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Experimental Results Contributed to Early Detection of Smouldering Milk

Powder as an Integrated Part of Maintaining Spray Drying Plant Safety
Li Vun Chonga; Xiao Dong Chenab; Anthony R. Mackerethc
a
Department of Chemical and Materials Engineering, The University of Auckland, Auckland, New
Zealand b Department of Chemical Engineering, Monash University, Clayton Campus, Melbourne,
Australia c Fonterra Research Centre, Palmerston North, New Zealand

To cite this Article Chong, Li Vun , Chen, Xiao Dong and Mackereth, Anthony R.(2006) 'Experimental Results Contributed
to Early Detection of Smouldering Milk Powder as an Integrated Part of Maintaining Spray Drying Plant Safety', Drying
Technology, 24: 6, 783 — 789
To link to this Article: DOI: 10.1080/03602550600685382
URL: http://dx.doi.org/10.1080/03602550600685382

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 Drying Technology, 24: 783–789, 2006
Copyright # 2006 Taylor & Francis Group, LLC
ISSN: 0737-3937 print/1532-2300 online
DOI: 10.1080/03602550600685382

Experimental Results Contributed to Early Detection of

Smouldering Milk Powder as an Integrated Part of
Maintaining Spray Drying Plant Safety
Li Vun Chong,1 Xiao Dong Chen,2 and Anthony R. Mackereth3
1
Department of Chemical and Materials Engineering, The University of Auckland, Auckland,
New Zealand
2
Department of Chemical and Materials Engineering, The University of Auckland, Auckland,
New Zealand, and Department of Chemical Engineering, Monash University, Clayton Campus,
Melbourne, Australia
3
Fonterra Research Centre, Palmerston North, New Zealand

during the incomplete combustion of milk powder is found

Smoldering milk powder lumps deposited on dryer walls or fall- in literature.
Downloaded At: 03:21 21 January 2011

ing through the hot air could potentially start a fire or even an
explosion in milk powder dryers. Explosive behavior is more fre-
quently experienced in the modern industry, where high production
throughputs are desired. It has been known that powder at such a
state emits carbon monoxide (CO). The work reported in this article
is the study of the characteristics of CO generation during the
incomplete combustion of milk powders. The powders used in the
study were whole milk and skim milk. Samples placed in a reactor
were heated using air at 300
C. The exhaust air of the reactor was
continuously measured for CO concentration using a highly sensi-
tive CO analyzer. Temperatures were monitored, and the smoke
produced during the combustion of whole milk powder was collected
and analyzed using gas-chromatography mass-spectroscopy (GC-
MS). Whole milk powder was found to produce significantly higher
amounts of CO than skim milk powder. Hydrocarbons, alcohols,
and carboxylic acids were tentatively identified during the GC-
MS analyses. Results from the study are definitely useful in optimiz-
ing the use of an early fire detection system in milk powder plants.
Keywords CO detection; Fire detection; Smoke point; Spray
drying; Volatile analysis
INTRODUCTION
It has been found that smouldering milk powder (before
ignition occurred) produced detectable amounts of carbon
monoxide, CO.[1] The results of earlier tests have since been
used by the Netherlands Institute of Dairy Research
(NIZO) in the design of an early fire detection system based
on measuring CO concentration in the exhaust stream of a
milk powder plant.[2] However, due to the confidentiality of
the results, little about the characteristics of CO generation
Correspondence: Xiao Dong Chen, Department of Chemical
and Materials Engineering, Private Bag 92019, Auckland 1001,
New Zealand; E-mail: d.chen@auckland.ac.nz
The work presented in this article was part of a larger
project in which the thermal ignition of dairy powders
was studied.[3] The thermal ignition characteristics of vari-
ous milk powders have been established using the novel
basket heating methods that have been reported already
in the literature[4,5] by the same authors. In these tests, steal
mesh baskets were used to contain milk powders with cer-
tain packing densities, which were heated in circulated hot
air oven. The transient method of measuring ignition para-
meters such as activation energies was developed and
used.[3]
The aim of this part of the work was to determine the
characteristics of smoldering milk powder by examining
the generation of CO per unit mass of milk powders and
the changes in temperature as milk powder samples under-
went external heating. A reactor was designed for this pur-
pose so that the uniform behavior of each powder for CO
emission can be assessed. Hot air was used to heat milk
powder samples. The air leaving the reactor was analyzed
for CO by a very sensitive CO analyzer. Fresh whole and
skim milk powders were tested. This article presents the
results of the tests carried out. The significance of the
results on the design of an early fire detection system is
outlined.
EXPERIMENTAL APPARATUS
The combustion test rig consisted of a temperature-
controlled furnace, a reactor, a smoke detector, gas filters,
sample air cooling unit, gas analysis instruments, a data
acquisition system and an optional air dilution line.
Figure 1 shows the schematic diagram of the experimental

