SCREENING STUDY TO DEVELOP
BACKGROUND INFORMATION AND
DETERMINE THE SIGNIFICANCE OF AIR
CONTAMINANT EMISSIONS FROM PESTICIDE
PLANTS

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      SCREENING STUDY TO DEVELOP BACKGROUND

 INFORMATION AND DETERMINE THE SIGNIFICANCE OF

AIR CONTAMINANT EMISSIONS FROM PESTICIDE PLANTS
                       by
                 •C.  N.  Ifeadi

                    BATTELLE
              Columbus Laboratories
              Columbus,  Ohio 43201
                     for the
          ENVIRONMENTAL PROTECTION AGENCY
           OFFICE OF PESTICIDE PROGRAMS
             .  STRATEGIC STUDIES UNIT
                   401  M St.,  S.W.
               Washington, D.C.  20460
           Jeff Kempter, Project Officer


                     March, 1975

                  EPA 540/9-75-034

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                               ABSTRACT
          In this study, available background information is developed
and the significance of air contaminant emissions from the manufacture of
six pesticides determined.  Pesticides studied are (1) insecticides:
methyl parathion and toxaphene; (2) herbicides:  MSMA and trifluralin;
(3)  Fungicide and wood preservation:  pentachlorophenol; and (4) fumigant:
paradichlorobenzene.                          N
          Background information is gathered from published data and
responses to the questionnaires sent to the pesticide manufacturing firms.
Based on the available data, production projections are made up to the
year 1980.  A list of manufacturers of each pesticide is presented.
Manufacturing processes, raw and waste material handling, air contaminant
emission sources, quantity or quality, and pollutants, together with their
present practical control methods are discussed.
          Significance of air contaminant emissions from the pesticide
industries is evaluated on the basis of available data on the emission
quantities and/or toxicity of the pollutant(s) emitted.  Gaps in the
data required to make a complete evaluation of significance are identified
and recommendations to fill those gaps are made.
                                   11

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                               SUMMARY

          The essential findings of this study can be summarized as
follows:
                    Pesticide Production Inventory
          (1)  A severe lack of availability of past and present production
data, on individual pesticides exists.  The U. S. Tariff Commission is the
main source of published data on production; however, its lists often are
incomplete.  Some of the lists are not presented by individual pesticides,
but instead by groups of pesticides, such as aldrin-toxaphene or methanearsonic
acid salts.
          (2)  Available published data and expert opinion from the industry
and other knowledgeable people outside the industry were carefully evaluated
to develop a production table for each pesticide from 1970 to 1980.  No
estimate on the number of new plants to be built and/or plants to be
significantly modified is made.
          (3)  A list of manufacturers of each pesticide in the United
States is included, including the plant (company) name and location.  Estimates
of the design capacity of existing plants and their production are provided.

                       Manufacturing Processes
          (1)  One manufacturing process for each pesticide is identified..
          (2)  The manufacturing process is briefly described in terms of
the steps involved in the production process, aided by simple reaction
chemistry and simple production flow sheets.

                   Raw and Waste Material Handling
          (1)  Essential raw materials are enumerated.  All hazardous
materials are identified.
          (2)  Precautionary safety measures taken by manufacturers
to safeguard the health of employees are described.
                                iii

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          (3)  Simple flowsheets for waste handling during the manufacture
of each pesticide are provided, identifying the waste disposal technique used.

             Air Contaminant Emissions. Sources, and Rates

          (1)  A table of air contaminant emissions and their sources from
manufacturing processes and waste disposal systems is developed.
          (2)  Where possible, air contaminant emission rates are calculated
on the basis of simple reaction chemistry or where available are provided
by manufacturing plants.

                         Air Contaminant Control

          (1)  Air contaminants arising from production processes are
controllable by most of the methods used in the general chemical industries
to prevent dusts, fumes, and gases from leaving the production plant and/or
its waste treatment site.
          (2)  The present level of the air contaminant control for each
pesticide industry is evaluated, where enough information is available
from the manufacturers.
          (3)  Nationwide air contaminant emissions and the present emission
control situation are estimated.

                             Control Costs

          (1)  Cost estimates are presented only for those companies which
submitted such information in response to the survey.  While a few companies
provided some data on the cost of control in their plants, the operating
conditions necessary for an adequate evaluation of the same are not provided.
This part of the research, together with the economic impact on the industry
due to the imposition of the best available control technique, is not
pursued because of resource limits for this study.
                                iv

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               Significance of Emissions from Pesticide Plants

          Determination of the significance of the air contaminant emission
in each pesticide industry is made by identifying the candidate pollutant(s),
their quality or emission (where possible), and toxicity.

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                           TABLE OF CONTENTS

                                                                   Page


                               SECTION I

CONCLUSIONS	    1


                               SECTION II

RECOMMENDATIONS	    3


                               SECTION III

INTRODUCTION 	    4

     Objectives of the Study	    5
     The Study Approach	    5

          Data Collection	    5
          Process Description	    7
          Analysis of Air Contaminant Emission and Control ....    7
          Analysis of Air Contaminant Emission Control Costs ...    8
                                      /

                               SECTION IV

BACKGROUND INFORMATION AND SIGNIFICANCE  OF AIR CONTAMINANT
  EMISSIONS	    9

     Insecticide - Methyl Parathion	13

          Production Inventory 	   13
          Future Production Trends 	   13
          Manufacturing Process	15
          Raw and Waste Material Handling	   15
          Air Contaminant Emissions,  Sources,  and Rates	18
          Air Contaminant Emission Control	18
          Control Costs
          Significance of Air Contaminant Emission 	   21

     Insecticide - Toxaphene	•	22

          Production Inventory 	   22
          Future Production Trends'	24
          Manufacturing Process	25
                                   vi

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                TABLE OF CONTENTS (Continued)
     Raw and Waste Material Handling.	25
     Air Contaminant Emissions, Sources, and Rates	27
     Air Contaminant Emission Control  	   27
     Control Costs	29
     Significance of Air Contaminant Emissions	29

Herbicide - Monosodium Acid Methanearsonate (MSMA)	29

     Production Inventory	   30
     Future Production Trends 	   30
     Manufacturing Process	   32
     Raw and Waste Material Handling	   33
     Air Contaminant Emissions, Sources, and Rates	33
     Air Contaminant Emission Control  	   36
     Control Costs	36
     Significance of Air Contaminant Emission	  .   37

Herbicide - Trifluralin 	   37

     Production Inventory 	 	   37
     Future Production Trends 	  	   37
     Manufacturing Process	38
     Raw and Waste Material Handling	   40
     Air Contaminant Emissions, Sources, and Rates.  	   40
     Air Contaminant Emission Control  	   43
     Control Costs	43
     Significance of Air Contaminant Emission	  .   43

Fungicide and Wood Preservation - Pentachlorophenol  	   43

     Production Inventory	,	44
     Future Production Trends 	   44
     Manufacturing Process	46
     Raw and Waste Material Handling	47
     Air Contaminant Emissions, Sources, and Rates.  .....   48
     Air Contaminant Emission Control  .	   48
     Cost of Control	48
     Significance of Air Contaminant Emissions	53

Fumigant - Paradichlorobenzene	53

     Production Inventory	   54
     Future Production Trends 	   54
     Manufacturing Process	56
     Raw and Waste Material Handling	  .   57
     Air Contaminant'Emissions, Sources, and Rates	57
     Air Contaminant Emission Control  	   57
                              vii

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                     TABLE OF CONTENTS (Continued)
          Control Cost	60
          Significance of Air Contaminant Emission 	   60


                               SECTION V

REFERENCES	61


                              APPENDIX A

SUMMARY OF THE SELECTED PESTICIDES AND THEIR PRODUCERS 	   A-l


                              APPENDIX B

SUMMARY OF NONPROPRIETARY INFORMATION OBTAINED FROM THE
  SURVEY OF PESTICIDE PLANTS 	   B-l


                              APPENDIX C

SAMPLE OF LETTER MAILED TO SELECTED PESTICIDE MANUFACTURING
  COMPANIES	C-l
                                   viii

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                            LIST OF TABLES
Table 1.

Table 2.

Table 3.

Table 4.



Table 5.

Table 6.


Table 7.

Table 8.


Table 9.


Table 10.

Table 11.


Table 12.


Table 13.


Table 14.


Table 15.

Table A-l.


Table B-l.


Table B-2.


Table B-3.
                                                       Page

Research Plan	   6

Production Estimates - 1970 to 1980	11

Producers of Methyl Parathion in the United States .  .  14

Air Contaminant Emissions, Sources, and Rates
from Methyl Parathion Manufacture and Waste
Treatment	19

Producers of Toxaphene in the United States	23

Air Contaminant Emissions, Sources, and Rates
from Toxaphene Manufacture and Waste Treatment ....  28

Producers of MSMA in the United States	31

Air Contaminant Emissions, Sources, and Rates
from MSMA Manufacture and Waste Treatment	35

Air Contaminant Emissions, Sources, and Rates
from Trifluralin Manufacture and Waste Treatment ...  42
Producers of PCP in the United States,
45
Air Contaminant Emissions, Sources, and Rates
from PCP Manufacture and Waste Treatment	49

Air Contaminant Control Methods Used in PCP
Manufacture	52

Producers of Paradichlorobenzene in the
United States	55

Air Pollution Emissions, Sources, and Rates from
Paradichlorobenzene Manufacture and Waste Treatment.  .  58

Air Pollution Control at Standard Chlorine 	  59

Uses, Classes, Producers, Production Volumes, and
Properties of Selected Pesticides	A-l

Summary of Air Contaminant Emissions, Sources,
and Rates	B-l

Summary of Air Emission Control Devices, Efficiency,
and Cost	B-3
List of Contacts Having Expertise and Sources of
Significant Information about Selected Pesticide
industries ...	 .
                                                                    B-4
                                    ix

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                            LIST OF FIGURES
Figure 1.

Figure 2.


Figure 3.


Figure 4.

Figure 5.


Figure 6.

Figure 7.

Figure 8.


Figure 9.


Figure 10.


Figure 11.


Figure 12'.
Manufacturing Sites of the Selected Pesticides ....  10

Production Estimates (1970-1980) for Selected
Pesticides	12

Production and Waste Handling Schematic for Methyl
Parathion (Monsanto)	16
Parathion Residue and Off-Gas Incinerator.
20
Production and Waste Handling Schematic for
Toxaphene	26

Production and Waste Handling Schematic for MSMA  ...  34

Simple Flowsheet for Trifluralin Manufacture  .....  39

Production and Waste Handling Schematic for
Trifluralin	41

Production and Waste Handling Schematic for
Pentachlorophenol. 	  46

Scrubbing Systems for the Control of HC1, Cl-
Emitted from PCP Reactor	50

Dust Collector Schematics for the Penta Emission
Control	51

Production and Waste Handling Schematic for
Paradichlorobenzene	56

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                   SCREENING STUDY TO DEVELOP BACKGROUND
               INFORMATION AND DETERMINE THE SIGNIFICANCE OF
              AIR CONTAMINANT EMISSIONS FROM PESTICIDE  PLANTS
                              SECTION I
                              CONCLUSIONS

          The prinicipal conclusions to be drawn from the information derived
in the study are as follows:
          (1)  Most companies are unwilling, for proprietary reasons, to
provide their production data to contractors.  Published data are incomplete
and do not provide a basis upon which to develop a definite trend for fore-
casting future production.  However, forecasts have been provided based on
projected raw material availability and demand in agricultural production
and other end uses.
          (2)  Essential health and safety precautionary measures adopted
by most firms are transport of materials in closed systems and requirement
for the use of protective clothing such as coveralls, rubber gloves, safety
glasses or goggles, hard hats, face shields, and respirators.
          (3)  Sources of air contaminant emissions vary from one pesticide
plant to another.  The usual sources are reactor vents, vents along the
transport lines, raw material unloading area, product packaging area, and
waste and by-product recovery and disposal systems.
          (4)  Simple process chemistry is not sufficient in determining
the quality and quantity of the air contaminant emissions because of
variations in the production process.

