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Wanna Laowagul*, Nittaya Milne*

Sunthorn Ngodngam*, Phaka Sukasem*

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ABSTRACTEmissions of particulates, polycyclic

aromatic hydrocarbons (PAHs), carbonmonoxide

(CO) and carbondioxide (CO2) from bagasse

combustion in the studied sugar refinery

factory was carried out. The samples were

taken at steady state of the process and at

isokinetic condition. The results showed

the quantities of particulates and PAHs in

the samples that collected after the furnace

was cleaned by blown out unburned

hydrocarbon and ashes were lower than

the samples that collected without cleansing

furnace. Moreover, total PAHs concentration

and their emission rate are found to be

correspondent with total particulates and CO

emissions. Concerning the characteristic

profiles of PAHs, in particulate matters the

most predominant was fluoranthene, the

second most predominant was pyrene. In

vapour phase, the most abundant PAHs

was napthalene, the second abundant was

phenanthrene.

1. IntroductionAt the most basic level, energy is

essential for all human activities. Present

energy use is mainly non-renewable fossil

fuels, which are accounting for 82% of all

energy consumption worldwide.1 However,

disadvantages of combustion of fossil fuels

are sulfur dioxide (SO2) and nitrogen oxide

(NOx) emissions into the atmosphere, causing

acid rain at the local and global scales, which

seriously damage ecosystem and human

health. Fur thermore, there are intrinsic

connection with worldûs problems of sustainable

development, climate change, global warming

and biodiversity.2 As a result of growing

worldwide concern about the environmental

impact of fossil fuel consumption, the world

is now apparent ly headed toward a

commitment to develop energy systems that

are less dependent on fossil fuels.3

To obtain sustainable and clean

environment and to substitute the fossil fuel

consumption, Thailand has elaborated on

a program to stimulate the development

and efficient use of renewable energy in the

country since 1997.4 Among renewable

energy, biomass is an important renewable

source of energy. It has been reported that,

in Thailand, biomass energy started playing

an important role, over 95% of all renewable

energy sources used are biomass.1 It has

been reported that the exploited biomass

energy resources account for 26% of gross

energy consumption in 1996.5 Supply of

biomass is available from many sources:

forests, wood plantations, agricultural and

industrial residues, and even municipal solid

wastes. Based on Thailand energy situation

1997,6 it was found that bagasses are mostly

used as source of energy in industries that

is accounting for 80% of total biomass used

as source of energy. The potential for

utilising biomass residues as fuel is in

various purposes such as fuels for steam or

power generation in conventional combustion

system and/or for combined power and steam

production in industrial sector. In Thailand,

direct combustion is one of the main

processes of thermochemical biomass

conversion for energy in industrial sector.

However , in general , the major

emissions from almost any means of

combustion of biomass materials are air

pollutants-notably par ticulates, methane

(CH4), carbondioxide (CO

2), carbonmonoxide

»Ÿπ¬å«‘®—¬·≈–Ωñ°Õ∫√¡¥â“π ‘Ëß·«¥≈âÕ¡ °√¡ àß‡ √‘¡§ÿ≥¿“æ ‘Ëß·«¥≈âÕ¡ §-35

(CO) and hydrocarbons. Besides, polycyclic

aromatic hydrocarbons (PAHs) can be formed

in any combustion process.7 These pollutants

may contribute to severe air pol lut ion

problems, especially, build-up of hazardous

substances such as PAHs in the atmosphere.

PAHs are toxic compounds and some of

them are carcinogenic or mutagenic which

make them have long been of concern as

a potential human health hazard.8 In the

atmosphere, PAHs can distribute between

the gas and particle phases according to their

volatility. PAHs are adsorbed predominantly on

suspended particulate matter in the respiratory

size range less than 5 µm.9 The study on

air pollution by airborne PAHs in industry area

indicated that PAHs were found mostly in

particulate matter less than 2.1 µm.10 Thus,

they can reach to human lung by inhalation

and might contribute to lung cancer, localized

skin effects, pulmonary and respiratory

problems, genetic reproductive and develop-

mental effect, behavioral, neurotoxic and other

organ system effect.11 The other pollutants

such as CO and particulate matter can have

an influence for the risk of cardiovascular

disease.12 CH4 and CO

2 can create greenhouse

effect which cause significant climate and

geohydrological changes. Therefore, it is

important to study their emissions from

biomass combustion in industry in order to

obtain a useful information for mitigation of

those air pollutants emitted from this process

in Thailand in which such studies are still

scarce.

