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Thermocouple thermometry

June, 2014
Dr. Yong-Gyoo Kim
Center for Thermometry,
Division of Physical Metrology
Korea Research Institute of Standards and Science
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Part I. Heat and Temperature


1. Unit and Scale of Temperature
2. Heat Transfer and Thermal Properties

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1. Unit and scale of Temperature

Lord Kelvin
Ludwig Boltzmann

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1.1 What is temperature ?

Temperature

Degree of hotness or coldness of objects


intuitively

Exactly, level of thermal energy (kT)

k : Boltzmann constant

Kinetic energy due to a microscopic motion of


particles, energy due to phonon

mv2 = kT

Phonon: quantum mechanical description of an


elementary vibrational motion

Heat is caused from the vibration of particles

Temperature is a quantitative description of this


vibrational motion.

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Some examples of temperature


Temperature

Kelvin

Degrees Celsius

100 pK

273.149 999 999 900 C

Triple point of water

273.16 K

0.01 C

Suns visible surface

5,778 K

5,505 C

Lightening bolts channel

28 kK

28,000 C

Suns core

16 MK

16,000,000 C

Thermonuclear weapon peak temperature

350 MK

350,000,000 C

Core of a high-mass star on its last day

3 GK

3,000,000,000 C

CERNs proton vs nucleus collisions

10 TK

10 1012 C

1.4171032 K

1.4171032 C

Coldest temperature achieved

Universe 5.3911044 s after Big Bang

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The first thermometer


In 1594, G. Galilei
A type of gas thermometer
Volume change with temperature

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1.2 Unit of temperature


International unit: K or oC
Absolute thermodynamic scale : Kelvin, K
degree Celsius (oC)
Common and practical unit
1 oC = 1 K
K = 273.15 + oC

Non SI unit
Fahrenheit scale: oF
In Europe and USA
oF = oC x 9/5 + 32

Rankine scale: oR
Chemical engineering in USA
oR = K x 9/5

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degree Celsius (oC)

A. Celsius (Sweden ) in 1742

Ice point : 100 oC

Water boiling point : 0 oC

Divided into 100 parts

In 1744, M. Strmer

After Celsius passed away

Reverse the two fixed point value

Ice point :0 oC, boiling point : 100 oC

Currently used with Kelvin internationally

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Kelvin, K

For a reversible Carnot engine,


Heat efficiency is proportional to temperature

Q2 T2
=
Q1 T1
Absolute temperature ,T, is defined as above.
For ideal gases,
PV = constant x T
At T = 0, volume of gas should be zero.

For real gases, extrapolated volume goes to zero


(T = 0 K).
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Volume vs Temperature (Charles Law)

T[K]

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1.3 Temperature scale


Before 1954, Celsius scale used
Ice point and boiling point of water

After 1954, thermodynamic scale used


Triple point of water (TPW) was defined as definition of
temperature scale
TPW
273.16 K

Definition of temperature scale


The unit of thermodynamic temperature, the kelvin,
symbol K, is defined as the fraction 1/273.16 of the
thermodynamic temperature of the triple point of
water
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Triple point cell of Water

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History of temperature scale

ITS-27

ITS-48

Current temperature scale

PLTS-2000

Down to TPW of H2 (13.81 K)


11 fixed-points
Change of interpolation equation of standard thermometer

ITS-90

Change of Ag fixed-point value


Change of interpolation equation of pyrometer
Include several secondary fixed-points

IPTS-68

Boiling point of oxygen (-182.970 oC) ~ radiation thermometer range


6 fixed-points

Down to 0.9 mK

Mise en Pratique of Kelvin (MeP-K)

Current definition of Kelvin

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Classification of thermometers

Primary vs. Secondary

Primary : Clear equation of state

Measurement of thermodynamic temperature

Secondary : Temperature-dependent parameter (voltage, current, length, etc)

Resistance thermometer, thermocouple, etc.

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Standard vs. Industrial thermometer


Standard : Realization of temperature scale

Gas thermometer
Vapor pressure thermometer
Standard platinum resistance thermometer
Pyrometer

Industrial : Except for the standards


Thermocouple, Glass thermometer, Thermistor, etc

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2. Heat Transfer and Thermal Properties


Temperature measurement is just measurement of the
heat exchange between thermometer and system.

