You are on page 1of 6

RHI Bulletin > 2 > 2013, pp.

44–49

Olaf Krause, Gerhard Urbanek and Hartmut Körber

Determining Resistance to Abrasion at Ambient


Temperature—Improving Comparability Between
Laboratories
To gain a deeper understanding of how highly accelerated particles affect the surface of a
refractory material during service, two test methods, ASTM C704 and EN ISO 16282, were
established. When performed as described, the tests provide informative data regarding
material abrasion, although it became evident there was a lack of interlaboratory comparabili-
ty. In order to enhance reproducibility, the latest revisions of ASTM C704 in 2009 and 2012
resulted in a more rigid definition of the testing device. However, this paper proposes a dif-
ferent route to perform blast abrasion tests that generates highly reproducible abrasion val-
ues even if the tests are performed in different laboratories. The key to obtaining consistent
values is that prior to the test the pressure supply for the blast gun must be adjusted until
the abrasion value of a standard float glass sample is 9.3 cm3 ± 0.3 cm3 using 1000 g of SiC
particles. The results of a round robin test performed at 10 laboratories with 6 different types
of refractory material confirmed that this alternative method increases interlaboratory test
reproducibility and is sufficiently robust to recommend revision of the current standards.

Introduction ASTM C704M - 09 in 2009. In this update the blast gun and
venturi system dimensions were defined in more detail and
Refractory resistance against abrasion is a key issue for
a new clause was added that describes known factors that
many industrial furnace applications where particle-loaded
affect the results. The findings in this clause are based on
gas jets are expected during the process. For example, they
a ruggedness test performed using float glass samples.
occur in furnaces for the petrochemical industry, waste
incineration, coal-fired power plants, and in steel reheating
pusher furnaces.
Pressure gauge

In the past, two test methods to evaluate abrasion resis­


tance were established, namely ASTM C704 first published
in 1972 and EN ISO 16282 published in 2008. More precisely
EN ISO 16282 is derived from the older ASTM C704 - 01
with minor editorial and technical changes. Basically the
tests determine the volume (cm3) of material abraded from
the flat surface of a sample positioned at right angles to a
nozzle through which 1000 g of size-graded SiC grain is
blasted by air at a defined air pressure using a blast gun
and venturi system (Figure 1). The bulk density, B, of the
Air supply
sample material is determined prior to the test by measur-
ing the sample weight, M1, and volume. The sample is also
weighed after the test, M2. The abraded volume loss, A, is
Venturi housing
calculated using the equation:
Venturi nozzle
A = (M1 – M2)/B (1)
Abrasive supply
Whilst the procedure generates reliable and reproducible
results within a single laboratory, when the values are com-
pared between different laboratories they show significant
and repeated deviations. This imprecision has led to unjus-
tified complaints from refractory user industries when a
third-party laboratory crosschecked the specified values for Glass tube and
abrasion resistance. The economic impact resulting from metal stabilizing
the test variability can be considerable for both refractory sleeve
producers and consumers.

To improve the reproducibility, the ASTM Committee C08


on Refractories revised ASTM C704 - 01 and published Figure 1. Schematic diagram of a blast gun and venturi system.

