EPA-670/2-74-091
December 1974
Environmental Protection Technology Series
DEVICES FOR ONBOARD TREATMENT OF
WASTES FROM VESSELS
National Environmental Research Center
Office of Research and Development
U.S. Environmental Protection Agency
Cincinnati, Ohio 45268
-------
EPA-670/2-74-091
December 1974
DEVICES FOR ONBOARD TREATMENT OF
WASTES FROM VESSELS
By
Thomas J. O'Grady
Peter E. Lakomski
Thiokol Corporation
Wasatch Division
Brigham City, Utah
Contract No. 68-01-0115
Program Element No. 1BB038
Project Officer
Leo T. McCarthy, Jr.
Industrial Waste Treatment Research Laboratory
Edison, New Jersey 08817
NATIONAL ENVIRONMENTAL RESEARCH CENTER
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
CINCINNATI, OHIO 45268
-------
REVIEW NOTICE
The National Environmental Research Center, Cincinnati, has reviewed this
report and approved its publication. Approval does not signify that the contents
necessarily reflect the views and policies of the U. S. Environmental Protection
Agency, nor does mention of trade names or commercial products constitute
endorsement or recommendation for use.
ii
-------
FOREWORD
Man and his environment must be protected from the
adverse effects of pesticides, radiation, noise, and
other forms of pollution, and the unwise management
of solid waste. Efforts to protect the environment
require a focus that recognizes the interplay between
the components of our physical environment—air,
water, and land.
The National Environmental Research Centers provide
the multidisciplinary focus through programs engaged in
• Studies on the effects of environmental
contaminants on man and biosphere, and
• A search for ways to prevent contamination
and to recycle valuable resources.
The research and development effort described in this
report involved demonstration of a sanitary waste
treatment system which prevented the discharge of
pollutants into the surrounding environment.
A. W. Bretdenbach, Ph.D.
Director
National Environmental
Research Center,
Cincinnati, Ohio
iii
-------
ABSTRACT
A program involving the demonstration of a pleasure craft zero discharge,
physical/chemical waste treatment system employing a unique filter-
incinerator device was conducted. Extensive test data from laboratory and
shipboard demonstration tests of the system are presented. Data on manu-
facture and installation costs for the pleasure craft system are also presented.
The program demonstrated the ability to zero discharge waste and comply
with the 23 Jun 1972 EPA no-discharge standard.
This report was submitted in fulfillment of Contract 68-01-0115, under the
sponsorship of the Environmental Protection Agency.
iv
-------
CONTENTS
Section Page
ABSTRACT iv
List of Figures vi
List of Tables viii
Acknowledgements &
I CONCLUSIONS 1
II RECOMMENDATIONS 2
HI INTRODUCTION 3
IV SYSTEM DEVELOPMENT 7
Program Description 7
Phase I - Laboratory Test Program 8
Design Objectives 8
Filter-Incinerator Development 8
Improved Design 14
Secondary Treatment 25
V SYSTEM DEMONSTRATION 32
Flow-Thru Tests 32
Zero Discharge Tests 39
Preliminary Phase II Design 41
System Design 42
Laboratory Test Phase 46
Field Testing 61
Fuel Oil Tests 72
VI SYSTEM ECONOMICS 77
VII COAST GUARD REVIEW 79
APPENDDC I—Summary of Filter-Incinerator Tests. . 80
APPENDDX II--Identification of Organic Compounds
in a Closed-Loop Hypochlorite
Wastewater Treatment System 89
-------
FIGURES
No. Page
1 Small Pleasure Boat Waste Treatment System 5
2 Houseboat Waste Treatment System Flow Diagram ... 6
3 Filter-Incinerator Design (Packed Bed) 10
4 Flow Diagram and Equipment for Filter-Incinerator
Tests 11
5 Profile of Filter-Incinerator Temperature and Bed
Pressure (Test 2) 15
6 Filter-Incinerator Cylindrical Test Unit for Cloth
Media 16
7 Glass Cloth Test Rig 17
8 Glass Cloth Filter 21
9 Refrasil Filter, Before Test 22
10 Refrasil Filter, After 40 Cycle Test 23
11 Catalyst Calibration Data - Static Reactor (65°-70°F) . . 27
12 Catalyst BOD Reduction, Ambient Temperature,
Static Reactor (WNC-1 Catalyst) 28
13 Effect of WNC-1 Catalyst on BOD and SS Removal .... 30
14 Effect of WNC-1 Catalyst on Cl2 Removal 31
15 Building M-85 Layout, EPA Houseboat 33
16 Houseboat Schematic Diagram 34
17 Prototype Filter-Incinerator Assembly 35
18 Typical Temperature Profile 39
vi
-------
FIGURES (Cont)
No.
19 Zero Discharge Installation Layout 43
20 Catalytic Tank Support 44
21 Incinerator Blower Assembly 47
22 Treatment of 24-1/2 Gal Sewage With a 100 In2
PEPCON Cell at a Nominal of 1 Amp/In2 55
23 Houseboat Waste Treatment System Installed
in Closet 60
24 Thiokol Houseboat 62
25 Thiokol Houseboat Waste Treatment System
Installation 63
26 Houseboat Waste Treatment System Closeup 64
27 Houseboat Waste Treatment System Electrical
Schematic 65
28 Hot Gas Duct and Mounting Flange, Right Three-
Quarter View 73
29 Hot Gas Duct and Mounting Flange, Left Three-
Quarter View 74
30 Fuel Oil Delivery Rate vs Fuel Pump Pressure
for 0.50, 0.60, and 0.65 gph Nozzles 76
VII
-------
TABLES
No.
1 Design Objectives 9
2 Composition of 10 In. Diameter Filter Column 12
3 10 In. Diameter Filter-Incinerator Testing 13
4 Filter Material Evaluation 18
5 Major Flow-Thru System Components 36
6 Summary of System Flow-Thru Testing 37
7 Projected Flow-Thru System Performance 40
8 Zero Discharge Operation Log 50
9 Zero Discharge Analytical Results, Treatment Tank ... 51
10 Zero Discharge Operation Log, Test Configuration III . . 53
11 Zero Discharge Operation Log, Test Configuration IV . . 56
12 Analysis of Treatment Tank Sludge 57
13 Houseboat System Flush Liquid 59
Vlll
-------
ACKNOWLEDGE ME NTS
This program which extended over a period of 30 months was accomplished
with the cooperation of many individuals in the Government and the contractor
organizations.
The support and guidance of the EPA, Edison, New Jersey, Water Quality
Laboratory, specifically Mr. Leo T. McCarthy and Mr. W. Librizzi are
acknowledged with sincere thanks.
Commander Albert Stirling, U.S. Coast Guard, Washington, D.C., provided
valuable assistance in reviewing the system design to establish compliance
with Coast Guard Regulations.
The development, design, and demonstration testing was carried out by a team
from the Thiokol Corporation, Wasatch Division. Key members of the team
were T. J. O'Grady, Program Manager; P. Woolhiser, who served as Project
Engineer during Phase I, and P. E. Lakomski, who served as Project Engineer
for Phase II; L. W. Poulter, S. Moore, and Dr. D. P. Clark, Development
Engineers; W. N. Christensen, Project Chemist; and O. W. Wilson, Biochemi-
cal Analyst.
IX
-------
SECTION I
CONCLUSIONS
1. As a result of the Pleasure Craft Waste Treatment System Development
Program a practical, economical physical-chemical zero discharge waste
treatment system has been demonstrated.
2. Because this system is a zero discharge system it fully complies with the
no-discharge standard adopted by the EPA on 23 Jun 1972 and the Federal
Water Pollution Control Act Amendments of 1972 (PL 92-500).
3. With minor modifications, the pleasure craft waste treatment system will
meet Coast Guard requirements for commercial vessels.
4. The program demonstrated that a device combining two unit operations
(filtration and incineration) will effectively and safely remove and destroy
sewage sludge.
-------
SECTION II
RECOMMENDATIONS
1. Continue system development by modifying the system for a commercial
vessel and conducting a demonstration program aboard such a vessel.
2. Submit the system for certification by the Coast Guard in accordance with
proposed Certification Procedures and Design and Construction Requirements.
3. Increase system utilization by conducting a development program for treat-
ment of other vessel wastes such as galley, bilge, and shower and washwater
waste.
4. Apply the system to the treatment of waste in recreation areas, campgrounds.
etc.
-------
SECTION III
INTRODUCTION
STATEMENT OF PROBLEM
The Coast Guard Registry for Boats under the 1958 Federal Boating Act includes
approximately 500,000 pleasure boats from 16 to 65 ft in length with over half in
the 16 to 26 ft class and most of the remainder in the 26 to 40 ft class. Most of
the 26 to 40 ft class boats are equipped with overnight accommodations for 4 to
10 people, and the number of these boats is increasing yearly. A new and very
popular class of these boats is the cruising houseboat. These vessels normally
operate in choice inland waters requiring strict control of discharge of waste.
One of the national environmental goals is to prevent the discharge of pollutants
into its navigable waters, and this goal was the prime motivation behind the
work conducted under this program.
OBJECTIVES
The objectives of the pleasure craft waste treatment program were:
1. Conduct engineering research as necessary to refine a
proposed treatment process into a system suitable for
recreational vessel conditions.
2. Assemble a prototype system, and laboratory test the
system to provide sufficient laboratory test data to
demonstrate that the system would provide satis-
factory treatment when installed aboard a recre*-
ational vessel.
3. Provide sufficient information to obtain a written
opinion from the Coast Guard that the system will
meet their safety requirements.
4. Install and demonstrate the prototype system onboard
a houseboat.
5. Provide estimated retail costs plus installation and
operating costs of the system.
-------
TECHNICAL APPROACH AND SYSTEM DESCRIPTION
The basic approach proposed and chosen for treatment of sanitary waste aboard
a pleasure craft was physical-chemical in nature. The program, as initially
contracted, involved the development of a flow-thru treatment system to prevent
the discharge of untreated waste. The process selected for development and
demonstration involved the following physical-chemical processes:
1. Filtration of influent waste to remove coarse and
suspended solids.
2. Incineration of the collected coarse and suspended
solid material.
3. Chemical treatment of the collected filtrate to reduce
BOD prior to discharge.
Steps 1 and 2 were accomplished in a single device developed by Thiokol, This
"filter-incinerator" device combined these two unit operations into a compact,
single component.
During the course of the development program, a no-discharge standard was
adopted by the EPA. This standard was adopted on 23 Jun 1972 and resulted in a
redirection of the program to develop a pleasure craft treatment system which
would totally prevent the discharge of waste.
The system finally developed and demonstrated is shown in Figures 1 and 2.
This system was installed on a houseboat and was in continuous use during the
summer boating season of 1973. During that period, the system handled the
waste of over 300 persons. Analysis of the recycle liquid showed a zero coliform
bacteria count. The treated water was acceptable for reuse as flushwater.
Operation of the system is simple. Chlorinated water from the treatment tank is
pumped to the toilet for flushing.
The system uses a standard camper-type low flush toilet. Toilet flushing is con-
trolled by a pushbutton switch to actuate the flushwater pump. The flushwater and
wastes accumulate in an 8 gal holding tank which is integral with the toilet. Gener-
ally, each evening, after a day of operation, the waste from the holding tank is
pumped to the filter-incinerator. During the night, liquid drains through the filter
and enters the treatment tank. In the morning, solids remaining on the filter are
incinerated. High test hypochlorite (HTH) tablets are added to the treatment tank
when the wastes are pumped to the filter-incinerator. The HTH oxidizes a ma-
jority of the wastes in the liquid and sanitizes it for reuse as a flush medium.
-------
Once each week ash and noncombustible solids are vacuumed from the filter-
incinerator for disposal with other trash which accumulates during regular use of
the vessel.
r FILTER
INCINERATOR
FUEL/SPARK
ASSEMBLY
BURNER
CONTROL
CHEMICAL
ADDITIVE PORT
TREATED WATER
HOLDING TANK
FLUSH WATER PUMP
Figure 1. Small Pleasure Boat Waste Treatment System
-------
HUMAN
WASTE
REST ROOM
8 GAL
HOLDING TANK
VENT
FILTER-
INCINERATOR
AIR
GASOLINE
CALCIUM
,HYPOCHLORITE
TREATMENT TANK
SLUDGE PUMP
RETURN PUMP
Figure 2. Houseboat Waste Treatment System Flow Diagram
6
-------
SECTION IV
SYSTEM DEVELOPMENT
PROGRAM DESCRIPTION
The program comprised two distinct phases as follows:
Phase I - Development and Inplant Testing of a Prototype
System
Phase II - Vessel Installation and Demonstration of the
Prototype System
The Phase I program was initiated in July 1971. Original effort centered on
development of a proposed packed bed filter-incinerator as the method for
removal and disposal of suspended solids in the waste stream. The packed bed
filter-incinerator had previously been demonstrated on a laboratory scale basis.
Initial testing with a "scale-up" packed bed filter-incinerator revealed a problem
in the form of excessive incineration time. The time required to raise the temper-
ature of the packed filter bed to a level which would incinerate the collected
sludge was several hours, an unacceptable time for a watercraft system. As a
result, Thiokol requested a 90 day Phase I schedule extension on 22 Oct 1971 to
permit incorporation of an advanced filter-incinerator design into the EPA
program. This advanced filter-incinerator design was the result of Thiokol
company-sponsored research on unique lightweight, low mass, high-temperature-
resistant filter materials.
Program effort was reinitiated in February 1972, using a fabric cartridge filter
element. The program was subsequently redirected on 17 Aug 1972 as a result of
the EPA zero discharge standards which were published in the Federal Register
on 23 Jun 1973. The redirection involved redesign of the system to "close-the-
loop" converting the flow-thru system design to an effluent recycle mode conform-
ing to the zero discharge standard.
The system was revised to investigate the zero discharge concept by adding
PEPCON cells to generate hypochlorite and thus eliminating a majority of the
chemical addition used previously. The subsequent program redirection with
emphasis on a zero discharge system rather than a flow-thru discharge system
resulted in reduced testing of the flow-thru system when the program was resumed.
A 3 week demonstration test of the zero discharge system was conducted as part
of the expanded program.
-------
The Phase II, Vessel Installation and System Demonstration, effort was initiated
on 20 Oct 1973. The program comprised fabrication and laboratory evaluation of
the prototype vessel system, installation and checkout of the system aboard a
Thiokol-provided 35 ft Nautaline houseboat and the conduct of a demonstration
program aboard the houseboat during the summer of 1973. The demonstration
program on the houseboat was conducted at Bear Lake, Utah, over the period
13 Jun 1973 thru 14 Sep 1973. During this period, 1,150 uses of the system was
experienced.
As a result of a Coast Guard review of the system design additional laboratory
tests were conducted on the system filter-incinerator using diesel fuel instead of
gasoline to fire the incinerator. Coast Guard regulations prohibit the use of
gasoline aboard commercial vessels.
PHASE I - LABORATORY TEST PROGRAM
Design Objectives
At the beginning of the Phase I, a set of design objectives was established based
on the EPA requirements contained in the RFP and the design requirements
established by Thiokol in responding to the RFP. Table 1 lists the design objec-
tives on which preliminary system sizing was based. The objectives were based
on a survey of small boat manufacturers and considered the waste producing
capabilities of boats equipped with toilets, washbasins, showers, and galleys as
well as the electrical power availability aboard typical boats. The fuel require-
ments were established subject to Coast Guard approval.
Filter-Incinerator Development
Testing on the program was initiated using an existing Thiokol laboratory filter-
incinerator. This incinerator was a scaled-up version of the basic laboratory
glass column incinerator which had provided the test data included in the Thiokol
proposal for the program. The incinerator was comprised of an internal and
external mild steel shell separated by an insulation barrier with the filter media
assembled inside the inner metal shell as shown schematically on Figure 3.
Figure 4 provides a more detailed schematic of the system test configuration.
Table 2 defines the makeup of the mixed media filter bed which was tested. Bed
dimensions were 10 in, diameter by 16-1/2 in. high. All six of the tests initially
conducted are summarized in Table 3. Heat for incineration was provided by a
high pressure oil burner manufactured by Thermal Research and Engineering
Corporation.
The mixed media filter bed had several operational problems that caused it to be
unsuitable for use on a pleasure craft. The major problems were: (1) extended
-------
TABLE 1
DESIGN OBJECTIVES
EPA
Requirement
Thiokol Goal
Influent Characteristics
Suspended Solids (mg/l)
BOD (mg/l)
PH
System Capability (Hydraulic Load)
Total Capacity (gal /day)
Peak Capacity (gal /day)
Effluent Characteristics
Suspended Solids (mg/l)
BOD (mg/l)
Coliform (mpn)
Physical
Weight
Envelope
Environmental
Maximum Temp (° F)
Minimum Temp (° F)
Electrical Power
Other Power
Not specified
Not specified
Not specified
Not specified
Not specified
90% removal
90% removal
240/100 ml
Not specified
Not specified
Not specified
Not specified
Not specified
Not specified
500
500
6.7 to 8.4
25
33
50
50
100/100 ml
Minimum
Not to exceed 3 x 3 x 5 ft
140
28
12 to 36 vdc, 1 KW max.
Adaptable for use with
110 vac when docked
Use of minimal quantities
of fuel oil, butane, propane,
or alcohol acceptable
-------
HARSHAW 1/8 IN. PELLET
(COATED WNC-1)
EXHAUST
MOLECULAR SIEVE
1/16 x 3/16 IN (COATED) — »
\
«„««.,- ,«v,_~
COATED SK-40 + 1
UNCOATED SK-40+
18-12 MESH, 3/8 IN.
GROUND MOLECULAR SIEVE
COATED SK-40+ ^
GROUND MOLECULAR SIEVES. /
MAI (TfMII AR CIPWPC /
MOLECULAR SIEVES, 1/8 IN. /
EXTRUSIONS (SK-134) //
HARSHAW CO 108T /4.
