Instruments for Testing Refractories

Thermal Conductivity Tester – TCT 426

Hot Modulus of Rupture – HMOR 422
Refractories under Load and Creep in Compression –RUL/CIC 421
Pyrometric Cone Equivalent – PCE 428
REFRACTORIES

Today, selection of the proper refractory material is more crucial than The testing of refractories – clearly
ever when it comes to maintaining the cost-effectiveness of a process an essential process – includes the
and prolonging the life cycle. Appropriate selection of the refractory following applications:
furnace lining can only be made with accurate knowledge of the
properties of the refractory materials and the stresses on the materials ∙∙ Characterization of new

∙∙
materials
during service.
Quality control of the process

∙∙∙∙
and the product
Thermomechanical properties are determined using high-temperature
Selection of material
test methods with external forces causing stresses on the tested material.

∙∙∙∙
Prediction of service conditions
The stress-strain behavior of refractories at high temperatures includes
Failure analysis
reversible elastic strain as well as non-reversible time-dependent defor-
Mathematical modeling for
mations. Therefore, the thermomechanical behavior of refractories must
product improvements
be considered as an interaction of stress, strain, temperature and time.

The efficiency of any technical

furnace plant depends – for the
most part – on the quality of the
refractory material and the correct
installation of the furnace lining.
2
NETZSCH Instruments for Testing Refractories under Thermal and Thermomechanical Stress

Thermal and Thermomechanical Stress Instrument Temperature Range

Refractoriness
Refractoriness under Load (RUL)
Creep in Compression (CIC)
Hot Modulus of Rupture
Thermal Expansion (DIL)
Volume Stability (DIL)
Pyrometric Cone Equivalent (PCE) RT to 1700°C
Refractoriness under Load/
RT to 1700°C
Creep in Compression (RUL/CIC 421)
Hot Modulus of Rupture (HMOR 422) RT to 1500°C
Dilatometer
-180°C to 2800°C
(DIL 402 E, DIL Expedis series)

Thermal Stress Instrument Temperature Range

Thermal Conductivity (TCT, LFA)
Specific Heat Capacity (LFA, DSC)
Specific Heat Capacity (LFA, DSC)
Thermal Diffusivity (LFA)
Thermal Conductivity Tester (TCT 426) RT to 1250°C
Laser/Light Flash Apparatus (LFA 427,
-125°C to 2800°C
LFA 457 MicroFlash®, LFA 467 HyperFlash®)
Differential Scanning Calorimeter -150°C to 1400°C
(DSC 404 F1/F3 Pegasus®) (2000°C)
Laser/Light Flash Apparatus (LFA 427,
-125°C to 2800°C
LFA 457 MicroFlash®, LFA 467 HyperFlash®)

International Standards for Testing Refractory Materials

Standard ISO DIN EN ASTM Instrument
Determination of Refractoriness under Load
1893 993-8 RUL 421
(Differential—with Rising Temperature)
Determination of Creep in Compression (CIC) 3187 993-9 C832-00 RUL 421
Determination of Pyrometric Cone Equivalent (PCE) 528 993-12 C24-01 PCE 428
Determination of Modulus of Rupture at Elevated Temperature 5013 993-7 C583-00 HMOR 422
Determination of Thermal Conductivity;
8894-1 993-14 TCT 426
Hot-Wire Technique (cross array: λ ≤ 1.5 W/(m·K))
Determination of Thermal Conductivity;
8894-2 993-15 TCT 426
Hot-Wire Technique parallel: λ ≤ 25 W/(m·K)
Determination of Thermal Conductivity; T(R) technique
C1113-99 TCT 426
(platinum resistance thermometer): λ ≤ 20 W/(m·K)

3
 RUL/CIC 421
 Refractoriness Under Load and
Refractoriness under load evaluates
the behavior of fired refractory bricks
under rising temperature and
constant load conditions.
4
Method
Refractoriness under load (RUL) is
a measure of the resistance of a
refractory product to subsidence when
subjected to the combined effects of
load, rising temperature and time. The
range in which softening occurs is not
identical with the melting range of
pure raw materials, but it is influenced
by the content and the degree of
distribution of low melting point
fluxing agents.
RUL
The RUL test method is described in
ISO 1893, Refractoriness under load
(RUL, differential – with rising temper-
ature). A cylindrical test piece (50 mm
in Ø and height with coaxial bore of
12.5 mm) is subjected to a specified
constant compressive load and heated
at a specified rate until a prescribed
deformation or subsidence occurs.
The deformation of the test piece is
recorded as the temperature increases,
and the temperatures corresponding
to specified proportional degrees of
deformation are determined.
CIC
The instrument can also be used
for the determination of creep in
compression (CIC) as described in ISO
3187. A cylindrical test piece is heated
under specified conditions (see RUL) to
a given temperature. While being held
at that constant temperature, the
deformation of the test piece is
recorded and the percentage change
is evaluated as a function of time.
Creep in Compression
Variable load

Gas outlet

Loading column
Protective tube Heating element
Inner thermocouple Sample
Outer thermocouple Control
thermocouple
Sample with
coaxial bore
Outer tube
and inner tube
Hood type Inner tube
furnace

Supporting Bellows
column
Vacuum-tight seal

Variable
Gastight contact force
casing

Evacuating
Inductive
system
transducer

Gas inlet

Schematic of the gas-tight RUL/CIC 421 G/6 for

measurements in protective gas atmosphere

Measuring Unit – Specimen Signal Generation – Expansion

The measuring unit consists of a console, furnace
guide frame, furnace (max. 1700°C), balance
weight of the loading device (max. 1000 N)
and a differential measuring system. To prevent
chimney effects and to guarantee a sufficient
zone of constant temperature, the furnace is
closed at the top. The test piece is placed on the
supporting column; the furnace is lowered and
load is applied by counterbalancing (minimum
of 100 cN increments) the weight of the furnace.
Thermocouples serve to control the furnace
and to determine the test piece temperature.
The length change is transmitted by a measuring
system consisting of an inner and outer tube which
act differentially. These tubes made of alumina are
connected to an inductive transducer. Its signal
is amplified and stored after A/D conversion.
The thermal expansion of the tubes is self-
compensating. Therefore, only the expansion of
that part of the inner tube which corresponds to
the test pieces must be considered. The differ-
ential measuring system can be used to measure
the length change of the test piece through its
center bore (ISO/DIN) or along the outside.