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          (5)  The identified omissions consist of participates,  gases, and
vapors.  Each pesticide plant emits into the atmosphere at least  one pollutant
which may require control.  Some are known to create odor nuisance and
visibility problems.  In some cases, odor nuisance may be experienced, but
the odorous compounds are not known.  Very little information is  available
on the emission rates because few companies conduct in-house sampling programs.
The popular and most pratically applicable technique used in controlling
emissions from the manufacture of the pesticides studied involves wet scrubbing
with water.  A smaller percentage of plants employ alkali absorption and
adsorption processes and filter bags (baghouses).  Wet scrubbing, absorption,
and adsorption processes are used mainly for controlling gases and vapors, with
particulates controlled to a lesser extent.  Filter bags are used primarily
for controlling particulate emissions.
          (6)  A factual, realistic assessment of the significance of emissions
from pesticides plants is impractical at this time because of the limited
quantitative emission data available.  This data limitation is compounded by
absence of state or Federal source emission standards on which to base such an
evaluation.  However, in the manufacture of pesticides, there are significant
emissions of such compounds as S09, H9S, and NO , and these are substantially
                                 ^   ^         X
higher than emission standards in other related process industries.

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                              SECTION II

                           RECOMMENDATIONS

          (1)  A more effective means of obtaining data than the currently
employed method of requesting information by letter from manufacturer needs
to be developed.  This new means of data collection must simultaneously
protect the legitimate proprietary claims of manufacturers, yet insure that
EPA and its contractor meet their obligations.  Working through an intermediary
such as a trade organization may be one of the general strategies needed
to accomplish this end.
          (2)  The air pollution control aspects of the pesticide industry
have not been studied as closely as its water pollution control aspects.  A
detailed study involving air monitoring and sampling at the manufacturing
plant and their waste disposal site should be pursued.  The author of this
report has relied heavily on published data and scanty responses from the
pesticide manufacturers.  It is recommended that this study be expanded to
include plant visits and sampling.
           (3)   The dearth of field measurements on pesticides  emission
prevents development  of  a firm  recommendation on  source performance  standards
for  the pesticide industry.  However,  the  intrinsic  toxicity of  intermediate
and  final products is  clear.  It  is,  therefore, recommended that a field
emission study  be undertaken at the earliest possible date to  obtain the
data  necessary  to fully  quantify  pesticides  emission standards.

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                             SECTION III

                             INTRODUCTION

          Pesticides are important to the nation's economic life because
tliey arc used to help in the production of food and fibre and to control
organisms that destroy materials or threaten public health.  However,  the manu-
facture and  use of the pesticides can create environmental and health  concerns,
Consequently, EPA, through its Office of Pesticide Programs, has engaged in
studies of various aspects of pesticide production, use, and effects on the
environment.
          Continuing in these important studies, the Strategic Studies Unit
of the Office of Pesticides Programs has noted a need to develop background
information and determine the significance of the air contaminant emissions
from the manufacture of some pesticides, in conformity with the 1970
Clean Air Act that requires the regulatory agencies to gather information and
develop standards for emissions from stationary sources.  Because there are
large numbers of pesticides manufactured in this country, only one or  two
pesticides from each class were selected for this background study.  Six
pesticides were selected in total as listed below.
          Insecticides - methyl parathion and toxaphene
          Herbicide - monosodium methane arsonate (MSMA) and trifluralin
          Fungicide and wood preservative - pentachlorophenol
          Fumigant - paradichlorobenzene.
          The choice of these specific pesticides by EPA was based on  a
previous EPA study, which found that the selected pesticides are characterized
by high production and use, environmental concerns, regulatory interest, and
                       (1) *
increased use forecast.
 * References are located on Page 61.

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                        Objectives of the Study

          The first general objective of this study has been to develop
background information on the manufacture of six pesticides described earlier.
Specific objectives have been:  (a) to prepare a list of manufacturers in the
United States specifying the plant name, location, capacity, and production;
(b) to describe the production processes for each pesticide; (c) to describe
the emission sources of air contaminants and their control, and estimate the
nationwide air contaminant emissions from the plants producing each pesticide;
and (d) to prepare a cost estimate of the best available emission control
systems and discuss the economic impact on typical firms in the industry if
such control were required.
          The second general objective has been to determine the severity of
air contaminant emissions from the pesticide manufacturing plants and thus
identify the need to develop emission standards for such plants.

                           The Study Approach

          The approach centered on the development of background information
on the manufacture of six selected pesticides.  The study of each pesticide
was divided into four tasks as given in Table 1.  The table contains the
specific information desired on each task.

Data Collection

          Information gathering was focused on a literature survey of the
manufacture of the six pesticides in the United States.  Principal information
sources were from BCL in-house data files and government, professional, and
trade association publications.  Letters requesting data (see Appendices B and C)
were sent to 9 manufacturing plants to obtain factual information on various
aspects of the selected pesticide manufacture.  Information sought included
plant capacities and production volumes; processes profiles such as flow
sheets, raw and waste materials handling descriptions; source, kind, and

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                          TABLE 1.   RESEARCH PLAN
         Tasks
    Desired Information
1.  Data Collection
2.  Process Description
3.  Air Contaminant Emissions and
    Control
4.  Control Cost
(a)  List of Manufacturers

     •  Plant name
     •  Location
     •  Capacity
     •  Production

(b)  Manufacturing Processes

     •  Nature of pesticide produced
     •  Raw materials
     •  Waste materials

(c)  Air Contaminant Emissions

     •  Control technology
     •  Level of control
     •  Waste disposal involving air
        pollution emission
(a)  Description of the pesticide
     produced

(b)  Description of raw and waste
     materials handling

(c)  Manufacturing methods and processes
     flowsheets

(a)  Types and sources of air
     contaminant emissions

(b)  Types and levels of control

(c)  Estimate of the present emission
     control situation

(d)  Estimate of future emissions

(a)  Estimated cost for best available
     control

(b)  Economics impact on the industry

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quantities of air contaminant emissions, currently applied control methods;
and costs of such controls.  Several telephone calls were made to the
manufacturing plants urging them to complete the forms; however, no plant
visits were made.

Process Description

          Using the information gathered, flow sheets were developed, and
process profiles employed in the manufacture of each pesticide were described.
Each flow sheet identified, where possible, the following:
          (1)  Steps of manufacturing processes
          (2)  Raw materials
          (3)  Sources and types of air contaminant emissions
          (4)  Waste material disposal methods
          (5)  By-products
          (6)  Final end products.
   /                                            '
Analysis of Air Contaminant Emission and Control

          The air contaminant emissions from the manufacture of each pesticide
and the disposal of the wastes were identified and quantified where possible
together with the currently employed methods of emission control.  The currently
employed emission controls were described in terms of gas and particulate
removal efficiency ranges, potential reduction of visibility, and odor.
          Projections of future emissions were made.  By relating these to
similar emissions from other sources, a quantitative estimate of the significance
of emissions from the manufacturing sector were made.
          The qualitative and quantitative estimates of the present and
future nationwide air contaminant emissions from the plants manufacturing each
pesticide were based on the plants' capacities and the air contaminant emissions
rates.

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Analysis of Air Contaminant Emission Control Costs

          Based on the information obtained from the foregoing tasks,
cost estimates were made on the currently employed control methods.   The
costs consisted of the operating and capital cost estimates.  Where  possible,
and on the basis of available information, cost estimates of the best available
emission control systems for a typical firm were made.  In addition, a
discussion of the economic impact on typical firms in the industry,  if such
controls were required, was presented.

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                              SECTION IV
                BACKGROUND INFORMATION AND SIGNIFICANCE
                     OF AIR CONTAMINANT EMISSIONS
          For the convenient presentation of the desired information, the
research program outlined in Table 1 was subdivided as follows:
          (1)  Production inventory in the United States
          (2)  Future production trends
          (3)  Manufacturing process
         '(4)  Raw and waste material handling
          (5)  Air contaminant emissions, sources, and rates
          (6)  Air contaminant emission control
          (7)  Control costs
          (8)  Significance of air contaminant emission from the plants.
          Available information on the individual pesticide is presented
sequentially under the above headings.  However, before the discussion, a
general look at the manufacturing sites and production quantities is
necessary.  The manufacturing sites of the selected pesticides are shown
in Figure 1.  These sites do not include the formulation plant sites but
only the active ingredient manufacturing sites.
          Quantitative information on the past, present, and future
production of the selected pesticides was difficult to obtain.  Information
on past production was obtained from the U. S. Tariff Commission published
data; however, some of these production values are listed in pesticide groups
instead of individual pesticides utilized in the program.  Present and
future production information was sought through the manufacturers, but
most failed to give the information for proprietary reasons.  Since the
past production data did not present a definite trend, an extensive effort
was made to forecast production of each pesticide up to 1980.  These
estimated production data are given in Table 2 and are graphically shown
in Figure 2.  As will be discussed under each pesticide, a.number of factors
such as availability of raw materials, demand of the pesticide, and other
influences can significantly alter the forecast, so that its reliability
decreases as the time interval increases.

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                                         WEST NORTH CENTRAL
                                                                    +       X
                                                              EAST NORTH CENTRAL
                                       WEST SOUTH-CENTRAL
     Pesticides      No.of Plonte
• Methyl  parathion      4
V Toxaphene
•  MSMA
-f*  Trifluralin
X  Pentachlorophenol
A  P-dichlorobenzene
4
3
 I
6
9
                     FIGURE 1.  MANUFACTURING SITES OF THE SELECTED PESTICIDES

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                                           TABLE 2.  PRODUCTION ESTIMATES -  1970 TO 1980
Pesticides 1970
Methyl Parathion (MPT) , ,
Production, 106 Ib. 41.4la'
Percent Growth
Toxaphene , . .
Production, 10 Ibs. 50^ '
Percent Growth
Kor.osodium Methanersonate(MSMA} .
Production, 10° Ib. 30.5
Percent Growth
Trifluralin -
Production, 10 Ib. NA
Percent Growth
Pentachlorophenol (PCP) . .
Production, 10° Ib. 47. 2W
Percent Growth
Paradichlorobenze(PDCB) , .
Production, 106 Ib. 69. 6^ '
Percent Growth
1971
37.2
io(e)
65 
30
24.5(a)
20
25(a)
16
50.9(a)
8
70.4
1
1972
5i.i«
37
85.1(C>
31
30.7(a)
25
2l(f)
10
49.7^
2(e)
77.3
10
1973
48i9(a)
4(e)
94.6
11
40.1
6(.)
85.0
10
1974
57
17
108 (d)
14
50.1
25
25.4
10
48.9
5
93.5
10
1975
65.6
15
124.2
15
62.6
25
27.9
8
51.4
5
95.4
2
1976
71.4
13
142.2
15
75.1
20
30.1
8
54.5
6
97.3
2
1977
81.5
10
162.8
14
90.1
20
32.5
8
57.8
6
99.3
2
1978
88.0
8
185.6
14
103.6
15
34.5
6
61.9
9
103.3
4
1979
93.3
6
207.9
12
119.1
15
36.6
6
68.1
10
107.4
4
1980
98.0
5
232.9
12
131.0
10
38.4
5
74.9
10
111.7
4
(a)  United States Tariff Commission Report-Synthetic Organic Chemicals. (Reference 2)
(b)  55 percent of Toxaphene-Aldrin Group-quoted by U.S. Tariff Commission.
(c)  65 percent of Toxaphene-Aldrin Group-quoted by U.S. Tariff Commission.
(d)  70 percent of Toxaphene-Aldrin Group-quoted by U.S. Tariff Commission.
(e)  Indicates percent of decrease in production.
(f)  Riimker et al, Reference 1.

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                                 12
   1000
XJ
c
3
O
a.

c
O
O

u
3
T>
O
100
      1970   1971   1972   1973   1974   1975   1976   1977   1978    1979   I960
    FIGURE 2.   PRODUCTION ESTIMATES  (1970-1980) FOR SELECTED PESTICIDES

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                                  13
                     Insecticide  - Methyl Parathion

          Methyl parathion  is a  broad-spectrum organophosphate Insecticide.
 It is highly toxic to humans, a  characteristic symptom being the impairment
 of the nervous system.  It  is a  nonpersistent contact pesticide being used
 extensively in cotton production.  Interest in its use in the production of
 soybeans and alfalfa is increasing.

 Production Inventory

          Methyl parathion  is manufactured in three southern states:
 Mississippi, Alabama, and Tennessee.  The manufacturing sites are under-
 standably clustered  in the major use region--the cotton production belt.
 The names, location, plant design capacity, and the 1974 estimated production
 volumes are given in Table 3.  Over half of the present production volume is
 manufactured by Monsanto Company.
          The total U. S. capacity for the manufacture of methyl and ethyl
 parathions [0,0-dimethyl 0-p-nitrophenyl) phosphdthioate] is 147 million Ib,
 but three plants with total capacity of 53 million Ib were not producing
 methyl parathion in  1974.  The 1974 estimated production of methyl parathion
 is 57 million Ib.