\
\
\
^
\
\
N
\
^
s/^
>
Oj
x
N
A
^
\
\A
^f
S(
cr
v .
A
\
\ '
T|
/
/
/,
/
/(
/I
' I
I 1
//
V)v
-f-
— \ — ]
U
^ i
V 2
< 3
f 4
r 6
r 7
. A
9
/ 1O
/
V\\\\\V
(l
I
-^
N\^
A
\
V
s
\
^
K
\
V
0
\
\
i
f
^~- 1/4 IN. THICK
GLASROCK
^- STEEL SHEL
—INSULATION
AIR
i
\ / — OIL BUF
-T: - j »/
L »!u
1
HARSHAW CO 502T.
1/4 X 1/4 IN.
COORS POROUS ALUMINA
PLATES
1 INCH THICK FUSED ALUMINUM
OXIDE (PAO) DISC
Figure 3. Filter-Incinerator Design (Packed Bed)
10
-------
1
©
CONC SLUDGE
CENTRATE
LEGEND
1. RAW SEWAGE STORAGE TANK
2. CENTRIFUGE PUMP
3. 20 IN. CENTRIFUGE
4. SLUDGE FEED TANK
5. SLUDGE FEED PUMP
6. FILTER-INCINERATOR
7. THERMAL OIL BURNER
8. FILTRATE STORAGE TANK
9. OIL RESERVOIR GAGE
10. OIL PUMP
11. AIR BLOWER
12. TEMPERATURE RECORDER
13. TEMPERATURE RECORDER
14. FEED PUMP POWER SUPPLY
15. H2O MANOMETER
16. INCLINED MANOMETER
FILTRATE
Figure 4. Flow Diagram and Equipment for Filter-Incinerator Tests
-------
TABLE 2
COMPOSITION OF 10 IN. DIAMETER FILTER COLUMN
Bed Support
1 In. Thick Fused Aluminum Oxide (FAO) Disc
Layer No.
1
2
3
5
6
7
8
9
10
Description
Harshaw 1/8 in. pellet (coated WNC-1)
Molecular Sieve 1/16 x 3/16 in. (coated)
Ground Molecular Sieve
Coated SK-40+18-12 mesh, 5/8 in.
Uncoated SK-40+18-12 mesh, 3/8 in.
Ground Molecular Sieve
Coated SK-40+30-18 mesh
Ground Molecular Sieves, SK-40+12-18 mesh
Molecular Sieves, 1/16 in.
Molecular Sieves, 1/8 in. extrusions (SK-134)
Harshaw CO 108T, 3/16 x 3/16 in.
Harshaw CO 502T, 1/4 x 1/4 in.
Coors Porous Alumina Plates
Total Column Height
Height (in.)
2
1
1
3/4
2
2
2
2
2
1
16-1/2
12
-------
TABLE 3
10 IN. DIAMETER FILTER-INCINERATOR TESTING
Filtration
Incineration
Dale
Test 1971
1 K-10
2 8-17
3 9-14
4 9-16
5 9-16
Bed
Height
(in.)
16-1/2
16-1/2
2
2
2
Bed
Composition
(a)
(a)
(0
(0
o
Feed
Volume
jgpm)
50
500/50(d'
30
10
20
Type
Feed
RS<»>
TS
TS
TS
TS
Feed Avg Feed
Contie Rate (gpm)
(c) 2-1/4
(c) 2.G
(c)
(c)
(c)
Suspended Solids (mg/1)
Feed Filtrate
1.670 310
970 'R
-,
413 64
448 297
'< Removal
81.5
92
—
84.5
33.8
Date
1971
8-12
8-18
9-14
9-15
9-16
9-16
Max Bed
Temp
885
1.100
970
-
1.080
Time to
Bed Temp
Increase (hr)
2
1-3/4
—
1/4
1/4
Bed
Pressure
inH2O
25-45
22-37
—
1/4
1/4
Time
to Final
Temp (hr)
3-3/4
2-S/4
—
3/4
3/4
Remarks
Filter effluent treated in
catalyst column - final
SS 7 mg/1.
Gas analysts taken on
stack.
Note: Clarified feed to
400/40°' TS*1' (c)
1/6
0.5-1.6
3/4
solids retained on filter
appeared to be washing
through bed.
(a) Bed composition - 16-1/2 in. deep bed located as per Table 1.
(b) RS - Indicates raw sewage Influent - no pretreatment.
(c) Feed configuration - subsurface draw off of stilled volume.
(d) 500 gal. RS concentrated with 20 in. centrifuge to 50 gal.
(e) TS - indicates treated sewage at dosage of I. 2 Ib HTH per 50 gal. (2.000 ppm OCl").
(f) Bed composition - 2 In. height 1/4 x 1/4 to. Harshaw pellets over 6 x 6 in. mesh screen support.
(g) Gas analysis of Stack - O2 - 14.9%: N2 - 81.5%; CO - None; CO^ - 3.4%.
(h) Bed composition - 2 in. of 1/4 x 1/4 in. pellets over FAO No. 24 - inch thick porous plate.
(i) TS -treated sewage 165 gm HTH (750 ppm hypochlortte).
(j) 400 gal. RS concentrated to 40 gal.
-------
combustion times, (2) high pressure drop across the filter bed during combustion
hence a high pressure burner system, and (3) the necessity to pretreat the waste
to assure development of a filter mat on top of the filter bed. Use of a settling
basin was also considered to preconcentrate the waste material prior to filtration.
Regardless of the pretreatment methods considered, the major problem associated
with the mixed media filter bed was excessive incineration time. This is illus-
trated in Figure 5 which provides profiles of bed temperature and pressure drop
as a function of time. As can be observed, approximately 2 hr of burn time were
required to raise the bed temperature to a level to initiate destruction of the
collected solid material and water in the bed. These incineration times and the
requirement for a high pressure burner system were considered incompatible
with the requirements for a simple, low cost pleasure craft waste treatment
system.
Improved Design
Specific filtration-incineration concepts which were evaluated comprised cloth and
porous ceramic type materials as filter elements in a gasoline-fired, single
element, test rig (Figure 6). Figure 7 is a photograph of the test setup. Tests
of various materials and filter elements were conducted over a 3 month period.
A detailed summary of the filter-incinerator tests conducted is presented in
Appendix I. Table 4 summarizes the results of the tests.
The following conclusions in addition to those noted in Table 4 were derived from
the data collected relative to the most promising filter element materials.
Refraail Cloth—Refrasil is a 99+% pure amorphous silica in a continuous filament
manufactured by Hitco Materials Division, Gardena, California. Refrasil was
created for the aerospace industry, where large quantities are used as ablative
compound reinforcement in rocket nozzles, combustion chambers, and reentry
shields. This material, which is also used as a thermal insulation and a flame
barrier in aircraft construction, was first evaluated at Thiokol as a filter element
in sheet form. The material was wrapped around a support tube and retained by
a wire mesh screen and clamps as shown on Figure 8. Two types of Refrasil
were evaluated: plain (C100-48), and "Irish" (C1554-48). The difference between
the two is that "Irish" Refrasil is impregnated with chromium oxide. As shown by
the test data on Table 4, both forms of Refrasil produced satisfactory filtrates
and throughputs, and both withstood the incineration temperature. Subsequent
tests with Refrasil were conducted with B2-1/2 Refrasil braid, a braided seamless
form of the C100 material, which is provided in long tubes. This braided material
was assembled over stainless steel perforated plate support tubes in one and two
layers for testing. Again satisfactory test results were obtained, and one element
was subjected to 40 consecutive filtration-incineration cycles (Runs GF-83 thru
GF-122). Figure 9 shows the element prior to the 40 cycle tests, and Figure 10
is the same element after the test. No material degradation was observed. Based
on test results in the single element test rig, the Refrasil braid was selected as
the prime candidate material for the multiple element demonstration test rig
14
-------
u
CO
w _
«o
& IM
Q X
W •
ffl g
50
COMBUSTION CHAMBER PRESSURE (IN.
-A
BYPASS VALVE CLOSED
F
1,600
COMBUSTION CHAMBER
TEMPERATURE
MAXIMUM TEMPERATURE 1,100° F
TEMPERATURE AT TOP OF BED
1.5 2.0
TIME PERIOD (HR)
Figure 5. Profile of Filter-Incinerator Temperature and Bed Pressure (Test 2)
-------
TEST CYCLE:
1. FILTER
2. INCINERATE
3. BACKWASH WITH WATER
TO REMOVE ASH
HOT
EXHAUST
GASES
SEWAGE
FLOW
WATER
Q-tXl -
FILTER-
INCINERATOR
FILTER MEDIA
S- HOT GAS
S GENERATOR
AIR
GASOLENE
SEWAGE
FILTRATE WASH
WATER
Figure 6. Filter-Incinerator Cylindrtcal Test Unit for Cloth Media
16
-------
Figure 7. Glass Cloth Test Rig
17
-------
TABLE 4
FILTER MATEMAL EVALUATION
Hitco
Material
Refrasil cloth, C1554-48
'Irish, " tested in 1-ply
Refrasil cloth C100-48
"Plain. " tested in 1- and 2-ply
Refrasil Cloth C1S54-48
"Irish, " tested in 2-ply
Refrasil batt (Fabbat) B-1570
Refrasil clothC 1554-48
Tested in 3-ply
Refrasil tube, tested in 1- and
2-ply, B 2-1/2
Refrasil tube, B 2-1/2, 2-ply
with Inconel support
Raybestos-Manhattan High temperature asbestos cloth
"Novatex"
L-70-791 16 oz 1-ply
L-70-652 24 oz 1-ply
L-70-652 24 oz 2-ply
L-70-652, 24 oz 2-ply
Thermal American Fused Quartz cloth
Quartz Co. Style 570 19. 5 oz/sq yd
0.027 In. thick, 5H satin weave
Quartz cloth
Style 581 8.4 oz/sq yd
0.011 in. thick, 8H satin weave
Test Results
Also tested (filtration tests)
C100-96, C100-28, C1554-96 and
C1554-28
Satisfactory filtration obtained
for all weights of cloth, Refrasil
tube, and Refrasil batt.
GF-51 thru 57 with same tube
1-ply, GF-60 thru 67 with same
tube, 2-ply. Incineration at 1,150°F
for all cycles
40 cycle (filtration- incineration)
test using HTH pretreated sewage.
Incineration was at 1,050° F for all
cycles. Element in excellent
condition after 40th test
Attack by sea water observed when
filtration was followed by incinera-
tion at 1,150°F. Lab tests have
indicated material is satisfactory
if temperature is reduced to 1,050° F
or less
16 oz 1-ply produced unsatisfac-
tory filtrate; 24 oz 1-ply marginal
filtrate; 24 oz 2-ply satisfactory
filtrate. Must be Incinerated at
less than 1,050°F
Lab tests indicate material Is
satisfactory for sea water
service at 1,050° F. Multiple
cycle filter-incinerator tests
with 2-ply cloth were conducted
successfully using 3% salted sewage
40 cycle filtration-incineration
test. First 7 cycles with HTH
treated sewage, remaining 33 with
3% salted sewage. Element in
excellent condition after 40th cycle.
Incineration at 1,050° F all cycles
Tested in 1- and 2-ply. Satisfac-
tory filtration with 2-ply. Satis-
factory incineration in fresh
water sewage. Unsatisfactory
after two incinerations in sea
water sewage. No plans to
further test.
Not tested - weave too coarse
Test
GF-l
GF-2
GF-44
GF-3
through GF-13
GF-59
GF-14 through
GF-25
GF-46
GF-47 through
GF-49
GF-51 through
GF-57
GF-60 through
GF-67
GF-83 through
GF-122
GF-26 through
GF-28
GF-29 through
GF-33
GF-68 through
GF-79
GF-l26 through
GF-165
GF-35 through
GF-42
18
-------
Electro Refractories and
Abrasives
Electro Refractories and
Abrasives
TABLE 4 (Coat)
FILTER MATERIAL EVALUATION
Material Test Results
Fused aluminum oxide porous
plates
4 in. dia x 7/16 in. thick
FAONo. 36
4 in. dia x 1 in. thick
FAONo. 24
8 in. dia x 1 in. thick
FAONo. 12
12 in. sq x 1 in. thick
V - groove. FAO No. 54
12 in. sq x 1 in. thick
BiPorous FAO No. 12-36
8 in. dia x 1 in. thick
FAONo. 12
Fused aluminum oxide
cylinders
3 in. OD x 2 in. ID x 12 in. L
FAO No. 80
3 in. OD x 2 in.
FAONo. 54
x 12 In. L
4 in. dia x 1/2 in. thick SIC disc,
"fine" porosity
8 in. dia x 1 in. thick SiC No. 12
Marginal filtration efficiency.
Thermal cracking experienced
during incineration with both
plates and cylinders. No plans
to conduct further tests
Satisfactory filtration - no Incinera-
tion test conducted
Quench test conducted at tempera-
tures up to 550° F, Saltwater
quench - no cracking experienced
Lab tests in sea water at 1.150 ° F
shows attack of binder
Test
PPF-2
through PPF-5
PPF-10
through PPF-11
PPF-6
through PPF-9
OF-1
through OF-4
OF-5and
OF-6
OF-7 and
OF-8
OF-9 and
OF-10
PPF-12,12
PPF-22,23
PPF-15
through
PPF-21
PPF-1
Fluid Dynamics, Inc
3 in. OD x 2 in. ID x 12 in. L
SiC No. 80
3 in. OD x 2 in. ID x 12 in. L
SiC No. 54
X-6 wire tube
2-3/4 in. OD x 10 in. L, 15
fibrous stainless steel
Tested for one filter Incineration GF-82
cycle - good throughput and filtrate
Tested for 2 filter-incineration GF-80
cycles. Good throughput using raw GF-81
sewage. Satisfactory filtrate
Filtrate data not conclusive. GF-50 and
Satisfactory incineration GF-58
Union Carbide
Zirconla cloth
(Zirconium dioxide)
Lab data Indicate this material
may not degrade at 1,100° F In
sea water. Material not as strong
as Refrasil. Larger sample
tested. Poor filtration - no plans
to evaluate further
GF-125
19
-------
TABLE 4(Cont)
FILTER MATERIAL EVALUATION
Supplier
Brunswick Corporation
GAF Corporation
Material
Metallic cloth
Brunsmet 304 SS fiber
Brunspore metal
Fiber media
Sintered stainless steel beads
Sintered cylinder
5 micron polypropylene bag
(non-reusable)
25 micron polypropylene bag
Test Results Test
Poor filtrate resulted during filtra- GF-124
tion test. No further tests
Same as Fluid Dynamics material -
Fluid Dynamics is a Division of
Brunswick
Low throughput - not incinerated, GF-34
no further tests
Satisfactory filtration, bag and None
collected solids successfully
incinerated. No further tests
due to nonreusability of bag
Bendix Filter Division
Poroplate 1 in. dia SS
5 layer wire mesh, 100/7
Screening tests were satisfactory.
Element was purchased as a
backup
None
Mott Metallurgical Corp
Sintered metal filters, approx
1 in. x 2 in. samples varying in
porosity from 1/2 micron to 100
microns.
Refractory Products Co WRP-X-AQ felt
(Al O - SiO fibrous insulator)
23 Lt
Screening tests were satisfactory.
Element was purchased as a
backup
Filter failed
GF-123
20
-------
Figure 8. Glass Cloth Filter
21
-------
Figure 9. Refrasil Filter, Before Test
22
-------
Figure 10. Refrasil Filter, After 40 Cycle Test
23
-------
because it exhibited the best temperature resistance of all materials evaluated
under all operating conditions. Refrasil does not melt or vaporize until tempera-
tures exceed 3,100° F, and will function continuously with little or no change in
properties. In the filter-incinerator, temperatures are controlled to 1,100° F
maximum, thus providing an adequate temperature margin.
Extensive testing was conducted on the Coast Guard program to determine if salt
(both NaCl and sea salt) had a measurable effect on Refrasil. Runs GF-60 thru
GF-67 (Appendix I) show typical results. No adverse effects were detected, thus
providing additional data in a more severe environment on the Refrasil material.
Noyatex—Novatex is an asbestos textile developed by Raybestos-Manhattan,
available in a variety of weaves and in three weights, 8, 16, and 24 oe/sq yd.
Its maximum operational temperature, as noted by the manufacturer, is 1,000°F.
The material was obtained by Thiokol in sheet form in both 16 aad 24 oz weights
and evaluated in the same manner as the Refrasil cloth. The Novatex also pro-
duced a satisfactory filtrate and throughput and withstood the incineration tempera-
ture as long as the temperature was maintained at 1,050° F or lower. A Novatex
filter element was also subjected to 40 consecutive filtration-incineration test
cycles. No material degradation was observed. This material was not selected
as the prime cloth material due to its lower temperature capability compared to
Refrasil. The additional temperature margin was considered necessary in a
production design.
Metallic Filter Elements—Initial screening tests (GF-34, 50, 58) conducted on
the Coast Guard program to determine the applicability of metallic filter elements
to the Thiokol filter-incinerator system placed these elements in a poor relative
position. The elements tested, a sintered stainless steel element (GF-34), and a
15 micron Fluid Dynamics woven element (GF-50 and 58), were both very fine
grained and were blinded rapidly by the sewage feed material. The total through-
put delivered by each of these elements was of the order of 2 to 3 gal/sq ft.
However, an entirely different picture was presented with the testing of a coarser
material. A 1 in. diameter Bendix Poroplate disc with a particle retention rating
of 100 microns delivered an equivalent flow of approximately 13.5 gal/sq ft.
With this success and the desire for a backup filter material as a motivating force,
metal elements were evaluated extensively on the Coast Guard program, which
had a need for much higher throughputs than required for the 15 gal/cycle house-
boat system.
