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Appendices

Agilent Electrothermal Temperature Controller ETC 60 User’s Guide

Appendix C — Sensitivity Test Record Sheet

Solution (concentration):

Matrix:

Date

Absorbance

Measured Concentration

__/__/____

Содержание ETC 60

Страница 1: ...Agilent Electrothermal Temperature Controller ETC 60 User s Guide ...

Страница 2: ...n this document that conflict with these terms the warranty terms in the separate agreement shall control Technology Licenses The hardware and or software described in this document are furnished under a license and may be used or copied only in accordance with the terms of such license Restricted Rights Legend U S Government Restricted Rights Software and technical data rights granted to the fede...

Страница 3: ...9 Notes and Tips 9 Warning Symbols 10 Information Symbols 10 Color Coding 11 2 Getting Started 13 Introduction 13 Unpacking 14 Temperature Control Module 15 Workhead 16 Pre Installation 17 Voltage Selector 17 Installation Overview 18 Installing the Workhead Bracket Flame Models 19 ETC 60 Workhead Bracket Installation on Zeeman Instruments 22 Installing the Workhead 23 Installing an Absorption Cell...

Страница 4: ...s 32 Manual Isothermal Method 33 Manual Step Method 33 Changing Settings 34 Unattended Operation 35 Shutdown Procedure 35 4 Analytical Notes 37 Arsenic 38 Mercury 38 Optimal Temperature Determination 39 5 Maintenance 41 Daily Maintenance 41 Replacing the Fuse 41 Quartz Absorption Cell 42 Replacing the Absorption Cell 42 Removing the Workhead 43 6 Appendices 45 Appendix A Specifications 45 Environm...

Страница 5: ...lent Electrothermal Temperature Controller ETC 60 User s Guide 5 Appendix B Errors 46 Warning Messages 46 Fatal Errors 47 Appendix C Sensitivity Test Record Sheet 48 Appendix C Sensitivity Test Record Sheet cont 49 ...

Страница 6: ...Contents Agilent Electrothermal Temperature Controller ETC 60 User s Guide 6 This page is intentionally left blank ...

Страница 7: ...l phases of operation maintenance and service of this instrument To ensure continued safety of the instrument after maintenance or service procedures verify the instrument is returned to a safe state for the user This includes running performance checks to verify the instruments safety systems are functioning correctly Check the general condition of the instrument during operation for wear or sign...

Страница 8: ...ecified by the manufacturer the protection provided by the equipment may be impaired Hazard Warnings In addition to the hazard warnings specified in your spectrometer operation manual specific hazard warnings have been included in this operation manual These warnings state the hazard describe how to avoid it and specify the possible consequences of not following the instructions Read all warnings ...

Страница 9: ...and rating stipulated in the text adjacent to the fuse holder Always ensure the accessory is turned off and disconnected from the mains supply before attempting any replacement Chemical Hazards Operation of an Agilent AA spectrometer may involve the use of materials that are corrosive or otherwise hazardous Careless improper or unskilled use of these materials can cause serious personal injury or ...

Страница 10: ... documentation or on the instrument itself are as follows Corrosive liquid Electrical shock Eye hazard Hot surface Noxious gas Sharp objects The following symbol may be used on warning labels attached to the instrument When you see this symbol refer to the relevant operation or service manual for the correct procedure referred to by that warning label Information Symbols The following symbols appe...

Страница 11: ...g on the instrument and any associated accessories have been color coded to represent the status of the instrument or accessory A green light indicates the instrument is in normal standby condition A blue light indicates that operator intervention is required An orange light indicates a potential hazard A red light indicates danger or an emergency ...

Страница 12: ...Safety Practices and Hazards Agilent Electrothermal Temperature Controller ETC 60 User s Guide 12 This page is intentionally left blank ...

Страница 13: ... incurred in flame heating of the tube due to the elimination of the costs of flame gases The ETC 60 workhead may also be used on Zeeman graphite furnace systems as the heat source to atomize analyte hydrides The ETC 60 consists of a Temperature Control Module and a workhead containing a quartz absorption tube It is designed to operate with an Agilent AA Series spectrometer and the Agilent VGA 77 ...

