HARARE INSTITUTE OF TECHNOLOGY

DESIGN OF A PROCESS FOR THE PRODUCTION OF 1.2 T/ DAY NICOTINE SULPHATE

FROM TOBACCO WASTE

BY

ASSURED PROGESS CHIDEMBESE H1214231J

SUPERVISED BY

MR ZULU

THIS DESIGN AND INNOVATION PROJECT WAS SUBMITTED TO HARARE

INSTITUTE OF TECHNOLOGY IN PARTIAL FULFILMENT OF THE BACHELOR OF
TECHNOLOGY (HONOURS) DEGREE IN CHEMICAL AND PROCESS SYSTEMS
ENGINEERING

2014
1|Page
Table of Contents
LIST OF TABLES .......................................................................................................................... 5
1 CHAPTER TWO: LITERATURE REVIEW.......................................................................... 6
1.0 Background ...................................................................................................................... 6
1.1 History of Tobacco ........................................................................................................... 6
1.2 History of nicotine and other tobacco extracts ................................................................. 7
1.3 The Toxicity of nicotine sulphate and related alkaloids. ................................................. 8
1.4 The Physiological action of nicotine sulphate.................................................................. 9
1.5 Factors influencing the nicotine content of tobacco....................................................... 10
1.5.1 Variation in Different Varieties. ............................................................................. 11
1.5.2 Variation in Different Parts of the Plant. ................................................................ 11
1.5.3 Influence of leaf position ........................................................................................ 12
1.5.4 Tobacco species or type .......................................................................................... 13
1.5.5 Soil type: ................................................................................................................. 13
1.5.6 Effects of topping and suckering ............................................................................ 13
1.5.7 Curing ..................................................................................................................... 15
1.5.8 Fertilizer treatments. ............................................................................................... 16
1.5.9 The effect of climate ............................................................................................... 17
1.6 The Nicotine Content of Tobacco Used In the Production of Insecticides .................... 18
1.7 The Nicotine Content of Zimbabwean Tobaccos ........................................................... 19
1.8 The Manufacturing of Tobacco Extract or Nicotine Sulphate. ...................................... 20
1.9 Uses of Nicotine Sulphate .............................................................................................. 23
1.10 A Comparison of Nicotine and Nicotine Sulphate ......................................................... 24
1.11 Physical and Chemical Properties of Nicotine sulphate................................................. 24
1.12 Technique of Sampling, Determinations of Moisture, Nicotine and Nor Nicotine. ...... 25
1.13 The Preparation of The Tobacco For The Production of Extracts ................................. 27
2 CHAPTER THREE: RESEARCH METHODOLOGY ........................................................ 28
2.0 Introduction .................................................................................................................... 28
2.1 Material and equipment .................................................................................................. 28
2.2 Chemicals ....................................................................................................................... 28
2.3 Experimental procedures ................................................................................................ 29
2.3.1 Determination of moisture content of tobacco waste ............................................. 29

2|Page
 2.3.2 Extraction of nicotine .............................................................................................. 29
2.3.3 Testing for the presence of nicotine ........................................................................ 29
2.3.4 Acidification of the nicotinized kerosene solution ................................................. 30
2.3.5 Centrifugation process. ........................................................................................... 30
2.3.6 Testing for the presence of nicotine sulphate ......................................................... 30
2.3.7 Alkalization of kerosene and solid waste residue ................................................... 31
2.3.8 Separation using simple distillation ........................................................................ 31
3 CHAPTER FOUR: EXPERIMENTAL RESULTS AND ANALYSIS ................................ 32
3.0 Introduction .................................................................................................................... 32
3.1 Results on the determination of moisture content of tobacco waste. ............................. 32
3.2 Results on the extraction of nicotine from waste tobacco .............................................. 33
3.2.1 Conclusion for extraction of nicotine ..................................................................... 33
3.3 Results on the testing for the presence of nicotine ......................................................... 34
3.3.1 Conclusion for testing for the presence of nicotine ................................................ 34
3.4 Results on the acidification of nicotinized kerosene ...................................................... 34
3.4.1 Analysis for the acidification of nicotinized kerosene ............................................ 35
3.4.2 Determining Nicotine Concentration ...................................................................... 36
3.4.3 Determining Nicotine sulphate Concentration........................................................ 36
3.4.4 Nicotine Neutralization with Sulfuric Acid ............................................................ 36
3.4.5 Conclusion .............................................................................................................. 37
3.5 Results on centrifugation process ................................................................................... 37
3.6 Results on the testing for the presence of nicotine sulphate .......................................... 37
3.6.1 Conclusion for testing for the presence of nicotine sulphate .................................. 37
4 CHAPTER FIVE: PROCESS DESIGN ................................................................................ 38
4.0 Introduction .................................................................................................................... 38
4.1 Process description ......................................................................................................... 38
4.2 Equipment list ................................................................................................................ 38
4.3 Determination of the input feed rate of tobacco stem crusher ....................................... 39
4.4 Block flow diagram ........................................................................................................ 40
4.5 Process flow diagram ..................................................................................................... 41
4.6 Balance calculations ....................................................................................................... 42
4.6.1 Material balances .................................................................................................... 42
3|Page
 4.6.2 Balance over the super centrifuge ........................................................................... 45
4.6.3 Mass balance over the acidification vessel ............................................................. 46
4.6.4 Energy balances ...................................................................................................... 47
4.6.5 Energy balance on the distillation column .............................................................. 49
5 CHAPTER SIX: EQUIPMENT DESIGN ............................................................................. 51
5.0 Introduction .................................................................................................................... 51
5.0.1 Horizontal shaft impact crusher .............................................................................. 51
5.0.2 Vertical shaft impact crusher .................................................................................. 51
5.1 Operating Principle of the Tobacco Impact Crusher ...................................................... 52
5.2 Design Parameters: ......................................................................................................... 52
5.3 Mechanical design of the tobacco impact crusher ......................................................... 53
5.4 Material of constructing the crusher............................................................................... 53
5.5 Designing the crusher volume ........................................................................................ 53
5.6 Designing of crusher diameter and height...................................................................... 54
5.7 Cross sectional area of the crusher ................................................................................. 54
5.8 Design of Hammer / Blow bars ...................................................................................... 54
5.9 Impact Bending Stress (Static) ....................................................................................... 55
5.10 Static Load Shearing ...................................................................................................... 58
5.11 Design of V-Belt Drive ............................................................................................................... 59
5.12 Design Of Rotor Shaft (Static Conditions) .................................................................... 61
5.13 Design of Grinding Screen ............................................................................................. 63
5.14 Summary of Final Design Parameters ............................................................................ 67
5.15 Proposed Designs ........................................................................................................... 69

4|Page
 LIST OF TABLES
TABLE 1.1: INFLUENCE OF LEAVE POSITION ON NICOTINE CONTENT (RASMUSSEN)......................................................12
TABLE 1.2: EFFECTS OF TOPPING, SUCKERING, AND MATURITY ON NICOTINE CONTENT (WARD. G. M)........................14
TABLE 1.3: INFLUENCE OF CLIMATE ON NICOTINE CONTENT (N. RUSTICA) ..................................................................18
TABLE 1.4: AVERAGE PERCENTAGE NICOTINE IN TOBACCO..........................................................................................20
TABLE 1.5: PHYSICAL AND CHEMICAL PROPERTIES OF NICOTINE SULPHATE ................................................................25
TABLE 3.1: RESULTS ON MOISTURE CONTENT DETERMINATION ...................................................................................32

LIST OF FIGURES

FIGURE 1:1: THE STRUCTURE OF NICOTINE SULPHATE COMPOUND ...............................................................................24

FIGURE 3:1: CRUDE NICOTINE EXTRACTED FROM TOBACCO WASTE .............................................................................33
FIGURE 3:2: EXPERIMENTAL RESULTS SHOWING THE PRESENCE OF NICOTINE ..............................................................34
FIGURE 3:3: SAMPLE OF PURE NICOTINE SULPHATE ......................................................................................................35
FIGURE 4:1: BLOCK FLOW DIAGRAM OF THE PROCESS ..................................................................................................40
FIGURE 4:2: PROCESS FLOW DIAGRAM OF THE PROCESS ...............................................................................................41
FIGURE 4:3: OVERALL MATERIAL FLOW DIAGRAM (CONSIDERING THE WHOLE BLOCK DIAGRAM) ...............................42
FIGURE 4:4: MASS BALANCE OVER SUPER CENTRIFUGE ...............................................................................................45
FIGURE 4:5: MASS BALANCE OVER THE ACIDIFICATION VESSEL ...................................................................................46
FIGURE 5:1: BENDING STRESS DIAGRAM ......................................................................................................................56
FIGURE 5:2: BENDING STRESS DIAGRAM WITH THE LOAD AT THE TIP OF CANTILEVER ..................................................58
FIGURE 5:3: CROSS SECTION OF V-GROOVED PULLEY (R. S. KHURMI AND GUPTA. A TEXT BOOK OF MACHINE DESIGN.
2005. P. 728)........................................................................................................................................................60
FIGURE 5:4: FREE BODY DIAGRAM OF ROTOR SHAFT ....................................................................................................61
FIGURE 5:5: BENDING MOMENT DIAGRAM....................................................................................................................63
FIGURE 5:6: GRINDING SCREEN PROCESS .....................................................................................................................64
FIGURE 5:7: FLOW CHART OF MATERIAL ON SCREEN ....................................................................................................66
FIGURE 5:8: PROPOSED DESIGN OF ROTOR PLATE..........................................................................................................69
FIGURE 5:9: PROPOSED DESIGN OF A HAMMER .............................................................................................................69
FIGURE 5:10: PROPOSED DESIGN OF ROTOR ASSEMBLY WITH ROTOR DISC, HAMMERS, SHAFT AND LOCKING PIN .........70
FIGURE 5:11: PROPOSED DESIGN OF CRUSHER ASSEMBLY WITH ROTOR, FLYWHEEL, IMPACTS BARS AND CASING (SIDE
VIEW) ................................................................................................................................................................... 70

5|Page
1 CHAPTER TWO: LITERATURE REVIEW
1.0 Background
Nicotine is extracted from tobacco or related Nicotiana species and is one of the oldest botanical
insecticides in use today. It's also one of the most toxic to warm-blooded animals and it's readily
absorbed through the skin. (Wear gloves when applying it, follow label directions and keep pets
away from application areas.) It breaks down quickly, however, so it is legally acceptable to use
on organically grown crops.

Nicotine sulfate is sold as a 40 percent nicotine sulfate concentrate under trade names that
include Black Leaf 40 or Tender Leaf Plant Insect spray. Nicotine kills insects by interfering
with the transmitter substance between nerves and muscles. It's commonly used to control
aphids, thrips, spider mites and other sucking insecticides on most vegetables, some fruits,
flowering plants and ornamental shrubs and trees. Roses are sensitive to nicotine. Choose
alternate pest control measures when treating insects on roses.

1.1 History of Tobacco

According to Ward (Nicotine - A Product of Tobacco 1941, p.33) the culture of tobacco and its
use in smoking and as a stimulant have been known to Europeans since the discovery of America
in 1492, although it is certain that the custom of smoking and chewing tobacco was known to the
natives of the New World, and practised by them, for many centuries before that time. Shepard
(The Chemistry and Toxicology of Insecticides, 1940, p. 213-2640) states that tobacco was
exported from America to Spain and Portugal in 1559 and shortly afterwards to France and Italy
and to England in 1585.

Tobacco is an agricultural product processed from the leaves of plants in the genus Nicotiana. It
can be consumed, used as a pesticide and, in the form of nicotine tartrate, used in some
medicines. It is most commonly used as a drug, and is a valuable cash crop for countries such as
Cuba, India, China, Zimbabwe and the United States. Tobacco is a name for any plant of the
genus Nicotiana of the Solanaceae family (nightshade family) and for the product manufactured
from the leaf and used in cigars and cigarettes, snuff, and pipe and chewing tobacco. Tobacco
plants are also used in plant bioengineering, and some of the 60 species are grown as
ornamentals. The chief commercial species, N. tabacum, is believed native to tropical America,
like most nicotiana plants, but has been so long cultivated that it is no longer known in the wild.
N.Rrustica, a mild-flavored, fast-burning species, was the tobacco originally raised in Virginia,
6|Page
but it is now grown chiefly in Turkey, India, Zimbabwe and Russia. The alkaloid nicotine is the
most characteristic constituent of tobacco and is responsible for its addictive nature. The harmful
effects of tobacco derive from the thousands of different compounds generated in the smoke,
including polycyclic aromatic hydrocarbons (such as benzpyrene), formaldehyde, cadmium,
nickel, arsenic, radioactive polonium-210, tobacco-specific nitrosamines (TSNAs), phenols, and
many others.