783
 784 CHONG, CHEN, AND MACKERETH

FIG. 2. Cross section of the reactor showing the positions of the ther-
mocouples and sample; the right-hand end was attached to the furnace’s
quartz tube.

sample containers used in the experimental study of the

self-ignition of fibrous materials.[6,7]
FIG. 1. Schematic diagram of the combustion test setup.
The powders tested were fresh whole and skim milk
powders. The composition of the fresh powders are given
setup. The sample air flowed through silicon tubes in in Table 1.
between the components. Air supply to the furnace flowed
through a plastic tube which was attached to the com-
pressed air supply pressure regulator. EXPERIMENTAL PROCEDURE
The condenser was used to cool the sample gas down Both analyzers were switched on at about half an hour
before it was filtered. Ice water was used as the cooling
Downloaded At: 03:21 21 January 2011

prior to each experiment for readings to stabilise. Samples

agent. The gas filter system consisted of two conical flasks were packed into the mesh ring. The ring was then posi-
with fittings to which flexible silicon tubes were attached. tioned in between a few stainless steel rings, the number
Cotton wool was packed into the glass flask fittings. The of which depended on the length of the mesh ring.
primary function of the system was to remove smoke par- Table 2 shows the amounts of powder used for all lengths.
ticles and liquid droplets, so that contamination in the ana- The first and the last stainless steel rings were the ones cov-
lyzers is minimized. A peristaltic pump was used to draw ered with mesh on one side. The whole set was slid into the
the sample gas through the densely packed cotton wool. main body of the reactor. The body was screwed in place.
A domestic smoke detector was positioned just above The cover was then attached, followed by the exhaust tube.
the outlet of the reactor. The signal from the detector The whole reactor was then covered with the insulation
was fed to the data acquisition system to indicate the pres- material.
ence of smoke in the gas stream. The sample temperature at
which a smoke signal was first picked-up was called the
‘‘smoke point.’’
The two gas analysis instruments used were a Model 48
Gas Filter Correlation CO analyzer (Thermo Environmental
Instruments Inc.) and a KM9003 combustion analyser
(Kane-May Ltd., England). The CO analyzer measured
CO concentration to the nearest 0.1 ppm. The combustion
analyzer was used to measure O2 concentration in the
sample air.
Figure 2 shows the cross section of the reactor. Three
temperatures were measured: the temperature of the inlet
air, sample temperature, and the temperature of the air
leaving the reactor. The powder sample was held in a stain-
less steel mesh ring with diameter of approximately 12 mm.
Three lengths of rings were used in this study. They were
16, 26, and 36 mm. The ring was sandwiched between
two, three, or four 1-cm-long, 1.5-mm wall thickness stain-
less steel rings, depending on the length of the mesh ring
used. The first and last stainless steel rings were covered FIG. 3. Diagram showing how the sample was held in place before
with mesh at one end (see Fig. 3). These were similar to being positioned in the reactor tube.
 MAINTAINING SPRAY DRYING PLANT SAFETY 785