44 <
RHI Bulletin > 2 > 2013

Statistically significant effects were reported if the inside the designated abrasion value of 9.3 cm3 ± 0.3 cm3 for this
diameter of the inlet air nozzle and the air pressure were material, the standard air pressure is altered, which is con-
not as defined in the standard. In the latest revision ASTM trary to the established standards where the pressure is fixed
C704M - 12, published in 2012, precision of the apparatus at 4.5 bar. Using the new method, the apparatus setup details
setup was further defined. Supplementary requirements for are of secondary importance. A number of tests were per-
highly abrasion-resistant materials were also added. The formed to examine various aspects of this approach in detail,
major task of this clause is to more precisely describe the including a round robin test that clearly demonstrated cali-
testing conditions that are attained, for example by mount- brating the system on the basis of a defined abrasion value
ing additional pressure gauges. It is evident from the inclu- provides reliable data to examine abrasive wear of refractory
sions that the ASTM Committee C08 is heading toward a materials.
more rigid definition of the apparatus dimensions, espe-
cially the particle acceleration system. Preliminary Examinations
Prior to the round robin test, investigations were undertaken
Main Factors Influencing Abrasion to understand how variable air pressures and different
During the Test amounts of abrasive material affect the results. In addition,
The refractory material volume loss is dependent principally an alternative material (i.e., B4C) was used for the nozzle
on the impact energy that is discharged when highly accel- tube.
erated SiC particles hit the sample surface. It is proportional
to both the particle velocity and weight (i.e., grain size). Air Pressure Influence
Therefore, only narrow SiC grain distributions are suitable In this preliminary test performed at two laboratories, boro-
for the test. It is also necessary to examine the grain size silicate glass samples from a European producer with a bulk
distribution within one batch if disintegration effects are density of 2.22 g/cm3 were abraded at predefined air pres-
obvious. In addition, the particle surface plays a role. The sures between 3 and 6 bar. All the other parameters were
particles should have angular, jagged edged surfaces and kept constant and in accordance with the procedure
therefore only be used once. The general grain shape can described in ASTM C704M - 09.
be checked by measuring the bulk density.
The results show there is a linear ascending correlation
Many factors affect the particle velocity during acceleration. between the volume loss and increasing air pressure over
Of major importance is the standard air pressure provided the measured range (Figure 2). However, the measurements
to the venturi system and both standards specify 4.5 bar. from the two laboratories have a different slope, indicating
However, particle acceleration inside the blast gun is not a slightly different setup of the testing devices. For example,
only dependent on the pressure but also on the chamber if an abrasion value of 7.4 cm3 is required, the air pressure
dimensions inside the blast gun and the specific dimen- must be adjusted to approximately 5.50 bar at Laboratory
sions of the venturi nozzle. The latter is described in detail A and 4.56 bar at Laboratory B.
in ASTM C704M - 09. However, for as long as ASTM C704
has existed, a simple but essential problem has been dis- Influence of the Abrasive Material Amount
cussed among those applying the standard outside the US: and Nozzle Tube Material
The specified blast gun is not available in Europe. More­
In the subsequent evaluation, borosilicate float glass samples
over, since 2009 the ASTM has stated that the described
from the European producer detailed above and standard float
blast gun is the only one permitted.
glass samples as recommended by ASTM C704M - 09 were
abraded with different amounts of SiC (i.e., 800–1200 g).
After the particles have been accelerated in the venturi
chamber, they pass through a glass tube with strictly
defined dimensions (i.e., length and diameter). Due to vari­
able surface roughness, the specific material used to manu-
facture the tube can cause different friction effects and may 10.0
decelerate the SiC grains to a greater or lesser degree dur- n Laboratory A
9.0 n Laboratory B
ing their passage through the tube. Since 2007, these and
additional factors known to affect the results have been
8.0
listed in ASTM C704, but without any quantification. y = 2.1255x - 2.2325
Abrasion [cm3]

R2 = 0.99439
7.0
In summary, the evolving standards have defined the test
conditions and the apparatus setup more and more strictly 6.0
y = 1.5113x - 0.8143
in order to get better interlaboratory reproducibility. How- R2 = 0.98207
5.0
ever, as a result it has become more difficult to assure the
apparatus achieves the predefined conditions and the 4.0
method has become more error-prone. Therefore, this
paper presents an alternative solution that is much easier to 3.0
perform and leads to highly reliable results. It proposes 3 4 5 6
deregulating the apparatus setup specifications but defining Air pressure [bar]
a preliminary step and adjusting the gas pressure to
achieve defined abrasion of a float glass test specimen,
Figure 2. Linear relationship between borosilicate glass plate vol-
described as the calibration standard in ASTM C704. This
ume loss (cm3) and the air pressure (bar) used to accelerate the
material, broadly used as a reference standard, is particu- abrasive particles. The results were derived in two independent
larly suitable because it is highly homogenous. To obtain laboratories.