 Future Production Trends

          Future production will depend on the demand and available raw
materials.  Major quantities of methyl parathion are exported;  hence,
 foreign demands will undoubtedly influence the volume of production in
 this country.   Increased application of methyl parathion to crops other
 than cotton also will increase demand.   Increased use is being  further
accelerated by recent world food production demands.   An absence of a
 strong competing pesticide in the marketplace will force an upward trend
 in production.   For example, the recent cancellation of DDT registrations
has helped to push upward the production of methyl parathion.  A factor
 that certainly may lower the bulk usage for methyl parathion is the development

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                                        14
           TABLE 3.  PRODUCERS OF METHYL PARATHION IN THE UNITED STATES
                                                                       (3,4)
Company
American Cyanamid Company,
Agricultrual Division ^ '
Hercules Inc. ., v
Synthetics Department
Kerr-McGee Corporation
Kerr-McGee Chem. Corp.
Monsanto Company .., v
Agricultural Division^ '
tauffer Chemical Company,, ,.
Agricultrual Chem. Div. '
Vicksburg Chemical Company
Velsicol Chemical Corp.

Annual Capacity
Location millions of Ib
Lindern, N. J.
Plaquemine, La.
Hamilton, Miss.

Ann! a ton, Ala.
Mt. Pleasant, Tenn.
Vicksburg, Miss.
Bayport, Texas
Total
28
15
17

50
30
3
10
153
Estimated
1974 Production
millions of Ib
--
--
15

30
10
2

57
(a)   Not operating by 1974.




(b)   Volume includes  ethyl parathion.

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                                     15

 of  a  more  effective  and  efficient way of packaging and applying the insecticide,
 such  as  encapsulation techniques.
           The  effect of  the  foregoing factors  on future production of the
 insecticide is difficult to  predict.   However, responding industries estimated
 that  the annual rate of  increase  in production will decline from the 1973-
 1974  level of  about  17 percent to about 5.0 percent by the year 1980.  On this
 basis,  1980 production will  be about 98.0 million pounds.

 Manufacturing  Process

           Methyl parathion is  commonly manufactured from sodium p-nitrophenolate
 by  the  reaction with 0,0-dimethyl phosphorothiochloridate.  There  are
 three steps involved in  the  synthesis of methyl parathion.  One common method
 involves the reaction of an  appropriate alcohol (methyl alcohol) with phosphorus
 pentasulfide,  followed by chlorination, and finally, the parathion formation in
 acetone.  The  three  steps are  as  follows:
                                             S
                    P2S5  + 4ROH"
               Diphosphoruspentasulfide            Hydrogen sulfide
                          S                     S
                          it                    ii
                     (RO). PSH + C10 	^(RO)0PC1 + HC1 + S
                        £•         i           f.
                             ONa
                                                 S
                                                      /s~^\
                                                                     NaCl
                  *•        S^—^x*                f-     \^^/      i
    0,0-dimethyl
 Phosphorothiochloridate   0  *J°2                     Parathion
                          Sodium  p-nitrophenolate
           Conditions  of  these  reactions are not  available  as  they  are
proprietary.

Raw and Waste Material Handling
          The raw materials are sodium p-nitrophenolate, methyl alcohol,
chlorine, and phosphorous pentasulfide.  In the production of methyl
parathion, by-products such as NaCl and HCl are formed along with waste
products such as H_S, mercaptan, and sulfur.  The production and waste*

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                               16
 S02
  t
 Flare
S & RHS
            i
                              S02
                               t
                           Incinerator
ROH-
         Dialkyl
         Ester
                              •S
                             -*-HCI-
                 Chlorinator
                   -^ Ch lor idothionate
  NaOC6H4NO2-
  Acetone	
                          Parathion
                          Unit
                                      T
                                      NaCl-
  Na2CO3-
                                    Waste
                                    Treatment
                                    Plant
                                                City
                                                Sewer
                                                     Partial
                                                     Recovery
Parathion
 Trace  Quantities
 of H2S, RHS, and
 HCI emitted  to air
 FIGURE 3.  PRODUCTION AND WASTE HANDLING SCHEMATIC FOR METHYL PARATHION
                           (Monsanto)(6)

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                                 17
handling schematic is shown in Figure 3.  The odorous compounds (H_S and
mercaptan) are flared and the sulfur i? incinerated, while liquid waste
effluents are neutralized with Na CO., and sent to a wastewater treatment
plant.
          Since methyl parathion is very toxic, specific handling
precautions are taken.  Kerr-McGee Corporation provides the following
precautionary steps in their plant:
          (1)  Raw materials except for SNP (sodium p-nitrophenolate)
               are stored in tanks located in diked areas or in
               submerged sumps.  SNP is stored in powder form out of
               doors.  The SNP is stored in reconditioned, open head
               type,  bolted top ring drums.  Drainage from the SNP
               drum storage area is to the chemical complex drainage
               ditches.
          (2)  Processing areas of the plant are curbed so that spills,
               gland  water from pumps, and contaminated runoff are
               contained and treated as process wastewater.
          (3)  Liquid parathion is stored in a new roofed warehouse
               that does not drain or discharge into any wastewater
               effluent systems.  The parathion is stored in 16 gauge,
               tight  head drums.  In the event of a parathion spill
               the following clean-up steps are taken in the order
               listed:
                  e  Put absorbent clay on the spill until the
                     spill is soaked up in the clay.
                  e  Remove the clay and absorbed parathion.
                  •  Put soda ash over the spill area.  Vigorously
                     scrub soda ash into floor with a broom.
                  •  Remove soda ash.
                  •  Repeat Steps 3 and 4 several times .
                  •  Wipe contaminated area with paper towel.
                  •  Soak paper towel in carbon disulfide to
                     extract methyl parathion*
                  e  Check carbon disulfide for methyl parathion
                     by infrared scan.

-------
                                   18
          •  If the test is positive repeat Steps 3 through 8 until
             the test is negative .
          •  Bury contaminated matter in closed drum.

Air Contaminant Emissions, Sources, and Rates

          The manufacture of methyl parathion produces solid, liquid, and
gaseous waste materials.
          The main sources of air contaminant emissions are:  the reactor,
the chlorinator, and the Methyl Parathion unit (Figure 3).  Odorous
pollutants arise from vents, liquid wastes, and residues.  During the
disposal of by-products (for example, flaring of H_S and mercaptans and
incineration of sulfur), sulfur dioxide is given off.  Also, during waste-
water treatment or lagooning, the odorous compounds such as H_S, mercaptans,
etc., are emitted.
          The companies contacted were unable to furnish any data on the
rate of air pollutant emissions from their plants.  Emission rates for
H_S, S, and NaCl were calculated as 460, 420, and 460 pounds per hour,
respectively, on the basis of 330 days per year and a 24-hour-per-day
operation.*  Sulfur dioxide emission rates based on H»S and S oxidation
are estimated to be 1,550 pounds per hour from the following reactions:
                       ZHjS + 303~> 2S02 + 2H20
                       S + 02	> S02
The air emission sources, compounds, and rates are given in Table 4.

Air Contaminant Emission Control

          Air contaminants arising from the production processes are
controlled by the methods used in general chemical industries to prevent
dusts, fumes, and gases from leaving the production plant into the outside
environment.
* These calculations are based on an annual production of 30 x 10  pounds
  of methyl parathion and the estimates by Rawless, et al

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                  TABLE 4.  AIR CONTAMINANT EMISSIONS, SOURCES, AND RATES FROM
                            METHYL PARATHION MANUFACTURE AND WASTE TREATMENT
Sources of Emission
Manufacturing Processes
Reactor
Chlorination

MPT Unit
t

Waste Treatment Processes
Incinerator and
T* \ ~» _ J 	
Rates,
Particulates Ib/hr
None
Acid Mist,
e.g. HC1 460
S 420

Basic Mist,
e.g. NaCl 460
Methyl Mono-
chloride
P2°5
Rates, Rate,
Gases/Vapors Ib/hr Odor Odor Unit/hr
diphosphorus — mercaptan
pentoxide kylene
mercaptan H-S
H2S
PCI-
PSCI3
Methanol
Methyl chloride
HC1
—

SO 1,550 None
T* r\
Waste Treatment Plant      None
Lagooning                  None
                                                                                                            VO
mercaptan


mercaptan
mercaptan


mercaptan

-------
                                   20
          Practical sulfur dioxide  emission control processes for H«S,
mercaptan, etc., available for methyl  parathion plants are incineration
in series with scrubbing system  and carbon adsorption.  Control of visible
fumes created by the emission of diphosphorous  pentoxide can be achieved
by a mist eliminator, while H_S  and mercaptan emission control during the
wastewater treatment can be achieved by  chemical oxidation and deodorization.
          The air emission control  system used  by Monsanto is shown in
Figure 4.  Incineration is used  for the  control of the off gases and residue,
while heavy chlorination is used for the control of the wastewater odorous
emissions.  The scrubbing system used  to control the incinerator emission
is quoted to achieve an efficiency  of  95 percent for the removal of
diphosphorous pentoxide.  The Brink Mist Eliminator provides about
99.9 percent visibility reduction.   Incineration of sulfur may be considered
a better practical control method than recovery because the sulfur that can
be recovered in this process is  inescapably contaminated with toxic methyl
parathion.
                                               TO ATMOSPHERE 	J>_
                  WATER SUPPLY -.       _^..
                             ff
           SCRUBBING
             TOWER
   INCINER/.TOR v
OFF GASC
•>p
                                •l.Vj
                                •;r-;,-»
     MIST ELIMINATOR

•\

\ STACK ,
Z
***• *' *

7]
I
s
                         LIMESTONE NEUTRALIZATION
                                              TO SEWER
                         V
                       RECOVERED
                        PRODUCT
         FIGURE 4.  PARATHION RESIDUE AND OFF-GAS  INCINERATOR
                                                              ,(7)
          Sulfur dioxide emissions presently  are  not  controlled in methyl
parathion manufacturing plants.  This means that  for  a  plant producing
about 30 million Ib of methyl parathion  per year, the S02 emission per year
will be about 12.3 million Ib or 1,550 Ib per hour; that is, by 1980 at the
present control status S0_ emission  from MPT  plants will be about 21.2
million Ib or 2,680 Ib per hour.

-------
                                   21
          On the basis of available information, Monsanto is the only
company manufacturing methyl parathion that is controlling air emissions;
the sulfur compounds by incineration, diphosphorous pentoxide by scrubbing,
and visibility by the Brink Mist Eliminator.  However, S0_ produced during
the incineration of sulfur compounds is not controlled.  It was estimated
that about 12.3 million Ib of SO  were emitted in 1974.  Both Kerr-McGee
Corporation and Stauffer Chemical Company vent their emission into the
atmosphere without any control.  According to them, there are occasional
complaints of odor problems from H_S, mercaptan, etc., emissions.  It was
estimated that H-S, S, and NaCl emissions from these plants were,
respectively, 3.2, 3.0, and 3.2 million Ib in 1974.
          The future trend in air pollution from the manufacture of methyl
parathion will tend to increase due to increased future production unless
efforts are made to control the emissions.  Large manufacturing companies,
such as Monsanto, tend to be able to install control equipment,  but the
smaller companies indicated that control was economically unfeasible.

Control Costs

          Monsanto declined to provide its air pollution control costs.
Estimation of the control costs by theoretical calculations are not possible
within the resources allotted for this study.
                    /
Significance of Air Contaminant Emission

          The present emission control situation in the manufacture of
methyl parathion shows that only Monsanto Company controls the primary
emissions such as FLS, mercaptan, S, and phosphorous pentoxide,  while
other companies do not control their emissions.  However, in the process
of controlling the primary emissions, a secondary emission (S0?) is produced
and emitted without control.
          Those companies that are not controlling lUS and mercaptan
emissions do have occasional odor problems; hence, control in the industry
is necessary.  Kraft pulp mills may be compared with the methyl parathion

-------
                                   22
plant in terms of odor problems.  The emission requirement in Mississippi
and Alabama for the total reduced sulfur (TRS) is 1.2 and 2.0 Ib/ton of
                   /D \
pulp, respectively;    whereas the calculated emission for HpS alone from the
methyl parathion plant was about 0.12 Ib/lb of active ingredient (AI).  Also,
S0_ emission standard from sulfur recovery plants may be compared with that
emitted at the Monsanto plant.  In Alabama, the standard is 0.08 Ib/lb of
sulfur processed, while the calculated emission from the Monsanto plant was
about 0.41 Ib/lb of AI.  Consequently, these odorous compounds and S02 are
emitted in an amount higher than prevailing state standards for other related
process plants.  Thus, the need for control of these emissions from the
methyl parathion plant is significant.
          The economic impact of controlling these pollutants is not
assessed since the control costs were not available.

