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               AIR POLLUTION ASPECTS

                        OF

                  HYDROGEN SULFIDE
                 Prepared for the
   National Air Pollution Control Administration
Consumer Protection & Environmental Health Services
   Department of Health, Education, and Welfare
            (Contract No. PH-22-68025)
             Compiled by Sydney Miner
               Litton Systems, Inc.
          Environmental Systems Division
                7300 Pearl Street
             Bethesda, Maryland 20014

                  September 1969

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                          FOREWORD


       As the concern for air quality grows, so does the con-

cern over the less ubiquitous but potentially harmful contami-

nants that are in our atmosphere.  Thirty such pollutants have

been identified, and available information has been summarized

in a series of reports describing their sources, distribution,

effects, and control technology for their abatement.

       A total of 27 reports have been prepared covering the

30 pollutants.  These reports were developed under contract

for the National Air Pollution Control Administration  (NAPCA) by

Litton Systems, Inc.  The complete listing is as follows:


    Aeroallergens (pollens)       Ethylene
    Aldehydes (includes acrolein  Hydrochloric Acid
      and formaldehyde)           Hydrogen Sulfide
    Ammonia                       Iron and Its Compounds
    Arsenic and Its Compounds     Manganese and Its Compounds
    Asbestos                      Mercury and Its Compounds
    Barium and Its Compounds      Nickel and Its Compounds
    Beryllium and Its Compounds   Odorous Compounds
    Biological Aerosols           Organic Carcinogens
      (microorganisms)            Pesticides
    Boron and Its Compounds       Phosphorus and Its Compounds
    Cadmium and Its Compounds     Radioactive Substances
    Chlorine Gas                  Selenium and Its Compounds
    Chromium and Its Compounds    Vanadium and Its Compounds
      (includ.es chromic acid)     Zinc and Its Compounds


       These reports represent current state-of-the-art

literature reviews supplemented by discussions with selected

knowledgeable individuals both within and outside the Federal

Government.  They do not however presume to be a synthesis of

available information but rather a summary without an attempt

to interpret or reconcile conflicting data.  The reports are

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necessarily limited in their discussion of health effects for

some pollutants to descriptions of occupational health expo-

sures and animal laboratory studies since only a few epidemio-

logic studies were available.

       Initially these reports were generally intended as

internal documents within NAPCA to provide a basis for sound

decision-making on program guidance for future research

activities and to allow ranking of future activities relating

to the development of criteria and control technology docu-

ments.  However, it is apparent that these reports may also

be of significant value to many others in air pollution control,

such as State or local air pollution control officials, as a

library of information on which to base informed decisions on

pollutants to be controlled in their geographic areas.  Addi-

tionally, these reports may stimulate scientific investigators

to pursue research in needed areas.  They also provide for the

interested citizen readily available information about a given

pollutant.  Therefore, they are being given wide distribution

with the assumption that they will be used with full knowledge

of their value and limitations.

       This series of reports was compiled and prepared by the

Litton personnel listed below:

       Ralph J. Sullivan
       Quade R. Stahl, Ph.D.
       Norman L. Durocher
       Yanis C. Athanassiadis
       Sydney Miner
       Harold Finkelstein, Ph.D.
       Douglas A. Olsen, Ph0D.
       James L. Haynes

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       The NAPCA project officer for the contract was Ronald C.




Campbell, assisted by Dr. Emanuel Landau and Gerald Chapman.




       Appreciation is expressed to the many individuals both




outside and within NAPCA who provided information and reviewed




draft copies of these reports.  Appreciation is also expressed




to the NAPCA Office of Technical Information and Publications




for their support in providing a significant portion of the




technical literature.

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                         ABSTRACT






        Hydrogen sulfide gas is very toxic to humans and at



concentrations over 1,000,000 |jg/m3 quickly causes death by



paralysis of the respiratory tract.  At lower concentrations



it causes conjunctivitis with reddening and lachrymal secre-



tion, respiratory tract irritation, pulmonary edema, damage



to heart muscle, psychic changes, disturbed equilibrium,



nerve paralysis, spasms, unconsciousness, and circulatory



collapse.  One outstanding episode in Mexico involving acci-



dental release of hydrogen sulfide killed 22 people and 50



percent of the exposed animals and hospitalized 320 persons.



The gas has a very obnoxious odor at low concentrations



(1 to 45 |-tg/m3 ).  At concentrations below 60,000 l-ig/m3 it



has very little effect on plants.  Hydrogen sulfide also



tarnishes silver and copper and combines with heavy metals



in paints to discolor or darken the paint surface.



        The primary natural source of hydrogen sulfide is



biological decay of protein material in stagnant water.  In-



dustrially, hydrogen sulfide is a by-product of many processes.



Main industrial producers are kraft paper mills, oil refin-



eries, natural gas plants, and chemical plants manufacturing



sulfur-containing compounds.  Hydrogen sulfide is also pro-



duced in sewers and sewage disposal plants.  Average concen-



trations of hydrogen sulfide in urban atmospheres are reported



to range from 1 to 92 ug/m3, with most urban averages reported



at less than 10 ug/m3.

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        The installation of black liquor oxidation systems



and scrubbers has substantially reduced emissions from kraft



paper mills.  Wet scrubbers using various absorbents and



iron oxide are used in refineries, natural gas plants, coke



ovens, and chemical plants to remove hydrogen sulfide from



gas streams.  Incineration is also used to reduce emissions



of the gas.



        Hydrogen sulfide corrosion of silver has required



substitution of gold contacts in electrical appliances at



an estimated increased cost of $14.8 million during 1963.



Abatement of air pollution resulting from the pulp and



paper industry, in which hydrogen sulfide is a major factor,



has cost approximately $10 million per year and is predicted



to increase to $15 million per year in the immediate future.



Major expenditures have been made by refineries and natural



gas plants to remove hydrogen sulfide from sour gases and to



recover sulfur as a valuable by-product.



        Analytical techniques based on the methylene blue



and molybdenum blue methods are available for laboratory



analysis of hydrogen sulfide.  The spot method for measuring



hydrogen sulfide,  based on tiles or paper impregnated with



lead acetate,  is also widely used.

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                       CONTENTS



FOREWORD

ABSTRACT

1.  INTRODUCTION 	   1

2.  EFFECTS	   2

    2.1  Effects on Humans	   2
         2.1.1  Odor Threshold	   3
         2.1.2  Pollution Occurrences  	   4
    2.2  Effects on Animals	   6
         2.2.1  Commercial and Domestic Animals  ....   6
         2.2.2  Experimental Animals 	   6
    2.3  Effects on Plants	11
    2.4  Effects on Materials	16
         2.4.1  Effects on Paint	16
         2.4.2  Effects on Metals	19
    2.5  Environmental Air Standards	20

3.  SOURCES	22

    3.1  Natural Occurrence  	  22
    3.2  Production Sources  	  22
         3.2.1  Petroleum Industry  	  23
         3.2.2  Petrochemical Plant Complexes	26
         3.2.3  Kraft Mills	28
         3.2.4  Coke Ovens	32
         3.2.5  Mining	35
         3.2.6  Iron-Steel Industry and Foundries   ...  36
         3.2.7  Chemical Industry   	  36
         3.2.8  Animal Processing Plants and
                  Tanneries	38
    3.3  Product Sources	40
    3.4  Other Sources	40
         3.4.1  Combustion Processes 	  40
         3.4.2  Polluted Water	42
         3.4.3  Well water	43
         3.4.4  Sewage Plants and Sewers	43
    3.5  Environmental Air Concentrations	44

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                 CONTENTS  (Continued)
4.  ABATEMENT	46

    4.1  Kraft Paper Mills   	 46
    4.2  Petroleum Industry  and Petrochemical Plants   .  • 50
    4.3  Coke-Oven Plants and Chemical Plants 	 51
    4.4  Coal Piles	52
    4.5  Tanneries	52
    4.6  Sewers and  Sewage Plants	53
    4.7  General Abatement Systems	54

5.  ECONOMICS	55

6.  METHODS OF ANALYSIS	59

7.  SUMMARY AND CONCLUSIONS	66

REFERENCES

APPENDIX

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                       LIST OF FIGURES
1.  Time-Mortality Toxicity Curve for Houseflies Exposed
    to 1,500,000 |ag/m3 Hydrogen Sulfide	    8

2.  Exposure Time Versus Concentration for Hydrogen
    Sulfide Effects 	   18

3.  Crude Capacity of U.S. Refineries	25

4.  Natural Gas Production and Plant Production of Ethane
    and Liquid Propane Gas (LPG) for Fuel and Chemical
    Use	27

5.  Relation Between Hydrogen Sulfide Production and
    Furnace Loading 	   31

6.  Approximate Cost of Gas Desulfurization Plants in
    1967	57

7.  Sulfur-Recovery Plant Investment  	   58

8.  Location of Kraft Mills in the U.S. in 1957	95

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LIST OF TABLES
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
Odor Detection Threshold of Hydrogen Sulfide ....
Protection Index of Sodium Nitrite and PAPP Pretreated
Time in Minutes Until 50% Injury to Exposed Plant
Surfaces at 1,500,000 M.g/m3 Hydrogen Sulfide ....
Sulfur Production From Hydrogen Sulfide in the U.S..
Hydrogen Sulfide Emissions from Kraft Mill
Estimated Hydrogen Sulfide Emissions from 650 ton/day
Frequency Distribution of Hydrogen Sulfide Concentra-
tions, 1961-62 	

Sources of Hydrogen Sulfide Emissions in Coke Plants
Hydrogen Sulfide Concentrations at Various Distances
Atmospheric Air Pollution by Hydrogen Sulfide at
Different Distances from Source of Pollution ....


Time Required for 50% Mortality of Subjects Treated
Typical Gross Findings at Autopsy of Rats and Mice
Which Died During Exposure to Hydrogen Sulfide . . .
Percentage of Leaf Area Marked by Hydrogen Sulfide .
Relative Sensitivity of Plants to Hydrogen Sulfide .
5
11
14
21
24
30
31
32
33
34
39
39
41
45
86
87
88
90
91

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                     LIST OF TABLES (Continued)






20.  Crude Oil Capacity in the U.S. as of  Jan. 1969  ...   92




21.  Kraft Pulp Production in the United States	   93




22.  U.S. Coke Production	   94

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1.  INTRODUCTION




            Hydrogen sulfide (H3S) is a colorless gas that has



    an obnoxious odor at low concentrations.  The odor threshold



    is in the |-ig/m3 range.  In higher concentrations, the gas is



    toxic to humans and animals and corrosive to many metals.



    It will tarnish silver and react with heavy metals in paints



    to discolor the paint.  In humans, it will cause headache,



    conjunctivitis, sleeplessness, pain in the eyes, and similar



    symptoms at low air concentrations and death at high air



    concentrations.  However,  the majority of the complaints



    arising from hydrogen sulfide air pollution are due to its



    obnoxious odor in extremely low air concentrations.



            Air pollution by hydrogen sulfide is not a widespread



    urban problem but is generally localized in the vicinity of



    an emitter such as kraft paper mills, industrial waste dis-



    posal ponds, sewage plants, refineries, and coke oven plants.

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2.   EFFECTS




    2.1  Effects on Humans




            Hydrogen sulfide/ which is very toxic to humans,




    generally enters the human body through the respiratory tract,




    from which it is carried by the blood stream to various body




    organs.  The hydrogen sulfide that enters the blood can lead




    to blocking of oxygen transfer, especially at high concentra-



          1 OP
    tions.^  In general, the hydrogen sulfide acts as a cell




    and enzyme poison and can cause irreversible changes in




    nerve tissue. 4'101




            At high concentrations (over 1,000,000 ug/m3),  hy-



    drogen sulfide frequently causes death quickly by paralysis



    of the respiratory center. °^  However, if the victim is




    moved quickly to uncontaminated air and respiration initiated


                                                              QQ

    before heart action stops, rapid recovery can be expected.




    At lower concentration,  hydrogen sulfide causes conjuncti-




    vitis, lachrymal secretion, respiratory tract irritation,




    pulmonary edema, damage to the heart muscle, psychic changes,




    disturbed equilibrium, nerve paralysis, spasms, unconscious-



    ness, and circulatory collapse. 0l'J-n2  gome common symptoms




    are metallic taste, fatigue, diarrhea, blurred vision,  in-




    tense aching of the eyes, insomnia, and vertigo.49'10!