5
RUL/CIC 421
Test Atmosphere
Measurements can be carried out
in static air (basic version) or using
an optional device for inert gas
n for purge within the test piece area.
t i g h t versio
Gas- oxyge
n-
testing pecimens
ve s
sensiti
Testing Carbon-Containing
Materials
For testing carbon-containing
materials (e.g., magnesia-carbon
graphite bricks), a reducing test
atmosphere can be realized with
a gas-tight test chamber (optional;
see figure on previous page). This
chamber can be evacuated and
then purged with protective gas.
Measurements can be carried out
up to 1600°C.
Variable Loading Device
Optionally, the loading device can
be equipped for load variation.
The preload can be up to 300 N
and the verifying load can be
applied in the range from 0 N to
700 N at a rate between 0.3 N/s
and 3 N/s.
6
Test Piece Dimension
Generally, the same test piece
dimensions of 50 mm in diameter
and 50 mm in height are used for
both the RUL and the CIC test. For
the high-precision differential
measuring system used in deter-
mining expansion and defor-
mation, the cylindrical test piece
has a coaxial bore of 12.5 mm.
The ground faces should be plane,
parallel and perpendicular to the
axis of the cylinder (ISO/DIN).
Other test piece dimensions are
also possible (e.g., 36 mm, GOST
4070-20000). The hood-type
furnace with counterweights
ensures reproducibility of the
selection and application of load
to the test piece.
Sample Preparation
Machines
NETZSCH offers the following
machines for the appropriate
preparation of optimum
test pieces:
∙∙∙∙
Drilling machine 421/11
∙∙
Grinding machine 421/12
Sawing machine 421/13
 Peak: 1387.0 °C
Evaluation Routines for 0.8
0.8
Peak: 1387.0 °C

RUL and CIC 0.6

0.6
0.8
Peak: 1387.0 °C

0.4
The upper plot shows a RUL 0.4
0.6

/%/%
measurement (differential) on a 0.2

dL/L0
0.2
0.4
test piece of a fireclay brick with

dL/L0
0.0
increasing temperature. At 1387°C,
dL/L0 /%
0.0
0.2
the test piece reaches its maximum -0.2
expansion. Deformations of 0.5% -0.2
0.0
dLmax = 0.724 %
and 1.0% occurred at 1565°C -0.4
T(dLmax) = 0.724
dLmax 1387.0%°C
-0.4
-0.2
(T0.5) and 1600°C (T1), -0.6
T 0.5
T(dLmax) 1564.7 °C
= 1387.0
1.0
T 0.5 1599.8 °C
= 1564.7
respectively. -0.6
-0.4 dLmax
T 1.0
= 0.724 %
= 1599.8 °C
T(dLmax) = 1387.0 °C
0 T 0.5 200
= 1564.7 °C 400 600 800 1000 1200 1400 1600
-0.6 0 T 1.0 200
= 1599.8 °C 400 600 Temperature/°C
800 1000 1200 1400 1600
Temperature/°C
Refractoriness
0 200
under400
Load; test600
conditions:
800
0.2 N/mm²,
1000
5 K/min,
1200
static air1400 1600
Temperature/°C

1.0
1.0

Peak: 1283.0 °C
1.0
0.8 Peak: 1283.0 °C
The lower two plots depict a CIC 0.8
measurement on a test piece of a
/%/%

Peak: 1283.0 °C
silica brick. The upper of these two 0.8
0.6
dL/L0

0.6
dL/L0

shows the dynamic heating

dL/L0 /%

segment and the lower one shows 0.6

0.4
the time-scaled creep at a constant 0.4
temperature of 1280°C.
0.4
0.2
0.2

0.2
0.0
0.0 200 400 600 800 1000 1200
200 400 600 800
Temperature/°C 1000 1200
0.0 Temperature/°C
200 400 600 800 1000 1200
Temperature/°C

cr (0.00, 1.00) = 0.063 %/h

cr (0.00, 1.00)
10.00) = 0.063
0.019 %/h
0.70 15.00) = 0.019
0.015 %/h
cr (0.00, 10.00) dLmax = 0.729 %
0.70 20.00) = 0.013
cr (0.00, 15.00) 0.015 %/h
cr (0.00, 1.00) = 0.063 %/h T(dL max) = 0.729
dLmax 1283.0%°C
25.00) = 0.011
cr (0.00, 20.00) 0.013 %/h T(2.5max)
T(dL h) = 1283.0
1280.4 °C
0.65 cr (0.00, 10.00) = 0.019 %/h
0.70 (0.25) 25.00) = 0.011 %/h
cr (0.00, ISO h) = 1280.4 °C
T(2.5
0.65 cr (0.00, 15.00) = 0.015 %/h dLmax = 0.729 %
cr (0.25) = 0.011 %/h Z 0.00 = 0.000 %
ISO
cr (0.00, 20.00) = 0.013 %/h T(dL max) = 1283.0 °C
0.60 cr (0.00, 25.00) = 0.011 %/h 5.00 = 0.136
Z 0.00 0.000 %
T(2.5 h) = 1280.4 °C
/%/%

0.65
0.60 10.00 = 0.136
Z 5.00 0.191 %
cr (0.25) = 0.011 %/h ISO
15.00 = 0.191
Z 10.00 0.228 %
dL/L0