                        Insecticide - Toxaphene

          Toxaphene, a nondefinite chemical compound, is a mixture of
polychloro-bicyclic terpenes with chlorinated camphene.  Toxaphene contains
67 to 69 percent chlorine.
          Toxaphene is less persistent in the environment compared with the
other compounds in this general group, e.g., aldrin, dieldrin, and endrin.
Toxaphene is severely toxic to aquatic ecosystems, especially to fishes.
It is also toxic to terrestrial ecosystems, but the effects are less
widespread than those caused by the more persistent chlorinated hydrocarbon
pesticides.
          Toxaphene is an important agricultural insecticide, especially
in preventing cotton plant damage.  It is normally applicable against the
boll weevil, boll worm, cotton aphid, and cotton flea hopper.

Production Inventory

          Toxaphene is manufactured in three southern states; namely,
Georgia, Texas, and Missouri, and by three companies, namely, Hercules,
Sanford, and Vicksburg.  Table 5 gives the inventory in the United States.

-------
                               23
      TABLE 5.  PRODUCERS OF  TOXAPHENE  IN THE UNITED STATES
                                                            (3)
Production
Design Estimate
Company
Hercules, Inc.
Synthetics Dept.
Sonford Chemical Co.
Tenneco Chemicals
Intermediates Div.
Vicksburg Chemical
r»^
LO.
Location Capacity
Brunswick, Ga. 50-75 ^b'

Houston, Tex. 40
Fords, N. J. 125 (b)

Vicksburg, Miss. 5
220-245
1974
65

20
20

3
108
(a)   Produces strobane,  a polychlorinated toxaphene-like
     insecticide.

(b)  Reference  1.

-------
                                   24
The distribution conforms with the general location of raw material--
southern  pine--and major use area--the  southern  cotton fields.
          The plant capacities and production volume tor toxaphene are
difficult to estimate reliably.  The firms contacted would not furnish
the information.  Also, the U.  S. Tariff Commission does not report
separately on toxaphene, but instead, as the aldrin-toxaphene group which
contains compounds:  aldrin, chlordane, endrin, dieldrin, heptachlor, strobane,
and toxaphene.  The production of this whole group showed a dramatic increase
from 1970 to 1972.  The U.  S.  production of toxaphene was estimated to be
50 million Ib in 1970.^  An estimate discussed below for 1974 is 108
million Ib, showing that the production has substantially increased.

Future Production Trends

          Estimates of toxaphene production are based on the trend in the
proportion of toxaphene in the aldrin-toxaphene group.  In 1970, toxaphene
                                             (2)
was about 55 percent of the group production.     In 1973, it was about
65 percent, and with the recent registration withdrawal of some
insecticides of this group by EPA, such as aldrin, endrin, and dieldrin,
the proportion and, hence,  the production of toxaphene is expected to
increase.
          Increases in agricultural production will provide an upward trend
in production.  However, like methyl parathion, new, more efficient, and
effective methods of packaging and application will tend to lower demands.
          On the basis of these factors, the percentage of increase in
production of toxaphene will tend to decrease from the present estimated
rate of about 25 percent to about 12 percent by the year 1980, giving a
production volume of 233.0 million Ib per year at the end of the decade as
shown in Table 2.  The above estimates have been made on the assumption
that no regulatory action will be taken to control the use of toxaphene or
that no substitute chemicals will be introduced.

-------
                                  25
Manufacturing Process

          The production of toxaphene involves two main steps:  the
production of camphene in a reactor from  ot-pinene, which is a compound
obtained from southern pine stumps; and the reaction of chlorine gas with
camphene in a solvent solution at the chlorinator.
          The reaction chemistry is given below.*
                Catalyst
                                   CH,
               Cl,
                                  CH3 UV or cat^
  o/-Pinene
Camphene
                                                  ~ C10H10C18 +  6  HC1
Toxaphene (mixed isomers
  and related compounds
  67-69% Cl)
          Details of the operating conditions in the manufacture are not
available since they are proprietary.

Raw and Waste Material Handling
          The raw materials  involved  in  the manufacture  of  toxaphene  are
camphene, chlorine, and solvent, plus other compounds used  in  the effluent
treatments.
          The production and waste material handling schematic  used by
Hercules  is presented  in Figure 5.  The  gaseous emissions from  the chlorinator,
chlorine  gas, hydrochloric acid, and  solvent vapors are  passed  through
condensers, caustic scrubbers, and a  tower containing limestone, while  the
liquid  toxaphene is filtered, stripped,  and formulated into marketable  forms.
The wastewater  is neutralized and subjected to primary treatment prior  to
discharge to the creek.
          Hercules claims to have rigorous safety  standards.   They maintain
a  fire  truck and crew  on site.  Production workers receive  annual checkups
and have  had an excellent health record, according to the company, with no

-------
     Southern
     Pine Stumps
                     -«»• 100 Other Products
<1 %
                           Pinene
                                 Main Plant
                                 Waste Stream
Reactor


Wastes
        Chlorine
        Solvent -
  H20


  Lime
NaOH

 Lime-
      •
 Stone
Surface^
Waters "
                 T
                            i
                       Camphene
                           I
                                                                  Mixed
                                                                  Xylenes
           Chlorinator
                  •HCI Gas
 Absorber
    T
 Scrubbers
   (2)
    I
Neutralizer
 Primary
 Waste
 Treatment
 Plant
                T
            Discharge to
            Tidal Creek
                     Toxaphene.
                     Solution
                              Recovered
                              Muriatic Acid
                                                                     L
  •Toxaphene —^-Solution
                                 Jo Solid
                                 "Waste
                                                  Dust
                                                  Formulation
                                                 Baghouse Dust
                                                 Collector
Atmosphere
                                                                          90 % Toxaphene
                                                                          k..,
                                                                                        ^Shipments
                                                                                                           ro
              FIGURE 5.   PRODUCTION AND WASTE HANDLING SCHEMATIC FOR TOXAPHENE
                                                                              C6)

-------
                                   27
correlations of death or illness with toxaphene handling.  The company
stated that they are in compliance with all air pollution control regula-
tions promulgated by the State of Georgia under the Federal Clean Air Act
of 1970.  Information on raw and waste material handling at other manu-
facturing plants is not available.

Air Contaminant Emissions, Sources, and Rates

          Main sources of air contaminant emissions are the reactor, the
chlorinator, and toxaphene formulations.  There is no information on
emissions from oi-pinene production.
          The main emission from the reactor is chlorine gas; the emissions
from the chlorinator are chlorine gas, hydrochloric acid, and solvent vapor,
and toxaphene particulates are released during formulation.  These compounds
and sources are given in Table 6.  The emission rates of these compounds
are not available,  except HC1 which is estimated to be 4,350 Ib/hr* from a
65-million-lb-capacity plant.

Air Contaminant Emission Control

          Most systems available in chemical industries for controlling
acidic gases are applicable to the control of emissions from- the manu-
facture of toxaphene.  There are three main control techniques:  scrubbing
(alkali or water),  stripping, and adsorption.
          Hercules uses these control techniques to control HC1, chlorine
gas, and solvent vapor emissions.  The emissions are initially passed
through condensers where the majority, of the solvent and hydrochloric acid
is removed.  Following the condensers are caustic scrubbers which remove
additional traces of hydrochloric acid and chlorine.  Finally, the effluent
is passed through large towers containing limestone, which Is said to remove
the "balance" of the hydrochloric acid.  The final rate of emissions from
the limestone towers is not known, but Hercules claims up to 100 percent
efficiency.
* Estimated at 0.53 Ib/lb AI.

-------
                TABLE 6.  AIR CONTAMINANT EMISSIONS, SOURCES, AND RATES FROM
                          TOXAPHENE MANUFACTURE AND WASTE TREATMENT
Sources of Emission
Participates
Rate,     Gases/     Rate,. .             Rate,
Ib/hr     Vapors     Ib/hr     Od°r  Odor Units/hr
Manufacturing Steps

      ^•-Pinene Production
     NA
           NA
   NA
      Camphene-Preduction
      (Reactor)
     NA
           NA
   NA
      Chlorination-Toxaphene      None
      Production
      Toxaphene Granular       Toxaphene
      Production                Dust
                          Cl, gas
                          HC1
                          Solvent
                           Vapor

                           None
                     4350
                         (6)
                                NA
                               None
                             N>
                             00
Waste Treatment Processes

  Wastewater Treatment Plant
    None
           Cl,
                                                         HC1
Possible
candidate
  CU

-------
                                   29
          In chemical industries various control technologies are available
for controlling particulates, such as electrostatic precipitators, baghouses,
scrubbers, etc.
          Hercules uses baghouses to control the toxaphene particulate
emissions.  No information is available on the uncontrolled and controlled
emissions.
          No definite statement can be made on the present air pollution
control status in the manufacture of toxaphene.  Control information is
unavailable from other manufacturing plants.

Control Costs

          Emissions from the manufacture of toxaphene are not controlled
separately; instead, they are passed together with emissions from the
manufacture of other pesticides in their class through the same control
system.  Consequently, control cost information is unavailable.

Significance of Air Contaminant Emission

          There is high emission of HC1 (about 0.53 Ib/lb AI) in the
manufacture of toxaphene.  It is recognized that HC1 is a liquid at normal
temperature and pressure.  However,  fumes of HC1 are emitted, although the
rate of emission is not known.
          A particularly important emission in the manufacture of toxaphene
is that of toxaphene particulates.  Toxaphene is toxic to mammals; for
example, the toxic level for dogs is 20 ppm.     However, data are
unavailable on the rate of emission from any plant.  Consequently, an
assessment of the significance of emission from the plants is not possible
at this time.

          Herbicide - Monosodium Acid Methanearsonate  (MSMA)

          MSMA is a selective herbicide of the organic arsenical group.
MSMA is not very toxic to animals and it degrades fairly readily in the

-------
                                    30
soil.  It is a postemergent herbicide used to control hard-to-kill grass
weeds.

Production Inventory

          Monosodium acid methanearsonate is produced in three states--
Wisconsin, Texas, and New Jersey—and by three companies—The Ansul
Company, Diamond Shamrock Chemical Company, and Vineland Chemical Company.
The plant design capacities of the producers and their production are shown
in Table 7.
          The U. S. capacities and production volumes are known for the
Ansul Company and Diamond Shamrock Chemical Company.  Their combined
estimated production for 1973 and 1974 were 33.1 and 32.4 million Ib,
respectively.  No information is available on the capacity and production
volume of Vineland Chemical Company.  However, it is estimated that the
total production for the methanearsonic acid salts for 1973 and 1974 is about
40 to 50 million Ib, respectively.

Fviture Production Trends

          The production of MSMA has been showing an upward trend since
1971.  Ansul has been producing at design capacity while Diamond Shamrock
Chemical Company has maintained a production of about 50 percent above
design capacity.  This means that either new plants will be built or
existing ones expanded, or both,  to meet the demand.  MSMA belongs to the
organic derivatives of the trivalent form of arsenic.  Its selective,
postemergent efficacy against hard-to-kill grass weeds makes MSMA an important
herbicide in agricultural production.  Therefore, its production in years ahead
will tend to increase with the recent increased demand in the production of
food and fibre.  The appearance of competing herbicide in the marketplace
may lower the production of MSMA.
          A conservative estimate for the production has been presented in
Table 1.  Again, an increase in production is projected, but this rate of
increase will tend to decrease from the present 25 percent annually to about
10 percent annually by the year 1980.