2. Methods and MaterialsThe toxic pollutants such as PAHs,

particulate, CO and CO2 will be investigated

from sugar refinery. PAHs will be measured

in both forms: gas and particulate. Eighteen

PAHs were determined: napthalene (NAP),

acenapthylene (ACY), acenapthene (ACE),

fluorene (FLU) phenanthrene (PHE), anthracene

(ANT), fluoranthene (FLA), pyrene (PYR),

benzo(a)anthracene (BaA), chrysene (CHR),

benzo(e)pyrene (BeP), benzo (b) fluoranthene

(BbF), benzo(k)fluoranthene (BkF), benzo (a)

pyrene (BaP), dibenzo(a,h) anthracene (DBahA),

benzo(g,h,i)perylene (BghiP), indeno (1,2,3-

cd)pyrene (IP), and coronene (COR). 8

Samples were collected from the flue

gas by isokinetic condition in accordance with

the U.S.EPA. Modified Method 5. The flue gas

samples were passed through a glass fiber filter

of pore size 0.45 µm and then onto an XAD-2

adsorbent (Styrene divinyl benzene polymer

beads).

PAHs in the samples were analysed

using High Performance Liquid Chroma-

tograph (HPLC). CO and CO2 in flue gas

samples were determined by Orsat Analyzer

in accordance with U.S.EPA. Method 3.

2.1 PAHs and Particulates

(a) Apparatus and Materials

(i) Isokinetic source sampler manual

method 5. Apex instruments Model MC-500

Series, it is designed to sample particulate

pollutants.

(ii) Modified method 5 glassware.

Apex source testing equipment instruments,

it contains a coolant recirculating pump, a

sorbent trap, a horizontal

(iii) Soxhelt extraction unit. Sibata, it

is used for cleaning XAD-2 and glass wool.

(iv) Glass fiber filter, size 8 cm

diameter. Pallflex Products Corp.

(v) Desiccator. Sibata

(vi) Balance. Mettler, AE 240

(vii) Glass wool

(viii) Forceps

(ix) Funnel

(x) Bottle, 100 ml

(xi) Aluminum foil

(xii) Ultrasonicat ion bath. Elma,

transsonic digitals

(xiii) Centrifugal vaporizer. Eyela,

§-36 »Ÿπ¬å«‘®—¬·≈–Ωñ°Õ∫√¡¥â“π ‘Ëß·«¥≈âÕ¡ °√¡ àß‡ √‘¡§ÿ≥¿“æ ‘Ëß·«¥≈âÕ¡

model CVE-200D

(xiv) Vortex genie 2, model G-560 E

(USA)

(xv) Dry thermo unit. Taitec, model

DTU-1B

(xvi) High performance liquid chroma-

tograph (HPLC).

(b) Chemicals(i) XAD-2 adsorbent (Styrene divinyl-

benzene polymer beads). Organo CO.(ii) Blue silica gel, size 6 mesh, Nacalai

tesque.(iii) Deionized distilled water(iv) Solvents: acetone, dichlorome-

thane, methanol, acetonitrile. Chromatographicgrade, Merck, Germany.

(c) Preparation of sampling equipment(i) Desiccate the filter at least 24

hours and weight until constant weight. Thisprocedure was done before and after collectingsamples.

(ii) Clean up the sampling trainbefore sample collection using acetone anddichloromethane.

(iii) Clean up XAD-2 adsorbent andglass wool before sample collection by soxhletextractor for 16 hours.

A schematic of the sampling trainis shown in Figure 1. Due to a lot of intercom-ponent connections in par ticular probeassembly and modular sample case, thesampling may be leak, therefore, the leak-checkis necessary.

(d) Leak checking procedure

(i) Pre-test leak check: Assemble

the sampling train, turn on and set the filter

and probe heating systems at the desired

operating temperature 120 ÌC. Then check if

there is any leak on the sampling train at

the sampling site by plugging the nozzle and

pulling 15 inch Hg vacuum. Start the pump

and stop when the desired vacuum is reached.

If the leakage rate is found to be no greater

than 0.00057 m3/min. or 4% of the average

sampling rate, the results are acceptable.

(ii) Post-test leak check: The leak-

check is done with the same procedures as

the pre-test leak check, except that it is

conducted at a vacuum greater than or equal

to the maximum value reached during the

sampling run. If the leakage rate is found to be

no greater than 0.00057 m3/min. or 4% of

the average sampling rate, the results are

acceptable.

Figure 1 Modified method 5 sampling train


In this study, five samples were taken

from 12 points grid across the stack of sugar

refinery industry at isokinetic condition during

bagasse combustion period. The shape of

stack is circular. Stack height is 33 m. Inside

stack diameter is 3.5 m. Its area is 9.62 m2.