    Some of the effects of hydrogen sulfide and the air concen-




    trations at which they occur are shown in Table 15 in the




    Appendix.

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        Hydrogen sulfide may produce synergistic effects in



mixtures with carbon disulfide hydrocarbons and carbon mon-



oxide. 01  In Russia, an increased effect was attained with


                                              102
a mixture of hydrogen sulfide and naphtha gas.    In addi-



tion, mixtures of carbon monoxide and hydrogen sulfide in



concentrations* that individually would not be dangerous


                                                        i o?
were harmful to animals after only 10 minutes' exposure. w<6



2.1.1  Odor Threshold



        Hydrogen sulfide has a characteristic smell of



rotten eggs,    and this odor is the most sensitive indica-



tor of its presence in low concentrations.  However, the



odor perception threshold varies considerably among indivi-



duals and apparently depends on the age and sex of the in-



dividuals, the size of the town they live in, and whether



they smoke.3  The reported odor threshold varies between 1



and 45 l-ig/m3 (see Table 1).  At 500 |~ig/m3, the odor is



distinct; at 4,000 to 8,000 ug/m3, the odor is offensive and



moderately intense; and at 30,000 to 50,000 ng/m3, the odor


                              99                / a
is strong but not intolerable.    At 320,000 ng/m , the



smell is not as pungent, probably due to the paralysis of



the olfactory nerves.102  The perception concentrations are



based on initial inhalations since continuous inhalation


                                     99
causes rapid olfactory sense fatigue.    At concentrations
        *Values not stated.

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over 1,120,000 M.g/m3 , there is practically no sensation of



odor and death can occur rapidly.     Loss of sense of smell



has even been reported at 150,000 p.g/m3 after exposures of


                     TOO
from 2 to 15 minutes.     Therefore, dulling of the olfactory



nerves constitutes a major danger to people who are exposed



to moderate and high concentrations of hydrogen sulfide


                     10?
for extended periods.



2.1.2  Pollution Occurrences



        The most serious episode reported involving hydro-



gen sulfide air pollution occurred in Poza Rica in Mexico



on November 24, 1950.  There was an accidental release of



gas from a hydrogen sulfide absorption unit in a natural



gas refining plant.    This resulted in the release of con-



siderable amounts of hydrogen sulfide, which quickly spread



to the residential areas where most people were asleep.  The



situation was aggravated by an atmospheric temperature in-



version with patches of haze and fog.  The gas was shut off



within 20 to 25 minutes, yet 22 persons died and 320 persons



were hospitalized as a result of this brief exposure. '



The effects were characteristic of hydrogen sulfide gas



poisoning: loss of sense of smell, cough, dyspnea, conjunc-



tival irritation, nausea, vomiting, severe headache, and



vertigo.    The incident was over before any atmospheric



measurements were made.



        In the Terre Haute, Ind., episodes in May and June

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                    TABLE 1

ODOR DETECTION THRESHOLD FOR HYDROGEN SULFIDE

    Odor Threshold
    	( ug/m3 )	Reference

         9-45                         3

         7.1a                        78

          .71b                       78

        15                           75

         6.8C                       142

        12-30                        41
             Hydrogen sulfide from sodium
             sulfide.

             Hydrogen sulfide gas.

            cMean value ratio of highest to
             lowest odor threshold concentra-
             tion detected by all observers
             in successive tests is 3.18.

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1964, hydrogen sulfide concentrations were sufficient to



cause foul odor, resulting in 81 public complaints of dis-



comfort and paint-blackening.  Of the complaints, 40 re-



ferred to property damage, and 41 referred to health effects,



The main symptoms reported were nausea, loss of sleep and



abrupt awakening, shortness of breath, and headaches.  How-



ever, almost none of those affected sought medical attention.



The source of the hydrogen sulfide was a 36-acre lagoon used



for biodegradation of industrial wastes.  Hydrogen sulfide



concentrations in the atmosphere during the episodes ranged



between 34 and 450 ug/m3.7



        A major pollution problem of kraft mills is the



emission of hydrogen sulfide and organic sulfide, causing



a disagreeable odor in the surrounding areas.  At times



atmospheric concentration of these gases adjacent to the



kraft mills have reached levels which are capable of pro-



ducing nausea, vomiting, headache, loss of appetite, dis-



turbed sleep, upset stomach, and hampered breathing.



2.2  Effects on Animals



2.2.1  Commercial and Domestic Animals



        Hydrogen sulfide produces about the same health



effects in domestic animals as in man at approximately the



same air concentrations.     The Air Pollution Control



Association Committee on Ambient Air Standards^ stated



(1964) that spontaneous injury to animals occurs at 150,000

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to 450,000 |-ig/m3 of hydrogen sulfide.  In the Poza Rica



incident, it was reported that all the canaries in the area



were killed and about 50 percent of the other animals died.



Among these were chicken, cattle, pigs, geese, dogs, and



cats.33'66



2.2.2  Experimental Animals



        Fyn-Djui -1 exposed 10 rats to 1,000 ng/m3 of hydro-



gen sulfide in chronic experimental conditions for 12 hours



per day for three months.  The exposure produced changes in



the functional state of the central nervous system, irrita-



tions in the mucosa of the trachea, and morphologic changes



in the brain cortex.  At concentrations of 20 |-ig/m3 , only



slight to negligible changes occurred in the functional



state of the nervous system, and there was barely perceptible



irritation to the mucosa of trachea and bronchi.^1  Weedon



et jil.139 exposed houseflies to hydrogen sulfide concentra-



tions of 1,500,000 jjg/m3 .  The percent of kill versus time



of exposure is shown in Figure 1.  They also exposed groups



of eight rats and four mice to hydrogen sulfide concentra-



tions of 1,500,000 |~ig/m3 , 380,000 |ag/m3 , 96,000 i-ig/m3 , and



24,000 Hg/m3 for periods up to 16 hours.  At 1,500,000 |~ig/m3



all the rats were active during the first 5 minutes.  At



the end of 5 minutes they lost their muscular coordination,



and by 11 minutes they were prostrate.  They all died in



29 to 37 minutes.  Similarly, the mice were active during

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                                                          8
    99
    90
  ^ 50


  0)
    10
       	I	I	I	I	I	L_
     i


      0.25     1      4     15     60    240    960


                     Minutes of Exposure
                        FIGURE 1




Time-Mortality Toxicity Curve for Houseflies Exposed
        to 1,500,000 |-ig/m3  Hydrogen  Sulfide
                                             139

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the first few minutes.  Marked lachrymation followed and




all died within 20 minutes.



        At exposures of 380,000 |-ig/m3 all the rats were



active, sniffing and rubbing their noses for the first 25



minutes, and then they became quiet.  Three rats were dead



when the experiment was discontinued at 22.9 hours.  The



mice exposed to the same concentrations exhibited the same



symptoms for the first hour of exposure.  At the end of 2



hours they were gasping and their abdomens were distended.



They all died at the end of 7 hours.



        The rats were not affected during the first hour of



exposure to 96,000 (jg/m3 .  Even after 16 hours, the surviving



rats seemed to be in fair condition, even though they were



lethargic and gasping.  The mice exposed to the same con-



centrations showed similar but more marked signs.  Only



one mouse survived after 16 hours' exposure, and it died 23



hours later.



        No abnormal symptoms were noticed at 24,000 iag/m3 .



A mouse exposed to the 24,000 i-ig/m3 concentration for 16



hours was sacrificed, and at autopsy all organs proved normal



throughout.  The time required to reach a 50 percent mor-



tality (TL50) rate in these experiments for the rats, mice,



and flies is shown in Table 16 in the Appendix.  Typical



gross findings at autopsy for exposed rats and mice are



shown in Table 17 in the Appendix.

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                                                          10
             QQ
        Patty   reported an experiment  in which a dog was


exposed to 1,500,000 lag/m3 of hydrogen  sulfide.  When first


placed in the atmosphere, the dog was frisky for a short


time; he then stopped, breathed laboriously for a moment,


fell, gasped, and remained motionless with legs extended.


At the end of 1 minute he was removed and given artificial


respiration, and he recovered fully in  1 to 2 minutes.

        Smith and Gosslen-'-^O found that pretreatment of


mice with sodium nitrate and p-aminopropinphenone (PAPP)


significantly prolonged their survival  during continuous


exposure to hydrogen sulfide.  The mice were exposed to


1,100,000 |-ig/m3 , 1,500,000 |~ig/m3 , and 2,840,000 |~ig/m3 ;


the greatest protection occurred at the intermediate concen-


tration as shown in Table 2.  Propylene glycol also prolonged


the life of the mice.  For the propylene glycol to be


effective at the middle concentration (1,100,000 p.g/m3 ),


exposure to hydrogen sulfide has to be  delayed for 30


minutes after treatment.  At the highest concentration


(2,840,000 |J.g/m3 ), propylene glycol did not have any effect,


even when exposure to the hydrogen sulfide was delayed 30


minutes.

        Baikov   found that there were  no noticeable adverse


effects to rats after exposure for 70 days, 24 hours per day,


to air containing 8 ug/m3 of hydrogen sulfide and 10 ug/m3


carbon disulfide (the Russian environmental standard).

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                                                    11
                    TABLE  2

THE PROTECTION INDEX* OF SODIUM NITRITE  AND PAPP
  PRETREATED MICE EXPOSED TO HYDROGEN SULFIDE120
           (Total Number of Mice = 107)
Hydroqen Sulfide (ppm)
Pretreatment
Nitrite
PAPP (no delay)
PAPP (30-minute delay)
*Protection index = mean
722 985
2.3 3.8
1.6 3.5
1.3
survival time of protected
1,872
1.4
2.4
2.2
mice
                 mean  survival 'time  of  control  mice

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                                                         12
2.3  Effects on Plants



        There is little evidence that hydrogen sulfide



causes significant injury to field crops at environmental



air concentrations.66'123


                84
        McCallan0^ observed that little or no injury occurred



to 29 species of plants when they were fumigated with less



than 60,000 i-ig/m3 of hydrogen sulfide for 5 hours.  After



5 hours at 600,000 iag/m3 , some species were injured, but



not all.  Boston fern, apple, cherry, peach and coleus



showed no appreciable injury at concentrations below 600,000



Hg/rn3 .  At concentrations between 60,000 and 600,000 |jg/m3 ,



gladiolus, rose, castor bean, sunflower, and buckwheat



showed moderate injury.  Slightly more sensitive were tobacco,


                             84 148
cucumber, salvia, and tomato. r"J-rr
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                                                          13
1,500,000 p-g/m3 for periods of 1, 4, 15, 60, 240, and 960



minutes.  They found that hydrogen sulfide was only mildly



toxic to plant tissue.  They also made measurements of pH




changes in leaf and stem tissue of tomato plants.  At low



hydrogen sulfide concentrations, they found no significant



changes in pH.  At high hydrogen sulfide concentrations



(1,500,000 |jg/m ) the whole plant showed only a slight drop



in pH.  Once the pH changed, there was no recovery.  They



found very little correlation between the hydrogen sulfide-



caused pH change and plant damage.



        The time in minutes until 50 percent of the exposed



plant surfaces were injured at 1,500,000 i-ig/m3 of hydrogen



sulfide is shown in Table 3.



        Barton   exposed dry and soaked radish and rye



seeds to hydrogen sulfide in concentrations of 380,000 |-tg/m3



and 1,500,000 ug/m3 for periods of 1, 4, 15, 60, 240, and



960 minutes.  He found that the gas is relatively nontoxic



to the seeds.  The germination percentages for both rye and



radish were similar to the control lots, and there was no



delay in germination for the dry seeds.  Germination for



the soaked seeds of both rye and radish was delayed 4 to 6



hours after 240 minutes' exposure and 21 to 24 hours after



960 minutes' exposure to 1,500,000 |ag/m3 .  At 380,000 |_ig/m3 ,



soaked radish seed had no delay in germination, but a 28-hour



delay in germination of soaked rye seed resulted from a 960-



hour exposure at 1,500,000 iag/m3 .

