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8 Operation

36

B40IB006EN-D

8 Operation

The HTK 1200N allows for measurements under
various atmospheric conditions (air, vacuum, inert
gas) in the temperature range from room tempera-
ture to 1200 °C.

8.1 Before Turning on Power

8.2 Operation under Air Atmosphere

8.2.1 Operation at Room Temperature

Operation is performed in the same way as with the
standard sample holder. No special precautions
have to be taken.

8.2.2 Operation as Heating Chamber

Operation is performed in the same way as with the
standard sample holder.

The CCU 1000 Combined Control Unit by Anton
Paar GmbH is available for the HTK 1200N. For de-
tailed ordering information, see

. The

temperature control unit is used to control the sam-
ple temperature by means of the chamber’s heating
system as well as the thermocouple.

Keep the following sequence, when starting the op-
eration of the HTK 1200N at high temperatures:

1. Mount the sample and insert the sample holder

flange into the chamber, as described in

and

2. Switch on the cooling water circuit.

3. Switch on the temperature controller and set the

required sample temperature.

NOTICE

Risk of damage

Make sure that the HTK 1200N is installed
according to the instructions in

.

Take care that the cooling water hoses con-
nected to the inlet/outlet nozzles are protected
against unintentional disconnection.

- for detailed information on

the requirements for cooling water quality.

Check the flow controller of the CCU 1000 peri-
odically for proper functioning.

Only turn on the mains supply of the CCU 1000
Combined Control Unit, when the instrument is
fully installed.

Always operate the HTK 1200N with the cooling
water circuit on. This is absolutely necessary to
avoid effects of the working temperature on the
goniometer.

Do not exceed the maximum permissible pres-
sure of 4 bar to prevent bursting of the hoses.

Make sure that the alignment slit is demounted
from the sample holder before operating the
chamber.

CAUTION

Hot surface

During operation and even after turning off the
instrument, temperatures at the sample holder
can reach up to 1200 °C. Make sure that the
sample holder is at room temperature before
handling it.

NOTICE

Risk of damage

Check the chemical resistance of the materials
in the HTK 1200N BEFORE the experiment.

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Содержание HTK 1200N

Страница 1: ...Measure what is measurable and make measurable that which is not Galileo Galilei 1564 1642 Reference Guide HTK 1200N High Temperature Oven Chamber with CCU 1000 Control Unit ...

Страница 2: ......

Страница 3: ...ion This document or any part of it may not be reproduced changed copied or distributed by means of electronic systems in any form print photocopy microfilm or any other process without prior written permission by Anton Paar GmbH Trademarks registered trademarks trade names etc may be used in this document without being marked as such They are the property of their respective owner Further informa...

Страница 4: ...nary Sample Holder and Sample Spinner 19 4 4 3 Connection of Sample Spinner Motor 20 4 4 4 Connection for Safety Circuit 20 4 5 Connecting CCU 1000 with a Computer 20 4 6 Installing the Cooling Water Circuit 21 4 7 Installing the Gas Supply 21 4 8 Installing the Vacuum Equipment 21 5 Putting HTK 1200N into Operation 23 5 1 Alignment of the Sample Holder 23 5 2 Height adjustment with Rigid Adapter ...

Страница 5: ...40 10 3 Error Analysis 40 10 4 Technical Support 42 11 Maintenance 43 11 1 Routine Maintenance 43 11 2 Check the Functioning of the Flow Controller 43 11 3 Exchanging of Parts 43 11 3 1 Switching off the Instrument 43 11 3 2 Replacing the Window Foil 43 11 3 3 Replacing the Thermocouple 45 11 3 4 Replacing the O rings 45 11 4 Checking and Replacing Main Fuses 45 Appendix A Technical Data 46 Append...

Страница 6: ...Contents 6 B40IB006EN D ...

Страница 7: ... the responsibility of the customer to provide all the set up tubings valves necessary for proper work with HTK 1200N Do not use any accessories or wearing parts other than those supplied or approved by Anton Paar GmbH Make sure all operators are trained to use the instrument safely and correctly before starting any applicable operations In case of damage or malfunction do not con tinue operating ...

Страница 8: ...nformation about the situation at hand DANGER Description of risk Danger indicates a hazardous situation which if not avoided will result in death or serious injury WARNING Description of risk Warning indicates a hazardous situation which if not avoided could result in death or serious injury CAUTION Description of risk Caution indicates a hazardous situation which if not avoided could result in m...

Страница 9: ... get very hot Do not touch this surface without adequate protective measures 1 CAUTION This symbol calls attention to the fact that the instrument must be connected to protective ground Service has to be done by qualified per sonal only Always disconnect power cord before serving Wear protective gloves Wear protective gloves when handling the HTK 1200N Wear safety goggles Wear safety goggles when ...

