ffect of temperature on the characteristics of bio-oil produced from Mallee biomass fast pyrolysis in a twin auger pyrolyser

Effect of temperature on the characteristics of bio-oil produced from Mallee biomass
fast pyrolysis in a twin auger pyrolyser

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To the best of my knowledge and belief, this report contains no material previously published
by any other person except where due acknowledgement has been made. This report contains
no material which has been accepted for the award of any other degree or diploma in any
university.
Signature :
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Table of Contents
List%of%Tables%.....................................................................................................................%4!
List%of%Figures%....................................................................................................................%4!
1.0%Introduction%................................................................................................................%5!
1.1%Background%..........................................................................................................................%5!
1.2%Objective%..............................................................................................................................%5!
1.3%Significants%...........................................................................................................................%6!
2.0%Literature%Review%........................................................................................................%7!
2.1%Background%..........................................................................................................................%7!
2.2%Pyrolysis%...............................................................................................................................%8!
2.3%Fast%pyrolysis%........................................................................................................................%9!
2.4%Mechanisms%of%Biomass%.....................................................................................................%10!
2.5%Effects%of%Pyrolysis%Temperature%
.........................................................................................%12!
2.5.1 Composition of Bio-oil!.......................................................................................................!13!
2.5.2 Effect of Residence times!...................................................................................................!15!
2.5.3 Physical Properties and Characteristics of Bio-Oil!.............................................................!15!
2.6%Fast%Pyrolysis%Reactors%.......................................................................................................%16!
2.6.1 The Auger Reactor!
..............................................................................................................!17!
3.0%Methodology%.............................................................................................................%18!
3.1%Biomass%preparation%
...........................................................................................................%18!
3.2%Cutting%Mill%.........................................................................................................................%18!
3.3%Size%separator%.....................................................................................................................%19!
3.4%Pyrolysis%process%................................................................................................................%19!
4.0%Discussion%
..................................................................................................................%20!
5.0%Research%Conclusion%..................................................................................................%21!
6.0%References%.................................................................................................................%22!
7.0%Appendices%................................................................................................................%24!
SCOPE%OF%WORK%FORM%............................................................................................................%24!
RISK%ASSESSMENT%FORM%
..........................................................................................................%31!
Chemical%Risk%Assessment%...............................................................................................%38!

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List of Tables
Table 1: Resulting product yield at different pyrolysis conditions..........................................10
Table 2: Component composition within pyrolysis liquid.......................................................13
Table 3: Physical properties of raw pyrolysis liquid product ..................................................14
Table 4: Physical properties and characteristics of Bio-oil .....................................................16
List of Figures
Figure 1: Percent Yield of bio liquid, char or gas at various pyrolysis techniques ...................7
Figure 2: Phase change of wood biomass at various temperatures............................................8
Figure 3. Biomass fast pyrolysis process schematic..................................................................9
Figure 4: The mass loss rate of the main biomass compounds at increasing temperature ......11
Figure 5: The resulting phases formed during the pyrolysis reaction......................................12
Figure 6: Yield of components through changing reaction temperature .................................12
Figure 7: Basic diagram of a single screw auger reactor.........................................................17
Figure 8: Cutting mill used to grind the Mallee wood.............................................................18
Figure 9: Retsch Vibratory Sieve shaker used to sift through the wood .................................19
Figure 10: Schematic diagram of auger reactor system for pyrolysis .....................................26
Figure 11: Schematic diagram of biomass feeding section of the auger reactor .....................27
Figure 12: Schematic diagram of heat carrier section of the auger reactor .............................28
Figure 13: Schematic diagram of auger reaction section of the auger reactor.........................29
Figure 14: Schematic diagram of product recovery section of the auger reactor ....................30

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1.0 Introduction
1.1 Background
Utilising renewable transportation fuels can significantly reduce our dependence on fossil
fuels resulting in green house gas emissions. Biomass is both inexpensive and almost
abundantly available around the world thus offering a potential option for producing energy
(Patwardhan 2010). Biomass resource can include agricultural crop residues, wood residue
from forests and milling industries as well as municipal solid waste (MSW) from urban areas.
Sunlight and CO2 is absorbed by the plant and converted into chemical energy through
photosynthesis making biomass an indirect form of solar energy and renewable carbon
source. The chemical energy stored in biomass can then be converted into bioenergy such as
heat and electricity as well as liquid biofuels, bio chemicals and many other bio-based
products (Brown 2009). The potential uses of bio oil mimics that of conventional fossil fuels,
it can be used as a renewable industrial fuel generating heat and electrical power as well as
the potential to be upgraded to transportation fuels and special chemicals. Both the char and
gasses can also be used as a fuel in the form of heat to dry the incoming biomass feedstock
and the heat carrier feed shot (Easterly 2002).
1.2 Objective
Considerable attention has been given to pyrolysis process of biomass because of an
opportunity for the processing of agricultural residues, wood wastes and municipal solid
waste into clean energy. This project investigates the effect of steel shot feed temperature on
the characteristics of bio-oil produced from fast pyrolysis of Mallee wood biomass in a twin
screw auger reactor. The operation conditions of the auger reactor will be kept constant such
as nitrogen flow rate, screw speed, biomass feed flow rate, heat carrier flow rate and
condenser conditions. The staged condensation temperature will be optimised to maximize
the bio-oil yield at different temperatures. The reaction temperature is critical for fast
pyrolysis and has effects on the product yield and qualities. Both the heat transfer rate and
reaction temperature are important as rapid heating to a reaction temperature that is too low
or high will affect the desired product compositions.

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1.3 Significants
The fast pyrolysis of biomass has the potential to contribute to the world’s need for liquid
fuels and, ultimately, for chemicals production. Crude oil is non-renewable, and the
accelerated rate of growth of energy consumption in Asia, China and India, raises this
incentive for all countries to continue research into the mass production of bio-oil from
biomass. In addition, the burning of fossil fuels producing carbon dioxide continues to have
serious environmental consequences. Significant changes will occur when, and if, either the
economic incentive arises or climate change regulations push Australia and the world in this
direction. Thankfully our chemical and engineering knowledge is now far more advanced,
making any technical advances occur more rapidly when economics dictates a change.

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2.0 Literature Review
2.1 Background
Biomass energy is a clean renewable energy that has gained significant momentum as the
worlds crude oil reservoirs deplete. The majority of biomass energy is created from wood,
municipal solid waste, agricultural waste and landfill gasses making biomass energy an
abundant resource (Demirbas 2007). Through photosynthesis, plants absorb sunlight and CO2
into stored chemical energy. The potential chemical energy stored can be converted into
electricity (heat), liquid fuel for transportation, speciality chemicals and other bio-based
chemicals. There are various biomass conversion pathways in different stages of
development. The pathways for these stages can be grouped into two major technology
platforms called biochemical and thermochemical (Brown 2009). This project will only focus
on the production of bio-oil through thermochemical pathways.
Thermochemical conversion processes offer promising methods for converting biomass to
gasoline combatable liquid bio-oil. Thermal conversion processes are more suited for the
conversion of wood and crop residues accounting for around 96% of the worlds biomass
(Stevens 1987). Thermochemical conversion techniques which include liquefaction,
pyrolysis, gasification and combustion all utilise heat energy to decompose biomass (Brown
2009). These process can convert around 85 to 95% of the organic feedstock material with
little sensitivity to the feed type material (Stevens 1987). Figure 1 below shows the
difference in product yield of the pyrolysis of wood by utilising reactor temperatures and
residence time to dictate the end product composition of pyrolysis liquid, char or gas.
Figure 1: Percent Yield of bio liquid, char or gas at various pyrolysis techniques

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2.2 Pyrolysis
Pyrolysis is a thermochemical change in organic matter in an enclosed heated environment
usually in an oxygen low or depleted environment (Demirbas 2007). This process has
traditionally been used to produce charcoal however, depending on the environment
conditions pyrolysis typically produces one third liquid, gas and solid bio-char. The pyrolysis
process is inefficient mainly due to the large quantities of low value liquids and gasses
formed as well as undesired solid char products (Stevens 1987). Thermochemical conversion
of biomass using either catalytic, non-catalytic pyrolysis and gasification aims at maximising
the production of valuable gaseous and liquid fuels (Demirbas 2007). Upon heating, any
moisture present is first driven off the material, once dried the pyrolysis reaction begins
before any remaining thermal processing occurs. Pyrolysis can occur over a range of
temperatures from 400 ºC to 600 ºC at atmospheric pressure. Fast pyrolysis involves rapid
high heating, short vapour times (seconds) and rapid cooling which favours the maximum
formation of liquids. Slow pyrolysis also know as conventional pyrolysis involves slower
heating rates and longer vapour residence times (minutes) yielding higher amount of solid
char bio material. Slow pyrolysis is typically used as a carbonising process for converting
wood to charcoal and yielding small amount of bio-oil and hydrocarbon gases (Brown 2009).
The possible reaction pathways for the pyrolysis of wood biomass include three lumped
product categories, starting with a first order reaction. At the beginning of the pyrolysis (250
°C–300 °C) process, most of the volatiles are released at a rate 10 times faster than the next
step. Relative proportions of the end products after pyrolysis of biomass at a range of
temperatures are shown in Figure 2.
Figure 2: Phase change of wood biomass at various temperatures

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2.3 Fast pyrolysis
Fast pyrolysis involves the reaction of biomass at atmospheric pressure and in an oxygen free
environment, the biomass is rapidly heated to a temperature of around 500 °C causing it to
decompose and convert to fractions of liquid bio-oil, solid bio char and non condensable
gasses within seconds. Around 60 to 80% of the starting mass of the bio material can be
condensed to liquid bio-oil, with the balance formed by approximated equal portions of bio
char and gasses (Brown 2009). The condensation of pyrolysis vapour and gasses yields a dark
brown liquid with a smoky odour considered as bio oil. The non-condensable fraction of
pyrolysis vapours consists of carbon monoxide, carbon dioxide, methane and hydrogen
vapours. Solid charcoal residue also forms through the pyrolysis process. The relative
portions of the solid, liquid and gas fractions are varied significantly by the process
conditions (Patwardhan 2010). The basic thermal process is shown in Figure 3 below, note
the energy input in the form of heat required to carry out the endothermic fast pyrolysis
reactions.
Figure 3. Biomass fast pyrolysis process schematic
Depending on the operating condition, pyrolysis can be classified into three main categories’;
conventional (slow), fast and plash pyrolysis. These differ in process temperatures, heat rates,
residence time, biomass particle size, type of feedstock etc. (Murray 2014). However, relative
distribution of products is dependent on pyrolysis type and pyrolysis operating parameters as
shown in Table 1. In addition, different types of pyrolysis processes are described in the
following three sub-sections.

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Table 1: Resulting product yield at different pyrolysis conditions
Liquid products from biomass fast pyrolysis are frequently termed bio-oil. However, this is a
somewhat a confusing terminology as the organic liquid product is generally hydrophilic
containing many oxygenated compounds and is present as a single aqueous phase making
some researchers prefer not to refer to it as oil and rather “pyrolysis liquid” (Brownsort
2009).
The reaction temperature is critical for fast pyrolysis and has effects on the product yield and
qualities. Higher char called bio-char occurs at temperatures less than 425°C, and non-
condensable gas production increases for temperatures above 600°C. Both the heat transfer
rate and reaction temperature are both important as rapid heating to a reaction temperature
that is too low or high will affect the product compositions (Brown 2009). as will a slow
heating rate to the optimal reaction temperature. The reaction pressure for fast pyrolysis is
typically near atmospheric, as higher pressures favour the formation of bio-char (Demirbas
2007).
2.4 Mechanisms of Biomass
Biomass is a complex organic-inorganic solid material produced by techno-genic and natural
processes. Biomass composes of polymers that have extensive chains of carbon atoms linked
into macromolecules (Abdullah 2010). Its major mechanism involves a mixture of
hemicellulose, cellulose, lignin and minor amounts of other organics compounds such as
lipids, proteins, water, simple sugars and inorganic species which each pyrolysis or degrade
at different rates, pathways and mechanisms (Bridgwater, Meier and Radlein 2016). If the
wood completely pyrolysed, hemicellulose compound is the first to decompose at around 470
to 530 K followed by cellulose decomposing at 510 to 620 K. Lignin is the last component to
pyrolyse at temperatures around 550 to 620 K (Demirbas 2007).

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For typical wood source biomass, the composition percentage of lignin (25 – 30%), cellulose
(35- 50%) and hemicellulose (20-30%) (Jahirul et al. 2012). Factors that influence biomass
pyrolysis characteristics include temperature, particle size, heating rate, feed rate, and
biomass composition (Yang and Wu 2014). Figure 3 shows the overlap in mass lost of
hemicellulose, cellulose and lignin.
Figure 4: The mass loss rate of the main biomass compounds at increasing temperature
The pyrolysis temperature is a critical factor affecting the yield and quality of bio-oil. The
temperature at which maximum yield of bio-oil is obtained coincides with the temperature at
which maximum yields of lignin-derived oligomers are produced (Zhou et al. 2013). The
pyrolysis of biomass with a high percentage of lignin can produce increase bio-oil yields
(Figure 5). This is because of the different physio-chemical characteristics of cellulose,
hemicellulose and lignin (Jahirul et al. 2012). The degree of secondary reaction and hence the
product yields of gas products is largely dependent on the time temperature during the
reaction to which they are subjected before collection. The separation and recovery of pure
forms of lignin and hemicellulose are difficult due to structural changes in their processing,
although pure cellulose is relatively easy to produce (Bridgwater, Meier and Radlein 2016).

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Figure 5: The resulting phases formed during the pyrolysis reaction
2.5 Effects of Pyrolysis Temperature
Biomass heating or heat transfer in pyrolysis reactors is one of the important aspects of the
process. These heat transfers could be either gas-solid where heat is transferred from the hot
gas to the pyrolysis biomass particles through convection, and solid-solid where conductive
heat transfer occurs between feed media balls (shot) and biomass feed. Along with
convection and conduction, some radiation heat transfer also occurs in all types of reactor
(Jahirul et al. 2012). Various temperatures for biomass pyrolysis will affect the rate of mass
loss as seen in Figure 6 below.
Figure 6: Yield of components through changing reaction temperature

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Yang and Wu studied on the biomass fast pyrolysis characteristics and products and
suggested that a temperature between 700 and 800 K (approximately 430 to 530 ºC) for
biomass fast pyrolysis maximizes the bio-oil yield. Temperatures above this range initiate a
volatile secondary reaction that decreases the rate of bio-oil production (Yang and Wu 2014).
2.5.1 Composition of Bio-oil
The product bio-oil contains a complex mixture of over 300 organic compounds formed
during the pyrolysis process. The compounds are essentially trapped in a liquid from and it is
often noted that the elemental bio-oil composition is very similar to that of the original
feedstock but in a much more convenient liquid state (Shanks and Czernik 2005). Bio-oil
contains a significant amount of oxygen which originates from the feedstock and water which
is a result from condensing any moisture contained in the feedstock as well as moisture
occurring during the reaction. Bio-oil has a lower heating value than petroleum based fuel-
oils, often reported around 40% – 50% less mainly due to the large amounts of water and
oxygen within the liquid (Brown 2009). Bridgewater identified the chemical composition of
bio-oil is dependent on many factors, and includes many classes of oxygenated species.
Bridgwater et al. describe the major chemical constituents of bio-oil as aldehydes (15 wt%),
carboxylic acids (12 wt%), carbohydrates (8 wt%), phenols (3 wt%), furfurals (2 wt%),
alcohols (3 wt%) and ketones (3 wt%) (Bridgwater, Meier and Radlein 2016). Various other
chemical compounds include hydroxyketones, hydroxyaldehydes, dehydrogugars, sugars and
phenolic compounds.
Another major constituent of bio-oil (15 wt% – 30 wt%) is a water-insoluble fraction
originated from the lignin portion of the biomass, often referred to as “pyrolytic lignin”.
Some of the interesting properties of bio-oil are based on the pyrolytic lignin fraction, as are
the processing challenges and opportunities associated with bio-oil. Typical characteristics of
fast pyrolysis liquid product can be seen in Table 2 and 3 below.
Table 2: Component composition within pyrolysis liquid

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Table 3: Physical properties of raw pyrolysis liquid product
The composition can vary considerably according to the feed material and its characteristics,
the pyrolysis process parameters and the liquid collection parameters of which temperature of
liquid collection system and method of collection are particularly important. Bridgewater also
identified that liquid yields decrease at high temperatures and/or long residence times. The
liquid also becomes increasingly deoxygenated and at very high temperatures (Bridgwater,
Meier and Radlein 2016).
The gaseous products from fast pyrolysis is referred to non-condensable gas (NCG). The non-
condensable gas fraction from fast pyrolysis is a combustible mixture, containing various
species including large amounts of carbon dioxide (CO2) carbon monoxide (CO) and with
lesser amounts of hydrogen (H2), methane (CH4), ethylene (C2H4), ethane (C2H6), propane
(C3H8), and other light hydrocarbons (Brown 2009). The non-condensable gas stream will
also contain any un-reactive gases that were used in the process for fluidisation, such as
nitrogen. As with bio-oil and biochar, the non-condensable gas yield and composition is
dependent on many factors including the process conditions and feedstock (Jahirul et al.
2012). The non-condensable gas yield is in the range of 10 wt% to approximately 20 wt%,
and commonly has a yield similar to that of biochar in the fast pyrolysis reaction (Guo and Bi
2015).
The solid product from the reaction is a powdery black substance known as biochar, or
charcoal. Biochar yields from fast pyrolysis range from approximately 10 wt% to around 25
wt% being common values for fast pyrolysis of wood biomass. Elementally, bio char is
composed mostly of carbon (approximately 60 %) with smaller amounts of hydrogen,
oxygen, sulphur and nitrogen depending on the biomass composition (Brown 2009).

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2.5.2 Effect of Residence times
The residence time of a any reactor is a probability distribution function that describes the
time a particle spent inside the reactor (Verclyte 2013). Liquid production of Bio-oil requires
very low vapour residence time mainly to minimise any secondary reactions occurring
reducing the yield of liquid. Typical residence time in a reactor is around 1second, however
yields can also be obtained at residence times up to 5 seconds if the vapour temperature is
kept below 400°C (Bridgwater, Meier and Radlein 2016). Residence time too short will result
in incomplete de-polymerisation of the lignin due to random bond cleavage and inter-reaction
of the lignin macromolecule resulting in a less homogenous liquid product, while longer
residence times can cause secondary cracking of the primary products, reducing yield and
adversely effecting bio-oil properties (Yang and Wu 2014).
2.5.3 Physical Properties and Characteristics of Bio-Oil
The general characteristics of bio-oil is a dark brown, free-flowing organic liquid that is
highly oxygenated and typically containing 15 to 30% water. Although it is called oil, it does
not readily mix with petroleum products. Bio-oil is acidic with a pH range from 2 to 4
(Dobele and Urbanovich 2007). The oil which contains hundreds of different organic
chemical compounds including acetic acid, methanol, aldehydes, ketones, alkyl- phenols,
alkyl-methoxy-phenols, sugars, and lignin-derived compounds. Low levels of nitrogen and
sulphur containing compounds are sometimes found in bio-oil, but give off little sulphur and
nitrogen pollutants when burned (Murray 2014). The physical properties of bio-oil can be
focused the products density, pH, Viscosity, moisture, heating value and elemental analysis.
Oxygen is present and together with water the overall oxygen content is around 35-40% of
the bio-oil. Bio-oil has a range of volatility’s as well as having a wide viscosity range of
between 35 - 1000 cP at 40 ºC. Phase separation of the oil will occur over time and the
corrosiveness can be relatively high due to the presence of organic acids (Patwardhan 2010).
However, the pyrolysis of bio-oils does have limitations particularly in fuel quality, stability,
phase separation, fouling issues on thermal processing and economic viability (Brownsort
2009). Some physical properties and characteristics of bio-oil are described in Table 4 below.

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Table 4: Physical properties and characteristics of Bio-oil
2.6 Fast Pyrolysis Reactors
Continual research over the years has led to the development of different reactor
configuration for the purpose of fast pyrolysis. Various reactors include fluidised bed reactor,
the circulating fluid bed reactor, Auger, rotating cone and vacuum reactor. Each of these
reactors possesses its inherent advantages in the area of heat supply, heat transfer, feed
preparation and operation complexity (Mohan, Pittman and Steele 2006). However, some
these attributes result in disadvantages of limited heat transfer to the reactor and some surface
area controlled systems moving parts at high temperatures (Bridgwater, Meier and Radlein
2016). The fluidizing bed and circulating fluid bed makes use of a mix of convection and
conduction heat to transfer heat from source to the biomass. The heat transfer limitation here
is the wood particle itself thus these reactors have the limitations of requiring very small
particle size less than 3mm to produce good oil yields. Also they require inert gas for
fluidisation and transport (Vigouroux 2001). Finally, the vacuum pyrolysis reactor where the
pyrolysis occurs under reduced pressure and slow heating rates has the advantage of also
using larger particle size. However, its limited by its higher equipment cost and low oil yields
(Mohan, Pittman and Steele 2006).

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2.6.1 The Auger Reactor
In an auger reactor, heat transfer medium is mixed with the feedstock, in comparison to other
pyrolysis reactors that have heated walls that induce the pyrolysis reactions. They involve the
mechanical mixing of biomass and a bulk solid heat transfer medium in an oxygen deficient
reactor environment (Jahirul et al. 2012). Mixing devices within the reactor vessel rotate
while the reaction vessel remains stationary. The biomass and heat carrier are independently
metered into the reactor, the heat carrier such as sand, silicon carbide, alumina ceramic, steel
shot media is pre heated before entering the reactor (Brown 2009). Figure 7 below is a typical
single screw auger reactor, as the biomass feed reacts in the tube, the difference in vapour
pressures flow through the series of vapour outlet collectors while the solid bio-char materials
and heat carrier exit the end of the reactor.
thermocouple
solid.canister
Pressure
Gauge
vapor.outlet heat.carrier
biomass
Feed.motor
with.controller
Nitrogen
Gas.Rotometer.4
Nitrogen
Gas.Rotometer.3
Figure 7: Basic diagram of a single screw auger reactor
The biomass feeding section consists of an airtight hopper with a pore through the lid tubed
with purge gas, the flow of which is controlled by a nitrogen fed gas roto-meter. Nitrogen
flow was used to keep the inert and remove volatile products from the reactor (Zheng et al.
2012). Biomass drying is important to avoid adverse effects of water on stability, viscosity,
pH, corrosiveness and other liquid properties in the pyrolysis product. By cutting and
grinding the biomass to a particle size between 250 to 500 microns and drying the wood prior
to reaction, the liquid bio-oil yields is increased (Jahirul et al. 2012). High moisture content
which eventually reduces its calorific value. In general, a proper pyrolysis process needs
moisture content below 5 –15 wt% (Dobele and Urbanovich 2007).

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3.0 Methodology
3.1 Biomass preparation
In Western Australia, Mallee eucalypts are being developed as woody crops for managing
dry-land salinity in the low-to-medium rainfall (300-600 mm average annual rainfall) wheat-
belt agricultural area. Mallee is a dedicated crop of multi-branched shrubs or short trees able
to be harvested on a short cycle and able to rapidly regenerate as coppice for every 3-4 years,
which make it an ideal candidate for biomass pyrolysis.
3.2 Cutting Mill
The initial 4 kg bad of Mallee biomass material contained pre chopped wood with average
wood chip sizes greater then 1 mm. The Auger reactor requires an average feed size between
250 to 500 microns. At least two or more passes through the cutting mill was required to
reduce the wood chip size to around 250 microns. After every cutting mill pass, the wood was
then sifted through laboratory sieves at various mesh aperture size ranging from 1mm down
to 250 microns.
Figure 8: Cutting mill used to grind the Mallee wood

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3.3 Size separator
A Retsch Vibratory Sieve shaker was used to assist with the size separation process.
Laboratory sieves with aperture mesh sizes of 1mm, 750 microns, 500 microns and 250
microns was used to separate the wood chip. The 1mm sieve was filled to around half its
height with wood and the shaker was timed to run for 10 minutes at an amplitude of 60 to 80
Hz. Only wood that passed through the 500 micron sieve was collected, i.e. the wood
collected in the 250 micron sieve as collected as the final product. Any particle that fell
through the 250 micron sieve is considered as dust and was collected in a separate bag as the
dust is considered too fine for the reactor given the high steel shot feed temperatures. All
wood chips greater than 500 microns are fed back through the cutting mill and re-sieved after.
It is important to ensure that least amount of wood was wasted throughout the process, this is
achieved by minimising the amount of wood dust (particles less than 250 microns) through
the cutting mill. Approximately 2 bags (8 kg) of the initial Mallee wood chips was used to
make a 4kg bag of wood with particle sizes between 250 – 500 microns. The final bag was
sealed and kept in a cool dry area ready for the fast pyrolysis experiment.
Figure 9: Retsch Vibratory Sieve shaker used to sift through the wood
3.4 Pyrolysis process
The pyrolysis experiment will begin in the second semester of this report.

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4.0 Discussion
In summery, it is established that the key pyrolysis parameters include residence time,
heating rate and reaction temperature. During pyrolysis, a series of processes reactions take
place. Firstly, heat is transferred from the heat source to the biomass particle, resulting a rapid
increase in the temperature inside the biomass. This initiates primary pyrolysis reactions at
the pyrolysis temperature, releasing volatiles and forming char. Secondary reactions of the
primary volatile product proceed in parallel with the simultaneous primary pyrolysis
reactions, other thermal decomposition reactions including reforming, water gas shift
reactions and dehydrations. As a result, a low temperature reaction with long vapour
residence time will tend to favour the production of solid bio-char. A high temperature
reaction and long residence time will show an increase in cracking of volatiles hence greater
yield of vapour while a moderate temperature and a short vapour residence time are optimum
for producing bio-oil. It was suggested in Browns report that for a heat carrier temperature
below 550 °C requires a lower auger screw speed to achieve high bio-oil yields. This may be
due to the increased mixing of biomass and shot media interaction that was observed for low
auger speeds increasing heat transfer residence time. However, at above 550 °C, higher auger
speeds are favourable to increase the pyrolysis liquid yield, which suggests that additional
mixing time between heat carrier material and biomass is not required and provides minimal
benefit. The hot temperature of the material at these conditions may sufficiently pyrolyze the
biomass quickly without the additional solids residence time given by slow auger speeds. As
the general response shows that heat carrier temperatures above 550°C are desired for
increasing bio-oil yield, the result from this interaction effect implies that high auger speed
are also desired to maximize liquid yield (Brown 2009).
This report will detail the yield of bio-oil as a function of heat transfer medium. Clear
relationships between product yields and composition with the reactor operating conditions
will be identified. The operation conditions of the auger reactor will be kept constant such as
nitrogen flow rate, screw speed, biomass feed flow rate, heat carrier flow rate and condenser
conditions. This will allow for only the feed shot media a changing variable. The
temperatures will range from approximately 450 to 600 ºC at 20 ºC increments (or depending
an amount of Mallee wood available). The contents within the bio-oil such as water,
hydrocarbons, oxygen etc. will be analysed as well as the product yields of gas and bio-char.

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5.0 Research Conclusion
Pyrolysis is one of the most efficient thermal pre-treatment processes to obtain liquid fuels
from biomass. Bio-oil is a low cost abundantly available biofuel produced from
lignocellulosis materials. Bio-oil production converts up to 50 to 60% of the biomass energy
into liquid. The thermal efficiency of liquid pyrolysis production is approximately 60 to 80%
depending on reactor operating conditions and biomass properties.
Reactor temperature has a significant influence on the pyrolysis process and resulting product
distribution. The effect of the pyrolysis temperature on the yield and composition of lignin
oligomers in industrially relevant conditions was studied on an auger reactor. It was identified
that as the reaction temperature increases, the moisture inside the biomass evaporates first
and thermal degradation of the dried portion of the particle takes place. At the same time, a
dark brown liquid is produced and volatile species are gradually released from the particles’
surface. The volatile species and liquid pyrolysis then undergoes a series of secondary
reactions such as decarboxylation, de-carbonylation, de-oxygenation de-hydrogenetaion and
cracking to form components of syngas. As a result, higher reaction temperatures favour bio-
oil decomposition, and even higher temperatures will further crack the bio-oil thus increasing
the yields of syngas and decreasing the oil and solid yields.

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6.0 References
Abdullah,!Hanisom!binti.!2010.!"High!Energy!Density!Fuels!Derived!from!Mallee!Biomass:!
Fuel!Properties!and!Implications."!Department!of!Chemical!Engineering,!Curtin!
University,!Perth!WA.!
http://espace.library.curtin.edu.au/webclient/StreamGate?folder_id=0&dvs=14665672
29735~700&usePid1=true&usePid2=true.!
!
Bridgwater,!Tony,!Dietrich!Meier,!and!Desmond!Radlein.!2016.!"An!Overview!of!Fast!
Pyrolysis!of!Biomass."!
https://www.researchgate.net/publication/222485410_An_Overview_of_Fast_Pyrolys
is_of_Biomass.!
!
Brown,!Jared!Nathaniel.!2009.!"Development!of!a!LabUScale!Auger!Reactor!for!Biomass!Fast!
Pyrolysis!and!Process!Optimization!Using!Response!Surface!Methodology."!Graduate!
Theses!and!Dissertations.!Paper!10996,!Mechanical!Engineering!Commons,!Iowa!
State!University!Ames,!Iowa.!
https://www.researchgate.net/publication/254610758_Development_of_a_lab-
scale_auger_reactor_for_biomass_fast_pyrolysis_and_process_optimization_using_re
sponse_surface_methodology.!
!
Brownsort,!Peter.!2009.!Biomass'Pyrolusis'Processes:'Performance'Parameters'and'Their'
Influence'on'Biochar'System'Benefits.!University!of!Newcastle!University!of!
Newcastle.!https://www.era.lib.ed.ac.uk/bitstream/handle/1842/3116/Brownsort PA
MSc 2009.pdf;jsessionid=D381C8D12B540ED3E6B70B6258940C36?sequence=1.!
!
Demirbas,!Fatih!M.!2007.!"Biomass!Pyrolysis!for!Liquid!Fuels!and!Chemicals:!A!Review."!
Mahallesi!University,!Mahallesi!University!Trabzon!Turkey.!
http://nopr.niscair.res.in/bitstream/123456789/1319/1/JSIR 66(10) (2007) 797-
804.pdf.!
!
Dobele,!Galina,!and!Igors!Urbanovich.!2007.!"Fast!Pyrolysys!U!Effect!of!Wood!Drying!on!the!
Yeild!and!Properties!of!BioUOil."!
https://www.ncsu.edu/bioresources/BioRes_02/BioRes_02_4_699_706_Dobele_UVK
S_Fast_Pyrolysis_WoodDrying_Bio_Oil.pdf.!
!
Easterly,!James!L.!2002.!Assessment'of'Bio9Oil'as'a'Replacement'for'Heating'Oil.!
http://www.nrbp.org/pdfs/pub34.pdf.!
!
Guo,!Min,!and!Jicheng!Bi.!2015.!Pyrolysis'Characteristics'of'Corn'Stalk'with'Solid'Heat'
Carrier.!
https://www.ncsu.edu/bioresources/BioRes_10/BioRes_10_3_3839_Guo_Bi_Pyrolysi
s_Charact_Corn_Stalk_Solid_Heat_Carrier_7057.pdf.!
!
Jahirul,!Mohammad!I.,!Mohammad!G.!Rasul,!Ashfaque!Ahmed!Chowdhury,!and!Nanjappa!
Ashwath.!2012.!Biofuels'Production'through'Biomass'Pyrolysis'—'a'Technological'

23 | P a g e
Review.!Central!Queensland!University.!http://www.mdpi.com/1996-
1073/5/12/4952/pdf.!
!
Mohan,!Dinesh,!Charles!U.!Pittman,!and!Philip!H.!Steele.!2006.!"Pyrolysis!of!Wood/Biomass!
for!BioUOil:!A!Critical!Review."!Department!of!Chemistry,!Mississippi!State!UniVersity,!
Mississippi!State!University,!Mississippi!State!USA.!
http://pubs.acs.org.dbgw.lis.curtin.edu.au/doi/pdf/10.1021/ef0502397.!
!
Murray,!Todd.!2014.!BioUOil:!An!Introduction!to!Fast!Pyrolysis!and!Its!Applications.!
Washington!State!University.!
http://cru.cahe.wsu.edu/CEPublications/FS140E/FS140E.pdf.!
!
Patwardhan,!Pushkaraj!Ramchandra.!2010.!"Understanding!the!Product!Distribution!from!
Biomass!Fast!Pyrolysis."!Iowa!State!University,!Ames,!Iowa.!!
!
Shanks,!Brent!H.,!and!Stefan!Czernik.!2005.!Selective!Thermal!Processing!of!Cellulosic!
Biomass!and!Lignin.!!http://www.ecs.umass.edu/biofuels/Presentations/Thrust1-
Overview.pdf.!
!
Stevens,!Don!J.!1987.!An'Overview'of'Biomass'Thermochemical'Liquefraction'Research'
Sponsored'by'the'U.S.'Department'of'Energy.!Richland!Washington!
https://web.anl.gov/PCS/acsfuel/preprint archive/Files/Merge/Vol-32_2-0007.pdf.!
!
Verclyte,!Alexander.!2013.!"Mass!and!Heat!Transfer!Modelling!in!Screw!Reactors."!Faculteit!
BioUingenieurswetenschappen,!Universiteitgent.!
http://lib.ugent.be/fulltxt/RUG01/002/063/502/RUG01-
002063502_2013_0001_AC.pdf.!
!
Vigouroux,!Rolando!Zanzi.!2001.!Pyrolysis'of'Biomass.!Stockholm.!http://www.diva-
portal.org/smash/get/diva2:8949/FULLTEXT01.pdf.!
!
Yang,!Shou!Yin,!and!ChihUYung!Wu.!2014.!Application'of'Biomass'Fast'Pyrolysis'Part'I:'
Pyrolysis'Characteristics'and'Products.!
https://www.researchgate.net/profile/Chih_Yung_Wu/publication/270190337_Applic
ation_of_biomass_fast_pyrolysis_part_I_Pyrolysis_characteristics_and_products/link
s/567354fb08ae04d9b099d7ae.pdf?origin=publication_detail.!
!
Zheng,!Anqing,!Zengli!Zhao,!Sheng!Chang,!Zhen!Huang,!Fang!He,!and!Haibin!Li.!2012.!Effect'
of'Torrefaction'Temperature'on'Product'Distribution'from'Two9Staged'Pyrolysis'of'
Biomass.!Washington!State!University.!
http://pubs.acs.org.dbgw.lis.curtin.edu.au/doi/pdf/10.1021/ef201872y.!
!
Zhou,!Shuai,!Manuel!GarciaUPerez,!Brennan!Pecha,!Sascha!R.!A.!Kersten,!Armando!G.!
McDonald,!and!Roel!J.!M.!Westerhof.!2013.!Effect'of'the'Fast'Pyrolysis'Temperature'
on'the'Primary'and'Secondary'Products'of'Lignin.!Washington!State!USA.!
http://pubs.acs.org.dbgw.lis.curtin.edu.au/doi/pdf/10.1021/ef4001677.!

24 | P a g e
7.0 Appendices
SCOPE OF WORK FORM
Project Title: Effect of Temperature on the characteristics of bio-oil produced from
Mallee biomass using fast pyrolysis in a twin auger pyrolysis.
Student Name: Date of submission: / /
Student No: Course:
Mobile Number: Project Supervisor:
Student Email:
Mid-Year Finisher 1 Semester Project 2 Semesters Project (Year) Vacation
Project Approved by:
Signature and Date of Supervisor: / /
Signature and Date of Area Technician: / /
Basic Project Outline:
The aim of this project is to investigate the effect of temperature on the characteristics of bio-
oil produced from fast pyrolysis of wood biomass in a twin auger reactor with staged
condensation. The condensation temperature will be optimised to maximize the bio-oil yield
at different temperatures.
What do you hope to achieve?
•! Produce bio-oil from biomass fast pyrolysis in a twin auger reactor with staged
condensation.
•! Investigate the effect of pyrolysis temperature on the composition of the produced
bio-oil.
•! Analyse the formation of different bio-oil fractions from the multi-stage condensation.

25 | P a g e
Proposed site of testing:
Becher building and 205:148
Proposed Equipment Required:
For Twin-Screw Auger Pyrolysis Reactor,
Cutting mill
Electrical shaker
Glass drying bottle
Drying oven
Desiccator
Gas rotometer 1 (4.5 L/min N2 max)
Feeder
Feeder motor (90 VDC)
Feeder controller
Metering auger (1.27 cm OD)
Heat carrier hopper (11.33 L)
Pre-heater 1 (450 W) (2)
Pre-heater 2 (450 W) (2)
Heating tape (4)
Heating tape controller (4)
Heat carrier pipe
Main Heater (1800 W) (2)
Main heater controller
Heat carrier pipe
Meter auger motor (90 VDC)
Metering auger controller
Metering auger (2.858 cm OD)
Gas rotometer 2-1&2-2 (4.5 L/min N2 max*2)
Reactor vessel
Reactor augers (2.54 cm OD) (2)
Reactor augers motor (90 VDC)
Compressed nitrogen cylinder
Nitrogen mass flow controller
Gas cyclone
Bio char collection canister (OD=3.81 cm; L=15.24 cm)
Condenser 1 (Cooled with room temperature water)
Condenser 2 (Cooled with chilled water)
Liquid rotometers (1.39 L/min H2O max) (2)
Electrostatic Precipitator (ESP)
Collection bottles (250 mL) (3); (50 mL) (1)
Vacuum pump
Volume meter
Gas leakage detector
Lab timers
Please attach a Chemical List (including gases and Liquid Nitrogen for instruments):
Mallee Wood

26 | P a g e
Nitrogen
Methanol
Chloroform
Please attach Drawings if applicable.
Figure 10: Schematic diagram of auger reactor system for pyrolysis
GAS
GAS
GAS
GAS
GAS
GAS GAS
GAS
GAS
GAS
GAS
GAS
GAS
GAS
GAS GAS GAS
GAS
GAS
GAS
GAS
GAS
GAS
Nitrogen
Tank
heat0carrier
biomass
vapor
thermometer
18#0standard0metering
auger
Nitrogen
purge
Nitrogen
purge
Non<condensable
Gas
Nitrogen
Pump
condenser01
condenser02
condenser
3
ice
bath
Volume
Meter
HEAT0CARRIER0SECTION
BIOMASS
FEEDING
SECTION
AUGER
REACTING
SECTION
PRODUCT
RECOVERY
SECTION
AUGER
REACTOR
SECTION
Gas
Outlet

27 | P a g e
Gas$Rotometer$1
Nitrogen
water$outlet
Feed$motor
with$controller
water$inlet
flow$meter
Figure 11: Schematic diagram of biomass feeding section of the auger reactor

28 | P a g e
pre$heater(1
pre$heater(2
Main(heater
heating(tape
Pipe
Feed(motor
with(controller
Nitrogen
Gas(Rotometer
2$2
Nitrogen
Gas(Rotometer
2$1
Figure 12: Schematic diagram of heat carrier section of the auger reactor

29 | P a g e
thermocouple
solid.canister
Pressure
Gauge
vapor.outlet heat.carrier
biomass
Feed.motor
with.controller
Nitrogen
Gas.Rotometer.4
Nitrogen
Gas.Rotometer.3
Figure 13: Schematic diagram of auger reaction section of the auger reactor

Faculty of Science and Engineering
30 | P a g e
Condenser(4
(Ice(bath)
cyclone
biochar(canister
condenser(1
water(inlet
water
(outlet
condenser(2
250mL
nalgene
bottle
25mL(nalgene
bottle
water(inlet
water
(outlet
ESP
volume(meter
flow(meter flow(meter
250mL
nalgene
bottle
250mL
nalgene
bottle
Figure 14: Schematic diagram of product recovery section of the auger reactor
Gas
Outlet

31 | P a g e
RISK ASSESSMENT FORM
1. Basic Project Step by Step
1.1 Pyrolysis Experiment using Auger Reactor
Brief Description: The Twin Screw Auger Pyrolysis Reactor is a new fast pyrolysis reactor
system with 4 sections as shown in Figure 1, namely, biomass feeding section (Fig.2),
heating carrier section (Fig.3), auger reactor section (Fig.4) and product recovery section
(Fig.5). The biomass feeding section consists of an airtight hopper with a pore through the
lid tubed with purge gas, the flow of which is controlled by gas roto-meter 1, and a metering
auger, the speed of which is adjusted by an attached metering auger controller. The main
component of the heating carrier section is a long tube (about 1 meter) connected with a
hopper on the top. The tube is separated into 2 parts: the preheating part with 2 pre-heaters
covered outside the tube and the main heating part with a main heater. The lid of the store
hopper is also tubed with nitrogen gas. The heating carrier is transferred by an auger
transferor under the tube, the speed of which is also controlled by an attached metering
auger controller. The auger reactor section uses two parallel rotating augers controlled by a
metering auger controller to transfer and mix the biomass and heat carrier. The pyrolysis
reaction happens during the transferring and mixing process. The vapours from the reactor
system are tubed to the recovery system, which consists of 4 condensers, the first 2 of them
are condensed with water flow, the 3rd
one is an electrostatic precipitator (ESP), and the 4th
in water bath. To ensure the temperatures of the pyrolysis reaction and the vapour, the main
reactor and the tubes connecting the cyclone and reactor section, as well as the cyclone, are
covered by heating tapes.
1. Wear an appropriate PPE (including in all experiments: long pants, long sleeve shirt and
Lab coat, covered shoes, heat tolerant gloves, Nitrile gloves, safety glasses and dust
mask).
2. Label all glassware and containers appropriately with user name, chemical name,
concentration and date before use.
3. Prepare the biomass samples by grinding them in a cutting mill. Clean the sieves first by
soap and clean water, followed by cleaning with Milli-Q water, and then drying in the
oven.
4. Sieve the samples on ~750 µm particle size in electrical shaker, and then use Milli-Q
water to wash the biomass samples to wash away the water soluble salts. The water
soluble salts should be disposed in a waste bottle.
5. Dry the samples in drying oven at 105 °C overnight in drying bottle and then cool down
to room temperature in desiccator. The biomass samples are then charge into the cutting
mill for further grinding to particle sizes less than ~120 µm.
6. Weigh ~1kg of milled biomass with electronic balance and load it into the biomass feed
hopper and ~20kg of heat carrier (sand) into the hopper of heat carrier section.
7. Weigh the cyclone and 4 oil containers (Fig.5) of the recovery section with electronic
balance. Then install them properly into the pyrolysis system. The data are all recorded
on the mass balance worksheet.
8. Turn on the extraction system of the lab first. Check the nitrogen gas cylinder and the

32 | P a g e
regulator for the pressure, and make sure the nitrogen gas is enough for experiment.
9. Turn on the gas and purge the biomass feeding section (Fig. 2), heat carrier feeding
section (Fig. 3) and auger reactor section (Fig.4).The volumetric flow rates are controlled
with gas flow roto-meters based on the desired value (~1.5 L/min).
10. Check the gas leakage after turning on the gas flow with leakage detector solution. If
there is any leakage, try to fix the leak first, and then wait for another 15 minutes and
then go to the next step. If there is no leakage, go on the gas for about 10 min and then go
to the next step.
11. Turn on the cooling water for the biomass injection auger at ~0.757 L/min, and
condensers 1 and 2 at ~1.26 L/min with flow meters. Provide cold water to condenser 2.
Around 15L of ice is added to condenser 4.
12. Start to heat the heat carrier and auger reactor, until all the temperature reach pre-set
temperature (500 ).
13. After sufficient heat carrier temperatures (about 500 ) are attained, the augers in the
reactor are initiated and set to the desired value (54 RPM) by the motor controller.
14. After the rotation of the auger reactor becomes stable, begin the heat carrier feed by
turning on the heat carrier feeding auger (~64 LPM) and record the start time with a lab
timer at the same time.
15. When the heat carrier inlet temperature becomes steady, begin the pyrolysis process. At
the beginning of the fast pyrolysis process, initiate the biomass feed and record the time
and the volume reading on the gas meter located at the gas vent (Fig. 5) of the recovery
section.
16. Continue the pyrolysis process for about 1 hour until the biomass or heat carrier is
depleted or the bio-oil collection bottles become full. Repeat test at varying heat carrier
temperatures, perform shutdown procedures when completed.
17. Stop the biomass feeding auger and the corresponding lab timer, and record the final
volume reading on the gas meter.
18. Stop the heat carrier feeding auger and the corresponding lab timer.
19. Shutdown all the heaters including pre-heaters, main heater and all the other heating
taps.
20. Continue the water and nitrogen flows to cool the system until the temperatures are
below 40 °C.
21. Turn off the water and nitrogen flows.
22. Remove the bio-oil recovery bottles, weigh the masses with electronic balance and
record the data on the mass balance worksheet.
23. After cooling to room temperature, remove the bio char collection canister and the solids
canister. The masses are determined and recorded
24. Put all the products (bio-oil, bio-char and non-condensable gas) into corresponding
containers under proper conditions (oils should be put into refrigerator, keep airtight of
the char canister) and wait for further analysis.
24. Disconnect the condensation system and clean the condensers with a mixture of
chloroform and methanol (v/v = 4:1) in the fume cupboard with appropriate PPE.
25. Waste chemicals must be collect in a separate container and labelled with “Hazardous
Waste”, their chemical compositions and relevant DG stickers, then can be provided to
the lab staff.

33 | P a g e
2. Hazards and Potential Hazards
1.! Chemical
!! Fire
!! Explosion (if some incompatible chemicals come into contact)
!! Asphyxiant
!! Corrosive
!! Oxidizing agent
!! Dust
!! Spillage
2.! Chemical incompatibilities
!! Cellulose incompatible with: oxidising agents (e.g. hypochlorites).
!! Nitrogen incompatible with: oxidising agents (e.g. hypochlorites).
3.! Gases
!! Leakage
!! Asphyxiant
4.! Electrical
!! Fire
!! Electrocution
5.! Thermal
!! Fire
!! Burns
6.! Pressure
!! A high pressure which is caused by pipes blocked when the pyrolysis experiment
is running, leads to burst and burn.
7.! Glassware
!! Breakages
!! Cuts
8.! Environment
!! Ventilation
!! Spills
!! Dust
!! Slip and trip hazards
9.! Mechanical
!! Cut injuries

34 | P a g e
3. Hazard Control, Safe Work Methods and Disposal of Waste Products, Chemicals or
Samples
PPE
Wear suitable PPE - protective clothing, gloves and eye/face protection
The minimum amount of PPE required in the lab is:
General PPE:
•! Safety glasses with side protection
•! Closed in shoes
•! Long pants
•! Long sleeved shirt or lab coat
Chemical PPE for Loading of biomass and sand into the auger reactor:
•! Dust mask. Wear a dust mask when weighing biomass samples and loading into the
biomass feeding section of auger reactor as well as loading of sand into the heat
carrier section of auger reactor. Ensure that other lab personnel in the area are also
wearing dust masks.
Chemical PPE for biomass cutting mill:
•! Leather gloves
Thermal PPE:
•! Heat tolerant gloves
Chemical
•! Ensure that the MSDS has been read and understood.
•! Complete a Chemical Risk Assessment for each chemical used.
•! Before use carefully read the product label.
•! Store samples in a cool, dry place (e.g. cupboard) away from ignition sources and
incompatible substances.
•! Store chemicals in the Chem Store.
•! Only store and use small quantities of chemicals in the lab.
•! Ensure that all samples are labelled.
•! Ensure that all samples and chemicals are sealed.
•! Use in dedicated areas.
•! Use signage.
•! Decant bulk chemicals into smaller containers.
•! Decant all chemicals into storage containers before use.
•! Use the correct type of containers to mix and store chemicals.
•! Use funnels for transferring chemicals
•! Ensure that equipment used is clean and dry before use.
•! Use spill trays.
•! Use bottle carriers.
•! Hold Winchester bottles by the neck and the base.
•! Do not mouth pipette
•! Add acid to water and not water to acid.

35 | P a g e
•! Acids must not be prepared in the vicinity of flammable solvents or oxidising agents
•! Supervision is required for decanting and the first use of a chemical.
Electrical
•! Ensure all electrical equipment is plugged into an approved RCD power point.
•! Ensure that all electrical equipment has been tested and tagged and that it is still “in
date”
•! Report any ‘out of date’ or damaged electrical equipment to the Technicians
•! Do not use any ‘out of date’, damaged or untagged electrical equipment
•! Check the rating of the power point (e.g. 10A) against the rating of the electrical
equipment before plugging it in
•! Take note of any warning signs or labels
•! Test electrical equipment to make that it works properly before using
•! Ensure electrical equipment and cords are placed away from fluids and ignition
sources
•! Ensure electrical cords are out of the way so that they can’t be accidently pulled out
•! Construct or consult a checklist for proper setting up procedure when setting up a
system that includes electrical equipment
•! Use electrical equipment under supervision
•! Proper start up and shut down procedures must be carried out in order not to damage
the electrical equipment
•! Switch off electrical equipment after use
•! Unplug electrical equipment before cleaning it
•! Know the location of the Emergency stop Buttons that shut down electrical power to
the labs
Thermal
•! Wear heat tolerant gloves.
•! Use tongs.
•! Use safety signs.
•! Keep away all flammable materials from the vicinity of the heat source.
•! Use in a dedicated area.
•! Observe any signs or labels.
•! Read the instructions before use.
•! Be trained in the use of the equipment.
•! Heat up and cool down at a steady rate.
•! Observe the heating device to make sure it reaches and stays at its set temperature.
•! Use a secondary device (thermometer, thermocouple) to confirm the temperature
readout.
•! Do not open the door of the furnace when it is operating.
•! Allow oven/furnace to cool down to room temperature before opening door and
removing samples.

36 | P a g e
Pressure
•! Understand working procedures, follow user manual.
•! Take note of any warning signs or labels.
•! Use safety signs.
•! Be trained on the equipment before you use it.
•! Only use equipment under supervision.
•! Use pressure gauges.
•! Bleed off pressure slowly.
•! Check that the system is fully sealed before use.
Glassware
•!Check glassware for any chips or cracks – do not use cracked glassware.
•!Take care when handling glassware.
•!Use heat resistant glassware (e.g. Borosilicate or Pyrex) when heating.
•!Heat glassware slowly to avoid cracking or breakage.
•!Allow glassware time to cool down after heating to avoid cracking or breakage.
•!Keep a clear bench so as to avoid knocking glassware over.
•!Check that the chemicals being used can be mixed and stored in glass.
Environment
•!Always know that the location of first aid kit, fire extinguishers and Emergency
Stop Button.
•!Learn the Emergency exits and Muster Point.
•!Do not run in laboratory.
•!Do not consume food and drinks inside the lab.
•!All experiments must be conducted and done with the supervisor’s guidance and
evaluation.
•!Follow the procedures and instructions from supervisor strictly.
•!All lab works must be done under the supervision of the supervisor or the lab
technician.
•!Ensure that all apparatus is sufficiently cleans before and after use.
•!Ensure the surroundings of the experimental area are free of any obstacles such as
wires/cables, boxes, glassware and so forth.
•!Ensure adequate ventilation such as fume cupboards and extraction systems.
•!Don’t attempt to carry too many items at once and use devices such as bottle
carriers.
Mechanical

37 | P a g e
•!Understand the working procedures and follow user manual.
•!Take note of the warning signs and labels.
•!Be trained on the cutting mill equipment before use.
•!Wear protective leather gloves to avoid cut on hands.
•!Test the equipment to make sure it works properly before use.
Always plan your work before you start
Disposal
•! No waste down the sink.
•! Dispose of all chemicals in the provided Winchester bottles and ensure that it is
labelled correctly and placed in the fume cupboard for collection.
•! Dispose of broken glassware in the glass bin.

