Valco Instruments Co. Inc. TCD Скачать руководство пользователя страница 20

16

Installation

The test chromatogram accompanying your TCD was obtained under the
following conditions:

Sample:

~100 ppm blend in Helium balance

Sample volume:

250 µl

Column:

10' x 1/16" x 0.040" molecular sieve 5Å micropacked

Column flow:

6 mL/min

Reference flow:

6  mL/min

Column temperature: 65°C
Detector temperature: 100°C
Filament temperature: 230°C (a setting of 5.0)
Carrier gas:

Helium

Balancing the Channels

 using LCD Display

The LCD display indicates the signal level from the recorder/chart output.

10. Set the recorder switch to A, and use the coarse and fine controls for

Channel A to adjust the signal level to about 300 mv.

11. Set the recorder switch to B and repeat the same process to adjust the

signal level to about 200 mv.

12. Set the recorder switch to A-B.  The display should read about 100 mv.  If

the signal levels drifts below zero, readjust the A & B channels.

The detector is now ready for analytical use.

Balancing the Channels 

using Recorder/Chart Output

10. Use the zero (or shunt) setting on the recorder to set the true zero on the recorder.

11. Set the Recorder switch to A, and use the coarse and fine zero controls

for Channel A to bring the recorder pen on scale and to a position
approximately 1-2 cm above zero.

12. Set the Recorder switch to B, and repeat the same process, bringing the

pen to a position 

half as far above zero as the pen for Channel A.

13. Set the Recorder switch to A - B, and observe the recorder pen position.

It should be above the true zero position, but below the position for
Channel A.  If the pen drifts below zero, readjust the A and  B channels.

The detector is now ready for analytical use.

Balancing the Channels 

using Unattenuated Outputs

10. Connect the output cable to the A connector, and use the coarse and fine

zero controls for Channel A to bring the baseline signal on scale and to a
position approximately 100 mV above zero.

11. Move the output cable to the B connector, and use the coarse and fine

zero controls for Channel B to bring the baseline to a position half as far
above zero as for Channel A (the value of A minus B).

12. Move the output cable to the A - B connector, and observe the baseline

signal. It should be above the true zero position. If the signal drifts below
zero, readjust the A and  B channels.

The detector is now ready for analytical use.

Single filament mode

The basic procedures and temperature settings described for referenced
mode operation can also be applied to operation in the single filament or
independent mode.  Both channels must have the same carrier gas; you
cannot use helium carrier in one channel and nitrogen in the other.  Also be
aware of the possibility of detector cross-talk when components elute from
the columns in concentrations greater than 1%.

Содержание TCD

Страница 1: ...struction Manual Valco Instruments Co Inc 800 367 8424 sales 713 688 9345 tech 713 688 8106 fax valco vici com VICI AG International Schenkon Switzerland Int 41 41 925 6200 phone Int 41 41 925 6201 fax info vici ch North America South America and Australia Oceania contact Europe Asia and Africa contact ...

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Страница 3: ...em Purity 7 Recommended Carrier Gas Purifiers 7 Carrier Gas Selection 7 GC Column Selection 8 Installation General Precautions 9 Mounting the Detector on the GC 9 Gas Connections 10 Column Connection 12 Electrical Connections 13 Initial Power Up 15 Troubleshooting Troubleshooting Chart 17 Heater Fault Determination 17 Detector Fault Determination 18 Maintenance Bake Out Procedure 19 Disassembly an...

Страница 4: ...This page intentionally left blank for printing purposes ...

Страница 5: ...lament with reference gas This constant temperature provides longer filament life and safeguards it from the extremely high temperatures and oxidation which can occur with high concentrations of oxidative or corrosive components Optional signal referencing is provided to minimize background variables such as column bleed and temperature programming Figure 1 Unique dual filament design Cell volume ...

Страница 6: ...ng terminals are connected to the protective earth contact of the mains inlet The instrument operates with a three conductor power cord having a pro tective earthing conductor and a plug with an earthing contact The mains line plug shall only be inserted in a socket outlet provided with a protective earth contact The protective action must not be negated by the use of an extension cord without a p...

Страница 7: ...mm ID x 0 8 mm OD capillary column 2 FS1R 8 1 16 zero dead volume nut 2 ZN1 1 16 zero dead volume ferrule 2 ZF1 Table 1 Components of the TCD2 NIFE system Description Quantity Product number Detector cell Tungsten Rhenium filament 1 TCD2 WRE Controller unit with power cord 1 TCD2 C Includes Cable output 2 I 24010 1 16 zero dead volume union 2 ZU1C Fused silica adapter for 0 53 mm ID x 0 8 mm OD ca...

Страница 8: ...tor should first be gently warmed without power applied The fail safe mechanism will also act under any condition resulting from loss of control e g over heating RTD failure etc If proper procedures have been followed and the controller will not heat the detector there is cause to suspect that the fail safe mechanism has been activated Consult the factory or an authorized representative Note that ...

Страница 9: ...igure 2 Front panel controls Figure 3 Actual filament temperature vs filament temperature knob settings ACTUAL TEMPERATURE IN C FILAMENT TEMPERATURE KNOB SETTING 0 1 2 3 4 5 6 7 8 9 10 0 50 100 150 200 250 300 350 400 ...

Страница 10: ...her recording means For convenience full scale 0 1V and 0 10V outputs are provided with an internal signal reference at zero volts For best noise performance the shield earth and signal reference should not be connected together DETECTOR connector For connection to the detector control and heating system NOTE These terminals are for connection only to equipment having no accessible live parts Intr...