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                                                         14
                         TABLE  3

 TIME IN MINUTES UNTIL 50 PERCENT  INJURY TO EXPOSED  PLANT
      SURFACES AT 1,500,000 ng/m3  HYDROGEN SULFIDE136
                                                    Time  in
Plant Surface	Plant	Minutes

Leaves                     Tomato                       30

                           Buckwheat                    60

                           Tobacco                     100



Stems                      Tomato                       45

                           Buckwheat                   120

                           Tobacco                     480

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                                                          15
                          20
        Benedict and Breen   fumigated 10 weeds which occur



widely throughout the United States with hydrogen sulfide



and other pollutant gases in an effort to develop a method



for identifying the pollutants causing damage in an area.



These plants included annual bluegrass, cheeseweed, chick-



weed, dandelion, Kentucky bluegrass, lamb's-quarters, mustard,



nettle-leaf goosefoot, pigweed, and sunflower,  which they



fumigated with 150,000 |ag/m3 and 750,000 (jg/m3  of hydrogen



sulfide for about 4 hours.  The hydrogen sulfide always



produced the greatest amount of marking on the youngest



leaves.  Very often the growing point was killed.  The



marking occurred between the veining network on the broad-



leaved plants.



        The narrow-leaved plants developed a general powdery



appearance between the tip and the bend of the leaf, except



in extreme cases where the entire leaf was killed.



        The color of the marking was usually white to tan,



except for sunflowers, where the leaves in the bud stage



took on an orange-brown cast.  The percentage of the leaf



marked by hydrogen sulfide is shown in Table 18 in the



Appendix.



        The six-week-old plants in dry soil showed more mark-



ing at the higher hydrogen sulfide concentration than the



plants in wet soil, while the reverse effect occurred at



the lower concentration, indicating that drought conditions

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                                                         16
may increase the plant's sensitivity to concentrations of


750,000 i-ig/m3 hydrogen sulfide and decrease it to concentra-


tions of 150,000 [jg/m3 .  The relative sensitivity of the 10


species to hydrogen sulfide is shown in Table 19 in the


Appendix.


2.4  Effects on Materials


2.4.1  Effects on Paint


        Hydrogen sulfide in the atmosphere reacts with paints


containing heavy metal salts in the pigment and the drier to


form a precipitate which darkens or discolors the surface.


Lead, mercury, cobalt, iron, and tin salts cause a gray or


black discoloration; cadmium salts cause a yellowish-orange


discoloration.  Lead is probably the most common metal to


exhibit discoloration caused by the formation of black lead


sulfides.        The most commonly used white pigment in


the past was basic lead carbonate.  Recently, titanium dioxide


pigments have been replacing the use of lead carbonate by


the paint industry.  However, lead pigments continue to be


used because of the added durability they impart to paint


films.

                             145
        Wohlers and Feldstein    reported that experiments


in the Bay Area of California showed that old lead-base


paints are more susceptible to hydrogen sulfide damage than


are new ones.  They also reported that darkening is dependent


on both duration of exposure and concentration and can occur

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                                                         17
after exposure to hydrogen sulfide concentrations as low as



75 ng/m3 for two hours.  The time-concentration relationship




for paint-blackening is shown in Figure 2.  These authors



suggested that paint darkening by hydrogen sulfide may vary



depending on (1) heavy metal content in paint,  (2) temper-



ature and moisture, (3) hydrogen sulfide concentration,  (4)



age and condition of paint, and (5) presence of other con-



taminants in the air.


                              PI

        Manganelli and Gregory   found that the extent of



darkening of basic lead carbonate films by hydrogen sulfide



increased as the relative humidity increased from 30 to  90



percent.  They also showed that the darkening for lead car-


                                           81
bonate films on wood was less than on tile.



        White lead paints darkened by hydrogen  sulfide often



revert to their original color by oxidation of  the sulfide



to white sulfate.147  Manganelli and Gregory81  found that



darkened films of basic carbonate faded in the  presence  of



light and oxygen and that the fastest rates of  fading were



obtained in sunlight or under a tungsten lamp.   They also



found that the fading capacity of fresh paint was not depen-



dent on the presence of atmospheric oxygen, indicating that



an oxidizing substance such as a peroxide was formed during



the drying of the film.



        Paint-darkening by hydrogen sulfide occurred in  the



Jacksonville area of Florida in 1961 due to hydrogen sulfide

-------
                                                                        18
           100
            10
          o
             1.0
            0.1
                    \
                      \
                       \
                         \
                            \
                                 Metal tarnishing
                             \
                              \
                                \
                                 \
\
                                     \
                                      \
                                        \
                                          \
                                           \
                                              v     Paint blackening
                                                \
                                                  \
                                                   \
                         California Standard of  -
                         Ambient Air Quality at
                            "Adverse Level"
                     \
                      \
                                                           \
                                                             \
                                                              \
                                                                \
                                                                 \
                                 10
                100
1,000
                         Hydrogen Sulfide Concentration, ppm vol
                                 (ppm  =  1,500 [ag/m3)
                                   FIGURE  2

Exposure Time  Versus Concentration for Hydrogen  Sulfide Effects145

-------
                                                         19
emitted from the city water aeration plant.117  Paint-darken-



ing also occurred in 1963 in New York City and in South



Brunswick, N.J.  In the New York incident, the hydrogen



sulfide was released from a polluted salt water channel.



An industrial dump was responsible for the incident in New



Jersey.  In Terre Haute, Ind., paint on houses close to the


                                              7

industrial waste disposal lagoon was darkened,  and in the



communities of Lewiston, Idaho, and Clarkston, Wash.,  damage



to house paint was caused by hydrogen sulfide emissions from


                   127
a kraft paper mill.



2.4.2  Effects on Metals



        In the presence of hydrogen sulfide,  copper and



silver tarnish rapidly. 4   Copper that has been exposed to



unpolluted air for some time resists attack by hydrogen


        123
sulfide.     Hydrogen sulfide tarnishes silver at room



temperature; however, both moisture and oxygen must be present



for tarnishing to occur.46'123  The sulfide coating formed



on copper and silver electrical contacts can increase con-



tact resistance when the contacts are closed.  In some



cases, this can result in the contacts becoming welded shut.14



Wohlers and Feldstein14^ indicated that hydrogen sulfide-



sensitive metals, like silver or copper, will tarnish when



exposed to hydrogen sulfide concentrations above 4 |_ig/m3



for 40 hours (Figure 2).



        Some alloys of gold—even such a high-carat alloy

-------
                                                          20
as 69 percent gold, 25 percent silver, and 6 percent plati-



num—will tarnish when exposed to hydrogen sulfide.  However,



in general, gold (14-carat and above) and gold leaf (95 per-



cent gold and above) will have adequate resistance to at-



mospheric hydrogen sulfide. 7



        Hydrogen sulfide will attack, zinc at room temperature,



forming a zinc sulfide film which prevents further corrosion.



At high temperatures the attack is quite vigorous.    At



concentrations normally found in the atmosphere and at am-



bient temperatures, hydrogen sulfide is not corrosive to



ferrous metals.11^



2.5  Environmental Air Standards



        The American Conference of Governmental Industrial



Hygienists (ACGIH), at their 29th Annual Meeting in 1967, set



the threshold limit value for hydrogen sulfide in air for an



eight-hour-day, 40-hour week, at 15,000 |jg/m3.137  The hydrogen



sulfide ambient air quality standards for various States and



governments are shown in Table 4.

-------
           TABLE 4




AMBIENT AIR QUALITY STANDARDS
Country or State
California
Missouri
Montana
New York
Pennsylvania
Texas
Czechoslovakia
Canada (Ontario)
Poland
U.S.S.R.
Federal Republic of
Germany
Basic Standard
lag/m"3
150
45
45
150
7.5
120
8
45
20
8
150
Avg Time
1 hr
30 min
30 min
1 hr
24 hr
30 min
24 hr
30 min
24 hr
24 hr
30 min
Permissible
Standard
uq/md

75
75

150
180
8


8
300
Avq Time

30 min
30 min

1 hr
30 min
30 min


20 min
30 min
Maximum single
Measurement
uq/m3






8


8

Reference
67, 125, 132
9, 67, 125
125
125
12, 22, 125
125
67, 125
125
62, 100, 125
93, 125
103, 125

-------
                                                             22
3.   SOURCES



    3.1   Natural Occurrence



            Hydrogen sulfide is produced in nature primarily



    through decomposition of proteinaceous material (vegetable



    and animal) by bacteria.  '     It develops principally in



    stagnant and insufficiently aerated water such as found in



    swamps and polluted water.  '   '101  Hydrogen sulfide also



    occurs naturally as a constituent of natural gas, petroleum,



    sulfur deposits, and numerous  volcanic gases and sulfur



    springs. 70*S1*-101


                                108
            Robinson and Robbins    have estimated that the



    annual worldwide production of hydrogen sulfide is around



    90 to 100 million tons, with 60 to 80 million tons coming



    from land sources and 30 million tons coming from ocean



    areas.  Other estimates range  as high as 202 million tons



    from ocean areas and 82 million tons from land areas.



    Data on background air concentrations of hydrogen sulfide



    due to the natural sources are scarce.  However,  it has



    been estimated to be between 0.15 and 0.46 (jg/m3 , which is



    well below the odor threshold  or the concentrations at which



    deleterious effects are known  to occur.



    3.2   Production Sources



            Hydrogen sulfide is produced as a  by-product in



    many industrial processes.   Production sources include the



    petroleum industry (refineries and natural gas plants),

-------
                                                         23
petrochemical plant complexes/ coke oven plants, kraft paper


mills, chemical processing industries, dye manufacture,


viscose rayon manufacture, sulfur production, manufacture of


sulfur-containing chemicals, iron and metal smelters, food


processing plants, and tanneries.


3.2.1  Petroleum Industry


        Sulfur enters the refinery as a constituent of


crude oil and is usually found in combination with hydrogen


as hydrogen sulfide and with hydrocarbons as various organic


sulfides.  Since removal of sulfur from both product and in-


termediate stocks is necessary to meet low sulfur requirements


for fuel oil and to prevent sulfur poisoning of catalysts,


processes such as hydrogen treating are employed.  During


the various steps employed in processing the crude oil, the


sulfur compounds are generally converted to hydrogen sulfide


and lower molecular weight mercaptans.-^, 57  From each


20,000 barrels of crude oil with high sulfur content pro-

                                                             QI
cessed, approximately 50 tons of hydrogen sulfide are formed.


        The main sources of air pollution in refineries are


untreated gas stream leaks, vapors from crude oil and raw


distillates, and process and condensate sewers. ^4  Typical


refinery processing systems that have hydrogen sulfide emis-

                                                    88
sions are cracking units, catalytic reforming units,   and

                      •I -3Q
sulfur recovery units.•LJO  The cracking process tends to


convert sulfur contained in crude oil into hydrogen sulfide

-------
                                                          24
in the heavier materials and into mercaptans in the gasoline



fractions.     Measurements were made in the El Paso, Tex./



area of the atmospheric hydrogen sulfide concentration adjacent



to an oil refinery.  The mean hydrogen sulfide concentration



was 6 ug/m3.  This varied from undetectable amounts to a



maximum of 91 i-ig/m0.5^




        In 1960 there were about 300 oil refineries distrib-



uted throughout the United States with a crude oil capacity



of approximately 10 million barrels per day.132  By 1969



there were approximately 263 refineries in the United States



with a crude oil capacity of approximately 12 million barrels


        130
per day.     The States in which the refineries are located



and their crude charge capacity in January 1969 are shown in



Table 20  in the Appendix.  The crude capacity of refineries



in the United States from 1964 projected to 1972 is shown in



Figure 3.



        A number of refineries and natural gas plants have



installed units to recover sulfur from hydrogen sulfide.



The plant capacities and yearly production rate for this



process are shown in Table 5.



                         TABLE 5



         SULFUR PRODUCTION FROM HYDROGEN SULFIDE

                 IN THE UNITED STATES48'94
Year
1961
1967
1968


Long
Tons/Year
Plant Capacity
1,
2,
3,
,659
,737
,036
,000
,000
,000



Actual

1,
1.
Production
858,
244,
400,
,000
,000
,000

-------
Million barrels per
  calendar day
  12.0

  11.5

  11.0

  10.5

  10.0

   9.5

   9.0

   8.5
                                                           25
I
I
I
I
      1964  1965 1966 1967 1968  1969  1970  1971  1972
                          Year
                        FIGURE  3

   Crude Capacity of United  States  Refineries
                                        95

-------
                                                          26
        Hydrogen sulfide occurs naturally in many areas in


association with natural gas.     In some areas, such as


Alberta, Canada, the sour natural gas can consist of over


50 percent hydrogen sulfide.  In processing, the natural


gas stream is treated to remove the hydrogen sulfide, which


is generally converted to sulfur.  Distributing companies


which sell the natural gas for heating and power generation


generally require that its hydrogen sulfide content be less


than 23,000 ug/m"" .     The amount of natural gas produced in


the United States in 1955 (projected through 1985) is shown


in Figure 4.