(e) Analysis

(i) PAHs in particulate

The filter sample was cut into 2 pieces

of 2.5 cm diameter by a puncher. The sample

was extracted with 15 ml of dichloromethane

using ultrasonic bath for 20 minutes. The

extract was then be analyzed using HPLC.

(ii) PAHs in gas phase

Twenty grams of XAD-2 adsorbent

was extracted with 150 ml of dichloromethane /

hexane mixture (2:1) using ultrasonic bath for

30 minutes. The extract was then be analyzed

using HPLC.

The probe and filter holder were also

extracted and analyzed using HPLC. The

remaining concentrations found on these

glasswares were added to each sample.

Fifty microliters of sample was injected

into an injector of HPLC. Acetronitrile and

water were used as the mobile phases, which

were deoxygenated by bubbling helium

through the solvent during the measurement.

The sample was carried over through the

column by 50% acetronitrile from pump A,

mixed with water from pump B by a dynamic

mixer for 5 minutes and changed by linear

gradient program. The analytical condition is

shown in Table 1.

The flow rate for the mobile phase

was 1.0 ml/min. The samples were separated

by octadecylsilane-bonded C18 (reversed-phase

column). The selected PAHs were detected

by scanning fluorescence detector of which

their excitation and emission wavelength

automatically set by a time program to detect

each PAHs selectively and sensitivity. Detection

wavelength for each PAHs was shown in

Table 2.

2.2 CO and CO2

(a) Apparatus

(i) Measuring burette with a water

jacket, 100 ml

(ii) Aspirator bottle, 125 ml

(iii) Absorption pipettes filled with

glass tubes, 3 sets

(iv) Manifold complete with four glass

stopcocks

(v) Manifold with a rubber bag

(vi) Inlet U-tube

There are rubber tube connections

between the manifold and the three pipettes,

and between the manifold and the burette.

Main Column: Wakosil II-5 C18 AR 4.6 mm I.D x 30 mmGuard Column: Wakosil II-5 C18 AR 4.6 mm I.D x 250 mmMobile Phase: Solvent Composition Time(min)

50% Acetonitrile/50% Water 585% Acetonitrile/15% Water 2085% Acetonitrile/15% Water 35100% Acetonitrile 40100% Acetronitrile 60

Column Oven: 40 ÌCFlow Rate: 1.0 ml/minInjection Volume: 50 µlDetector: Scanning fluorescence detector

Table 1 Analytical conditions


There is also tubing for the aspirator bottle

connection.

(b) Chemicals

(i) Distilled water

(ii) Cuprous chloride (CuCl)

(iii) Ammonia

(iv) Ammonium chloride (NH4Cl)

(v) Pyrogallol (C6H

3 (OH)

3)

(vi) Potassium hydroxide (KOH)

(vii) Sodium chloride (NaCl)

(viii) Sulfuric acid (H2SO

4)

(ix) Methyl orange

(c) Preparation of Absorption Reagents

(i) Absorbing solution for CO (Cu-

prous Chloride Solution)

Dissolve 12 g of NH4Cl with 360 ml of

distilled water. Add 120 g of cuprous chloride

and 570 ml of 25% ammonium hydroxide to

the NH4Cl solution. This solution should be

kept in the container, which has small pieces

of copper.

(ii) Absorbing solution for O2 (Pyro-

gallol solution)

Dissolve 60 g of pyrogallol with 100 ml

of distilled water and 30 g of KOH with 100 ml

of distilled water. Mix the solution of pyrogallol

and KOH before use.

(iii) Absorbing solution for CO2 (Po-

tassium Hydroxide Solution)

Dissolve 200 g of KOH with 400 ml of

distilled water.

(vi) Blocking water

Dissolve 22 g of NaCl with 78 g of

distilled water and add small amount of sulfuric

acid and methyl orange.

CO, CO2, O

2 and N

2 gas were collected

in 20 Tedlar bag and analyzed by Orsat

analyzer.

3. Results and DiscussionEmissions of particulate, CO, CO

2 and

PAHs from bagasse combustion in the

studied sugar refinery factory in Ratchaburi

Province, Thailand were investigated. Five

samples were taken at isokinetic condition

from stack of sugar refinery industry at

Ratchaburi Province in the central region of

Table 2 Determination of selected PAHs by HPLC/scanning fluorescence detector

PAHs CompoundConcentration

mg/mlExcitation

WavelengthEmission

WavelengthRetentionTime (min)

%RSD

0.200.100.240.170.120.110.070.090.170.270.170.150.100.060.080.100.110.07

NapthaleneAcenapthyleneAcenaptheneFluorenePhenantheneAnthraceneFluoranthenePyreneBaAChryseneBePBbFBkFBaPDbahABghiPIndeno(1,2,3-cd)pyreneCoronene

0.0180.0100.0130.0160.0060.0030.0080.0090.0020.0040.0080.0040.0020.0080.0060.0060.0120.006

280280288259250250250270250250290290290290290290300302

335330322306370450450390405405410410410410410410500445

16.0319.3919.4219.4620.3121.3922.3323.2225.6126.1628.0328.4829.9031.6233.8236.1637.4847.34


Thai land during 24-26 February 2000.