Several types of metal elements were evaluated with the conclusion that metal
elements would work. Several metal elements were purchased for the houseboat
program. Due to the higher cost of the metal elements, they were maintained as
"backup." The need for use of the backup elements did not arise.
24
-------
Burner Assembly—An important component of the filter-incinerator is the burner.
The laboratory studies indicated 80 to 100 SCFM of 1,100°F air was needed for
incineration. Numerous manufacturers were contacted to locate burner equipment
to meet these requirements; however, the combination of relatively high tempera-
tures and low air flow rates eliminated most of the available equipment. The
Model 8304A "Southwind" heater made by Stewart-Warner was found to be suitable
for the filter-incinerator.
The Southwind heater is used on numerous motor vehicles as an engine preheater
in one form and as a passenger compartment space heater in another form. The
burner uses gasoline as a fuel and the hundreds of units presently in service attest
to the safety and reliability of this type of unit.
The use of gasoline as a fuel for a pleasure craft waste treatment system is very
convenient, since most boats have gasoline powered engines. Some safety pre-
cautions must be taken when using gasoline, such as venting of vapors and flame
assurance devices. These precautions have been included in the incineration
equipment. Discussions with the Coast Guard have indicated that the use of pro-
pane or other low boiling point gaseous fuels is not desirable (although propane
fueled stoves are in common use on pleasure craft). Although gasoline could not
be approved for use on commercial vessels, no serious objections were raised to
its use on pleasure craft (which are not governed by U.S.C.G. regulations). In
view of the reliability, safety in motor vehicular applications, and accessibility
of gasoline, it was decided to fuel the incinerator with gasoline, and consider the
use of a less volatile fuel (such as fuel oil) at a later date based on a Coast Guard
review of a prototype system design. Use of gasoline eliminated the need for a
separate fuel tank for the waste treatment system installed aboard a pleasure
craft.
Secondary Treatment
Secondary treatment is that portion of the waste treatment system that reduces the
BOD and suspended solids of the filtrate issuing from the filter-incinerator. The
Thiokol approach to secondary treatment for the pleasure craft system was to
oxidize the dissolved organic material in the filtrate using a strong oxidizing agent,
hypochlorite. Two methods of providing hypochlorite were considered; chemically
adding the hypochlorite in the form of sodium or calcium hypochlorite or onsite
generation of the hypochlorite by an electrolytic process from a NaCl solution.
Both methods were evaluated in the development program. All of the initial
laboratory tests were conducted by adding hypochlorite in the form of sodium or
calcium hypochlorite. Since reaction of the hypochlorite with the dissolved organic
material is a time -dependent process these early tests also involved the use of a
chemical catalyst developed by Thiokol to accelerate the oxidation process.
25
-------
A measure of effectiveness of the catalyst is the rate at which the catalyst will
lower the concentration of available chlorine in an aqueous solution. Figure 11
depicts a laboratory test in which solutions containing about 2, 000 ppm Cl£ were
placed in containers in contact with various amounts of two Thiokol-developed
catalysts (WNC-1 and CCC-6). The catalyst was placed on the bottom of the
container and there was no agitation of the liquid during the test. The CCC-6
catalyst showed higher initial activity, and in 24 hr the chlorine level was reduced
to 50 ppm. Later tests indicated the CCC-6 catalyst loses activity and, at ambient
temperature, could have a performance very similar to WNC-1 catalyst after
1 to 2 weeks of service. Previous tests at Thiokol showed that catalyst activity
could be increased by increasing temperature, but this approach was not con-
sidered for the pleasure boat system due to the limited power available on such
a vessel.
Laboratory secondary treatment tests involved evaluation of various treatment
levels and catalyst amounts. Tests were conducted using 1 qt samples with the
catalyst deposited at the bottom of the quart jar. Figure 12 is typical of the
results obtained. Reduction in BOD was the primary criteria for judging test
results. These tests with the varying amounts of catalyst gave the following
results:
1. With a feed BOD of 300-400 ppm, 1, 000 ppm
Cl2 was too low a treatment level; 2, 000 ppm
seemed optimum.
2. 100 gm of catalyst per 500 ml of solution
appeared optimum.
3. The catalyst had the definite effect of lowering
BOD and free chlorine levels in a hypochlorite
treated solution.
Later tests used 3 gal tanks, and the effects of catalyst placement and circulation
of solution through a catalyst column were studied. The catalyst was either
deposited in the bottom of the 3 gal tank, suspended in porous nylon bags in the
tank, or located in a column adjacent to the tank. In the latter case, a pump was
used to circulate the liquid through the catalyst column. Results are shown below.
Dispersed catalyst generally gave the lowest effluent BOD; circulation did not
appear beneficial, although circulation did cause the chlorine level to drop faster
than in other schemes. Indications were that circulation causes increased free
chlorine destruction, but did not appreciably improve BOD reduction.
26
-------
WT WNC-1 fSRAMS)
50 100 150
WT CCC-6 (GRAMS)
50 100 150
NaOCl CONC AT 0 HR
5 HR
24 HR
1,800 1,800 1,800
1,125 850 725
410 270 210
1,950 1,950 1,950
950 550 650
130 80 50
2,500
ro
246
CATALYST CONCENTRATION (GRAMS-HOUR/MILLILITER)
Figure 11. Catalyst Calibration Data - Static Reactor {65°-70° F)
-------
9-10 FEE DATA
00
400
CATALYST WEIGHT
D 0 GM
CLOROX DOSAGE
PER 500 ML FILTRATE
U 10 ML
O 100 GM
A 150 GM
O 20 ML
0
CLOROX DOSAGE (ML/500 ML FILTRATE)
TIMES 100 = PPM FREE C10
50 100
CATALYST WEIGHT (GM)
150
Figure 12. Catalytic BOD Reduction, Ambient Temperature, Static Reactor (WNC-1 Catalyst)
HORIZONTAL. - i
-------
PILOT CATALYST TEST RESULTS
(BOD'S IN PPM)
Feed
236 57 51 58
370 58 57 49
279 70 68 45
Tank 1 had catalyst at bottom of solution.
Tank 2 utilized circulation through a catalyst column.
Tank 3 had cylinders of catalyst suspended in the
solution.
All tests utilized WNC-1 catalyst.
Total contact time 22-25 hr.
One additional phase of the laboratory secondary treatment investigation was a
test to determine the effectiveness of catalyst in reducing BOD at room tempera-
ture. Figures 13 and 14 depict a test where three 3 gal containers were filled
with a sewage solution containing 215 ppm BOD, 124 ppm suspended solids, and
950 ppm Cl2- One container had catalyst present the entire 22 hr test period,
one container had no catalyst the entire period, and the remaining container had
catalyst added after 9 hr of chlorine contact time.
Testing on other systems has shown that higher treatment temperatures will speed
the reduction of BOD in the presence of catalyst. However, Figure 13 shows no
discernible effect of catalyst on BOD or suspended solids at ambient conditions.
Figure 14 does show that the use of catalyst will remove free available chlorine.
Further confirming tests with catalyst were conducted during the demonstration
program.
During the laboratory tests it was noted that addition of an alkaline hypochlorite
to sewage produced a white precipitate. The secondary treatment section was
designed to include a solids settling section to prevent discharge of this material.
29
-------
A NO CATALYST
O NO CATALYST FIRST 9 HR, CATALYST USED THEREAFTER
D CATALYST USED ENTIRE TEST
140
20
6 8 10 12 14 16 18 20 22
TREATMENT TIME (HR)
4?U
20*
160
s
&
* 140
8
ffl 100
60
20
C
M
\
\
4
V
N
L
r
— ^.
-«-
n^^B^^^^"
^Mi^H^^BH
— I
1 2 4 6 8 10 12 14 16 18 20 22
TREATMENT TIME (HR)
Figure 13. Effect of WNC-1 Catalyst on BOD and SS Removal
30
-------
A NO CATALYST
O NO CATALYST FOR 9 HR CATALYST USED THEREAFTER
D CATALYST USED ENTIRE TEST
1,000
800
Pu
*«•••'
w
600
400
o
200
CATALYST ADDED
16 18 20 22
0246 8 10 1^
TREATMENT TIME (HR)
Figure 14. Effect of WNC-1 Catalyst on C12 Removal
31
-------
SECTION V
SYSTEM DEMONSTRATION
FLOW-THRU TESTS
Upon completion of the laboratory system testing previously described, a proto-
type" system waa. designed, fabricated, and installed in Thiokol's waste treatment
test laboratory, which comprised an actual restroom equipped with a marine toilet
and a prototype pleasure craft waste treatment system (Figure 15). The treat-
ment system was located adjacent to the restroom in the same manner planned for
the later vessel installation. The laboratory work force utilized the restroom.
Figure 16 provides a more detailed schematic of the treatment system and
Figure 17 is a photograph of the filter-incinerator assembly. Table 5 lists major
system components. The filter-incinerator was equipped with three Refrasil
2-3/4 in. OD by 22 in. long filter elements resulting in a filter surface area of
4 ft . Operation of the system was as follows.
Macerated waste from the marine toilet collected in the holding tank until the high
liquid Level in the tank (as determined by a level sensor) was reached. A pre-
measured quantity of hypochlorite was added to the tank at this time and the batch
processing of the collected waste was initiated. The liquid from the holding tank
was pumped to the filter-incinerator using the 2-1/2 gpm rotary screw pump and
circulated through the filter-incinerator back to the holding tank. At the same
time, the 1 gpm vacuum pump was operated to draw filtrate through the filter ele-
ments and transfer this filtrate to the catalyst tank. This process continued until
the Level sensor in the holding tank indicated all waste had been processed.
Liquid remaining in the filter-incinerator was then drained back to the holding
tank, and the collected solid material was incinerated. Upon completion of the
incineration cycle, the system was ready to accept another batch of sewage. The
compartments in the secondary treatment tanks hold approximately 15 gal each
and the average batch size processed through the system was 15 gal. Thus, the
average residence time of each batch in the secondary treatment tank was the time
required to process two batches of sewage. This time varied throughout the test
program but was generally in excess of 12 hr.
Flow-thru testing was initiated on 22 May 1972. Forty-five batches of sewage
were processed. Sewage for all but six batches was obtained from the limited
flush marine toilet. In an effort to supplement the human sewage, dog food was
added to six of the batches. Test results are shown on Table 6. The first 36 tests
utilized the sewage from the marine toilet. The next six (37 thru 42) were con-
ducted with dog food addition and the last three with sewage from the marine toilet.
The summary table gives BOD and suspended solids data for feed sewage, filtrate,
and effluent. 32
-------
CATALYST
TREATMENT
TANK
FILTER-
INCINERATOR
PLAN VIEW
WATER
SUPPLY
ELEVATION VIEW
Figure 15. Building M-85 Layout, EPA Houseboat
33
-------
y— FUEL PUMP, 0.5 GPH
GAS TANK, 5 GAL
BLOWER, 1/3 HP
BURNER
EXHAUST
OUTLET
3 IN. STACK
MACERATOR
OPTIONAL CL.
INJECTION
7U44748
FILTER-INCINERATOR
CATALYST
OVERBOARD
DRAIN
HOLDING TANK
25 GAL
CATALYST TANK
35 GAL
DRAIN
Figure 16. Houseboat Schematic Diagram
-------
BURNER
ASSEMBLY
FILTER
INCINERATOR
Figure 17. Prototype Filter-Incinerator Assembly
35
-------
TABLE 5
MAJOR FLOW-THRU SYSTEM COMPONENTS
Component
Toilet/macerator
Burner assembly
Vacuum pump
Filter feed pump
Blower
Holding and
catalyst tank
Settling tank
Filter incinerator
Description
Limited flush marine toilet
Fuel pump and burner
11 to 20 in. Hg vacuum,
1/4 hp, 115 vac
Rotary screw pump,
2-1/2 gpm, 115 vac
160 cfm at 5 in.,
1/3 hp, 115 vac
37 gal polyethylene
30 gal conical bottom
polyethylene
Three element filter
incinerator
Manufacturer and Model
Raritan Crown Head
"Southwind" Model 83 04 A
by Stewart-Warner
Vanton Flex-i-liner,
size 18
Teel - W. W. Grainger's
S/N 1P555
W. W. Grainger's
P/N 2C820
Nalgene
U.S. Plastics - S/N 06311
Nalgene Series 16000
Thiokol
36
-------
TABLE 6
SUMMARY Or SYSTEM FljOW-THRl! TESTING
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37*
38*
39*
40*
41*
42*
43
44
45
6/2
6/5
6/5
6/6
6/6
6/7
6/7
6/8
6/8
6/8
6/9
6/12
6/12
6/12
6/U
6/13
6/13
6/14
6/14
6/16
6/19
6/19
6/20
6/20
6/20
6/21
6/21
6/22
6/23
6/26
6/29
6/30
8/21
8/21
8/22
8/23
8/24
8/25
8/28
8/29
8/30
250
None
None
250
250
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
hime
tend
g»H
21
19
9
19
25
IS
IS
15
13
20
20
IS
IS
15
10
15
15
15
15
IS
16
2»
IS
20
15
15
15
15
IS
25
12
21
12
12
9
8
IS
10
15
11
9
IS
15
15
10
Filtration
Time
(mini
8.4
11.5
—
—
15
7
7
10
8.4
16
15
9.4
9.4
9.6
7
8.3
8.9
9.0
10
10
11
23
14
14.8
34
54
8.8
10.8
11.5
14.3
8.3
IS
8.8
7.6
10
8
25
30
30
30
30
30
25
IS
10
Influent
S/S**
(mg/l)
305
242
2.820
965
1,035
1,855
1.690
5.540
7,675
320
218
520
--
—
5.860
1.678
902
3,435
1.168
1.820
908
„
705
„
2.340
1,008
616
600
720
—
—
..
1,750
605
—
--
1,450
760
4,002
8,400
650
5,005
534
—
4,252
Filtrate
S/S
ftnt/1)
75
52
133
200
202
180
4
173
48
110
25
205
—
--
285
112
113
132
140
66
72
—
73
41
69
—
108
78
79
—
—
51
52
20
—
—
21
20
130
29
40
38
25
—
337
*
Reduction
S/S
75
90
96
80
80
90
99
97
99
66
89
60
—
—
95
93
88
97
87
96
92
—
89
—
99
—
82
86
89
—
—
—
97
97
—
—
98
97
99
99
93
99
96
—
92
Influent
BOD
(mg/1)
430
—
950
700
720
814
914
2,820
3,270
541
385
475
—
—
1.894
846
846
1,132
—
—
—
—
—
—
1,064
1.094
850
514
974
_
—
„
—
„
—
_
1,060
683
1. 456
3.760
2,330
3,700
2,260
—
3,400
Effluent
BOD
(rot/1)
—
—
—
108
219
188
327
307
130
—
79
—
153
—
—
—
—
—
—
—
—
66
--
179
—
165
69
66
—
—
_-
—
—
—
—
—
--
541
388
416
1,140
512
—
160
%
Reduction
BOD
__
__
._
—
85
73
79
88
91
76
—
83
—
—
—
—
—
—
—
—
—
—
—
83
—
80
92
93
—
—
—
—
—
—
—
—
—
63
90
82
69
77
—
95
Filtrate
Treatment
(ml of
Superchlor
added)
None
None
None
1.250
None
—
—
1,200
1.200
1.200
,200
,200
,200
.200
.200
,200
.200
.200
,200
1,200
1,200
•t
600
500
?
1,000
?
?
?
?
?
?
750
?
lot
iqt
iqt
2/3 qt
2qt
2qt
«qt
7qt
7qt
»qt
6qt
Incineration
Time
(mjq)
41
40
44
41
75
65
35
30
25
75
30
40
45
30
t
None
None
80
None
None
60
65
60
None
None
75
None
None
60
65
60
None
30
45
45
2
None
35
50
40
None
60
70
70
45
Cumulative
Incineration
Cycles
1
2
3
4
1
2
3
4
5
6
7
8
9
10
11
—
—
12
—
—
13
14
15
—
—
16
—
—
17
18
19
—
20
21
22
23
—
24
25
26
—
1
2
3
4
Original elements Improperly Installed.
Two ply B-2 1/2 elements were reinstalled.
Replaced outer ply of all elements after test.
•Tests with dog food addition
"S/S - suspended solids
-------
The effluent BOD values listed in Table 6 range from 66 mg/l to 327 mg/l, exclud-
ing the tests conducted with dog food added to the sewage. While BOD values in
excess of 150 mg/l are considered high, they must be evaluated on the basis of
the feed values of BOD which were generally high, ranging from 300 to as high as
3,400 mg/l. An average BOD reduction of 82% was obtained. Additional chemi-
cal treatment to further reduce BOD was considered but not investigated due to
the issuance of a program stop order and the subsequent program redirection to
evaluate a zero discharge system.
Runs 37 thru 42 had high effluent BOD values (between 388 and 1,140 mg/l) due to
the type of sewage used (a mixture of human sewage and dog food) in the tests.
Dog food contains a quantity of fat and numerous other ingredients not normally
found in actual body waste. Dog food proved useful in checking filtration perform-
ance of the system, but did not give an accurate indication of the system's BOD
removal capability and was discontinued.
Performance of the filter elements with suspended solids reduction of 60 to 90%
was considered good. Durability of the elements was also good, although the outer
ply of the initially installed elements was observed to be torn after the first four
tests. This failure was determined to be caused by faulty installation. After
replacement of the initial elements with new elements, no element deterioration
was observed for 37 filtration cycles (26 incineration cycles).
During the dog food tests, filter thru-put dropped to about 15 gal before inciner-
ation was needed. In an attempt to improve thru-put, a water backwash cycle
was initiated. Inspection of the elements after test number 41 showed a small
tear in the outer ply of one element, but no deterioration of the inner plies. The
outer ply of filter cloth was replaced on all three elements.