Z 0.00 = 0.000 %
0.55 20.00 = 0.228
Z 15.00 0.258 %
dL/L0

0.60 Z 5.00 = 0.136 %

0.55 25.00 = 0.258
Z 20.00 0.282 %
dL/L0 /%

Z 10.00 = 0.191 %
Z(5.25)
Z 25.00 = 0.146
0.282 %
0.50 Z 15.00 = 0.228 %
Z(5.25) = 0.146
0.55 Z 20.00 = 0.258 %
0.50
Z 25.00 = 0.282 %
0.45 Z(5.25) = 0.146
0.50
0.45
0 5 10 15 20 25
0.45 0 5 10 Time/h 15 20 25
Time/h
0 5 10 15 20 25
Creep in Compression; middle: heating segment at a heating rate of 5 K/min;
Time/h
bottom: isothermal creep at 1280°C, 2.5 h in static air

7
RUL/CIC 421
Applications
Refractoriness under Load 0.8

(RUL) of Andalusite Bricks 0.6

This plot shows three measure- 0.4

ments on andalusite bricks fired at 0.8
three different temperatures: 0.2
Expansion/%

1430°C, 1470°C and 1510°C. At 0.6

approx. 1425°C, the test piece 0
reaches its maximum expansion. 0.4
After sample or calibration curve -0.2
Firing at T0.5 T1 T2
correction, the software calculates 0.2 (°C) (°C) (°C) (°C)
Expansion/%

the characteristic T0.5, T1 and T3 -0.4 1430 1625 1675 >1700

temperatures from the RUL tests 0

1470 1650 1695 >1700

where 0.5%, 1% or 3% shrinkage -0.6 1510 1670 >1700 >1700

is reached after the maximum -0.2

T0.5 T1 T2
Firing at
expansion. The influence of the -0.8 (°C) (°C) (°C) (°C)
0 200 400 600 800 1000 1200 1400 1600 1800
firing temperature can be -0.4 1430 1625 1675
Temperature/°C
>1700
clearly seen. 1470 1650 1695 >1700
RUL behavior of andalusite
1510 bricks
1670 >1700 >1700
-0.6
(approx. 65% Al2O3) fired at
three different temperatures; test
-0.8 conditions: 0.2 N/mm2, 5 K/min,
0static air200 400 600 800 1000 1200 1400 1600 1800
0.7 Temperature/°C

0.6
Expansion/%

0.5

Creep in Compression (CIC)

0.7
0.4

of Andalusite Bricks 0.6

0.3
Expansion/%

0.5
Test pieces of the andalusite bricks 0.2 Firing at (°C)
fired at different temperatures are 1430
0.4
used for CIC tests. In these tests, 0.1 1470
the load is applied once the 1510
0.3
temperature is reached (here, at 0
0 5 10 15 20 25
1425°C). This is contrary to RUL 0.2 Firing at (°C) Time at 1425°C/h
tests, where the load is applied 1430
from the very beginning of the 0.1 1470
measurement. This plot only 1510
shows the time-scaled creep at 0
constant temperature (the heating 1.5 0 5 10 15 20 25
segment is not depicted). Time at 1425°C/h
1.0

RUL behavior of andalusite bricks (approx. 65% Al2O3) fired at three different
0.5 temperatures; test conditions: 0.2 N/mm2, 5 K/min, static air, 25 h at 1425°C
Expansion/%

1.5
0.0

8 1.0
-0.5
 0.8

Key Technical Data

0.6

0.4

0.2
Expansion/%

0 RUL/CIC 421
-0.2
Firing at T0.5 T1 T2
Model RUL/CIC(°C)421 E/6
(°C) (°C) (°C) General Data
-0.4 1430 1625 1675 >1700
Temperature range RT1650
to 1700°C Test piece Ø 50 mm, height 50 mm
1470 1695 >1700
1510 1670 >1700 >1700
-0.6
Heating elements 4 Super-Kanthal 1800 1 N to 1000 N;
Load range
steps of 1 N to 100 N
-0.8
0 Static air;
800 optional inert
Test200 400
atmosphere 600 1000 1200 1400 1600
Max.1800
stress 0.5 N/mm2
purge gas
Temperature/°C

20 mm; resolution
Safety switch Failure of test piece Measuring range
4,000,000 steps

Measuring system Differential

0.7 Model RUL/CIC 421 G/6
Digital resolution 5 nm
0.6 Temperature range RT to 1600°C
Thermocouples Type B
Heating elements 4 Super-Kanthal 1800
∙∙
Expansion/%

0.5
Electronics : 230 V/70 A/
Power Supply

∙∙
50 Hz; max 15 KW
0.4 Protective tube Al2O3 Electronics
Furnace: 230 V/10 A/50 Hz
0.3 Ability to evacuate Up to 10-2 mbar
∙∙Measuring unit: ≈ 1200 mm x

∙∙
610 mm x 2400 mm
0.2 Firing at (°C) Static/dynamic air and Dimensions
Test atmosphere Control unit: 562 mm x
1430 inert gas 555 mm x 1183 mm

∙∙∙∙
0.1 1470
1510 Failure of test piece, Measuring unit: ≈ 480 kg
Safety switches Weights
0 cooling water Control unit: ≈ 220 kg
0 5 10 15 20 25
Time at 1425°C/h

1.5
Quality Control of Castable
1.0 Refractories by RUL Tests
0.5 Castables are mixed with water
Expansion/%

and then installed by either

0.0 pouring or pumping. These
measurements were carried out on
-0.5 finished construction parts.
Castables have to be prepared
-1.0 exactly as instructed by the product
Lab Test
manufacturer. Field tests show that
Product 1; poor result
-1.5 the product depicted here by the
Product 1; good result
red sample curve was improperly
-2.0
0 200 400 600 800 1000 1200 1400 1600 1800
handled. The divergent shrinkage
Temperature/°C behavior (as compared to the
green test pieces) causes failures in
RUL test as quality control for a finished construction part the finished product.