> 45
RHI Bulletin > 2 > 2013

Two sets of tests were performed, one with conventional deeper pits with a smaller eroded area at the surface, namely
glass nozzle tubes and a second with abrasion resistant B4C the blast jet appeared to be more focused. However, the
nozzle tubes. Each test was repeated twice with the same slope of all the tests was very similar. Therefore, it can be
tube. All other parameters were kept constant and in accord- concluded that the nature of the blast jet is of minor impor-
ance with the procedure described in ASTM C704M - 09, for tance for reproducibility of the method, if the air pressure or
example the predefined air pressure was 4.5 bar. All tests the amount of abrasive material is the adjustable parameter.
were performed using the same abrasion tester.
Interlaboratory Study—Round Robin Test
In all the tests performed, the abrasion loss showed a strict
As previously described, the performance and reproducibility
linear correlation with the amount of SiC used over the
of the standard test methods according to ASTM C704 or ISO
measured range (Figure 3). Therefore, the amount of SiC
16282 are highly dependent on the particle size and velocity
can also be used to standardize the abrasion tester. For this
before they hit the sample surface. Therefore, it is very diffi-
approach, the mass of SiC has to be adjusted until the mea­
cult to reproduce the precise test conditions defined in the
sured abrasion value is equivalent to the standard value of
standards. As the preliminary test results described above
9.3 cm3 ± 0.3 cm3, as defined in ASTM C704M - 09 for the clearly show, the abrasion loss is significantly and systemati-
reference float glass plate. cally controlled by the air pressure, which generates the SiC
particle acceleration in the venturi system. The round robin
The linear correlation between the amount of SiC used and test was performed to examine the interlaboratory reproduci-
the abrasion level indicates that materials with a low abra- bility of the test when performed according to ASTM C704M
sion resistance (> 20 cm³) can be tested using a decreased - 09 and how the reproducibility is affected if prior to testing
amount of SiC (e.g., 500 g instead of 1000 g). This would the air pressure is adjusted until the abrasion value of a
reduce the possibility of blasting through the sample. Fur- standard ASTM float glass sample is 9.3 cm3 ± 0.3 cm3.
thermore, abrasion values obtained using a different amount
of SiC can be used to determine the equivalent values for
Round Robin Test Setup
1000 g SiC.
In the round robin test, 6 different shaped and monolithic
In addition, Figure 3 clearly demonstrates that the actual refractories were examined in 10 laboratories. The materials
abrasion values measured are influenced by the nozzle tube were selected with the aim of covering a wide range of
material used. For example, the B4C tubes typically led to abrasion values (i.e., 5–30 cm3). Table I details the refractory
higher abrasion loss than the conventional glass tubes. How- materials tested.
ever, it was also evident that B4C tubes increased the repro-
ducibility of individual measurements since the results from
Sample Bulk density Refractory type Abrasion
repeat tests had the same linear regression. In contrast, the
(g/cm3) (cm3)
results obtained using glass tubes showed variations of up
A 2.15 Fireclay FC40 brick 30
to 2% for the same test conditions. As a result of the stan­
dard glass tube erosion after a single test, this nozzle type B 3.00 Alumina-chromia ACr80/5 brick 15
must be changed after every test whilst the B4C nozzles C–D 3.15 Magnesia-chromite MCr50 brick 7
have the advantage that they can be used approximately E 3.00 Sintered magnesia based brick 15
100 times because the erosion rate is very low. F 2.20 Conventional refractory concrete 8
G 2.80 Ultra low cement castable 5
When the erosion pits were examined after the test it was
evident that the blast jet slightly differed according to the Table I. Overview of the refractory materials examined in the
tube type. For example, the B4C tubes typically produced interlaboratory test, including the approximate abrasion value.