        Another possible source of hydrogen sulfide air


pollution in the petroleum industry is the production of


asphalt.  Mel' ster ^t a_l^®7 have reported that during the


distillation and oxidation of petroleum for the production


of asphalt, hydrogen sulfide is produced, but they gave no


production or emission data.


3.2.2  Petrochemical Plant Complexes


        Hydrogen sulfide is produced in petrochemical plants

                                                    QQ
during cracking and other desulfurization reactions.


Krasovitskaya &t .al_.71 reported on atmospheric hydrogen


sulfide concentrations around a petrochemical industrial


complex in Russia.  The complex consisted of three oil re-


fineries, a synthetic alcohol plant, a chemical plant, and


three power plants.  Measurements made of air concentrations

-------
                                                        27
                                                  T3

                                                  3
                                                  O
                                                  CL.


                                                  O
                                                  CO

                                                  in
                                                  TD
                                                  '5
                                                  CT
             1955 1960  1965  1970  1975 1980 1985
             * mcf :  million cubic feet
                          FIGURE  4


Natural  Gas Production and Plant  Production of Ethane and

  Liquid Propane Gas  (LPG) for  Fuel and Chemical  Use

-------
                                                           28
of hydrogen sulfide showed 17 to 150 Ug/m3 inside the indus-

trial complex, 8 to 70 |ag/m3 at 2.5 km from the complex, and

1 to 50 i-ig at 20 km from the complex.71

3.2.3  Kraft Mills

        Hydrogen sulfide and organic sulfide are produced

and released to the atmosphere in kraft mills in a number of

locations.  This emission imparts the characteristic odor

in the vicinity of kraft paper mills and has been the cause

of major air pollution problems.  Over 50 percent of the

pulp produced in the United States comes from the kraft or
                68                      108
sulfate process.    Robinson and Robbins    estimated that

in 1960 about 64,000 tons of hydrogen sulfide were emitted

from kraft paper mills throughout the world.

        In the kraft process, wood chips and a solution of

sodium sulfide and Sodium hydroxide (white liquor) are cooked

in a digester for about 3 hours at elevated temperatures and

pressures.  The solution dissolves the liquor from the wood.

The spent liquor (black liquor) is then separated from the

cellulose fiber in the blow tank.  The fiber is then washed and

processed into paper.  The remainder of the process involves

the recovery and regeneration of the cooking chemicals from

the black liquor.  The recovery process is initiated by

concentrating the black liquor by evaporation.  The concen-

trated black liquor is then burned in the recovery furnace,

and the inorganic chemicals collect on the floor of the

-------
                                                          29
furnace in a molten state (smelt).  Hot combustion gases



from the recovery furnace are used in the direct contact



evaporation to concentrate the black liquor.68'125



        The major sources of hydrogen sulfide emission in



kraft mills are the stack gases from the recovery furnace,



including the direct contact evaporator; the stack gases from


               OQ

the lime kilns;   and the noncondensibles from the digester



relief- the blow tank, and the multi-effect evaporator.21'127



The quantities of emissions from each source are given in



Table 6.  The amount of these emissions actually reaching



the environment depends upon the efficiency of each of the



abatement systems that are installed and operating at each



mill.  Table 7 shows the emissions from a kraft mill in



Lewiston, Idaho.  The mill produces 450 tons per day of


                                                         127
bleached paper board and 200 tons per day of market pulp.




        The single largest source of hydrogen sulfide in a



kraft mill is the recovery furnace, and the amount produced



is very sensitive to furnace loading.  The hydrogen sulfide



produced in the furnace rises very rapidly when the furnace



is operated above design conditions.  The relationship



between hydrogen sulfide production in the recovery furnace



and the furnace loading is shown in Figure 5.



        Measurements were made during a six-month period in



1961 and 1962 of ambient hydrogen sulfide concentration in



the Lewiston, Idaho area, where the paper mill is the major

-------
                                                        30
                        TABLE 6




HYDROGEN  SCJLFIDE EMISSIONS FROM KRAFT MILL  PROCESSORS
Sources
Digester blow (cooking
time 3.75 hr, temp 172°C,
sulfidity 22%)
Digester relief and blow
(no data on conditions)
Digester blow (no data on
conditions)
Digester relief and blow
(cooking time 3.45 hr,
temp 172°C, sulfidity 22.5%)
Digester relief (no data on
conditions)
Recovery furnace
Recovery-furnace stack gases
Recovery furnace
Multiple-effect evaporators
(potential)
Multiple-effect evaporators
(normal )
Multiple-effect evaporators
Lime kiln
Pounds/Dry
Ton Produced
0-0.45
0.43
0.9
0.66
0.01-0.05
3.6-28

9.0
1.2
0-0.06
1.2

l-ig/m3
Emitted
0-600,000
208,000



198,000-
1,500,000
750,000-
1,150,000




0-900,000
Ref .
68
141
106
127
116
68,116
141
106
68
68
106
125

-------
                                                           31
                           TABLE  7

         ESTIMATED HYDROGEN  SULFIDE  EMISSIONS* FROM
        650 TON/DAY KRAFT MILL  IN LEWISTON,  IDAHO127
       Process or Equipment
              Source
Ib/day
       Digester gases

       Evaporators

       Recovery furnaces

       Lime kilns

          Total
     9

   390

 3,120

   737

 4,256
     *Includes oxidation towers  for black  liquor and
chlorination for digester gases  (see  Abatement,  Section 4)f
             0)
             c
             I
             TJ
             I
                                      Design Limits
                          Furnace Loading
                            FIGURE 5

                Relation Between Hydrogen Sulfide
                Production and Furnace Loading125

-------
                                                           32
contributor of gaseous pollutants.  The measurements are

summarized in Table 8.  During an incident in November 1961,
                                                     29
peak 2-hour concentrations of 77 (-ig/m3 were measured.
                           TABLE 8

         FREQUENCY DISTRIBUTION OF HYDROGEN SULFIDE
                CONCENTRATIONS, 1961-196229
Hydrogen Sulfide
Concentrat ion
(ng/m3)
0-3
4-14
> 15
%Frequency at Sampling Station
Lewiston
Orchards
92.2
7.3
0.5
Lewiston
Residential
District
89.1
8.6
2.3
Lewiston
Commercial
District
68.1
28.2
3 .7
        In 1957, about 12.8 million tons of pulp were made

by the kraft process in mills located as shown in Figure 8

in the Appendix.  The United States production of pulp by

the kraft process from the year 1957 to 1967 is shown in

Table 21 in the Appendix.

3.2.4  Coke Ovens

        Hydrogen sulfide is produced in the coking operation
                                                        70
at the rate of about 6.7 pounds per ton of coal charged.

The effluent gas from coke ovens contains about 6,000 to
                                 107
13,000 Hg/m3 of hydrogen sulfide.     During cooling and

scrubbing, approximately 50 percent of the hydrogen sulfide

-------
                                                          33
is removed.  The remaining gas is either used as is for

firing the coke ovens; purified further (partial desulfuri-

zation) and then used for firing of coke ovens; or completely

desulfurized and used for municipal gas.  The hydrogen

sulfide content of nonpurified, partially purified, and

municipal gas is shown in Table 9.
                           TABLE 9
                                                 107
        HYDROGEN SULFIDE CONTENT OF COKE-OVEN GAS
        Type of Gas	|J.q/m3

        Nonpurified                     5,000-13,000

        Partially desulfurized          1,500-5,000

        Municipal gas or
           pipeline gas                 None
        Hydrogen sulfide emissions can occur throughout the

complete coking cycle from coke-oven charging to hydrogen
                                  64
sulfide removal (desulfurization).    The sources of these

emissions, other than charging and discharging emissions,

and their causes are shown in Table 10.  No data were found

on the magnitude of hydrogen sulfide concentration in the

atmosphere in or around coke ovens.  However, one reference

indicated that it is rarely of sufficient magnitude to

create problems or evoke complaints from nearby residents.

-------
                                                           34
                          TABLE 10

  SOURCES OF HYDROGEN SULFIDE EMISSIONS IN COKE PLANTS107
Source of Emission
Cause of Emission
Condensation

Unburnt gases escaping from the
   gas torches

      In normal operation with
         torch shut off

      With torch open during
         operational failures

Gases escaping from water seals

Outflow collectors on coolers;
   collector and separator
   tanks

Ammonia Scrubber

Outflow collectors and collec-
   tor tanks

Secondary coolers for primary-
   cooler outflow (in semi-
   direct process)

Benzol Scrubber and Plant

Outflow receivers of scrubbers
   and washing oil tanks

Cooler-ventilating lines
Desulfurization of Gas

Outflow receivers and tanks for
   scrubbing fluid
Leakage at stop valves


Failure of ignition device


Defective seals

Gas escape from liquids
Gas escape from washing of
   fluid

Escape of hydrogen sulfide
   with the cooling-tower
   vapors
Gas escape from washing
   fluid

Escape of sulfur-containing
   compounds with low boiling
   point, together with ven-
   tilating gases
Gas escape from washing
   fluid

-------
                                                          35
        In 1966 about 66 million tons of coke were produced

in the United States in 66 coke oven plants.   The valu« of

the coke at the coke oven was estimated to be  $1,144 million.

The production rate of coke from 1957 to 1968 is shown in

Table 22 in the Appendix.

3.2.5  Mining

        Burning coal refuse piles have been a continual

cause of air pollution, and one of the combustion products
                                              131
emitted to the atmosphere is hydrogen sulfide.      Approxi-

mately 20 percent to 50 percent of the raw anthracite

processed in cleaning plants is rejected as refuse.  At

many operations the refuse discarded amounts to about 33

percent of the tonnage produced.  This refuse over the years

has accumulated in coal refuse piles, some of which contain
                 125
millions of tons.     The piles ignite either through

spontaneous combustion, carelessness, or deliberate action.

A recent survey indicated that there are approximately
                               125
500 burning piles in 15 States.

        The hydrogen sulfide generated during combustion

disperses into the atmosphere.  Significant concentrations

of hydrogen sulfide gas have been measured in communities
                                                    131
adjacent to burning coal piles.  Sussman and Mulhern

reported that measurements made in July 1960 adjacent to a

large burning anthracite refuse pile showed an hourly

-------
                                                          36
maximum average of 600 |-ig/m3 .  The minimum hourly average

was 140 ug/m3 .

        Other possible sources of hydrogen sulfide from

mines include underground mine fires and sulfide ore mines.

However, no  information was found on these sources.

3.2.6  Iron-Steel Industry and Foundries

        Small amounts of hydrogen sulfide are given off
                                      6
when blast furnace slag is granulated.   Woehlbier and
          143
Rengstorff    showed experimentally that the amount of

hydrogen sulfide formed is proportional to the amount of

hydrogen formed during the quenching process.  No information

was given on the amount of hydrogen sulfide released to the

atmosphere by plant granulation operations.  Typical hydrogen

sulfide exhaust emissions from foundries are 0.002 tons per

non-ferrous  foundry producing 50 tons of castings per day,

and 0.023 tons per gray iron foundry producing 200 tons of
                 69
castings per day.

3.2.7  Chemical Industry

        Hydrogen sulfide is a by-product of many chemical

operations.  In general, it is formed when sulfur or §ulfur

compounds are associated with organic materials at a high

temperature.  For example, it is a by-product in the manufac-

ture of carbon disulfide.  The process of producing thiophene

by the reaction of sulfur with butane at elevated temperatures
                               107
also produces hydrogen sulfide.

-------
                                                           37
        Other sources of hydrogen sulfide in the chemical



industry are the manufacture of sulfur dyes83 and the



production of viscose rayon, ethyl and methyl parathion



(pesticides),128 organic thiophosphate,86 and many other



organic sulfur chemicals.  In addition, hydrogen sulfide



is evolved from some grease and fatty acid-making processes.