9
 RUL/CIC 421
Software

State-of-the-Art Software Including Various Evaluation Routines

∙∙ Graphic and tabulated results,

calculated according to ISO/DIN
∙∙
Possibilities for temperature
control (max. 96 isothermal or
∙∙
Determination of relative length
changes at preset times

∙∙ ∙∙
dynamic temperature program
Correction of the measured steps) Calculation of creep rates in

∙∙
data by calibration curves preset time intervals

∙∙ ∙∙
Presentation of the measuring
Determination of characteristic values temperature- or time- Simultaneous analysis of up to
data according to user’s require- scaled for RUL and time-scaled 8 curves/temperature segments
ments for CIC (curve comparison)

∙∙ Automatic softening point

detection
∙∙
Determination of the absolute
maximum in the length
∙∙
Calculation of single values,
physical and technical

∙∙
dilatation spectrum (RUL) expansion coefficients

∙∙ ∙∙
Derivation of curves for deter-
mination of the temperature- Determination of the sample Calculation and graphic display
or time-dependent linear temperature 2.5 h after start of of the 1st and/or 2nd derivative,
expansion rates isothermal phase (CIC) peak determination

10

The RUL/CIC runs under
Proteus® software on
Windows® for the fully
automatic test run, data
acquisition, storage and
off-line evaluation.
∙∙Semi-automatic routines for the
determination of reaction steps
as extrapolated onset, point of
inflection, peak, peak end
∙∙Output or ASCII file export of
the corrected measuring data
∙∙Graphic export
∙∙Data transfer of the sample
length from an
external gauge (optional)
PCE 428
Pyrometric Cone Equivalent
Test Bench for Determination of the Pyrometric
Cone Equivalent (Refractoriness) PCE 428
Because of the heterogeneity of their composition and structure,
ceramic refractories do not exhibit a uniform melting point. The
refractoriness is characterized by the optical determination of the
pyrometric cone equivalent (according to Seger); i.e., the tempe-
rature at which the tip of a cone made of the sample material
softens to the point that it touches the base plate. Reference
cones with well-established pyrometric cone equivalents at
temperature intervals of 10°C and above (designated SK xx or ISO
xxx) are heated along with test cones made of the sample material
in the same furnace, so that it is possible to make an accurate
comparative temperature determination for the softening point
of the refractory material to within approx. 20°C.
The NETZSCH PCE 428 test bench has a mechanical lever which
positions the base plate for the sample and reference (“Seger”)
cones in the hood furnace from below; a viewing window in the
furnace lid with a radiation filter and surface mirror allows for
visual determination of the pyrometric cone equivalent. The
maximum temperature for this melting point determination is
1700°C (complies with SK 31, ISO 170), in accordance with DIN EN
993-12. The furnace is equipped with a single temperature
controller.
11
TCT 426
 Thermal Conductivity Tester
Knowledge of a refractory material’s
thermal conductivity is crucial
when it is being used for the
lining of industrial equipment.

Low values are required where heat

losses engineering are to be kept to
a minimum (insulation), while high
values are necessary for materials
in areas where the transfer of heat
is important (e.g., the control of
hot surface temperatures).

Thermal conductivity (λ with the unit

W/(m·K)) describes the transport
of energy – in the form of heat –
through a body of mass as the result
of a temperature gradient. It is thus
a material-specific property used for
characterizing steady heat transport.

The NETZSCH TCT 426 operates

according to the hot-wire method
using three possible techniques:

∙∙∙∙
Cross-Wire Technique

∙∙
Parallel-Wire Technique
T(R) Technique
Cross-Wire and Parallel-Wire Technique
The only internationally standardized method for the determination of the thermal conductivity of refractory
and heat insulating materials at elevated temperatures is the hot-wire method (ISO 8894). The hot-wire method

∙∙∙∙
is a dynamic, absolute method based on the measurement of the temperature increase:
of a linear heat source (hot wire); cross-wire technique: λ ≤ 2 W/(m·K) or
at a certain location at a specified distance from a linear heat source; parallel-wire technique: λ ≤ 20 W/(m·K).

Both the hot wire and thermocouple are embedded between two test pieces which form the test assembly. The
increase in temperature as a function of time, measured from the moment the heating current is switched on, is
a measure of the thermal conductivity of the test pieces.

Cross-Wire Technique Parallel-Wire Technique

t2 r2
U · J In ( t1 ) U · J Ei ( 4·a·t )
λ = –––––– · –––––– λ = –––––– · ––––––––
4 · π · I T2 - T1 4 · π · I Ti (t) - Tr

T2 14
50 5
12
ΔT -0.15
40 ΔT(2t) 4
10
T1
λ in W/m·K

30 8 3
ΔT in K

ΔT in K

ΔT in K

λ -0.1
ΔT(t)
6
20 2
4 -0.05

10 1
2

0 0
1 10 t1 100 1000 t2 0 500 t 1000 2t 1500 2000
Time in s Time in s

Schematic diagram: Cross-wire technique, Schematic diagram: Parallel-wire technique,

equation and signal equation and signal

13
 TCT 426 Advantages of the T(R) Technique

∙∙No “focal-point” temperature measurement on the

hot wire as in the cross-wire technique; i.e., there
is compensation for the influences on the signal
T(R) Technique caused by inhomogeneities of the test piece (e.g.,
large pores).

The “Platinum Resistance Thermometer Technique”

is described in ASTM C1113. An integral temper-
∙∙No heat transmission through the legs of the
thermocouple, which are perpendicular to the hot
ature measurement is carried out over the length wire (cross-wire technique) – and therefore, no
of the hot wire between the voltage taps. Here, falsification of the monitored temperature increase.
the hot wire itself functions as both heat source
and temperature sensor. The temperature increase
of the hot wire is determined from its change in
∙∙Higher evaluation range in the temperature/time
diagram. Here, the feedback from the edge of the
resistance; calculation of the thermal conduc- test assembly is detected by the temperature sensor
tivity is the same as for the cross-wire technique. later than in the parallel-wire technique due to the
axial arrangement of the hot wire.

T(R) Technique: λ ≤ 15 W/(m·K) ∙∙The application field ranges from approx.

0.03 W/(m·K) for such materials as aerogels up to
approx. 15 W/(m·K) for magnesia bricks – main-
taining the temperature range from RT to 1250°C.