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2.1 Heat transfer


3 transfer mode
Conduction, Convection, Radiation

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A. Conduction
transfer of thermal energy between regions of matter due to a
temperature gradient
In solid, liquid, gas, and plasma
Vibration of solid atoms, collision or diffusion of liquid (gas) atoms
(molecules, radicals)

Heat flow rate (watt, W)

T
Q = kA
x

k : thermal conductivity (W/m K )


A : area
T : temperature gradient
x : distance

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Thermal conductivity, k, of various materials

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Thermal conductivity, k, of various materials


Material
Silica Aerogel
Air
Wood
Hollow Fill Fibre Insulation
Alcohols and oils

Thermal conductivity
W/(mK)

Material

0.004 - 0.04
0.025
0.04 - 0.4
0.042
0.1 - 0.21

Thermal epoxy

1-7

Glass

1.1

Soil

1.5

Concrete, stone

1.7

Ice

Polypropylene

0.25

Sandstone

Mineral oil

0.138

Stainless steel

Rubber

0.16

Lead

LPG

0.23 - 0.26

Thermal conductivity
W/(mK)

Aluminum

2
2.4
12.11 ~ 45.0
35.3
237 (pure)120180 (alloys)

Cement, Portland

0.29

Gold

318

Epoxy (silica-filled)

0.30

Copper

401

0.12 - 0.177

Silver

429

Epoxy (unfilled)
Water (liquid)

0.6

Diamond

900 - 2320

Thermal grease

0.7 - 3

Graphene

(4840440) - (5300480)

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B. Convection
transfer of heat from one place to another by the physical
movement of fluids
In liquids, gases
Natural (free) convection
Forced convection by fan, pump, etc

Heat flow rate (watt, W) between solid and fluid

Q = hA(Ts Tenvironm )

h : convection heat transfer ( W/m2K)


A : area
Ts : surface temperature of solid
Tenvironm: temperature of fluid far from the surface

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Some examples of convection


Mantle convection

Heat sink radiator

Foehn phenomenon

Atmospheric convection
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Convection heat transfer coefficient, h, of some phases

h [Wm-2 K-1]

Process
Gases

2 25

Liquids

50 1 000

Gases

25 250

Liquids

50 20 000

Boiling or
condensation

2 500 100 000

Free Convection

Forced Convection
Convection with phase
change

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C. Radiation

Energy in the form of electromagnetic waves with continuous spectrum

All matter higher than absolute zero temperature

Sunlight is thermal radiation generated by the hot plasma of the Sun.

Stefan-Boltzmann law

E = T4

E : energy radiated per unit area (W/m2)

: emissivity

: Stefan-Boltzmann constant

T: Absolute temperature

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2.2 Thermal properties


Three important properties
Thermal conductivity, heat capacity, latent heat

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A. Heat capacity (C)


Heat (q) required to raise the temperature by 1 K
C = q/(T2-T1)

Higher C, larger q need more time to stabilize


For fast measurement, sensor having higher k and smaller C
required.

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Heat capacity of some materials


Material
Copper
Gold
Silver
Aluminum
Zinc
Tin
Mercury
Stainless steel
Silicon
water
Ice
Pyrex
Alumina (Al2O3)
Magnesia (MgO)
Polystyrene
Silicone oil

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Per unit mass


JK-1kg-1
385
129
235
903
389
227
139.3
480
712
4 179
2 040
835
800
960
1 300
1 548
27

Per unit volume


JK-1cm-3
3.44
2.49
2.47
2.44
2.78
1.66
1.88
3.83
1.65
4.17
1.88
1.85
3.04
3.46
1.37
1.45

B. Latent heat

Heat associated with phase change


solid liquid gas

Fixed-points use latent heat of materials

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Simple melting and freezing of pure solid

melting plateau

Freezing
temperature

temperature

Melting

freezing plateau

supercooling
and recovery

time

For melting, Qin = latent heat


For freezing, Qout = latent heat
Basically, Tmelting = Tfreezing

time

But little difference due to impurities, solid structure

During freezing, supercooling and recovery observed

Require more heat for solidification at initial to overcome the surface energy
between solid and liquid
There is a critical size for nucleation of solid

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Nucleation in pure metal


freezing

Liquid

Liquid
Solid

Energy

G1

G2 = G1 + G

S,L: solid, liquid


V: volume
A : surface area
: surface energy
r : radius of solid
Lv : latent heat
T : undercooling

Gibbs free energy change, G

G = Vs Gv + ASL SL

Gv = GvL GvS

4
= r 3 Gv + 4r 2 SL
3

Lv T
Tm

Critical value to solidify

2 SLTm 1
*

r =
Lv T
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3
16 SL
Tm2 1

G =
2
2

3
L
T
(
)
v

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2.3 Errors in Use of Thermometers


Thermometer indicates the temperature of a system.
In many cases, perfect measurement is not possible.
No thermal equilibrium between thermometer and system
Insertion of thermometer disturbs the equilibrium.

