Variables Affecting The ASTM Standard C 311 Loss On Ignition Test For Fly Ash

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Variables Affecting the ASTM Standard C 311 Loss on Ignition Test for Fly Ash
Article in Journal of ASTM International · January 2006

DOI: 10.1520/JAI100286
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Journal of ASTM International, Vol. 3, No. 8
Paper ID JAI100286
Available online at www.astm.org
Nathan J. Harris,1 Kenneth C. Hover,2 Kevin J. Folliard,3 and Tyler Ley4
Variables Affecting the ASTM Standard C 311 Loss

on Ignition Test for Fly Ash
ABSTRACT: The loss on ignition 共LOI兲 test as an indicator of carbon content in fly ash is a useful screening
tool for fly ash for use in concrete. Despite the importance and relevance of the LOI test, the LOI test results
are sensitive to procedural variations that are within the requirements of the ASTM C 311 test standard. A
suite of LOI tests on fly ash samples was performed that varied several procedural details. The effects of
cooling time, cooling method, sample size, ignition duration, and ignition temperature were evaluated.
KEYWORDS: loss on ignition, fly ash, pozzolans, variability, quality control
Background
Fly ash from coal combustion is used as a supplement to portland cement in concrete production. Its use
can improve fresh and hardened concrete properties 关1,2兴. However, residual, unburned carbon in fly ash
interacts with air entraining and possibly other organic admixtures, resulting in increased dosages for
adequate air entrainment 关3兴. To control carbon content, ASTM Standard C 618-03 关4兴 limits loss on
ignition 共LOI兲 of fly ash to 6.0 percent by mass. Although LOI is a standard index for carbon content of
ash, LOI and carbon content are not necessarily equivalent. In addition to the oxidation of carbon during
the LOI procedure, dehydration and decomposition of certain minerals and volatile organic compounds
also occur at the high temperatures of the test, affecting LOI results 关5,6兴. Some researchers suggest
alternative methods of measuring carbon content be used in addition to LOI 关5–7兴. The work reported in
this paper makes no attempt to differentiate between LOI and carbon content. The term “ignition” nor-
mally implies the oxidation of organics but its use in this paper refers to the phase of the test when the ash
is subjected to 750° C ± 50° C.
Introduction
The loss on ignition test is performed by subjecting an oven-dried ash sample to 750° C ± 50° C in a muffle
furnace 共a front-loading, high-temperature oven with an air atmosphere兲. The LOI value of the sample is
the percentage of mass lost during ignition; i.e., or the high-temperature phase. The LOI procedure for fly
ash and natural pozzolans is standardized in ASTM Standard C 311-04 关8兴 which modifies ignition
temperature and other details of the LOI procedure for hydraulic cement described in ASTM Standard C
114-05 关9兴. Heiri et al. showed that the LOI test results of lake sediments were strongly affected by furnace
temperature, exposure time, and sample size, while the effects of furnace spatial variability were minor
关10兴. Heiri et al. concluded that the use of a detailed test standard reduced interlaboratory differences.
These and other factors may also influence LOI test results for fly ash. This paper evaluates variations of
sample size, ignition temperature, ignition duration 共length of time sample is exposed to 750° C ± 50° C兲,
cooling method, and cooling time within the procedural tolerances of the LOI test standard for fly ash, and
the consequent variations in results.
Manuscript received December 14, 2005; accepted for publication May 18, 2006; published online July 2006.
1
Graduate Research Assistant, School of Civil and Environmental Engineering, Cornell University, Ithaca, NY 14853.
2
Professor, School of Civil and Environmental Engineering, Cornell University, Ithaca, NY 14853.
3
Associate Professor, Civil, Architectural and Environmental Engineering, The University of Texas at Austin, Austin, TX 78712.
4
Graduate Research Assistant, Civil, Architectural and Environmental Engineering, The University of Texas at Austin, Austin, TX
78712.
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2 JOURNAL OF ASTM INTERNATIONAL
ASTM Standard C 311 LOI Procedure