Страница 14: ...lly open the packages and inspect all parts for damage in transit Report damaged or incorrect items immediately In addition to this manual you should have received one of each of the following items Figure 2 Workhead Figure 3 Adapter for flame instruments Figure 4 Pack of cells Figure 4 Temperature control module Figure 5 Power cable Figure 6 Temperature sensor cable ...

Страница 15: ...s not exceed 1025 C On start up the system checks that the temperature sensor is working correctly The front panel consists of a two line display and five keys The display keys correspond to menu items on the display Display Keys k5 k4 k3 k2 k1 Figure 9 Front panel of the ETC 60 Mounted in the back panel are the following connectors Mains power inlet with mains power switch and fuse holder which a...

Страница 16: ... element is a specially designed high temperature filament The temperature sensor is in direct contact with the quartz tube to enable a rapid temperature response The quartz cell heating element and temperature sensor are insulated by inert alumina and silica wool WARNING Sharp Objects Broken glass can cause severe cuts to hands Handle the workhead with care as the sidearm of the quartz tube is fr...

Страница 17: ...trol Module immediately below the mains power supply socket as shown in Figure 11 The ETC 60 operates on 100 120 VAC 220 240 VAC 50 60 Hz It is shipped with 220 240 V selected Figure 11 Power switch mains connection and fuse holder voltage selector Do not replace power cord with one of a lower rating than specified Use only Agilent supplied power cord for your country Check that the correct voltag...

Страница 18: ...tate the holder selector so that the required voltage range is at the bottom 4 Remove the fuse from the upper left side of the fuse holder and place it into the socket on the right side of the holder 5 Replace the holder selector into its socket so that the triangles on the lower edge of the holder selector line up and indicate the selected voltage range Installation Overview While the individual ...

Страница 19: ...cedure ensure the instrument has had ample time to cool down to avoid burning your hands Installing the Workhead Bracket Flame Models To install the workhead bracket 1 Remove the upper and lower flame shields from the spectrometer Figure 13 Removing upper left and lower right flame shields 2 Remove the chimney Figure 14 Removing the chimney ...

Страница 20: ...er s Guide 20 3 If it is fitted remove the burner from the spraychamber Figure 15 Removal of burner in flame models 4 Remove the spraychamber and store it in the stand provided Figure 16 Spraychamber in stand 5 Loosen the two heat shield screws Figure 17 Heat shield screws ...

Страница 21: ...hode lamp signal in your instrument Search for Aligning lamps in the SpectrAA Help Open Aligning Lamps 55B 240 280 AA for instructions 8 Fit the two lugs on the workhead bracket into the two holes on top of the burner adjuster Figure 19 Preparing to fit the workhead bracket Figure 20 Workhead bracket fitted to the burner adjuster Bracket Bracket support Thumb screw not shown Burner adjuster Bracke...

Страница 22: ...Bracket Installation on Zeeman Instruments Additional steps must be performed before installing the ETC workhead bracket on a Zeeman instrument 1 Remove the PSD 120 autosampler if present 2 Remove the Zeeman workhead from the instrument Refer to the 240 280 instrument user manuals for detailed instructions Cell Holder and Adapter Removal The standard cell holder must be removed to allow installati...

Страница 23: ...he Zeeman Workhead removed hook the adapter fitted with the ETC 60 bracket on the top rear edge of the sample compartment See Figure 25 on Page 24 3 Continue to Installing the Workhead on Page 23 Installing the Workhead Figure 23 The ETC 60 workhead Temperature cable connection Quartz cell Spray chamber adapter Inlet cell stem Back of workhead Front of workhead Pivot point Pivot point Bracket Brac...

Страница 24: ...mperature cable connected to the workhead An older style cell heater cable is shown NOTE The pins on the connector are sized differently and will only fit one way 2 Fit the ETC 60 workhead into the hole in the bracket and push down firmly to seat it in the bracket See Figure 20 on Page 21 Figure 25 ETC 60 workhead installed Flame instruments left and Zeeman instruments right ...