Prior to the round robin test, the various material samples


12.0
AS1 AN1 were cut or cast to meet the regulations defined in ASTM
11.0 AS2 AN2 C704M - 09 and ISO 16282. To determine the homogeneity
ES3 EN3 of the samples, they were examined using the impulse exci-
10.0
ES4 EN4
Abrasion [cm3]

9.0
tation technique (IET) and ultrasonic measurements were
also performed in three dimensions. The results of these
8.0
tests enabled the dynamic Young’s modulus to be calcu-
7.0 lated and compared (Figure 4). Determining this material
6.0 property was important because the abrasion resistance is
highly dependent on the homogeneity of the test samples.
5.0
This is exemplified by the series of fireclay brick FC40 sam-
4.0 ples (i.e., refractory sample A) that were examined in one
800 900 1000 1100 1200
laboratory and show that the abrasion resistance is strongly
SiC [g] dependent on the sonic velocity (Figure 5). A scatter in the
sonic velocity of ≤ 10% for any refractory sample set was
Figure 3. Linear relationship between the volume loss (cm3) and
amount of SiC abrasive (g) accelerated using a constant air pres-
regarded as admissible for the round robin test.
sure of 4.5 bar. Standard float glass (A/continuous lines) and boro-
silicate glass (E/dashed lines) samples were tested using standard A preliminary result at this stage in the investigation was
glass nozzle tubes (S/blue lines) and B4C nozzle tubes (N/red lines). that determining the sonic velocity is a powerful tool to
All the conditions were measured twice without changing the
tube. The repeat measurements determined with B4C tubes were evaluate the abrasion resistance of a single refractory mate-
very close; therefore, only a single regression line is visible. rial type, for example material A.

46 <
RHI Bulletin > 2 > 2013

For the round robin test, every laboratory was instructed to air pressure was adjusted to attain an abrasion value of
follow the same procedure. Initially, a test run was performed 9.3 cm3 ± 0.3 cm3 with ASTM standard glass samples.
with the standard ASTM float glass plates using the test con-
ditions defined in ASTM C704M - 09 (i.e., at a fixed air pres- In summary, 10 laboratories examined 6 different refractory
sure of 4.5 bar). The measurements were repeated multiple materials under standard conditions and with the adjusted
times. Since the samples were highly homogeneous, the air pressure. Typically, three glass plates were necessary to
results obtained were particularly useful to examine the inter- adjust the air pressure to within the tolerance range. In addi-
laboratory reproducibility. Duplicate refractory samples (see tion, the standard glass plates were tested at least 4 times.
Table I) were then examined under the standard test condi- The results were evaluated with the PROLab Plus (QuoData
tions. Subsequently, a second series of duplicate tests was GmbH, Germany) software, which is in accordance with ISO
performed on standard ASTM float glass plates and the six 5725-6:1994. The results and precision statistics are detailed
different refractory materials. However, prior to the tests the in Table II.

Abrasion resistance test Sample Average abrasion SR Sr R r


(cm )
3
(%) (%) (%) (%)
ASTM C704M - 09 A 30.857 14.11 11.9 39.51 33.31
B 14.518 26.72 26.72 74.81 74.81
C 7.902 62.65 7.96 175.42 22.29
D 7.62 34.9 2.48 97.72 6.93
E 13.859 31.5 5.73 88.2 16.04
F (mould side) 6.284 28.25 79.1
G (mould side) 5.054 30.74 86.06
Standard float glass 8.998 28.25 1.87 79.1 5.24
Average 31.48 8.19 88.15 22.92
Adjusted air pressure A 33.911 7.05 2.52 19.74 7.06
(sample yields 9.3 cm3 ± 0.3 cm3)
B 12.872 23.31 23.31 65.27 65.27
C 7.72 9.45 6.57 26.46 18.4
D 6.93 19.86 1.82 55.6 5.08
E 12.841 9.18 5.47 25.71 15.32
F (mould side) 8.56 22.01 7.94 61.63 22.24
G (mould side) 5.304 23.85 4.31 66.78 12.06
Standard float glass 9.266 1.72 1.57 4.82 4.4
Average 14.81 7.54 41.46 21.1