TABLE 1 TABLE 3
Composition of the whole milk powder (WMP) and skim Experimental parameters for the combustion tests
milk powder (SMP) used Whole Skim
Component WMP SMP Parameter milk powder milk powder
Protein 28.0 37.8 Inlet air 300 300
Lactose 36.8 49.8 temperature (
C)
Fat 26.5 0.8 Rate of increase 3.3 3.3
Moisture 2.8 3.8 in temperature (
C=min)
Ash=minerals 5.9 7.8 Air flow rate 10 11
(L=min at STP)
Dilution of sample air 10 times None
The pressure regulator and rotameter were adjusted to
give the desired air flows for the reactor and dilution
stream. For whole milk powder tests, the air flow rate in
The inlet temperature of 300
C was found to be neces-
the dilution stream was such that the sample gas was
sary to ensure the ignition to occur, which guaranteed the
diluted ten times. The speed controller for the peristaltic
smoldering and then combustion states to be established.
pump was set to draw sample air from the reactor exhaust
Dilution was required for powders that produced more
tube at a rate of 0.3 L=min at STP. To dilute this sample air
than 1000 ppm of CO. This was because the highest output
ten times, the flow rate of the air for dilution was adjusted
range for the analyzer was 1000 ppm over a 10 V range.
to 2.7 L=min at STP. Temperature set-point and ramp were
Although readings above 1000 ppm continued to be dis-
entered on the controller, and the pump for the cooling
played on the analyzer’s LED display, the analyzer could
water was switched on.
not send an output signal of greater than 10 V.
Downloaded At: 03:21 21 January 2011