Страница 25: ...al RS232 cable if required NOTE The RS 232 connector on the back panel of the control module is used to download software upgrades to the ETC 60 Plug in the RS 232 cable option to this connector and connect the other end of the cable to your computer This connection allows direct control of the temperature settings from within the SpectrAA software version 5 or later 7 Optimize the workhead positi...

Страница 26: ...lass can cause severe cuts to hands Handle the workhead with care as the sidearm of the quartz tube is fragile and easily broken 2 Undo the latches on the ETC 60 workhead cover and open the cover 3 Carefully place the cell into the workhead Ensure that the inlet stem is located in the groove at the front of the workhead Figure 29 Cell placed in workhead 4 Carefully close the workhead cover and sec...

Страница 27: ...7 Installing the VGA 1 Mount the VGA on to the instrument as outlined in the manual that ships with the accessory 2 Carefully connect the other end of the black fluoroelastomer tubing on the inlet cell stem to the outlet of the VGA gas liquid separator The system is now ready for use ...

Страница 28: ...Getting Started Agilent Electrothermal Temperature Controller ETC 60 User s Guide 28 This page is intentionally left blank ...

Страница 29: ...being pumped under pressure If a leak occurs these acids could cause serious personal injury Always wear approved safety glasses warranted to protect the eyes Never pump concentrated sulfuric acid through the VGA The ETC replaces the air acetylene flame as a heat source to atomize the analyte hydrides When using the Agilent ETC 60 you will need to select the ETC 60 option in the Vapor mode paramet...

Страница 30: ...ition is attempted with the card in place the flame will light but will be extinguished when the ignite button is released Power Up Ensure that the ETC 60 is correctly installed as previously detailed turn on the power switch to power up the module The ETC 60 will perform a self test that takes a few seconds If all functions are operating correctly the display will show the following M V1 30 ETC 6...

Страница 31: ...operated normally due to the error New software can be downloaded to the ETC 60 from a PC by the serial interface Contact Agilent for more information or to obtain assistance from an Agilent field service engineer NOTE If the temperature control module is switched on without the thermocouple connected the ETC 60 will go into a permanent error state when the self test is complete To clear this erro...

Страница 32: ...ious menu start start the method increase decrease the selected parameter Methods With the ETC 60 you can run the following types of methods Predefined isothermal Manual isothermal Manual step Predefined Isothermal Methods The following standard methods are predefined in the ETC 60 all are for 15 minutes for use with earlier versions of SpectrAA software Table 1 Predefined isothermal methods As Sb...

Страница 33: ... parameters according to the Changing Settings section Page 34 NOTE Any changes to a method are saved automatically even if the temperature control module is switched off To start the method select start The display changes METH As T_start Time 15 00 138 C stop 925 C 15 00 hold When the start temperature is reached the time will start to count down Key k1 is now a toggle switch to hold or restart ...

Страница 34: ...ompletion of the previous step so the time is already running while the cell is heated to the set temperature of the next step The last step in the step program is just large enough to reach the end temperature Changing Settings To change a setting select the key corresponding to the parameter you want to change You will see the change menu OK To change the setting press and hold the appropriate k...

Страница 35: ...oximately 50 mL min of inert gas will flow through the VGA Timer sockets are available from most commercial electrical or department stores You should carefully check that the equipment connected to the timer socket does not exceed the rated capacity of the socket When calculating the required setting for a timer switch be sure to consider the time taken for on going instrument calibration The ope...

Страница 36: ...ld cause severe burns Always ensure that the workhead is allowed to cool before attempting to remove it from the sample compartment The ETC 60 MUST be switched off at the power switch and the mains cable disconnected from the mains supply BEFORE any attempt is made to remove or replace the workhead or the cables connecting the workhead to the Temperature Control Module ...

Страница 37: ...mization of analyte hydrides at the appropriate temperature for each analyte The temperature of the electrically heated quartz tube is generally lower than that of the flame heated quartz tube and so the residence time of atoms in the quartz tube is longer than when a flame is used This results in greater residence times for the atoms in the light path resulting in an increase in sensitivity Typic...