Possible and common errors

Immersion errors
Heat capacity errors
Settling response errors
Lag errors with steadily changing temperature
Radiation errors

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A. Immersion errors
Thermometer stem, sheath and lead wires are acting as path
for a continuous heat flow.
Heat absorbed by thermometer

Heat lost from thermometer

A simple model for error

Tm = (Tamb Tsys ) K exp(


Temperature profile
along thermometer stem

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L
)
Deff

Tsys : Temperature of system


Tamb : Temperature of ambient
L : depth of immersion of sensor
Deff: effective diameter of thermometer
K : constant (~ 1)

Relative immersion error


For K = 1

For 1 % accuracy

Relative temperature error (%)

For 0.01 % accuracy

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to 10 diameters + sensor
length

For 0.0001 % accuracy,

Immersion (diameter)

to 5 diameters + sensor
length

to 15 diameters + sensor
length
Highest level using fixedpoint measurement

B. Heat capacity errors


If a thermometer is immersed into system, the temperature of
system should be changed to lower or higher temperature.
This is due to heat flow to (from) thermometer from (to) system.
In adiabatic condition (there is no heat flow !),

Tmeasured

Ct
(Tini Ts )
= Ts +
C s + Ct
T

: Measured temperature
Ts : Temperature of system
Tini : Initial temperature of thermometer
Cs, Ct : heat capacity of system and thermometer
measured

Tini, Ct
equilibrium
Ts, Cs

Tmeasured

system
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C. Settling response error

Temperature

In practical cases, for control system, it will take time to


replace heat change of thermometer.
If insufficient time is allowed, error due to response will
occur.


Tm = (Tini Ts ) exp
0

1/e

Tm : temperature error
Ts : Initial temperature of system
Tini : Initial temperature of thermometer
: time
0 : 1/e time constant

Time

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Relative error
For 1 % accuracy
Percentage relative temperature error

industrial
Wait 5 0

For 0.01 % accuracy


laboratory
Wait 10 0
For 0.0001 %
accuracy,
Standard lab
Wait 15 0
Time (units of 0)

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Part II. Thermocouple Thermometry


1. Thermoelectric Effects
2. Type and Features of Thermocouples
3. Measurement Systems
4. Errors and Usage
5. Calibration and Uncertainty
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1. Thermoelectric Effects
Seebeck effect

Temperature difference Electric power

Peltier effect

Electric power Temperature difference

Thomson effect
Combine of above two effects

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1.1 Seebeck effects


In 1821, T.J.Seebeck found

Hot

current

Cold

B
A and B are two different metallic wires.

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Basic principle
For a single conductor under the temperature gradient
Th

Tc

Th side is in higher thermal energy state than Tc.


So, electrons in Th side move toward Tc side.
Then, number of electrons in Tc side is larger than those in Th
side. It means a non-equilibrium state.
Finally, there is a driving force for the movement of electrons
in Tc side toward Th side.
This is the thermoelectric voltage, in other words, Seebeck
voltage.
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Temperature coefficient
Seebeck coefficient, S (voltage per oC)
Th

Tc

E depends on the material and temperature gradient.

E
S = lim
t = 0 t
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For a specific material


Th

Tc

Temperature is an intrinsic property, so it is continuous.

E = S (t )dt
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Thermocouple itself is.batteries !

Temperature

A series of batteries which is operated using


temperature gradient.

Position
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Circuit analysis
Two different conducting wires
Single conductor can not be used as a thermocouple.
EA
T1

T0

EB

Enet = EA + EB
T1

T0

T0

T1

= S A dt + S B dt
T1

= ( S A S B )dt = T S
T0

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Enet

Same wires are connected to the circuit.


EA

EC
T1

T2
EB

T0
EC

Enet = EC + EA + EB + EC
T1

T2

T1

T0

T0

T1

T2

T1

= SC dt + S A dt + S B dt + SC dt
T2

= ( S A S B )dt = T S
T1

If T1 = zero ?
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Enet

Some part is damaged.


EA

EA
T1

T2

T3

T0

Enet

EB

Enet = EA + EA'+ EB
T1

T2

T3

T2

T1

T0

T0

T1

T2

T3

T2

T1

= S A dt + S A' dt + S A dt + S B dt + S B dt + S B dt
T1

T2

T3

T0

T1

T2

= ( S A S B )dt + ( S A' S B )dt + ( S A S B )dt


T1

T2

T3

T0

T1

T2

T3

T2

T0

T1

Let SA = SA + S

Enet = ( S A S B )dt + ( S A + S AB S B )dt + ( S A S B )dt


= ( S A S B )dt + (S AB )dt

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If T1 = T2 ?
46

Ideal vs Practical
For ideal and homogeneous wires
E only depends on the temperature gradient and Seebeck
coefficients.