Each test was run until smoldering or combustion

occurred and was aborted when temperature and CO con-
centration readings were back to normal. The data
recorded were inlet air, sample and outlet air temperatures,
CO and O2 concentrations, and signal from the smoke
detector. The experimental parameters for the two powders
are listed in Table 3.
There was a slight variation in experimental setup for
skim milk powder tests. Due to the low concentration of
CO generated, the sample air delivered to the CO analyzer
was not diluted. Instead of the peristaltic pump (which had
a low flow capacity), a diaphragm pump (Charles Austin
LX2 Capex pump) was used to draw the sample air
through the cooler and filter system. This pump delivered
the sample air at a rate of 6 L=min to both analyzers. To
ensure the two analyzers receive enough flow, a clip was
used to decrease the flow to the combustion analyzer so
that the flow rate to the CO analyzer was at least 4 L=min
min (the pressure drop in the line to the combustion analy-
zer was much lower than the pressure drop in the line to the
CO analyzer).
TABLE 2
Mass of powder for each sample size
Mass of powder (g)
Mesh length (mm) Whole milk Skim milk
16 2.0 2.1
26 2.9 3.7
36 4.2 5.1
RESULTS AND DISCUSSION
The maximum attainable concentration for whole milk
powder was in excess of 5000 ppm. On the other hand,
the maximum level for skim milk powder was less than
200 ppm. In general, the maximum CO concentration and
sample temperature increased with increasing sample size.
The minimum recorded O2 concentration decreased with
increasing whole milk powder sample size. This was due
to more O2 being consumed by the larger mass of powder.
The change in O2 concentration during the smoldering of
skim milk powder was negligible.
The amounts of CO generated during the smoldering
of whole and skim milk powders were quite different.
Figures 4 and 5 show typical plots of measured CO and
O2 concentrations against time for whole and skim milk
powders, respectively, for the time immediately before
and during the smoldering period. The maximum sample
temperature attained during a whole milk powder test
was significantly greater than that of a skim milk powder
test. Figures 6 and 7 show plots of sample temperature
and corresponding CO concentration versus time for whole
and skim milk powder tests, respectively. The main results
of both types of milk powder of various sample size are
listed in Table 4.
As the sample size was increased, the maximum tem-
perature attained was higher, which is consistent with the
larger sample producing more heat in the assembly but
poorer heat transfer for losses. The per unit mass produced
CO level detected downstream was in fact lower for the
larger samples. It is possible that due to the higher
 786 CHONG, CHEN, AND MACKERETH
FIG. 4. CO and O2 concentrations measured during a whole milk
powder test with inlet temperature ¼ 300
C (sample ¼ 1.6 g); the time
axis indicates time elapsed since the beginning of the experiments.
Downloaded At: 03:21 21 January 2011
FIG. 5. CO and O2 concentrations measured during a skim milk powder
test with inlet temperature ¼ 300
C (sample mass ¼ 2.1 g).
temperature in the larger samples, the greater conversion of
CO to CO2, and the lower CO content per unit mass.
The CO level per unit mass is much higher for whole milk
FIG. 6. Sample temperature and CO concentration measured during
a whole milk powder test with inlet temperature ¼ 300
C (sample
mass ¼ 1.6 g).
FIG. 7. Sample temperature and CO concentration versus time mea-
sured during a skim milk powder test with inlet temperature ¼ 300
C
(sample mass ¼ 2.1 g).
powder than for skim milk powder. This may be due to the
large fat content, which is the most oxidative component
in milk powder. This suggests that it is more difficult to
capture an early fire warning when producing skim milk
powder.
A significant difference observed during the whole milk
and skim milk powder tests was the amount of smoke gen-
erated leading up to and during the period when the
maximum CO concentration was detected. The smoke pro-
duced during the smoldering of whole milk powder was
thick and had a strong, pungent smell. On the other hand,
the smoke generated during a skim milk powder test was
light, and the amount was far less than that of a whole milk
powder test.
The smoke points for both whole and skim milk powders
decreased with increasing sample size. It should be pointed
out that with the setup of the reactor, one end of the sample
was exposed to the hot air coming into the reactor (see
Fig. 2). The reactor was designed such that the tip of the
thermocouple measuring sample temperature was always
in the middle of the sample (to ensure this, the position of
the sample was adjusted by shifting the positions of the
rings that held the mesh sample holder in place). As such,
as the sample size increased, the distance from the thermo-
couple to the end that faced the incoming hot air increased.
The sample end facing the incoming hot air would start to
smolder and generate smoke before the temperature at mid-
dle of the sample reached the smoke temperature.
At the end of the tests, and after the reactor had cooled
down to room temperature, the samples were taken out of
the reactor tube. Whole milk powder samples that had
ignited produced ash-like material, which remained in the
sample holder. The ash was between 6 and 7 wt.% of the
original sample mass. At the end of a skim milk powder
test, a charred, charcoal-like sample remained. The heat
generated by the reactions that the skim milk powder sam-
ple had undergone, together with the heat supplied by the
 MAINTAINING SPRAY DRYING PLANT SAFETY 787

TABLE 4
Maximum CO concentration, sample temperature and minimum O2 concentration measured for the smoldering
of milk powders
Maximum CO generated Maximum T Minimum Smoke
Powder Mass (g) (ppm) and per unit mass (ppm.g1) (
C) O2 (%) point (
C)
Whole milk 2.0 5890  440 (2945) 854  18 19.3  0.3 188  6
2.9 6360  200 (2193) 937  18 18.8  0.3 175  20
4.2 7850  550 (1869) 965  6 17.9  0.3 154  7
Skim milk 2.1 118  14 (56) 305  5 N=A 240  15
3.7 158  4 (43) 318  6 N=A 216  3
5.1 188  10 (37) 322  3 N=A 214  12