Approximately 6 tons of hydrogen sulfide are formed for every


                                   81
100 tons of viscose rayon produced.    Inorganic processes


                                                             122
which evolve hydrogen sulfide are zinc smelting and refining,



manufacture of barium chloride from barium sulfide, and



production of phosphorus compounds, pigments, lithopone,



and sodium sulfide.101  Hydrogen sulfide is also emitted



during the manufacture of stove clay and glass.69'101



The only data found on the magnitude of hydrogen sulfide



emissions were 0.024 tons reported per chemical and allied



products plant consuming 10" BTU per day, and 0.17 tons per


                                             en

cement plant producing 4,830 barrels per day. ^



        Yanysheva1^6 measured the hydrogen sulfide concen-



tration in the atmosphere at distances of 200 to 2,500



meters from an electric power plant and chemical combine



and up to 800 meters from a phenol production plant.  The



chemical combine produced sulfuric acid, nitric acid,



chlorine, and chlorinated lime.  The atmospheric hydrogen



sulfide concentration measured varied between 600 and

-------
                                                           38
                         28
1,600 |ag/m3 .  Burakhovich   reported on hydrogen sulfide

measurements made in the vicinity of Lisichansk and Rubezhnoe

chemical plants in Russia.  The Lisichansk plant manufactures

mineral fertilizers, synthetic monomers, ammonia, alcohols,

and plastics.  The Rubezhnoe plant produces high quality

dyes, dye  intermediates, and various poisonous chemicals.

The atmospheric hydrogen sulfide measurements are shown

in Table 11.
               44
        Glebova.   measured the concentration of hydrogen

sulfide in the atmosphere at 1 km from a viscose rayon plant.

The maximum  single concentration was 50 l-ig/m3 .  Measurements

were also made in the vicinity of the Dorogomelovsk Chemical

Manufacture  Plant, which produces sulfur dyes and mercapto-

benzothiazole rubber accelerators.  The hydrogen sulfide

concentrations at various distances from the plant are shown

in Table 12.

3.2.8  Animal Processing Plants and Tanneries

        Hydrogen sulfide is generated in animal processing
                                                    125
plants during the decomposition of protein material.
      129
Summer     reported that hydrogen sulfide and organic sulfur

compounds  are produced in an offal cooking plant when hooves

and horns of cattle and other animals are treated with

high-pressure live steam.  Hydrogen sulfide is also produced

during the cooking of meat.  In stale meat, approximately

-------
                                                      39
                     TABLE 11

  HYDROGEN SULFIDE  CONCENTRATIONS AT VARIOUS
              DISTANCES FROM PLANTS 28
           (One-Time Maximum in l-ig/m3 )
Year
1963
1964
1965
Lisichansk Plant
2,000m 4,000m
40 21
50

Rubezhnoe Plant
500m

35
17
1,000m

64
18
2 , 000m

>8
15
4,000m

>8
9
                     TABLE 12

ATMOSPHERIC AIR  POLLUTION BY HYDROGEN SULFIDE AT
 DIFFERENT DISTANCES FROM SOURCE OF POLLUTION41
Distance
in
Meters
100
200
300
400
500
750
1,000
1,250
Maximum
Concentrat ion
66
58
59
40
35
26
22
11
Min imum
Concentrat ion
( uq/ma )
16
35
39
26
20
15
14
05

-------
                                                          40
0.15 pounds of hydrogen sulfide is formed per ton of raw

              ,  Or
              129
meat at 100 C.  Only a trace is formed during the cooking
of fresh meat.

        During the 1920 's and the early thirties,  there

were many cases of poisoning among tanners (some fatal)
                                  119
mainly caused by hydrogen sulfide.     The air concentrations
                                                  119
at those times varied from 1,000 to 540,000
However, recent results of a nine-year-study on tanneries

in Russia showed that the hydrogen sulfide has been almost
                               119
eliminated in modern tanneries.     No information was

found on United States tanneries, but it can be assumed that

the hydrogen sulfide problem has been largely eliminated.

        Other sources of hydrogen sulfide are stockyards,
                                                   101
cheese and dairy plants, and wool scrubbing plants.     No

information was available on emissions from these sources.

3.3  Product Sources

        This category is not applicable since hydrogen

sulfide is produced only as a by-product.

3.4  Other Sources

3.4.1  Combustion Processes

        Hydrogen sulfide is released when coal, oil, or gas

is burnad.  The amount of hydrogen sulfide depends upon the

amount of sulfur in the fuel and the efficiency of the

combustion process.  In an efficient combustion system, the

-------
                                                          41
hydrogen sulfide is oxidized to sulfur dioxide.  In a study

of sulfur released from domestic boilers, it was found that

hydrogen sulfide was given off from open fires during heavy

smoke emission, mainly just after refueling.  The emission

factors for fuel combustion are given in Table 13.


                          TABLE 13

              HYDROGEN SULFIDE EMISSION FACTORS



Combustion Source	Emission Factor	Reference

Coal                   .0045*/lb coal            110

Fuel oil               1 lb/1,000 Ib oil        8,121

Natural gas            0.13 lb/1,000 Ib gas       8
   (density 0.0475)


        *lb/sulfur/lb coal.


Hydrogen sulfide is also given off by apartment incinerators
                                  37
and sanitary land fills.  Eliassen   reported in 1959 on

estimates of hydrogen sulfide discharged daily from domestic

and municipal sources in a metropolitan area of 100,000

persons.  According to this estimate, domestic heating would

produce 1,000 pounds of hydrogen sulfide daily from coal

combustion, 500 pounds from oil, and 0.1 pounds from gas;

apartment incineration would produce 24 pounds daily, and

sanitary land fill would produce trace amounts.

-------
                                                           42
3.4.2  Polluted Water

        In some localized situations,  air pollution due to

natural biological processes in polluted waters includes

hydrogen sulfide air concentrations that can produce black-

ening of paint as well as odors above the hydrogen sulfide
                        34
odor threshold.  Denmead   reported on the hydrogen sulfide

emissions from a shallow tidal inlet in Auckland,  New Zealand.

This inlet was polluted by untreated domestic sewage and

food processing sewage.  Surveys conducted during 1957

showed that the average daily concentration of hydrogen

sulfide in the air was 380 t-ig/m"3 .  This was computed to
represent about 1,500 ug/m  during night hours, a concen-

tration high enough to produce paint-blackening and the

foul odor.  The problem cleared up when the domestic and

food processing wastes were treated in a new sewage treatment

plant prior to discharge into the tidal inlet.

        A similar incident occurred on the island of Oahu

in March 1958 when rainwater filled a natural basin and

remained there due to inadequate drainage.  The water in the

basin destroyed 80 acres of Akulikuli grass growth.  The

stagnant water caused the plant life to decompose, producing

a strong fecal stench.  Two weeks later, hydrogen sulfide

was quantitatively measured in the air.  The hydrogen sulfide

was never present in levels dangerous to health, but did

-------
                                                          43
cause tarnishing of copper and silver.  House paint also

was visibly affected.  Measurements made at the drainage

ditch where water was pumped into a concrete culvert showed

hydrogen sulfide concentrations as high as 30,000 ng/ma.

The hydrogen sulfide phase of the pollution lasted for a
                        45
period of about 10 days.

        In Terre Haute, Ind., during late May and early

June 1964, the concentrations of hydrogen sulfide in the

atmosphere were sufficient to cause public complaints

because of paint-blackening and physical discomfort.

Atmospheric concentrations exceeding 460 ^g/m* were measured.

The main source of the pollution was found to be a 36-acre

industrial lagoon used for biodegradation of organic
                  7,123
industrial wastes.

3.4.3  Well Water

        Another hydrogen sulfide source is municipal plants

for removing hydrogen sulfide from well waters.  Sheeley
      117
et al.    reported that water aeration plants in the city

of Jacksonville, Fla., emit about 0.15 tons per day of

hydrogen sulfide.  They state that the plants are a particu-

larly troublesome cause of nuisance complaints.

3.4.4  Sewage Plants and Sewers

        Hydrogen sulfide is produced biologically in sewers

from organic compounds formed by hydrolysis of materials like

-------
                                                          44
cystine and methionine and by reduction of sulfates.  Sewage

usually contains 1 to 5 ppm of organic sulfur compounds,

while some industrial wastes, such as from wool, contain
                         90
as high as 50 to 100 ppm.    Sulfates are present in sewage

almost entirely as inorganic sulfates and enter the system

in waste water, saline ground water, or through industry

discharge of tidal or sea water to sewers.  The factors that

influence hydrogen sulfide generation in sewers include

sewage temperature, content of sewage, velocity of flow,

age of sewage, pH value of sewage, sulfate concentration,

and ventilation of the sewer.  Hydrogen sulfide is also
                                                    77
generated and released from sewage treatment plants.    The

hydrogen sulfide is formed in digesters during anaerobic
                                                     90
digestion of the sewage sludge and industrial wastes.

Atmospheric measurements made at a sewage treatment plant

in El Paso, Tex., in 1958 showed that the hydrogen sulfide

concentration varied between 24 M-g/m  and 2,120 ng/rn ,

with the average concentration 610 t-ig/m3 .  At a sampling

station 100 yards from the sewage plant, the maximum
                                             55
hydrogen sulfide concentration was 205 Ug/m .

3.5  Environmental Air Concentrations

        Routine measurements of the concentration of hydrogen

sulfide in the environmental air are not made by the National

Air Sampling Network.  Data from selected areas for various

time periods indicate average levels of hydrogen sulfide in

the atmosphere of 1 to 92 M.g/m3 , as indicated in Table 14.

-------
                                                  45
                 TABLE 14
ATMOSPHERIC HYDROGEN SULFIDE CONCENTRATIONS
                  (ng/m3)
Location
New York City
1956-61
1962
Elizabeth, N. J-
Aug.-Oct. 1963
Hamilton Township, N. J.
May-Oct. 1962
Woodbridge Township, N. J.
April-May 1961
Greater Johnstown Area, Pa.
1963
Wins ton- Sal em, N. C.
Nov. -Dec. 1962
Lewiston-Clarkston Area,
North Lewiston, Idaho, near
pulp mill, 1962
Great Kanawha-River Valley
Industrial Area
Feb. 1950-Aug. 1951
Cama s , Wa sh .
1962
Santa Barbara, Calif.
1949-1954
St. Louis, Mo.
1964
Terre Haute, Ind.
May- June 1964
Average Maximum
1 13
1 6
1 247
1 49
1 305
3 210
3 Oil
37
3-92 410
0-1 6
1,400
2-6 94
>460
Ref
81
13
81
81
81
47
85
1
16
8
58
39
7

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                                                             46
4.   ABATEMENT




            A number of systems and types of equipment have been




    developed for removal of hydrogen sulfide from gas streams.




    Many of these systems are designed to recover the hydrogen




    sulfide for subsequent conversion to valuable by-products,




    such as sulfur and sulfuric acid.  Many of the removal systems




    are based on scrubbing the gas streams with a suitable absor-




    bent and then removing the absorbed gas from the absorbent




    for disposal by burning or conversion to a valuable by-product.



    Some of the absorbents convert the hydrogen sulfide to an




    innocuous compound which may be useful in some cases as a




    fertilizer.  Such chemicals as aqueous solutions of diethanol-




    amine and moraoethanolamine, sodium hydroxide, tri-potassium




    phosphate, and aqueous solutions of chlorine and sodium




    carbonate have been used as absorbents.  Different types of




    contacting devices (wet scrubbers) have been used, including




    conventional and novel design spray towers, plate towers,




    and venturi scrubbers.




    4.1  Kraft Paper Mills



            In kraft paper mills,  the greatest reduction of




    hydrogen sulfide emissions was achieved by the black liquor




    oxidation process.  This process consists of oxidizing the




    sulfides in the weak black liquor (before the multiple-effect




    evaporation) or strong black liquor (after the multiple-




    effect evaporation) by contacting it with air in a packed-




    tower, thin-film, or porous-plate black liquor oxidizing unit.

-------
                                                           47
The oxidation converts the sulfides to less volatile compounds
                                                             68
which are also less odorous and have less tendency to escape.

This conversion has the effect of reducing the hydrogen

sulfide emissions from the direct-contact evaporator and the
                                           51,68,74
recovery-furnace stack by 80 to 95 percent.          Since

these evaporators and furnace stacks are the principal emitters
                                   101
of hydrogen sulfide in kraft mills,    the net result is a

substantial reduction of hydrogen sulfide emission.  The weak

black liquor oxidizing process also reduces emission from the

multiple-effect evaporators.