The three filter elements contained a total of 4 ft2 of filtration area. Even with
the heavy sewage feed during tests with dog food, 15 gal of sewage were processed
through the elements indicating an adequate surface area for filtration. Runs 27
thru 29 represented a total filter thru-put of 45 gal before incineration as did
runs 31 thru 33, thus verifying the adequacy of the filter elements.
Figure 18 depicts a typical incineration cycle. An exit temperature of over 800° F
is necessary for complete combustion of solids. Several runs were stopped before
the 800° F exit temperature was reached; inspection of the interior of the inciner-
ator revealed several areas having unburned solids. Later runs were made with
the blower shut off simultaneously with the fuel, and no adverse effects resulted.
During all incineration cycles, odors were never detected In the vicinity of the
equipment or from the exhaust stack. Visible discharge of smoke or particulate
matter was not detected in the exhaust.
38
-------
RUN NO. 3 WITH FILTER-INCINERATOR USING
3 REFRASIL ELEMENTS
1,200
u
06
a
a
S
W
H
20 30
TIME (MIN)
40
50
Figure 18. Typical Temperature Profile
From the preceding tables and other operating experience, expected operating
parameters were developed for the flow-thru system as shown on Table 7.
ZERO DISCHARGE TESTS
To demonstrate the feasibility of using a recirculating system onboard pleasure
craft, certain of the components used in the flow-thru tests were utilized to treat
the Building M-85 flushwater for reuse.
The system was assembled similarly to that shown in Figure 15. The fresh water
supply line to the flushwater tank was capped and treated effluent from the cata-
lyst tank was recycled to the flushwater tank instead of discharging the effluent.
Since the addition of solid hypochlorite would have resulted in buildup of the dis-
solved salt level in the system and liquids in the system would have increased by
39
-------
TABLE 7
PROJECTED
FLOW-THRU SYSTEM PERFORMANCE
BOD reduction « 90 to 95%
SS reduction = 90% by filtration, 95% overall
Effluent pH * 10 to 12
Effluent coliform * negligible
Effluent C12 level * 50 to 100 ppm
Chlorine use = 1 gal Clorox/7 gal feed sewage
at 2, 000 to 4, 000 ppm BOD
Filtration time » 15 min for 15 gal batch
Incineration time » 45 min
Gasoline/Incineration = 1/2 gal
Electrical power:
Fuel/spark = 3 amp, 12 v, 45 aria (*. 03S kwfc)
Filter feed = 7 amp start, 3 amp ma,
115 v, 15 min (0. •*• kwh)
Blower « 15 amp start, 3 amp run, 115 v,
50 min (0.288kwh)
Vacuum = 15 amp start, 3 amp run, 115 v,
15 min (0.086 kwhl
Total power use per cycle 0.460 kwh
40
-------
liquid hypochlorite addition, initial zero discharge tests were conducted using an
electrolytic process to generate hypochlorite. In this process, the only chemi-
cal addition necessary is sodium chloride, and electrolytic cells are used to con-
vert the sodium chloride to sodium hypochlorite. PEPCON cells, manufactured
by Pacific Engineering and Production Company of Nevada, were selected for use
in the system.
There is a contribution to the salt level in the system by body waste; however,
prior experience with other systems has shown this to be negligible.
Normal ship power (12 v) is used to power the PEPCON cell system. Three
PEPCON cells (10 in2 each) are connected in series electrically with parallel
liquid flow. This scheme allows minimum hydraulic pressure drop and a voltage
drop of 4 v across each cell. With a 4% NaCl solution, an amperage drain of 5 to
6 will result. The current and rate of hypochlorite production is adjusted by
changing the salt concentration.
The system used a 1/35 hp pump (115 v, 200 w) to circulate system liquid through
the PEPCON cells; each cell had a flow of about 1/4 gpm.
The system was filled with salt water on 1 September and the solution was cir-
culated through the PEPCON cells to generate the hypochlorite level. The hypo-
chlorite/salt solution was then used as the M-85 toilet flush media. On 7 Sep-
tember sufficient liquid waste had been collected for the initial filtration run.
Since current levels in the PEPCON cells were dependent upon the salt level
(voltage is fixed), there was an initial adjustment of salt levels to find the proper
operating level. The system had a poor electrical connection upon startup and
excess salt was added. Later, the faulty connection was discovered and the
solution had to be diluted to bring cell current down to the 5 to 6 amp range.
Operation was unstable the first week as solution was dumped and replaced with
fresh salt water. After the startup period, no difficulties were experienced with
the PEPCON system and current levels were very stable. The data from this
initial test provided sufficient information for the preliminary Phase II design.
PRELIMINARY PHASE II DESIGN
System testing in Phase I indicated that the concept of a zero discharge system
was sound. There were several modifications suggested by the test results which
would greatly simplify system manufacture, installation and operation.
During the filtration tests, it was observed that a filtration rate of 100 ml/min
was possible without using a vacuum pump. The new Phase II filter-incinerator
design was consequently based on gravity flow during filtration which allowed the
unit to be placed directly above the secondary treatment tank and eliminated the
need for one pump.
41
-------
Figure 19 depicts the basic system Layout planned for the pleasure craft. A por-
tion of the closet located next to the toilet was chosen to house the treatment
system. The mode of operation (based upon use of a marine toilet) was as
follows:
1. The toilet and holding tank, 1 and 2, was precharged with
a hypochlorite solution. The Monomatic toilet held about
4 gal of solution which was used for a number of flushes.
2. After 30 to 40 uses, the holding tank contents, 2, were
pumped out into the filter-incinerator, 3, for gravity
filtration.
3. The holding tank was then refilled with treated water from
the catalyst tank, 4.
4. Filtrate via gravity entered the catalyst tank, 4 (filtration
required 10 to 14 hr).
5. After a majority of the filtrate entered the catalyst tank,
a pump automatically initiated circulation through the
PEPCON cells, 5. A timer stopped circulation after
adequate treatment.
6. Prior to pumping another batch into the filter, the solids
remaining on the filter were incinerated.
The desired degree of automation was not initially determined. It appeared
possible that all operations could be controlled by a timer and the entire filtra-
tion/incineration/treatment cycle could occur with no operator attention after
initiation of the cycle (pushing the START button). It was decided to initiate test-
ing in a semiautomatic mode in the laboratory and incorporate automation at a
later date.
System Design
The zero discharge system concept for Phase II provided a safe, compact waste
treatment package with the potential for low initial cost and low operating costs.
Virtually all of the system components were located in the closet adjacent to the
washroom, as shown in Figure 19. The toilet, holding tank, and recirculating
flush pump were an integral unit to minimize the loss of usable living space in the
washroom. All components were readily accessible for routine maintenance.
The 30 gal catalyst tank was constructed of Nalgene to provide the necessary
corrosion resistance. An aluminum support cage (Figure 20) was provided to
42
-------
\
\
\
\
1) TOILET
2) HOLDING TANK
?) FILTER-INCINERATOR
2) CATALYST TANK
7) PEPCON CELLS
EXHAUST |
~i
j
ENGINES
J —
Figure 19. Zero Discharge Installation Layout
-------
i (Figure 20. Catalytic Tank Support
(Sheet 1 of 2)
-------
.U
v\
L
-O2 A55'Y
B7.I3
Figure 20. Catalytic Tank Support
(Sheet 2 of 2)
5 DIA THRU
F=t-AC£S>
21.50 KEF
-------
increase the structural integrity of the tank and support the PEPCON cells. The
catalyst was contained either in individual porous bags inside the tank or in
separate columns outside the tank. Valves and piping in the system are either
stainless steel or corrosion resistant plastic.
The filter-incinerator (Figure 21) was constructed of stainless steel throughout.
The Refrasil heat resistant filter cloth was supported by a porous plate and held
in place by a retaining ring. Hot gases provided by a commercial blower and a
gasoline burner entered the incinerator tangentially just above the filter media to
induce a vortex flow pattern to promote complete combustion. Temperature taps
were provided in the prototype model to monitor possible cold spots and air flow
requirements. A damper valve was installed in the exhaust stack to control com-
bustion temperature. An access hatch was located in the top of the incinerator
for removal of ash and replacement of the filter cloth. The entire incinerator
and exhaust stack was insulated and tagged for the protection of personnel.
Electric power was supplied by a 110 vac generator on board the pleasure craft.
Direct current power for the PEPCON hypochlorite generators was supplied by a
standard automotive-type battery charger. Fuel for the burner was taken from
the craft's fuel tanks via a small commercial fuel pump.
The entire treatment system (Items 3, 4, and 5 of Figure 19) occupied a volume
31 by 29 by 40 in. (L x Wx H). On small crafts, with limited interior space, the
system could be placed in a weatherproof cabinet and then installed on deck.
There was also the option of separating components to fit available space. The
basic approach for Phase II was to evaluate the Phase II design in the laboratory
prior to installation aboard the vessel.
Laboratory Test Phase
The objective of the Phase II laboratory test phase was to fabricate and evaluate
the system prior to actual field tests on board the boat. The initial system was
installed in a Thiokoi facility for use by laboratory personnel. The system con-
sisted of a low volume flush toilet, a filter-incinerator for removal and disposal
of suspended solids, and a method for addition of chlorine to remove the color
and disinfect the wastewater. The treated water was stored for reuse. Four
basic system configurations were tested.
Configuration I—Configuration I consisted of the following items of major
equipment:
1. A Raritan crown head marine toilet.
2. A vacuum filter-incinerator.
46
-------
Figure 21. Incinerator Blower Assembly
(Sheet 1 of 2)
47
-------
00
-02 X1S5V VIEW D-D .»oo ».
Figure 21.
Incinerator Blower Assembly
(Sheet 2 of 2)
-------
3. Four 10 in2 electrolytic cells.
4. Catalyst.
The system was initially charged with salt water. The water was pumped, on
demand, to the marine toilet for flushwater. The wastewater was collected in a
surge tank and held for subsequent treatment. Periodically the wastewater was
pumped to the filter-incinerator for suspended solids removal.
Filtrate was withdrawn from the filter with a positive displacement pump and
transferred to a treatment tank. At the conclusion of the filtration cycle, the
filter-incinerator was drained and the filter cake incinerated in place.
The filtrate was circulated through the electrolytic cells and catalyst for chlorin-
ation. The treated water was stored for reuse.
This system was tested from 7 Sep until 24 Sep 1972. An operation log for sys-
tem operation during this period is presented in Table 8. Samples of treated
water were removed periodically for analysis. The results of these analyses are
presented in Table 9 defining system performance. Suspended solids concentra-
tions ranged from 162 to 800 mg/1. BOD concentrations ranged from 95 to
1,500 mg/1. Coliform tests were negative. Testing was terminated when a
piping connection failed and the water inventory was lost from the system.
Configuration II—The only difference between Configurations I and n was the sub-
stitution of a Monomatic toilet in Configuration n.
The system was initially charged with chlorinated salt water. Salt water (4 gal),
containing a chlorine concentration of 275 ppm, was added to the holding tank of
the Monomatic toilet. These 4 gal were recycled through the toilet bowl during
each flush sequence. After several uses, the 4 gal of wastewater were pumped
to the filter-incinerator for suspended solids removal. System operation was the
same as Configuration I.
This system was tested from 27 Sep to 9 Oct 1972. Objectionable odors prompted
the addition of several commercial masking agents, Fresh Up (quaternary am-
monium salt) and T-5 (zinc sulfate), to the Monomatic holding tank. These
chemicals were not compatible with the wastewater and did not provide satis-
factory results. Testing was terminated on 9 Oct 1972. Limited analytical data
obtained during this test period are presented in Table 9 indicating suspended
solids and BOD concentrations of 492 and 582 mg/1, respectively. Coliform tests
were negative.
rnnflpruration Illy-Configuration ffl was the same as Configuration n, except that
a modified Monomatic toilet was used.
49
-------
TABLE 8
ZERO DISCHARGE OPERATION LOG
Test Filtration
Configuration Date Volume (gal) Inventory (gal) Remarks
I 9/7 11
9/8 14 35
9/13 16 27 Dumped 7 gal excess
9/18 18-1/2 31
9/20 ~ 33-1/2
9/22 18 36-1/2
9/24 — 2 Connection ruptured, losing
system inventory
n 9/27 ~ — Started recirculation of
toilet contents as flush-
water
10/2 17 21 Bag filter used
10/5 5 — Gravity filtration with flat
element
50
-------
TABLE 9
ZERO DISCHARGE ANALYTICAL RESULTS
TREATMENT TANK
Before or
Chlorine
Test After Filtrate
Configuration Date Addition
I 9/7/72
9/8/72
9/8/72
9/13/72
9/13/72
9/18/72
9/18/72
9/22/72
9/22/72
II 10/2/72
m 10/13/72
10/18/72
10/18/72
10/20/72
10/20/72
10/25/72
W 11/30/72
11/30/72
12/19/72
1/2/73
1/22/73
After
Before
After
Before
After
Before
After
Before
After
After
After
Before
After
Before
After
After
Filtrate
After HTH
addition
—
~
__
BOD S/S Chloride
(mg/1) (mg/1) (ppm Cl~)
310 282 32,684
95 — 21, 010
283 ~ 22, 670
217 254 23,201
672 198 23,257
326 162 25,022
1, 500 494 23, 684
475 246 24, 193
1,220 800 22,050
New Solution
582 492
New Solution
305 112
170
370
319 100
728 142
730
1,338
696
1, 147
._
1,692
Collform
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
~
~
—
—
—
~
7.15
6.4
158
348
Neg
51
-------
The system was charged with 32 gal of 1.5% salt water. The Monomatic toilet
was modified such that freshly treated water was supplied for each flush sequence.
The wastewater was accumulated in the holding tank of the Monomatic toilet.
Periodically, the holding tank contents were transferred to the filter-incinerator
for suspended solids removal. System Operation was the same as Configura<-
tions I and II.
This system was tested from 10 Oct to 20 Nov 1972. An operation log for this
period is presented in Table 10. Samples were withdrawn from the system
periodically for analysis (Table 9). Suspended solids concentrations ranged from
100 to 142 mg/l. BOD concentrations ranged from 170 to 730 mg/l. Coliform
tests were negative.
During the last 2 to 3 weeks of this test period, components for the onboard model
of the houseboat waste treatment system were received and intermittently imple-
mented in the laboratory tests for evaluation and checkout. These tests are
described below:
Gravity filter-incinerator evaluation—After fabrication of the filter-incinerator,
several days were retired to adjust the burner to deliver a stable flame. A
burner cup was added to stabilize the flame and insure positive ignition. With a
wide open damper, the gases entering the incinerator were 1,050° to 1,150° F.
On 17 Nov 1972, approximately 10 gal of concentrated Monomatic wastes were
filtered. The starting filtrate rate was 0.4 gpm, after 12 min the rate dropped
to 0.25 gpm. Total filtration time was 2 hr. Two factors caused the filtration
rate to decrease during the filtration cycle: plugging and decrease of head (liquid
height above the filter).
The incineration time was 10 min, which was the length of time for the outlet
temperature to approach 1,150° F. At the end of the incineration, the temper-
ature switch located just above the filter cloth was starting to cycle indicating
a temperature at this point of near 1,050° F. Inspection of the filter upon open-
ing the incinerator showed complete incineration with no unburned material
remaining.
The second batch of material would not filter by gravity alone; it was necessary
to run the vacuum pump briefly to initiate flow. After the brief run with the
pump, filtration continued solely by gravity at about 0.065 gpm. The first two
runs were made with macerated sewage (a "MONO" pump was installed on the
outlet of the Monomatic toilet). On the third run, the sewage was transferred to
the filter via a diaphragm pump. The unmacerated sewage resulted in a 20 min
filtration time for 8 gal of filtrate with gravity flow, substantially better results
than experienced with macerated sewage. Indications were that use of a transfer
52
-------
TABLE 10
ZERO DISCHARGE OPERATION LOG
TEST CONFIGURATION IB
Date
OctlO
Oct 11
Oct 12
Oct 18
Oet 1€
ti
^'
*Oct 17
Oct 18
Oct 19
Oct 20
Oct 23
Oct 24
Oct 25
Oct 26
Oct 27
Oct 30
Oct 31
Liquid Discharge
4
14
9
10
7
9
17
8
7
7
8
10
13
13
12
16
Fittratioa
Volume
Solid Discharge (gal)
1
1
3
2 20
3
4
2 16
3
2
3
2
2 6
2
1 13
3
2
Inventory
(atii
26
—
32
—
33
—
32
—
—
—
—
—
—
30
—
— —
Remarks
Recharged system
Added 12 gal fresh water
Changed toilet flush switch
to momentary contact
-------
pump that does not break up the sewage solids will result in much shorter
filtration times and may eliminate the need for a vacuum pump.
100 in2 electrolytic cell evaluation—For simplification of design, one larger
PEPCON cell was evaluated in place of the four small cells. The 100 in2 cell
was first run on 7 Nov 1972, treating a 20 gal batch of sewage with a BOD of
about 1,315 ppm. After 2 hr of treatment, the solution was decolorized from a
dark brown to a light yellow and had a Cl£ residual of about 200 ppm. Four
additional hours of treatment did not change the color and raised the C\% level to
650 ppm.
An extended run was started 17 Nov 1972. Results are given in Figure 22.
Concentrated sewage (24-1/2 gal) was treated with the 100 in2 PEPCON cell.
Cell amperage was maintained near 1 amp/in2. Color removal was indicated
by the trans mi ttance increase of the solution. Initial trans mittance was 5%,
after 3 hr was 22%, after 5 hr was 50%, after 8 hr was 60%, and after 35 hr of
treatment was 91%. A true color test was not performed; however, the trans-
mittance gives an indication of solution clarity. After several hours of treat-
ment the solution was light yellow and was clear after 35 hr.