For practical thermocouples


E = f(t, S, x)
t : temperature
S : Seebeck coefficient
x : position

Due to the thermoelectric inhomogeneity


Epractical = Ehomo + Einhomo

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Thermoelectric inhomogeneity
Caused from the factors affecting the Fermi energy level of
material
Composition change
Oxidation or evaporation
Structural change
Defects
Plastic or Elastic deformation

Produced in the local area


No temperature gradient, No effects !

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Calibration uncertainty by KRISS, Type S


0.6

0.5

UncertIainty / C

Type S

Ref TC
Other factors
Inhomogeneity
Combined

0.4

0.3

0.2

0.1
0

10

12

TC

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14

16

18

20

22

Calibration uncertainty by KRISS, Type R


0.6
Ref TC
Inhomogeneity
Other factors
Combined

Uncertainty / C

0.5

Type R

0.4

0.3

0.2

0.1

0.0
0

TC

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Calibration uncertainty by KRISS, Type S


6

Uncertainty / C

Type B

Ref TC
Inhomogeneity
Other factors
Combined

0
0

TC

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Change of inhomogeneity with temperature

Type S / R t/c

Little dependence on temperature


within 0.01 %

Possible to estimate
inhomogeneity at whole
temperature range.

2002 Temperature Symposium by M. Ballico

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KRISS Inhomogeneity Test System

Vertical Liquid bath

Operation temperature : 180


oC ~ 200 oC

Maximum immersion depth of


43 cm

Stepping motor driven by


computer

Bath temperature is monitored


by F250 thermometer.

Emf is measured using


Keithley 2000 DMM.

Ice point as reference


temperature

TCs are protected using quartz


tubes.

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Motor

Motor
controller
TCs
Thermometer

Ice
bath

DMM

Control PC
Bath

53

Example 1, Type S thermocouple

Emf difference (Em - E180 oC) /V

Type S
0

Inhomogeneity =

-20
0

-40

-2

-60

-4

-80

-6

-100

-8

E = 1.8 V

E
100 %
E180o C E25o C
1.8
100 %
1273.3 142.6

= 0.159 %

-10

-120

100

200

300

400

-140
0

100

200

300

400

500

Immersion depth /mm

(0.00159 10756.5) / 2
Uncertainty at 1100 oC due to inhomogeneity =
3
(Rectangular distribution)
= 4.94V
= 0.42o C

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Example 2, Type B thermocouple


Type B

Emf difference (Em - E180 oC) /V

-2

E
Inhomogeneity =
100 %
E180o C E25o C

E = 2.2 V

-4

-6

-8

-10

2.2
100%
140.5 + 0.3

= 1.56 %

-12

-14
0

100

200

300

400

500

Immersion depth /mm

Uncertainty at 1500 oC due to inhomogeneity


(Rectangular distribution)

(0.0156 10099.1) / 2
3
= 45.5V
=

= 3.93o C

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Dependency of inhomogeneity in KRISS


Type

Combined Uncertainty
/oC

Uncertainty from
Inhomogeneity /oC

Dependency

3.45

2.87

83 %

3.91

3.42

86 %

0.47

0.44

93 %

0.40

0.36

90 %

0.49

0.46

93 %

0.53

0.50

94 %

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2. Type and Features of thermocouples


Letter-designated
Noble metal thermocouples
Base metal thermocouples

Non letter-designated
Pure metal thermocouples
W/Re thermocouples
Others

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2.1 Thermocouple Types


Temperature vs. Emf relation of commercial
thermocouples

EMF (mV)

100
80

60

K
N

40
20

R
S

0
-20
-250

250 500 750 1000 1250 1500 1750 2000


Temperature (oC)

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2.2 Features of Thermocouples


Composition

Type
+

Properties
-

S
R
B

Pt90Rh10
Pt87Rh13
Pt70Rh30

Pt
Pt
Pt94Rh6

Most stable in air.


o
o
S and R can be used to 1450 C, B is to 1700 C.
Very sensitive to the metallic impurities.
Should not be used in vacuum without protecting tube.

Ni90Cr10
(Chromel)

Ni95(Mn,Al,Si)5
(Alumel)

Most well-known thermocouple.


In air or inert atmosphere.
Severe degradation at high temperature

Ni84.5Cr14.2Si1.3
(Nicrosil)

Ni95.5(Si,Mg)4.5
(Nisil)

Alternative to the type K


Enhance the high temperature stability
Newest developed one

T
J
E

Cu
Fe
Ni90Cr10

Cu55Ni45
(Constantan)

T is usually used in low temperature range, below 0 C.