         The majority of the black liquor oxidizing systems

installed in the United States  are based on oxidation of weak

liquor, and are located in the Western part of the country-

In the Southern part of the country, the woods used in kraft

processes cause excessive foaming problems in the weak black
                         74,96
liquor oxidizing process.       To alleviate this, a few

Southern mills have installed a process based on oxidizing
                        96,97
the strong black liquor.

         The key to minimizing hydrogen sulfide emissions from

the recovery furnace, even in those systems employing black

liquor oxidizing systems, is proper furnace-operating condi-
      51
tions.    From Figure 5 in Section 3.2.3, it can be seen

that at furnace loading greater than design capacity, hydrogen

sulfide emissions rise substantially.  For minimum emissions

from the recovery furnace, the furnace should not be operated

above design conditions.  There should be 2 to 4 percent

excess oxygen leaving the secondary burning zone (i.e., leaving

-------
                                                          48
the furnace), and there should be adequate mixing (turbulence)


in the secondary combustion zone.



        In the direct-contact evaporator, where the flue



gases from the recovery furnace are used to concentrate the



black liquor, the carbon dioxide in the flue gases reacts



with the sulfite in the black liquor to release hydrogen



sulfide.    Even where the black liquor oxidizing process is



employed, some sulfite remains after oxidation.  This releases



some hydrogen sulfide when contacted with flue gases.  There-



fore, removal of the direct-contact evaporator from the stream



further reduces sulfide emissions.



        In the Scandinavian countries the recovery furnaces



are designed and operated in such a manner that black liquor



can be fed directly to them from the multiple-effect evapora-



tors.  These furnaces efficiently burn all malodorous compounds;



the necessity ccor oxidizing black liquor prior to burning is



therefore eliminated.  Approximately 45 mills in Sweden use



additional multi-effect evaporators to replace the direct-


                                                    32
contact evaporator and burn unoxidized black liquor.


                                                              3 2
Three such installations are being installed in North America.



The exact location of these units was not specified.



        Another approach to burning unoxidized black liquor



while still minimizing the emission of malodorous compounds



was described by Hochmutch.    in this system, the combustion



gases from the recovery furnace are used to preheat air in a



recuperative air preheater.  The hot air is then used to

-------
                                                          49
concentrate the black liquor in the direct-contact evaporator.



The air from the direct-contact evaporator is then used as



primary and secondary air in the recovery furnace, where



malodorous compounds in the air are incinerated in the



high-temperature combustion zones.



        To reduce recovery-furnace particulate emissions,



some mills have installed a secondary wet scrubber to follow



the primary scrubber (direct-contact evaporator).   Secondary



scrubbing does not remove hydrogen sulfide unless a basic



solution such as weak caustic is used.  Limited pilot plant



studies and some plant experience have shown that weak wash



(i.e., weak caustic solution) has removed hydrogen sulfide



from the stack gases.  In other instances, no hydrogen



sulfide removal has been obtained under such a system.  In



general, the removal of hydrogen sulfide from flue gases



containing 11 to 14 percent carbon dioxide with a caustic



solution has not been developed.23'24'26'74



        Other sources of hydrogen sulfide emissions from



kraft mills are the noncondensible gases released from



digesters and multiple-effect evaporators.  Various systems



developed and installed for minimizing these emissions are



generally based on collecting the noncondensible gases in a



gas holder, then oxidizing or burning them at a constant




flow rate.  The various methods used are the following:

-------
                                                          50
         (1)  Burning the gases in the recovery furnace or

lime kiln.116

         (2)  Oxidizing the gases in a separate catalytic
                                                74, 114
oxidizing furnace or a direct-flame incinerator.

         (3)  Oxidizing the gases in an absorption tower

with aqueous chlorine solutions, such as chlorine bleach

water from the bleach plant, waste chlorine, hypochlorite,

etc.  Sometimes this is followed by processing in another

absorption tower, where the absorbent is either a weak

chlorine solution or a caustic solution.  '     '

         (4)  Absorbing the gases with a caustic solution in
           61
a scrubber.

         In the lime kiln, the use of wet scrubbers with an

alkaline-absorbent,  efficient control of combustion,  and

proper washing of lime mud will substantially reduce hydrogen

sulfide emissions.  Scrubbing smelt tank gaseous emissions

with weak wash or green liquor in an absorption tower will
                                                   116
reduce hydrogen sulfide emissions from this source.

         Around 1951, masking of odors by adding aromatic

compounds to the digester, the black liquor, and the stack

gases was tried in the United States.  This strictly makeshift

approach did not solve the basic pollution problem and is not
                         141
used at the present time.

4.2  Petroleum Industry and Petrochemical Plants

         In refineries and petrochemical plants, small

quantities of hydrogen sulfide associated with gas streams

-------
                                                          51
                                                     op

can be burned in the plant full system or in a flare.    In



refineries and natural gas plants where larger quantities of



hydrogen sulfide are associated with gas streams (sour gas),



the hydrogen sulfide is generally extracted in an absorption



tower using a number of different absorbents,  such as



aqueous amines (Girbatol process); sulfalone (Shell process);



alkaline arsenites and arsenates (Giammarco-Vetrocoke process);



organic solvents such as propylene carbonate,  glyceral



triacetate, lutoxy-dethylene-glycol acetate, methoxy-triethy-



lene glycol acetate (Fluor solvent process); and many others.



These processes are regenerative—that is,  the absorbent is



regenerated by removing the hydrogen sulfide and reused.



In the case of the Giammarco-Vetrocoke process,  sulfur is



recovered directly as part of the absorbent regeneration



process.  In the other processes the hydrogen sulfide from



the regeneration process is converted to sulfur by the



Glaus process.3®'79'91  The sulfur can be further processed



into sulfuric acid if this is the end product desired.



4.3  £oke-Oven Plants and Chemical Plants



        In coke-oven plants, the coke-oven gases are often



purified of hydrogen sulfide by passing the gases through


                                     11 *3ft 1 9 fi
iron-oxide-impregnated wood shavings.  '  '     This process



is generally nonregenerative, although methods for regenerat-


                                                fto
ing the iron oxide have recently been developed.    Regener-



ative liquid absorption systems using such absorbents as

-------
                                                          52
ammonium carbonate, sodium thioarsenate, and sodium arsenate
                              38,42
solutions have also been used.       Similarly, various liquid

absorbents have been used in the chemical industry for removal

of hydrogen sulfide in gas streams.  For example, hydrogen

sulfide liberated in the production of sulfur dyes in

aniline plants is effectively absorbed by alkali in scrub-
     83
bers.    Another OJommonly used method for preventing release

of hydrogen sulfide to the atmosphere in the chemical

industry is to collect the various gaseous vents and destroy
                     128
them by incineration.

4.4  Coal Piles

         The pollution of the atmosphere in the vicinity of

burning coal refuse piles oan be minimized by constructing

the refuse piles in such a manner that ignition is minimized
                                               131
and it is possible to easily extinguish a fire.

4.5  Tanneries

         In the tanning industry, practices adopted in modern

tanneries in Russia have essentially eliminated the hydrogen

sulfide problem.  These consist of more rapid processing of

raw material, use of lime solutions to destroy hide .proteins

and alkalize sodium sulfide, and neutralization of the

semimanufactured products to Eliminate residual sodium sulfide
                                                     119
which previously contaoninated acid-tanning solutions.

-------
                                                           53
4.6  Sewers and Savage Plants

         In sewage plants, the most comprehensive elimination

of hydrogen sulfide is accomplished by enclosing the process
                                        77
and venting the gases to an incinerator.    Other methods of

removing hydrogen sulfide are absorbing or chemically

oxidizing the gas.  The oxidation process is utilized in New
                            77
York City and Sarasota, Fla.     Other methods consist of

odor-masking with scented mint, catalytic combustion, and
                   77
odor counteraction.

         In sewers, the production and release to the atmo-

sphere of hydrogen sulfide can be minimized by maintaining

sufficient velocities of sewage to avoid sulfide buildup

and minimizing lines of pressure and points of high

turbulence.  Atmospheric pollutions may also be controlled

by adequate ventilation, injection of air to maintain aeration

conditions, cleaning of sewers to remove slime and silt,

use of chemicals such as chlorine and ozone for suppressing
                    90
biological activity,   and addition of specific biological

life to suppress the development of organisms producing
                     114
the hydrogen sulfide.     A method of preventing release

of hydrogen sulfide to the atmosphere which has had some

degree of success is trapping the gas in laterals, branches,
                                                 114
and mains by use of specially designed junctions.     A

method utilized by the County Sanitation District of

-------
                                                          54
Los Angeles to control hydrogen sulfide  is to add lime
                                                             114
slurry to sewage periodically in relatively large quantities.

4.7  General Abatement Systems
                          63
         Kalyuzhnyi et al.   reported that reduction of hydro-

gen sulfide and other pollutants in air  was achieved by

placing a green vegetation belt between  the industrial emitter

and the residential areas.  They observed that hydrogen

sulfide concentrations outside the green belt then decreased

from 70 |ag/m3 to 30 M-g/m3 at 500 meters, while inside the

green belt the hydrogen  sulfide concentrations decreased

from 70 |ag/m3 to 25 |ag/m3 ; this difference was considered

significant by the author.

-------
                                                              55
5.   ECONOMICS

            Incidents in which hydrogen sulfide caused metal-

    tarnishing and paint^blackening have been reported in areas

    adjacent to kraft paper mills, industrial waste lagoons,

    and water aeration plants, as outlined in the section on

    Effects.  In one instance in Terre Haute, Ind., effects

    on health were reported.  However, few persons sought

    medical attention.  The economic inpact of the losses was

    not reported.  The major economic effect of hydrogen sulfide

    pollution on the general public is the nuisance effect (due

    to the foul smell), with the resultant decrease in property

    values in areas adjacent to emitters.  No information was

    available on the value of property in a hydrogen sulfide-

    polluted area in relation to an area not polluted by

    hydrogen sulfide.

            Tarnishing of metals has necessitated the use of

    gold in electrical contacts instead of silver,- which is

    sensitive to hydrogen sulfide corrosion.  It has been

    estimated that if silver could be used instead, in 1963

    a savings of approximately $14.8 million could have been
             67
    realized.

            In cases of severe hydrogen sulfide pollution, the

    economic inpact is substantial.  For instance, in Poza Rica,

    Mexico, 22 people died, 320 persons were hospitalized, and

    100 percent of the canaries and 50 percent of the livestock

-------
                                                          56
and domestic animals died.  However, no information was

found on the magnitude of the cost to residents of the

area.

        Major expenditures have been made in kraft plants,

natural gas plants, coke-oven plants, and chemical plants

to minimize the release of hydrogen sulfide and other odor-

producing sulfur compounds to the atmosphere.  However, no

studies were found on the total dollar value of abatement

equipment or systems or their operation.  The pulp and

paper industry has spent $75 million to date to control air

emissions.  This includes $40 million spent over the last

four years.  In the next four years the industry expects

to spend $60 million.  The cost includes the amounts spent

for all phases of air pollution, including process changes
               40
in kraft mills.    The percent of the total expenditure

associated with hydrogen sulfide abatement is not known.

        Major expenditures have been made by refineries and

natural gas plants to remove hydrogen sulfide from sour

gases and to recover the sulfur.  The cost of desulfuriza-

tion plants and sulfur-recovery plants is shown in Figure 6

and Figure 7.  However, the value of the sulfur recovered

generally exceeds the cost of construction and operation of

the facilities required to recover it.  Data on the produc-

tion of hydrogen sulfide are presented in Section 3.

