background image

 
 

Page 38 of 48 

Heatpipe Furnace Models 17702W, 17702P, 17702S (13

07/20) 

THERMOMETRIC FIXED POINTS; A TUTORIAL 

 
The International Temperature Scale, the scale most used in science and industry, is based on a series of 
fixed point temperatures.  Fixed points involve two-phase or three-phase equilibria of, ideally, pure 
materials to which constant temperature values have been assigned by primary thermometry.  Defining 
fixed points are chosen to be as few in number as is consistent with the need to establish satisfactory 
interpolation procedures. 
 
There are secondary reference points which, also, are two-phase or three-phase equilibria of very pure 
materials, whose temperature values have been established by measurements made with interpolation 
instruments calibrated at the defining fixed points.  Secondary reference points are useful for the calibration 
of thermometers having total ranges shorter than the interpolation ranges of the Scale.  Generally, 
secondary points are admitted to the Scale only if the material is generally available in high purity and if 
sufficient reproducibility of the equilibrium temperature has been confirmed by measurements made 
independently by a considerable number of investigators.  An average value (weighted according to 
individual uncertainties) is then used as the ITS temperature value. 
 
Two-phase equilibria may be solid-liquid, liquid-vapour, or solid-vapour.  From the Phase Rule of Gibbs: 
 
P + F = C + 2 
 
P is an integer equal to the number of phases present, C is the number of components present - for a pure 
material C = 1 - and F is an integer representing the number of degrees of freedom.  It is evident that the 
temperatures of two-phase equilibria are pressure-dependent (one degree of freedom only) whereas 
equilibria in which all three phases are present (triple points) are characterised by unique values of 
temperature and pressure (zero degrees of freedom). 
 
A necessary condition to establish a triple point is to contain the appropriate material in a sealed enclosure 
from which all other materials, including air, have been evacuated, leaving a space to be filled by the 
vapour phase at a pressure appropriate to the temperature.  When the three-phase (solid, liquid, vapour) 
condition has been established, these parameters will settle to their unique triple-point values. 
 
The defining fixed points above 0°C are liquid-solid equilibria of high-purity metals.  Pressure-dependence 
is small and thermal capacity and thermal conductivity are relatively high.  Metals are generally available 
with a purity of 99.999% ("five-nines") or 99.9999% ("six-nines"). 
 
The metal is contained in a crucible of purified graphite, with a graphite cover and a graphite re-entrant 
sleeve.  The crucible is enclosed in an envelope of fused quartz, which extends into the sleeve interior to 
form the thermometer well.  The cell is charged with a pure metal, purged and filled with sufficient argon (or 
another inert gas) to give a pressure of 101kPa (1 standard atmosphere) at the freezing temperature and 
then sealed.  Thus, it is at once protected from contamination and supplied with an inert atmosphere at the 
required pressure at the equilibrium temperature.  A correction for the effect of change in ambient pressure 
on freezing point need not be made.  Sealed cells of this type have shown no measurable change after 15 
years of use. 
 
In general, sealed fixed-point cells are used in vertical-tube furnaces which provide good temperature 
control and sufficient cell immersion to make axial temperature gradients, in the measurement zone, 
negligible.  With the cell in the furnace, the controller is first set about 5°C above the anticipated value 
corresponding to the melting temperature of the metal in the cell.  The onset of melting is indicated by a 
cessation of temperature rise because of the latent heat required to produce the phase change.  This melt 
plateau can last for a considerable period of time.  When melting is complete, the cell temperature will rise 
to the furnace temperature. 
 

Содержание 17702P

Страница 1: ...PR9 9AG England Tel 44 0 1704 543830 Fax 44 0 1704 544799 Internet www isotech co uk E mail info isotech co uk The company is always willing to give technical advice and assistance where appropriate E...

Страница 2: ...S PARTS ARE NOT COVERED BY THIS GUARANTEE INTERFERENCE WITH OR FAILURE TO PROPERLY MAINTAIN THIS INSTRUMENT MAY INVALIDATE THIS GUARANTEE The company is always willing to give technical advice and ass...

Страница 3: ...uipment 21 To change the DATE and TIME or LANGUAGE 22 The NETWORK INTERFACE 22 To access the NETWORK INTERFACE 22 Data Logging 22 FTP Server Archiving 23 PROGRAMMER Function 23 To create install and r...