38 | P a g e
Chemical Risk Assessment
Worksheet)
)
) ) INTRODUCTION)
The!questions!in!this!Worksheet!are!designed!to!prompt!you!to!think!about!the!risks!you!
face!when!using!chemicals!and!whether!you!believe!the!current!controls!will!adequately!
protect!you.!!You!should!not!proceed!with!the!use!of!a!product!if!you!believe!it!is!unsafe.!
There!are!two!elements!to!the!Risk+Assessment:!You!will!need!a!Safety+Data+Sheet+(SDS)!
for!the!product!(obtained!from!Chem)Alert!or!from!the!supplier)?!and!you!will!need!to!
consider!circumstances!of!use!in!your!area.!!Complete!the!Risk+Assessment!in!consultation!
with!your!supervisor.!
SECTION)1:)) SUMMARY)(from!SDS))
Chemical)/)Product)Name) Storage)Location))
Chloroform! Building:!205!!!!!!!!!!!!!!Room:!147b! ! ! ! ! !
Manufacturer)/)Supplier) Lab)for)Intended)Use)
Chem!Supply! Building:!Becher!!!!!!!!!!Room:!Lab!A!
Safety)Data)Sheet) Hazardous)and)Dangerous)Goods)
Is!a!current!SDS!Available?!(You+must+
obtain+it)!
!!Yes! !!No!!
Is!the!chemical!classified!as!Hazardous?!
!!Yes! !!No!!
Assessment!Date:!!!
6th
!April!2016!
Is!the!chemical!classified!as!Dangerous!
Goods?!!
!!Yes! !!No!(if+applicable)!
Class:!!6.1!!Sub!Class:!!!N/A!
Assessor) Supervisor)
!!
SECTION)2:)) USE)
Task!Description:!
(Including!any!storage!or!disposal!
requirements)!
Chloroform!will!be!used!to!clean!the!
condences,!once!used!the!!chemical!will!be!
collected!in!a!container!labelled!Hazardous!
Chemicals!waste!.!
Concentration:!
(%)!
100+
%!
Quantity:!!
(including!
units)!
!!1!ltr! Duration!
of!Use:!
1+sem! Frequency!
of!Use:!
Daily+!
Note:) Substances!that!are!not!classified!as!a!Hazardous)Substance!or!Dangerous)
Good!require!!
) no)further)assessment)(i.e.!you!do!not!need!to!compete!the!remaining!sections).!!!
SECTION)3:)) HOW)CAN)EXPOSURE)OCCUR?)
!!Dermal!
(Skin):!
Solid!
Aerosol!
Liquid!
!!Eyes:!!
Dust!
Aerosol!
Liquid!
!!Inhalation:!
Vapour!
Aerosols!
Gas!
Dust!
!!Ingestion:!
Dust!
! Aerosols!
!Liquid!
Hygiene!
!!Injection:!
Pressure!
Sharp!objects!
Open!wounds!
Who!is!potentially!exposed?!:!
(e.g.+Students,+Lab+Staff,+Researchers,+
Others)!
Lab!staff,!Supervisor,!Student!!

39 | P a g e
SECTION)4:)) POTENTIAL)HEALTH)EFFECTS)
Acute)(Immediate))Effects) Chronic)(Delayed))Effects)
!!Eye!and!skin!Irritant!/!Corrosion!! !!Sensitising!Agent!(Skin/Inhalation)!
!!Central!Nervous!System! !!Carcinogenic!
!!Asphyxiant!(Inhalation)! !!Liver/Kidney!Disease!
!!Respiratory!Tract!Irritant! !!Brain/Nerve!Disease!
!!Toxic!by!Skin!Exposure! !!Respiratory!Disease!
!!Toxic!by!Ingestion! !!Reproductive!System!Disease!
!!Other!(Specify):!!! ! ! ! ! ! !!Other!(Specify):!!My!result!in!skin!and!
eye!burns!with!prolonged!contact!
SECTION)5:)) RISK)RANKING)WITH)EXISTING)CONTROLS)IN)PLACE)
Risk)Matrix)
)
)
! ! LIKELIHOOD))DESCRIPTION)
!
! LIKELIHOOD)
The!event!may!
occur!only!in!
exceptional!
circumstances!
Not!expected!
but!the!event!
may!occur!at!
some!time!
The!event!
could!occur!at!
some!time!
The!event!will!
probably!occur!
in!most!
circumstances!
The!event!is!expected!to!
occur!or!has!occurred!
and!is!continuing!to!
impact!
) IMPACTS) Likelihood)Level)
CONSEQUENCE)DESCRIPTION
)
Health)and)Safety)!
Consequence)Level)
) Rare) Unlikely) Possible) Likely) Almost)Certain)
Fatality!
Permanent!Total!
Disability!
Critical)
) ) ) Extreme) )
Significant/extensive!
injury!or!illness.!!
Permanent!Partial!
Disability!
Major)
) ) High) ) )
Serious!injury!or!
illness.!!!!!!!!!!!!!!
Lost!time!injury!>10!
days!!
Moderate)
) Medium) ) ) )
Injury!or!illness!
requiring!medical!
treatment!!
Lost!time!injury!<10!
days!
Minor)
Low) ) ) ) )
Injury!or!illness!
requiring!First!Aid!
treatment!!
No!lost!time!injury!
days!
Insignificant)
) ) ) ) )

40 | P a g e
So)the)questions)are:)based)on)the)above)matrix:)
What!could!be!the!consequences?! Moderate!!
What!is!the!likelihood!of!that!happening?! Unlikley!!
What!is!the!risk!rating?!!
Note:+ If+the+rating+is+above+LOW,++
+ Risk+Management+action+is+required.!
Low!
Risk)Management)Action)
Risk)Level) Response)
Extreme)
Immediate! action! required! to! reduce! exposure.! A! detailed! mitigation! plan! must! be!
developed,!implemented!and!monitored!by!senior!management!to!reduce!the!risk!to!
as!low!as!reasonably!practicable.!!
High)
A!mitigation!plan!shall!be!developed!and!authorised!by!area!manager!or!supervisor!to!
reduce!the!risk!to!as!low!as!reasonably!practicable.!!The!effectiveness!of!risk!control!
strategies!shall!be!monitored!and!reported!to!management!and!relevant!committee.!!
Medium)
A!mitigation!plan!shall!be!developed.!!Control!strategies!are!implemented!and!
periodically!monitored.!
Low)
Manage! by! documented! routine! processes! and! procedures.! Monitor! periodically! to!
determine!situation!changes!which!may!affect!the!risk.!

41 | P a g e
SECTION)6:)) REQUIRED)CONTROL)MEASURES)TO)REDUCE)RISK)
Control) Example) Intention)to)
apply)
!1.! Elimination! Eliminate!materials!or!elements!of!the!process!that!
carry!significant!risk.!
!!!
!2.! Substitution! Substitute!a!safer!chemical!or!safer!process.! !!!
!3.! Isolation! Barriers,!enclosures,!remote!operation.! !!!
!4.! Engineering! Local!exhaust!ventilation,!dilution!ventilation.! !!!
!5.! Administrative! Supervision,!use!of!safe!work!procedures,!
housekeeping,!organisation!of!work!to!limit!
contact,!standards,!training,!signage.)
!!!
!6.! PPE! Face!shields,!safety!glasses,!goggles,!gloves,!
aprons.!
!!!
SECTION)7:)) SPECIFIC)ACTIONS)TO)REDUCE)RISK)
List!specific!actions!that!will!be!carried!out!for!each!of!the!controls!you!nominated!in!Section!
6.!!!
Control) Action)
1.! Elimination! !
2.! Substitution! !
3.! Isolation! !
4.! Engineering! Well!ventilated!area!and!under!a!fume!cupboard,!fire!extinguishes!
nearby!!
5.! Administrative! MSDS,!Supervision,!CRAs,!Housekeeping!and!labeling!!!!
6.! PPE! Lab!coat,!pants,!gloves,!safety!glasses,!gloves,!apron,!closed!in!
shoes!
Note:! If! after! the! implementation! of! all! of! the! controls! above,! the! risks! of! using! the!
assessed!chemical!remain!MODERATE!or!higher!(based!on!the!Risk+Matrix!in!
Section! 5)?! expert! advice! must! be! obtained! so! as! to! reduce! risk! before!
proceeding.!
!
The!Occupational+Health+and+Safety+Regulations+(1996)!require!that!Risk+Assessments!are!
retained.!Risk+Assessments!must!be!revised!if!procedures!change!and!are!to!be!reviewed!
every!5!years.!Save!a!copy!of!this!Risk+Assessment,!to!be!retained!in!your!area.!Give!it!a!
unique!name!(eg!CRA!+!product!name!+!your!name).!Send!a!copy!to!Health!and!Safety.!!
Any!queries!should!be!directed!to!the!!Health!and!Safety!Ext.!4900.!
!