hot air, was insufficient to cause ignition of the sample. The
combustion behavior of skim milk powder was therefore
quite different to that of whole milk powder. Although
no visual inspection was possible (the reactor was made
of solid stainless steel), the sample temperature (at times
in excess of 750
C) indicated that whole milk powder was
probably red hot at the peak of the combustion process,
Downloaded At: 03:21 21 January 2011
reaction to form CO. Based on the simple reaction of car-
bon and O2, 2C(s) þ O2(g) ! 2CO(g), the amount of O2
consumed (initial O2 concentration minus the recorded
minimum O2 concentration) was used to calculate the
amount of CO formed. Table 5 compares the calculated
maximum CO concentration based on the maximum
amount of O2 consumed (O2 concentration in air minus

while there was only a brief smoldering period in the com- measured minimum O2 concentration) with the maximum
bustion of skim milk powder. CO concentration measured in the experiments for the
To examine the effect of temperature on CO generation, whole milk powder samples.
CO concentration was plotted against temperature. Figures It was obvious that the predicted CO concentrations
8 and 9 show the graphs of change in the exhaust air’s CO from O2 concentrations were significantly higher than the
concentration with sample temperature for three samples measured values from experiments. The calculated results
of whole and skim milk powders. Figure 8 shows that the indicated that the consumption of O2 was not solely for
first significant increase in CO concentration occurred at the oxidation reaction to form CO. The exaggerated pre-
200
C for the two larger samples of whole milk powder. diction indicated that only a small amount of O2 was actu-
The second and even greater increase in CO concentration ally involved in the formation of CO. It was also possible
occurred when the sample temperature was about 260
C that some of the O2 consumed was involved in the forma-
for the 4.2-g sample and about 320
C for the 3.1-g sample. tion of CO2. Unfortunately, due to the lack of equipment,
The smallest sample showed a more gradual increase in CO no analysis on the formation CO2 was carried out.
generation with temperature. Another possible mechanism that consumed some of the
The increase in CO concentration for skim milk powder O2 was in the propagation stage of the autoxidation of the
was gradual for all three sample sizes. The two larger sam-
ples emitted similar amounts of CO for temperatures up to
about 240
C. At a given temperature above 150
C, the
amount of CO generated by the smallest sample was always
less than the two larger samples.
The main reason for the difference in amounts of CO
generated during the smoldering of the two types of pow-
der may be the composition of the powders. The major dif-
ference in the compositions of whole and skim milk
powders was the fat content, with whole milk powder hav-
ing a much higher amount of fat. It was suspected that
oxidation of fat was the main CO-generating reaction that
occurred during the heating of the sample. With a higher
fat content, more CO was generated during the smoldering
of whole milk powder.
The O2 concentration in the exhaust air was measured to FIG. 8. Change in CO concentration with sample temperature during
determine the amount of O2 consumed in the oxidation the smoldering of three whole milk powder samples of different mass.
 788 CHONG, CHEN, AND MACKERETH
FIG. 9. Change in CO concentration with sample temperature during
the smoldering of three skim milk powder samples of various mass.
unsaturated fatty acids in milk powder. It has been found
that the principal reaction pathways for low- and high-tem-
perature autoxidation of fatty unsaturated fatty acids were
basically the same, and at elevated temperatures, the reac-
tions proceeded very rapidly.[8] The reaction of unsaturated
lipids or fatty acids with O2 to form hydroperoxides
Downloaded At: 03:21 21 January 2011
involved three stages.[9–12] These can be summarized in a
simple form as follows:
Initiation:
heat; light; metals
Fatty acids=phospholipids ! free radicals
Propagation:
Free radicals þ O2 ! peroxylradicals
Termination:
 The majority of the compounds in the smoke were made
Free radicals þ peroxyl radicals ! peroxides
Free radicals þ free radicals ! non - radical products
Using a combined gas chromatography–mass spec-
troscopy (GC-MS) analysis, it was found that hydrocarbons
were the main volatile products formed during the smolder-
ing of whole milk powder (the analysis will be described in a
later section). This may indicate that thermal oxidative reac-
tions of fatty acids took place, and, if this was the case, some,
TABLE 5
Comparison between maximum CO concentration measured in the experiments with the
concentration calculated using the maximum O2 consumed for three whole milk powder tests
Mass (g) O2 consumed (%)
1.6 1.7
2.9 2.2
4.2 3.1
if not most, of the O2 would have been consumed during the
propagation stage of the reactions. There was also a possi-
bility that some of the volatiles formed reacted with O2. This
could also contribute to the decrease in O2 concentration.
It should be noted that, although the amount of CO
generated was measured, it was beyond the scope of this
project to determine the exact chemistry and kinetics
involved in the formation of CO. In spite of this, the
implication for the commercial development of an early
fire detection system based on CO measurement is signifi-
cant. The result for skim milk powder suggests that an
increase in CO concentration at the exhaust of plant
would be detectable if a large amount of powder is smol-
dering. Plant trials as part of the current were carried out
and results have been reported.[3] It was found that for a
plant with an air throughput of 64 m3s1, CO generated
by the equivalent of between 25 to 30 kg of smoldering
skim milk powder would be detectable. Although this
suggests that an increase in CO levels would only be
detectable if a rather large amount of powder was smol-
dering, actual experience has shown that this amount of
powder had indeed been smoldering by the time it was
detected and the plant was shut down. A detector would
therefore be able to signal a warning for the presence of
smoldering powder.
Figure 10 shows the GC-MS profile generated during
the analysis for the smoke produced in the combustion test
of whole milk powder. The peak numbers correspond to
the compounds, which were tentatively identified and listed
in Table 6. Two smoke samples were analyzed, and the
similarity in results indicated reproducibility in the tech-
nique. Although the peak heights were not identical, the
same peaks were observed in both analyses.
up of straight chained saturated hydrocarbons. This agreed
with Nawar,[12] who found that when triglycerols were
heated in air at temperatures greater than 150
C, a homolo-
gous series of hydrocarbons were produced. Alcohols and
acids have also been reported as the products of lipid auto-
xidation. However, it should be emphasised that the
compounds in Table 3 were only tentatively identified.
Each peak must be compared to the peak of a standard
to properly identify the compound it was associated with.
Calculated CO Measured CO
concentration (ppm) concentration (ppm)
34,000 5890
44,000 6360
62,000 7850
 MAINTAINING SPRAY DRYING PLANT SAFETY 789