Страница 11: ...2 which utilize a rare earth gettering alloy to effectively remove contaminants are recommended for ppm level analysis of permanent gases For other applications economical and convenient VICI Mat Sen purifiers are appropriate Order the P300 1 for nitrogen P200 1 for hydrogen or the P100 1 for helium and other inert carrier gases Carrier Gas Selection The detector s response to a component is based...

Страница 12: ...d be adequate for other components There is no absolute best choice of carrier gas For any situation the choice must take into account all of the parameters involved column characteristics components of interest and their concentrations safety considerations carrier cost etc GC Column Selection Cell volume has been minimized to accommodate capillary megabore and micropacked columns and to optimize...

Страница 13: ... column inlet extending into the oven If you are replacing an existing detector you can usually just remove it and set the TCD2 in its place If not use a drill or chassis punch to drill a hole of the proper size and set the detector in position While trying to match base plate mounting holes to every GC on the market is impractical we have located the mounting holes so that at least two of them wi...

Страница 14: ... below illustrates gas connections for a typical TCD2 detector system in referenced and unreferenced modes Since the distance from the carrier supply to the GC varies from installation to installation we do not supply tubing to go from that point to the GC Installation GAS CHROMATOGRAPH COLUMN INJECTOR TEE ZT1 PURIFIER CARRIER GAS 99 999 purity FLOW CONTROLLERS DETECTOR CHANNEL A INLET gold ferrul...

Страница 15: ...is system Installation Installing and Purging a Purifier 1 If the pressure regulator has a 1 8 male cone type outlet port install the Valco 1 8 external to 1 16 internal reducer EZR21 if it has a 1 4 male cone type outlet port install the Valco 1 4 external to 1 16 internal reducer EZR41 For other regulator outlet fittings a wide variety of Valco adapters are available 2 Remove the cap from the in...

Страница 16: ...y one channel with the other capped off as long as the filament temperature control knob of the unused channel is set to zero The unreferenced mode has certain limitations there is a possibility of detector cross talk interference if compound concentrations exceed 1 and baseline drift and background noise are greater than with the referenced mode To make column connection as convenient as possible...

Страница 17: ...er on To test for leaks 1 Insure that both outlets are capped 2 Pressurize the entire system with helium to 138 kPa 20 psi 3 If the system does not hold pressure check all the fittings with an electronic helium leak detector DO NOT use leak detecting liquids Electrical Connections Before connecting the detector cable to the control module make sure that the control module power cord is unplugged 1...

Страница 18: ...V INLET A INLET B CHANNEL A CHANNEL B MODEL TCD2 C 115 230 175VA MAX T2 0A 250V MAINS Figure 9 Electrical connections 2 Connect the data output s The A B A B outputs are used with an integrator or PC based data acquisition system the chart output is for a strip chart recorder Polarities and full scale range are indicated in the figure below Set the recorder DAQ for the same voltage scale 3 Connect...

Страница 19: ...tlet Initial Conditioning 4 Turn on the control module main power switch and set the detector temperature to 220 C 5 Turn on the filament power switch and set both filament temperature knobs at 8 0 6 Condition the detector by allowing it to bake at these settings for at least 12 hours Temperature Settings 7 After the initial bakeout period set the detector temperature at 100 C or at the column tem...

Страница 20: ...the same process bringing the pen to a position half as far above zero as the pen for Channel A 13 Set the Recorder switch to A B and observe the recorder pen position It should be above the true zero position but below the position for Channel A If the pen drifts below zero readjust the A and B channels The detector is now ready for analytical use Balancing the Channels using Unattenuated Outputs...

Страница 21: ...assistance from Valco Instruments call 713 688 9345 or email tech_usa vici com Try referenced mode page 12 Heater Fault Determination The heater control circuit is designed to disable itself in the event of a fault such as over temperature shorted heater short open temperature sensor etc Once disabled circuit operation is restored by turning off the controller disconnecting and reconnecting the de...

Страница 22: ...low shows the pin numbering and connections for the detector cable view into pins Nominal resistance values in ohms at 25 C are shown Unshaded boxed without numbers represent open circuits and should in no case be blow 1 MΩ Resistance values given should be within 10 of the nominal values Pin 1 2 3 4 5 6 8 9 11 12 13 2 3 4 0 5 25 25 6 108 8 9 0 11 12 25 25 13 0 14 50 Troubleshooting ...

Страница 23: ... taken in its use Bake Out Procedure Under normal conditions theTCD requires no routine maintenance However if the detector is exposed to chemicals which may condense or polymerize within the detector and adversely affect performance the detector cell can be baked out at elevated temperatures up to 300 C Inert carrier gas flow other than hydrogen oxygen or air should be maintained during the recon...

Страница 24: ... devices to the goods This Limited Warranty does not cover expendable items This warranty is VOID when repairs are performed by a nonauthorized service center or representative For informa tion about authorized service centers or representatives write Customer Repairs Valco Instruments Company Inc P O Box 55603 Houston Texas 77255 or phone 713 688 9345 At Seller s option repairs or replacements wi...

Страница 25: ...r Model Serial Number Date of purchase Operator Filament temp C Detector temp C Detector flow Noise level Sample Comments Initial power up IPU 100 IPU detector to analysis temp IPU column installed Ambient IPU column to analysis temp TCD2 A B ...

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