-------
                        31
TABLE 7.  PRODUCERS OF MSMA IN THE UNITED STATES
       Company
                               Location
                        Design
                    Plant Capacity
                      million Ib
                                                      Production
                                                       Estimate
                                                       .million Ib
                                                      1973   1974
The Ansul Co., Chemical
  Div.
                             Marinette, Wise.
Diamond Shamrock Chemical    Greens Bayo, Tex.
  Co., Agricultural Div.
                           10
                           17
                                                      16.1   15.7
                                                      17.0   16.7
Vine land Chemical Co.
Vine land, N. J.
                                                       NA     NA

-------
                  32
Manufacturing Process

          Three main steps are involved in the manufacture of MSMA:
production of sodium arsenite, methylarsonic acid, and MSMA.
          The first step in the production of MSMA begins with the formation
of sodium arsenite by the reaction of arsenic trioxide and 50 percent caustic
soda solution.  In the next step, 25 percent solution of the sodium arsenite
is treated under pressure with methyl chloride to give the disodium methane
arsenate (DSMA).  Some companies sell a portion of the DSMA for herbicide
uses, but since DSMA is less soluble, it requires a higher application rate.
Most companies go a step further to prepare MSMA.
          MSMA is prepared by adjusting the pH of DSMA with sulfuric acid
in a reactor.  The material is centrifuged to remove salts such as sodium
sulfate and sodium chloride (which are waste by-products) and the resulting
solution is concentrated by evaporating the water.  Hydrogen peroxide is
added to oxidize the unreacted trivalent arsenic to the pentavalent form.
The final product is formulated with a wetting agent and packaged into
1-gallon, 5-gallon, 30-gallon, or 55-gallon containers.  The active
ingredient of MSMA is sold at a number of concentrations, but approximately
58 percent is the maximum concentration that can be prepared without undue
viscosity effects.
          The simple process chemistry is given below.

          As203 +  6NaOH 	>  2Na3As03  + 3H20

          Arsenic               Sodium
          Trioxide              Arsenite

          Na3As03 + CH3C1
          Methyl
          Chloride

          2CH3AsO(ONa)2 + H2SO^
DSMA
                CH3AsO(ONa)2 + NaCl

-------
                                  33
Raw and Waste Material Handling

          Raw materials used to produce MSMA are arsenic trioxide, sodium
hydroxide, methyl chloride, and sulfuric acid.  Arsenic trioxide is the
most toxic species, and it is imperative that this compound be handled
with care.
          It is unloaded under a hood equipped with an exhaust blower that
pulls the dust through ducts to a dust collector, or scrubber.  Employees
use respirators, and frequent employee health screening to check any
health danger is required by most firms.
          The production and waste schematic    is shown in Figure 6.
          A major concern in the wastewater  treatment  is  the  disposal of
the mixture of sodium sulfate and sodium chlorate contaminated with arsenic.
Diamond Shamrock handles this by precipitation and centrifugation.  After
washing, they are disposed of in a landfill which is registered with the
State of Texas.  No information on air emissions from the disposal site is
available.  Methanol, a side product of methyl chloride hydrolysis and
water, is recycled.

Air Contaminant Emissions. Sources, and Rates

          The main source of air contaminant emissions during the
manufacture of MSMA is in the sodium arsenite production during the
unloading of arsenic trioxide.  Minor emissions may occur during the
processing of the MSMA by evaporation from vents of the reactors.
          The main emission during the production of sodium arsenite is
arsenic trioxide, which is very toxic.  Diamond estimates the controlled
                              -8                     8
emission of As 0~ to be 6 x 10   Ib/ton or 6.44 x 10   Ib/hr.   During the
production of DMSA and MSMA,  vapors of CH-jCl, Na^O^, and CH.O,  are given off.
          Arsenic-contaminated solid materials including NaCl, Na_SO,,
and MSMA are landfilled.  No information is available on the emissions  from
these disposal sites.  The list of the pollutants from various sources  is
given in Table 8.

-------


1
A O
KJ0f\LJ
H O



3













Dust
Collector
t


, k*. I |n;f





















25%No3AsO3
Storage

1
Methylarsonic
> Acid Unit
\
Crude . .fei Purification 	 fe. D^MA Salei
DSMA
i
... ^ ""SMA _.^ [•.,_»«.._»,.. »^ I^.^IT -_ fc TITy AA?I
j^ Reactor -•

1 1
Stripper « Aqueous By-Product
CH3OH Salts
i "2°r^ 1
CH-sOH \A/«eUar ^ No^SOx
3 Washer -^^2, 4
Recovered LLlqu5d T<> Approved
j Land Fill
                                                                                            u>
FIGURE 6.  PRODUCTION AND WASTE HANDLING SCHEMATIC FOR MSMA
                                                           (1)

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                  TABLE 8.  AIR CONTAMINANT EMISSIONS, SOURCES AND RATES
                            FROM MSMA MANUFACTURE AND WASTE TREATMENT
Sources of Emissions
                               Particulates
                                                Rates,
                                                Ib/hr
    Gases/
    Vapors
Rates,
ib/hr
         .  Rates,
Odor   Odor Unit/hr
Manufacturing Steps

  Sodium Arsenite Production
   (Reactor Vents)
                                   AS?°T      6.44x10
                                                     —8
  DMSA Production
    (Reactor Vents)
  MSMA Production
   (Reactor Vents)
                                   None
                                   None
   CH3C1

   CH3OH
   NaCl
                                                            MSMA
                                                                                         Same
             Same
  MSMA Processing
   (Evaporator and
   Centrifuge)
                                   MSMA
Waste Disposal Processes

  Landfill


  Ponds
                                    NA


                                    MA
Not Identified
         Not Identified —

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                                  36
Air Contaminant Emission Control

          The only air pollutant controlled in this industry is As20,..
The compound is emitted as particulates and various control techniques
are available, such as baghouses, scrubbers, and electrostatic precipitators.
          Diamond Shamrock operates the As20_ drum opening and dump bin
under a hood equipped with a blower that will pull the As20_ into a
bagfilter for collection.  Ansul's plant controls the arsenic trioxide
emission by a scrubbing system.  Efficiencies of these control systems
,are not known by the firms.  The best control technique for this highly
toxic arsenic trioxide is to have both baghouses and scrubbers in series.
The bag filter is useful in recovering As20,, while the scrubber removes the
smaller size particles that normally will not be collected by the bag
filter.  Unfortunately, the scrubbing system may create water pollution
problems.
          Assuming an industry estimate of a controlled emission rate of
6.44 x 10"b Ib/hr As203,  it is estimated that the amount emitted per year
by a plant of 17 million Ib capacity is 5.1 x 10*  Ib.
          Ansul Company observed occasional odor nuisance, but no
identification of the odor-producing compounds has been made.
          A definite statement on the level of emission control is not
                                N
possible because of incomplete data.  However, it can safely be stated that
all companies control arsenic trioxide emission but controlled emission
rates are not known.  A definite need exists to monitor the emission of this
very toxic pollutant.
          Future emissions will increase on the order of the production
projections if the present level of control is maintained.  Assuming an
emission rate of As Q  given by Diamond Company as 6.44 x 10"® Ib/hr AsoOs
emission for the industry by 1980 will be 0.0393 Ib/year.

Control Costs

          Diamond Shamrock--with design capacity of 17 million Ib per year--
gives the cost for controlling As203 as $8,000 for capital cost,  and $200
per year for the operating costs.   An acidifier vent scrubber is  said to

-------
                                   37
cost $500 for the capital, and $100 per .year as the operating cost.  Air
flow rates and hence sizes and efficiencies of the equipment were not
provided for verification purposes.

Significance of Air Contaminant Emission

          Of importance in the industry is the control of As20_ emissions
because of their high toxicity and carcinogenic property.  As of this date,
the responding firms do control As~0, emissions but the level of control
is not known.

                          Herbicide -  Trifluralin

           Trifluralin Is  a  selective  soil-applied or  preemergence
herbicide of the class  Nltroaromatic.  It is  used to  control annual  grass
weeds  and some  annual broad-leaves.   About 60 percent of  the trifluralin
is  used  in the  production of soybeans, 30 percent cotton, and 10 percent
others.^
           Toxicity of trifluralln to  mammals  is low,  but  it  is  highly
toxic  to fish.   It is degradable  by microbial activity, and  moderately
persistent in the soil, with about 85 percent of  the  applied rate  degrading
during the growing season.'^'

Production Inventory

           Trifluralin is  manufactured by  only one firm, Eli  Lilly  and
Company,  at  their Tippecanoe Labs at  Lafayette, Indiana.   The plant  capacity
is  estimated to be 35 million pounds  per  year.  Production volumes for
1971 and 1972 were estimated respectively as  25 and 21 million  pounds.

Future Production Trends

           The future production of trifluralin will depend on availability
of  raw materials and sale of trifluralin.   The impact of  the availability

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                                        38
     of raw materials on trifluralin production is difficult to assess because
     of many unpredictable influencing factors.
               Since trifluralin is mainly used in agricultural production such
     as cotton, soybeans,  etc.,  the future growth rate of these crops will
     influence the growth in production of trifluralin.
               The production of these crops in the years ahead will increase
     because of the current demand in agricultural production.
               In the projections given in Table 1, increased agricultural
     production was reflected in increased trifluralin production while the
     appearance of potential competing herbicides was reflected in a decreased
     percentage of growth.   By 1980,  it is projected that about 38 million pounds
     will be produced.

     Manufacturing Process
               The manufacture of trifluralin involves two main steps:   nitration
     and amination.  The simple process chemistry is given below while  the flow
     diagram is shown in Figure 7.
      CF,
OH
             HNO,
p-chlorobenzotrifluoride
                              CF,
                                            Dipropylamine
                                          Sodium Carbonate
                                               Water
                           3,5-dinitro-4-chloro
                            benzotrifluoride
    CF,
trifluralin
               Nitration involves the reaction of the following compounds in
     reactors:  p-chlorobenzotrifluoride, sulfuric acid, and nitric acid.  The
     product of the reaction is 3,5-dinitro-4-chlorobenzotrifluoride, and the
     by-product is spent sulfuric acid which is recycled.  The main off-gases
     are nitrogen oxides.
               Amination is the second-stage reaction involving the reaction of
     3,5-dinitro-4-chlorobenzotrifluoride, dipropyl amine, and sodium carbonate
     in solution.   The product of the reaction is trifluralin and the effluent is
     brine solution which is treated for recovery.

-------
                                       39
p-Chlorobenzotrlfluoride
Sulfuric Acid
Nitric Acid
Off Gases to Scrubber
               NITRATION
                                3.5-Dinitro-4-chiorobenzotrifluoride
                                Dipropyl Amine
                                Sodium Carbonate
          Spent Sulfuric Acid
                                Water
                                                AMINATION
                                 Trifluralin v
                                          Brine Solution to
                                          Treatment Facility
            FIGURE 7*  SIMPLE FLOWSHEET FOR TRIFLURALIN MANUFACTURE

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                                   40
Raw and Waste Material Handling

          The raw materials used in the manufacture of trifluralin are
nitric acid, sulfuric acid, sodium carbonate, dipropylamine, and
p-chlorobenzotrifluoride.  The main toxic materials are the acids, and their
handling practices in chemical industries are well-known.
          Eli Lilly provided information of the measures adopted to protect
the health of their employees.  These included wearing protective
clothing.including self-contained breathing apparatus for certain unloading
operations, isolation piping and tanks for each raw material, containment
procedures and facilities for accidental spills, routine review procedures
between operators, and safety and material handling personnel.
          Greater detail of the production and waste handling schematic
is shown in Figure 8.

Air Contaminant Emissions. Sources, and Rates

          The main sources of air contaminant emissions are the nitration
reactor and condenser.
          The main gaseous emissions from the nitration reactor are sulfur
dioxide, sulfur trioxide, hydrogen fluoride, hydrogen chloride, and nitrogen
oxides, while particulate emissions from the reactor consist of nitrate,
sulfate, and chloride.  Emissions from the condensers are mainly aerosol
consisting of trichloromethane and trifluralin.  The wastewater from the
plant is neutralized, and subjected to the conventional waste treatment
of primary clarification and secondary aerated biological treatment.  There
are no odors or other air contaminant emissions during the wastewater
treatment.  Table 9 is a list of the contaminants emitted and their
rates as measured by the company.

-------
 PCBT

HNO3-
    Monon it rotor
'  Oleum.