Страница 4: ...D DATA 40 GENERAL NOTE ON ISOTECH METAL FREEZE POINT CELLS 41 PRECAUTIONS TO PREVENT DEVITRIFICATION OF QUARTZ ENVELOPES 42 GENERAL COMMENT 43 SEALED METAL FREEZING POINT CELL 44 SEALED METAL FREEZING...

Страница 5: ...l IEC 417 Caution Hot Surface ELECTRICAL SAFETY This equipment must be correctly earthed This equipment is a Class 1 Appliance A protective earth is used to ensure the conductive parts cannot become l...

Страница 6: ...is hot or cold unless wearing the appropriate protective clothing and having the necessary training 6 Do not drill modify or otherwise change the shape of the apparatus 7 Do not dismantle the apparat...

Страница 7: ...1 Slacken the central nut using the required tube spanner the insertion of a screwdriver through the tube spanner will prevent the central stud turning 2 Remove the 3 screws securing the transit clam...

Страница 8: ...of up to four thermometers but removed for transit purposes Please see the below image for a guide to the installation of the support to the furnace 1 Thermometer support 2 Screw locations Please scre...

Страница 9: ...ply lines are live with respect to earth then the neutral fuse link should be replaced with a fuse A spare fuse is supplied with the furnace FUSE AND NEUTRAL LINK REPLACEMENT Hazardous voltages are ex...

Страница 10: ...Furnace Models 17702W 17702P 17702S 13 07 20 GENERAL LAYOUT Front View 1 USB socket 2 Ethernet socket 3 Main controller 4 Overtemperature controller 5 Mains power on switch Top View 1 Heatpipe furnac...

Страница 11: ...Page 11 of 48 Heatpipe Furnace Models 17702W 17702P 17702S 13 07 20 Rear View 1 Cooling coil connection not on W version 2 Cooling coil connection not on W version 3 Mains Power cable...

Страница 12: ...Isotech can provide heat pipe furnaces to suit Indium Tin Zinc Aluminium Silver and Copper fixed points Plateau length is determined by the difference in temperature between the heat pipe and cell thi...

Страница 13: ...ompassing the fixed points of indium and tin MODEL 17702P Contains a potassium heat pipe with a temperature range from 400 C to 1000 C thus encompassing zinc aluminium and silver freeze points MODEL 1...

Страница 14: ...ontroller 1 Press the Scroll button to display A1 HI 2 Use the up down buttons to scroll to the desired alarm setting This would normally be 10 20 C above the target temperature 3 To enter the value y...

Страница 15: ...ing the up down buttons enter a new temperature for the overtemperature protection Initially this can be quite a low value say 500 C for test purposes Now press the SCROLL and PAGE buttons together on...

Страница 16: ...he controller please read this manual thoroughly to get the best performance from the equipment Certain features used in this controller require different levels of access The Operator access requires...

Страница 17: ...LL button to display the SUPERVISOR screen as above 9 When logged in as the SUPERVISOR the equipment will control in the normal way How to log in as the Engineer 1 Press the Page button to display the...

Страница 18: ...utton 3 SCROLL button 4 DOWN button 5 UP button The HOME page 1 Heatpipe temperature 2 Heatpipe setpoint 3 Setpoint adjust box 4 Data Record icon 5 PAGE button 6 SCROLL button 7 DOWN button 8 UP butto...

Страница 19: ...used to control the ramp rate These parameters are set at 445 C for Sodium and 395 C for Potassium and 7 5 C min and should not be changed Changing the Set Point The main controller will control the H...

Страница 20: ...se follow the procedure below to linearise the controller display value 1 For the heatpipe furnace set the furnace up as it will be used with a fixed point cell using either a cell or a simulation of...

Страница 21: ...the best values for this temperature After two cycles it will install the calculated values and use these for the control loop You are not required to log in to access this feature To enable the AUTO...

Страница 22: ...RK tab and enter with the SCROLL button 3 Scroll to INTERFACE and enter with the scroll button 4 Scroll to and adjust desired parameter using the pop out soft keyboard Data Logging The equipment will...

Страница 23: ...two formats 5 ftp instrument IP address This allows a user to log in as the anonymous user if the recorder has any account with the user name set to anonymous with a blank password 6 ftp user name pa...

Страница 24: ...d program for pasting either from the internal drive to the USB device or vice versa This is useful if you wish to transfer a program to other instruments Copy All As above for Copy but copies all the...