Measuring Inserts Interchangeable by the

Operator

The hot wire and thermocouples are affixed to a

measuring frame made of Al2O3 which is mounted
onto the carrier. The frame is adjustable to various
heights allowing for the three measuring arrange-
ments: the cross-, parallel- wire and T(R) technique.
The voltage taps to the hot wire are embedded in
t2
U · J In ( t1 ) the test assembly. The software-controlled power
λ = –––––– · –––––– is held constant electronically. Except for the T(R)
4 · π · I T2 - T1
technique, the temperature change is measured
relative to a reference thermocouple (the position
depends on the technique in use).
T2
50

40 Measuring Unit with Motorized Sample Lift

T1
λ in W/m·K

30 The measuring unit consists of the furnace, the

ΔT in K

carrier system for the test assembly, and a motor-

20 driven hoist to raise the carrier into position inside
the furnace. The carrier system and hoist are
10 arranged in a console. The upper part of the carrier
system (made of insulating material) is mounted
1 10 t1 100 1000 t2 between two telescopic guides. It can be pulled
Time in s out of the console when in its lowered position
and raised by the hoist for easy positioning of the
Schematic diagram: T(R) technique,
equation and signal test assembly.

14
 10
High alumina brick Refractory Testing by the
Parallel-Wire and T(R) Techniques

Magnesia brick In this example, the thermal

conductivities of different
Thermal Conductivity/W(m·K)

refractory materials were

measured using the parallel-
0
Fire clay brick wire and T(R) techniques. Nearly
Parallel-wire technique identical results were obtained
T(R) technique by the two techniques. Of course,
due to the variances in compo-
sition, different room-temper-
Calcium silicate ature values and temperature
dependencies were measured
0.1 for the different materials.
200 400 600 800 1000 1200 1400
Temperature/°C

Operation
Special Arrangement for Materials with
Carbon Content
All aspects of operation are easy, from placing the test
pieces on the carrier to arranging the hot wire and For measuring carbonaceous bricks using the parallel-
thermocouples in the test assembly. Plug-in connec- wire or T(R) technique, an outfit is available for a brick
tions also allow the measuring frame to be changed (max. 230 x 115 x 76 mm in size) and four sheathed type
out quickly. After the test assembly is prepared, the K thermocouples. The outfit contains, among other
carrier is raised into the furnace. The measurement is elements, one set of platinum wire with two-hole capil-
controlled by the software. laries and insulating tubes to prepare the hot wire with
voltage taps and current leads. The thermal conduc-
tivity of carbon-containing bricks can be measured up
Special Arrangements for Bulk Materials, Powders to 1000°C. The technique is not standardized. Possible
and Ground Materials reactions between the hot wire and sample may occur.
However, carbon-containing materials can also be
For determining the thermal conductivity of bulk easily tested using the laser flash method (LFA). LFA
materials with the T(R) technique, a muffle case allows for tests in a temperature range above 1000°C;
(volume approx. 4.5 l) made of Al2O3 is available. This the measurement setup averts reactions between the
muffle case consists of two rectangular frames of 250 specimen and LFA parts (see page 18).
x 125 x 11 mm along with one bottom plate and one
top plate of 250 x 125 x 11 mm each.

Features
n-
i t y o f Carbo
uctiv 00°C
e r m a l Cond ks up to 10
Th ri c
ining B
Conta

15
 TCT 426
Software

∙∙
Measurement methods: Parallel and cross-wire. Optional thermometer
resistance technique T(R); the parallel-wire and T(R) methods can be
combined in a single measurement

∙∙
Database-oriented saving of series of shots with their material
properties, definable with a maximum of 6,000 signal points per shot
at intervals of 0.1 s or greater

∙∙
Definition of any number of temperature levels and shots per level;
insertion, deletion and annexation of temperature segments

∙∙
Parameter window and three online graphs for equilibrium phase/hot
wire signal, temperature increase and calculated λ values in [W/(m·k)]

∙∙
Online evaluation of the running measurement

∙∙
Comparative analysis of up to 16 series of shots from the same
database

∙∙
Calculations can be carried out in the automatic, manual or NRL
(non-linear regression) mode

∙∙
Ability to average shots at the same temperature level

∙∙
Approximation of shots as a curve via various mathematical functions
(splines, polynomials, etc.)

16
 TCT 426

Method Hot-wire, absolute method

Furnace type Rectangular chamber-hood type

Heating elements 12 Super-Kanthal pins

Insulation Aluminum silicate fiber

Heating and cooling rates 0.01 K/min to 5 K/min

Temperature range RT to 1250°C (max. working temperature range 1500°C)

Temperature measurement ∙∙∙∙

Type S thermocouples
Type K for muffle box

Atmosphere Static air

Construction of carrier system

Multilayered, insulating structure
assembly

Operation area 300 mm x 200 mm

Sample supporting plate 196 mm x 200 mm

Max. three test pieces

NF1: 230 mm x 115 mm x 65 mm
Test assembly
NF2: 250 mm x 123 mm x 65 mm
Two test pieces: 230 mm x 114 mm x 76 mm

Motorized sample lift Yes

Measuring frame Al2O3

∙∙∙∙
Cross-wire technique: λ < 2 W/(m·K)

∙∙
Parallel-wire technique: λ < 20 W/(m·K)
Measuring techniques /
T(R) technique: λ < 15 W/(m·K)
thermal conductivity ranges
→ Frames are adjustable to different test piece sizes
→ Interchangeable measuring inserts

Measuring range 50, 500, 5000 μV

∙∙∙∙
Software-controlled, continuously adjustable power in two zones
Hot-wire power control Range: 0.1 to 5 W; 1 to 50 W
Resolution: 104 digits

Muffle case for special materials ∙∙Muffle case for measurements on dielectric powders or granular

∙∙
materials, volume ≈ 4.5 l
(optional)
Muffle case for measurements on carbonaceous materials

International standards ISO 8894-1, ISO 8894-2; DIN EN 993-14, DIN EN 993-15, ASTM C1113-99