                  ±
Dinitrator
                        J
              NO,

               f
            Scrubber
             Waste
             Water
                                               Excess Acid
                                               Sold
                 Acid
                 Recovery
                         Condenser
                                              Vac
                                              Exhaust
                                                                  NH(C3H7)2
                                                                  HoO
      Na2CO3
                                                      I
Amination
Reactor
                                                                      I
                                                                    Filter
                                                              Salt
                                                              Water
                                                              Waste
              Aromatic
              Naptha
                                             Trifluralin (e.c.)
      FIGURE 8.  PRODUCTION AND WASTE HANDLING SCHEMATIC FOR TRIFLURALIN(6)

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                 TABLE  9.  AIR CONTAMINANT  EMISSIONS,  SOURCES, AND RATES FROM
                          TRIFLURALIN MANUFACTURE AND WASTE TREATMENT
Sources
Manufacturing Process
Nitration

Condenser
Participates

nitrate
sulfate
chloride
cue 13
Trifluralin
Rate,
Ib/hr

1
1
1
NA
NA
Gases /Vapors

sulfur dioxide
sulfur tioxide
hydrogen fluoride
hydrogen chloride
nitrogen oxides

Rate,
Ib/hr

3
1 •
1
10
3

Rate,
Odor Odor Unit/hr

None

None
Was tewater Treatment
                                   None
None

-------
                                   43
Air Contaminant Emission Control

          Air contaminant emissions from the manufacture of trifluralin
are primarily gases and particulates.  Control of these compounds in the
chemical industry is achieved by many methods, but those directly applicable
to the trifluralin industry are wet scrubbers.
          Eli Lilly uses wet scrubbers and their quoted efficiency is about
90 percent.

Control Costs

          The Eli Lilly emission control system consists of 1- and 2-stage
venturi scrubbers and tri-mer wet scrubbers.  The total flow through the
system is about 20,000 standard cubic feet per minute.  Eli Lilly estimates
that capital cost so far is about one million dollars.  They have no information
on the operating cost.

Significance of Air Contaminant Emission

          There are a large number of air contaminant emissions in the
industry.  The State of Indiana has no stationary source emission standard
for sulfur and nitrogen compounds from the process industry.  However, the
emission rates of these compounds are small when compared with the State of
Massachusetts standards which are 10 Ib/hr for nitrogen oxides and 25 Ib/hr
for the process industry which are 10 Ib/hr for nitrogen oxides and 25 Ib/hr
                 (8)
for sulfur oxide.     The toxic material emitted to the environment is
trifluralin which, according to present knowledge, is highly toxic only to
fish and not to mammals.  Unfortunately, data are not available on emission rates,

          Fungicide and Wood Preservation - Pentachlorophenol

          Pentachlorophenol (PCP) is a wood preservative, but it is also
used as a contact herbicide.  About 75 percent of the PCP is used as a
wood preservative for poles, crossarms, and pilings.

-------
                                   44

          It is hazardous Co man primarily because it is capable of
causing eye injuries such as conjunctival redness, iritis, and slight
corneal damage.  In solution, it can be absorbed through the skin to toxic
amounts.  Consequently, its handling requires due precautions.
          PCP is biodegradable and thus gives no long-term pollution
problems.

Production Inventory

          Pentachlorophenol is manufactured at five chemical companies in
five states.  Unlike some agricultural pesticides, which are restricted
to the area of intense application, it is not restricted to one geographical
area.  Because of its wide application in the field of industrial pres-
ervation, and  logistics of distribution, it is produced in states widely
separated — Washington, Kansas, Texas, Michigan, and Illinois.
          The present annual U.S. capacity for the manufacture of PCP is
about 97 million pounds.  In 1973, the production was 46.6 million pounds(3)
and the estimate for 1974 is about 48.9 million pounds.  The manufacturers
of PCP, their capacities, and estimated production for 1974 are shown in
Table 10.

Future  Production Trends

          With the  increased  cost  of other wood  preservatives  such as
crude oil and  coal  tar  crudes  (creosote), the demand for  PCP as a wood
preservative may increase.
          However,  since PCP  is  used almost exclusively as a wood pre-
servative for  power and phone  transmission poles, the increasing use of
underground transmission and  nonwood-related materials  for poles,  such  as
concrete and glass  fibre, will  tend to force PCP  to peak  about 1980 and
then diminish.  Production projections to 1980 are given  in Table 1.  A
gradual  increase in production  is  forecast from  the present 5 percent to
10 percent by  1980.  The greatest  impetus to production appears to be
the lack of a>  competing product  like crude oil, which is  supported by the

-------
                                      45
               TABLE  10.  PRODUCERS OF  PCP  IN THE UNITED  STATES
                                                                (3,9)
   Company
      Location
Annual Capacity,
 million  Ib
Eat. 1974
Production,
million Ib
Dow Chemical Co.
Monsanto Indiat. Chems,
Reichhold Chems.; Inc.
sonford Chemical Co,,
Vulcan Materials Co.
  Chemicals Division
      Midland, Michigan
Co.   Sauget, Illinois
      Tacoma, Washington
      Houston, Texas
      Wichita, Kansas
               Total
      18
      26
      16
      18
      19

      ?7
     5
    10
    10
     5.2
    18.7

   "4879

-------
                                   46
estimates of some of the companies who think that their production will
double by 1980.  The projected 1980 production is 74.9 million pounds.


Manufacturing Process


          Almost all of the PCP produced in the United States is manufactured
by the chlorination of phenol.  A simple reaction chemistry of the process
is shown below; and the simple schematic in Figure 9.
                OH
             Phenol
                      + 5C1
Catalyst
- >
Elevated
temperature
+ 5HC1
    Phenol
  Chlorine

 Aluminum
 .Chloride
 (Catalyst)
           Pentachlorophenol
            Chlorine
            Scrubber
                               I	
           C6CIXOH
             -1
           Recovery
                          HCI
          Recycle to
          Chlorine
          Plant
  FIGURE 9.   PRODUCTION AND WASTE HANDLING SCHEMATIC FOR PENTACHLOROPHENOL
                                                                          (10)

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                                   47

          The general manufacturing process can be described as follows.
          The chlorination is performed at substantially atmospheric
pressure in a reactor.  The temperature of the phenol in the primary
reactor at the start is in the range of 65-130°C  (preferably 105°C) and
is held in this range until the melting point of  the product reaches 95°C.
About three or four atoms of chlorine are combined at this point, and the
temperature is progressively increased to maintain a temperature of about
10°C over the product melting point, until the reaction is completed in
5-15 hours.  The mixture is a liquid, and a solvent is not required, but
the catalyst concentration is critical; about 0.0075 mole of anhydrous
aluminum chloride is usually'used per mole of phenol.
          The PCP from the reactions may be further treated  (formulated)
to effect more marketable products.  At Reichhold, the PCP undergoes ingot
casting and shotting operation.

Raw and Waste Material Handling

          The raw materials used in the manufacture of PCP are phenol, chlorine,
and a catalyst — aluminum chloride.  Sources of  raw materials vary from firm
to firm.  Some manufacturers produce these materials on site, while others
purchase the same.
          Dow Chemical makes phenol from benzene  (via monochlorobenzene),
but this method of making phenol is being generally replaced by the
cutnene oxidation process.   Monsanto also makes both the phenol and chlorine;
while Vulcan makes the chlorine, but purchases the phenol; and Reichhold
makes the phenol,  but purchases the chlorine.
          While some companies report that no particular precautions are
taken at PCP plants, others point out specific precautions such as handling
chlorine and phenol in closed systems, and the use of plant coveralls,  rubber
gloves,  safety glasses, goggles, and hard hats.  There are occasional face
shields and respirators for employee protection when the situation calls
for their use.

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                                   48

Air Contaminant Emissions. Sources, and Rates

          In the manufacture of pentachlorophenol, there are three main
sources of air emissions:  the PCP reactor, ingot and shotting operation,
and the acid system reactors.  At the PCP reactor, the following compounds
are emitted:  chlorine gas, hydrochloric acid vapor  (HC1), and chlorinated
phenols.  At the acid system reactors and process vents the chlorinated
phenol and chlorine are emitted.  The particulate emission from the manu-
facturing process is limited to PCP dust from the ingot casting and shotting
operation.
          There are no air contaminant emissions reported from the waste-
water treatment.  The sources of emissions and pollutants are given in
Table 11.

Air Contaminant Emission  Control

          Major emissions from the manufacture of PCP are gases and parti-
culates, which are amenable to chemical industrial air pollution control
techniques.  Practical controls used in the industry are scrubbers for the
gaseous emissions, and filter bags for the partlculates.
          Reichhold by-product recovery systems and air pollution control
systems for gaseous and particulate emissions are shown in Figures 10 and
11, respectively.  The control methods in terms of efficiencies are described
in Table 12.
          Firms responding to our questionnaires reported that under
proper operation of these control devices,  exhaust effluents are invisible
and free from odor.

Cost of Control

          Reichhold gave the following control costs for their 12-million-
pound-capacity plant:

-------
                        TABLE 11.  AIR CONTAMINANT EMISSIONS, SOURCES, AND RATES
                                   FROM PCP MANUFACTURE AND WASTE TREATMENT
Sources of Emission     Particulates
             Rates,
             Ib/hr
   Gases/Vapors
Rates,               Rates,
Ib/hr      Odor   Odor Units/hr
Manufacturing Process

PCP Reactor
Acid System Reactors
Ingot Casting

Shotting Operation

Wastewater Treatment
None
None
PCP

PCP
(1) chlorinated phenol
(2) chlorine gas
(3) Hydrochloric acid
    vapor

(1) chlorinated phenol
(2) chlorine gas
(3) Hydrochloric acid
    vapor

    None

    None
                                                                                                                -P-
                                                                                                                vO
            PCP

            PCP

            None

-------
                                                                         Vent
Chlorinated phenol feed
I
1
1
1
1
I
1
1 ,
t



PCP
reactor

1
i
PCP
























H

4
HCI + CI2 i.
gas
c

.




c

r* k

L.
ID
JQ
J3
•3
|UJ1
O
cn

O
c
a>
JZ
Q.



3


'



D


•"•




;


•y
_r


i



HCI gas
HCI |
gas /*3r^
v * ^ 1 ^ S\ A _: -i 	 1 	
* phenol ^VKJ Acid cooler
^*r*^
> 	 1 Phenol 	
1 1 i )
/ \
/ - . _ . \ ,
1 Phenol scrubber] ROW
V storage /pncnoi
	 ^-rk
















J

C






c


-J

^

Vent

V


X3
O
jQ
O
O


^L

1



JVater
3









L

JT





/
*



1

•A


JC
0
O









„ Water
spray










"~X To waste
L__^-

Acid tank
vent
HCI
storage

FIGURE 10.  SCRUBBING SYSTEMS FOR THE CONTROL OF HCI, C12 EMITTED FROM PCP REACTOR

-------
 Vent
Dust
collector
                        From PCP reactor
Dust I
            Fume hood
             Ingot
             casting
                                                                                      Dust
                                                                                      collector
                                                                                                    •Vent
                                                                             Return to
                                                                             shot pot
Forced draft
    air
               To product
               packaging
                 FIGURE 11.  DUST COLLECTOR SCHEMATICS FOR THE  PENTA EMISSION CONTROL

-------
                                  52
                 TABLE  12.  AIR  CONTAMINANT  CONTROL METHODS
                            USED IN  PCP MANUFACTURE
Control
Sys tern
Wet Packed and
Venturi Scrubber
(with water)
Efficiency,
percent
99-100
Compound Controlled
Controlled Emission, Ib/ton
C12 N.A.
HC1 N.A. ,
Phenol 2 -' ,
Sodium Penta- 4.32 -'
                                            chloro phenate
Dust Collector
(bay filters) at
ingot casting
at shotting operation
99
95
PCP
Fume
PCP
0.1 -'
1 b/
(a)   Controlled  emission reported  by Monsanto based on 1974 production.

(b)   Controlled  emission reported  by Reichhold based on 1974 production.

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                                   53

                                                                  Operating
Name of Control Device            Size         Capital Cost($)    Cost ($/yr)
Bag filter  (2)               (1) 2000 ft2*    $ 70,000           $ 6,000
                              (2)  450 ft2
Mechanical Seals (for PCP reactor)               50,000             6,250
Phenol and Acid Scrubber                         80,000             1,000
      Area of bag filter.
          According to Reichhold, the greatest problem arose from the dust
collectors because of the lack of reliability.  They consider dust emissions
less than the present 1.0 Ib/ton to be too restrictive, since this will
require additional capital expenditures in excess of $100,000 and operating
costs of $10,000/year for their plant capacity of 16 million Ib/hr.