Sampling condition is shown in Table 3. Stack

temperature is ranging from 224 ÌC to 229 ÌC.

Percentage of isokinetic ranged from 95%

to 101%. For sample collection, it has to be

mentioned that the sample no.1 and no.4

were collected after the furnace was cleaned

and unburned hydrocarbons and ashes

were blown out, while other samples were

collected without cleansing state. This would

lead to the different in concentration of each

parameter. The results of particulate, CO and

CO2 in five samples are shown in Table 4.

In case of CO and CO2

It can be seen that CO:CO2 proportion

in sample no.1, 3, 4 and 5 are about 1:37,

1:30, 1:34 and 1:22, respectively. But CO:CO2

proportion in sample no.2 is about 1:11. It

can be explained that during sampling of

sample no.2, incomplete combustion of

hydrocarbon might have been occurred.

Therefore, the rate of CO formation was found

to be higher than the rate of CO2 formation.

Possible react ions mechanism of CO

formation are as follows: 13

ConditionSample

No.1 No.2 No.3 No.4 No.5

Pitot coefficient 0.85 0.85 0.85 0.85 0.85

Probe tip diameter (cm.) 1.10 1.10 1.10 1.10 1.10

Pitot tip area (m2.) 0.000095 0.000095 0.000095 0.000095 0.000095

Volume H2O vapor, standard 0.198 0.140 0.331 0.171 0.164

conditions* (m3.)

Total H2O collected (ml.) 146 104 244 126 121

Water vapor in gas stream 0.184 0.169 0.198 0.162 0.123

Dry molecular weight, stack 30.0 29.5 29.8 29.9 29.8gas (g/g-mole)

Molecular weight, wet basis 27.7 27.6 27.5 28.0 28.4(g/g-mole)

Average stack gas velocity 10.5 10.5 14.0 9.0 13.3head (mmH

2O)

Stack pressure, absolute (mmHg) 762 763 762 763 762

Average stack temperature ( ÌC ) 226 228 224 225 229

Average stack gas velocity (m/sec.) 14.8 14.9 17.1 13.6 16.5

Stack flowrate, dry standard 250091 255548 285719 237236 299121condition (m3/h)

Net time of run (min) 32 26 32 36 25

Volume dry gas, meter 1.076 0.841 1.494 1.050 1.267conditions (m3)

Volume dry gas, standard 1.046 0.823 1.472 1.029 1.252condition (m3)

Percent isokinetic % 98.5 95.2 96.0 98.9 101

Note : * Standard Condition at 25 ÌC, 760 mmHg

Table 3 Sampling condition of bagasse combustion at sugar refinery industry in Ratchaburi Province


or CO may be formed from decomposition of

unstable intermediate present during thermal

cracking of biomass species. This can be

explained by the reaction below:

It is also suspected that during sampling

of sample no.2, the remaining unburned

hydrocarbon in the furnace from previous

combustion process might have undergone

fur ther combust ion that result in CO

formation.

In case of particulate matters emissionIt is found that concentration of

particulate matter of sample no.1, 3, 4 and 5

are still below the maximum permitted quantity

in the Thailand Industrial Emission Standards,

which was issued under Factory Act, B.E.

2535 (1992) (particulate matter equal to 400

mg/Nm3).14 For sample no.2, the concentration

of particulate matter is over the above

standard. This may be caused by

1. Particulate matter emitted from

combustion of biomass has three possible

sources:

(i) Matter which was not combustible;

(ii) Matter which was capable of

being burned but was not burned; and

(iii) Matter formed during the process

of combustion.