42 | P a g e
Chemical)Risk)
Assessment)
Worksheet)
)
) ) INTRODUCTION)
Methanol! Building:!!Becher!!!!!!!!!!!!!!!Room:!!
!!!Chem!Supply! Building:!Becher!!!!!!!!!!!!!!!Room:!!Lab!D!!
obtain+it)!
!!Yes! !!No!!
!!Yes! !!No!!
Assessment!Date:!!!
!!6th
!April!2016!
Goods?!!
!!Yes! !!No!(if+applicable)!
Class:!!!!3!!!!!!Sub!Class:!!6.1!!
!
SECTION)2:)) USE)
Task!Description:!
requirements)!
Methanol!is!used!to!clean!the!condensers.!
Stored!in!a!cool,!dry,!well!ventilated!area,!
removed!from!incompatible!substances,!
heat!or!ignition!sources!and!foodstuffs.!The!
used!chemical!will!be!disposed!in!a!
container!labelled!Hazourdes!Chemicals.!!
Concentration:!
(%)!
100%! Quantity:!!
(including!
units)!
!!1000!
ml!!
Duration!
of!Use:!
1!sem! Frequency!
of!Use:!
Daily!!
Good!require!!
!!Dermal!
(Skin):!
Solid!
Aerosol!
Liquid!
!!Eyes:!!
Dust!
Aerosol!
Liquid!
!!Inhalation:!
Vapour!
Aerosols!
Gas!
Dust!
!!Ingestion:!
Dust!
! Aerosols!
!Liquid!
Hygiene!
!!Injection:!
Pressure!
Sharp!objects!
Open!wounds!

43 | P a g e
Others)!
Lab+Staff,+Researchers+performing+
experiment+!
!!Other!(Specify):!!! ! ! ! ! ! !!Other!(Specify):!Damage!to!the!optic!
nerves!may!occur!with!chronic!or!high!level!
exposure,!causing!visual!problems!and!
possible!blindness.
!
Risk)Matrix)
)
)
!
! LIKELIHOOD)
The!event!
may!occur!
only!in!
exceptional!
circumstances!
Not!
expected!
but!the!
event!may!
occur!at!
some!time!
The!event!
could!
occur!at!
some!time!
The!event!will!
probably!
occur!in!most!
circumstances!
The!event!is!
expected!to!
occur!or!has!
occurred!and!is!
continuing!to!
impact!
)
Health)and)
Safety)!
Consequence)Level)
Fatality!
Permanent!Total!
Disability!
Critical)
) ) ) Extreme) )
Permanent!Partial!
Disability!
Major)
) ) High) ) )
Serious!injury!or!
illness.!!!!!!!!!!!!!!
days!!
Moderate)
) Medium) ) ) )
Injury!or!illness!
requiring!medical!
treatment!!
days!
Minor)
Low) ) ) ) )
Injury!or!illness!
treatment!!
days!
Insignificant)
) ) ) ) )

44 | P a g e
What!could!be!the!consequences?! Major!!
!
What!is!the!likelihood!of!that!happening?! Unlikely!!
!
Low!

45 | P a g e
Risk)
Level)
Response)
Extreme)
developed,!implemented!and!monitored!by!senior!management!to!reduce!the!risk!to!as!
low!as!reasonably!practicable.!!
High)
Medium)
Low)
apply)
!!!
!4.! Engineering! Local!exhaust!ventilation,!dilution!ventilation.! !!
!
aprons.!
!!
6.!!!
Control) Action)
1.! Elimination! !
2.! Substitution! !
3.! Isolation! !
4.! Engineering! Well!ventilated!area,!fume!cupboard,!fire!extinguisher!nearby!!
5.! Administrative! MSDS,!CRAs,!Supervisions,!Training,!Housekeeping!and!Labelling!
6.! PPE! Gloves,!Safety!glasses,!pants,!Lab!coat,!closed!in!shoes!
assessed!chemical!remain!MODERATE!or!higher!(based!on!the!Risk+Matrix!in!
proceeding.!
!
!

46 | P a g e
Chemical)Risk)
Assessment)
Worksheet)
)
) ) INTRODUCTION)
Nitrogen! Building:!Becher!!!!!!!!!Room:!Gas!Cage!3!
BOC! Building:!Becher!!!!!!!!!Room:!Lab!D!
obtain+it)!
!!Yes! !!No!!
!!Yes! !!No!!
Assessment!Date:!!!
6th
!April!2016!
Goods?!!
)!Yes! !No! (if+applicable)!
Class:!2.2!!!Sub!Class:!!!N/A!
! !
SECTION)2:)) USE)
Task!Description:!
requirements)!
Nitrogen!is!fed!with!the!heat!carrier!in!a!
scealed!feed!hopper.!The!cylinder!will!be!
stored!in!a!dry!well!ventilated!area!in!a!
upright!secure!position!and!at!room!
temperature.!!
Concentration:!
(%)!
100%! Quantity:!!
(including!
units)!
!1!Ltr! Duration!
of!Use:!
1+sem! Frequency!
of!Use:!
Daily!
Good!require!!
!!Dermal!
(Skin):!
Solid!
Aerosol!
Liquid!
!!Eyes:!!
Dust!
Aerosol!
Liquid!
!!Inhalation:!
Vapour!
Aerosols!
Gas!
Dust!
!!Ingestion:!
Dust!
! Aerosols!
!Liquid!
Hygiene!
!!Injection:!
Pressure!
Sharp!objects!
Open!wounds!

47 | P a g e
Others)!
Students,+Lab+Staff,+Supervisor+!
!!Other!(Specify):!!! ! ! ! ! ! !!Other!(Specify):!!! ! ! ! ! !
Risk)Matrix)
)
)
!
! LIKELIHOOD)
The!event!
may!occur!
only!in!
exceptional!
circumstances!
Not!
expected!
but!the!
event!may!
occur!at!
some!time!
The!event!
could!
occur!at!
some!time!
The!event!will!
probably!
occur!in!most!
circumstances!
The!event!is!
expected!to!
occur!or!has!
occurred!and!is!
continuing!to!
impact!
)
Health)and)
Safety)!
Consequence)Level)
Fatality!
Permanent!Total!
Disability!
Critical)
) ) ) Extreme) )
Permanent!Partial!
Disability!
Major)
) ) High) ) )
Serious!injury!or!
illness.!!!!!!!!!!!!!!
days!!
Moderate)
) Medium) ) ) )
Injury!or!illness!
requiring!medical!
treatment!!
days!
Minor)
Low) ) ) ) )
Injury!or!illness!
treatment!!
days!
Insignificant)
) ) ) ) )

48 | P a g e
What!could!be!the!consequences?! Insignificant!
!
What!is!the!likelihood!of!that!happening?! Rare!
!
Low!

49 | P a g e
Risk)
Level)
Response)
Extreme)
developed,!implemented!and!monitored!by!senior!management!to!reduce!the!risk!to!as!
low!as!reasonably!practicable.!!
High)
Medium)
Low)

50 | P a g e
apply)
!!!
!10.! Engineering! Local!exhaust!ventilation,!dilution!ventilation.! !!!
!!!
aprons.!
!!!
6.!!!
Control) Action)
7.! Elimination! !
8.! Substitution! !
9.! Isolation! Gas!flows!in!a!scealed!storage!hopper!containing!the!heat!carrier!
10.! Engineering! Operated!in!a!well!ventilated!area!
11.! Administrative! MSDS,!CRA,!Supervision,!training!
12.! PPE! Safety!glasses,!lab!coat,!pants,!closed!in!shoes!
assessed!chemical!remain!MODERATE!or!higher!(based!on!the! Risk+Matrix!in!
proceeding.!
!

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