Weights and dimensions ∙∙∙∙

Measuring unit: 1750 mm x 740 mm x 640 mm; 280 kg
Control unit: 1180 mm x 560 mm x 542 mm; 150 kg

Regulating and power unit

Two separate circuits: 1 x 230 V, 10 A; 1 x 230 V, 23 A
electrical connections

Key Technical Data

17
 Thermal Diffusivity and
Specific Heat Capacity
Laser/Light Flash Analysis –
An Alternative Method for Refractories

For decades, thermophysical properties (thermal diffu-
sivity [a], specific heat capacity [cp], and thermal
conductivity [λ]) have been determined using sta-
tionary methods (e.g., guarded hot plate technique) or
standardized transient techniques such as the hotwire
method according to ISO 8894 (TCT 426). However,
these methods are time-consuming and limited to
large sample sizes and materials of low thermal
conductivity.
Light/Laser Flash methods (LFA) are absolute,
non-contact measurement techniques and can handle
high thermal conductivity materials without any
difficulties. Modern LFA systems often also allow for
simultaneous measurement of the specific heat
capacity so that thermal conductivity can be deter-
mined, without additional measurements, per the
following formula:
λ(T) = a(T) · ρ(T) · cp(T)
In addition, the rapidity of the flash methods allows
for testing on a larger number of samples (up to
25.4 mm in Ø).
Precise determination of the thermal diffusivity is
offered by the NETZSCH LFA 427, LFA 457 MicroFlash®
and LFA 467 HyperFlash® systems.

LFA 467 HyperFlash®

LFA 457 MicroFlash®

LFA 427

18
LFA Measurements on Three Brick Samples with Silicon Carbide Content

The thermal diffusivity of even 2.0 8 5

#1
inhomogeneous samples can be #2 7
measured with the LFA. This

Conductivity /(W/(m·K)

Heat Capacity /(J/g·K)

4

Diffusivity /(mm2/s)
#3
example depicts LFA measure- 1.5 6
ments on three brick specimens 2.0 8 5
#1
with silicon carbide content (#1, 5
3
#2 7
#2 and #3) cut from the same

/(W/(m·K)

Specific/(J/g·K)
brick. The tests were conducted in 1.0 #3 4 4
/(mm2/s)

1.5 #1 6
the temperature range between
Thermal

#2 2
3

Thermal
20°C and 1400°C. In addition to

Specific Heat Capacity

#3 5

Thermal Conductivity
Thermal Diffusivity

3
the measured thermal diffusivity 0.5 2
(red curves) and specific heat 1.0 #1 4 1
#1
capacity (black curves), the plot #2
#3 1
#2 2
also shows the calculated results 3
#3
for the thermal conductivity (blue 0.0 0 0
0.5 0 200 400 600 800 1000 1200 1400 2
curves). Only very minor deviations #1 1
Temperature /°C
are observed within one specimen. #3
#2 1
Thermal diffusivity, thermal conductivity and specific heat capacity of
a brick containing 45% Al O , 29% SiO2 and 25% SiC; three specimens
0.0 cut from the same brick. 2 3 0 0
0 200 400 600 800 1000 1200 1400
Temperature /°C

9
K)

TCT 426
Magnesia Spinel Brick 8
LFA 427 #1
K)/(W/(m·K)

LFA 427 #2
/W/(m

7
LFA 427 #3
9
Magnesia alumina spinel brick is 6 Average
Conductivity

widely used in the transition TCT 426 ±10%

Conductivity

(LFA/TCT)
8
zones of cement rotary kilns, glass 5 LFA 427 #1
/(W/(m·K)

LFA 427 #2
/W/(m

tank regenerators and lime kilns. 7

4 LFA 427 #3
Elevated kiln capacity and the Average
Thermal

6
Conductivity

increasing use of alternative fuels 3

Thermal
Thermal Conductivity

(LFA/TCT) ±10%
present a challenge to basic 5
2
refractories for the burning zone
of cement rotary kilns. When 4
1
using alternative fuels, thermal 3
Thermal

stress can be caused by local 0

overheating in the first lining 2 0 200 400 600 800 1000 1200 1400 1600

zones. This has a weakening Temperature /°C

1
effect on the microstructure of
the brick. This plot compares TCT 0
and LFA thermal conductivity 0 200 400 600 800 1000 1200 1400 1600
results for a magnesia spinel Temperature /°C
brick. Over the entire measu-
Magnesia spinel brick made of 85% MgO and 12% Al2O3.
rement up to 1450°C, all results
are within the range of ± 10%.

19
 HMOR 422
High-Temperature
Bending Strength Tester
Determination of the Hot Modulus of Rupture HMOR 422 Models

NETZSCH offers two HMOR

The hot modulus of rupture (HMOR) is an important parameter in the models:

∙∙
characterization of refractories. Along with other thermophysical
properties, the maximum load at high temperatures plays a significant HMOR 422 D/3 for continuous
role in the quality control and development of furnace linings. operation up to 1500°C and a
maximum load of 5000 N with
optional devices for:
∙∙∙∙
Load and deformation tests
Constant deformation rate

∙∙HMOR 422 E/4 for 4-point

measurements up to 1450°C

Method

The Modulus of Rupture is defined

as the maximum stress a rectan-
gular test piece of specific dimen-
sions can withstand in a 3-point
bending test until it breaks,
expressed in N/mm² or MPa.

Standard and Test Piece

Dimensions

The international standard test

method is described in ISO 5013.
The test piece dimensions are
150 mm x 25 mm x 25 mm.
Up to 30 samples can be loaded
onto the sliding rails and
measured in succession.