Страница 10: ...s extension the HTK 1200N can be converted into a capillary heater up to 1000 C To ensure reliable operation of the HTK 1200N High Temperature Oven Chamber the instrument must be operated with 135004 CCU 1000 Combined Control Unit 164877 Flow controller TIP Please refer to Appendix Efor detailed informa tion 2 2 Design of the Instrument The HTK 1200N is a heating stage for powder XRD with a temper...

Страница 11: ...a very uniform temperature distribu tion inside the oven TIP The foamed alumina shell is very porous with a large internal surface Even when operated with a vacuum pump small amounts of adsorbed gas in particular oxygen are continuously released from the alumina If the sample material is very sensitive to oxygen this can lead to undesired sample oxida tion at elevated temperature 2 2 2 Lid Fig 4 C...

Страница 12: ...carrier 2 Fixing ring for sample carrier 3 Sample holder body 4 Thermocouple 5 Temperature shielding with fixing clamp 6 Flange 7 Motor 8 Electronic motor control 9 Flange fixing screws 4 pcs 10 Cable connection between thermocouple and CCU 1000 The sample holder assembly consists of the flange and the actual sample holder which is fixed to the flange by a fixing nut TIP The sample spinner is actu...

Страница 13: ...lding closes the opening of the alumina insulation and provides a uniform temperature distribution TIP Please refer to chapter 7 for further informa tion The sample holder is inserted into the HTK 1200N chamber with two guide pins and fastened by four screws 2 3 Connector Box The connector box terminates the supply hose of the HTK 1200N which contains the control wires for the temperature sensor f...

Страница 14: ... sample chamber It is a water flow dependent switch which is connected to CCU 1000 If there is not enough water flow CCU 1000 switches to Standby mode heater off the Error LED on the front panel starts to flash and shows an alarm message E03 In addition a thermoswitch is mounted in the safe ty switch box for flange control Fig 3 7 to protect the device from being overheated in case of a mal functi...

Страница 15: ...f your diffractometer manufacturer or Anton Paar GmbH in Graz Austria Table 3 1 Supplied Parts Pcs Item Cat No 1 HTK 1200N with stationary sample holder including Heating chamber Stationary sample holder Sample carrier 0 8 mm deep 2x Fixing ring for sample carrier Cable for sample holder flange 16407 or 1 HTK 1200N with sample spinner including Heating chamber Sample Spinner Sample carrier 0 8 mm ...

Страница 16: ...es delivered with the HTK 1200N for completion by comparing the parts to those listed in the appropriate packing lists NOTICE Risk of damage Always use the original packing material when shipping the instrument or parts of it Store the packing material carefully for later use ...

Страница 17: ...l min temperature 15 to 25 C pressure max 4 bar 4 2 Mounting the Adapter on HTK 1200N An appropriate adapter is necessary to mount the HTK 1200N High Temperature Oven Chamber on a goniometer For detailed ordering information refer to Appendix E 1 Alignment equipment 2 Allen screw 4 pcs 3 Adapter version depends on the goniometer used 4 HTK 1200N base plate To mount the adapter proceed as follows 1...

Страница 18: ...l connectors and that the slot is sufficiently ventilated to avoid heat accumula tion behind the CCU 1000 The connector for temperature measurement flange control and sample spinner are located in the connection box described in chapter 2 3 The instrument is delivered together with the current cables for the HTK 1200N heater and the connec tion cable for the HTK 1200N temperature sensor Connect th...

Страница 19: ...e Holder and Sample Spinner For correct installation please follow this instruction Stick the plug in connection 1 of the cable for sam ple holder flange into the locknut 2 of the sample holder at the bottom of the sample holder flange Then connect the other end of the cable to the con nector Temperature Sensor on the connector box Fig 8 3 WARNING Risk of injury This instrument must be connected t...

Страница 20: ...r box Fig 8 4 4 4 4 Connection for Safety Circuit At the rear of the HTK 1200N is a small safety switch box for flange control and overheating pro tection Connect the extension cable from the safety switch box on the back of the HTK 1200N to the connector Flange Control on the connector box Fig 8 2 4 5 Connecting CCU 1000 with a Com puter The RS 232 serial port at the rear panel of CCU 1000 allows...

Страница 21: ...he lid see chapter 2 2 2 The gas exhaust tubing can be connected to the adapter The type of gas connector depends on the adapter type TIP Refer to Appendix F for further information 4 8 Installing the Vacuum Equipment The HTK 1200N can be operated under a vacuum of approx 10 4 mbar TIP Anton Paar GmbH offers a suitable vacuum equipment for the HTK 1200N All required compo nents for the installatio...