Table II. Results of the round robin test conducted at 10 laboratories on the 6 refractory samples detailed in Table I and standard float
glass samples. The abrasion tests were conducted according to ASTM C704M - 09 or using the modified test procedure where the air
pressure was adjusted so a standard float glass sample had an abrasion value of 9.3 cm3 ± 0.3 cm3. Abbreviations include standard
deviation of reproducibility (SR), standard deviation of repeatability (Sr), reproducibility interval (R), and repeatability interval (r).

90 3300
Median
Dynamic Young´s modulus [MPa]

80 25%–75% 3200
70 Range without
Sonic velocity [m/s]

outlier
3100
60 Outlier
50 3000
40
2900
30
2800
20
10 2700
A B C D E F G 22 24 26 28 30 32 34 36 38
Refractory type Abrasion [cm3]

Figure 4. Box plot of the dynamic Young’s modulus determined Figure 5. Approximate linear relationship between the abrasion
using the impulse excitation technique. The results are shown loss and sonic velocity for six different fireclay brick FC40 sam-
for the six different refractory materials detailed in Table I, name- ples (i.e., refractory type A) within the range defined.
ly fireclay FC40 brick (A), alumina-chromia ACr80/5 brick (B),
magnesia-chromite MCr50 brick (C and D), sintered magnesia
based brick (E), conventional refractory concrete (F), and an ultra
low cement castable (G).

> 47
RHI Bulletin > 2 > 2013

Round Robin Test Results Refractory Materials

Standard Glass Samples The refractory material abrasion results from the round
robin test are summarized in Table II. Whilst the data
The round robin abrasion results for the standard ASTM
shows that calibrating the equipment by adjusting the air
float glass material are shown in Figure 6. The mean
pressure only slightly enhances the repeatability (Sr)
empirical value was 9.294 and the tolerance limits were
within laboratories (i.e., 7.54% compared to 8.19%), it is
fixed at 8.620 and 9.992 cm3, which corresponds to a
clearly evident that this procedure significantly decreases
Zu-score of < 2.00. With a single exception, only the abra-
the standard deviation between laboratories (SR). Across
sion values determined after calibrating the equipment by
all the tested samples, the average relative standard devia-
adjusting the air pressure fell within the statistical tolerance
tion between laboratories was more than halved from
limits. The scatter of results in a single laboratory is indi-
cated by the boxes. Laboratory 5 showed the widest scat- 31.48% to 14.81%. Furthermore, the results clearly show
ter. On further examination, it transpired that this labora- that the abrasion testers are capable of producing reliable
tory had specific problems with fluctuations in the air pres- and consistent results.
sure supply that were solved by installing a pressure ves-
sel. In summary, when the standard glass material abrasion If only the results of the standard glass plates are consid-
results from all the laboratories were combined it was clear ered, the enhancement achieved by adjusting the air pres-
that calibrating the equipment by adjusting the air pressure sure is profound. While the standard deviation for all the
significantly reduces the scatter of results (Figure 7). sample types between laboratories was improved by a fac-
tor of 2, the highly homogenous glass plates really dem-
onstrate the improvement, namely the relative SR was
0 12 decreased almost 20 fold from 28.25% to 1.72%. This
clearly indicates that the gas adjustment method can pro-
11 duce very precise results and that the heterogeneity
between refractory samples is the limiting factor.
Tolerance threshold (9.992 cm3)
10
Average
Abrasion [cm3]

When compared to the round robin test results published


9 in ASTM C704M - 09, the advantages of the gas adjust-
Tolerance threshold (8.620 cm3) ment method are also evident from the average relative
8 standard deviations between laboratories for the plate
glass plates, namely 16.27% using the ASTM test and
7 1.72% for the improved method reported in this paper.