20
HMOR 422 D/3

The HMOR 422 D/3 is designed

Loading
for continuous testing in 3-point device
bending to determine the Sliding
weight
modulus of rupture of refractories
up to a temperature of 1500°C
under a maximum load of 5000 N Furnace
Transport chamber
(60 N/mm²). The test pieces – mechanism
heated to a predetermined Sliding
temperature – are transported rails
to the pressure rod on sliding
rails made of Al2O3, and their
positioning is precisely controlled.
An increasing load is then applied
continuously until failure occurs;
the load at failure is recorded.
Upon completion of the test, the Schematic diagram of the high-temperature bending strength tester 422 D/3
broken test piece is transported including a detailed view of the 3-point bending device with support width of 125 mm
out of the furnace and falls into
a waste bin.

Measurement of Load and

Deformation – HMOR 422 D/3/G
Sliding
weight
with Pressure Measuring Cell
Driving
unit In the standard version (HMOR
422 D/3), the sliding weight stops
at breakage, the force is read on the
scale and the bending strength is
calculated.
Pressure
cell Optionally, deformation of the test
piece can be recorded as a function
of the increasing load. For this set
Inductive
displacement up, the pressure measuring cell is
transducer required.
Reference
rod

Inductive
displacement
Measurement at Constant Deformation Rate – HMOR 422 D/3/G transducer

Loading column
The measuring unit can be equipped with a driving unit for a constant
deformation rate. In this optional version, the sliding weight is fixed in Refrence rod
the 2500 N position and the downward movement of the loading
column is controlled by the driving unit. The load is monitored by a
pressure cell. Both load and deformation (displacement transducer) Test piece
are recorded. The data can be used for the calculation of stress/strain
curves and Young’s modulus for elastic deformation.

21
 HMOR 422

HMOR 422 E/4 – Recording of Load Loading device

and Deformation
Sliding weight
The HMOR 422 E/4 performs bending
strength measurements on test pieces
with dimensions of 45 mm x 4.5 mm x Split shell furnace
3.4 mm. In contrast with the 422 D/3 Test piece
model, deformation of the test piece is
here measured at the bottom via a
differential measuring device. The
internal tube comes into contact with
the bottom of the test piece and the
external tube is attached to the bottom Differential measuring system
flange of the 4-point bending device as
a reference point. The split shell furnace
(max. 1450°C) is hinged and opens for
easy insertion of the test piece. The HMOR 422 E/4 with detailed view of the 4-point bending device
loading device is the same as that used
for the 422 D/3.

Comprehensive HMOR Software

∙∙∙∙
Graphic interface (MS Windows)
Integrated HELP system
∙∙ Following measurement, option to select
specimen files, calculate the load at
∙∙
Transfer of specimen dimensions via the
external gauge (optional)
failure or modulus of rupture and transfer
to MS EXCEL
∙∙
Predefinition of a measurement run for
up to 32 specimens, with the option of
∙∙ Determination of modulus of rupture
at elevated temperatures with
adapting the parameters and extending measurement of specimen deformation
to a maximum of 64 specimens while the
experiment is in progress
∙∙ Presentation of the results in a single
graph
∙∙∙∙
Control of the temperature program
Determination of modulus of rupture
∙∙ Continuous recording of test data until
specimen failure is detected; saved with
∙∙
Start of load increase until specimen failure
is detected ∙∙
the test parameters
Determination and storage of calibration
∙∙
Display and storage of results, temperature,
maximum load (at the moment of ∙∙
curve (optional)
Transfer of measured data to MS EXCEL
specimen failure) and test parameters and option to calculate Young's modulus

22
Key Technical Data
HMOR 422 D/3 HMOR 422 E/4

Bending mode 3-point 4-point

Temperature range RT to 1500°C RT to 1450°C

Chamber furnace with

Furnace Swing-open furnace
pre-heating zone

Thermocouples Type S Type S

Mode of operation Continuous Single measurement

Test piece dimensions 150 mm x 25 mm x 25 mm 45 mm x 4.5 mm x 3.5 mm

Distance between support edges 125 mm 40 mm

Distance between
N/A 20 mm
bending edges

Loading device with

∙∙∙∙
Weighing lever
Load range:
∙∙∙∙
Weighing lever
Load range:

∙∙ ∙∙
0 ... 500 ... 1250 ... 2500 ... 5000 N; 0 ... 500 ... 1250 ... 2500 ... 5000 N;
movable weight
Load rate: Load rate:
4 speeds (2, 4.2, 8, 12 N/s) 4 speeds (2, 4.2, 8, 12 N/s)

Inductive system with Differential measuring

Measurement deformation
reference rod (optional) system (standard)

Measuring range Max. 10 mm Max. 5 mm

Digital resolution 2.5 nm 1.25 nm

Constant deformation rate Optional N/A

Load rate 10 ... 2000 μm/min N/A

Measuring unit dimensions 2200 x 1800 x 870 mm; 540 kg 2100 x 1600 x 750 mm; 430 kg

Control unit dimensions 1120 x 565 x 452 mm; 250 kg 1120 x 565 x 452 mm; 250 kg

23
 HMOR 422
Applications
Quality Control – Modulus of Rupture of a Kiln
Furnace Product
The HMOR yields information on the maximum stress a rectan-
gular test piece can withstand prior to bending when it is tested
in a three-point bending device. The deformation under
increasing load (stress-strain curve) can additionally be measured
using the optional load and deformation device.

The test results on three kiln furnace products below clearly show
that the average modulus of rupture decreases by a factor of
nearly two between 1100°C and 1300°C. Scattering in the data
of the samples at the same temperature is most likely due to
inhomogeneities in the material.

kiln furniture product A kiln furniture product C

1300°C 1200°C 1100°C 1300°C 1200°C 1100°C

40 45
35 40
35
HMOR/(N/mm2)

HMOR/(N/mm2)

30
25 30
25
20
20
15 15
10 10
5 5
0 0
1 6 11 16 21 26 31 1 2 3 4 5 6 7 8 9 10 11
sample no. sample no.

kiln furniture product B mean values

1300°C 1200°C 1100°C Produc A Product B Product C

40 40
35 35
HMOR/(N/mm2)

30 30
HMOR/(N/mm2)

25 25
20 20
15 15
10 10
5 5
0 0
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 1100°C 1200°C 1300°C
sample no. temperature

24
 TEST PIECE PREPARATION
Depending upon user needs, a variety of accessory
machines is available for the preparation of test
pieces for each instrument, as follows:

Machine Required for

Column-type drilling machine RUL/CIC 421

Column-type grinding machine RUL/CIC 421 HMOR 422

Test piece grinding machine (200 mm cup) RUL/CIC 421 HMOR 422 TCT 426

Stone sawing machine RUL/CIC 421 HMOR 422 TCT 426

Stone cutting machine TCT 426

25
 Column-Type Drilling Machine

The NETZSCH column-type drilling machine is used for drilling cylindrical test pieces
from refractories, stone, ceramics or products similar to ceramics.