The ASTM standard LOI test procedure for fly ash and natural pozzolans is composed of two steps. First,
the moisture content of the material is determined by heating a weighed 1 g sample in an oven at 105° C
to 110° C to a constant mass. The sample is oven dried before ignition so that mass loss due to the
evaporation of surface moisture is not counted as a portion of the ignition losses. Next, the sample is
exposed to temperatures of 750° C ± 50° C1 in a muffle furnace where it typically experiences a loss in
mass. The sample is exposed to the test temperatures until the sample mass becomes constant. An uncov-
ered porcelain crucible is required to hold the sample during the LOI test and can also be used to contain
the sample during the oven-drying phase to expedite the test. The sample is weighed after the oven-drying
phase and again after the ignition phase. The loss on ignition value is then determined as the percentage of
mass loss during the ignition phase expressed as a percent of the oven-dried 共prefurnace兲 sample mass. The
procedure requires that the time duration in the furnace be at least 15 min, and, if multiple ignition
durations are necessary to reach a constant mass, then subsequent heating periods are to be at least 5 min
in length. There is no maximum time limit for the high temperature phase.
The LOI value is calculated as
Loss on ignition, % = 共A/B兲 ⫻ 100 共1兲

where A is the loss in mass between 105° C and 750° C 共mass of sample after ignition− B兲, B is the mass
of moisture-free sample, and LOI calculations are made to the nearest 0.1 %.
Experiment
Overview
The five factors of LOI variability selected for investigation 共sample size, ignition temperature, ignition
duration, sample cooling method, and length of cooling time兲 were chosen because they were either not
mentioned in the test standard or are allowed to vary through either a given or implied range. Each of these
factors can be controlled with the proper test equipment. The goal of the following experiments was to
understand the individual influence of the five selected factors on LOI results. Separate experiments were
conducted for each test factor where the target factor was isolated and varied while other factors were held
constant. It must be noted that not all factors are independent, for example, the ignition duration 共the
length of time sample must be kept in furnace to reach a constant mass兲 is dependent on both sample size
and ignition temperature 共and possibly furnace type and other related factors兲. While interdependence of
the test factors exists, the experiments conducted for this paper focused on trends in LOI results when only
a single isolated factor was manipulated.
Laboratory Equipment
All experiments were performed in a laboratory equipped with a Fisher Scientific Isotemp 0.14 m3 oven
and Fisher Scientific2 Isotemp 0.03 m3 muffle furnace. Both oven and furnace have digital controls capable
of maintaining internal temperatures within ±1.0° C of the programmed temperature provided the oven/
furnace door is kept closed. Mass measurements were made on a Denver Instrument DI-100 precision
scale precise to 0.1 mg. The standard deviation in LOI for samples tested under like conditions was
0.03 %.
Four glass desiccators, each with glass lid and grease seal, were used as follows: one Pyrex 25 cm
diameter 23 cm tall 共referred to hereafter as “large desiccator”兲, two Pyrex 20 cm diameter 20 cm tall
共“medium desiccators”兲 and one Pyrex 15 cm diameter 15 cm tall 共“small desiccator”兲. A desiccator is an
airtight chamber containing a desiccating agent used to maintain a low humidity environment.
DRIERITE™3 Indicator desiccant, composed of 97 % CaSO4 and able to reduce moisture in 25– 30° C air
1
Note: ASTM Standard C 311-04 LOI procedure for hydraulic cement requires a sample be ignited in a covered platinum crucible at
950° C ± 50° C.
2
Fisher Scientific International Inc., Hampton, NH.
3
W. A. Hammond DRIERITE Co. LTD, Xenia, OH.
HARRIS ET AL. ON ASTM C 311 LOSS ON IGNITION TEST 3
TABLE 1—Crucible number, sample set, and fly ash mass for LOI of samples of varying mass.
Crucible Moisture-free
number Sample set mass, g
1 1 0.50
2 1 0.50
3 2 1.00
4 2 1.00
5 3 1.50
6 3 1.49
7 4 1.99
8 4 2.00
to 0.005 mg/ liter, was used as the desiccating agent. All fly ash samples were ignited in Coors™4 10 ml
glazed porcelain crucibles. The crucibles were handled with tongs and only placed on clean surfaces
throughout the tests to avoid contamination that would alter mass measurements. Time measurements were
recorded to the nearest minute unless otherwise noted.
An infrared imager was used during the cooling experiments to make surface temperature measure-
ments of cooling crucibles. Temperature differences between a crucible and ambient air can cause mass
measurement errors. The imager was used to determine both the length of cooling time of a fresh-from-
the-furnace crucible and the error in mass associated with a given crucible temperature.
The vibrating atoms of the hot crucibles emit electromagnetic waves with frequencies in the infrared
range. The infrared imager detects differences in radiation intensity and maps these on a false color image
for visualization. The imager used in this study was a midrange infrared imager Prism-DS manufactured
by FLIR Systems, Inc. The imager accuracy, as reported by the manufacturer, was the greater of ±2 ° C or
±2 % with a precision of 0.1° C. Digital images produced by the imager included a time print utilized to
compare temperature versus cooling duration. The infrared image or “thermograph” was post processed
using Thermocam Researcher software to correct for emissivity and to determine the average temperature
of the crucibles.
Temperature measurement corrections for emissivity and path radiance are typically made on images
produced by infrared imaging systems. Emissivity is a measurement of the ability of a surface to emit
energy and is equal to 1 for an ideal blackbody and 0 for an ideal reflector. A default emissivity of 1.0 is
used by the infrared imager used in this study. This value was adjusted during post processing to give
accurate temperature readings but was not critical since the temperature of the cooling crucible was
compared to a room temperature crucible with identical surface characteristics. The value for emissivity of
glazed porcelain used in this study was 0.92 关11兴.
Path radiance is the interference of atmospheric aerosols and water vapor in the line of sight between
the object of interest and the infrared imaging system. Matter in this region can both absorb and emit
radiation which is independent of the observation object and is not differentiated by the imaging system.
The influence of path radiance is increased with increased distance between object and imager. At dis-
tances less than 10 m the influence of path radiance is negligible 关11兴. For this study, distances between the
object and imager were less than 2 m.
Two ASTM Standard C 618 Class F fly ashes were used in this study. The ashes are characterized as
having LOI values of 0.6 % and 0.9 %. The ashes are commercially available in Texas and frequently used
in industry.
Study 1. Sample Size