Страница 22: ... equipment 1 Combined vacuum gauge ITR 90 2 Cross piece DN25 3 Venting valve 4 Reducer DN25 DN40 5 Flexible stainless steel hose 0 25 m length 6 Turbomolecular pump 7 Plastic hose 3 m length 8 Rotary slide vacuum pump 9 Oil mist filter 10 Display 3 2 1 5 6 7 9 8 4 10 ...

Страница 23: ...ometer In struction Manual for detailed information Good beam alignment is important because HTK 1200N is aligned relative to the X ray beam zero line 5 2 Height adjustment with Rigid Adapter 1 Install the chamber into the already aligned goniometer use the standard sample holder to align the goniometer 2 Remove the sample holder flange and place the alignment slit onto the sample holder such that...

Страница 24: ...ter no inaccuracies due to tolerances at mechanical parts The alignment stage allows re alignment to be performed at any temperature and while the X ray beam is on The alignment stage offers an accuracy of 5 µm Digital display of the chamber position is possi ble TIP For information about the operation of the mo torized alignment stage read the Alignment Stage Instruction Manual 5 4 Adjustment of ...

Страница 25: ...set of the maximum of the intensity profile TIP For diffractometers rotate source detec tor around the centre axis of the goniometer For 2 diffractometers rotate the chamber around the centre axis of the goniometer When starting with the alignment do the scan with 3 As the alignment gets better reduce the scan range 6 Depending on the offset rotate the chamber as described in the instruction manua...

Страница 26: ...n CCU 1000 is in the following status the temperature set point SP is set to the default value of 25 C the HEATER is off the Error LED is flashing the display shows E03 to indicate that there is no water flow 2 Turn on the cooling water supply The alarm message disappears and the flashing of the Error LED stops 3 Press the HEATER button to start control of the sample holder temperature If the inst...

Страница 27: ...0 is not possible on the controller itself However the delivered software for the controller allows to pro gram a temperature profile see the corresponding software manual that was delivered with the instru ment 6 1 Front Panel of the Instrument The front panel of CCU 1000 contains the keypad the status LEDs and the display which are described in the following section Fig 13 Front panel of CCU 100...

Страница 28: ...t show depending on the LEDs on the right side of the display see chapter 6 2 1 different informa tion In the normal operation mode process value LED is green the display shows the actual tem perature of the sample holder of HTK 1200N By pressing the SCROLL button the set point LED is green which means that the target set point tem perature can now be changed by using the UP or DOWN button By pres...

Страница 29: ...ue C min Default value 20 C min rEF cAP Configuration for reflection or for use with capillary exten sion Limits the operating tem perature depending on the used equip ment Reflection max 1200 C Capillary Extension max 1000 C 24 Par Conf 25 3E04 rate ref cap rot s rate drat dSP PROCESS VALUE SET POINT ERROR PROCESS VALUE SET POINT ERROR PROCESS VALUE SET POINT ERROR code protected read only read o...

Страница 30: ...and set the desired target temperature by using the UP DOWN buttons 4 Wait until the displayed sample holder tempera ture has reached the target value TIP If you have chosen a large heating cooling rate wait 1 minute before you start the X ray scan to make sure the sample surface has reached a con stant temperature 6 6 Remote Control of CCU 1000 Usually CCU 1000 is integrated in the software that ...

Страница 31: ... holder mounted The procedure of mounting the sample holder is the same for both sample holder flanges To replace the sample holder proceed as follows 1 Disconnect the cable from the sample holder at the bottom of the sample holder flange Prepare the supplied stand for the sample holder flange 2 Hold the sample holder flange with one hand and unscrew the four fixing screws with the other hand Remo...

Страница 32: ...dy To replace the sample holder body from the sample holder flange first demount the sample holder flange from the chamber refer to chapter 7 1 and then fol low the instruction below 1 Unscrew the two screws at the bottom of the sample holder flange and demount the panel 2 Loosen the locknut at the bottom of the sample holder flange with 4 5 rotations 3 Remove the whole sample holder unit from the...

Страница 33: ...ignment stage For samples thicker than 2 5 mm 3 5 mm the sample holder height can be varied by demounting the spacer ring 1 The 4 mm spacer ring is includ ed in the delivery and is already mounted TIP Before removing the spacer ring make sure that the HTK 1200N is aligned properly If not re align by means of the alignment slit refer to chapter 5 for further information To remove the spacer ring 1 ...