J and E are rarely used.

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Non Letter-designated
Composition

Type

+
Au/Pt
Pt/Pd
Au/Pd

Properties
-

Au
Pt
Au

Pt
Pd
Pd

Very high purity wires (5N up)


Strong resistance to the composition change
Most stable and accurate thermocouples

W3Re/W25Re

W97Re3

W75Re25

W5Re/W26Re

W95Re5

W74Re26

Up to 2300 C
Specially designed ones for very high temperature.
Only for inert, vacuum or hydrogen atmosphere

More than several hundreds of thermocouples

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3. Measurement Systems

Thermocouple probe
Reference junction
Insulator and protecting tube
Compensating wire
Readout

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3.1 Thermocouple Probe


Sheath vs. Unsheathed
Quick connector

Reference thermocouple
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Color codes

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3.2 Reference junction

Silicon oil

Stability of 5 mK
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Cold junction

3.3 Protecting tube


Temperature
Strength
Surrounding atmosphere
Material composition of protecting tube
Chemical composition of environment
For base metal TCs, metallic tube
For noble metal TCs, ceramic tube

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Some insulators

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3.4 Compensating wire


Economic point of view
For noble metal thermocouples

Type
B
S, R
K
J
E
T
N

Composition
+
Copper
Copper
Chromel
Iron
Chromel
Copper
Nicrosil

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Copper
Copper Alloy
Alumel
Constantan
Constantan
Constantan
Nisil

67

Temperature

error

0 ~100
0 ~ 200
0 ~ 200
0 ~ 200
0 ~ 200
-60 ~ 100
0 ~ 200

0
5.0
2.2
2.2
1.7
1.0
2.2

3.5 Readouts
Digital volt(multi)meters (0.1 V resolution)
Digital indicators (with internal reference
Junction)

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4. Errors and Usage

Error tree of thermocouple


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4.1 Composition change at high temperature

Type S, 1400 oC, 1440 h


Negative
leg

SEM image

Negative : 95% Pt + 5% Rh
Positive
leg

(originally 100 % Pt)

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4.2 Thermocouples in different atmosphere


Test temperature: 1600 K
Type

Temperature
Result
change
- 19 ~ -28 K Completed

Gas

Time /h

Argon

10,000

Vacuum

1,610

- 1.5 K

Failed

Air

10,000

- 4.9 K

Completed

Argon

10,000

- 7 ~ - 18 K

Completed

Vacuum

2,780

- 3.2 K

Failed

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4.3 Effects of microstructual change of type K


Chromel : Short-range ordering
of Cr between 200 oC ~ 600 oC

Chromel

Increase of emf due to shortrange ordering


Alumel

Net emf

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4.4 Effects of protecting materials


Thermocouples in various
protecting tubes at about
1000 oC
Type S in Pt10Rh, Pt20Rh,
Inconel, S.steel
Type B in Inconel and
S.steel

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4.5 Annealing treatments

-1450 oC, 1 h
-1100 oC, 10 h
Emfannealed-Emfas-received
~ 2 oC difference

Temp. Diff /K

Standard annealing

0
0

200

400

600

800

Temperature /oC

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1000

1200

4.6 Inhomogeneity of type K and N


1/4", IN Sheath, Type N, Grounded junction
190

182

180

180

Temperature / C

170

Temperature / C

1/4", IN Sheath, Type K, Grounded junction

48 oC

160

150
1000 h
600 h
300 h
As-received

140

178

176

1000 h
600 h
300 h
As-received

174

130

172
0

100

200

300

400

500

Immersion depth /mm

100

200

300

400

Immersion depth /mm

1000 oC annealing treatment with time


Type K: inhomogeneous temperature variation of about 48 oC
Type N: very small change ( ~ 1 oC)
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500

5. Calibration and Uncertainty


Calibration method
Procedures of comparison calibration
Uncertainty of calibration

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5.1 Calibration method


Fixed-point method
At the defining fixed-points by ITS-90

Comparison method
Compare with the standard (reference)

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5.1.1 Fixed-point method


Most accurate method
o

PtPd thermocouple at Cu Point (1084.62 C)


13247

13246

Emf /V

o
0.05 C

13245

13243

Freezing cell

Pd V (=1 mK)
Standard deviation: 0.02

13244

TC wire

13242
15:40

16:00

16:20

Time /h.min

Typical freezing curve


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16:40

Calibration uncertainty of thermocouple


Expanded uncertainty (k=2)

Temperature/ C

Au/Pt

Pt/Pd

231.928 (Sn)