The ASTM Standard C 311 LOI test procedure states that a sample size of 1 g of oven-dried fly ash be
ignited, thus sample sizes ranging between 0.5 g to just under 1.5 g could be used within test specifica-
tions. The following test varied sample size to determine the effect on LOI test results.
Samples: 8 porcelain crucibles containing varying amounts of fly ash. The masses of the oven-dried
samples are shown in Table 1.
Procedure: The samples were ignited at 750° C for 15 min± 0.5 min, cooled in a desiccator for
60 min± 1 min, then weighed. LOI values were calculated for each sample.
4
CoorsTek Inc., Golden, CO.
FIG. 1—LOI of 0.5, 1.0, 1.5, and 2.0 g fly ash samples ignited at 750°C for 15 min.
Results—Figure 1 plots the LOI of each fly ash sample against the sample’s initial moisture-free mass.
A trend of decreasing LOI with increasing sample size is clearly illustrated, although the maximum
difference in LOI is 0.06 %.
Discussion—The decreasing trend in LOI values in Fig. 1 for progressively larger samples suggests
that for a given ignition time larger samples have lower losses. However, the difference in mass loss of the
samples is small enough that they become lost in the precision 共LOI values calculated to the nearest 0.1 %兲
of the test. Perhaps 15 min of exposure to high temperatures was insufficient to react all reactive species
in the 1.50 g and 2.00 g samples as evidenced by the lower average LOI values. If this is so, additional
exposure time would be necessary until the sample mass became constant. The exposure time is addressed
further in Study 3. In summary, variation of the sample mass within the limits allowed by the ASTM test
standard is not a significant source of variability in test results for the ashes studied.
Study 2. Ignition Temperature