Tobacco is cultivated similarly to other agricultural products. Seeds are sown in cold frames or
hotbeds to prevent attacks from insects, and then transplanted into the fields. Tobacco is an
annual crop, which is usually harvested mechanically or by hand. After harvest, tobacco is stored
for curing, which allows for the slow oxidation and degradation of carotenoids. This allows for
the agricultural product to take on properties that are usually attributed to the "smoothness" of
the smoke. Following this, tobacco is packed into its various forms of consumption, which
include smoking, chewing, snuffing, and so on. Most cigarettes incorporate flue-cured tobacco,
which produces a milder, more inhalable smoke. Use of low-pH, inhalable, flue-cured tobacco is
one of the principal reasons smoking causes lung cancer and other diseases association with
smoke inhalation.

The tobacco plant belongs to the genus Nicotiana and according to Holman (A Survey of
Insecticide Materials of Vegetable Origin, 2005, p.42-58) about hundred species of the genus are
already known. Shapard and Holman maintain that only the two species Nicotiana tabacum and
Nicotiana rustica are of importance as sources of tobacco or nicotine. In Zimbabwe mainly
Nicotiana tabacum is cultivated for the manufacture of snuff, chewing and smoking tobacco, but
Nicotiana rustica Nicotiana glauca are also found here.

1.2 History of nicotine and other tobacco extracts

Nicotine is an alkaloid found in the nightshade family of plants (Solanaceae) that acts as a
nicotinic acetylcholine receptor agonist. The biosynthesis takes place in the roots and
accumulation occurs in the leaves of the Solanaceae. It constitutes approximately 1.6% – 15.0%
of the dry weight of tobacco and is present in the range of 2–7 μg/kg of various edible plants. It
functions as an ant herbivore chemical; therefore, nicotine was widely used as an insecticide in
the past and currently as a starting raw material for the production of nicotine sulphate and also
nicotine analogs such as imidacloprid are currently widely used.

7|Page
According to Holman (Survey of Insecticide Materials of Vegetable Origin 1939, p.42-58)
tobacco extracts were first used unsuccessfully by Jean de la Quintinye in 1690 against a bug
attacking the leaves of pear tree. In 1746 Peter Collinson advised the use of water, in which
tobacco leaves had been soaked, to protect nectarines from attacks of the insect “plum curculio”.
In 1763 tobacco dust was recommended in France as a remedy for plant lice and in 1773 Weston
invented fumigating bellows for destroying insects with tobacco smoke. Early in the nineteenth
century tobacco dusts and extracts were in fairly common use as insecticides and it was quite
usual to employ smoke for fumigating greenhouses. Concentrated tobacco extracts are referred to
as far back as 1882, but the first standardized extract was put on the market in the United States
in 1892, and contained slightly less than 3 per cent nicotine. In Africa, however, standardized
extracts did not make their appearance until after the beginning of the twentieth century.

The presence of nicotine in tobacco was demonstrated for the first time by Vanquelin in 1809,
according to Ward and Henry, (The Plant Alkaloids 3rd Edition, Alkaloids of Nicotiana, 1939, p.
42-58) although it had been known and used before that time in the form of “Qleum tabaci "(oil
of tobacco) since 1656 . These authors also point out that it was not, however, until 1828 that
nicotine was isolated in its pure state by Posselt and Reiman. Since that time many further
investigations on this subject have been conducted and it has been found that tobacco contains a
whole series of related alkoids.

In low doses (an average cigarette yields about 1 mg of absorbed nicotine), the substance acts as
a stimulant in mammals, while high amounts (30–60 mg) can be fatal. This stimulant effect is the
main factor responsible for the dependence-forming properties of tobacco smoking. According to
the American Heart Association, nicotine addiction has historically been one of the hardest
addictions to break, while the pharmacological and behavioral characteristics that determine
tobacco addiction are similar to those determining addiction to heroin and cocaine. The nicotine
content of popular American-brand cigarettes has slowly increased over the years, and one study
found that there was an average increase of 1.6% per year between the years of 1998 and 2005.
This was found for all major market categories of cigarettes.

1.3 The Toxicity of nicotine sulphate and related alkaloids.

Several authors state further that the presence or absence of a CH, group attached to the
pyrrolidine nitrogen of a pyridyl pyrrolidine is not essential for toxic action to "Aphis rumicis ",
and that racemic nicotine sulphate is about half as toxic as natural nicotine.

8|Page
Campbell, Sullivan and Smith (Alkaloids in Certain Species and Inter-specific Hybrids of
Nicotiana. Journal of Agricultural Research, Vol. 65. 2011 p. 347-59) compared the relative
toxicities of nicotine sulphate, anabasine and rnethylanabasine for culicine mosquito larvae and
found that the concentration necessary to kill the larvae in eight hours at 29, 3° C could be
tabulated as follows:

1) Nicotine sulphate: 17
2) Anabasine: 38
3) methylanabasine 21

In this case again nicotine sulphate is twice as toxic as anabasine. They also found that nicotine
sulphate and anabasine are much less toxic than rotenone (the active constituent in derris root) to
mosquito larvae and house-flies. This clearly demonstrates the fact that insecticides do not show
the same toxic action on different insects and must be tested specifically on each insect species.

1.4 The Physiological action of nicotine sulphate

Shepard (The Chemistry and Toxicology of Insecticides, 1990, p. 300-320) maintains that
nicotine sulphate is absorbed very rapidly from the tongue, eye and rectum but more slowly from
the stomach, probably because of the acidity of the gastric juice. According to Shepard (The
Chemistry and Toxicology of Insecticides, 1990, p. 98-140) and Janssen ( Chemical Reviews.
Alkaloids of Tobacco. Vol. 2010 p.29, 123-97) free nicotine is absorbed very rapidly and in
dangerous amounts through the human skin. Janssen ( Chemical Reviews. Alkaloids of Tobacco.
Vol. 2010 p.39, 223-97) points out that lethal quantities (4 milligrams) may be inhaled during
spraying of enclosed spaces. Blyth (Poisons: Their Effects and Detection. Tobacco Nicotine,
1998, p. 374-385) states that nicotine is absorbed into the blood and excreted unchanged, in part
by the kidneys and in part by the saliva.

The symptoms of nicotine or tobacco poisoning are, according to Blyth (Poisons: Their Effects
and Detection. Tobacco Nicotine, 1998, p. 74-85) and Janssen (Private Communication.), as
follows: Complete nervous exhaustion, severe headache, secretion of saliva, difficult breathing,
tetanic cramps, vomiting and irregular pulse followed by diarrhoea, helplessness and collapse.
This is accompanied by paleness, coldness of the arms and feet and convulsive muscular spasms,
and finally death supervenes.

9|Page
Rosenthal and Krocker came to the following conclusions according to Blyth (Poisons: Their
Effects and Detection. Tobacco Nicotine, 1998, p. 74-85), “Nicotine acts energetically on the
brain, at first exciting it and then lessening, its activity; the spinal marrow is similarly affected.
The convulsions appear to have a cerebral origin; paralysis of the peripheral nerves follows later
than that of the nerve centres, whilst muscular irritability is unaffected. The convulsions are not
influenced by artificial respiration, and are therefore to be considered as due to the direct
influence of the alkaloid on the nervous system. Nicotine has a striking influence on the
respiration, first quickening then slowing and lastly arresting the respiratory movements: section
of the vagus is without influence on this action. Death is evidently due to the rapid benumbing
and paralysis of the respiratory centre. Death never follows from heart-paralysis although
nicotine powerfully influences the heart's action, small doses exciting the terminations of the
vagus in the heart, and causing a slowing in the beats. Large doses paralyze both the controlling
and exciting nerve-centres of the heart; the heart then beats fast, irregularly, and weakly. The
blood-vessels are first narrowed and then dilated, and, as a consequence, the blood-pressure first
rises then falls. Nicotine has a special action on the intestines, there is a strong contraction of the
whole tract, especially of the small intestine, the lumen of which may be, through a continuous
tetanus, rendered very small. This is ascribed to peripheral excitation of the intestinal nerves and
the ganglia. The uterus is also excited to strong contraction by nicotine sulphate, the secretions of
bile and saliva are increased

Because of the toxicity of nicotine sulphate it is advisable to take care that it does not come into
contact with the skin. If the dinger exists, rubber gloves should be worn.

1.5 Factors influencing the nicotine content of tobacco.

Nicotine level is a key index for evaluating the quality and quantity of nicotine sulphate, and is
closely related to a lot of factors. According to the authors Ward (Nicotine - A Product of
Tobacco 1941, p.54), Shepard (The Chemistry and Toxicology of Insecticides, 1990, p. 513-
640), Kobert (16), and Martin (18), Jackson (Chemical Reviews. Alkaloids of Tobacco. Vol. 29,
2009 p.123-97) and Allen (Allen’s Commercial Organic Analysis, Fifth Edition, Nicotine and
Tobacco, Vol. VII, 1999, p. 625-641.). Nicotine usually exists in the plant in combination with
citric, malic, oxalic and other organic acids. Ward (Nicotine - A Product of Tobacco 1941, p.63)
adds that some of the nicotine is always present as free nicotine. The free nicotine is directly

10 | P a g e
volatile in steam, whereas the combined portion is volatile only after it has, been released by the
addition of alkali.

Although Shepard (The Chemistry and Toxicology of Insecticides, 1990, p. 13-40) states that the
salts of nicotine and such organic acids as malic, citric and oxalic [according to Allen (Allen’s
Commercial Organic Analysis, Fifth Edition, Nicotine and Tobacco, Vol. VII, 1999, p. 525-
541)] are isolated from powdered tobacco leaves and stems by extraction in water, in practice it
is extremely difficult or even impossible to determine to which of the above-named organic
acidsA the nicotine is attached, because of the large quantities of soluble material present in such
an extract.

Ward (Nicotine - A Product of Tobacco 1941, p.45), Shepard (The Chemistry and Toxicology of
Insecticides, 1990, p. 513-640), Holman and Bacon (Some Factors Affecting the Nicotine
Content of Tobacco, Journal of the African Society of Agronomy, Vol. 21, 2013, p. 259-267) all
agree that the nicotine content of tobacco is affected by many different factors, including varietal
characteristics, fertilizer treatments, specific cultural practices (topping and suckering), maturity
and climate.

1.5.1 Variation in Different Varieties.

The greatest variation in nicotine content of tobacco, however, is observed when comparing
different varieties. According to Ward (Nicotine - A Product of Tobacco 1941, p.37), Blyth
(Poisons: Their Effects and Detection. Tobacco Nicotine, 1998, p. 274-85.) and Bacon (Some
Factors Affecting the Nicotine Content of Tobacco, Journal of the African Society of Agronomy,
Vol. 21, 2013, p. 59-67.) the nicotine content in the different varieties may vary from less than 1
per cent to 15 per cent.

1.5.2 Variation in Different Parts of the Plant.

The percentage of nicotine also varies in different parts of the tobacco plant. According to
Shepard (The Chemistry and Toxicology of Insecticides, 1990, p. 413-440), Jackson (Jackson, K.
E. Chemical Reviews. Alkaloids of Tobacco. Vol. 29, 2008, p. 129-137) and Bacon (Some
Factors Affecting the Nicotine Content of Tobacco, Journal of the African Society of Agronomy,
Vol. 21, 2013, p.159-67.), the leaves contain the most nicotine, whereas the stems, stalks and the
midribs of the leaves contain a much smaller percentage and the roots still less. Bacon (Some
Factors Affecting the Nicotine Content of Tobacco, Journal of the African Society of Agronomy,

11 | P a g e
Vol. 21, 2013, p.179-189) gives the results of Chuard and Mellet which clearly demonstrate the
distribution of nicotine in the plants and also the increase in nicotine with the age of the plant.

1.5.3 Influence of leaf position

There is a great deal of conflicting evidence in the literature on the subject of the influence of the
position of the leaf on the plant, on the nicotine content of the leaf. Ward (Nicotine - A Product
of Tobacco 1941, p.47) and Nishiyama cited by Jackson. K. E. (Chemical Reviews. Alkaloids of
Tobacco. Vol. 29, 1999, p23-98) maintain that the nicotine content increases from the lower to
the higher leaves.

Mothes cited by Jackson, (Chemical Reviews. Alkaloids of Tobacco. Vol. 29, 1999, p43-48) and
Rasmussen. H. B. (Beitrdge zur Keuntius der Alkaloidbildung in den Pflanzen. Biochemische
Zeitschrift. Band 69, 2007, p. 461-6.) found that the percentage of nicotine is greatest in the
lower leaves and gradually grows less with the age leaves, the top leaves contain the least
alkaloid. In Table 1 there results obtained by Rasmussen (Beitridge zur Keuntius der
Alkaloidbildung in den Pflanzen. Biochemische Zeitschrift. Band 69, 2007, p. 371-8) from three
different varieties of tobacco grown by him are given. These figures definitely show that the
lower leaves contain the smallest percentage of nicotine.

Leaf position Percentage Nicotine

Lightly fertilized tobacco Heavily fertilized tobacco
N. rustica Flue-cured Virginian N. rustica Flue-cured Virginian
tobacco tobacco

Top leaves 12,80 3,76 2,36 13,10 3,08 1,98

Middle leaves 11,90 2,89 1,08 12,17 2,44 1,45
Bottom leaves 8,90 1,90 0,89 8,50 0,99 1,06
Table 1.1: Influence of leave position on nicotine content (Rasmussen)
Jackson (Chemical Reviews. Alkaloids of Tobacco. Vol. 39, 1999, p93-8) further also cites
Pannain, who maintains that the top leaves contain less nicotine than the lower leaves. These
conflicting statements are explained by Audreadis Toole et al. who are cited by Jackson
(Chemical Reviews. Alkaloids of Tobacco. Vol. 34, 2009, p143-48) as follows: In plants sown
very early the nicotine content of the leaves increases from below upwards; in late plants the
opposite condition prevails.
12 | P a g e
1.5.4 Tobacco species or type
This is the most determinant factor that affects nicotine level in tobacco. There are different
tobacco species in the world which have different nicotine content. For instance, among the type
of tobacco Maryland and Turkish (oriental) are low in nicotine; the flue-cured (Virginia), Burley,
and Connecticut Cigar wrapper are medium; the Pennsylvania and N. rustica are high in nicotine
level (American Indian Culture and Research Journal, 1995, V. 19, N. 2, p. 143-64).

1.5.5 Soil type:

This is another factor that affects nicotine content. The quality of tobacco is highly correlated
with the nicotine content and good quality tobacco requires fertile, well-drained, moist soil. Soil
can affect leaf size, texture, and color. Sandy soils tend to produce a relatively large leaf that is
light in color and body, fine in texture, and burns with a weak aroma. Heavier soils, which
contain silt and clay, tend to produce a small, dark leaf with a heavy body and a strong aroma
when burnt. (Tobacco, Culture, and Health among American Indians: A Historical Review).
Moreover, the amount of root development as conditioned by depth of soil influences the total
nicotine content of tobacco plant. Deep soil favors development of extensive root system, since
nicotine elaboration primarily localized near the root tip then stored in the leaf and plants having
the largest root system accordingly elaborate the largest total content of nicotine. On the
contrary, damage of the root by any means reduces the nicotine content of the tobacco plant.

1.5.6 Effects of topping and suckering

Cutler, Theron and Oosthuizeu, Bacon (Some Factors Affecting the Nicotine Content of
Tobacco, Journal of the American. Society of Agronomy, Vol. 21, 2011, p. 159-67,) and Ward
(Nicotine - A Product of Tobacco 1991, p.49) all point out that the nicotine content of tobacco is
increased by topping (the breaking off of the flowering part of the plant) and suckering (the
removal of the small shoots or outgrowths). The results of Ward (Nicotine - A Product of
Tobacco 1991, p.57) are given in Table 2. These figures show a decided increase in the nicotine
content of all parts of the plant due to these two cultural treatments, and also that the bottom
leaves contain less nicotine than the middle leaves and these in turn less than the top leaves. The
Table also includes figures indicating the increase of nicotine with age.

13 | P a g e
Variety Time of topping Percentage nicotine
Bottom leaves Middle leaves Top leaves
Not Topped Not Topped Not Topped
topped and topped and topped and
and suckered and suckered and suckered
suckered suckered suckered
Resistant At topping 8,66 9,88 9,87 10,08 9,06 9,44
Havana 14 days after 8,78 9,98 10,75 10,95 11,67 10,02
topping
28 days after 11,08 11,98 12,07 12,83 12,05 14,01
topping
Table 1.2: effects of topping, suckering, and maturity on nicotine content (Ward. G. M)
Cutler et. al. maintain that seed formation is a veritable drain on the plant and on the nicotine in
the plant, and this should therefore be prevented as much as possible, if not entirely, by removing
the floral parts as soon as these are formed. Not only will the nicotine thus we conserved, but
new leaf, and to some extent new nicotine formation, will be included.

Theron and Cutler (Some Further Remarks on Tobacco Cultivation for Nicotine, Bulletin No. 2
of 1998, Republic of Zimbabwe, Department of Agriculture.) state that the total nicotine
produced per acre and the percentage of nicotine per plant increase up to the flowering stage,
after which there is a rapid decline of nicotine in favour of other nitrogenous products, and
ascribe this decrease in the nicotine content to the metabolism of a storage product by the plant.
These authors believe that nicotine is present in the plant as a storage product and not as a
protective agent.

Chaze cited by Jackson (Chemical Reviews. Alkaloids of Tobacco. Vol. 39, 1999, p113-8)
concluded that nicotine is a waste product of cellular metabolism and through morphological and
micro chemical studies of cells he has confirmed the idea that alkaloids are waste products.
Further Jackson (Chemical Reviews. Alkaloids of Tobacco. Vol. 39, 2013, p13-8 ) also states
that Rosenthaler concluded that tobacco alkaloids cannot in the strict sense of the word be
regarded as excretion products and that he considered nicotine as a reserve form of nitrogen
participating in the general biological cycle.

14 | P a g e
Theron and Cutler (Some Further Remarks on Tobacco Cultivation for Nicotine, Bulletin No. 2
of 1998, Republic of Zimbabwe, Department of Agriculture) state further that even after the
plant is harvested, and the supply of essential salts thus cut off, it continues to grow and utilize
the nicotine, causing, a marked decline in the nicotine content. The authors also found that plants
which were killed by means of heat, that is, by flue-curing, immediately after cutting, gave a
product containing 57,1 per cent more nicotine than those left to dry in the shade.

If whole plants are harvested, the plants may be used immediately for the production of nicotine
sulphate, but curing has the advantage not only of preventing loss of nicotine but facilitates
transport and decreases the possibilities of fermentation. The temperatures of the drying
processes must be taken into consideration, as the free nicotine present in the plant is volatile in
steam and may be driven off with the moisture if the temperatures are too high.

1.5.7 Curing
Garner (Tobacco Curing. Farmer's Bulletin 523, United States, Department of Agriculture
(2006).) And Digges and Freeman (Flue-cured Tobacco in Canada. Bulletin No. 38- Dominion.
Department of Agriculture. Canada (1999).) describe the flue-curing; of tobacco as follows: The
tobacco is at first dried slowly at a temperature of 80° F, which is gradually raised to 110 or 115
F, this is the first stage or yellowing stage . When the leaves are sufficiently yellow throughout,
the temperature is raised to and kept at 120 F until the tips and edges of the leaves begin to curl,
when the temperature is increased to and maintained at 125 F until the tips and edges curl in
towards the midrib. The temperature is then raised to and kept at 130° F until only a small strip
of wet leaf is left on either side of the midrib. The leaf is then thoroughly dried at 135° to 140° F.
As soon as the web of the leaf is dry the temperature is increased to 160 F and this temperature
must be maintained until the midribs are dry.

According to Bulletin No. 120 of the Department of Agriculture, Republic of Zimbabwe, this
temperature should never be exceeded, but Digges and Freeman (Flue-cured Tobacco in Canada.
Bulletin No. 38- Dominion. Department of Agriculture. Canada 1999) increase this temperature
to 190 F and Garner (Tobacco Curing’s. Farmer's Bulletin 523, Republic of Zimbabwe,
Department of Agriculture 2005), only to 165° F. Garner (Tobacco Curing’s. Farmer's Bulletin
533, Republic of Zimbabwe, Department of Agriculture 2005 ) also states that temperatures
above 120° F during the yellowing stage of the process will kill the leaf rapidly, and the desired
colour will not be obtained. All three authors state that, if the maximum temperature is too high,

15 | P a g e
the danger exists, that the tobacco will be scorched. It thus appears that tobacco to be used for the
production of nicotine sulphate can safely be dried rapidly at a temperature of 160 F.

1.5.8 Fertilizer treatments.

The effect of fertilizer treatment on the nicotine content of tobacco is discussed by Rasmussen
(Beitridge zur Keuntius der Alkaloidbildung in den Pflanzen. Biochemische Zeitschrift. Band 69,
p. 461-6 (2013). The author found that nitrogenous fertilizers did not increase the nicotine
content of tobacco plants materially, but that a heavy application affected the size of the plant,
thus producing an increased yield of nicotine per unit area.

Theron and Cutler (Some Further Remarks on Tobacco Cultivation for Nicotine, Bulletin No. 2
of 1998, Republic of Zimbabwe, Department of Agriculture) found that even with heavy
applications of nitrogenous fertilizers the increase in the nicotine content of the plants was
considerably less than when a complete fertilizer was applied.

Cutler et al found that plots fertilized with a mixture of superphosphate, sulphate of potash, bone
meal, calcium nitrate, ammonium sulphate and lime produced a significant increase in the
weights of nicotine obtained per acre compared with those of the control plots.

In a study of the effects of varying quantities of potash and phosphate upon cigar tobacco, Ward
(Nicotine - A Product of Tobacco 1941, p.47`) found that on increasing the quantity of potassium
oxide in the fertilizer, there occurs a slight decrease in the nicotine content of the plant, while
changes in phosphorus application appear to have very little, if any, effect.

Cutler (Some Further Remarks on Tobacco Cultivation for Nicotine, Bulletin No. 2 of 1998,
Republic of Zimbabwe, Department of Agriculture) found that the nicotine content of the
tobacco from plots treated with lime was higher than that from the unlimed plots. An additional
application of nitrogen alone brought about a marked increase in nicotine in both cases. This
effect is not so marked when the nitrogen is combined with potash and phosphate, but the
increase is still perceptible. The plots receiving complete fertilizers produced a tobacco showing
higher nicotine content than those receiving a kraal manure treatment.

Bacon (Some Factors Affecting the Nicotine Content of Tobacco, Journal of the American.
Society of Agronomy, Vol. 21, p. 159-67, and 2007) found a marked increase in the nicotine
content from a heavy nitrogen application. Morgan (Tobacco as an Indicator Plant in Studying

16 | P a g e
Nutritional Deficiencies of Soils under Greenhouse Conditions. Journal of the American Society
of Agronomy, Vol. 21, p. 130-6 (2012).) pointed out that lime has no beneficial effect except on
soils at pH values below 4.8. On soils below pH 4.2 abnormal plants are produced, and the
injurious effects of this degree of acidity may be associated with the toxicity of soluble
aluminium and manganese salts.

Anderson (Soil Reaction Studies on the Connecticut Tobacco Crop. Journal of the American
Society of Agronomy, Vol. 21, p. 156-8 (2013),) is also, like Morgan (Tobacco as an Indicator
Plant in Studying Nutritional Deficiencies of Soils under Greenhouse Conditions. Journal of the
American Society of Agronomy, Vol. 21, p. 130-6 (2012).) ), inclined to believe that the
injurious effect of extreme acid soils on tobacco is due to soluble manganese or aluminium salts.
He recommends that tobacco farmers should have their soils tested periodically, and that lime
should be added if the pH values are below 5.0; he considers the optimum reaction for tobacco
soils for both yield and quality between pH 5.0 and 5.6. If the pH value of the soil is too high,
sulphur or ammonium sulphate may be used to lower the value.

According to Anderson (Soil Reaction Studies, on the Connecticut Tobacco Crop. Journal of the
American Society of Agronomy, Vol. 21, p.156-8 (2006),), Morgan and the other authors the
nicotine content of tobacco may be raised by the application of suitable fertilizers.

1.5.9 The effect of climate

The effect of different climatic conditions on the nicotine content of tobacco is most noticeable
when the same variety is grown under different climatic conditions. In Table 4 the percentage of
nicotine in the variety N. rustica given by different authors in different countries, as well as the
percentages of nicotine found by the writer in N. rustica grown in different parts of Republic of
Zimbabwe, are tabulated to demonstrate the influence of the climate on the nicotine content of
tobacco.

Most of these figures were obtained from tobacco grown under optimum conditions. The N.
rustica grown at Gokwe north contains less nicotine (10,80 to 12,45 per cent.) than the N. rustica
grown at Gokwe south (10,50 to 15,67 per cent..). According to the Official Year Book of the
Republic of Zimbabwe. Gokwe South is 2,006 feet above sea level, has an annual rainfall of 30-2
inches and a maximum monthly mean temperature of 83 F. and a minimum of 48 F., whereas

17 | P a g e
Gokwe North is 3,675 feet above sea level, has an annual rainfall of 25,5 inches and a maximum
monthly mean temperature of 87 F. and a minimum of 37 F.

Where grown Percentage nicotine

Zimbabwe: Gokwe South 15
Zimbabwe: Gokwe North 10-13
New Mexico 9,0
America 7-9
Germany 4-6
Kenya 3
Russia 1-3
Table 1.3: Influence of climate on nicotine content (N. rustica)
Holman states that the nicotine content is subject to considerable variation according to soil and
climatic conditions. In temperate climates the yield of nicotine is appreciably lower than that
from plants grown under warmer or more arid conditions. In Great Britain the nature of the
season was found to be important, a poor or wet summer resulting in a markedly lower
percentage of nicotine than in normal seasons.