0.02 C

419.527 (Zn)

0.02 C

660.323 (Al)

0.03 C

961.78 (Ag)

0.03 C

0.04 C

1084.62 (Cu)

0.05 C

1154 (Fe/C)

0.15 C

1324 (Co/C)

0.65 C

0.65 C

1554.8 (Pd)

0.8 C

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0.03 C

S, R, B

0.03 C

0.03 C

o
o
o
o

79

0.04 C
o

0.05 C
o

0.06 C
o

0.08 C
o

0.09 C
o

0.2 C
o

5.1.2 Comparison calibration


Most common method
Compare with Reference thermometer in
furnace or liquid-bath

PRT s
Thermocouples
Liquid-in glass thermometers
Bi-metal etc.

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Calibration uncertainty by comparison calibration

Sensors

Temperature range

Expanded uncertainty
(k=2)

0 oC ~ 1100 oC

0.2 oC

1100 oC ~ 1554 oC

2.0 oC

-80 oC ~ 0 oC

16 mK

0 oC ~ 250 oC

16 mK

250 oC ~ 550 oC

20 mK

S, R, B

IPRT

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Type of calibration
Single point
At a specific temperature

Temperature vs. temperature (or emf)

Multiple points
Point to point calculation

Make a result at each calibration temperature

Continuous calculation

Make a result with finite temperature interval


Normally, interpolation used
Above the maximum point, extrapolation applied

It is very general to calculate the deviation emf.

It is used to minimize the interpolation error.


Deviation emf = Measured emf Standard emf
Standard emf is from the reference table (ASTM E230, IEC 584-1)

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5.2 Procedures of comparison calibration


Inspect the test item
Place the reference standard and test item into the
temperature enclosure
Set the temperature enclosure to specified temperature
Confirm the temperature stable
Read the indications from reference and test item
Repeat

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Step 1 : Visual inspection

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Step 2 : Dismentle

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Step 3 : Cleaning

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Step 4 : First heat treatment

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Step 5 : Wire insertion

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Step 6 : Re-assemble

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Step 7 : Making hot junction

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Step 8 : Second heat treatment

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Step 9 : Ice point preparation

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Step 10 : Installing pyrex tubes for ice point

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Installation of thermocouples
Weld the hot junctions
Or, use the temperature

Welding

equalizing block made of Pt


Install at the uniform
temperature zone

Pt block

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Measurement procedures
From low to high temperature
Measure if temperature change is below (0.05 ~ 0.1)
oC/min

Repeat 10 times at each point


About interval of 100 oC ~ 200 oC is suitable.

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Plot the deviation emf with temperature


12

Ei = Ex - Er
10

Deviation Emf /V

E = (Ex Es)+ Efit


E : deviation emf
Ex : DUT emf
Er : standard emf
Efit :interpolation fit
correction

Efit

E(=a0+a1t+a2t2+a3t3)

6
4
2

Example of interpolation fit of the


deviation emf

0
200

400

600

800

Temperature /oC

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1000

1200

Making a new reference function

E = E + E
= (c0 + c1t + .+ c8t8) + a0+a1t+a2t2+a3t3
= ( c0+a0) + (c1+a1)t + (c2+a2)t2 + (c3+a3)t3
+ c4t4 + . + c8t8

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5.3 Uncertainty of calibration


Comparison with reference thermocouple
Normally Pt/Rh-based noble thermocouples are
used as reference thermometer.
Au/Pt or Pt/Pd can be used as higher grade
standards.

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5.3.1 Measurement equation

Ed = (Ex Es) + Efit

(1)

Ed : Deviation emf /V
Ex : Measured emf of DUT /V
Es : Standard emf of DUT /V
Efit : Correction due to interpolation /V

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Measured emf of DUT

Ex = Em,x + Eex + Ert,x

(2)

Em,x : Read emf of DUT


Eex : Correction due to compensation(extension) wire
Ert,x : Correction due to room temperature
compensation

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Standard emf of DUT

Es = f(tr)
tr = g(Em,r + Ert,r)

(3)
(4)

tr : Reference temperature from the certificate of reference


thermocouple /oC
f(tr) : Standard emf from the IEC table
Em,r : Measured emf of reference thermocouple
Ert,r : Correction due to room temperature compensation

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Combined Standard Uncertainty

uc ( Ed ) = u 2 ( E x ) + u 2 ( Es ) + u 2 (E fit )

(5)

u ( E x ) = u 2 ( Em, x ) + u 2 (Eex ) + u 2 (Ert , x )

(6)

u ( Es ) = u 2 ( f ) + 2u 2 (tr )

(7)