The drilling machine is a sturdy boxtype construction with a complete casing for all
rotating parts. The drilling table can be swung 360° to include the water-protective
case. In addition, it has a working table light incorporated and infinitely variable
speed control for the drilling spindle via a V-belt control system. The water-protective
case, two clamping angles to hold the workpiece and a water-flushing box with
plug MK2/B16 (without drills) are included.

Various drills are available for the outer diameter of the test piece:

∙∙∙∙Diamond hollow drill, outer Ø 30 mm, inner Ø 25 mm, drilling depth 100 mm

∙∙∙∙
Diamond hollow drill, outer Ø 42 mm, inner Ø 36 mm, drilling depth 100 mm
Diamond hollow drill, outer Ø 56 mm, inner Ø 50 mm, drilling depth 100 mm
Diamond hollow drill, outer Ø 08.4 mm, inner Ø100 mm, drilling depth 120 mm

To fulfill DIN/ISO standards, these drills for the inner coaxial bore are also available:

∙∙∙∙Diamond hollow drill, outer Ø 12 mm, inner Ø 7 mm, drilling depth 100 mm
Diamond hollow drill, outer Ø 12.5 mm, inner Ø 7.5 mm, drilling depth 100 mm

Column-Type Grinding Machine

The column-type grinding machine with swingable grinding head and precision
grinding spindle for mounting cup grinding wheels (Ø 125 mm) is available for the
preparation of test pieces used for RUL/CIC and HMOR measurements. The vertical
fine adjustment has a reading accuracy of 0.01 mm. The permanent magnet plate
(Ø 125 mm) is designed for clamping steel support devices. The wet grinding
device consists of a cooling agent vessel with a clearing tank, an electric immersion
pump, and a water-collection plate with a plate slide, cock and hose line. A
ceramic cup grinding wheel (Ø 125 x 60 x Ø 20 mm) is included. Clamping devices
and grinding wheels include:

∙∙∙∙
Clamping device for holding test bodies, Ø 100 mm, height 25 mm
Clamping device for machining one test body, Ø 50 mm, height 50 mm, with

∙∙
reducing clamp rings for Ø 35.7 mm and Ø 30 mm
Cup grinding wheel made of a ceramic compound for soft to medium- hard test

∙∙
pieces, Ø 125 mm, height 60 mm, hole 20 mm
Diamond cup grinding wheel for special hard ceramic materials, Ø 125 mm,
hole 32 mm, coating width 5 mm, coating height 2 mm, grain size Ø 100 mm

∙∙
for rough grinding
Diamond cup grinding wheel for special hard ceramic materials, Ø 125 mm,
hole 32 mm, coating width 5 mm, coating height 2 mm, grain size Ø 30 mm
for finish grinding

26
Sawing Machine for RUL/CIC, HMOR and TCT Systems

The NETZSCH sawing machine is used for cutting test pieces from refractories, stone,
ore, ceramics, glass and hard metals.

The circular blade cuts from bottom to top, plunging into the cooling agent tank
below the table and drawing the cooling agent into the cut over the shortest path.

The sawing machine consists of a plate (700 x 600 mm) with spindle for cutting
wheels of Ø 200 mm to 350 mm, a pole-reversible three-phase motor with motor
protection and foot switch revolutions of 3500 min-1 and 1750 min-1, and a feed
table. In addition, it comes with a clamping device, yoke support, prism support with
column, stop angle and guide pulley for automatic feed. Included are also a swing
and spindle along with hand bar and counter weight (with angle support). There is
a two-jawed vise that can be both turned and swung, and a three-jawed vise that
can be turned.

We offer two cutting wheels for the sawing machine:

∙∙Diamond wheel (Ø 200) mm made of a bronze compound,

∙∙
cutting width 1.5 mm, max. cutting depth 45 mm, hole Ø 30 mm
Diamond wheel made of a bronze compound (Ø 350) mm,
cutting width 1.8 mm, max. cutting depth 120 mm, hole Ø 30 mm

Stone Cutting Machine

For mounting the wire slots in the bottom of brick test pieces, a stone cutting
machine is available for the TCT 426. The machine includes one diamond cutting
disk (Ø 125 mm x 1 mm thick) and one diamond cutting disk (Ø 125 mm x 0.3 mm
thick). The supply voltage is 230 V / 50 Hz.

ource!
ro m one s
All f

27
 The NETZSCH Group is a mid-sized, family-owned German company
engaging in the manufacture of machinery and instrumentation with
worldwide production, sales, and service branches.

The three Business Units – Analyzing & Testing, Grinding & Dispersing and
Pumps & Systems – provide tailored solutions for highest-level needs. Over
3,400 employees at 210 sales and production centers in 35 countries across
the globe guarantee that expert service is never far from our customers.

When it comes to Thermal Analysis, Calorimetry (adiabatic & reaction) and

the determination of Thermophysical Properties, NETZSCH has it covered.
Our 50 years of applications experience, broad state-of-the-art product line
and comprehensive service offerings ensure that our solutions will not only
meet your every requirement but also exceed your every expectation.

NGB · Refractory Materials · EN · 0717 · NWS · Technical specifications are subject to change.

NETZSCH-Gerätebau GmbH
Wittelsbacherstraße 42
95100 Selb
Germany
Tel.: +49 9287 881-0
Fax: +49 9287 881 505
at@netzsch.com