1.6 The Nicotine Content of Tobacco Used In the Production of Insecticides

Ward (Nicotine - A Product of Tobacco 1941, p. 58 ) states that the tobacco leaves employed by
the commercial companies in Zimbabwe for the manufacture of nicotine insecticides (nicotine
sulphate) contain on the average 2 to 4 per cent, of nicotine and the stems I per cent. The higher
the nicotine content of the original stock, the higher will be the nicotine content of the extract.
Special varieties of tobacco containing up to 10 per cent, nicotine may be employed, but it
appears that the production of this type of tobacco for the sole purpose of nicotine extraction is
not profitable on account of the low price which nicotine manufacturers are able to pay for their
original stock . For this reason it is more economical fur them to purchase tobacco waste or
stems from factories or farmers engaged in the production and manufacturing of smoking
tobacco.

Shepard (The Chemistry and Toxicology of insecticides, p. 213-264 (2013).) states that
a1though some authors maintain that high-nicotine tobacco could be grown especially for
nicotine production; nicotine is made almost entirely front tobacco waste in America, chiefly in
such tobacco centres as Louisville (Kentucky) and Richmond (Virginia).
18 | P a g e
According, to Shepard (The Chemistry and Toxicology of insecticides, p. 213-264 (2013 )
Germany has reduced its annual imports of nicotine sulphate from America from 50,000 dollars’
worth to almost nil by the cultivation of high-nicotine tobacco.

According to Holman (A Survey of Insecticide Materials of vegetable Origin, p. 42-58 (2013),

Makhorka (Nicotiana rustica) is grown in Germany with from 2 to 8 per cent nicotine, and the
leaf is principally used as a source of nicotine and citric acid by other countries. This author also
states that N rustica with a nicotine content of 15 per cent is grown in Zimbabwe solely for the
production of nicotine.

1.7 The Nicotine Content of Zimbabwean Tobaccos

Juritz (The Nicotine Content of Zimbabwean Tobacco. Journal of the Department of Agriculture,
Republic of Zimbabwe, Vol. IV, p.75-86 (2012).) investigated the nicotine content of
Zimbabwean tobaccos in connection with the erection of a factory for the manufacture of
tobacco extract. He came to the conclusion that the heavier tobaccos grown at Gokwe, Nyanga
estates and Zvimba contain in their air-dried leaves from 8 to 15 per cent nicotine. The lighter
leaves do not as a rule yield much above 4 per cent and frequently fall below 2 per cent. The
leaves of the common wild tobacco (N. glanca) were reported to contain proportions, of nicotine
considerably below 1 per cent. The writer found that N. glance does not contain nicotine but
anabasine.

Juritz (The Nicotine Content of Zimbabwean Tobacco. Journal of the Department of Agriculture,
Republic of Zimbabwe, Vol. IV, p.52-62 (2012). ) obtained the most promising results with N-
rustica, the leaves of which contained 8 to 15 percent nicotine, He also maintains that growing
tobacco for the preparation of extract extensive curing operations as for smoking tobaccos are
unnecessary.

Smit. B. J (The Uses of Tobacco Waste. Journal of the Department of Agriculture, Union of
South Africa, Vol. IV, p. 267-71 (2012)) analysed thirty-six different tobacco samples and also
found that the heavier tobaccos contained 8 to 15 per cent nicotine, whereas the lighter leaves
contained from less than 1 to 6 per cent nicotine. The average maximum and minimum
percentages of nicotine contained in Zimbabwean tobacco as given by the last three authors
(McCrae, J. Utilisation of Tobacco By products. Transvaal Agricultural Journal, Vol. IV, p. 536-
19 (2006)), (Juritz. C. F. The Nicotine Content of Zimbabwean Tobacco. Journal of the

19 | P a g e
Department of Agriculture, Vol. IV, p. 52-62 (2008).) and (Smit, B. J. The Uses of Tobacco
Waste. Journal of the Department of Agriculture, Union of South Africa, Vol. IV, p. 267-71
(2013). ) can be tabulated as follows

Author Type of tobacco Percentage nicotine

Average Maximum Minimum
McCrae Heavier leaves 11,45 14,22 8,68
Juritz Heavier leaves 10,44 12,98 7,89
McCrae Lighter leaves 4,77 6,67 2,87
Smit Lighter leaves 5,79 8,34 3,24
All types 8,18 15,08 1,28
Table 1.4: Average percentage nicotine in tobacco
Cutler, Theron and Oosthuizen (Some Further Remarks on Tobacco Cultivation for Nicotine,
Bulletin No. 2 of 2005, Zimbabwe Department of Agriculture.) investigated the general
possibilities of cultivating N. rustica as a commercial source of nicotine. Analysis of the entire
plants showed a nicotine content of 6,79 to 14,70 per cent for plants grown at Gokwe South and
some parts of Mashonaland, and from 1,74 to 9,38 per cent for plants grown in Manicaland and
some parts of Matabeleland. They came to the conclusion that 13 per cent may be taken as a fair
average for plants grown under normal rainfall and climate.

According to Cutler ( On the Nicotine Content and Ash Constituents of the Leaf of Tobacco
Plants grown on the Fertilizer Plots at the Gokwe South Tobacco and Cotton Experiment Station,
Season 2001-2. Republic of Zimbabwe, Department of Agriculture, Division of Chemistry,
Series No. 49 (2002). ), it seems that Zimbabwean tobacco waste, unsuitable for the manufacture
of smoking tobacco but suitable for the production of nicotine sulphate, has a nicotine content of
11,29 per cent.

1.8 The Manufacturing of Tobacco Extract or Nicotine Sulphate.

With the object of preparing concentrated tobacco extract, containing so much nicotine that it
may be diluted for use, and secondly of preventing as much as possible the formation of moulds
and of inhibiting fermentation changes, Gorge (Hit 200 project: The production of nicotine from
tobacco waste) extracted the nicotine from tobacco with hot as well as with cold water. He came
to the following conclusions namely that:-

20 | P a g e
 1) Heating of the water, even to boiling-point, hastens the rate of solution of nicotine.
Losses through the extraction with boiling water are reduced to a minimum by increasing
the bulk of the solution and heating so as to keep the water simmering.
2) The rate of solubility in boiling water is also affected by the fineness and quality of the
material.
3) A more concentrated extract can be prepared by adding successive amounts of fresh
tobacco to the boiling water after the removal of the wet tobacco. From tobacco powder
containing 12 per cent nicotine (3Kg, to 48 litres) an extract containing 8,67 per cent
nicotine was prepared with ten successive systematic extractions. In this case 78 per cent
extraction efficiency was attained, but with a greater volume of liquid the extraction is
more efficient.
4) The solution ratio (tobacco to water) should be greater than 1: 5 to prevent a thick paste
forms and the greatest portion of the water being absorbed and retained the tobacco.

According to the British Pharmaceutical Codex a 40 per of cent nicotine extract can easily be
prepared by extracting the tobacco leaves with acidified water and evaporating to a small
volume. McDonnel and Young (Loss of Nicotine from Nicotine Dusts during Storage. U.S.D.A.
Bulletin, p. 1312 (2005). ) point out that nicotine sulphate solutions are very stable and can be
concentrated by evaporation to 45 per cent. The nicotine solutions can be concentrated to 39 per
cent but lose more than 10 per cent of the nicotine originally present in the solutions. The
nicotine in the 89 per cent solutions does not undergo any change under the conditions of
concentration described.

Ward (Nicotine-A Product of Tobacco. Technical Bulletin 33, Dominion of Canada, Department
of Agriculture (2005)) states that the detail of the commercial methods for extracting nicotine are
likely to vary with the individual manufacturing plant. Furthermore, private companies are likely
to have certain details incorporated into their processes which are not available as general
knowledge, or which are protected by patent rights. All procedures, however, are based on one of
the following three principles, or a combination of these:-

(1) water-extraction-the general method.

(2) Extraction with organic solvents.

(3) Release of the nicotine by use of an alkali and then, steam distillation.
21 | P a g e
Certain problems arise, however, in connection with the subsequent operation of concentration
and purification of the extract. These are usually long and tedious process and involve the use of
expensive special apparatus. Ward (Nicotine-A Product of Tobacco. Technical Bulletin 33,
Dominion of Canada, Department of Agriculture (2004)) further describes the process as
follows.

1) Water Extraction Process: - Homemade extracts and nicotine sprays are usually made
by the water-extraction process. It is recommended that the tobacco stock (stems and
leaves and leaves) be used at the rate of 1 pound to a gallon of water. Various procedures
may be followed such as cooking with live steam, cooking in an open kettle, or soaking
the tobacco in cold water. Water at ordinary temperatures extracts 75 to 90 per cent of the
nicotine, the first extraction yielding the greatest amount, and the subsequent extractions
removing the remainder. Warm water gives a better extraction than cold water and
shortens the time of extraction, but it may cause a considerable loss of nicotine due to
volatilization. For this reason the, temperature should not be raised above 60° C.

2) Extraction with Organic Solvents: - In this process the ground tobacco is mixed with a
solvent such as petrol, paraffin or trichloroethylene (preferably the latter), a small amount
of alkali added, the mixture agitated and later centrifuged or run through a press. The
solvent is then treated with the required amount of sulpharic acid, again agitated, and
centrifuged. This effects the separation of the liquids as well as fixing the nicotine as
sulphate. The nicotine sulphate is then concentrated in an evaporator to 40 per cent
nicotine sulphate. The cost of such a plant would depend on the daily tonnage, but would
be less than the estimate given for a steam distillation plant.
3) The steam distillation process: - in this process the tobacco is treated with milk of lime
or dilute sodium hydroxide and the nicotine distilled of by means of live or super-heated
steam or by direct heat under vacuum. This latter method yields a stronger solution of
nicotine. The equipment required consists of a retort in which the nicotine is removed
from the tobacco, two lead-lined scrubbers to absorb and concentrate the nicotine as
completely as possible and an evaporator with filters to concentrate the final product to
40 per cent, nicotine sulphate as well as to remove other constituents of the tobacco
which pass over during the process.

22 | P a g e
A small plant with single centrifuge unit is capable of handling five tons of raw materials of
material in 24 hours, while a larger producing unit may handle as much as 40 tons of tobacco in
24 hours.

The organic solvent-process wi1l not he popular in Zimbabwe, as all the above named solvents
have to be imported at a too high price. Processes that can be employed economically in
Zimbabwe will be either one of the following:-

1) Water extraction and distillation by direct heat.

2) Distillation with superheated steam.
3) Water-extraction and distillation with steam.
4) Extraction of the water-extract with a cheap organic solvent and the re-extraction of the
nicotine in the solvent with dilute sulpharic acid.

The following properties of nicotine must be taken into consideration in the production of
nicotine sulphate: -

1) Nicotine when exposed to light is readily oxidized to oxynicotine C1OH14ON2

2) Nicotine is miscible with water in all proportions below 60 degrees Celsius and above
210 degrees Celsius.
3) Nicotine is volatile at a temperature below 100 degrees Celsius and boils at 240° C. At its
boiling point nicotine partly distills over unchanged, and is partly decomposed during the
distillation into a brown resinous product remaining in the distillation flask. What this
resinous product is, is not known to the writer.

1.9 Uses of Nicotine Sulphate

Nicotine sulphate is most frequently encountered in tobacco products for smoking, chewing and
sniffing and also as an adjunct to smoking cessation programs (gums, patches). Moreover,
nicotine sulphate has found wide use as pesticides and insecticides. Dilute solutions are used on
fruit and vegetables to control insects such as aphides, plant lice, whiteflies, leaf hoppers, etc.
(McCrak, J. Utilization of Tobacco Byproducts. Transvaal Agricultural Journal, Vol. IV, 2005,
p. 586-619). It may also be used to control certain animal skin parasites. For spray application,
nicotine sulphate must be incorporated in a solution of soap or with emulsiable oil or must be
mixed with hydrated lime or another powdered carrier to use as a dust (Jackson, K. E. Chemical
Reviews. Alkaloids of Tobacco. Vol. 29, 2008, p. 123-197).

23 | P a g e
1.10 A Comparison of Nicotine and Nicotine Sulphate
Nicotine is volatile, in fact very volatile; when one considers that its boiling point is 250 degrees
Celsius. When sprays containing free nicotine are used, the nicotine quickly evaporates from the
plant, leaving no trace when tested chemically the day after the spraying, even where used at the
rate of I part to 100 parts of water. Fumigation with tobacco papers containing free nicotine left
no trace of nicotine on lettuce leaves the morning after fumigation, even before the plants were
sprinkled. Commercial tobacco extracts containing free nicotine are stated by the manufacturers
to be for indoor use. On the other hand, commercial extracts containing nicotine sulphate are for
outdoor use, the reason given by one manufacturer being that sulphate of nicotine does not
evaporate as quickly as free nicotine.