Significance of Air Contaminant Emissions

          The quality of air contaminant emissions in the manufacture of
PCP is significant due to the fact that large numbers of compounds are emitted
at high emission rates.  The control of the emissions is desirable as a
method of recovery of materials.  Since PCP is toxic to human respiratory
tracts and eyes, its very efficient control is recommended.  The present control
method which uses inadequate cloth area of bag filters needs augmentation.


                    Futnigant - Paradichlorobenzene

          About 50 percent of the paradichlorobenzene  (PDCB) is used as
lavatory space deodorant, about 40 percent in moth control, and the rest
as reactive intermediates in the production of chemicals such as agricul-
tural pesticides and as an industrial porosity control agent.
          PDCB causes moderate irritation to the human eye, throat, nose,
and skin, with severe problems on long exposure.  Continued exposure to
PDCB vapors for months or years causes headache, portal cirrhosis, or
atrophy of the liver.'^'
          PDCB undergoes biological, nonbiological, and sunlight degrad-
ation at a moderate to rapid rate.

-------
Production Inventory

          Paradichlorobenzene  is manufactured by  eight  companies  in nine
 states.   These  companies,  their plant design capacities,  and  estimated  1974
 production  are  given  in  Table  13.
          The annual  U.S.  capacity  is about 150 million pounds.   Capacities are
 flexible  and throughput  depends on  demand and available feedstocks.   Benzene
 has been  in very  short supply  recently due to decreased petroleum supplies.
 The production  for  p-dichlorobenzene in  1972 and  1973 was 77.3 and 85 million
 pounds, respectively, and  the  1974  production is  estimated to show a  moderate
 increase  of about 93.5 million pounds.   Generally,  production has varied
 from  50 to  60 percent of plant capacity.

 Future Production Trends

          Based on  demand  and  raw material availability,  production of  PDCB
 is estimated to increase by about 2 percent per year through  1977.^   '
 Various arguments have been presented for growth  projection.  Some feel
 that  the  growth rate  will  be at least in line with  gross  national product and
 an increase in  disposable  income, while  others feel that  continued rise
 of polyester and  newer synthetic fibre at the expense of  wool and cotton
 would tend  to level off  production.
          Two smaller suppliers of  PDCB  have withdrawn  from the market
 since 1970, but expansions by  others in  the business have more than
 compensated.  Most  producers see little  or no growth for  p-dichlorobenzene.
 Still, there is strong feeling by some that the demand  for the space
 deodorant used  in restaurants, public buildings,  etc.,  will continue  to
 grow  and  the moth control  market will hold its own.^11^ Projections up  to
 the year  1980 were  provided in Table 1,  and the production by the end of
 the decade  is estimated  at 112 million pounds.

-------
                                   55
             TABLE  13.   PRODUCERS  OF PARADICHLOROBENZENE
                        IN  THE UNITED STATES(3>4>
Company
Allied Chemical Corp.,
Industrial Chems . Div.
Chemical Products Corp.
Dow Chemical Co.
Monsanto Industrial
Chemical
PPG Industries, Inc.
Industrial Chem. Div.
Solvent Chemical Co., Inc.
Specialty Organics, Inc.
Standard Chlorine Chemical
Co., Inc.

Location
Syracuse (Solvay) , N.Y.
Cartersville, Ga.
Midland, Mich.
Sauget, 111.
Natrium, W. Va.
Maiden, Mass.
Niagara Falls, N.Y.
Irwindale, Calif.
Delaware City, Del.
TOTAL
Annual
Capacity,
Ib x 106
12
3
16
12
21
5 (a)
10
2(b)
60(b)
141
1974
Production
Ib x 106
9.0
NA
NA
NA
NA
12.0
2.0
24.0

(a)   Production will be phased out in late 1974.

(b)   These are processors — they buy crude mixed chlorinated benzenes
     and purify them.

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                                    56
Manufacturing Process

           Paradichlorobenzene Is  produced almost entirely as a by-product
from the manufacture of monochlorobenzene, which is produced by the
chlorination of benzene.  Generally,  prolonged chlorination is used to
produce various by-products besides  PDCB, as shown in  the following reaction
chemistry:
              C12
Benzene    Chlorine
Monochloro
 benzene
 (70-75%
  yield)
                                        Cl
            Cl
Ortho        Para
Dichlorobenzenes
 (10-207. yield)
                                              Clx  +  HC1
Polychloro
benzenes
           Benzene and chlorine are  reacted in a chlorinator.   The product
is neutralized by sodium hydroxide  with the recovery of  dichlorobenzene.
The production and waste material handling are shown in  Figure 12.
                     Beruent or
                     chlorobenjena
                                  Wat*
                                      •Vtnt
Bcnrene
Chlorine


Hydrochloric
acid *"
Chlorinator



-^Scrubber j


li
•"T Hydrochloric
Sodium «cid *
hydroiuda
Ntutraliiinc ». f
tank "'[
                              B«nztn« and water
                              Beniena and cMorobanzan*
                              CMorobinimi
                                                     Oichloro- and
                                                    polychlorobantantt
                                                     to distillation
                                          DicMorobtntan*
                                             sludft
                                            to f•covwy
               FIGURE  12.
     PRODUCTION AND WASTE HANDLING     x10N
     SCHEMATIC FOR PARADICHLOROBENZENE

-------
                                   57
Raw and Waste Material Handling

          The essential raw materials used in the manufacture of PDC8
are:  benzene, chlorine, and sodium hydroxide.  The main toxic materials
that  need  special handling during PDCB manufacture are chlorine, HC1,
and PDCB.  Most firms do adopt some precautionary measures for their em-
ployees such as wearing of plant coveralls, rubber gloves, goggles,
safety glasses, hard hats, and face shields and respirators when necessary.
          The material flow within a typical plant is shown in Table 12.
At Dow Chemical, the HC1 by-product is apparently recycled to chlorine
production while trichlorobenzenes are recovered.
          At Monsanto, the HC1 is recovered as muriatic acid with only
small amounts escaping through vents or going to a waste treatment plant.
The PDCB work area is ventilated and the exhaust air goes to a wet scrubber.
Monsanto is reported to monitor the PDCB concentration level.

Air Contaminant Emissions, Sources, and Rates

          Sources of air emissions are chlorinator, PDCB recovery system,
and the press room.  The pollutants emitted are hydrochloric acid, chlorine,
benzene, chlorobenzene, and PDCB.  Data are unavailable on the rates of
emission of these compounds, making the nationwide emission status difficult to
estimate.  Pollutants emitted from various sources are presented in Table 14.
          Minor emissions such as chlorine and HC1 are given off at the
wastewater treatment plant.

Air Contaminant Emission Control

          Among the pollution control equipment used to control the gaseous
and particulate emissions are wet scrubbers and absorption columns.   An
estimate of control efficiencies at the Standard Chlorine Company is pre-
sented in Table 15.

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                       TABLE 14.  AIR POLLUTION EMISSIONS, SOURCES, AND RATES FROM
                                  PARADICHLOROBENZENE MANUFACTURE AND WASTE TREATMENT
Sources of Emissions
Participates
Rates,
Lb/hr
Gases/Vapors
Rates,                Rates,
Ib/hr      Odor   Odor Units/hr
Manufacturing Processes

  Chlorinator
  P-dichlorobenzene
   Recovery

  Press Room
  PDCB
  Chloride

  PDCB
           (1)  HC1
           (2)  Benzene
           (3)  Chlorobenzene
           (4)  C12

                Chlorobenzene
                             Same
                             Same
                             Same
                             Same

                             Same
                                          Same
                                                                   oo
Uastewater Treatment
                                                         (1)  Cl.
                                                         (2)  HC1
                                                           Same

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                                59
        TABLE 15.  AIR POLLUTION CONTROL AT STANDARD
                   CHLORINE
Water Device
Efficiency,*
 percent
     Compound
    Controlled
Water Scrubber
Absorption
 Column
    90
    95
(1)  HC1
(2)  Benzene
(3)  Chlorobenzene
(4)  Dichlorobenzene
(5)  Paradichlorobenzene
(1)  HC1
(2)  Chlorobenzene
(3)  Benzene
* Controlled emission data were not provided by any one
  company.

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                                  60

          borne companies, for example, Allied, Solvent, and Specialty,
with annual capacities around 10 million pounds, do not utilize control devices,
They argue that it will be too restrictive if they are compelled to have all
p-dichlorobenzene operating areas confined and exhaust air sent through a
scrubbing system.  The size of the control hood will be too large due to the
extensive area involved.
          However, Standard Chlorine has controls in place (water scrubber
and column absorber as given above) and the Monsanto Industries controls by
means of water scrubber only.  The press room is not controlled.  Emission
from this area is primarily PDCB.~
          The acceptable level of paradichlorobenzene used as the Threshold
Limit Value by American Conference of Governmental Industrial Hygienists
(ACGIH) is 75 ppm.  It is not known whether the concentration in the press
room exceeds this range, since there are no measured data.

Control Cost

          Standard Chlorine provided the following control costs.  Standard
has an annual design capacity of 50 million pounds.

                                            Capital      Operating
          Control System        Size        Cost($)      Cost($/vr)
          Water Scrubber^2)   48" & 16"      28,000       40,000
          Carbon Absorption                 100,000         NA
            Columns

Significance of Air Contaminant Emission

          The nature of the pollutants emitted during the manufacture of
PDCB requires that these substances be controlled.  The control of PDCB
to about 75 ppm in the working area is significantly Important because of
its high toxicity to humans.*  There are no source emission standards for
these compounds for the industry.  Comparison with standards, if any,
established for similar industries is not possible since the emission rates
are not known.  Further study is, therefore, required to be able to adequately
assess the significance of these emissions.
 * 75 ppm is the toxic level for humans.

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                                    61
                               SECTION V
                               REFERENCES


 (1)   Rumker,  Rosetnarie Von,  E.  W.  Lawless,  and  A.  F.  Meiners,  "Production,
      Distribution,  Use, and  Environmental  Impact Potential of  Selected
      Pesticides", For Council  on Environmental  Quality,  Washington,  D.C.,
      Contract No. EQC-311 (15  March 1974).

 (2)   United States  Tariff Commission Report - Synthetic  Organic Chemicals
      (1970, 1971, 1972, 1973).

 (3)   1974 Directory of Chemical Producers-Chemical Information Services
      Stanford Research Institute,  Menlo Park, California, pp 513,  747,
      753, 755, 759, and 761  (1974).

 (4)   Chemical Marketing Reporter,  Vol.  203, No. 21, p 9  (1973).

 (5)   "Controlled-Release Pesticides Attract Interest", Chemical and  Engineering
      News (September 30, 1974).

 (6)   Lawless, Edward W., Rosemarie Von  Rumker,  and Thomas L. Ferguson, "The
      Pollution Potential in  Pesticide Study Series 5", EPA Technical Studies
      Report:   TS-00_72-04 (June, 1972).

 (7)   Stutz, C. N.,  "Treating Parathion  Wastes", Chemical Engineering Progress,
      Vol. 62, No. 10 (October,  1966).

 (8)   Abel, Dorothy  J., "Guide  to State  Stationary Source Emission  Standards",
      Buyers'  Guide  Issue, p  27  (1975).

 (9)   Chemical Marketing Reporter,  Vol.  201, No. 12 (March 20,  1972).

(10)   U.S. Patents Nos. 2, 131,  and 259  (Dow, 1938) and 2,447,790 (Reichhold, 1960),
      Also, Chemical Process  Review, No. 5,  Pesticide  Production Processes  -(1967).

(11)   Chemical Marketing Reporter,  Vol.  203, No. 15 (April, 1973).

(12)   Faith, W. L.,  D. B. Keyes, and R.  L.  Clark, Industrial Chemicals. Third
      Edition, John  Wiley and Sons, Inc., New York (1965).

(13)   Atkins,  Patrick R., "The  Pesticide Manufacturing Industry-Current Waste
      Treatment and  Disposal  Practice",  For  Environmental Protection  Agency,
      Project #12020FYE (January, 1972).