-------
                                                                 57
    S2
    to
    in
    •o

    I
    O
    O
    o

   (O
   O)

    0)
    CO
    E

    1
    Q.
2,500
1,500
1,000
 500
 400
 300
 200
        100
700
500
400
300

200
150
100
 70
 50
 40
 30
                     5  7  10
                                        20 30   50 70 100
                                                       a
                                                       ~«j
                                                               a>
                                                               o
     0)
     §
      c
      £
20  S
                                                   10
                   Million Standard Cubic Feet Per Day
                              ( Capacity )
       Key
       	  Approximate 1967 cost.
       	b Sulfur plant recovery, based on 96% recovery of hydrogen sulfide,
              and 90% recovery of sulfur in sulfur plant.
       1 - 20  a Hydrogen sulfide in gas, % .
                              FIGURE  6

Approximate Cost of Gas  Desulfurization  Plants  in 1967
                     (amine  or  other  types)
                                                            92

-------
In Thousands
  of  Dollars
                                                               58
o
O
(O
cr>
ra
E
1
a
a.
    10,000
1,000
  100
        10
             50
             100
                              y
                10       100
              Long Tons / Day*
                                      1,000
     Product capacity based on:

     Hydrogen  Sulfide in Sour Gas,
                 10
                 20
                 50
                 100
                                   iSulfur Recovery in Sulfur Plant
                                              89
                                              91
                                              93
                                              95
     % Hydrogen Sulfide in gas.
                       FIGURE  7
       Sulfur-Recovery Plant  Investment
                                               48

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                                                              59
6.  METHODS OF ANALYSIS


            The methods used in air pollution studies for


    hydrogen sulfide analysis are mainly based on iodometric


    methods such as titrating with iodine, methylene blue methods,


    molybdenum blue methods, and various modifications of the


    lead acetate paper and tile methods.  The methylene blue


    method is based on precipitating cadmium sulfide from


    alkaline suspension of cadmium hydroxide by hydrogen sulfide


    in a known air sample.  The alkaline suspension of cadmium


    hydroxide is contained in a standard impinger (0-1 CFM),


    through which is drawn the sample of air to be analyzed.


    The sulfide ion is then reacted with a mixture of p-amino-


    dimethyl-aniline, ferric ion, and chloride ion (ferric


    chloride) to yield methylene blue.  The concentration of


    hydrogen sulfide is then determined optically by a colori-


    meter or spectrophotometer.           This method is good


    for hydrogen sulfide determinations down to the ng/m3


    range.  Lahmann and Prescher^ found that the cadmium


    sulfide suspensions are unstable at low concentrations and


    are decomposed by light.  From tests run on samples of air


    containing from 7 to 170 l-ig/m3 , they concluded that the


    method of sampling Ci.e,, amount of light which penetrates


    the sample) will affect the analytical results.  Recently

                       1 p
    Bamberger and Adams-1-0 claimed to have minimized these

-------
                                                          60
problems by adding arabinogalactan, avoiding exposure to

light, and analyzing the samples as soon as possible after

collection.  By this procedure they claim a sensitivity of

a few ppb of hydrogen sulfide in a 240 liter sample taken

over a 2-hour period.  This improvement gives about an 80

percent recovery of hydrogen sulfide.

        Variations on the methylene blue method include the

absorption of the hydrogen sulfide in zinc acetate instead

of the cadmium salts.  However, this variation is not as

accurate as the cadmium salt method because zinc acetate

loses hydrogen sulfide during sampling by air stripping and

aging if allowed to stand for more than 2 hours.  In addition,

the collection efficiency for cadmium hydroxide is reported
                                   52
to be higher than for zinc acetate.

        The molybdenum blue method is based on absorbing

the hydrogen sulfide from the air sample in an acid solution

of ammonium molybdate.  The color developed in the ammonium

molybdate by the hydrogen sulfide is determined optically by
              27,112
a colorimeter.

        The cadmium sulfide method is an example of the

iodometric methods for determining hydrogen sulfide concen-

tration in air.  A known quantity of air is passed through

two bubblers in series containing ammoniacal cadmium chloride

solution.  The collected samples are then stripped of any

-------
                                                           61
trapped sulfur dioxide, and the cadmium sulfide precipitate

is dissolved in concentrated hydrochloric acid.  The solution

is then titrated with iodine using starch as the indicator.

The hydrogen sulfide concentration in the air can be

calculated from the amount of iodine added.  Other cadmium

solutions—cadmium acetate, for example—can be used as the
                   59
absorbing solution.    This method is accurate to about 700
                                59
|-Lg/m3 for a 30-liter air sample.

        The spot method using paper or tiles impregnated with

lead acetate has been widely used to measure low concentra-

tions of hydrogen sulfide in the atmosphere.  The tiles are

preferred in air pollution work.  The unglazed tiles are

impregnated with lead acetate and exposed in a place where

they will be protected from rain.  After exposure, the shade

of the tiles is compared with Known standards to estimate

the concentration of hydrogen sulfide.  In general, this

method does not give accurate quantitative results, but

rather, an indication of relative exposures of various
                               59,124
localities to hydrogen sulfide.        Gilardi and
          43
Manganelli   did experimental studies on the light absorbence

of lead acetate-impregnated tile surfaces after exposure to

various concentrations of hydrogen sulfide to develop an

accurate quantitative measurement technique.  From their

experiments they concluded the following:

-------
                                                          62
        (1)  Exposure unit (mcf~j^) is a useful parameter in
representing hydrogen sulfide exposure.
        (2)  Average concentrations of hydrogen sulfide
between 150 and 1,500 |ag/m3 can be determined by the measure-
ment of surface absorbency of lead acetate.
        (3)  Fading of darkened tiles is accelerated by
air turbulence and light.
        Chiarenzelli and Joba^° also found that the tiles
faded on standing and that oxidation products formed.  From
these facts they concluded that the lead acetate tile method
is unsatisfactory for periods greater than a day or two.
        Automatic tape samplers based on lead acetate-
impregnated filter paper have been developed for field air
pollution application which continuously measure the
hydrogen sulfide content of the atmosphere.  The AISI or
Hemeon tape sampler draws a known quantity of air through
lead acetate-impregnated filter paper.  If hydrogen sulfide
is present in the atmosphere, a dark spot is formed which
is measured by determining the optical density of the spots
as compared to a standard.^  Sanderson, Thomas, and Katz11^
reported that field experience has shown that large measure-
ment errors can occur due to fading of the color of the
precipitated lead sulfide spots by action of light, sulfur
dioxide, ozone, or any other substance capable of oxidizing

-------
                                                          63
lead sulfide.  This fading may even occur during the

sampling period.  The fading can occur in a short time and

a negative result is therefore not indicative of the absence
                    113
of hydrogen sulfide.     Other factors that affect the

accuracy of the AISI tape sampler are relative humidity of

the air and the consistency of absorbence of the blank
      113                                         52
paper.     On the positive side, High and Horstman

reported obtaining results with the AISI tape sampler that

were in reasonably good agreement with results obtained by

the methylene blue method.  They stated that the lead sulfide

stains produced on the lead acetate filter paper did not

fade significantly during an 8-week storage period when

stored in vapor- and moistureproof bags.
            98
        Pare   suggested that mercuric chloride-impregnated

filter paper be used in tape sampler paper as an improvement

over the lead acetate-impregnated paper.  He reported that

the mercuric chloride paper tape is sensitive and reliable

for determination of hydrogen sulfide in air and the spots

are stable even in the presence of high levels of ozone/

nitrogen oxides, and sulfur dioxide.  He stated that it

provided an adequate sensitivity on the order of 700 ug/m3.
                  36
Dubois and Monkman   reported that although the spots formed

by hydrogen sulfide on the mercuric chloride tape are

resistant to fading effects, sulfur dioxide in the air

-------
                                                         64
results in a substantial change in hydrogen sulfide threshold

of the tape.
                           38
        Falgout and Harding   reported a method based on

drawing air through a silver membrane filter.  The hydrogen

sulfide reacts to form silver sulfide, which results in a

decrease in the reflectance of the silver surface.  The

reflectance of the membrane is measured before and after

exposure, and the decrease in reflectance is proportional

to the hydrogen sulfide exposure.  This method is also

sensitive to mercaptans in the air.  Other methods have been

used whereby silver coupons or coupons coated with lead-

base paint are exposed to air.  The sulfide formed is removed

and analyzed by the methylene blue method.  Silver tarnishing

of coupons as measured by light reflectance has also been

used as a tool for measuring relative concentrations of
                                      52
hydrogen sulfide at various locations.    Detector tubes

containing inert particles coated with silver cyanide or

lead acetate have been developed for testing for hydrogen
        111
sulfide.     The sensitivity of this method is 0.04 |jg

with a detection limit of 140 ng/m3.

        Gas chromatographs with minimum detection threshold

for hydrogen sulfide of 150 l-ig/m  have been used in air
                              14,82                 2
pollution and industrial work.       Adams and Koppe

determined that with a gas chromatograph, the bromine

-------
                                                          65
microcoulometric titration cell had the greatest potential

for rulfur-specific analysis at a sensitivity required for

direct analysis of small-volume samples.  Hydrogen sulfide

concentrations in the range of 15 l-ig/m3 to 1,200,000 l-ig/m3

can be measured by an electrolytic titrator which is

preceded by a gas scrubber train to remove interfering sulfur
          133         72
compounds.     Lahmann   reported that a sensitive new

instrument based on galvanic measuring cells has been

developed in Germany for measuring the hydrogen sulfide

content of air.

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                                                              66
7.   SUMMARY AND CONCLUSIONS




            Hydrogen sulfide is highly toxic to humans, and at



    concentrations over 1,000,000 Hg/rn3 quickly causes death



    by paralysis of the respiratory system.  At lower concen-



    trations, hydrogen sulfide may cause conjunctivitis with



    reddening and lachrymal secretion, respiratory tract



    irritation, psychic changes, pulmonary edema, damaged heart



    muscle, disturbed equilibrium, nerve paralysis, spasms,



    unconsciousness, and circulatory collapse.



            The odor threshold for hydrogen sulfide lies between



    1 and 45 l^g/m3 .  Above this threshold value, the gas gives



    off an obnoxious odor of rotten eggs, which acts as a



    sensitive indicator of its presence.  At these concentrations,



    no serious health effects are known to occur.  At 500 i-ig/m ,



    the odor is distinct; at 30,000 to 50,000 LLg/m3 the odor



    is strong, but not intolerable; at 320,000 t-ig/m3 , the odor



    loses some of its pungency, probably due to paralysis of



    the olfactory nerves.  At concentrations over 1,120,000 |ag/m3 ,



    there is little sensation of odor and death can occur



    rapidly.  Therefore, this dulling of the sense of smell



    constitutes a major danger to persons exposed to high



    concentrations of hydrogen sulfide.



            Hydrogen sulfide produces the same health effects on



    domestic animals as on man, and at approximately the same



    concentrations.

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                                                          67
        An episode occurred at Poza Rica, Mexico, where the



accidental release of hydrogen sulfide from a natural gas



plant killed 22 persons, hospitalized 320 people and killed



50 percent of the commercial and domestic animals and all



the canaries in the area.  No measurements were made of the



environmental hydrogen sulfide concentrations at the time



of the episode.  In Terre Haute,  Ind., hydrogen sulfide



emanations from an industrial waste lagoon caused foul



odor, public complaints, and discomfort.  However, very



few people sought medical attention.  Hydrogen sulfide



concentration in the atmosphere during the episode ranged



between 34 and 450 Hg/m3.



        There is little evidence that significant injury



to field crops occurs at hydrogen sulfide concentrations



below 60,000 ug/m3.  At higher concentrations, the hydrogen



sulfide injures the younger plant leaves first, then middle-



aged or older ones.



        Hydrogen sulfide combines with heavy metals in



paints to form a precipitate which darkens or discolors the



paint surface.  Air concentrations as low as 75 (-Lg/m3 have



darkened paint after a few hours' exposure.  White-lead



paints often fade in the absence of hydrogen sulfide due to



oxidation of the sulfite to sulfate.  Paint darkening has



occurred in Jacksonville, Fla., New York City, South Brunswick,

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                                                         68
N.J., Terre Haute, Ind., and in the areas near Lewiston,



Idaho, and Clarkston, Wash.  Hydrogen sulfide will also



tarnish silver and copper.  The sulfide coating formed on



copper and silver electrical contacts can increase contact



resistance and even weld the contacts shut.



        The States of California, Missouri, Montanfc, New



York, Pennsylvania, and Texas have ambient air quality



standards.  The standards vary from a level of 150 ng/m3



averaged over 1 hour in California to a 24-hour average



of 7.5 l~ig/m  for Pennsylvania.



        Hydrogen sulfide is produced naturally by biological



decay of protein material, mainly in stagnant or insuffi-



ciently aerated water such as swamps and polluted water.