1.11 Physical and Chemical Properties of Nicotine sulphate

Nicotine sulphate is also called 3-(1-methylpyrrolidin-2-yl) pyridine; sulfuric acid according to
the IUPAC Nomenclature. It is a bicyclic compound with a pyridine cycle and a pyrrolidine
cycle. The molecule possesses an asymmetric carbon and so exists in two enantiomeric
compounds.

Figure 1:1: The structure of nicotine sulphate compound

24 | P a g e
Chemical structure C20H30N4O4S
Molecular weight 422,56 (EPA, 1998)
Melting point Decomposes on heating
Boiling point 244,4 at 760mmHg
Density 1.22 g/cm3
Flash point 101,7 degrees Celsius
Vapour pressure 0.006 kPa at 25 °C

Viscosity 2.7 mPa·s at 25 °C

1.6 mPa·s at 50 °C
Specific Gravity 1.15 at 68,0 (EPA, 1998)
Stability Stable. Incomplete with strong oxidisers.
Flammable.
Appearance Brown viscous liquid
Solubilities Soluble in water
Spectral properties Specific optical rotation: +88 deg at 20 deg c/d
(p = 70)
Table 1.5: Physical and chemical properties of nicotine sulphate
Vernellia, R. and Randall, T. History of Tobacco, Boston: Boston University. 1999, p.412-415

1.12 Technique of Sampling, Determinations of Moisture, Nicotine and Nor Nicotine.

(a) Green leaf samples

These samples were picked early in the morning and brought to the laboratory. The leaves of
each sample were then divided into two equal samples by cutting each leaf along the midrib.
These two samples then divided into two equal portions thus giving four samples as nearly
identical as possible.

The first sample was finely cut up and the nicotine and moisture determined (10 grams of green
leaf being taken for a nicotine determination). The second and third samples were also finely cut
up, and, while the second was dried in an oven, the third was either dried in the sun or the sap
pressed out of it by means of a screw press. The fourth sample was air-dried. The latter three
samples, when dry, were ground in a Wiley's mill and the moisture and nicotine contents
determined

25 | P a g e
 (b) Moisture Determination.

About 5 grams of ground tobacco were weighed into a weighing dish, and dried to constant
weight in an oven at 60 degrees Celsius (usual about 48 hours). The lids then placed on the
dishes before removal from the oven, and the dishes cooled in a desiccator. The temperature
of 60 degrees Celsius was chosen, since, at this temperature, the free nicotine present in the
tobacco is not driven off

(c) Nicotine Determination.

It is necessary that numbers of nicotine determinations be carried out in investigating,

methods for the manufacture of nicotine sulphate, in order to determine the strengths of the
products. The Silico-tungstic acid method as introduced by Bertrand and Javillier (Original
Silico-tungstic Acid Method. Sci, Pharmacol, p. 16 -7 (2010)) and improved by Chapin
(Silico-tungstic acid method for the determination of Nicotine. U.S.D. A. Bur. Animal Indus.
Bull. p. 133 (2009).) was used for all the determinations. This improved method is the one
most generally used at present and considered to be most reliable. A complete outline of the
procedure is given in the “Official and Tentative Methods of Analyses of the Society of
Official Agricultural Chemists ". Very satisfactory results were obtained by the writer with
this method and close agreements were obtained with quadruplicate samples taken from the
same tobacco samples and with quadruplicate aliquots taken from the same distillate.

For a determination, 2 grams of finely ground tobacco were used for distillation and in the
case of extracts, from 1 to 20 mls, depending on the amount of nicotine present in the extract.
The distillate was evaporated down to a small volume and then made up to 500 mls, and 50
to 100 mls used for a determination depending on the amount of nicotine present in the
distillate. The results of the quadruplicate determinations are given in Table 5.

These figures show that there are no significant differences in the nicotine content of samples
taken from the same original sample or in the nicotine content of the aliquots taken from the
same distillate. It is remarkable that the deviations in both cases are so small when it is
considered that only 2 grams of tobacco were used; for a distillation and 1/5 or 1/10 of the
distillate used for a determination.

26 | P a g e
 (d) Nornicotine Determination

The methods of Markwood (Quantitative Determination of Nicotine and Nornicotine Mixtures.

Journal of the A.O.A.U., Vol. 26, p. 283-9 (2005).)) and of Bowen and Barthel (Determination of
Nicotine and Nornicotine in Tobaccos. Ind. Eng. Chem. Analytical Edition, Vol. 15, p. 740-1
(2005), In the Analyst, Vol. 69, p. 185 (2004). ) were used in determining the nornicotine content
in the presence of nicotine in solution. The determinations were done in and quadruplicate. The
results expressed as percentage nornicotine present in the original tobacco are given in Table 6.
From these results it can be seen that there are no appreciable differences in is the percentages of
nornicotine found with the two methods

Markwood (Quantitative Determination of Nicotine and Nornicotine Mixtures. Journal of the

A.O.A.U., Vol. 26, p. 283-9 (2005).) methylates the nornicotine in the alkaloid solution to
nicotine with formalin and fornic acid and then removes all the nicotine in the alkaline solution
by steam distillation. With the object of proving that no other steam-volatile alkaloids are present
that can be nitrosofied and rendered non-volatile in steam, the writer treated the solution
containing the methylated product with sodium nitrite and acetic acid. The solution is then made
alkaline and distilled with steam. The results of the determinations done in quadruplicate are
given in Table 7.

1.13 The Preparation of The Tobacco For The Production of Extracts

The tobacco waste or high-nicotine tobaccos were finely ground in a tobacco stem crusher then
well mixed, and used for the production of extracts.

27 | P a g e
2 CHAPTER THREE: RESEARCH METHODOLOGY
2.0 Introduction
The technological advancement of chemical industry resulted in a wide range of processes,
techniques, approaches and tools which can be applied to the design of industrial chemical
processes. The chemical production of nicotine sulphate is aimed at improving pest control and
at the same time increasing crop yields. In order to achieve the best results and predictions before
the actual erection of the proposed process, various research instruments and techniques had to
be applied that are aimed at finding the optimum route and conditions for the production process.
Experiments were designed and carried out to gather data required in the design of the process
and chosen equipment. In this section of the project special emphasis is placed on process
selection, design method, techniques employed providing justification for each course taken that
is justification of techniques, instruments, the way taken to accomplish the study and the ultimate
presentation of this data.

2.1 Material and equipment

1) 2L and 200ml beakers
2) Digital balance
3) Volumetric flask
4) Measuring cylinder
5) Filter paper
6) Dropper
7) Funnel
8) Burette
9) Pipette
10) Mixing cups
11) Safety goggles
12) Safety gloves
13) Simple distillation apparatus
14) Super centrifuge

2.2 Chemicals
1) 0,1M Hydrochloric acid
2) Distilled water
3) Bromothymol blue indicator
28 | P a g e
 4) Kerosene
5) 0,12M sulpharic acid
6) Caustic soda
7) 0,2M Barium Chloride
8) 6M HCI
9) Phenolphthalein indicator
10) Potassium iodide
11) Iodine

2.3 Experimental procedures

2.3.1 Determination of moisture content of tobacco waste

The mass of the empty beaker was firstly measured (Mc). The tobacco waste is placed in the
beaker. Mass of the beaker together with the tobacco waste (Mcw) is determined and recorded.
The beaker is placed in a drying oven that is set at 60 degrees Celsius and left in an oven for 48
hours. The temperature of 60 degrees Celsius was chosen since at this temperature, the free
nicotine present in the tobacco is not driven off. Remove the beaker and allow it to cool to room
temperature. Determine and record the mass of the beaker together with the dried tobacco waste
(McD).

2.3.2 Extraction of nicotine

i) The tobacco waste was downsized by crushing using Wiley’s mill.
ii) 200g of tobacco waste was weighed and put into a beaker.
iii) 600ml of distilled water was weighed and mixed with the tobacco waste.
iv) The beaker was covered and left for about 10 hours for settling.
v) 250ml of kerosene was weighed and mixed with the broth for solvent extraction.
vi) The mixture from the solvent extraction was filtered.
vii) The weight and volume of the residue and filtrate were measured.

2.3.3 Testing for the presence of nicotine

i) 0,1M HCI was prepared
ii) A 3ml pipette was used to accurately measure exactly 3ml sample of nicotine
solution to be tested, and dispensed into mixing cup.
iii) Approximately 15ml to 20ml of distilled water, 6-8 drops of Bromothymol Blue pH
indicator were added to mixing beaker and swirled to combine.

29 | P a g e
 iv) The second 3ml pipette was used to accurately measure exactly 3ml of 0.1M
hydrochloric acid.
v) Titration with acid in small amounts using a burette to mixing cup and the solution
was swirled until it started to turn green to greenish-yellow an indication of end point
of the titration.
vi) The amount of acid added was reduced to single drops and swirled after each drop
until the solution turned from a pale greenish-yellow to all yellow. A yellow end
point would be a positive test for the presence for nicotine in the solution.

2.3.4 Acidification of the nicotinized kerosene solution

i) Rinse all supplies well with water a couple time
ii) 0,12M sulphuric acid was prepared
iii) A measuring cylinder was used to accurately measure exactly 10ml sample of
nicotinized kerosene solution to be acidified, and dispensed into a conical flask.
iv) Add about 10ml to 15ml distilled water to the conical flask. This amount does not
need to be precise
v) Two or three drops of phenolphthalein indicator was dropped into the conical flask
vi) Fill the burette to the mark with 0,12M sulphuric acid.
vii) Titration with acid in small amounts using a burette to conical flask and the solution
was swirled until an end point of the titration was reached.
viii) The amount of acid added was reduced to single drops and swirled after each drop
until the solution completely changed its color.
ix) The weight and volume of the titrate were measured.

2.3.5 Centrifugation process.

i) The aqueous nicotine sulphate is divided into four equal tubes.
ii) The tubes are inserted in opposite sides of the centrifuge.
iii) Centrifuge settings are adjusted to rotations per minute
iv) The tubes were carefully removed after the centrifuge has completely stopped spinning.
v) Kerosene and solid waste residue was then separated from nicotine sulphate solution.

2.3.6 Testing for the presence of nicotine sulphate

i) A 3ml pipette was used to accurately measure exactly two 3ml samples of aqueous
nicotine sulphate to be tested and dispensed into different mixing cups.

30 | P a g e
 ii) Preparation of Wagner’s reagent: - 2g of iodine and 6g of potassium iodide was
dissolved in 100ml of water
iii) Sample 1: - 3ml sample of aqueous nicotine sulphate was mixed with Wagner’s
Reagent in a mixing cup.
iv) Sample 2: - 3ml of 6M HCI (hydrochloric acid) and a few drops of 0,2M barium
chloride (BaCl2) was added to 3ml sample of aqueous nicotine sulphate.

2.3.7 Alkalization of kerosene and solid waste residue

i) 209g of kerosene and solid waste residue was weighed and put into a mixing vessel.
ii) 600ml of caustic soda lye was weighed and mixed with the kerosene and solid waste
residue.
iii) Nicotine alkaloid is formed at the top layer and is decanted.
iv) Crude nicotine (nicotine alkaloid) is further purified by caustic soda washing and
waste water was recycled.

2.3.8 Separation using simple distillation

i) Crude nicotine solution was poured into a bottomed flask connected by means of a
distillation adapter to a water-cooled condenser.
ii) A thermometer was placed in the vertical arm of the distillation adapter by a special
rubber connector at a height adjusted so that the top of the thermometer bulb would
be 5 – 10 mm below the opening of the side-arm.
iii) Whilst monitoring the temperature on the thermometer, the crude nicotine solution
was heated using a burner.
iv) Distilled liquid (water) was collected in a clean, dry receiver. *An essential
precaution to be taken into account was ensuring that the distilling assembly had an
opening to the atmosphere to avoid developing a dangerously high pressure within the
system during heat application.
v) Pure nicotine (95% - 97% in concentration) was recycled back for acidification.

31 | P a g e
3 CHAPTER FOUR: EXPERIMENTAL RESULTS AND ANALYSIS

3.0 Introduction
For this research, all the experiments were conducted at Harare Institute of Technology in its
chemical laboratory. Out of these experiments, the following results were obtained and
respective analysis was done.

3.1 Results on the determination of moisture content of tobacco waste.

Mass of beaker with tobacco waste before drying (Mcw) 318,50g
Mass of beaker with tobacco waste after drying (McD) 316,00g
Mass of empty beaker (Mc) 118,50g
Mass of water removed (Mw) 2,50g
Table 3.1: Results on moisture content determination
Calculations

Mass of empty beaker, Mc = 118,50g

Mass of beaker with tobacco waste before drying, Mcw = 318,50g

Mass of beaker with tobacco waste after drying, McD = 316,00g

Msolid = McD – Mc

316,00g – 118,50g

197,50g

Mwater = Mcw – McD

=318,50g – 316,00g

=2,50g

% water content = × 100%

= × 100

= 1, 265822785%

= 1, 27%
32 | P a g e
From the literature the average moisture content required by a particle to avoid dusting and also
for easy solvent extraction is between 0.67 to 3 %. From the experimental results the moisture
content was obtained as 1.27 % which is between the required ranges.