and temperatures of samples attained when subjected to air

FIG. 10. GC-MS profile of smoke generated during the smoldering of
whole milk powder.
TABLE 6
Tentatively identified volatile compounds in the smoke
generated during the smoldering of whole milk powder
Peak no. Compound
1 Aliphatic hydrocarbon (heptane)
2 Aliphatic hydrocarbon (octane)
3 Aliphatic hydrocarbon (nonane)
4 Aliphatic hydrocarbon (nonane)
5 1-Heptyl-2-methyl-cyclopropane
6 Aliphatic hydrocarbon (undecane)
7 Aliphatic hydrocarbon (undecane)
Downloaded At: 03:21 21 January 2011
at high temperatures (up to 300
C).
Whole milk powder was found to produce significantly
higher amounts of CO than skim milk powder. Whole milk
powder samples attained much higher temperatures than
skim milk powder. For both powders, the amount of CO
generated increased with increasing sample size. Maximum
sample temperature also increased with increasing sample
size.
The volatiles formed during high-temperature oxidation
of whole milk powder have been analyzed using GC-MS.
The volatiles formed by during high temperature oxidation
have been tentatively identified as hydrocarbons, alcohols,
Retention and carboxylic acids.
time (min) The results of this work form a basis for further work in
developing an effective early fire detection system for
8.21
spray-drying plants for milk powder production.
8.87
10.16
12.45 ACKNOWLEDGEMENT
13.74 This work was funded by the New Zealand Dairy
15.71 Board.
19.91

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