, VA 22161
        Telephone: 703-487-4650
The EPA Project Officer can be contacted at:
        Industrial Environmental Research Laboratory
        U.S. Environmental Protection Agency
        Cincinnati, OH 45268
                                                                                           
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