ASTM Standard C 311 allows a 100° C variability in ignition temperature 共700– 800° C兲. A test was
performed to determine the effects of ignition temperature variations on LOI results. The following test
varied ignition temperature by 100° C for a range of temperatures spanning 200° C to 900° C.
Samples: 14 crucibles containing 1.0 g oven-dried fly ash.
Procedure: 2 samples were ignited at 200, 300, 400, 500, 600, 700, 800, and 900° C for 15 min
共±0.5 min兲 then cooled in a desiccator for 1 h 共±5 min兲 and weighed.
Results—The results of the varying ignition temperature test are shown in Fig. 2. For the ashes
evaluated here the LOI values increase slowly to 400° C then rapidly between 400° C and 600° C. LOI
peaks at an ignition temperature of 600° C after which it decreases between 600° C and 700° C where it
remains constant up to 900° C.
Discussion—Varying ignition temperatures in the range of 700° C to 800° C does not appear to affect
the LOI results since LOI values remain constant over this region. Two interesting features of the data in
FIG. 2—LOI of fly ash samples ignited for 15 min at temperatures ranging from 300° C to 900° C.
FIG. 3—Variation in LOI with respect to ignition time of four fly ash samples.
Fig. 2 are the increase in LOI corresponding to a loss in mass that occurs between room temperature and
400° C and a maximum value that occurs at 600° C. The loss in mass before 400° C and the gain in mass
between 600° C and 700° C could be explained as the dehydration, decomposition, or oxidation of certain
minerals and volatile compounds referred to earlier. In summary, varying the temperature of the LOI test
within the limits specified by the standard does not contribute significantly to variations in LOI results for
this ash.
Study 3. Duration of High Temperature Exposure

The ASTM Standard C 311 LOI test procedure states that the initial ignition duration be a minimum of
15 min and subsequent ignition periods necessary to achieve constant mass be at least 5 min in length. A
test was done to determine the effects of ignition duration on LOI results. The objective of the following
test was to determine the length of time needed for 1 g samples of ash to reach constant mass and the
affect of prolonged ignition time on LOI results.
Samples: Four crucibles containing 1.0 g of oven-dried fly ash.
Procedure: Samples were ignited at 750° C for an initial 15 min 共±0.5 min兲 period followed by two
5 min 共±0.5 min兲 periods and a final 60 min period. After each ignition period the crucibles were imme-
diately placed in a desiccator to cool for 1 h and then weighed. Values of LOI were calculated for each
mass measurement made.
Results—Figure 3 displays the change in apparent LOI of the four fly ash samples over the ignition
duration. During each ignition period, the initial temperature of the fly ash was room temperature 共ap-
proximately 20° C兲 as it was placed in the oven. As a result, for a portion of the “ignition time” shown in
Fig. 3, the temperature of the fly ash was less than 750° C. Hence, 15 min of ignition time on the chart is,
in reality, somewhat less than this.
Based on Fig. 3, mass loss occurs quickly and is mostly completed after the first 15 min of ignition.
For each of the four fly ash samples, peak LOI values occur after 15 min of ignition and then decreased
slightly by 85 min.
Discussion—The ASTM test standard states that samples be exposed to ignition temperatures until
reaching constant weight. Samples 1, 2, and 4 in Fig. 3 show no change in mass between 20 min and
25 min of exposure. Sample 3 experiences a decrease in mass but the resulting increase in LOI value is
less than the 0.1 %, the required precision. According to the standard and from the viewpoint of the
technician, the test is complete for samples 1, 2, and 4 after 25 min. Whether or not the test is complete for
sample 3 after 25 min is not clear since a change in mass did occur and the precision used for determi-
nation of the test endpoint is not explicitly given in the standard.
Extended exposure to ignition temperatures after a peak LOI value is reached decreases the LOI values
of all four samples. The differences between the peak LOI values and those after 85 min of exposure,
shown in Table 2, vary between 0.01 % to 0.07 %. Changes in the LOI value of one or two-tenths of a
percent is not negligible in some ashes where small changes in LOI correspond to significant changes in
TABLE 2—LOI values of samples after various ignition durations. LOImax is the peak LOI measured, LOI85
corresponds to mass measured after 85 min of exposure to ignition temperatures.
Sample 1,% Sample 2,% Sample 3,% Sample 4,%

LOImax 0.86 0.89 0.92 0.89
LOI85 0.79 0.88 0.88 0.84
Difference −0.07 −0.01 −0.04 −0.05
ash surface adsorption. Whether the “true” LOI value is the peak value or is at some other point in the test
is debatable and is not addressed in this paper. However, for meaningful comparison of LOI values
between laboratories, a standard ignition duration should be established.
Variations in ashes and other factors may affect exposure time. For example, it is the authors’ expe-
rience that the degree of compaction of the sample and the amount of sample surface area exposed to the
air, while difficult to measure, do affect the exposure time required to reach a stable mass. Samples that are
consolidated in the crucible due to tapping the crucible or by compressing the sample with a spatula
require longer ignition times than do samples that are gingerly placed in crucibles in a manner that
maximizes the surface area of the sample.
In summary, the times of exposure to ignition temperatures must be similar for samples that are to be
compared; otherwise the comparison may be invalid. Based on the results of the test shown in Fig. 3, the
author proposes that 30 min of exposure time be established as the test standard.
Study 4. Cooling Method (Countertop versus Desiccator)