Страница 34: ... Insert the sample holder flange into the cham ber 7 2 1 Powder Samples To apply the sample use a spatula to press the powder into the groove of the sample carrier and subsequently smooth the powder s surface by means of a glass platelet TIP Make sure that the contact surfaces between sample carrier and top of the sample holder body are free of dust and sample residues to provide for a good therma...

Страница 35: ... not only influenced by its design but also by the thickness thermal conductivity emissiv ity of the sample and the thermal contact of the sam ple to the sample holder To account for temperature deviations in heating at tachments for non ambient X ray diffraction a tem perature calibration should be performed Temperature calibration can be done by observing known phase transitions either melting p...

Страница 36: ...tch on the temperature controller and set the required sample temperature NOTICE Risk of damage Make sure that the HTK 1200N is installed according to the instructions in chapter 4 Take care that the cooling water hoses con nected to the inlet outlet nozzles are protected against unintentional disconnection Refer to Appendix B for detailed information on the requirements for cooling water quality ...

Страница 37: ... CCU 1000 peri odically for proper functioning CAUTION Hot surface During operation and even after turning off the instrument temperatures at the sample holder can reach up to 1200 C Make sure that the sample holder is at room temperature before handling it NOTICE Risk of damage Check the chemical resistance of the materials in the HTK 1200N BEFORE the experiment NOTICE Risk of damage Always opera...

Страница 38: ...t is the responsibility of the customer to provide all the set up tubings valves necessary for proper work with the HTK 1200N This implies that the local safety regulations especially for work at elevated temperatures need to be ful filled Make sure that all fittings are tight and mounted properly and an appropriate exhaust hose is connected to the safety valve s outlet Do NOT work with poisonous ...

Страница 39: ... the sample and put the sample holder back into the sample chamber 4 Turn off the cooling water 5 Turn off CCU 1000 completely In order to remove HTK 1200N from the diffractom eter continue as follows 1 Completely turn off CCU 1000 mains switch 2 Disconnect all electrical cables from the sample chamber 3 Disconnect the couplings of the cooling water hoses 4 Dismount the sample chamber from the gon...

Страница 40: ...h does not detect the current cable E09 CCU 1000 Air Cool ing Fail The protective thermoswitch inside CCU 1000 is acti vated E10 Other Messages Internal errors of CCU 1000 con tact Anton Paar GmbH E11 Sensor Spread Failure Activated in case of too big temperature difference between the sensors sample holder and heater E12 Flow Con trol Exten sion missing Activated in case of missing flow control l...

Страница 41: ...er hoses dis connected Connect the water hoses on HTK 1200N to the cooling water circuit no cooling water Turn on the cooling water flow controller disconnected Connect the water flow con troller to the CCU 1000 insufficient cool ing water supply Make sure the water pres sure is between 2 4 bar and the flow rate is 0 7 1 5 l min flow controller does not switch Contact Anton Paar GmbH cooling ducts...

Страница 42: ... RS 232 cable null modem required and con nectors wrong settings in diffractometer software check settings for COM port baud rate string for mat and device address conflicting set tings in CCU 1000 and diffractometer software contact your diffractome ter manufacturer or Anton Paar GmbH cause action Cables between chamber and CCU not prop erly connected Check connections between chamber and CCU cau...

Страница 43: ...intenance work regu larly to ensure the smooth long term operation of the instrument 11 3 2 Replacing the Window Foil The window in the housing is covered by either of the following foils When operating the HTK 1200N at tempera tures up to 1000 C an aluminium coated Kap ton foil of 125 µm thickness is used to cover the housing window This foil guarantees minimum absorption For temperatures above 1...

Страница 44: ...l Put the new foil centrically over the window opening The aluminium coated side has to be inside Combination of graphite foil and non coated Kapton foil Place the graphite foil within the O ring first and then put the non coated Kapton foil centrically over the graphite foil 5 Mount the two clamps again 6 Fasten the screws of the clamps beginning from the side where the cooling tube 1 is fas tene...

Страница 45: ... box 4 Insert the O ring into the O ring groove 11 4 Checking and Replacing Main Fuses Two mains fuses are located in the fuse box 1 on the backside of the CCU 1000 Exchange the mains fuse as follows 1 Switch off CCU 1000 and disconnect all cables from the rear side 2 Use a small screw driver to push out the fuse holder on both sides 3 Check the fuse or exchange the defective fuse The two mains fu...