The background air concentration due to this source is



estimated to be between 0.15 and 0.46 t-Lg/m3 .  Industrial



emitters of hydrogen sulfide are refineries, kraft paper



mills, coke-oven plants, natural gas plants, chemical



plants manufacturing sulfur-containing chemicals, viscose



rayon plants, food processing plants, and tanneries.  The



emission of hydrogen sulfide and other organic emlfides—



the cause of the foul odor in the vicinity of kraft paper



mills—is the major kraft paper mill air pollution problem.



        The average concentrations of hydrogen sulfide in



the urban atmosphere vary from undetectable amounts to

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                                                         69
92 l-ig/m  (based on limited data).  However, measurements



as high as 1,400 |-ig/m3 have been recorded, but these have



generally been in the vicinity of high hydrogen sulfide



emissions.



        The largest reduction in hydrogen sulfide emission



from kraft mills was achieved by the addition of the black



liquor oxidation process to the chemical recovery system.



In addition, hydrogen sulfide emissions can be minimized



if 2 to 4 percent excess oxygen is maintained in recovery-



furnace flue gas, if the furnace is not operated above



design conditions, and if noncondensible gases from the



digesters and multiple-effect evaporators are scrubbed in



a wet scrubber using weak caustic or chlorine water or are



incinerated.



        In refineries and natural gas plants, the hydrogen



sulfide associated with sour gas stream is generally extracted



in an absorption tower using absorbents such as aqueous amines.



The hydrogen sulfide is recovered from the absorbent and in



most cases further processed to produce valuable products



such as sulfur or sulfuric acid.



        The hydrogen sulfide associated with coke-oven gases



is often removed by iron oxide-impregnated wood shavings.



Liquid scrubbers using ammonium carbonate and sodium arsenate



solutions can also be used.  In chemical plants, liquid

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                                                          70
scrubbers and incinerators are used to minimize hydrogen



sulfide emissions.



        Proper design, cleaning,  and aeration of sewers



can minimize emissions of hydrogen sulfides.   The most



effective method of eliminating emissions of  this material



from sewage plants is to enclose the process  and vent the



gases formed to an incinerator.



        No information has been found on the  economic costs



of hydrogen sulfide air pollution or on the costs of its



abatement.



        The primary methods used in air pollution studies



for analyzing hydrogen sulfide are based on iodometric



methods (cadmium sulfide method), methylene blue method,



molybdenum blue method, and various modifications of the



lead acetate paper and tile methods.  The automatic tape



samplers based on the lead acetate paper method have been



developed for field air pollution application.  However,



there is evidence that the spot formed on the lead acetate



tape fades in the presence of oxidants, producing measurement



errors.  To solve this problem, mercuric chloride-impregnated



tape has been developed for use in automatic  tape samplers.



        Based on the material presented in this report,



further studies are suggested in the following areas:



       (1)  Determine whether continuous exposure to low



concentrations of hydrogen sulfide is harmful to health.

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                                                         71
       (2)  Survey all hydrogen sulfide emitters and the



magnitude of the emissions from them.



       (3)  Develop an improved, simple, accurate method



for field analysis.



       (4)  Determine the effectiveness of existing abatement



systems at kraft mills and develop more effective systems



which will essentially eliminate hydrogen sulfide emissions



from kraft mills.

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                                                               72
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113.   Sanderson, H. P., R. Thomas, and M. Katz, Limitations of the
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114.   Santry, I. W. , Jr., Hydrogen Sulfide Odor Control Measures, J..
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116.   Shah, I. S., Pulp Plant Pollution Control, Chem. Eng. Prog. 64(9)
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118.   Sherwood, P- W.,  How Atmospheric Conditions Can Corrode Refinery
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                                                                82
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                                                                 83
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                                                                84
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APPENDIX

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APPENDIX
                                                          86
                          TABLE 15
   EFFECTS OF HYDROGEN SULFIDE ON HUMANS
                                        41,49,101,102,140
Concentrat ion
                                       Effects
1-45


10


150

500

15,000


30,000



30,000-60,000



150,000




270,000-480,000



640,000-1,120,000


900,000

1,160,000-1,370,000
Odor threshold.  No reported injury
  to health

Threshold of reflex effect on eye
  sensitivity to light

Smell slightly perceptible

Smell definitely perceptible

Minimum concentration causing eye
  irritation

Maximum allowable occupational
  exposure for 8 hours (ACGIH
  Tolerance Limit)

Strongly perceptible but not in-
  tolerable smell.  Minimum con-
  centration causing lung irritation

Olfactory fatigue in 2-15 minutes;
  irritation of eyes and respira-
  tory tract after 1 hour; death
  in 8 to 48 hrs

No serious damage for 1 hour but
  intense local irritation; eye
  irritation in 6 to 8 minutes

Dangerous concentration after 30
  minutes or less

Fatal in 30 minutes

Rapid unconsciousness, respiration
  arrest, and death, possibly
  without odor sensation
1,500,000+
Immediate unconsciousness and rapid
  death

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APPENDIX
                                                         87
                          TABLE 16

TIME REQUIRED FOR 50 PERCENT MORTALITY OF SUBJECTS TREATED
                  WITH HYDROGEN SULFIDE 66
                        (In Minutes)
Sub i ect
Flies
Mice
Rats
Number
Studied
250
4
8
H2S Concentration (in l-iq/m )
1,500,000
7
18
14
380,000
>960
410
>960
96,000

804
>960
24,000

>960
>960

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APPENDIX
                                                 TABLE 17


                          TYPICAL GROSS FINDINGS AT AUTOPSY OF RATS AND MICE
                            WHICH DIED DURING EXPOSURE TO HYDROGEN SULFIDE139
Orqan
Brain
Trachea

Lungs
Heart
Liver
Gall
bladder
Concentration of Hydrogen Sulfide Gas (in uq/m° )
1,500,000
Rats (8)
Very slightly
congested
Natural

Well collapsed,
dark pink, cut
surface wet,
rare small
hemorrhages
In systole,
atria dilated,
blood fluid
Much congested
Not distended
Mice(4)

Same as
rats
Same as
rats
Same as
rats
Same as
rats
Same a s
rats
380,000
Rats (8)
Congested
Natural

Partly distended,
extremely
hemorrhagic
Distended
Congested
Not distended
Mice (4)
Slightly
congested
Natural

Massive
hemorrhages
of all lobes
Moderate dila-
tation of
right side
Moderately en-
larged, very
pale, lobules
not exaggerated
Definitely but
moderately
distended
96,000
Rats (8)
Congested
Natural

One-half col-
lapsed, many
small hemor-
rhages
Moderate dila-
tation of
right side
Medium
dark red
Not distended
Mice (4)
Congested
Natural

Deep red,
apparently
massive hemor-
rhage
Moderately
dilated
Pale, nutmeg
color, large
Not distended
to moderately
distended
                                                                                                       CD
                                                                                                       00

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APPENDIX
                                          TABLE 17 (Continued)

                          TYPICAL  GROSS  FINDINGS AT AUTOPSY OF RATS AND MICE
                            WHICH  DIED DURING EXPOSURE TO HYDROGEN SULFIDE
Drqan

Stomach





Intes^-
tines

Adrenals

Kidneys



Concentration of Hydrogen Sulfide Gas (in t-iq/m0 ) '
1,500,000
Rats (8)

Moderately to
greatly distended,
few small
hemorrhages


Natural or with
a few small
hemorrhages
Na t ura 1 , p ink

Much congested



Mice(4)

Same as
rats




Same as
rats

Same as
rats
Moder-
ately
conges-
ted
380,000
Rats (8)

Distended, few
small hemorrhages




Large, partly
distended

Pink

Congested



Mice (4)

Definitely but
moderately
distended, rare
minute hemor-
rhages

Small intestine
slightly dis-
tended
Pale

Pale



96,000
Rats (8)

Definitely but
moderately
distended, mod-
erate number of
small hemor-
rhages
Cecum moderately
distended

Natural

Medium dark
red


Mice (4)
[
Moderately dis-«
tended, few !
hemorrhages of
moderate size


Duodenum
dilated

Natural
t
Pale



                                                                                                      03

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APPENDIX
90
                             TABLE 18

       PERCENTAGE OF LEAF AREA MARKED BY HYDROGEN  SULFIDE20
                       (Four-Hour Fumigations)
Concentration of


Plant
Lamb ' s-quarters
Nettle-leaf goosefoot
Chickweed
Dandelion
Sunflower
Kentucky bluegrass
Pigweed
Annual bluegrass
Mustard
Cheeseweed
750
3 wka
Moist*5
100
91
100
75
53
70
52
66
52
32
,000 uq/m
6 wka
Moist*5
69
54
55
45
45
28
31
18
20
34
o
6 wka
Dry*5
100
83
88
76
78
77
53
64
65
53
Hydro q en
150
3 wka
Moist*5
53
64
41
16
28
21
12
17
16
10
Sulf ide
,000 Uq/
6 wka
Moist*5
100
88
34
26
26
18
23
9
13
10

m"3
6 wka
Drv*5
28
24
29
13
17
16
32
7
11
3
        aAge of plants.
        t>Soil condition,

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                                                             91
APPENDIX
                           TABLE 19

                                                        9O
      RELATIVE SENSITIVITY OF PLANTS TO HYDROGEN SULFIDE
	Sensitive	Intermediate	Resistant

Lamb's-quarters          Dandelion             Annual bluegrass
Nettle-leaf goosefoot    Sunflower             Mustard
Chickweed                Kentucky bluegrass    Cheeseweed
                         Pigweed

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                                                        92
 APPENDIX
                         TABLE 20

CRUDE OIL CAPACITY IN THE UNITED STATES AS OF JANUARY 196913°
 State
  No.
Plants
      Crude  Capacity5
                                                   b/sdc
 Alabama
 Alaska
 Arkansas
 California
 Colorado
 Delaware
 Florida
 Georgia
 Hawaii
 Illinois
 Indiana
 Kansas
 Kentucky
 Louisiana
 Maryland
 Michigan
 Minnesota
 Mississippi
 Missouri
 Montana
 Nebraska
 New Jersey
 New Mexico
 New York
 North Dakota
 Ohio
 Oklahoma
 Oregon
 Pennsylvania
 Rhode Island
 Tennessee
 Texas
 Utah
 Virginia
 Washington
 West Virginia
 Wisconsin
 Wyoming

    Total
   6
   1
   6
  32
   4
   1
   1
   2
   1
  11
  10
  12
   3
  16
   2
   8
   3
   4
   1
   9
   1
   6
   6
   2
   2
  11
  14
   1
  13
   1
   1
  47
   5
   1
   6
   2
   2
 	9

 263
    34,620
    20,000
    93,500
 1,529,075
    42,900
   140,000
     3,100
     9,500
    35,000
   704,100
   565,700
   389,300
   128,500
 1,190,850
    19,400
   146,050
   138,300
   168,700
    83,000
   128,200
     4,000
   523,500
    42,610
    76,900
    55,000
   491,600
   449,367
    11,000
   628,920
     7,500
    28,500
 3,118,250
    11,950
    43,600
   219,000
     8,570
    29,500
   132,900

11,522,512
    36,820
    21,000
    94,985
 1,606,985
    46,235
   150,000
     3,150
    11,000
       NR
   732,300
   588,800
   407,300
   132,600
 1,230,000
    20,500
   152,000
   144,000
   181,500
    84,700
   137,500
     4,500
   555,000
    44,400
    81,000
    57,000
   525,900
   464,250
    12,000
   659,100
    10,000
    29,750
 3,244,300
   116,400
    45,000
   226,000
     9,100
    30,600
   146,686

12,079,201
         astate totals include figures converted to calendar-day
 or stream-day basis.
         bb/cd = barrels per calendar day.
         cb/sd = barrels per stream-day.

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                                                             93



APPENDIX
                           TABLE 21




         KRAFT PULP  PRODUCTION IN THE UNITED  STATES105
Year
1957
1958
1959
1960
1961
1962
1963
1964
1965
1966
1967
Million
Tons/Year
12.8
13.1
14.9
15.3
16.1
17.4
18.7
20.4
22.3
24.4
23.9

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                                                          94
APPENDIX
                        TABLE  22
             UNITED STATES COKE PRODUCTION89
_Year

1957-59
1964
1965
1966
Tons/Year
6
60.5 x 10
60.9 x 106
65.2 x 106
66.0 x 106
Number of
Oven Slots

15,993
14.639
14,357
14,720

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                                                           95
APPENDIX
                        FIGURE  8
    Location of Kraft Mills  in United  States  (1957)
68

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