2. The mechanisms for the formation

of soot involve the dehydrogenation of

organics and polymerization leading to

formation of large carbonaceous particles.15

In this study, eighteen compounds of

PAHs; NAP, ACY, ACE, FLU, PHE, ANT, FLA,

PYR, BaA, CHR, BeP, BbF, BkF, BaP,

DBahA, BghiP, IP, COR were determined in

considerat ions of carcinogenicity and

prevalence in the atmosphere. These PAHs

were analyzed by HPLC with equipped with

scanning fluorescence detector. It was found

that the peak of acenapthylene, acenapthene

and fluorene could not be separated, in which

they may be co-eluted together at the

excitation wavelength of 280 nm and the

emission wavelength of 330 nm. Therefore,

acenapthylene, acenapthene and fluorene

were be detected and quantified at fixed

O + CO2

O2 + CO

CO + OH CO2+ H

No. 1 24/2/00 226 35.7 0.3 11.0 319.3 47.8(3000)

No. 2 24/2/00 228 21.3 0.8 8.5 669.6 102.2(8000)

No. 3 25/2/00 224 30.2 0.4 10.6 368.1 59.1(4000)

No. 4 25/2/00 225 31.0 0.3 10.2 344.4 52.4(3000)

No. 5 26/2/00 229 25.7 0.5 10.1 375.5 67.3(5000)

Note : * = condition at 250 ( ÌC), 760 mmHg

Table 4 Flue gas condition of bagasse combustion and emissions of particulate, CO and CO2

Sample DateStack

Temperature( ÌC)

%ExcessAir

%CO(ppm)

%CO2Concentration of

Particulate(mg/m3)*

Emission Rate ofParticulate

(kg/hr)

RCO R + CO


excitation wavelength at 280, 288 and 259,

respectively, and fixed emission wavelength

at 330, 322 and 306, respectively. These

conditions were studied and approved by

previous researcher.16 The typical chromatogram

for PAH standard solution is shown in

Figure 2.

In this study, repeatability test and

cal ibrat ion curve for each PAH were

performed. It was found that the percentage

of relative standard deviation for repeatability

of retention time, peak area and peak height

was less than 10%. For the standard

calibration curves for each PAH, the peak

area of each curve is directly proportional

to the concentrat ion of PAH; and the

correlation coefficient (r) of each curve is

above 0.9866. The peak height of each

PAH also is directly proportional to the

concentration of PAH; and the correlation

coefficient (r) of each curve is above 0.9959.

In case of PAHs emissionIt is noticed that in all samples,

DBahA was not found in both particulate

and gas phase. Total PAHs concentration in

particulate was found to be correspondent

with total particulate concentration. In addition,

total PAHs emission rate in particulate was

also found to be correspondent with total

particulate emission rate (see Figure 3).

Concerning the characteristic profiles

of PAHs in this study, it is evidenced that

the most predominant PAHs in particulate was

fluoranthene. The second most predominant

was pyrene. The rest were BaP, naphthalene,

BeP, acenapthene, phenanthrene, BbF,

chrysene, anthracene, BaA, BghiP, indeno (1,2,3-

cd)pyrene, BkF, coronene, fluorene and

acenapthylene. The most abundant PAHs in

gas phase was naphthalene. The second most

abundant was phenanthrene. The rest were

fluorene, fluoranthene, pyrene, acenapthene,

anthracene and acenapthylene. The minor

concentration of PAHs in gas phase were

coronene, BkF, indeno(1,2,3-cd)pyrene, BghiP,

BbF, chrysene, BaA, BeP and BaP, which

were generally high molecular weight PAHs.

About 3.7% of total PAHs in particulate were

trapped on glass fiber filter, which has a pore

size of 0.45 µm. The major percentage of

PAHs was passing through the filter, then

trapped by the XAD-2 resin, and then be

analysed. In Figure 4, it was found that the


percentage contribution of napthalene,

acenapthylene, acenapthene, f luorene,

phenanthrene, anthracene, fluoranthene and

pyrene appear predominantly in the vapours

which have particle size of less than 0.45 µm.

When compare PAHs concentration

among samples, it is remarkably indicated

that the total PAHs concentration and emission

rate in samples No.2 are highest. This can

be explained that incomplete combustion may

have been occurred or the hydrocarbon

species in the vapours may be undergone

further reaction to form PAHs especially low

molecular weight PAHs such as napthalene.

4. ConclusionFrom the finding of this study, it is

concluded that the factory could improve their

process and reduce pollutant emissions by

better maintenance and regular cleaning or

good house keeping. The alternative options are

improve biomass feed rate or fuel blending.

5. AcknowledgementsThis study was sponsored by the

Swedish International Development Coope-

ration Agency (Sida). We gratefully acknowledge

Figure 3 Relationship between totalparticulate and total PAHs emission

Figure 4 PAHs profiles of bagasse combustion from sugar refinery factory


the Asian Institute of Technology for project

cooperation. We are extremely grateful to

the Banpong Sugar Refinery Factory staffs for

their assistants. We also deeply grateful to

Mr. Pornchai Patiwanaruk, Environmental

Research and Training Center, for his assistant

to collect the samples from stack.

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