Configuration IV—Configuration IV consisted of the following items of major
equipment and unit operations:
1. A Monomatic toilet (modified).
2. A gravity filter-incinerator.
3. Chemical (HTH) addition.
The system was charged with 20 gal of effluent from the Configuration III test.
Flushwater was supplied to the toilet in one of two modes, as described below.
The accumulated wastewater was transferred to the filter-incinerator for sus-
pended solids removal. The filtrate drained by gravity flow into a treatment
tank. Calcium hypochlorite pellets or powder (tradename "HTH") was added to
the treatment tank as a source of chlorine. An extended reaction period (over-
night) was used in lieu of catalyst used in previous test configurations. The
treated water was stored for reuse.
The system was tested from 21 Nov to 20 Dec 1972 with the Monomatic toilet
modified to provide freshly treated water for each flush sequence. The system
was operated from 20 Dec 1972 to 23 Jan 1973 with the Monomatic toilet modified
to recirculate the toilet chamber contents during each flush cycle. Operating
data obtained during the test period are presented in Table 11. The analytical
test results are presented in Table 12. The continual addition of chemicals to
54
-------
en
en
18
17
16
15
C4 14
S
!! 13
S1
Pi
5 12
I
« 11
10
9
8
7
400
Pi
&
2
a
o
40
Cl, = 1,140 PPM
Z
AT 35 HR
BOD
8 10 12 14 16 18 20 22 24 26 28 30 32
TOTAL TREATMENT TIME (HR)
34
Figure 28. Treatment of 24-1/2 Gal Sewage With a 100 In2 PEPCON Cell at a Nominal of 1 Amp/In2
-------
TABLE 11
ZERO DISCHARGE OPERATION LOG
TEST CONFIGURATION IV
Date
22 Nov 1972
27 Nov 1972
27 Nov 1972
29 Nov 1972
29 Nov 1972
30 Nov 1972
30 Nov 1972
30 Nov 1972
30 Nov 1972
30 Nov 1972
1 Dec 1972
5 Dec 1972
18 Dec 1972
22 Dec 1972
4 Jan 1973
11 Jan 1973
22 Jan 1973
Uses in Batch
Liquid Solids
_-
—
--
__
_-
—
..
_
„
46 4
7 2
26 2
55 4
29 6
37 8
22 4
17 1
HTH
Added Total HTH
(Em) Addition
1,587.0 1,587
254 1,841
720 2,561
324 2,885
—
450 3,335
2,885
450
1, 184
713
1,040
737
840
2, 089
C12
(ppm)
140
800
150
1,900
• 3, 100
560
700
—
—
—
—
--
~
--
Remarks
—
—
—
—
~
Dissolution of
previous addition
HTH added to toilet
before pumpout/
filtration.
After filtrate
addition
—
57. 7 g HTH/use
50 HTH/use
42.3 HTH/use
12. 1 HTH/use
29. 7 HTH/use
16. 4* HTH/use
32.3 HTH/use
116. 2 HTH/use
•First batch in recirculating mode.
56
-------
TABLE 12
ANALYSIS OF TREATMENT TANK SLUDGE
(8 Dec 1972)
CaCl = Principal compound
A
Na = 1.5%
SO4 = 0.45%
Si = 0.27%
Mn = 0.015%
Fe * 0.27%
Mg = 0.1%
Al = 0.38%
Sn = 0.021%
Cu = 0.1%
Zn = 0.29%
Ti = 0.025%
57
-------
the wastewater resulted in a saturated solution with respect to calcium chloride.
Consequently, crystallization was observed in the treatment tank. An analysis of
the solids sample from the bottom of this tank confirmed calcium chloride as the
principal constituent (Table 12).
At the conclusion of the extended test period, two water samples were taken for
detailed analysis and evaluation. The first sample was analyzed for BOD, virus,
and conventional inorganic properties (Table 13). As noted in Table 13, the sys-
tem is saturated with respect to calcium chloride. Virus tests were negative.
Although a high residual BOD concentration was observed, suspended solids were
low and the water was concluded to be satisfactory for reuse as a flush media.
The second water sample was submitted to the Utah Water Research Laboratory
at Utah State University, under an independent research grant funded by Thiokol
Corporation, for isolation and identification of those ingredients comprising the
high residual BOD concentration. The results of these tests are presented in
detail in a separate report (Adams, V. Dean & Middlebrooks, E. Joe, "Identific
cation of Organic Compounds in a Closed-Loop Hypochiorite Wastewater Treat-
ment System, " Utah State University, Logan, Utah, May 1973) which is included
in the Appendix. It was concluded that the material was a complex mixture con-
sisting mainly of saturated chlorinated fatty acids, presumably a reaction product
of Uplds in feces, by free radical chlorination and chlorine addition.
During the early part of March, the waste treatment system (test Configurai-
tion IV) was installed in a closet which had dimensions identical to the closet on
the Thiokol houseboat. The installation (Figure 23) simulated boat operation.
Operation of the system in the confined space disclosed no operational problems.
The closet doors were kept closed during incineration and as much as possible
during normal operation to detect odor or heat problems. During incineration
periods (10 min of burner operation) the closet temperature did not rise over
15° to 20° F above ambient, indicating sufficient insulation. The combustion air
is drawn from the closet interior which maintains an even closet temperature
and gives odor-free incineration.
Usually the system had 20 to 25 liquid uses and 4 solid uses in each treated batch.
The number of uses in each batch was very dependent upon the orientation given
toilet users. A degree of user care is necessary to prevent excess use of
flushwater.
An average of 1-1/2 Ib of powdered HTH was added to each batch to oxidize
organics and sanitize the solution. No odor problems were experienced; the
recycle liquid remained clear, containing between 120 and 350 ppm C12. Since
the water does not remain in the bowl of the toilet, but immediately flows to a
sewage hold tank, the high C\2 content of the flushwater has no objectionai
effects.
58
-------
TABLE 13
HOUSEBOAT SYSTEM FLUSH LIQUID
(10 Oct 1972 to 23 Jan 1973)
Analysis
Virus
Biochemical oxygen demand
Calcium
Magnesium
Sodium
Potassium
Copper
Lead
Zinc
Iron
Total organic nitrogen
Albuminoid ammonia
Free ammonia
Nitrite (NOg-N)
Nitrate (NOg-N)
Carbonate
Hydroxide
Sulfate
Chloride
Total solids
Phosphate (PO4)
Suspended solids
Results
No detectable virus present
2,125 ppm
17,360mg/l
182 mg/1
12,000mg/l
945 mg/1
0.35 mg/1
5.36 mg/1
2.18 mg/1
3.10 mg/1
2.50 mg/1
0.13 mg/1
0.00 mg/1
3.65 mg/1
4.20 mg/1
0.00 mg/1
0.00 mg/1
705 mg/1
46,500 mg/1
89,620 mgA
5.20 mg/1
48.0 mg/1
59
-------
Figure 23. Houseboat Waste Treatment System Installed in Closet
60
-------
Testing was completed during April and system installation on board the Thiokol
houseboat was initiated.
Field Testing
During April and May, the system was removed from the Thiokol/Wasatch test
facility and installed on the Thiokol houseboat (Figures 24 and 1). Lake testing
was originally scheduled for late May. However, Bear Lake, selected as the
best site for testing the houseboat system, was unseasonably cold until mid-June.
Photographs of the actual houseboat installation are shown in Figures 25 and 26,
indicating the general location of the treatment system in the rear portion of the
houseboat and a closeup view of the filter-incinerator, holding tank, and control
panel. Figure 27 is a schematic diagram of the electrical system.
In May, the waste treatment system, installed on the houseboat, was charged
with water and chemicals. The system was activated to check all operational
modes, and plant personnel were encouraged to use the system. Two batches
of sewage were processed before shipment to Bear Lake on 13 June.
To field test the system, Thiokol employees with their families and friends were
invited to spend vacations, weekends, and holidays aboard the boat. The boat
was furnished with six beds plus floor space for sleeping bags. Because of the
high turnover of personnel using the boat, a local full-time operator was em-
ployed to pilot the craft, perform routine maintenance, and keep records. Four
documents were used to aid monitoring system performance on board the
houseboat.
1. Toilet Use Record.
2. Houseboat Waste Treatment System Usage
Questionnaire.
3. Houseboat Waste Treatment System Log,
4. Boat Log.
Items (1) and (2) were voluntary data furnished by the users of the system; items
(3) and (4) were log b&oks maintained by the boat operator. Samples were
obtained by each returning party for laboratory analysis.
61
-------
Figure 24. Thiokol Houseboat
-------
09
W
Figure 25. Thiokol Houseboat Waste Treatment System Installation
-------
Figure 26. Houseboat Waste Treatment System Closeup
64
-------
OUSEBOAT
12 V
^
r\
)
Lx
15 V 60 HZ
PUMP (3
SWITCH 1°
RANSFER /*®\
PUMP ( j
1
JL
n
J
/
"1 7 1
1
1
l_
OVE
iTEI\
i-SWI
HI
VOL'
LE
'-
J
]
Ml
1'
^
FUEL SPARK
r SWITCH
-^
BLOWER
.X? SWITCH
BLOWER
OUTLETS
v
« y N p & B
<=rf KRP-3AH
"T\ 1 o) 115V,
J'' J 60 HZ
^^^7 v
i
CONTROL BOX
,H-
1PERATURE 11 BLOWER PLUG
TCH \~S (CONNECTS TO
X^\ j] BLOWER OUTLET
f(\^_J ON CONTROL BOX)
INCINERATOR
BLOWER
GH
FACE
AD
H
^ r
^ -
SPARK
COIL
li FUEL
rfn SPARK
pi PLUG
FUEL
PUMP
^ V BREAKER
*p ^^ POINTS '
^V
X*®^ FUEL PUMP -
I ft / SPARK MOTOR
. .
Figure 27. Houseboat Waste Treatment System Electrical Schematic
65
-------
A summary of the houseboat waste treatment system usage is presented below.
USAGE SUMMARY—HOUSEBOAT WASTE TREATMENT SYSTEM
Month
Jun
Jul
Aug
Sep
Operating
Days
15
18
20
_4
57
Total
Visitors
59
161
201
30
451
Waste Treatment System Uses
Liquid
179
351
358
40
928
Solid
50
68
90
14
222
Total
229
419
448
54
1,150
It is estimated that one-third to one-half of the total visitors were daytime visi-
tors, with the balance spending the night on board the boat.
HTH dosage over the entire test program averaged a little more than 1 Ib per day.
HOUSEBOAT SYSTEM CHLORINE CONSUMPTION
Month HTH Used (Ib)
Jun 7-1/2
Jul 22
Aug
Sep
25
6
60-1/2
The appearance of the recycled liquid varied from colorless to a light straw
color during the test period. Only a few users of the system commented on the
appearance of color of the flushwater, and only one stated that it was objection-
able. Some negative comments were made concerning the poor flushing action
of the toilet and the small holding tank capacity. It appears, however, that
users of the system with previous experience with camping toilets had the least
difficulty and objections.
66
-------
Analyses of the treatment tank liquid are summarized in the following table.
TREATMENT TANK LIQUID ANALYSES
Date
15 Jun 1973
17 Jun 1973
23 Jun 1973
1 Jul 1973
7 Jul 1973
20 Jul 1973
26 Jul 1973
8 Aug 1973
9 Aug 1973
13 Aug 1973
BOD
2,120
3,050
2,500
6,700
4,100
3,450
3,640
2,920
3,170
4,780
~*2
56
247
201
720
550
237
359
161
233
276
Celiform
—
None
None
None
None
None
—
—
—
—
5.8
5.8
5.4
5.9
6.4
6.2
5.6
67
-------
A total of 55 responses to the questionnaire were received during the field test
program.
HOUSEBOAT WASTE TREATMENT SYSTEM
USAGE QUESTIONNAIRE
Yes No
Have you used portable toilets previously ? 30 25
Did you experience difficulty flushing the
houseboat toilet? 11 43
Did you notice objectionable odors issuing
from the toilet (not from the user) ? 18 37
Did you notice objectionable odors or
smoke during the incineration cycle ? 23 26
How would you compare the houseboat Better Same Worse
system to other portable systems ? 34 3 0
(circle one)
If you were a boat owner, how much
would you pay to have a system similar $553 Avg
to the houseboat's installed on your boat? (24 no comments)
A "dry bowl" type toilet causes problems for some people. If toilet paper is
folded and placed in the toilet before use, flushing problems usually are elimi-
nated. In some cases, the objectionable odors issuing from the toilet were from
chlorine, not sewage. The reaction to chlorine is often a matter of personal
preference—some people define a slight chlorine odor as a "clean" smell.
During the times sewage odors were detected, addition of extra chlorine elimi-
nated the problem.
The odors noticed during incineration were apparent only on the top deck of the
houseboat. No odors have been apparent inside the boat. Until the exhaust is up
to about 500° F (first 3 to 4 min), a mild "wet paper" odor is noticeable.
Many of the questionnaire respondents didn't feel qualified to compare the house-
boat system to other portable systems.
The following is a chronological summary of the operating problems encountered
during the field demonstration program.
68
-------
June—During late June, difficulty was experienced starting the incinerator. The
problem was determined to be due to insufficient fuel supply caused by a low level
in the boat's gasoline tanks. A supplemental electric fuel pump was added to sup-
ply fuel to the incinerator at all times. Another boat problem encountered was
loss of the flush pump. The pump was not secured adequately, fell over, and the
water ruined the dc motor.
Fourteen gallons of water were removed from the system on 27 June. There is
some question as to whether the liquid accumulation was due to user input or
from a leaky valve on the toilet.
Through 25 June, the toilet was emptied eight times and solids were incinerated
three times. On 23 June, the burner would not fire due to a ruptured fuel pump.
The toilet was emptied into the filter-incinerator several times before the burner
was placed back into operation. A firing time of 30 min was necessary to burn
off the excessive solids, compared to the 10 min normally required. The failure
of the fuel pump diaphragm had not been experienced before and is thought to be
due to a defective diaphragm.
July—The houseboat waste treatment system received heavy use during July,
interrupted only by a brief period when the houseboat hull was damaged and the
boat took on 1-1/2 ft of water. The partial swamping of the boat was caused by
a depth indicator probe being loosened. The boat was tilted with the port side
(where the waste treatment system is located) being considerably higher than
starboard. Consequently, there was no change in liquid inventory in the waste
treatment system. The boat was out of the water from 12 to 16 July for repairs
and drying the interior.
1 July - The hose between the toilet and the toilet discharge pump apparently
plugged and prevented complete solids removal from the toilet.
2 July - Filtration time was excessive on one day possibly because the preceding
incineration had been inadequate. In general, overnight filtration (by gravity)
had been adequate after the filter cloth was incinerated once. A new cloth seemed
to give slow filtrations.
5 and 9 July - The filter cloth was changed. Inspection on 9 July showed the
filter cloth had been cut with an excessive diameter—the resulting wrinkles
failed rapidly.
6, 8, and 9 July - The problem of solids not transferring from the toilet continued.
On the 9th the accumulated solids in the toilet were flushed out by adding several
5 gal washes of fresh water through the toilet. The solids were pumped to a
separate container. The solids, with about 4 gal of system liquid, were disposed
of on shore. Quantities of lettuce and other foodstuffs were observed floating on
69
-------
top of the discharged solids, indicating the toilet was used as a receptacle for
more than body wastes.
7 July - Additional HTH was added because of odor problems.
A problem was occasionally experienced with ignition of the F/I burner. A fuel
pressure gage was installed before the fuel nozzle which indicated a lack of
gasoline pressure to the burner when ignition would not occur (7/23 and 7/24).
The system inventory increase noted in June was not experienced during July;
conversely on 25 July the tank level had dropped below the filtrate line allowing
smoke to enter the passenger cabin during incineration. One gallon of water was
added to maintain the proper level.
The incineration cycle was monitored on 26 July. A thermocouple in the exhaust
stack gave the following readings:
HOUSEBOAT INCINERATION
Time After Exhaust Temperature
Starting Incineration (°F)
3 min 400
5 min 920
8 min 940
9 min 1, 000
10 min 1,100
Fire off at 10 min
15 560
The incinerator interior was inspected after cooldown; incineration was complete.
During the 26 July test, the 12 vdc line which supplied current to the fuel/spark
assembly contacted the exhaust stack. The resulting short circuit destroyed
much of the 12 v system wiring. The damaged wires were replaced and rerouted
to prevent a recurrence.
August—On several occasions, solids plugged the transfer line from the toilet to
the filter-incinerator. In addition, the flat bottom arrangement of the toilet
70
-------
holding tank caused solids separation, bridging, and dewatering of the sewage.
This condition required stirring and/or additional water to dislodge the solids.
To correct this situation, the toilet was modified by making the toilet seat and
upper section removable. The lower section, or holding tank, was provided
with a dished bottom by laying in a molded epoxy-fiberglass section. Tests were
conducted with simulated sewage, and showed that the new design was effective
in providing positive drainage from the toilet.
On 9 August, the modified toilet was installed on the houseboat. At the same
time the transfer line from the toilet to the filter-incinerator was rerouted to
shorten the distance and eliminate unnecessary bends. A standard Monomatic
macerating transfer pump was also installed in place of the hand-operated dia-
phragm pump in an effort to prevent line plugging.
Several days of operation with these modifications proved disappointing. Although
no problems were encountered in transferring sewage, excessively long drain
times were required in the filter-incinerator to produce a dense mat suitable for
incineration. Believing this to be the result of shredding and particle size
reduction, the macerator pump was removed and the diaphragm pump reinstalled
in the waste treatment system compartment. For the remainder of the test pro-
gram, through September, no further difficulty was reported in either transfer-
ring sewage or draining in the filter-incinerator. Generally, 10 to 15 strokes on
the diaphragm pump was sufficient to transfer a full tank and as little as 23 min
of filtration was observed.