0
L1 L2 L3 L4 L5 L6 L2 L1 L3 L10 L5 L9 L7 L8 L9 L7
Conclusions
st st st ad ad ad ad ad ad ad st ad ad ad st st The round robin test was performed using a broad range
Laboratory
of shaped and unshaped refractory materials that had
diverse blast abrasion resistances (i.e., 5–30 cm3). The
Figure 6. Round robin abrasion results for standard ASTM float
glass material. The tests were performed at 10 laboratories major outcome of this work is that to provide interlabora-
according to ASTM C704M - 09 with a fixed air pressure (st) or tory comparability it is better to adjust the air pressure of
using the modified test procedure where the air pressure was the venturi system and calibrate the equipment with
adjusted so a standard float glass sample had an abrasion value
of 9.3 cm3 ± 0.3 cm3 (ad). The triangles indicate measured
respect to the abrasion rate of a standard float glass sam-
results. ple rather than define rigid regulations for the apparatus
setup as recommended by ASTM C704M - 12. When the
air pressure was adjusted in this manner the overall stan­
dard deviation between laboratories was reduced by a fac-
0 tor of 2 when refractory materials were tested (i.e., SR
Median
25%–75% decreased from 31.48% to 14.81%) and by a factor of 20 if
12
Range without outlier only the results of the standard glass samples are consid-
Outlier
ered (i.e., SR decreases from 28.25% to 1.72%). The poorer
Abrasion value [cm3]

11
precision regarding the refractory materials can be attri­
10 buted to the heterogeneity inherent in the samples. Sonic
velocity measurements prior to the abrasion test can help
9
identify outlier samples. The SR can also be positively
influenced by multiple measurements due to enhanced
8
repeatability.
7
Over the measured range, the refractory material abrasion
0 loss showed a linear correlation with the air pressure and
Standard Adjusted the amount of abrasive used. Therefore, these parameters
can be adjusted over a broad range without a significant
Figure 7. Box plot of all the standard glass sample measure- decrease in the precision of the method. However, it is
ments performed at the 10 laboratories according to ASTM important to note that the air pressure supply should be
C704M - 09 with a fixed air pressure (standard) or using the checked carefully. Temporary pressure fluctuations caused
modified test procedure where the air pressure was adjusted
so a standard float glass sample had an abrasion value of by an insufficient air supply will cause poor repeatability
9.3 cm3 ± 0.3 cm3 (adjusted). and deliver in most cases lower values.

48 <
RHI Bulletin > 2 > 2013

The linear correlation between the amount of SiC used and


the abrasion values indicates that materials with a low
abrasion resistance (> 20 cm³) may be tested with an alter-
native amount of SiC (e.g., 500 g instead of 1000 g). This
would reduce the possibility of blasting through the sample
as well as avoid swirling of the SiC particles in deeper
holes. The abrasion values obtained using a different
amount of SiC can be used to recalculate the values equiv-
alent to abrasion with 1000 g SiC.

The test results also showed that the use of abrasion-resis­


tant materials for the venturi nozzle are beneficial to pro-
duce constant operating conditions during the test and that
tubes made of B4C can be highly recommended. Further-
more, if the air pressure is appropriately adjusted, highly
abrasion resistant refractory materials can be effectively
examined.

The study findings will be relayed to the national and inter-


national standardization boards for evaluation. Changes to
the current version of ISO 16282 will be proposed and dis-
cussed by the ISO Technical Committee (i.e., ISO/TC 33
Refractories) and the European Committee for Standardiza-
tion (i.e., CEN/TC 187) during forthcoming meetings.

Authors
Olaf Krause, University of Applied Sciences Koblenz, Höhr-Grenzhausen, Germany.
Gerhard Urbanek, RHI AG, Technology Center, Leoben, Austria.
Hartmut Körber, Deutsches Institut für Feuerfest und Keramik GmbH, Höhr-Grenzhausen, Germany.
Corresponding author: Gerhard Urbanek, gerhard.urbanek@rhi-ag.com

> 49

You might also like