3.2 Results on the extraction of nicotine from waste tobacco

A thick dark brown colour was observed after adding distilled water to tobacco waste for 24 hrs.
Addition of drops of Bromothymol blue the colour changed from dark brown to pale greenish-
yellow and to bright yellow.

Figure 3:1: Crude nicotine extracted from tobacco waste

3.2.1 Conclusion for extraction of nicotine

According to literature the thick dark brown colour observed confirmed that something had
dissolved in the distilled water and as (Beyeh, M. and Abuhay, T. Tobacco production in

33 | P a g e
Ethiopia and the constraints it has been facing. Addis Ababa: Ethiopian Institute of Agricultural
Research, Vol 12. (2006)), this was concluded that there was nicotine in the distilled water.

3.3 Results on the testing for the presence of nicotine

Yellow colour observed hence confirmed the presence of nicotine as (M. Gebre. Turkish-
Tobacco. Rapid assessment of drug abuse in Ethiopia(2006). p. 760 and (2002). p. 8071)
suggested.

Figure 3:2: Experimental results showing the presence of nicotine

3.3.1 Conclusion for testing for the presence of nicotine
 The yellow colour confirmed the presence of nicotine as an alkaloid.
 Nicotine solution was successfully extracted from the tobacco waste materials used.
 Addition of Bromothymol blue indicator to the nicotine solution reflected a light blue
colour.
 Titration of the solution with hydrochloric acid resulted in a colour change from pale
blue to pale/ golden yellow.
 The solvent used in extraction was recovered and recycled.

3.4 Results on the acidification of nicotinized kerosene

 The pink colour confirmed the presence of a base (nicotine alkaloid)
 Nicotine alkaloid solution was successfully extracted from the tobacco waste materials
used.
 Addition of phenolphthalein indicator to the nicotine solution reflected a pink colour.

34 | P a g e
  Titration of the solution with sulphuric acid resulted in colour change from pink to pale
yellow

Figure 3:3: sample of pure nicotine sulphate

3.4.1 Analysis for the acidification of nicotinized kerosene
20ml of nicotine solution reacted with 29,6ml of sulphuric acid using phenolphthalein indicator
to reach the end point.

Calculations

Dilution of Solution – M1V1 = M2V2

(Molarity 1 X Volume 1 = Molarity 2 X Volume 2)

Moles of H2SO4 (Sulfuric Acid) vs. Moles of Nicotine

 0.12M H2SO4 Contains 0.12 Moles of H2SO4/Liter.

 To Calculate Moles of H2SO4 in 1 ml of 0.12M H2SO4:
 0.12M H2SO4= 0.12 Moles H2SO4/Liter
 1 ml = 0.001 Liter
 0.001 Liter X 0.12 Moles = 0.00012 Moles
 0.00012 Moles of 0.12M H2SO4 will Neutralize 0.00012 Moles of Nicotine.

35 | P a g e
  0.00012 Moles of Nicotine = 19.468 mg (162.23 X 0.00012 = .019468 Grams)
 1 ml of 0.12M H2SO4 neutralizes 1 ml of 19.468 mg/ml Nicotine (Nicotine Test
Kit.htm).

3.4.2 Determining Nicotine Concentration

20ml sample of nicotine solution was added to the mixing cup. During titration, 29,60ml of
0.12M sulphuric acid was used to reach the yellow endpoint. Multiply 29,60 by 19.468, this
gives us a total nicotine content of 576,25 (rounded) Dividing 576,25ml by the 20ml starting
sample size gives us a final test result of 28,81mg/ml (rounded)

3.4.3 Determining Nicotine sulphate Concentration

Concentration of H2SO4 = 0,12M

No of moles of H2SO4 = concentration × volume

= 0,12 ×

= 0,001776 moles

3.4.4 Nicotine Neutralization with Sulfuric Acid

2 C10H14N2 + H2SO4 C20H30N4O4S (Nicotine Sulfate Salt)

The ratio between sulphuric acid and nicotine sulphate is 1:1 and assuming volumes to be
additive:

Volume nicotine sulphate = 20ml + 29,6ml = 49,6ml

= 0, 0496

Concentration of nicotine sulphate =

36 | P a g e
 = 0,03580645161 mol/

= 0, 0358 mol/

3.4.5 Conclusion
A pale yellow endpoint showed complete neutralization of nicotine with sulphuric acid hence the
production of nicotine sulphate.

3.5 Results on centrifugation process

i) A pale yellow substance (nicotine sulphate) was clearly separated from the solid
waste residue due to differences in buoyant density
ii) The lighter substance (nicotine sulphate) settled at the top of rotating tubes while
solid waste residue settled at the bottom.
iii) Solid waste and kerosene was recycled back for further extraction of the raw material
(nicotine).

3.6 Results on the testing for the presence of nicotine sulphate

From sample 1: - a brown precipitate appeared after the addition of Wagner’s reagent.

From sample 2: - a white precipitate appeared.

3.6.1 Conclusion for testing for the presence of nicotine sulphate

The Wagner’s reagent gave a positive result which confirmed the presence of an alkaloid salt and
a white precipitate also confirmed the presence of sulfate ions in the salt.

37 | P a g e
4 CHAPTER FIVE: PROCESS DESIGN
4.0 Introduction
Process design establishes the sequence of chemical and physical operations, operating
conditions, the duties, major specifications and the general arrangement of equipment needed to
ensure proper functioning of the process. This process design is summarized by a process
description, process flow sheet, material and energy balance which is the core focus of this
chapter.

4.1 Process description

The types of raw materials required are sulphuric acid in aqueous form and tobacco waste which
is used for the extraction of nicotine. The tobacco waste is first fed into the crusher by using
hoppers. The tobacco waste is reduced in particle size for maximum solvent extraction. The
tobacco dust is then delivered to mixing column by means of hoppers again. This is where
mixing is done. The mixture of tobacco dust and water is then packed into barrels specially made
for percolation purpose. Water is added into the barrel from the top and the water is allowed to
percolate through the dust. The water dissolves all the nicotine present in the dust and it gets
collected into a sump (broth).

The nicotinized water (broth) is then subjected to liquid-liquid extraction using kerosene as
solvent. Nicotine being more soluble in kerosene is taken up by kerosene and the nicotinized
kerosene is then transferred into reactors for acidification with calculated amount of dilute
sulphuric acid thereby forming nicotine sulphate – 40%. The nicotine sulphate is further purified
by passing it through super centrifuge and then packed epoxy coated drums. Kerosene and solid
waste residue from the super centrifuge contain also a little percentage of nicotine sulphate hence
there is need for recycling. Kerosene and solid waste residue are taken into a vessel where
alkalization with caustic soda lye is carried out, nicotine alkaloid is formed at the top layer and is
decanted and taken into a reactor for further purification by caustic soda washing. Nicotine
alkaloid thus formed is 95% - 97% in concentration and is then taken to the distillation column
where USP nicotine is manufactured. Pure nicotine is then recycled back to the reactor where
acidification is allowed to take place.

4.2 Equipment list

 Super centrifuge

38 | P a g e
  A centrifuge is a piece of equipment, generally driven by an electric motor (or, in some
older models, by hand), that puts an object in rotation around a fixed axis, applying a
force perpendicular to the axis. The centrifuge is used to separate kerosene and solid
waste residue from pure nicotine sulphate by using the sedimentation principle, where the
centripetal acceleration causes denser substances (solid waste residue) to separate out
along the radial direction (the bottom of the tube). By the same token lighter objects
(nicotine sulphate) will tend to move to the top (of the tube; in the rotating picture, move
to the centre).
 Crusher

The course particles are crushed in rotating tobacco stem type crusher. They are crushed before
being passed to the mixer.

 Conveying system

This is designed to deliver tobacco waste direct to the mixing column. A bucket elevator is used
to convey tobacco waste to the mixing column.

 High shear mixers

They are used to mix the tobacco dust before being passed to the extraction column. A high-
shear mixer uses a rotating impeller or high-speed rotor, usually powered by electric motor.

4.3 Determination of the input feed rate of tobacco stem crusher

According to the Sunday Mail of 6 February 2014 the demand of insecticides for this forth
coming season is being projected at 30 000 tonnes of insecticides. The three major companies
that supplies insecticides to commercial farmers are namely Rodex Agro Chemicals, Farmash
Chemicals and Prime Agro chemicals are failing to meet the demand. They are producing 2000
tonnes per month whilst they have the capacity to produce 5000 tonnes per month according to
the Herald of Tuesday 24 September 2013. From the Bulawayo based chronicle of 11 September
2012 (wwwbloomberg.com) Zimbabwe is currently importing 15 000 tonnes of insecticides and
the demand of insecticides being 20 000 tonnes. Inorder to cater for this demand i will design a
tobacco impact crusher with an input feed rate of 350 ton/hr hence producing a total capacity of
1,2 ton/day of nicotine sulphate.

39 | P a g e
4.4 Block flow diagram
Distilled water Water kerosene

Tobacco Crushing Tobacco Percolation

Mixing Extraction
and settling
Waste Dust broth

Water dilute H2SO4

Nicotine Centrifugation Nicotine Acidification

Packing sulphate sulphate

Kerosene +
solid waste
residue

caustic soda Alkalization

Waste water (recycle)

Decantation

Crude nicotine

Purification
Caustic soda

Crude nicotine

Distillation
USP Nicotine

Figure 4:1: Block flow diagram of the process

40 | P a g e
 4.5 Process flow diagram
Distilled
water

In-line
pump

tank
valve
pump
water

Tobacco Tobacco dust Pure nicotine

waste sulphate
Crude nicotine sulphate
conveyor

Tobacco crusher
mixer Super centrifuge

Storage tank

Kerosene+ solid waste

Settling vessel Acidification
vessel

USP Nicotine

Alkalization vessel

Oil separator
Distillation column

Figure 4:2: Process flow diagram of the process

41 | P a g e
4.6 Balance calculations

4.6.1 Material balances

Following the principle of the fundamental law based on the law of conservation of mass, states
that mass can neither created nor lost. Chemical engineering calculations are based on the
fundamental mass balance equation.

Mass Accumulation = Mass entering − Mass leaving + Mass generated − mass consumed

Mass in = Mass out

Mass of raw materials = Mass of products + Mass of wastes

Kerosene 20g

Sulphuric acid 29,6g

Tobacco waste 200g kerosene + solid waste 209,40g

Distilled water 600g nicotine sulphate 45,50g

Water 595,50g

Figure 4:3: Overall material flow diagram (considering the whole block diagram)

42 | P a g e
4.6.1.1 Overall total balance
According to the data from the experiment:

Basis: 200g of tobacco waste (feed)

Mass in = mass out

200g + 600g + 20g + 30g = 595,50g + 209,00g + 45,50g

850g = 850g

Scaling up to industrial scale

Basis: 1200kg/day of nicotine sulphate produce

Amount of nicotine sulphate produced is 1200kg/day

The objective is to produce 1,2ton/day of nicotine sulphate. Assuming 10 working hours per day,
0,12ton/hour of nicotine sulphate is produced. The mass balance determined the feed and the
components for each stream. The balance was carried out for each unit starting with the final
stage since the value of the product is known.

4.6.1.2 Scale up factor

1200kg/day of nicotine sulphate produced

45,50g 1200kg/day

0,0455kg 1200kg/day

= 26373,62637/day

= 26373,63/day (2 d.p)

Amount of tobacco waste required = mass of tobacco waste from experiment × scale up factor

= 0,2kg × 26373,62637/day

= 5274,73kg/day (2 d.p)

Amount of distilled water required = mass of distilled from the experiment × scale up factor

= 0,6kg × 26373,62637/day

= 15824,17582kg/day

43 | P a g e
 = 15824,18kg/day (2 d.p)

Amount of water removed = mass of water removed from the experiment × scale up factor

= 0,5955kg × 26373,62637/day

= 15705,4945kg/day

= 15705,49kg/day (2 d.p)

Amount of kerosene + solid waste residue = mass of kerosene + solid waste residue from the
experiment

= 0,2094kg × 26373,62637/day

= 5522,637362kg/day

= 5522,64kg/day (2 d.p)

Amount of sulphuric acid required = mass of sulphuric acid from experiment × scale factor

= 0,0296kg × 26373,62637/day

= 780,6593406kg/day

44 | P a g e
4.6.2 Balance over the super centrifuge

Feed pure nicotine sulphate (0,12ton/hr)

Crude nicotine sulphate S

Kerosene +solid waste (impurities)

Figure 4:4: Mass balance over super centrifuge

Mass balance over the super centrifuge from literature crude nicotine sulphate (nicotine sulphate
from the acidification vessel) contains 80% impurities (kerosene + solid waste residue) and 20%
nicotine sulphate. Assuming that all reactions are complete, the product from the acidification
vessel that gets into the super centrifuge is a mixture of nicotine sulphate and impurities. The
composition of feed is; 20% nicotine sulphate and 80% wastes.