Страница 46: ...p time RT to 1200 C In air 15 min Temperature sensor Pt10Rh Pt thermocouple type S Temperature accuracy1 2 C Temperature stability1 0 5 C Heating method Oven heater 1 Sample holder temperature values depending on operating conditions Voltage supply DC 6 5 V and 12 V Power consumption max 2 Watt Angle of incidence 0 164 2 Window opening 10 mm 200 Foil material Aluminium coated Kapton up to 1000 C o...

Страница 47: ...approx 26 kg Voltage mains AC 230 V 10 Frequency mains 50 60 Hz Power consumption max 1671 VA Mains fuses 2 x T 8 A H 5 x 20 mm ceramic tube Overvoltage category II according to EN 61010 1 Voltage output AC 45 V Current output max AC 35 A Thyristor fuse Semiconductor protection fuse FF 12 5 A 10 x 38 mm Flow rate 0 7 to 1 5 l min Temperature 15 to 25 C Pressure Max 4 bar Ambient temperature 15 35 ...

Страница 48: ... requirements The product is classified as a class B equipment and is not intended for the use in industrial area Low Voltage Directive 2014 35 EU OJ L 96 357 of 29 3 2014 Applied standards EN 61010 1 2010 Safety requirements for electrical equipment for measurement control and laboratory use Part 1 General requirements IEC 61010 2 010 2014 Safety requirements for electrical equipment for measurem...

Страница 49: ...oned range Saturation index SI pH pH s Ryznar Index RI 2 pH s pH pH Is obtained and corrected by the addition of chemicals as stated before pH s Is calculated according to pH s 9 3 A B C D with the following values A Conversion value of total dissolved material in milligrams per liter mg l B Conversion value of the temperature of the cool ing water in degrees Celsius C C Conversion value of the ca...

Страница 50: ...tal dissolved material Temperature Ca hardness Ca Bi carbonate content HCO3 mg l A Deg C B Deg D C chem D eq l 50 300 0 1 10 2 3 0 6 0 6 0 2 1 0 400 1000 0 2 15 2 2 1 4 1 0 0 5 1 4 24 2 0 2 2 1 2 1 3 1 8 35 1 8 3 5 1 4 2 0 2 0 47 1 6 5 5 1 6 3 2 2 2 60 1 4 7 0 1 7 4 1 2 3 76 1 2 9 0 1 8 5 2 2 4 11 5 1 9 6 4 2 5 14 5 2 0 7 9 2 6 18 0 2 1 22 2 2 2 1 D 10 mg l CaO 1 chem 61 mg l ...

Страница 51: ...rigid sample hold er in vacuum and air The indicated values are comparable for the rigid sample holder and for the sample spinner and are supposed to give a rough idea about the magnitude of vertical expansion Vertical sample holder expansion in air Vertical sample holder expansion in vacuum Temperature C Vertical expansion mm 25 0 00 100 0 02 200 0 06 300 0 09 400 0 13 500 0 18 600 0 22 700 0 27 ...

Страница 52: ...endix D Warranty The warranty regulations for the HTK 1200N High Temperature Oven Chamber are in accordance with General Terms of Delivery of the Austrian Electrical and Electronic Industry Anton Paar GmbH gives no warranty for ceramic parts ...

Страница 53: ...Spare Parts 58963 HIGH VACUUM EQUIPMENT 176757 HIGH VACUUM EQUIPMENT 100V 15913 HTK 1200N SAMPLE CARRIER 0 8MM DEEP 16411 HTK 1200N SAMPLE CARRIER 0 4MM DEEP 16412 HTK 1200N SAMPLE CARRIER FLAT 15914 FIXING RING FOR SAMPLE CARRIER HTK 1200N 75850 SET OF WINDOW FOILS AL COATED KAPTON 2600 SET OF GRAPHITE FOILS 2601 SET OF KAPTON FOILS 75851 SET OF O RINGS 6650 SPARE PARTS PACKAGE 182226 CABLE FOR S...

Страница 54: ...ibe the nut at the 6 o clock position 3 Hold the fitting body steady with a backup wrench and tighten the nut 1 1 4 turns Watch the scribe mark make one complete revolution and continue to the 9 o clock position By scrib ing the nut at the 6 o clock position as it appears to you there will be no doubt as to the starting position When the nut is tightened 1 1 4 turns to the 9 o clock position you c...

Страница 55: ...position 2 Insert tubing with pre swaged ferrules into the fitting body until the front ferrule sits 3 Tighten nut by hand Rotate nut to the original position with a wrench An increase in resis tance will be encountered at the original posi tion Then tighten slightly with the wrench Smaller tube sizes will take less tightening to reach the original position while larger tube sizes will require mor...

Страница 56: ...Appendix G Declaration of Conformity 56 B40IB006EN D Appendix G Declaration of Conformity ...

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