Страница 38: ...ll WARNING Noxious Gas Mercury Hg vapor is highly toxic Always ensure that laboratory safety practices governing the use handling and disposal of mercury containing materials are strictly observed These safety practices should include ensuring adequate ventilation to minimize exposure to the vapor and adherence to local environmental regulations regarding its subsequent release into the atmosphere...

Страница 39: ...nt time to read 30 s four replicates and Delay time to 0 s 4 Set the signal graphics to display 0 250 sec and an Absorbance range of 0 20 1 00 A 5 Pump a solution of the analyte 10 20 ppb through the system 6 Press Read and monitor the signal graphics When a stable signal has been achieved increase the temperature by 50 C and then monitor the signal graphics NOTE Do not exceed 300 C when optimizin...

Страница 40: ...Analytical Notes Agilent Electrothermal Temperature Controller ETC 60 User s Guide 40 This page is intentionally left blank ...

Страница 41: ... Replacing the Fuse WARNING Electrical Shock To prevent reduced safety protection or unwanted fusing a blown fuse should be replaced with one of the size and rating stipulated in the text adjacent to the fuse holder Always ensure the accessory is turned off and disconnected from the mains supply before attempting any replacement To replace the fuse 1 Remove the fuse holder from the rear panel of t...

Страница 42: ...the Y tail Typically less than 0 5 mL will be collected during 8 hours of operation The best indication of whether a quartz cell has reached the end of its lifetime is sensitivity You should keep a record of cell sensitivity for each of the elements you determine and update it at the start of each analysis An example of a table for tracking sensitivity is provided in Appendix C The quartz absorpti...

Страница 43: ...fully close the workhead cover and secure the latches 8 Reconnect the black fluoroelastomer tubing from the outlet of the VGA gas liquid separator to the inlet cell stem taking care not to shift the workhead position If necessary reoptimize the workhead position using the burner adjuster controls 9 Reconnect the mains power cable to the ETC 60 temperature control module The system is now ready for...

Страница 44: ...Maintenance Agilent Electrothermal Temperature Controller ETC 60 User s Guide 44 Removal of the workhead is the reverse of the installation procedure outlined in Installing the Workhead section Page 19 ...

Страница 45: ...perature range Ambient 1025 C Temperature precision 1 C Power consumption 550 VA max Fuse rating 100 120 VAC T6 3AH250V 220 240 VAC T3 15AH250V Thermocouple Type K NiChrome Nickel Operating voltage 100 120 VAC 220 240 VAC Frequency 50 60 Hz Mains power connector Three pin male standard IEC type Environmental Condition Altitude Temp C Humidity RH non condensing Non operating transport 0 2133 m 0 70...

Страница 46: ...atile memory where the calibration data is stored The default calibration data is reloaded and this might slightly decrease the temperature accuracy Please check with your Agilent field service engineer WAR_ALL_DFLT_EEPROM Checksum error in the nonvolatile memory where methods LCD contrast and LCD backlight are stored The default settings are restored Check settings and change if necessary then sw...

Страница 47: ...Possible cause is a defective power circuit ERR_HARDWARE General error in the main printed circuit board ERR_AMB Ambient temperature is out of range for correct operation or the ambient temperature measurement is faulty Check the operating environment ERR_T_HIGH_OR_TH_CPL or ERR_THERMO_CPI Probably a disconnected or faulty thermocouple cable Switch off the ETC 60 check the thermocouple cable and t...

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Страница 50: ...Appendices Agilent Electrothermal Temperature Controller ETC 60 User s Guide 50 This page is intentionally left blank ...

Страница 51: ......

Страница 52: ...ing Started Operation Analytical Notes Maintenance Appendices This information is subject to change without notice 8510137200 8510137200 8510137200 Edition 08 21 Issue 10 Printed in Malaysia Agilent Technologies Inc 2021 Agilent Technologies Australia M Pty Ltd 679 Springvale Road Mulgrave VIC 3170 Australia ...

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