Fly ash is hygroscopic and when dry will absorb moisture when left uncovered in moist air. If moisture
from the air adsorbs onto the fly ash surface after removal from the furnace the apparent mass of the ash
will increase and apparent LOI will decrease. While a desiccator can be used to keep the ash dry during the
cooling period between removal from the furnace and weighing the ignited sample, use of a desiccator is
not required in ASTM Standard C 311. The effects of desiccator use on fly ash sample mass and LOI
results were explored in the following experiment.
Samples: Six porcelain crucibles each containing 1 g oven-dried fly ash.
Procedure: Crucibles were ignited in the muffle furnace at 750° C for 2 h ± 5 min. After removal from
the furnace, two crucibles were set on the counter top in an air-conditioned laboratory space, two were
placed in a medium size desiccator with desiccant regenerated at 210° C in accordance with DRIERITE™
specifications 关12兴 and two were placed in a medium desiccator containing exhausted desiccant 共based on
the color of the indicator-type desiccant兲. The crucibles were cooled for 1 h 共±5 min兲 and then weighed,
returned to their cooling locations, cooled for an additional 17 h 共±5 min兲 and weighed again. No cooling
time requirements are stated in ASTM Standard C 311. For each sample, two LOI values were calculated
corresponding to the mass measurements taken during cooling.
Results—Table 3 shows the average apparent LOI of the samples at 1 h and 18 h after removal from
the furnace. The term “apparent LOI” is used because of the influence of post-ignition exposure. After a
single hour, the average apparent LOI values differ at most by only 0.02 %. At 18 h after removal from the
furnace, the range of LOI values has increased to a maximum of 0.09 %. The greatest change in LOI
occurred with the countertop-cooled samples followed by the samples cooled in a desiccator containing
exhausted desiccant. For these two values, an apparent decrease in LOI corresponds to an increase in
sample mass during the cooling period. The samples cooled in the desiccator containing regenerated
desiccant experienced the lowest change in LOI.
TABLE 3—Apparent average LOI of fly ash samples at 1 h and 18 h after ignition.
Apparent Average LOI
Cooling location 1h afterignition,% 18 h afterignition,%

Desiccator, regenerated desiccant 0.53± 0.01 0.54± 0.02
Desiccator, exhausted desiccant 0.51± 0.01 0.48± 0.01
Countertop 0.52± 0.00 0.45± 0.03
Discussion—Mass measurements were not made until the samples had cooled to room temperature.
After 1 h of cooling, the temperature of the samples had equilibrated with the cooling environment.
共Sample cooling is reviewed in depth in the following section.兲 Based on the data in Table 3, the apparent
LOI of the samples is not measurably affected by the cooling environment after a single hour. Thus it
appears that use of a desiccator to protect the sample is not necessary if the sample is to be weighed within
one hour after removal from the furnace.
At 18 h after removal from the furnace, the average apparent LOI value of the countertop-cooled
samples dropped noticeably from 0.52 % to 0.45 %. A drop in LOI corresponds to an increase in sample
mass 共see Eq 1兲. A likely explanation for the gain in mass is the adsorption of moisture from the environ-
ment on the hygroscopic fly ash. A decrease in average apparent LOI is also observed in the samples kept
in the desiccator with exhausted desiccant, though the difference is not as great as that seen in the
countertop samples. A possible explanation for this behavior is that the exhausted desiccant in the desic-
cator did little to remove the moisture from the desiccator air which was then available to interact with the
fly ash surfaces for 18 h. The desiccator seal may have kept additional moisture from entering the chamber
and contacting the fly ash so that the gain in mass was less than that seen with the countertop samples.
When a precision of 0.1 % for LOI calculation is used in accordance with ASTM Standard C 311, the
change in apparent LOI of all the samples tested becomes inconsequential. However, varying fly ash
properties and atmospheric moisture content may affect the rate of moisture adsorption. Since the use of a
desiccator containing regenerated desiccant was shown to control mass gain due to moisture adsorption
after removal from the furnace, its use is recommended.
Study 5. Cooling Time