Recurring reports of black smoke and strong odor from the filter-incinerator
exhaust stack prompted a close examination of the system. Suspecting an
improper air/fuel mixture, both the fuel supply system and air blower were dis-
mantled and inspected. It was found that the blower functioned erratically and
delivered less than its rated capacity. Inspection of the operating records indi-
cated that the blower motor had probably been damaged by corrosion and dirt
when one user of the system pumped an excessive quantity of liquid to the filter-
incinerator, allowing it to back up into the blower. Replacing the blower motor
eliminated the black smoke and the odor associated with incomplete combustion
of the sewage solids. The Refrasil filter cloth was also examined and found to
be in excellent condition, requiring no changes for the remainder of the test
program.
In discussions with EPA representatives, the desirability of converting the house-
boat filter-incinerator from a gasoline-fired system to a diesel fuel-fired system
was reviewed. In developing the houseboat system, all applicable standards
established by the U. S. Coast Guard for pleasure craft were complied with.
However, Section 58.01-10 of Marine Engineering Regulations, CG-115, pro-
hibits the use of gasoline-fired devices on commercial vessels. Therefore, in
order to extend the applicability of this waste treatment system to passenger
71
-------
vessels, additional work was needed to demonstrate a diesel fuel-fired filter-
incinerator. This effort could be accomplished without change in contract fund-
ing, but an extension of the period of technical performance was required. A
formal Technical Change Proposal was submitted, requesting this extension, to
the Negotiated Contracts Branch of the EPA. On 14 September, the test program
on the lake was terminated and the houseboat returned to the Wasatch Division
for removal of the waste treatment system.
Fuel Oil Tests
In October, the waste treatment system was removed from the houseboat and
placed in a test facility at the Wasatch Division. The interior of the filter-
incinerator was examined and showed evidence of corrosion and/or oxidation of
the metal walls. The Refrasil filter, however, appeared to be intact with a coat-
ing of ash and charred residue.
Preliminary experiments were carried out to determine if the gasoline-fired
burner could be operated with fuel oil. The existing fuel nozzle, air blower and
ignition system were used with a high pressure fuel oil pump, available from a
standard, domestic oil burner. Ignition was erratic requiring adjustment of the
spark gap relative to the fuel jet. Steady burning was achieved, but poor com-
bustion was evident by a trickle of fuel oil and a spray of oil droplets issuing
from the combustion chamber pipe. It was concluded that this condition resulted
from a poor combination of spray pattern, droplet size, chamber geometry and
air mixing. With gasoline as the fuel, combustion is enhanced by the higher
volatility which vaporizes the fuel and promotes rapid mixing with air. Fuel oil,
on the other hand, requires mechanical action and a high degree of turbulence to
form an aerosol suitable for stable ignition and combustion.
To achieve these conditions, a standard commercial oil burner (Nu-Way,
Model 1002 FM) was mounted on the filter-incinerator with a modified hot gas
inlet manifold.
The existing vertical downfiring gasoline parts were removed and the inlet hot
gas duct blanked off. A new incinerator cover was fabricated from 1/8 in. thick
304 stainless steel. A 7 in. long standard oil burner draft tube was welded to
the outer edge of the cover at a 45° angle to provide a hot gas duct and mounting
flange for the burner (Figures 28 and 29). The unit was later modified with a
12 in. draft tube to provide greater clearance between the incinerator and the
burner/blower.
72
-------
Figure 28. Hot Gas Duct and Mounting Flange, Right Three-Quarter View
73
-------
Figure 29. Hot Gas Duct and Mounting Flange, Left Three-Quarter View
.74
-------
In November, the unit was test fired under the following conditions:
Test No. 1 Test No. 2 Test No. 3
1. Draft tube length (in.)
2. Fuel nozzle (gph/angle)
3. Calculated delivery rate (gph) 0.50
4. Fire ring/flame retention
7
0.50/80W
0.50
Fire ring
12
0. 65/80W
0.65
Flame ret
12
0. 65/80W
0.57
Fire ring
5. Fuel pressure (psi)
6. Busbar
7. Equilibrium temp (°F)
8. Firing time (min)
9. Remarks
100
Clamped
15
Slight roar;
leaks fumes
100 100
Clamped Soldered
1, 400
5 30
Cover and
discharge
flue hot;
slight roar;
no leakage
of fumes.
Test No. 3 showed excellent results and indicates only minor changes are
required to achieve the desired 1,200° F incinerator temperature. This can be
accomplished with a lower fuel rate by either throttling fuel pressure (Figure 30),
or reducing the fuel nozzle orifice size. Reducing the orifice increases the risk
of plugging the nozzle, as was encountered in Test No. 1. In all cases, no
ignition failures were encountered during the tests. However, it is recom-
mended that filter-incinerator exhaust stack diameter be increased from 3 in.
to 5 in. to decrease back pressure and assure flame stability.
No tests were carried out with filtered sludge in the incinerator because of a
lack of a suitable sewage source during the test period.
75
-------
0,65 GPH NOZZLE
•- 0.60 GPH NOZZLE
0.50 GPH NOZZLE
0.80
~ 0.70
H
H
S
w
u
0
o
1-1
w
P
0.40
80 100 120 140
FUEL PUMP PRESSURE (PSIG)
Figure 30. Fuel Oil Delivery Rate vs Fuel Pump Pressure
for 0.50, 0.60, and 0.65 gph Nozzles
76
-------
SECTION VI
SYSTEM ECONOMICS
A study was made to determine the production cost of the system tested on the
houseboat. The estimate was based on a marine recirculating system with low
flow (1 qt) toilet and houseboat type filter-incinerator capable of 15 gpd or
60 flushes/day. The estimated selling price of each unit, assuming 20 units per
year production rate, is $2,760. This price is considerably higher than the $553
average that the users of the houseboat indicated that they would be willing to
pay. The selling price, however, is largely dependent upon volume of production,
and a 50% price reduction could readily be achieved in mass production.
Installation costs could vary considerably, depending on the craft design. There
are a number of potential installation locations on most vessels. The installation
location decision would be based not only on costs, but also on simplifying oper-
ation and preserving the esthetics of the entire vessel. Tabulated below is an
estimate of the installation costs based on placing the system in a closet adjacent
to the head, with minimum piping runs and incinerator exhaust ducting.
COST OF SYSTEM INSTALLATION
Item Cost
Boat modification labor $21.00
Boat modification material 10.00
Piping installation 14.00
System assembly checkout 14.00
Electrical labor 7.00
Electrical material 5.00
Total $71.00
Based on labor at $7. OOAr
77
-------
The following table summarizes the operating costs of the system.
"COST OF SYSTEM OPERATION
Item Cost ($)
Electrical power at $0.05/kwh
Fuel pump/spark motor 0.025 kwh
Blower 0.126 kwh
Flush pump 0.002 kwh
Exhaust fan 0.104 kwh
0.257 kwh 0.02
Gasoline (1/2 gal) 0.30
HTH (1 Ib) 1.00
Filter media 0.05
TOTAL 1.37
*Based on one cycle of 20 to 30 toilet uses or transfer of one 6 gal batch to
the filter-incinerator.
78
-------
SECTION VII
COAST GUARD REVIEW
A portion of the work that was to be included in Phase I of the "Devices for On-
board Treatment of Wastes from Vessels" contract was to supply sufficient in-
formation to the U. S. Coast Guard to enable them to issue a written opinion.
Communications began in August of 1971 and a preliminary technical package
was sent to Commander Albert Stirling at the Washington, D. C., office.
On 24 Mar 1972, Chief William M. Robinson, who was with the local Coast
Guard, visited the Wasatch Division and viewed the houseboat prototype. Chief
Robinson indicated the use of gasoline as a fuel was acceptable on a privately
operated boat, but that diesel fuel would be required for a commercial vessel.
On 13 Aug 1972, a complete waste treatment system design package was sent to
Commander Stirling with a duplicate directed to Mr. L. McCarthy of the EPA.
On 24 Aug 1972, Commander Sipes informed us he had received the design
package, that he was handling duties previously performed by Commander
Stirling, and that the package was sent to the Regulation Drafting Section for
review.
On 28 Aug 1972, Commander Schumacher of the Regulation Drafting Section
informed us the review could take up to 1 month.
On 4 Oct 1972, Richard Landin of the Marine Engineering Branch informed us
it would be several weeks before an evaluation could be made of our system.
In a letter dated 27 Oct 1972, Captain M. B. Lemly, Chief, Merchant Marine
Technical Division, advised Thiokol Corporation that the sewage treatment
meets applicable Coast Guard safety requirements with the exception of the
gasoline preheater in the incineration chamber. This letter confirmed that
gasoline-fired devices were prohibited on commercial passenger vessels.
79
-------
APPENDIX I
SUMMARY OF
FILTER-INCINERATOR TESTS
80
-------
00
SUMMARY OF FILTER-INCINERATOR TESTS
Results
Test
Test Configuration
Thiokol IH It D Tests. Single Clement
GF-1
GF-2
OF -3
GF-4
GF-S
GF-6
GF-7
GF-8
GF-9
GF-10
GF-11
GF-12
GF-13
GF-14
GF-15
GF-16
GF-17
GF-18
GF-19
GF-20
GF-21
GF-22
GF-23
GF-24
5 Polypropylene Bag
C1554-48 Refrasil, 1 Layer
C1554-48 Refrasil, 1 Layer
C 100-4 8 Refrasil, 1 Layer
C 100-48 Refrasil, 1 Layer
C 100-48 Refrasil, 1 Layer
C 100-48 Refrasil, 1 Layer
C100-48 Refrasil, 1 Layer
C 100-48 Refrasil, 1 Layer
C 100-48 Refrasil, Z Layers
C 100-4 8 Refrasil, 2 Layers
C 100-48 Refrasil, 2 Layers
C100-48 Refrasil, 2 Layers
C 100-48 Refrasil, 2 Layers
C1554-48 Refrasil. 2 Layers
C 1554-48 Refrasil. 2 Layers
C 1554-48 Refrasil. 2 Layers
C 1554-48 Refrasil. 2 Layers
C 1554-48 Refrasil. 2 Layers
C1554-48 Refrasil. 2 Layers
C 1554-48 Refrasil. 2 Layers
C 1554 -48 Refrasil, 2 Layers
C1554-48 Refrasil. 2 Layers
C 1554-48 Refrasil. 2 Layers
C 1554-48 Refrasil, 2 Layers
SS In SS Out
(mg/1) (mg/1)
425 60
284 120
284 137
364 110
364 118
212 97
212 112
435 219
435 239
675 60
675 90
—
352 108
352 90
445 153
780 103
126 84
126 55
126 67
71 80
71 69
(water)
(water)
(water)
(water)
Gal /Sq Ft
33
8
6
10
10
5
7.5
7.5
8
8
7.5
6
7
5.8
10.4
30
12
35
13
10
13
20
20
20
20
Fill
Time (min)
80
12
9
10
11.5
5
8
7.5
9
3
7
5.5
5
8
5
25.5
8
34
9
8.3
9.2
3.3
3.3
3.3
3.3
No. of
Cycles
1
1
2
1
2
3
4
5
6
1
2
3
4
5
1
2
3
4
5
6
7
8
9
10
11
Remarks
Holes cut in cloth by clamps
Cloth In excellent condition
Cloth in excellent condition
-------
SUMMARY OF FILTER-INCINERATOR TESTS
-------
SUMMARY OF FILTER-INCINERATOR TESTS (Cont)
Results
Test
SS In SS Out Fill
Test Configuration (mg/1) (mg/1) Gal /Sq Ft Time (min)
Coast Guard, Single Element (Cont)
PPF-14
PPF-15
PPF-16
PPF-17
PPF-18
PPF-19
00
W PPF-20
PPF-21
PPF-22
Fused A12O3 Cylinder 330 148 18.5 15
FAO No. 54, 3 in. OD, 2 in. ID, 12 in. L
Fused A12O3 Cylinder 588 163 16.5 15
FAO No. 54, 3 in. OD, 2 in. ID, 12 in. L
Fused A12O Cylinder 588 118 29.5 15
FAO No. 54, 3 in. OD, 2 in. ID, 12 in. L
Fused Al O Cylinder 177 148 57 20
FAO No. 54, 3 in. OD, 2 in. ID, 12 in. L
Fused A12O3 Cylinder 177 128 25 9
FAO No. 54, 3 in. OD. 2 in. ID, 12 in. L
Fused A12O3 Cylinder 177 101 25 7
FAO No. 54, 3 in. OD, 2 in. ID, 12 in. L
Fused A12O3 Cylinder 403 186 25 9
FAO No. 54, 3 in. OD, 2 in. ID, 12 in. L
Fused A12O3 Cylinder 403 184 6.5 4.5
FAO No. 54, 3 in. OD, 2 in. ID, 12 in. L
Fused A12O3 Cylinder 406 149 7.5 5
FAO No. 80, 3 in. OD, 2 in. ID, 12 in. L
No. of
Cycles
1
1
2
3
4
5
6
7
1
PPF-23 Fused AlgOg Cylinder
FAO No. 80, 3 in. OD, 2 in. ID, 12 in. L
406
206
3.5
7.5
Remarks
Filter test only, H2O,
backflush not effective
Salted sewage. 3% salt, incineration
test conducted
Salted sewage, 3% salt. Filter back-
flushed with H2O three times during
filtration. Incineration test conducted
3% salt, A P = 4 psi
3% salt, A P = 2 psi
3% salt, AP = 2 psi
3% salt, A P = 2 psi
3% salt, A P = 5-10 psi. Filter appeared
plugged. Filter was cracked
3% salt. Backwash ineffective for
throughput increase. Slow heatup and
cooldown to avoid thermal shock. Element
cracked. Conclusion: can't use fused
Al-O, elements. Will try SiC elements
£i O
3% salt. Backwash ineffective for
throughput increase. Slow heatup and
cooldown to avoid thermal shock. Element
cracked. Conclusion: cant use fused
A12O3 elements. Will try SiC elements
-------
SUMMARY OF FILTER-INCINERATOR TESTS (Cont)
Results
Test
Test Configuration
Coast Guard, Single Element (Cont)
GF-43 4 in. D x 1/2 in. Thick Fiberfrax Long Staple
Coarse Felt
GF-44 C1554-48 Refrasil, 1 Ply
GF-45 B 2-1/2 Ref Tube, 4 in. D Leaf Test. 1 Ply
GF-46 B-1570 Refrasil Fabbat
OF-47 C1554-48 Refrasil, 3 Ply
GF-48 C1554-48 Refrasil, 3 Ply
GF-50 FE-1021-X6 Fluid Dynamics Cylinder
GF-51 B 2-1/2 Ref Tube, 2-3/4 in. D x 12 In. L, 1 Ply
GF-52 B 2-1/2 Ref Tube, 2-3/4 in. D x 12 in. L, 1 Ply
00 GF-53 B 2-1/2 Ref Tube, 2-3/4 in. D x 12 in. L, 1 Ply
GF-54 B 2-1/2 Ref Tube, 2-3/4 in. D x 12 in. L, 1 Ply
GF-55 B 2-1/2 Ref Tube, 2-3/4 in. D x 12 in. L, 1 Ply
GF-56 B 2-1/2 Ref Tube, 2-3/4 in. D x 12 in. L, 1 Ply
GF-57 B 2-1/2 Ref Tube, 2-3/4 in. D x 12 in. L. 1 Ply
GF-58 FE-1021-X6 Fluid Dynamics Cylinder
GF-59 C100-48, 2 Ply Refrasil
GF-60 B 2-1/2 Refrasil, 2 Ply
GF-61 B 2-1/2 Refrasil, 2 Ply
GF-62 B 2-1/2 Refrasil, 2 Ply
GF-63 B 2-1/2 Refrasil, 2 Ply
SSIn
(mg/1)
760
~
760
760
760
526
290
170
170
660
660
660
206
206
188
295
718
718
SS Out
{mg/lL
150
—
156
176
70
80
136
85
76
193
162
148
67
150
214
84
120
99
Gal /
Sq Ft
10
4
5
5
6
6
3.3
28
28
11
11
28
6.3
5.6
1.7
4
5.5
10
Fill
Time
(min)
—
2
3
1
10
8
2.4
9
13.3
6.6
4
8
8.3
8.3
3.3
4
5
15
No. of
Cycles
1
1
1
1
1
2
1
1
2
3
4
5
6
7
2
1
1
2
Filt
Ap
ipsi}.
10
—
5
5
6
7
8
5
5
5
5
5
5
4
10
7-9
8
10
Salt
Used
—
—
—
—
__
—
—
—
—
—
—
—
—
—
—
Sea
Sea
Sea
718
718
104
72
10 10
8.3 10
3
4
8 Sea
£ Sea
Remarks
Filtration only. 4 in. diameter test leaf
Run made simply to obtain filtrate sample
Filtration test only
Filter test, 4 in. diameter test leaf
15 micron porosity, 2 backwashes
1 Ib HTH per 50 gal. sewage (Floe 3678 SS)
1 Ib HTH per 50 gal. sewage (Floe 3678 SS)
15 micron porosity, 1 backwash
Cloth cemented to support with Sauereisen
No. 65. Cloth broke adjacent to cement
during incineration. Filtered Hydrasieve
underflow. Raw sewage SS = 720
Hydrasieve underflow. 1,100'F gas inlet.
Hydrasieve underflow. 1,100*F gas inlet.
Static plus backwash
Hydrasieve underflow. 1,200*F gas inlet.
1 backwash
Hydrasieve underflow. 1,200°F gas inlet.