2
2 2
2 2
u (t r ) = u ( g ) + u ( Em ,r ) + u (Ert ,r )

(8)

: Coefficient of voltage with temperature, V/oC


: Reverse of , oC/V
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5.3.2 Example of Comparison

Reference(REF): type R, DUT: type S


Calibration at 8 points (230 oC, 500 oC, 600 oC, 700 oC, 800 oC, 890 oC, 980
oC, 1060 oC)
10 measurements at each point
Calibration uncertainty and long term stability of REF are 0.4 oC (k =2) and
0.1 oC.
Calibration uncertainty and long term stability of DVM(Res. 0.1 V) are 10
V/V (k = 2) and 20 V/V.
The accuracy of selector switch is 0.5 V, and extension wires are not used.
Two thermocouples are welded at their measuring junction.
The stability of ice point (water and ice mixture) is 0.05 oC.
The inhomogeneity of DUT at 180 oC is 0.078 %.
The maximum deviation of interpolation is 0.15 V.
The combined standard uncertainties are calculated at each point.
In this case, we calculate the uncertainty at 1060 oC.

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Results of calibration
Reference thermocouple
Cal.
point
()

DUT

Deviation
emf

Temperature
/

Standard
deviation
/

230

1 887.30

246.25

0.21

1 840.62

0.18

1839.26

1.36

500

4 465.73

499.37

0.23

4 230.18

0.27

4225.86

4.32

600

5 578.02

599.26

0.31

5 235.63

0.39

5229.98

5.65

700

6 745.01

699.80

0.24

6 279.13

0.24

6271.93

7.20

800

7 955.13

799.91

0.35

7 351.66

0.36

7342.8

8.86

890

9 217.93

900.40

0.42

8 462.70

0.40

8452.49

10.21

980

10 258.31

980.54

0.46

9 372.94

0.45

9361.89

11.05

1 060

11 328.53

1 060.84

0.58

10 304.97

0.69

10293.77

11.20

Average

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Average

104

Standard
deviation
/

Standard
emf from
IEC table

5.3.3 Standard uncertainty of DUT, u(Ex)


Standard uncertainty of emf measurement, u(Em,x)
u 2 ( Em, x ) = u 2 ( EVD , x ) + u 2 ( EVC , x ) + u 2 ( EVL , x ) + u 2 ( ERe, x )
+ u 2 ( ESC , x ) + u 2 ( EEN , x ) + u 2 ( E IH ) + 2u 2 (t hj )

u(EVD,x): Resolution of DVM


u(EVC,x): Calibration uncertainty of DVM
u(EVL,x): Long-term stability of DVM
u(ERe,x): Repeatability of measurement
u(ESC,x): Accuracy of selector switch
u(EEN,x): Electrical noise
u(EIH): Inhomogeneity of DUT
u(thj): Tip temperature difference due to temperature gradient

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Standard uncertainty of compensation wire, u(Eex)

In case of using compensating or extension wires


Correction through the measurement of
temperature of connecting point/ Or apply the
specification
Direct measurement : - 2.3 V 0.3 V

u(Eex) = 0.15 V

Using the specification


5 oC
u (Eex ) =
3

In this case, it is not used.


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Standard uncertainty of room temperature compensation, u(Ert,x)

Factor due to the change of reference point


Usually, use the ice temperature (0 oC)
Apply the rectangular distribution
In this case, it is 0.05 oC.
0.05 oC
u (Ert , x ) =
3
= 0.029 oC

ui ( y ) = 0.029 oC 5.40 V / oC
= 0.16 V

Apply the sensitivity coefficient of type S at 0 oC


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5.3.4 Standard uncertainty of REF, u(Es)

Standard uncertainty of IEC table, u(f)


Internationally approved value, so it is zero.

Uncertainty reference temperature, u(tr)


From the calibration certificate of reference
thermocouple

tr = g(Em,r + Ert,r)

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5.3.4.1 Uncertainty of reference temperature, u(g)


Certificate of reference thermocouple
Normal distribution
In this case, it is 0.4 oC (k = 2).
u ( g ) = 0.2 oC

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5.3.4.2 Uncertainty of reference temperature, u(tr)


Standard uncertainty of emf measurement, u(Em,r)
u 2 ( Em,r ) = u 2 ( EVD ,r ) + u 2 ( EVC ,r ) + u 2 ( EVL ,r ) + u 2 ( ERe,r )
+ u 2 ( ESC ,r ) + u 2 ( EEN ,r ) + 2u 2 (t LS )

u(EVD,r): Resolution of DVM


u(EVC,r): Calibration uncertainty of DVM
u(EVL,r): Long-term stability of DVM
u(ERe,r): Repeatability of measurement
u(ESC,r): Accuracy of selector switch
u(EEN,r): Electrical noise
u(tLS): Long-term stability of reference thermocouple

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Room temperature compensation, u(Ert,r)

In this case, it is 0.05 oC.