Chemistry texts state that objects being weighed on precision scales must be weighed at room temperature
to prevent errors due to heat-induced air currents 关13,14兴. During the LOI test, the crucibles are removed
from the furnace at 750° C and a finite amount of time is required for the crucibles to cool to ambient
temperatures. No information regarding sample cooling time is mentioned in the test standard. The fol-
lowing experiments were done to determine 共1兲 the effect of the sample temperature on mass measure-
ment, 共2兲 the cooling time to ambient temperature, and 共3兲 the affect of the use of desiccators on cooling
rate.
Cooling Experiment A: Effect of crucible temperature on mass measurement.
Samples: Two porcelain crucibles containing 1 g oven-dried fly ash and two empty porcelain crucibles
all heated at 750° C for 30 min.
Procedure: The crucibles were removed from the furnace and placed on a countertop to cool at time
zero and then weighed at intervals. A 75 mm tall inverted porcelain crucible was placed on the scale
weighing-pan to protect the pan from high temperatures. The warm crucible was placed atop the inverted
crucible for weighing. The crucibles were weighed at least six times over approximately 30 min. Apparent
LOI values of the ash samples were calculated for each mass measurement.
Cooling Experiment B: Relationship between sample temperature and mass measurement error.
Sample: A porcelain crucible containing 1 g oven-dried fly ash heated in a muffle furnace at 750° C for
30 min.
Procedure: The crucible was removed from the furnace to the countertop to cool. Cooling time
measurements began at the time of removal from the furnace. Over the span of the cooling period, three
measurements were made at intervals: time passed after removal from the furnace, the crucible mass, and
the crucible temperature 共by means of the infrared imager兲. The experiment was ended when the tempera-
ture of the crucible was less than 2 ° C above ambient temperature 共approximately 30 min兲.
Cooling Experiment C: Effect of desiccator on cooling rate.
Cooling crucibles in a desiccator is likely to affect cooling time in comparison to countertop cooling
because the environment is altered. The mass of the desiccator is likely to be a factor due to its capacity
to insulate the hot crucible from ambient air, and the tendency of the glass to absorb heat. The objective
of this test is to determine what affect the desiccator has on the cooling rate of the crucibles.
Samples: Twelve empty crucibles heated to 750° C.
Procedure: At time zero, the crucibles were removed from the furnace and four crucibles each were
placed in large, medium, and small glass desiccators 共shown in Fig. 4兲. The infrared imager was used to
determine the temperature of the crucibles at intervals. To make accurate temperature readings, the lids of
FIG. 4—Three glass desiccators containing cooling porcelain crucibles (a), a thermograph of the desic-
cators during cooling (b), a thermograph of the crucibles inside the center desiccator during cooling (c).
the desiccators were rapidly removed for each thermal image, temporarily changing the cooling environ-
ment. Cooling was observed until the temperature deviation from a room temperature crucible was less
than 3 ° C.
Results—Cooling Experiment A
As shown in Fig. 5共a兲, weighing hot crucibles with or without fly ash immediately after removal from the
FIG. 5—Variation in mass measurement of fly ash samples during cooling (a) and corresponding change
in LOI values (b).
FIG. 6—Changes in sample mass measurement error and sample temperature for 30 min following re-
moval from the furnace (a), sample mass measurement error (as difference in mass measurement from
room temperature) plotted with respect to sample temperature above ambient temperature (b).
furnace causes mass readings to be less than the mass of the samples at room temperature 共sample mass at
60 min after removal from furnace兲. Though small with respect to the mass of the crucible + fly ash
sample, mass error during the first 15 min after removal from the furnace results in the large 共initially
greater than 200 %兲 differences in LOI seen in Fig. 5共b兲.
Cooling Experiment B—Figure 6共a兲 shows the mass measurement error, the difference in mass of the
hot sample to its cooled mass over the cooling period, as well as the sample’s temperature above ambient
temperature. The mass measurement error approached zero at approximately 20 min after removal from
the furnace when the temperature of the crucible was approximately 2 deg above ambient temperatures.
Figure 6共b兲 shows an approximate linear relationship between the mass measurement error and the
difference in temperature between the crucible and its surroundings. This graph shows that as the tem-
perature of the sample approaches ambient temperature, the error in mass measurement approaches zero.
Cooling Experiment C—Figure 7共a兲 shows that the size of the desiccator affects the initial cooling
rates of the samples. The average temperature of the samples in the large desiccator decreased most rapidly
between time zero and 12 min after removal from the furnace. The medium desiccator cooled at a slower
rate and the small desiccator cooled least during the same time period. However, after 35 min, the rates of
cooling and average crucible temperatures were approximately equal in all three desiccators.
Figure 7共b兲 compares the cooling rates of four crucibles in the large desiccator to two crucibles in the
large desiccator. Two crucibles in the desiccator cooled more rapidly than four crucibles in the same
desiccator and the same initial temperatures.
Discussion—The apparent increase in mass of the samples in Fig. 5共a兲 cannot be the result of the
adsorption of moisture since 共1兲 the temperature of the samples in the region of highest mass change is
greater than 100° C, 共2兲 the apparent increase in mass was measured in both the crucible with ash and the
empty crucible, and 共3兲 based on the conclusions from study 4 that negligible moisture is adsorbed during
the first hour of cooling in an unprotected environment. The errors in mass measurements shown in Fig.
5共a兲 are the result of measuring hot samples on a room-temperature scale and support the general lab
FIG. 7—Comparison of cooling rates of four crucibles in large, medium, and small desiccators (a),
comparison of cooling rates of four crucibles to two crucibles in large desiccator (b).
protocol that samples be cooled to ambient temperatures before making mass measurements.
Having established that weighing samples too soon after removal from the furnace can cause signifi-
cant mass and LOI errors, the length of time that must pass to allow sufficient cooling is considered.
Because the precision of LOI values established by the standard is 0.1 %, mass measurements must be
precise to 1 mg for 1.0 g samples. To achieve this required level of precision, and as can be seen in Fig.
6共b兲 it is therefore necessary to cool specimens to 10° C or less above ambient temperature. The time
required to cool the specimen of Fig. 6共b兲 on a countertop from 750° C to within 10° C of room tempera-
ture 共20° C during this test兲 was 8 min. Analysis of the cooling crucible using Newton’s law of cooling
suggests that changes in room temperature of ±10° C have little effect on crucible cooling time for an
initial temperature of 750° C 关15兴.
The use of a desiccator increases sample cooling time in comparison to countertop-cooled samples.
Placing samples in a desiccator immediately after removal from the furnace can increase the total cooling
time to 18 min to 24 min, as shown in Fig. 7共a兲 depending on the size of the desiccator. Figure 7共b兲 shows
that increasing the number of samples cooling within the desiccator can also increase the cooling time
共4 min increase in cooling time for four crucibles compared to two in the medium desiccator.
Conclusions
The following are based on the ashes evaluated in this study:
1. Variation of the sample mass within the limits allowed by the ASTM test standard is not a
significant source of variability in test results.
2. Varying the temperature of the LOI test within the limits specified by the standard does not
contribute significantly to variations in LOI results.
3. The length of time to which samples are exposed to ignition temperatures can cause variations
in test results. Exposure times must be similar for samples that are to be compared; otherwise
the comparison may be invalid. A standard ignition time of 30 min is proposed for all LOI tests.
4. Desiccator use does not affect LOI results if the samples are weighed within 1 h after removal
from the furnace. The use of a desiccator with regenerated desiccant is recommended if the
samples will not be weighed for more than 1 h after removal from the furnace.
5. The difference in temperature between the crucible and room temperature affects weighing
accuracy. To produce LOI results that are accurate to the nearest 0.1 %, crucibles should be
cooled to within 10° C of the room temperature. For the ceramic crucibles used in this study,
sufficient cooling occurs within 10 min for initial specimen and lab air temperatures of 750° C
and 20° C, respectively. The use of desiccators during cooling and the number of samples in the
desiccators can increase cooling time to 25 min or more.
Recommendations for Improvements to ASTM C 311