1 backwash
-------
SUMMARY OF FILTER-INCINERATOR TESTS (Cont)
Test
Test Configuration
00
Coast Guard, Single Element (Cont)
GF-64 B 2-1/2 Refrasil, 2 Ply
GF-65 B 2-1/2 Refrasil, 2 Ply
GF-66 B 2-1/2 Refrasil, 2 Ply
GF-67 B 2-1/2 Refrasil, 2 Ply
GF-68 L-70-652 Novatex, 24 oz, 2 Ply
GF-69 L-70-652 Novatex, 24 oz, 2 Ply
GF-70 L-70-652 Novatex, 24 oz, 2 Ply
GF-71 L-70-652 Novatex, 24 oz, 2 Ply
GF-72 L-70-652 Novatex, 24 oz, 2 Ply
GF-73 L-70-652 Novatex, 24 oz, 2 Ply
GF-74 L-70-652 Novatex, 24 oz, 2 Ply
GF-75 L-70-652 Novatex, 24 oz, 2 Ply
GF-76 L-70-652 Novatex, 24 oz, 2 Ply
GF-77 L-70-652 Novatex, 24 oz, 2 Ply
GF-78 L-70-652 Novatex, 24 oz, 2 Ply
GF-79 L-70-652 Novatex, 24 oz, 2 Ply
GF-80 FAO No. 50, 3 in. OD x 2 in. ID x 12 in. L
GF-81 FAO No. 50, 3 in. OD x 2 in. ID x 12 in. L
GF-82 FAO No. 50, 3 in. OD x 2 in. ID x 12 in. L
Results
SS In
(mg/1)
718
~
190
190
262
262
262
245
305
305
305
305
490
490
490
272
190
190
190
SS Out
(mg/1)
61
111
61
69
146
86
140
212
89
87
99
56
107
136
113
196
138
~
132
Gal /
SqFt
7.6
15.3
12.5
34*
25*
25*
40*
38*
18
27
20
14
28
20
30*
16.5
20.7
27.4
19.8
Filt
Time
(min)
10
10
16.7
21.7
16.7
10
16.2
15
20
10
15.7
16.7
18.4
16.7
12.5
5.3
6
17.8
11.6
No. of
Cycles
5
6
7
8
1
2
3
4
5
6
7
8
9
10
11
12
1
2
3
Filt
AP
(psi)
8
8
8
8
8
5-9
5
5
4-10
8-10
10
10
10
10
10
10
7
8
8
Salt
Used
Sea
Sea
Sea
Sea
Sea
Sea
Sea
Sea
NaCl
NaCl
NaCl
NaCl
NaCl
NaCl
NaCl
NaCl
—
--
—
Remarks
Hydrasieve underflow.
1 backwash
Hydrasieve underflow.
No backwash
Hydrasieve underflow.
2 backwashes
Hydrasieve underflow.
1 backwash
Hydrasieve underflow.
1 backwash
Hydrasieve underflow.
No backwash
Hydrasieve underflow.
No backwash
Hydrasieve underflow.
No backwash
Raw sewage. 1,05 0°F
Raw sewage. 1,100°F
Raw sewage. 1,100°F
Raw sewage. 1,100°F
Raw sewage. 1,15 0°F
Raw sewage. 1,125°F
Raw sewage. 1,125°F
Raw sewage. 1,100°F
Raw sewage. 1,175°F
Raw sewage. 1,175°F
Raw sewage. 1,175°F
1,200°F gas inlet.
1,200°F gas inlet.
1,200°F gas inlet.
1,200°F gas inlet.
1,000°F gas inlet.
1,000°F gas inlet.
1,050"F gas inlet.
1,150°F gas inlet.
gas inlet
gas inlet
gas inlet
gas inlet
gas inlet. 3% salt
gas inlet. 3% salt
gas inlet. 3% salt
gas inlet. 3% salt
gas inlet.
gas inlet.
gas inlet.
*Ran out of sewage. Filter not plugged.
-------
SUMMARY OF FILTER-INCINERATOR TESTS (Cont)
Results
Test
Test Configuration
EPA Houseboat, Multiple Cycle Tests
GF-83 Refrasil B 2-1/2 Braid, 2 Ply
GF-84 Refrasil B 2-1/2 Braid. 2 Ply
GF-85 Refrasil B 2-1/2 Braid. 2 Ply
GF-86 Refrasil B 2-1/2 Braid, 2 Ply
GF-87 Refrasil B 2-1/2 Braid, 2 Ply
GF-88 Refrasil B 2-1/2 Braid. 2 Ply
GF-89 Refrasil B 2-1/2 Braid, 2 Ply
GF-90 Refrasil B 2-1/2 Braid, 2 Ply
GF-91 Refrasil B 2-1/2 Braid. 2 Ply
g> GF-92 Refrasil B 2-1/2 Braid, 2 Ply
GF-93 Refrasil B 2-1/2 Braid. 2 Ply
GF-94 Refrasil B 2-1/2 Braid. 2 Ply
GF-95 Refrasil B 2-1/2 Braid, 2 Ply
GF-96 Refrasil B 2-1/2 Braid, 2 Ply
GF-97 Refrasil B 2-1/2 Braid. 2 Ply
GF-98 Refrasil B 2-1/2 Braid, 2 Ply
GF-99 Refrasil B 2-1/2 Braid, 2 Ply
GF-100 Refrasil B 2-1/2 Braid. 2 Ply
GF-101 Refrasil B 2-1/2 Braid, 2 Ply
GF-102 Refrasil B 2-1/2 Braid, 2 Ply
GF-103 Refrasil B 2-1/2 Braid. 2 Ply
GF-104 Refrasil B 2-1/2 Braid, 2 Ply
GF-105 Refrasil B 2-1/2 Braid, 2 Ply
GF-106 Refrasil B 2-1/2 Braid, 2 Ply
GF-107 Refrasil B 2-1/2 Braid, 2 Ply
SS In
(mg/1)
878
878
878
270
270
270
270
270
460
460
460
460
460
460
460
485
485
485
485 .
485
485
485
485
229
229
SS Out
(mg/1)
38
45
58
36
13
32
286
42
4
12
2.5
52
302
32
30
168
46
22
18
12
17
29
16
10
8
Gal /
SqFt
6.2
4.9
4.9
5.2
5.9
6.2
5.9
5.9
4.2
4.9
4.6
14.6
13.9
13.2
12.9
3.1
3.5
3.8
3.7
3.5
3.5
4.2
3.5
4.2
3.1
Fill
Time
(min)
5.8
6.7
6.7
8.3
10
10
10
10
8.3
8.3
8.3
11.7
11.7
11.7
11.7
10.4
10.8
13.3
10
10
10
10
10
11.7
10
No. of
Cycles
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
Filt
<-P
(psi)
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
8
~
~
8
~
8
End-of-Run
Gas Temp
(*F)
1,040
1,000
1,020
1,075
1,075
1,080
1,080
990
1,000
1,100
1,080
1,080
1,080
1,075
1,080
1,080
1,080
1,050
1,050
1,050
1.050
1,050
1,060
1,100
1,090
Remarks
-------
SUMMARY OF FILTER-INCINERATOR TESTS (Cont)
Results
00
Test
Test Configuration
EPA Houseboat, Multiple Cycle Tests
GF-108 Refrasil B 2-1/2 Braid. 2 Ply
GF-109 Refrasil B 2-1/2 Braid. 2 Ply
GF-110 Refrasil B 2-1/2 Braid, 2 Ply
GF-111 Refrasil B 2-1/2 Braid. 2 Ply
GF-112 Refrasil B 2-1/2 Braid. 2 Ply
GF-113 Refrasil B 2-1/2 Braid, 2 Ply
GF-114 Refrasil B 2-1/2 Braid, 2 Ply
GF-115 Refrasil B 2-1/2 Braid. 2 Ply
GF-116 Refrasil B 2-1/2 Braid, 2 Ply
GF-117 Refrasil B 2-1/2 Braid, 2 Ply
GF-118 Refrasll B 2-1/2 Braid. 2 Ply
GF-119 Refrasil B 2-1/2 Braid, 2 Ply
GF-120 Refrasil B 2-1/2 Braid, 2 Ply
GF-121 Refrasil B 2-1/2 Braid, 2 Ply
GF-122 Refrasil B 2-1/2 Braid, 2 Ply
GF-123 WRP-X-AQ Felt
GF-124 Stainless Steel Cloth (Karma yarn 1/1 basket
weave)
GF-125 Zirconia Cloth
SS In
(mg/1)
229
229
229
229
229
282
282
282
282
282
282
282
282
282
282
SS Out
(mg/t)
15
16
16
20
22
8.5
8
176
26
68
45
26
33
10
4
Gal /
Sq Ft
4.2
5.2
5.2
4.2
4.5
3.8
5.5
4.5
4.9
4.2
4.5
3.8
4.2
3.8
3.1
Flit
Time
(min)
10.8
10.8
10.8
10.8
10.8
10
10
10
10
10
10
10
10
10
10
No. of
Cycles
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
Fill
-P
(psi)
8
8
8
8
8
10
10
10
10
10
10
~
~
10
8
End-of-Run
Gas Temp
fF) Remarks
1,100
--
1,060
1.000
1,020
1,050
1.050
1,050
1.055
1.055
1,055
1.050
1.050
1.100
1.100
S1O2-A12O3 refractory felt, second
cycle. No test, filter failed
Filter ineffective
Filter ineffective
-------
Test
Test Configuration
EPA Houseboat, Multiple Cycle Tests
GF-126 L-70-652 Novatex, 24 oz, 2 Ply
GF-127 L-70-652 Novatex, 24 oz, 2 Ply
GF-128 L-70-652 Novatex. 24 oz, 2 Ply
GF-129 L-70-652 Novatex. 24 oz, 2 Ply
GF-130 L-70-652 Novatex, 24 oz. 2 Ply
GF-131 L-70-652 Novatex, 24 oz, 2 Ply
GF-132 L-70-652 Novatex, 24 oz, 2 Ply
SUMMARY OF FILTER-INCINERATOR TESTS (Cont)
Results
SSIn
(mg/1)
300
300
300
300
300
300
300
SSOut
(mg/1)
89
196
98
71
—
32
41
Gal /
Sq Ft
9
12.5
5
5.8
4
3.5
3.3
Filt
Time
(min)
10
5.8
8.3
10
6.7
10
8.3
No. of
Cycles
1
2
3
4
5
6
7
Filt
AP
(pst)
10
10
10
10
8
8
8
End -of -Bun
Gas Temp
fF)
1,050
1,040
1,050
1,050
1,050
1,040
1,040
Remarks
00
03
-------
APPENDIX II
IDENTIFICATION OF ORGANIC COMPOUNDS
IN A CLOSED-LOOP HYPOCHLORITE
WASTEWATER TREATMENT SYSTEM
by
V. Dean Adams
E. Joe Middlebrooks
Utah Water Research Laboratory
College of Engineering
Utah State University
Logan, Utah 84322
May, 1973
89
-------
TABLE OF CONTENTS
Page
INTRODUCTION 92
DESCRIPTION OF PROCESS 92
PROCEDURES 94
RESULTS AND DISCUSSION 94
Carbon Analyses 94
Ether and Chloroform Extractions 96
Alcoholic Silver Nitrate Reaction 103
Deuterium Exchange Reaction 104
CONCLUSIONS 105
RECOMMENDATIONS FOR ADDITIONAL STUDIES ... 110
REFERENCES 113
ADDENDUM to Appendix II 114
90
-------
LIST OF FIGURES
Figure Page
1 Small Pleasure Boat System Schematic 93
2 Infrared Spectrum T-UWRL No. 1 97
3 Nuclear Magnetic Resonance Spectrum T-UWRL No. 1 . 98
4 Nuclear Magnetic Resonance Spectrum T-UWRL No. 2 . 101
5 Nuclear Magnetic Resonance Spectrum T-UWRL No. 3 . 102
6 Nuclear Magnetic Resonance Spectrum T-UWRL No. 3a . 106
7 Nuclear Magnetic Resonance Spectrum T-UWRL
No. 3a + DO 107
Lt
8 Nuclear Magnetic Resonance Spectrum T-UWRL No. 6 • 108
9 Nuclear Magnetic Resonance Spectrum T-UWRL
No. 6 + HO 109
ft
LIST OF TABLES
Table Page
1 Distribution of carbon concentration in the
treatment facility effluent 95
2 Identification of various peaks in the infrared
and nuclear magnetic resonance spectra of
Figures 2 and 3 99
3 Approach to identifying components of highly
chlorinated wastewater treatment plant effluents .... 112
91
-------
INTRODUCTION
The most significant problem occurring in a recycled effluent
process utilizing physical treatment in conjunction with a catalyzed
hypochlorite generating wastewater treatment process is the accumula-
tion of organic compounds in the recycled effluent. Although these
effluents are discharged to the environment infrequently, care must be
exercised to ensure that unexpected consequences are not produced.
However, the greatest concern for these accumulated compounds
results in the reuse of the effluent for flushing operations. If the
chlorine residual were to be exhausted before the effluent were
returned to the treatment plant, biological activity and discoloration
could occur. The discoloration is of aesthetic concern and most users
of the process would insist upon an odorless and clear flush water.
To prevent the recurrence of this type of difficulty in the pro-
cess, it was first necessary to identify these compounds. The results
presented herein describe a preliminary study utilizing advanced
chemical detection techniques to identify the compounds that accumu-
late in the recycled water.
DESCRIPTION OF PROCESS
Figure 1 shows a flow diagram of the physical-chemical process
designed for use aboard recreational vehicles or in isolated areas
where water is in short supply (1). The process package is compact,
92
-------
FUEL
PUMP
VO
U)
Figure 1. Small Pleasure Boat System Schematic
-------
easily operated, requires little maintenance or operation, and can be
operated seasonally without any variation in efficiency.
PROCEDURES
The sample used in the following evaluation was collected from a
prototype unit treating wastewater produced by five people, and the unit
had been operating for 40 days at the time the sample was collected.
The waste system contained approximately 30 gallons of water.
Additional detailed information about the operation of the process is
contained in two letters from Thiokol Chemical Corporation personnel
presented in the Appendix.
Direct extraction and extractions of concentrates of the treatment
process effluent were performed with redistilled ether and chloroform
using continuous extraction equipment. The products of these extrac-
tions were examined by nuclear magnetic resonance (NMR), infrared
absorption (IR), the addition of alcoholic silver nitrate, and total and
inorganic carbon analyses.
RESULTS AND DISCUSSION
Carbon Analyses
To establish that organic carbon compounds did exist in the pro-
cess effluent, total and inorganic carbon concentrations were performed.
As shown in Table 1, over 60 percent of the total carbon present in the
sample was in the organic form.
94
-------
Table 1
Distribution of Carbon Concentration in the
Treatment Facility Effluent
_ ... , Concentration
Constituent .,
mg/1
Total Carbon 655
Inorganic Carbon 245
Organic Carbon 410
95
-------
Ether and Chloroform Extractions
The first extraction was carried out for three days on approxi-
mately 500 ml of the treatment facility effluent using redistilled ether
and continuous extraction equipment. The ether extract was then dried
over magnesium sulphate, filtered and concentrated. A yellow-orange
viscous liquid remained. Infrared (IR) and nuclear magnetic resonance
(NMR) spectra were obtained for this liquid. The results are shown in
Figures 2 and 3, respectively. Table 2 shows a summary of the inter-
pretation of the spectra presented in Figures 2 and 3. The isolated
liquid appears to be a complex mixture. The IR spectrum indicates
the presence of -OH or -NH and -C = 0 functional groups. It also has
strong absorption in the area for aliphatic -CH bonds.
The most intense signals given in the NMR spectrum occurred
at 5 = 0. 88 to 6 = 1. 63 and indicates that the major portion of the mix-
ture was of an aliphatic -CH nature. Peaks from 6 2. 10 to 6 4. 88
indicate substituted aliphatic type protons. The intensity of these
peaks indicates that the substituted proton was present to a much
lesser extent that the aliphatic -CH species. There was also an indi-
cation of some aromatic or-OH protons at 5 7.12.
Two additional extractions were made on the houseboat effluent.
Approximately 2000 ml of effluent were concentrated to - 190 ml using
a roto flash-evaporator. Care was taken to keep the temperature
under 35 C. Upon concentration to this point some solid materials
(crystals, etc.) were observed. This concentrate solution was then
96
-------
IR— T-UWRL*!
FIG. 2
Figure 2. Infared Spectrum T-UWRL No. 1
-------
NO DOWN FIELD ABSORPTION (20OCPS)
AROMATIC OR HYDROXYL
PROTON CHEMICAL
SHIFT
ALIPHATIC + ALIPHATlC,8~SUBSTITUTED
ALIPHATIC, ec SUBSTITUTED PROTON
CHEMICAL SHIFT 1*. HC-X WHERE X
CHEMICAL SHIFTS I* ALIPHATIC-»CH,-
ALIPHATIC./? SUBST.-*«HC-C-X ~3
WHERE X COULD BE CJt, BP.OH, N0a, ET
COULD BE —•> Bt,C/,N02,OH. OR. SH.SR. ETC
Figure 3. Nuclear Magnetic Resonance Spectrum T-UWRL No. 1
-------
Table 2
Identification of Various Peaks in the Infrared and
Nuclear Magnetic Resonance Spectra
of Figures 2 and 3
Infrared Spectrum (Figure 2)
3250 cm" | Broad OH or NH STR
nil -
1680 cm C = 0 STR
1420 cm^
1350 cm *
Nuclear Magnetic Resonance Spectrum (Figure 3)
5 = 0.88
0.95
1 14
* , Aliphatic type proton chemical shifts and some
' with electronegative P-substituents
Jl • 4 M
1.53
1.63
6 = 2.10
2.20
2 30
Aliphatic type proton chemical shifts with
•* a-substituents. Some possibility of
' Jt olefinic or acteylenic but not likely
' _ . under the conditions used
2. 76
2.84
2.92
3.00
3.45 ... ,
. multiple
4.45
4.88
5 = 7.12 Aromatic or-OH type proton chemical shift
99
-------
extracted with double-distilled chloroform for five days. The chloro-
form was then dried and evaporated leaving - 0. 1 g of a yellow-orange
liquid. An NMR of this material was taken, but the spectrum was very
poorly resolved (Figure 4).