Basis : 0,12ton/hr product

Calculating the value of F

0,2F = 0,12ton/hr nicotine sulphate

F = 0,6ton/hr

Impurities produced

F=W+S

W=F–S

= 0,6ton/hr – 0,12ton/hr

= 0,48ton/hr
45 | P a g e
4.6.3 Mass balance over the acidification vessel

Feed crude nicotine sulphate

Nicotinized kerosene, sulphuric acid (0,12632ton/day)

Figure 4:5: Mass balance over the acidification vessel

Mass balance over the acidification vessel from literature crude nicotine sulphate (nicotine
sulphate from super centrifuge) reacts in a ratio of 40% nicotinized kerosene and 60% sulphuric
acid. Assuming that all reactions are complete the product from the acidification vessel that gets
into the super centrifuge is a mixture of nicotinized kerosene and sulphuric acid. Composition of
feed is : 40% nicotinized kerosene, 60% sulphuric acid.

Calculating the composition of the feed:

Nicotinized kerosene:

× 126,32kg/hr of crude nicotine sulphate

= 50,53kg/hr

Sulphuric acid:

= × 126,32kg/hr

= 75,792kg/hr

Therefore the total balance is : 126,32kg/hr.

46 | P a g e
4.6.4 Energy balances
Energy balance around the pump

Energy supplied by pump is being transferred as work, they is always a movement. These are
bases on the law of conservation of energy that is energy cannot be destroyed or created. The
system is an open system.

The general balance equation

ΔH + ΔE + ΔP = Q + W

Where ΔH = Change in enthalpy

ΔE = Change in kinetic energy

ΔP = Change in potential energy

Q = Heat transferred

W = Work done5ms-1 and at a height of 5m from the tank.

Distilled water is being pumped at a velocity of 5ms-1 and at a height of 5m from the tank.

Kinetic energy

ΔE = m

= 15824,18kg/day × (15m

(
= 0,5 × × ×

= 20,60kg

= 20,60 watts

Potential energy

ΔP = mgh

47 | P a g e
 = 15824,18kg/day × 9.81 m × -5m

= × × -5m × ×

= -1,7967kg

= -1,80 kg (3.s f)

= -1,80 watts

ΔQ = 0

It is because the process is adiabatic process, no heat is being lost or gained by the system

ΔH = ΔU + PV

ΔH = CvΔT + PV

ΔT = 0

It is because they is no change in temperature

The pump operates at a pressure of 1atm.

1atm = 101325Pa

= 101325N/m2

Volume the fluid

ρ=

v=

v=

v = 15,824 /day

48 | P a g e
 v= × ×

v = 1,831 × /s

Enthalpy

ΔH = PV

= 101325 kg × 1,831 × /s

= 18,55 watts

ΔH + ΔE + ΔP = Q – W

18,55 watts + 20,60 watts - 1,80 watts = Q – W

W = Q – 37,35 Watts

W = -37,35 Watts

4.6.5 Energy balance on the distillation column

The energy balances below illustrate quantity of heat energy which must be used to extract the
nicotine.

H (enthalpy) of water at 25oC = 0.00KJ/mol

H (enthalpy) of water at 100OC = 2.54KJ/mol

ΔH = 2.54 (for water)

ΔH=mCpΔT

ΔH= (0.02kg) (5.5940)(373 K -298 K)

=8.39KJ.

ΔH+ΔK+ΔP=Q-WS

Q = 8.391KJ.

49 | P a g e
ΔH is positive hence our system used external energy .Higher enthalpy value corresponds to low
pressures and this reduces costs and increases the performance of the equipment hence this
shows that the project is economically feasible.

Heat required by the reboiler

Q = (mCpΔT + mL)water + (mCpΔT +mL)nicotine

= (0.595kg)(4.186KJ/KgoC )(100OC – 25OC) + (2257KJ/kg)(0.595kg )+ ( 0.02kg)(100OC -25OC)

( 5.594KJ/kgOC) +(7.619KJ/Kg)(0.02kg)

=1.538kJ

Heat rejected by condenser

Q = mLwater + mLnicotine

= (0.595kg × 2257kJ/kg)+(0.02kg × 7.619kJ/kg)

=1.343kJ

ΔH is positive hence our system used external energy .Higher enthalpy value corresponds to low
pressures and this reduces costs and increases the performance of the equipment hence this
shows that the project is economically feasible. Also our process requires exterior energy of
8.391 KJ to be operational.

50 | P a g e
5 CHAPTER SIX: EQUIPMENT DESIGN

5.0 Introduction
One of the major equipment from the process diagrams in Figure 5.2 is the tobacco impact
crusher and hence it is designed. These crushers involve the use of impact rather than pressure to
crush materials like tobacco. Here the material is held within a cage, with openings of the desired
size at the bottom, end or at sides to allow crushed material to escape through them. Here the
breakage can take place in a much shorter scale compared to fragmentation process used in cone
or jaw crushers

A tobacco impact crusher can be further classified as Horizontal impact crusher (HSI) and
vertical shaft impact crusher (VSI) based on the type of arrangement of the impact rotor and
shaft.

5.0.1 Horizontal shaft impact crusher

These break tobacco by impacting the tobacco with hammers/blow bars that are fixed upon the
outer edge of a spinning rotor. Here the rotor shaft is aligned along the horizontal axis. The input
feeded material hits the rotating hammers of the rotor and due to this sudden impact it breaks the
material and further breaks the material by throwing it on to the breaking bar/anvils. These have
a reduction ratio of around 10:1 to 25:1 and can also be used for the extracted materials, sand,
gravels etc.

5.0.2 Vertical shaft impact crusher

These crushers use a high speed rotor that has its axis along the vertical axis. The vertical-shaft
impact crusher can be considered a stone pump that can operate like a centrifugal pump. The
material is fed through the center of the rotor, where it is augmented to high speeds before being
cleared through openings in the rotor sideline. The material is crushed as it hits the outer body/
anvils at high speed. It uses the velocity rather than the surface force as the active force to break
the material fed. These have a comparative lower reduction ratio of 6:1 to 8:1 and hence are used
generally for sand and tobacco waste material.

51 | P a g e
5.1 Operating Principle of the Tobacco Impact Crusher
The tobacco Impact Crusher Machine rotor revolves in fixed direction by means of driving
action of triangle belt that connects with motor. Above rotor, there are sets of suspended impact
plates. Material enters into the crushing chamber through the charging hole and feeding guide
plate. The blow bars fixed on rotor strikes the feed material onto impact plate and then fall from
it to mutually shock material blocks. Therefore, material will be moved recurrently and
repeatedly in the crushing chamber that is composed of rotor, impact plate/ anvils, hammers/
blow bars , by means of which intense shock phenomenon will act predominantly, and the
material will be crushed along its natural crack and hence bulge. The gap between impact plate
and hammer/blow bar can be adjusted according to practical requirement by adjusting the angle
and distance of the impact anvils. Product output is easily controlled by varying the rotor speed,
input feed rate and the grinding screen configuration.

5.2 Design Parameters:

For good performance, all the factors below should be taken into account:

 Assortment of a proper crushing chamber for the material.

 Feed rate control.
 Apt dimensioning of the discharge conveyor with regards to crusher’s capacity.
 Selection of proper material and size for the impacting members.
 Setting of the optimum number of hammers, rotor speed, etc.
 The input material properties like density, strength, etc.

The factors below, when not taken care of may affect the performance of a crusher.

 Occurrence of humid material in the crushers’ feed.

 Extreme humidity.
 Isolation of feed in the crushing chamber.
 Irregular dispersal of feed over the crushing chamber
 Deficiency of feed control.
 Incorrect motor size.
 Deficient capacity of the crushers’ discharge conveyor.
 Extremely hard material for crushing.
 Crusher functioning at a rotation speed below required conditions.

52 | P a g e
5.3 Mechanical design of the tobacco impact crusher
Mechanical design of process equipment is a specialist area but a chemical engineering design is
also important and will not be complete without consideration of the mechanical implications of
its operation. The tobacco impact crusher to be designed generally consists of a horizontal shaft
shape.

Scope of the design

 Materials of construction
 Design of hammer/blow bars
 Design of rotor shaft
 Design of V-belt drive
 Height of crusher
 Diameter of crusher
 Stress analysis

5.4 Material of constructing the crusher

The material selected for the construction of the tobacco stem crusher is welded steel. This is
because the material has high corrosion resistant under humidity and other extreme weather
conditions keeping maintenance, replacement and other up keep costs down and is also able to
withstand high stresses. Welded steel has a high strength resistance and an excellent resistance to
thermal shock and also high fire resistance with no toxic fume emissivity. Welded steel does not
fade. Its visual appearance stays fresh, and it’s physical durability. It is also able to withstand
high design stress.

5.5 Designing the crusher volume

Density =

Volume =

Assuming that the density of the raw material inside the crusher will remain the same during the
process

Mass of raw materials = 5274,73kg and the density of tobacco waste at 250C is 750kg/m3

Volume =
53 | P a g e
 = 7,03m3

Hence in cooperating a safety factor of 5%

Volume = 7.0m3

5.6 Designing of crusher diameter and height

The crusher is cylindrical in shape

Volume = ×h

But D = 0,5h

(
Volume = ×h

(
7,03m3 = ×h

28,12m3 = ( ×h

28,12m3 = 0,785 × h3

h = 3,30m

since D = 0,5 h

D = 0,5(3,30)m

D = 1,65m

5.7 Cross sectional area of the crusher

Cross sectional area =

= × 1,65m

= 5,18m2

5.8 Design of Hammer / Blow bars

The hammers or the blow bars are subject to shear force at the point of fixation, centrifugal force
due to rotation, bending force due to striking of the material.
54 | P a g e
When a sudden impact is observed by the blow bars due to input feed striking over , it
experiences an impact load. The effect of impact loads differs appreciably from that of the static
loads as with a suddenly applied load, both the magnitude of the stresses produced and resistance
properties of materials are affected.

Hammers or blow bars can be made using different sections like, I section, T section, S section,
cylindrical bars, rectangular bars etc. The shape of the hammers decides the impacting capacity
as well as the strength of the crusher. Hammers are mounted of the rotor plates or rotor drum
using lock pin mechanism.

Let us consider a hammer or the blow bar made of Manganese steel and having a rectangular
cross section.

Length of bar = 1500 mm

Width of bar = 400 mm

Thickness of bar = 114 mm

Material = Manganese steel

Density ρ = 7.8 g/c

Young’s Modulus E= 165

GPa = 165 X 103 N/m

Yield Stress σys = 350 MPa = 350 N/mm2

Height of fall of material h= 36 inch = 914.4 mm

Wt. of each hammer/ blow bar = 477 Kg

The hammer is considered to act like a cantilevered beam with 1/3 of its width inserted in to
rotor plate slots for the fixation purpose.

5.9 Impact Bending Stress (Static)

a) When the cantilever is subjected to a concentrated load at the mid of its span.

55 | P a g e
Figure 5:1: Bending stress diagram

Total open screen area per hammer

= 67% of area of the hammer plate

= (67 X 1500 X 400)\100 = 4.02 X

Now from a feed rate of 350 ton/hr and a revolution of 480 revs/min of the rotor we have 8
impacts by 4 rotors in one second. i.e. 1 rotor has 2 impacts.

So Tonnage/impact W = = 119,21 N

Let y be the bending

Applying impact equation we get:

W( h + y) = Py/2 Where P is the equivalent static force

Also for a cantilevered beam subjected to a load the deflection is given as

y=P Where I is the moment of inertia

therefore P=

119,21 (914,4 + y) =

56 | P a g e
 Here I = = 1500 = 1,85 ×

Therefore EI = 3.05 × Nm

So we get

119,21 (914,4 + y) =

y = 2,8mm (deflection)

therefore P= = = 75911,11 N

so Max Moment, = 75911,11 × = 1,518 × Nmm

now we have allowable stress

σys = 500 MPa = 500 N/m

So max allowable moment

= σys Xz = σ × = 500 × 1500 × 114 × 114 × = 1,625 × Nmm

Since ……….. The design is safe for this condition

b) When the cantilever blow bar is subjected to a concentrated load at the tip of the
cantilever.