It is recommended that ASTM C 311 13.1 be modified by establishing an ignition duration of 30 min. The
standard should state that mass measurements may not be made until the sample has cooled to within
10° C of room temperature. Also, the use of a desiccator should be used if the samples will not be weighed
within 1 hr after removal from the furnace.
The authors recommend that the tests performed for this work be repeated with ashes of varying LOI
values in other laboratories to verify or modify the conclusions made herein.
References
关1兴 Helmuth, R., Fly Ash in Cement and Concrete, Portland Cement Association, Skokie, Illinois, 1987.
关2兴 Joshi, R. C., and Lohita, R. P., Fly Ash in Concrete: Production Properties and Uses, Gordon and
Breach Science Publishers, The Netherlands, 1997.
关3兴 Freeman, E., Gao, Y. M., Hurt, R., and Suuberg, E., “Interactions of Carbon-Containing Fly Ash with
Commercial Air-Entraining Admixtures for Concrete,” Fuel, Vol. 76, No. 8, 1997, pp. 761–765.
关4兴 ASTM Standard C 618-03, “Standard Specification for Coal Fly Ash and Raw or Calcined Natural
Pozzolan for Use in Concrete.”
关5兴 Fan, M., and Brown, R. C., “Comparison of the Loss-On-Ignition and Thermogravimetric Analysis
Techniques in Measuring Unburned Carbon in Coal Fly Ash,” Energy Fuels, Vol. 15, 2001, pp.
1414–1417.
关6兴 Brown, R. C., and Dykstra, J., “Systematic Errors in the Use of Loss-On-Ignition to Measure Un-
burned Carbon in Fly Ash,” Fuel, Vol. 74, No. 4, 1995, pp. 570–574.
关7兴 Paya, J., Monzo, M. V., Borachero, M. V., Amahjour, F., and Peris-Mora, E., “Loss on Ignition and
Carbon Content in Pulverized Fuel Ashes 共PFA兲: Two Crucial Parameters for Quality Control,” J.
Chem. Technol. Biotechnol., Vol. 77, 2002, pp. 251–255.
关8兴 ASTM Standard C 311-04, “Standard Test Methods for Sampling and Testing Fly Ash or Natural
Pozzolans for Use in Portland-Cement Concrete.”
关9兴 ASTM Standard C 114-05, “Standard Test Methods for Chemical Analysis of Hydraulic Cement.”
关10兴 Heiri, O., Lotter, A. F., and Lemcke, G., “Loss on Ignition as a Method for Estimating Organic and
Carbonate Content in Sediments: Reproducibility and Comparability of Results,” Journal of Pale-
olimnology, Vol. 25, 2001, pp. 101–110.
关11兴 Holst, G. C., Common Sense Approach to Thermal Imaging, JCD Publishing, Winter Park, Florida,
1998.
关12兴 DRIERITE™ technical data URL: https://secure.drierite.com/catalog3/page19b.cfm
关13兴 Harris, W. E., and Kratochvic, B., Chemical Separations and Measurements: Background and Pro-
cedures for Modern Analysis, W. B. Saunders Company, Philadelphia, 1997, pp. 5–17.
关14兴 Skoog, D., West, D. M., and Holler, F. J., Analytical Chemistry, 6th ed., Saunders College Publishing,
Philadelphia, 1994, pp. 531–563.
关15兴 Incropera, F. P., and Dewitt, D. P., Fundamentals of Heat and Mass Transfer, 5th ed., John Wiley and
Sons, New York, 2002, pp. 8–9.
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Variables Affecting The ASTM Standard C 311 Loss On Ignition Test For Fly Ash

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Article in Journal of ASTM International · January 2006

Nathan Harris Kevin J. Folliard

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Variables Affecting the ASTM Standard C 311 Loss

ASTM Standard C 311 LOI Procedure

Loss on ignition, % = 共A/B兲 ⫻ 100 共1兲

Study 1. Sample Size

Study 2. Ignition Temperature

Study 3. Duration of High Temperature Exposure

Sample 1,% Sample 2,% Sample 3,% Sample 4,%

Study 4. Cooling Method (Countertop versus Desiccator)

Apparent Average LOI

Cooling location 1h afterignition,% 18 h afterignition,%

Study 5. Cooling Time

Recommendations for Improvements to ASTM C 311

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