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            APPENDIX A
SUMMARY OF THE SELECTED PESTICIDES
      AND THEIR PRODUCERS

-------
                             TAIU A-I.  1*1*1 cuua, rtopuauu, ROMCUM vauna A*D normm of SIUCTU
o u Coapouada Producara
1. Inaactlclda Hatbyl paratoloa tarr.HcCaa
Corporation

IHonaanto Conpany
Agricultural
DUlalon
Itauffar Chaaical
Conpany
Agricultural
Chnlc-1 Dl«.
„ Vlckaburg Chaalcal
t Conpany
Vatilcol Chaa.'
Corporation
l.'ln-actlalda Toxaphana Harcula-. Inc.
 aalld
a.p. «9-
H a







Claai Mlatioa Solution coacantrati

                            Agricultural
                            OlTlaloa

                          Tlnaland Chaaleal
                            Coapany
Vlnaland,      Waad-Hoa«,
  Ha« Jaraay   Haad-g-lao*
              Dai-l-taJ*
4. Harblclda \ Trlfluralln Ell Lilly and
5 Coapany
*-*
|
1
&
j. pumtclda Pantachlorophanol
and wood 0^ Ch*«lcal
^•••rv«tlv« coSaJIIy
Hoaiatnto tnduit.
ChaHical CoBpcny
•± UlehholdChaic.il
I
K Itutford CtiMtcal
QeBptty
•* • Vulcan lUttriali
Cimptnj. Cl»i-
c«U DlvUlcm
i. Pt-«i,|«i.c Fatrtdichioco* Allied Chmlcal
iMtiMD.* Corpor«clon
InduitrUl Cheat-
1 Chemical Produce*
I Corporation
Dow Ch«ie«l
Coa^Ot
Nonaanto Induat.
Chaalcal Coapany
PP5 Induatrlaa,
loo., Industrial
Chaalcal Dlvialon
tolvant Chealcal
Coapany, Inc.


tpaelalty Organtca ,
Inc.
Standard Chlorlna,
Chanleal Ccmpany
Inc.
tafayatta, TraflaafJ
Indiana



I
Midland, Dowieldaft
Michigan
Saugat,
llllnola
Tacoaa, Chloraphan*
Kaahlngtoa
Houatoa. Taxaa

Ulehlta, bnaaa


Syracuaa,
(Solvay)
Na» York
Cartarrtlla,
Gaorgla
Hldlaad,
Mlchlgm
Saugat.
Illlnota
Hatrla.Uaat
Virginia

Haldan,
Haaiachuaatta
llagarn Falla,
KM York
Irvlndila.'
California
Dalowara City,
D-lawara

23




19

16

16
1*

It


12


1

U

12

21


S

10

I

40


XA Q.iOiorTr-l'taoro.i t-cllnltro-H,*- Yallua ayaaga lanlalflBbla con*
tlanajrl-a-tolaldlna b.p. •»- caatrata, granular
an 17 C
/ 	 (^ «..ctLO. «•»• *••»•
•' \ S**! ^^ 4*C
/ *
HOj "™1 ~»^~J
• M ••••«fci Ha.it* ..... _. 	 ..
aall* caatrata. vatlabla
,0.0 •">. »-» « K-*"
CI CI
«> — v.
>— ?^
ci a
K.7


-•" ' klata aolld CtyaUla
a.p. U C

IA

IA

IA / ^<
• \^ y *•
M


11.0

IA

2.0

24.0


• Hoc -v-lUbla.

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                APPENDIX B
SUMMARY OF NONPROPRIETARY INFORMATION OBTAINED
     FROM THE SURVEY OF PESTICIDE PLANTS

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        TABLE B-l.   SUMMARY OF AIR CONTAMINANT EMISSIONS,  SOURCES,  AND RATES
Pesticide
       Sources
                                  Major Compound     Rates,
                                     Emitted         Ib/hr
Methyl Parathion
1.  Reactor

2.  Chlorinator

3.  MPT Unit
4.  Waste Treatment Incinerator

                Wastewater
                                  P2°5
                                                        HC1
                                                        S
                                                        NaCl
                                                        P2°5
                                                        H2S
                                                        Mercaptan
                                                      460

                                                      420
                                                      460
                                                     1550
Toxaphene
1.  <& -Pinene Production
2.  Camphene-Production
3.  Chlorination - Toxaphene
                      4.  Toxaphene Granular
                          Production
                      5.  Wastewater Treatment
                                  N.A.
                                  HC1

                                  Toxaphene

                                  C12
                                  HC1
                                                                           4350
MSMA
1.  Sodium Arsenite Production
2.  DMSA
                      3.   MSMA Production

                      4.   MSMA Processing
                      5.   Waste Treatment
                                  As203
                                  CH3C1
                                  (CH3)20
                                  N2S°4
                                  MSMA
                                  MSMA
                                  N.A.
6.44 x 10"8
Trifluralin
1.  Nitration
                      2.   Condenser
                                  Salt of Nitrate,
                                  sulfate, chloride
                                  HF
                                  Nitrogen oxides
                                  CHCU
                                                                               1
                                                                               3
                                                                               3
                                                        Trifluratin

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                                         B-2
           TABLE B-l.  SUMMARY OF AIR CONTAMINANT EMISSIONS,  SOURCES, AND RATES
Pesticide
       Sources
Major Compound     Rates,
   Emitted         Ib/hr
Pentachlorophenol
1.   Pentachlorophenol
                      2.   Acid System Reactors
Chlorinated
  Phenol
C12
HC1
Chlorinated
  Phenol
HC1



^fcaradichloro-
^^ benzene
3.
4.
5.
1.
Ingot Casting
Shotting Operation
Wastewater Treatment
Chlorinator
PCP
PCP
N.A.
HC1
                      2.   Recovery

                      3.   Press  Room
                      4.   Wastewater Treatment
                                  Chlorobenzene
                                  C12
                                  PDCB
                                  Chlorobenzene
                                  PDCB
                                  C12
                                  HC1
(a)  Not available.

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                                   TABLE B-2.   SUMMARY OF AIR EMISSION CONTROL DEVICES, EFFICIENCY, AND COST
Pesticide
Methyl Par a th ion


Toxaphene

KSMA


Trifluralin
Pen tach lorophenol


Paradichlorobenzene



Source of
Information
Monsanto
Monsanto
Monsanto
Hercules
Hercules
Hercules
Hercules
Diamond
Ansul
Diamond
Eli Lilly
Reichhold
Reichhold
Reichhold
Standard Chlorine
Standard Chlorine
Standard Chlorine
Standard Chlorine
Control Device
(a)
Incinerator (H S, S, mercaptan)
Water Scrubber (P2°5» Hcl>
Brink Mist Eliminator (P20 for visibility)
Alkali and Water Scrubber (solvent vapor, HC1, Cl.)
Stripping (solvent vapor, HC1, Cl )
Limestone Adsorption (solvent vapor, HC1, Cl )
Baghouse (toxaphene)
Baghouse (As 0_)
Water Scrubber (As.O.)
Acidifier Vent Scrubbers
1- and 2-Stage Venturi Scrubber and Tri-mer
Wet Scrubber
Packed and Venturi Scrubber (Cl., Phenol, acids)
Bay Filters (PCP)
Mechanical Seals (for PCP reactor)
Water Scrubbers
(HC1, benzene, chlorobenzene, etc.)
Absorption Column
(HCl, benzene, chlorobenzene)
Efficiency Capital
(b)
95
99.9

100
8,000

500
90 1,000,000
99-100 80,000
95-99 70,000
50,000
90 28,000

95
100,000
Operating





200

100

1,000
6,000
6,200
40,000



(a)  Compounds in parentheses are controlled by the preceding control device.
(b)  Blanks show data not available.

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                                        B-4
             TABLE B-3.  LIST OF CONTACTS HAVING EXPERTISE AND SOURCES OF
                         SIGNIFICANT INFORMATION ABOUT SELECTED PESTICIDE INDUSTRIES
Representative, Affiliation, Address
      and Telephone Number
                                       Comment on
                                 Usefulness of Contact
The Ansul Company
Alan L. Haase
Marinette, Wisconsin
(715) 735-7411
54143
Diamond Shamrock Chemical Company
W. R. Taylor
1100 Superior Avenye
Cleveland, Ohio
(216) 694-5000

Hercules Incorporated
H. E. Hicks
Brunswick, Georgia  31520
Eli Lilly and Company
Arlie J. Ullrich
Indianapolis, Indiana
 46206
Monsanto Industrial Chemicals Company
P. E. Heisler
Sauget, Illinois  62201
(618) 271-5835

Reichhold Chemicals, Inc.
J. C. Manlove
P. 0. Box 1482
Tacoma, Washington  98401

Standard Chlorine Chemical Company, Inc,
P. F. Romano
1035 Belleville Turnpike
Kearny, New Jersey  07032
(201) 997-1700

Stauffer Chemical Company
Dan Simmons
Mt. Pleasant, Tennessee
(203) 226-1511

Vulcan Materials Company
R. A. Bondurant, Jr.
P. 0. Box 545
Wichita, Kansas  67201
(316) 524-4211
                               Production data and control
                               given.
                               Production data, control
                               method, and costs given.
                               No production data, simple
                               statement on process.
                               No production data.
                               Emission data given.
                               No production estimates,
                               but control methods and
                               costs were provided.
                               Very good response.
                               Estimates of production data,
                               production and control flow
                               sheet and costs.

                               Production data, control
                               method, and cost given.
                               Production data only.
                               Production data, control
                               method, and cost provided.

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             APPENDIX C
SAMPLE OF LETTER MAILED TO SELECTED
 PESTICIDE MANUFACTURING COMPANIES

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August   , 1974
Gentlemen:

Battelle's Columbus Laboratories under contract to the Strategic Studies
Unit of  the Office of Pesticide Programs, Environmental Protection Agency
is working to develop background information and determine the significance
of emissions from pesticide plants.

For this study, the following six pesticides have been selected:

     (1)  Insecticides - Methyl Parathion and Toxaphene

     (2)  Herbicides - MSMA and Trifluralin

     (3)  Fungicides and Wood Preservative - Pentachlorophenol

     (4)  Fumigant - P-Dichlorobenzene.

One of the objectives of this information gathering is to obtain factual
information from the manufacturing industries so that determination can
be made of

     (1)  The extent of ambient emission of the pesticides

     (2)  The type of compounds emitted

     (3)  Currently employed methods of emission control.

From the above data, the study will seek to project future emissions, relate
it to similar emission from other sources, and thus obtain a quantitative
estimate for the significance of pesticide emissions from the manufacturing
sector.

Please find attached a list of six questions, which we request you to complete
and return to us at your earliest convenience.  We will keep any information
you supply within BCL files so that the confidentality of your data is preserved,

We appreciate your willingness to cooperate and would like to assure you that
any assistance you will provide will be of immense value to this study required
under the Clean Air Act of 1970.

Cordially,
C. N. Ifeadi
Research Scientist
Waste Control and Process
  Technology Section

Attachment:  Questionnaire

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                                       C-2
        Manufacturing Company
Address
Name, position, and phone number of person responding
Name of pesticide produced
Question 1.  Design Capacity and Production
                     Design Capacity,       Months          Actual Production,
    Year             millions of Ib      In Operation         millions of Ib  .
1970                    	           		
1971                    	           	             	
1972                    	           	             	
1973                    	           	.            	
1974  (Estimate)         	           	             	
1975  (Estimate)         	           	             	
Provide details of any technical or economic situation that may affect future
          or decreases in your plant production.
Question 2.  Process Description
Give a brief description of the processes used to produce the pesticide.  Specify
the raw materials, by-products, and waste materials.  Amplify with simple production
chemistry and attach simple flow sheets.

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                                       C-3
Question 3.  Raw and Waste Material Handling with the Plant

Particular attention is generally paid to materials handling within the plant,
since the raw and waste materials may have high toxicity.  Briefly descrube the
precautions taken in your plant.
Question 4.  Air Contaminant Emissions and Control
Manufacturing Plant
Site
Particulates
^pes
Odor
Waste Disposal Site
Particulates
Gases
Odor
Emission
Sources






Compounds
Emitted






Controlled
Yes or No






Method of
Control






Emissions
(lb/ton)*






Efficien<
(%)






* Or any other unit employed by your facility.
Describe briefly the emission control system used in your plant for particulates,
gases, odor, and visibility control.  Describe problems of visibility and odor, if
any, around your plant.  Information or nature of odor complaints, if any, from
the public in your area will be useful in obtaining an idea of the odor problems
associated with your plant.

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                                       C-4
Question 5.  Cost of Emission Control System
Name of Control System     Size      Capital Cost ($)     Operating Cost  ($/yr)
Question 6.


Please indicate the status of air emissions from your facility as (a) acceptable
(b) needs improvements?  Comment on the economic impact of restricting the
emissions from your plant to levels considered (a) reasonable (b) too restrictive,
State what you think these levels should be.

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