Another 2000 ml of effluent were concentrated to - 200 ml using
the roto flash-evaporator. This concentrate was then extracted with
distilled ether, and approximately 0. 35 g of a yellow-orange liquid was
obtained. The NMR spectrum (Figure 5) of this material was very
similar to the one shown in Figure 3. The main differences occurred
in the distribution and magnitude of some of the peaks. In the aliphatic
region of & 1. 0 - 5 2. 0 the peak intensities showed a decrease; whereas
in the region of 6 2. 1 - 5 4. 0 there was an increase. Attempts to
separate these aliphatic mixtures using thin-layer chromatography
were unsuccessful.
Of the two distilled solvents used for extraction of the treated
effluent, ether was found to be more efficient than chloroform. Con-
centration of the effluent apparently resulted in the loss of some
volatile organics. Also, the possibility exists that the character of
the constituents in the wastewater was modified by the procedures used
to concentrate the samples. However, only accepted procedures were
employed.
Complete extraction of the organic material is impossible
because of inadequate solvent partition, solvent polarity, etc. To be
sure that the best solvent for extracting the organics from the
100
-------
I
5.0
30_
*
I (I)
T"
400
NMR-T-UWRL
RESOLUTION NOT GOOD
BUT IN GENERAL SHOWS
SAME GENERAL PATTERN AS
THE OTHER SPECTRA.
Figure 4. Nuclear Magnetic Resonance Spectrum T-UWRL No. 2
-------
AROMATIC OR
ff HYOROXrL PROTON
CHEMICAL SHIFTS
300
N MR- T-UWRL *3
I (I)
TMS
ALIPHATIC, a SUBSTITUTED PROTON ALIPHATIC + ALIPHATIC ff SUBSTITUTED^
CHEMICAL SHIFT it. H.C-X WHERE X PROTON CHEMICAL SHIFTS ie ALIPHATIC
COULD BE-»-Br ,C/. NO2,OH, OR, SH, SR, ETC. •*>CJ13~ i -CHg-; -C H- ALIPHATIC.rf SUBST.
| - —"-HC-C-X WHERE X COULD BE C,£, Br,OH, NO,,, ETC
T
T
Figure 5. Nuclear Magnetic Resonance Spectrum T-UWRL No. 3
-------
chlorinated effluent has been employed, it will require that many others
be evaluated. However, ether does appear to yield good reproducible
data that should give a good approximation of the types of compounds
present in the effluent.
After the aqueous effluent material had been extracted, it was
left out in the laboratory and growth appeared. This indicates that the
compounds remaining after ether extraction are readily biodegradable
and supports the results obtained by Middlebrooks (2) using a similarly
chlorinated sewage sample.
Under the conditions used for treatment of the sewage effluent,
the majority of the excreted nitrogen compounds (urea, amino acids,
etc.) should be oxidized to lesser components.
Chlorination of most organic species should recur in the treat-
ment process employed. Some free radical chlorination would proceed
on alkane species present in the effluent and alkene type compounds
would readily be converted by chlorine to saturated compounds which
contain two atoms of chlorine attached to adjacent carbons.
Alcoholic Silver Nitrate Reaction
In many cases, the presence of halogen in an organic compound
can be detected without a sodium fusion reaction. Organic halides
react with alcoholic silver nitrate by the reaction below:
R:X + Ag -* R+ + Ag*X"
103
-------
The ether extract (yellow- orange viscous material) reacted with
silver nitrate to give a white precipitate which upon standing turned
grayish-black. The precipitate was not soluble in dilute nitric acid.
Halogen was thus indicated.
Deuterium Exchange Reaction
A comparison of the downfield signal in the NMR spectra shows
a slight variation between the different spectra which is unusual for
aromatic protons. NMR adsorption by a hydroxyl or carboxylic acid
proton (-OH, -Cv^rr) ordinarily gives rise to a singlet in the NMR
spectrum: its signal is not split by nearby protons, nor does it split
their signals. Proton exchange between two molecules which contain
hydroxyl or carboxylic acid protons is so fast that the proton - now in
R DH*
one molecule, and in the next instant in another - cannot "see" nearby
protons in their various combinations of spin alignments, but in a
singlet average alignment.
This particular characteristic can then be used to further identify
hydroxyl or carboxylic proton containing species by a deuterium
exchange reaction. Because a deuteron has a much smaller magnetic
moment than a proton, it absorbs at a much higher field, and does not
give a signal in the proton NMR spectrum. As a result, the replace-
ment of a proton by a deuteron removes from an NMR spectrum the
104
-------
signal from that proton as if there were no hydrogen at all at that
particular position in the molecule.
A deuterium exchange reaction was performed and indeed
(Figures 6 and 7), the downfield peak (6 7. Z) disappeared. The remain-
ing part of the spectrum remains relatively unchanged. Thus, the peak
seen downfield (5 7-8) was not attributable to aromatic protons, but
rather to hydroxyl or carboxylic acid protons (-OH, -CC-jr,)*
Ordinarily, the signal produced by a hydroxyl proton will occur
in the range of 6 1. 0 to 5 5. 5, and a signal from a carboxylic acid pro-
ton in the range of 5 10. 5 to 6 12. 0. A hydrated carboxylic acid proton
under certain conditions can be seen in the area of 5 6. 5-8. 5, a
position intermediate between a water proton signal and carboxylic
acid proton signal. Figure 8 shows the spectrum for a long chain
fatty acid with a carboxylic acid proton signal at 6 12. 3. Figure 9
shows the same sample hydrated with the intermediate signal appearing
at 5 7.7.
CONCLUSIONS
Present evidence suggests that the material isolated by extrac-
tion techniques is a complex mixture which consists mainly of saturated
chlorinated fatty acids. The presence of lipids in feces provides a
significant quantity of material that would result in saturated chlori-
nated fatty acids. Lipids are in feces because dietary lipids are not
quantitatively absorbed by the human body and direct excretion occurs
105
-------
2 0
I 0
NMR-T-UWRL *3o
Figure 6. Nuclear Magnetic Resonance Spectrum T-UWRL No. 3a
-------
I
50
0 PPM «>
o
-J
LOSS OF-OH
FAST EXCHANGE
SIGNAL DUE Q Q
TODEUTER.UM «-* :+«»20 ==R-C--«. OTHER WATER SPEC.ES
U n O D
EXCHANGE
p ^vH^>v^w lU^*^^
NMR-T-UWHL *3o*02O
Figure 7. Nuclear Magnetic Resonance Spectrum T-UWRL No. 3a + D O
£t
-------
I
50
r
s
00
^A_
6-12.3 (INCREASED AMPLITUDE
+ OOWNFIELD SCAN OF 250 opt)
MMR-T-OWRL-*6
(LONG CHAIN FATTY ACID)
I
Figure 8. Nuclear Magnetic Resonance Spectrum T-UWRL No. 6
-------
1
3
3
1
o
vo
i i i y i i i i , , , , i '? y i i -i- I0 *° " " 10 OPPM(I)
» ' ' ' ••'••-. ' i • 1 ' • n-1 • 1 ' ' i ' ' ' '' I L- 1 ' 1
0 *» MO 200 loo o^cre
0
0 NMR-T-UW«L*6*H2O
1
6*11.6 (INCREASED AMPLITUDE
LfDOWNFIELD SCAN OF250ep»)
NEW PEAK
1 ..,.,
I _ J
(LONG CHAIN FATTY ACIW
V^A^ i
» -^ 1"
I.I.I 1 I.I.I . I.I I . 1 i 1 . 1 ,1 :
.. 1 ...!... 1 ......... 1 .... I' .... 1 ...... ...] ......... 1 ........ 1 . l
tO 10 *0 5.0 40 30 20 1.0 0 WM (i)
Figure 9. Nuclear Magnetic Resonance Spectrum T-UWRL No. 6 + H2O
-------
across the intestinal barrier. These excreted lipids are not as easily
broken down or oxidized to lesser components as are the nitrogen type
compounds (NH , urea, amino acids, etc. ) in a high chlorine concentra-
tion treatment process. The treatment process probably converts the
lipids by free radical chlorination and chlorine addition to give the
saturated chlorinated fatty acids.
RECOMMENDATIONS FOR ADDITIONAL STUDIES
To further refine and specifically identify the types of volatile
acids and perhaps other compounds that are not detectable by the solvent
extractions used in this study, it is recommended that a wide range of
solvents be evaluated. Although ether extractables apparently give well-
defined spectra in both infrared and in NMR analyses, there are many
other excellent solvents available, and perhaps several of these should be
examined before accepting the conclusions of this study. The extraction
studies could be expanded by completely evaporating effluent samples
and then using Soxhlet apparatus to extract the residue obtained upon
evaporation. Many other extraction techniques exist such as acid-base
back extractions. There are an unlimited number of possible combina-
tions of extraction techniques that could be further evaluated to speci-
fically identify the compounds produced by the Thiokol recycled
effluent process.
In all of the studies reported herein, it was assumed that complete
reduction of all of the nitrogen compounds had occurred. This is very
110
-------
likely in view of the chemistry involved in the process; however, it
would be prudent to analyze the nitrogen content in a sample of the waste
to establish that all of the organic nitrogen has been destroyed. This is
a relatively simple experiment and would have been performed in this
series of tests if we had not exhausted our supply of effluent.
A highly desirable activity would be to conduct an extensive review
of the literature with respect to reactions between high concentrations
of chlorine and various types of organic compounds. It is quite possible
that many pure compound studies have been conducted utilizing high
concentrations of chlorine. If this is the case, it would make it very
convenient to design experiments that would significantly reduce the
•work load in the event that additional studies are felt desirable by
Thiokol.
Gas chromatography has not been applied to any of the extracts
obtained in this study. Utilizing esterification in conjunction with gas
chromatography could lead to the identification of several specific com-
pounds in the effluent. Deuterium labeling of known and unknown
compounds could also provide significant results.
The above mentioned techniques are just a few of the additional
tests that could be performed on the effluent samples to further refine
the identification of the organics remaining after treatment with high
concentrations of chlorine* Table 3 lists some of the above and
several additional techniques that might be employed in isolating the
effluent compounds.
Ill
-------
Table 3
Approach to Identifying Components of Highly Chlorinated
Wastewater Treatment Plant Effluents
1. ISOLATION OF ORGANIC MATERIAL
a. Extraction (solvent partition)
or concentration and then extraction
b. Lyophilization
2. SEPARATION AND PURIFICATION
a. Chromatography (thin-layer, column, gas, etc. )
b. Recrystallization
c. Sublimation
d. Distillation
3. IDENTIFICATION
a. Melting point or boiling point
b. Infra-red (IR)
c. Nuclear magnetic resonance (NMR)
d. Ultra-violet (UV)
e. Mass spectrometry (MS)
f. Gas chromatography (GC)
g. Carbon, nitrogen and hydrogen analysis
4. VERIFICATION
a. Comparison of properties with knowns
b. Synthesis
112
-------
REFERENCES
1. Nance, P. D. and O'Grady, T.J., "Nonbiological Waste Disposal
System, " Thiokol Chemical Corporation, Brigham City, Utah.
1972.
2. Middlebrooks, E.J., Unpublished Data, 1973.
113
-------
ADDENDUM
TO
P.O. Box 524. Brigham City, Utah 84302 APPFNTJTY TT
801/863-3511 AFFtWUlX U
WASATCH DIVISION
12 December 1972
2690-72-117
Dr. E. J. Middleb rooks
Utah State University
Water Laboratory
Logan, Utah
Dear Dr. Middlebrooks :
With reference to our telephone conversation on 8 December, Orson Wilson
will deliver 10 gallons of effluent to your laboratory this week«
The effluent had been in our closed loop waste treatment system being tested
in our Building M-85. The waste system contained about 30 gallons of water
and was handling the body wastes from about five people from 10 October to
20 November. The liquid was treated periodically during the 40-day run;
treatment consisted of hypochlorite addition by means of a PEPCON cell
(electrolytic production of hypochlorite from a Nad solution). Solids were
removed by rough filtration and incinerated.
On 22 November a run of 35 hours of PEPCON treatment was completed. The
solution was "PEPCON treated" until it was colorless and a 1, 140 ppm chlorine
residual was measured. (Previous runs consisted of only several hours of
PEPCON treatment* which did not decolorize the solution completely and gave
chlorine residuals in the 300 to 500 ppm range.)
After the extended chlorine treatment a BOD of 712 ppm was measured. A
similar 500 ml sample of system liquid was slugged with 10.5 grams of HTH,
a chlorine residual of 3, 000 ppm was measured after 1 hour of contact. The
HTH treated sample had a BOD of 696 ppm.
The above results indicate to us that there exists a substance in our system that
is not oxidized by hypochlorite and which can be utilized in a biological process.
Please determine the identity of the BOD producing substance.
114
A DIVISION OF THIOKOL CHEMICAL CORPORATION
-------
Dr. £. J. Middlebrooks .2- 12 December 1972
On 11 December the solution we are sending you had a 100 ppm Cl_ residual.
I assume there has been no biological activity in the liquid since the last BOD
analysis was performed several weeks ago, however, I imagine you will want
to perform a BOD analysis yourself to confirm the presence of a substance
with a biochemical oxygen demand.
This work is to be performed under the recent waste treatment aid grant.
Sincerely,
P. H. Woolhiser
115
-------
WASATCH DIVISION
15 January 1973
2690-73-010
Dr. £. J. Middlebrooks
Utah State University
Water Laboratory
Logan, Utah
Dear Dr. Middlebrooks:
Supplemental information to my 12 December letter follows as you requested
during your telephone conversation with Dr. D. P. Clark on 11 January.
The 10 gal. water sample you received from us about a month ago was a portion
of the water used as a flush medium in our closed-loop sewage treatment system
in one of our plant buildings. The system received human waste material from
10 October to 17 November.
Initial system volume 32 gal.
NaCl addition 1, 600 grams
(1.33% by wt.)
Calcium Hypochlorite added (70% Cl ) 243 g.
Lime added 120 g.
Cl added by 10 in PEPCON cells 1,230 grams
, (51-1/3 hr.)
Cl added by 100 in PEPCON cells 2, 550 grams
(42-1/2 hr.)
System temp during PEPCON treatment 90 to 100°F
System temp during idle period 70°F
Total events resulting in solids addition to the
system 51
Total events resulting in only liquid addition to
the system (does not include above 51 events) 285
After filtering the sewage, the solids remaining on the filter media are incinerated.
Succeeding sewage batches enter the filter, contact the ashes from preceding
incineration runs, and the filtrate runs into the treatment tank where PEPCON
cells add hypochlorite. (Any possibility of the incineration performing a high
temperature synthesis of organics which is washed into the treatment tank?)
116
-------
Dr. Middlebrooks
-2-
15 January 1973
The PEPCON treatment was segmented into one or two days of treatment each
week. It wasn't one continuous run.
At the end of the use cycle (17 November), the system volume was just slightly
more than the initial 30 gal. charge. About 1 gallon had been removed as
samples during the run and an undetermined volume was lost by evaporation
and incineration.
As you continue the evaluation of our system effluent, please inform us of any
questions that arise.
Sincerely,
P. H. Woolhiser
cc: Dr. D. P. Clark
117
-------
TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing)
1. REPORT NO.
EPA-670/2-74-091
3. RECIPIENT'S ACCESSIOI*NO.
4. TITLE AND SUBTITLE
DEVICES FOR ONBOARD TREATMENT OF WASTES FROM VESSELS
5. REPORT DATE
December 1974; Issuing Date
6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
8. PERFORMING ORGANIZATION REPORT NO.
Thomas J. O'Grady and Peter E. Lakomski
9. PERFORMING ORG \NIZATION NAME AND ADDRESS
Thiokol Corporation
Wasatch Division
Brigham City, Utah
10. PROGRAM ELEMENT NO.
1BB038; ROAP 21APK; Task 18
11. CONTRACT/GRANT NO.
EPA, Contract 68-01-0115
12. SPONSORING AGENCY NAME AND ADDRESS
National Environmental Research Laboratory
Office of Research and Development
U.S. Environmental Protection Agency
Cincinnati, Ohio 45268
13. TYPE OF REPORT AND PERIOD COVERED
Final-July 1971 thru Dec. 1973
14. SPONSORING AGENCY CODE
15. SUPPLEMENTARY NOTES
16. ABSTRACT
A program involving the demonstration of a pleasure craft zero discharge, physical/
chemical waste treatment system employing a unique filter-incinerator device was
conducted. Extensive test data from laboratory and shipboard demonstration tests of
the system are presented. Data on manufacture and installation costs for the pleasure
craft are also presented. The program demonstrated the ability to zero discharge
waste and comply with the 23 June 1972 EPA no-discharge standard. This report was
submitted in fulfillment of Contract 68-01-0115, under the sponsorship of the
Environmental Protection Agency.
7.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.IDENTIFIERS/OPEN ENDED TERMS
c. COS AT I Field/Group
Sewage treatment
Sludge disposal
Ships
Filtration
Incineration
Chlorination
Cost analysis
Zero discharge waste
treatment
Physical/chemical treat-
ment
Fi1ter-i nci nerator
Waste water recycle
13B
8. DISTRIBUTION STATEMENT
RELEASE TO PUBLIC
19. SECURITY CLASS (TlliSReport)
UNCLASSIFIED
21. NO. OF PAGES
128
20. SECURITY CLASS (Thispage}
UNCLASSIFIED
22. PRICE
EPA Form 2220-1 (9-73)
118
#U.S.WVEMU»BimillTII«;OFfia: 1975-657-591/5342 Region No. 5-1
------- |