Note

5.29 V / oC
ui ( y ) = 0.029 C
13.48 V / oC

0.05 oC
u (t hj ) =
3
= 0.029 oC

= 0.011 oC

Coefficients at ice point and 1060 oC are different each other.


Apply the coefficient of type R thermocouple at each temperature

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5.3.5 Interpolation, u(Efit)

Uncertainty due to curve fit to get a deviation


function
Apply the maximum difference between the
measured and fitted value
Apply the rectangular distribution
Apply the maximum difference as the half width of
distribution
In this case, it is 0.15 V.
0.15 V
u (E fit ) =
= 0.09 V
3
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5.3.6 Combined Standard Uncertainty uc(Ed)

u ( E x ) = u 2 ( Em , x ) + u 2 (Eex ) + u 2 (Ert , x )
= 4.67 2 + 0.0 2 + 0.16 2 V
= 4.67 V

u ( Es ) = u 2 ( f ) + 2u 2 (t r )

Sensitivity of DUT

u (t r ) = u 2 ( g ) + 2u 2 ( Em ,r ) + 2u 2 (Ert ,r )

= 0 + 11.73 0.218 V
= 2.56 V
2

Note !

= 0.2 2 + 0.074 2 1.012 + 0.392 2 0.029 2 oC


= 0.218 oC

uc ( Ed ) = u 2 ( E x ) + u 2 ( Es ) + u 2 (E fit )
= 4.67 2 + 2.56 2 + 0.09 2 V
= 5.33 V

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5.3.7 Uncertainty budget u(Ex)


Std.
uncertainty

Sensitivity
coefficient

u(xi)

ci

10304.97

4.676

10304.97

4.67

Quantity

Estimated

Xi

xi

Ex
Em,x

Uncertainty
ui(y)
4.67
4.67

Distribution

Deg.
Freedom

Normal

Normal

EVD,x

0.03

0.03

Rectang.

EVC,x

0.05

0.05

Normal

EVL,x

0.12

0.12

Rectang.

ERe,x

0.22

0.22

Normal

ESC,x

0.58

0.58

Rectang.

EEN,x

0.58

0.58

Rectang.

EIH

4.58

4.58

Rectang.

thj

0.058

11.73 /

0.68

Rectang.

Eex

Rectang.

Ert,x

0.029

0.16

Rectang.

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5.40 /
114

Uncertainty budget u(Es), u(Efit)


Quantity
Xi

Estimated
xi
10 293.77

Es

Std.
uncertainty
u(xi)

Sensitivity
coefficient
ci

Uncertainty
ui(y)

Distribution

Deg.
Freedom

Normal

Normal

0.2 oC

Normal

0.086 oC

Normal

2.56

2.56

f(tr)

tr

0.218 oC

11.73 /

g(tr)

0.2 oC

Em,r

1.16

0.074 oC/

2.56

EVD,r

0.03

0.03

Rectang.

EVC,r

0.06

0.06

Normal

EVL,r

0.13

0.13

Rectang.

ERe,r

0.18

0.18

Normal

ESC,r

0.58

0.58

Rectang.

EEN,r

0.58

0.58

Rectang.

tLS

0.058

13.48 /

0.78

Rectang.

Ert,r

Rectang.

Rectang.

Efit

0.14

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0.029
0.09

0.392
1
115

0.011 oC
0.09

5.3.8 Uncertainty with temperature


Calibration point
/

Combined standard
uncertainty /

Expanded
uncertainty (k = 2)
/

Expanded
uncertainty (k = 2)
/

246.25

2.55

5.10

0.58

499.37

3.19

6.38

0.64

599.26

3.51

7.02

0.69

699.80

3.87

7.74

0.73

799.91

4.27

8.54

0.79

900.40

4.70

9.40

0.84

980.54

5.07

10.14

0.88

1 060.84

5.33

10.66

0.91

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5.3.9 Report of uncertainty


Choose the maximum uncertainty among the calculated
values
Expanded uncertainty is determined with k = 2.
In this case, U95 = 0.9 oC

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Further reading
T.D. McGee, Principles and methods of temperature measurement,
1988, John Wiley & Sons
J.V.Nicholas and D.R.white, Traceable Temperatures, 2nd edition,
2001, John Wiley & Sons
Manual on the use of thermocouples in temperature measurement, 4th
edition, 1993, ASTM

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