We have

W( h + y) = Py/2

Therefore 119,21 × (914,4 + y) = Py/2

Where P=

Therefore W × (h + y) =

57 | P a g e
Figure 5:2: Bending stress diagram with the load at the tip of cantilever

Therefore 119,21 × (914,4 + y) =

y = 2,8 mm (deflection)

therefore P= = = 75911,11 N

Max. Moment = P × l = 3,036 × Nmm

Max. Allowable = = σZ = 1.625 X N mm

Since hence the design is safe

5.10 Static Load Shearing

By using strain energy method and approximating the loading to be a static one, Shear stress
produced due to force F at any distance y is:

ӷ= = ( ( + )

ӷ= ( - )

Shear strain energy for the small volume

dv = (volume)

58 | P a g e
 = [ ( - ) ×(bdy) × (dx)

⁄
So the total strain energy = ∫ ∫

⁄
= ∫ ∫ ( × (bdy) × (dx)

⁄
= ( b×∫ + - dx =

Work Done W = F × where = displacement

So we get

Here P = 119,21N; G = bulk modulus = 80GPa = 80 × N/mm2

So ys =

= 0,0000031mmm

5.11 Design of V-Belt Drive

A V- belt drive mechanism drives the rotor. Power to be transmitted = 450 Hp = 335 KW
(calculated from the crushing requirement and its drive power required)

59 | P a g e
Figure 5:3: Cross section of V-grooved pulley (R. S. Khurmi and Gupta. A text book of
machine design. 2005. p. 728)

So according to the V belt standards [Khurmi R S, Gupta, V-belt and rope drives, A text book of
machine design, 2005]

Minimum pitch dia. D of pulley = 500 mm

Pulley dia. at sheave d2 = 300 mm

Top width of v belt, b = 38 mm

Thickness of v - belt, t = 23 mm

2β = 36º (assumed)

For pulley

w = 32 mm ; d = 33 mm ; a=9.6 mm

c=23.4 mm ; f= 29 mm ; e=44.5 mm ; No. of sheave grooves (n) = 20

N2 = 480 rpm

For belt

2
Coeff. Of friction = µ = 0.25 (leather); = 7N/mm

ρ = 1.2 X 103 Kg/m2

N1 = 1000rpm

N1/N2 = d2/d1

So d1 = 144 mm

Let the overhang be, x= 1000 mm

So we have

sin α = (r2-r1)/x ‫ ؞‬α = 22.9º

60 | P a g e
Angle of lap on the driving pulley Θ =180º-2α = 134.2º = 2.34 rad

Mass of belt per length = area X density = 0.841 Kg/m

Velocity of belt V = = 37,6 m/sec

Centrifugal tension Tc= mv2 = 1193.88 N

Max tension in the belt T= σ X a =7 X 701.5 = 4910.5 N

Tension on the tight side = T2 = T – Tc = 3716.6 N

Also we know that: 2,3 log

=> T2 = 561.6 N

5.12 Design Of Rotor Shaft (Static Conditions)

Material of Shaft = Cast Iron

Density of Cast Iron, ρ = 8000 Kg/m3

Shaft diameter, d = 300 mm

1500

400 400

Figure 5:4: Free body diagram of rotor shaft

Weights on rotor shafts

Weight of rotor plates = 12600 Kg

Weight of Rotor hammers = 4 X 477 Kg

Volume of shaft = π/4 d2 I = π/4 X 3002 X 2300 mm3 = 0.000162 m3

61 | P a g e
So self-weight of rotor shaft = volume X density = 1300 Kg

Now in for the two shaft mounting points A and B… the reaction forces have the relation

RA + RB = {1300 + 12600 + (4 × 477)} × 9,8

As ΣMb = 0…. So

RA × 2300 – {1300 × 2300/2 ×9,81} – {9,672 × 1500 × 2300/2 × 9,81} = 0

 RA = 77538.25N
 RB = 77538.25N

We can see that, since it is a completely symmetric figure. The bending moment will be max at
the center of the shaft.

Hence max. Bending moment

( (
= × -

= 82,782 Nmm

Now allowable bending moment M = σZ =σπ /32 = = 450,4 × Nmm

Hence we can see that the design is safe.

Now considering the bending moment due to tension on both sides of belt we get

T1+T2 = 4278 = R1 + R2

also Ra X 2300 = 4278 X (2300/2)

Ra = 2136 N
Rb = 2136 N

62 | P a g e
 T1 + T2

2300mm

Ra Rb

Figure 5:5: Bending moment diagram

Max Moment = Ra X l/2 = 2456400 N mm

M=√

=√

= 82,81 × 106 Nmm

Now turning moment acting T = p/ω = 53.34 X 106 N mm

Thus equivalent Me =0.5(M+(M2+T2)0,5 ) = 90.7 X 106 N mm

And equivalent Te = (M2+ T2)0,5 = 98.58 X 106 N mm

So stress induced = τs = Te/Z = 37.21 N/mm2

Hence the design is safe when compared to the ultimate stress. With FOS = 276Mpa / 37.21Mpa
= 7.4

5.13 Design of Grinding Screen

These screens are fitted below such that they help in segregating the output material according to
their sizes and channel the outflow of the required size particles. Once the particles are on the
Screen there are two process that occurs on it

Stratification: - here the large sized particles rise to the top of the vibrating material bed due to
the vibrating motion effect.
63 | P a g e
Factors that affect the stratification are material travel flow, bed thickness, screen slope, stroke
characteristics like amplitude, frequency, rotation etc. and also the surface moisture.

Figure 5:6: Grinding screen process

The vibrating motion is generally produced by the vibrating mechanism based on eccentric
masses with amplitude of 1.5 to 5mm and operation in range of 800 to 900 rpm.

It should have proper amplitude and frequency so that the material while travelling on the screen
neither falls on the same opening nor jump over many subsequent openings.

So if we have larger openings we require higher amplitude and lower speed. But in case of
smaller openings we require lower amplitude and higher speed.

The screens can be horizontal as well as inclined. In horizontal screen the motion/vibration
should be capable of conveying the material without the need of gravity. So a straight line
motion / vibration at an angle of 45º to the horizontal can produce lifting component for the
stratification and conveying.

Low screening efficiency leads to over load of the closed crushing circuit as well as it may lead
to products that are non-compliment with specification.

It was also studied that the efficiency of screen depends on the feed on the screen. As in the
earlier lower feed the efficiency increases with increase in feed but later on the efficiency
decreases with further increase in the feed rate. The mesh openings should always be slightly
larger than the specified separation size.

64 | P a g e
For our assumed input feed for the screen, feed rate = 350 tph

Solid density = 1.6 t/m3

Max feed size = 100 mm

Moisture content = 3%

Particle shape = flaky; Screening process = dry

Desired products = larger than 1,50 mm (that are circulated back to crusher input) ; and below
1,50 mm and 1,00 mm.

Screen selection

85% of the passing material in collected in the first deck of the screen. Since the passing
percentage for the deck is very high we use multislope screen. The flaky material shape leads to
the choice of square opening screen.

We assume the use of steel screening mesh

Dimensioning

At the first deck particles with size greater than 50 mm should be retained and the rest should be
passed to the conveyor.

To obtain 1,5 mm separation the square opening screen must be 3 mm and with an opening of
73% [Jarmo Eloranta, Crushing and Screening Handbook, Kirjapaino Hermes, Tampere, sept
2006, sc 4-1. p. 4-15]

65 | P a g e
Figure 5:7: Flow chart of material on screen

Area = (Qfeed X P)/Qdeck

Qfeed=350 X 0.75 = 298 TPH

Qdeck = A X B X C X D X E X F X G X H X I X J X K X L

Where A= capacity factor =75

B= retained material factor for 15% oversized = 1.45

C= Half size factor =1

D=1 ; E=1 ( dry screening) ; F=0.6; H=1 ; J= 1; K=1.3; L=1, I=0.9

G= 1.46

(Jarmo Eloranta, Table for D,E,F,H,I,K,L, Crushing and Screening Handbook, Kirjapaino
Hermes, Tampere, sept 2006, sc 4-11, 4-14)

So Area = 262/111.46

= 2.35 m2

Layer thickness D =

66 | P a g e
Where feed = transported capacity ;

S= material travel speed

W= screen width (m) ;

Bd = material bulk dist.

Optimal speed s= 30 -35 m/min

Optimal Layer thickness, D= 83-120-163 mm

Casing

The crusher case can be made up of welded steel construction and built in three or more sections.
The lower half is made up of one piece and upper half is made up of two sections. The feed
intake section is in the upper half and is bolted to the lower half resulting in a lasting dust type
connection between the feed and crusher intake.

The rest of the top section is hinged for access to interior of the crusher for changing hammers,
hammer pins and screens. All the mating surfaces are built-up for an accurate, dust tight fit.
Single latch door is provided for easy maintenance and cleaning and a Gasket door is provided
for dust tight operation. The casing of the crusher does not experiences and larger forces but still
they should be able to bear abrasive forces acting on it. The impact bars are attached to the
casing through a mechanism which may help in changing the angle of impact on the bar , by
moving or tilting the bar.

5.14 Summary of Final Design Parameters

Density of tobacco/ particle ρ = 1600 Kg/m3

Input feed rate = 350 TPH

Top feed size = 70 mm

Max speed of rotor rotation N= 480 rpm

Power req. from motor = 450 HP

End size of particle = 1,5 mm

67 | P a g e
Dia. of rotor = 1500 mm

Width of rotor plate assembly = 1500 mm

No of rotors (plates) used = 9

Rotor material = Manganese steel

Hammer dimension = 1500 X 114 X 400 (mm)

Hammer material = Manganese steel

Density of Manganese steel used = 7.7 g/cu. cm

Weight of rotor plates (total) = 4850 Kg

Weight of hammer (each) = 477kg

Shaft Dia. for rotor = 300 mm

Young’s modulus of elasticity for manganese steel E = 165 X103 N/mm2

Yield stress σys = 350 N/mm2

Height of fall of material = 36” = 914.4 mm

Total area of hammer/ bar exposed for impact = 67 % of area of Bar surface area

Tonnage/ impact on bars = 119.21 N

Material for rotor shaft = Cast Iron

Diameter of Fly wheel / pulley at end of rotor = 1500 mm

Over hang between the driving and drive pulley = 1000mm

Number of Belts = 2

Pitch length of V- belt = 5.64 m

Dia. of Motor shaft pulley = 144mm

Hole size in square mesh of screen = 75 mm

68 | P a g e
Grinding screen area = 2.5 m2

5.15 Proposed Designs

Figure 5:8: proposed design of rotor plate

Figure 5:9: Proposed design of a hammer

69 | P a g e
Figure 5:10: Proposed design of rotor assembly with rotor disc, hammers, shaft and
locking pin

Figure 5:11: proposed design of crusher assembly with rotor, flywheel, impacts bars and
casing (side view)

70 | P a g e
References
1) NEI. R. I and STUBBINGS, W. A. K. Coding Moth control in the western province.
Farming in Zimbabwe, Vol 14, 1999, p. 366-9.
2) WARD, G. M. Nicotine - A Product of Tobacco. Technical Bulletin 33, Dominion of
Canada, Department of Agriculture (1941), p. 17.
3) Shepard. H. The Chemistry and Toxicology of insecticides, 2005, p. 213-264
4) Holman, H. J. A Survey of Insecticide Materials of Vegetable Origin, 2007, p. 42-58.
5) Henry, T. A. The Plant Alkaloids 3rd Edition. Alkaloids of Nicotiana, 1995 p. 42-58.
6) PICTET, A, and Rotschy, A. Berichte, 1991, p. 696.
7) Csoke, B., Racz j., 1998. Estimation of the breakage and selection functions for
comminution in hammer mill. In: Proceedings of the 9th European Symposium on
Comminution, ALbi, France, 1. Pp. 393-401.
8) 12. [King, R.P. (2000), continuing education course on simulation and modeling of
mineral processing plants, Univ. of Utah course, Tech. notes 5, Crushers, pp.5]
9) 13. Jarmo Eloranta, Chart B, Crushing and Screening Handbook, Kirjapaino hermes,
Tampere, sept 2006, sc 4-11, 4-12
10) 14. Jarmo Eloranta, Chart C Crushing and Screening Handbook, Kirjapaino hermes,
Tampere, sept 2006, sc 4-13, 4-14
11) Herbet, R. (2001) What is new in nicotine & tobacco reservoir: Nicotine tobacco. Addis
Ababa: Ethiopian Institute of Agricultural Research
12) Hawkins, B. etal (2002) Smoking and inschemic stock: a role for nicotine, Newdeli:
Gilberts.
13) Lyon, H. (2007). International Agency for Research on cancer IAAC Monographs on the
evaluations of caranogenic risk to humans,Washington: McGraHill.
14) Demirbas, E. and Nas, M. (2009). Batch kinetic and equilibrium studies of , Newdeli:
Gilberts.
15) Hailu, W. and Kassa, W. (1979) Handbook of cultural practice for flue-cured Tobacco;
london: Pan book.
16) Wikipedia, the free on line Encyclopedia, URL:http://en.wikipedia.org/wiki/Nicotine,
accessed on March 12, 2014.
17) Gebre, S. and Selassie, A. (1996) Rapid assessment of drug abuse in Ethiopia; London:
Chatto and Windus.

71 | P a g e
 18) Brockley, M. (2004) Tobacco, TED Case Studies an Online Journal, .
19) Vernellia, R. and Randall, T. (1999). History of Tobacco, Boston: Boston University.
20) Beyeh, M. and Abuhay, T. (2006.) tobacco production in Ethiopia and the constraints it
has been facing.Addis Ababa: Ethiopian Institute of Agricultural Research

72 | P a g e