Страница 25: ...e set in the individual segment configurations Rate A Ramp Rate segment is specified by a target set point and the rate at which to ascend descend to that set point Time A Ramp Time segment is specifi...

Страница 26: ...RRENT PROGRAM will display TEST_1 10 TEST_1 is now the default program 11 To RUN the program TEST_1 exit the PROGRAM EDIT page using the PAGE button until you see the PROGRAM homepage 12 Press SCROLL...

Страница 27: ...ween the controller and the heat source itself Holdback can be configured to hold either the segment or the complete program The USER defined value is used to define the actual value applied to it Thi...

Страница 28: ...cooling coil is accessed from the rear panel and this will need to be removed to make any connections or service of the connections The cooling medium can be any number of substances but in most case...

Страница 29: ...of published information and of available apparatus for the safe treatment of these sophisticated devices DESCRIPTION Sufficient information now exists at Isotech to allow introduction of a new appara...

Страница 30: ...heated to 400 C if the cell is zinc 650 C for aluminium or 900 C for silver During conditioning thermometers are protected from contamination by a slow air flux around them CAUTION it is essential wh...

Страница 31: ...be accomplished by blowing air at ambient temperature across them by means of a free standing fan 1 By adjusting the set point to a few degrees above the appropriate melting point the cell aluminium...

Страница 32: ...ting the set point to a few degrees above the appropriate melting point the cell tin or indium is melted in the essentially temperature gradient free water filled heat pipe When the cell s contents ar...

Страница 33: ...to 1000 C and return it to ambient temperature without altering the water triple point resistance value by more than 0 5mK equivalent Instructions in the Isotech 962 and 96178 thermometer manuals exp...

Страница 34: ...least 2 hours This operation outgases the basket and insulation which may smoke and discolour during this first temperature excursion The cell can then be inserted into the basket in readiness for us...

Страница 35: ...Page 35 of 48 Heatpipe Furnace Models 17702W 17702P 17702S 13 07 20...

Страница 36: ...Page 36 of 48 Heatpipe Furnace Models 17702W 17702P 17702S 13 07 20...

Страница 37: ...Page 37 of 48 Heatpipe Furnace Models 17702W 17702P 17702S 13 07 20...

Страница 38: ...necessary condition to establish a triple point is to contain the appropriate material in a sealed enclosure from which all other materials including air have been evacuated leaving a space to be fill...

Страница 39: ...rgon In practice the difficulties of setting up conditions to facilitate this measurement can conveniently be circumvented by carrying out the alternative procedure of comparison calibration in which...

Страница 40: ...3 3 ITL M 17668 ITL M 17701 3 4 7 TIN FP 231 928 505 078 3 3 2 2 ITL M 17669 ITL M 17701 3 4 7 ZINC FP 419 527 692 677 4 3 2 7 ITL M 17671 ITL M 17701 2 3 6 ALUMINIUM FP 660 323 933 473 7 0 1 6 ITL M...

Страница 41: ...eau temperature The cell is a fragile device Although it is as rugged as is consistent with its materials and purpose it must still be regarded as a kilogram or more of mass loosely contained in a fra...

Страница 42: ...l can no longer be assumed to be gas tight It may leak its enclosed gas and atmospheric air may leak into it The pressure at the freeze point may as a consequence be incorrect and more seriously conta...

Страница 43: ...However the technique requiring association of cells with other equipment involves subtlety and operator sensitivity Before relying upon measurements made in them the operator should perform enough f...

Страница 44: ...17702S 13 07 20 SEALED METAL FREEZING POINT CELL A High purity graphite crucible and cover B High purity graphite sleeve C High purity metal D Fused quartz envelope filled to give a pressure of 1 sta...

Страница 45: ...Page 45 of 48 Heatpipe Furnace Models 17702W 17702P 17702S 13 07 20 SEALED METAL FREEZING POINT CELL BODY DIMENSIONS...

Страница 46: ...s 17702W 17702P 17702S 13 07 20 ACKNOWLEDGEMENT The Isotech dual furnace owes its origin to Dr P Marcarino of Italy His research and development solved many of the problems of contamination and handli...

Страница 47: ...a license is purchased it allows for fully automatic calibration including certificate printing and the calculation of coefficients Refer to the Isotech I Cal EASY handbook and help system for more d...

Страница 48: ...this database to the chart or spreadsheet The chart spreadsheet can be configured to include one or more channels from one or all connected instruments It is also possible to archive instrument histo...

Отзывы: