Performing an Instrument and Detector Calibration

The Calibration tab is accessed by clicking 'Calibration' in the navigation panel on the left of the Instrument window. 

• Detector calibration
• Instrument calibration

Performing a Detector Calibration

A detector calibration can only be performed with the plasma off and the chiller will need to be on to cool the camera to -40 °C. The Instrument Calibrate button will be unavailable until the detector calibration is done.

The detector calibration performs a dark current calibration to correct for detector and electronic background signals.

To perform a detector calibration, once the camera has reached the correct temperature, click Calibrate in the Detector section.

Performing an Instrument Calibration

The following information explains how to perform an instrument calibration. The calibration consists of a wavelength calibration. To perform the instrument calibration, you will need to use a pre-made calibration solution or make up a calibration solution. To do this see Preparing the instrument calibration solution.

An instrument calibration needs to be performed the first time the instrument is run, when new software is loaded, when drift correction lines are added or removed, and when the Polychromator purge gas is changed. The gases that can be used for purge are either Ar or N₂.

It is recommended that an instrument calibration be performed monthly thereafter.

An instrument calibration can only be performed if a valid detector (dark current) calibration has been performed on the instrument.

Before starting the system, carefully read the Safety practices and hazards section in your ICP-OES User's Guide and ensure that the laboratory is set up according to the specifications listed in the Agilent ICP-OES Site Preparation Guide. Check that the snout, cone, torch and all tubing on the spray chamber, nebulizer and peristaltic pump are correctly connected.  

To perform an instrument calibration:

Ensure a standard glass concentric nebulizer, a double pass spray chamber and the appropriate torch are installed. Use manual sampling. Use 'white/white' peristaltic pump solution tubing and 'blue/blue' tubing for the drain. The tubing tab color denotes the tubing size.

1. Turn on the external instrument exhaust and ICP-OES power to the instrument (if you have not already done so).
2. Open the ICP Expert software.
3. Turn on the plasma by clicking Plasma On or by pressing F5 on the keyboard.

The plasma will take approximately 60-80 seconds to ignite. If it fails to ignite, see Plasma not igniting for further information.

Tip Calibration can only be done when the polychromator has heated to 35 °C and stabilized. If starting from instrument shut down, this can take approximately 2 hours. For optimum analytical performance, it is recommended that the plasma is turned on from standby mode at least 20 minutes prior to analysis to allow it to stabilize. If the instrument has been turned off for an extended period of time, a longer warm up may be necessary.

4. Click Instrument in the top toolbar.
5. Click the Status tab and then select Polychromator Boost (used if analyzing UV wavelengths below 189 nm*).

   Leave the polychromator boost purging for at least 20 minutes prior to performing the instrument calibration.

6. Select Snout purge (when using the radial viewing mode and analyzing below 189 nm*) on the Status tab.

   If you are not going to be analyzing UV wavelengths below 189 nm, you can choose not to have the polychromator boost and snout purge on. However, wavelengths below 189 nm will have a red cross next to them on the results table.

   *It is highly recommended that the Polychromator Boost purge and Snout (when using the radial viewing mode) purge be on when performing an instrument calibration. If you do not intend to measure wavelengths under 189 nm, turn off the Polychromator Boost and Snout purge after the calibration is finished.

7. If you are using an AVS accessory click the link for instructions. Otherwise, continue to Step 8.
   • AVS 6/7
   • AVS 4 using an autosampler
   • AVS 4 performing the procedure manually
8. Place the solution tubing from the peristaltic pump into the wash solution and the drain tubing into the drain vessel.
9. Turn on the pump to begin aspirating the solution.
10. Adjust the pressure bars for even sample flow. See Adjusting the pressure on the pump tubing.
11. Click Instrument in the top toolbar and then click Calibration on the left navigation bar.
12. Select Use axial configuration during calibration ONLY if you plan to perform the instrument calibration in axial view (for VDV/SVDV instruments only). If this option is not selected, the instrument calibration will be performed in radial view.
13. Select Organic wavelength calibration ONLY if you plan to perform a calibration using wavelengths and settings specific to organic analysis.
14. Remove the solution tubing from the wash solution. Wipe the tubing with a lint free tissue and transfer it into the instrument calibration solution.
15. Once the instrument calibration solution is aspirating, click Calibrate in the Instrument section.

After a short while, an indication of the success or failure of the calibration will appear, as well as an indication of the wavelength offsets.

The results of the wavelength calibration are stored as text files and are saved to text files entitled 'Calibrationdetaillog.txt' and 'Calibrationsummarylog.txt' located in the following directory:
C:\ProgramData\Agilent\ICPExpert\Log\Instrument serial number\Result.txt
 

Tip If the calibration fails, check the sample introduction system components. If the system components seem fine, prepare a new instrument calibration solution and try again. If the calibration failure is with the low UV wavelengths such as Al it is most likely that a longer polychromator (optics) purge time is required or the Polychromator boost is off and/or the snout purge is off. If the failures are more wide spread, prepare a new wavelength calibration solution and try again. You can also examine the Calibrationdetaillog.txt or Calibrationsummarylog.txt file and determine which elements failed the calibration.

Performing a wavelength calibration with an AVS 6/7

1. Disconnect the rinse/carrier supply tubing from the inlet end of the peristaltic pump tubing.
2. Connect appropriate tubing (if required) and place it into wavelength calibration solution.
3. Turn on the pump to begin aspirating the solution.
4. Adjust the peristaltic pump pressure bars for even sample flow (if needed). See Adjusting the pressure on the pump tubing.
5. Click Instrument in the top toolbar and then click Calibration on the left navigation bar.
6. Select Use axial configuration during calibration ONLY if you plan to perform the instrument calibration in axial view (for VDV/SVDV instruments only). If this option is not selected, the instrument calibration will be performed in radial view.
7. Select Organic wavelength calibration ONLY if you plan to perform a calibration using wavelengths and settings specific to organic analysis.
8. Once the wavelength calibration solution is aspirating, click Calibrate.
9. When the calibration is complete, reconnect the rinse/carrier supply tubing.
10. Rinse thoroughly before beginning an analysis.

After a short while, an indication of the success or failure of the calibration will appear, as well as an indication of the wavelength offsets.

The results of the wavelength calibration are stored as text files and are saved to text files entitled 'Calibrationdetaillog.txt' and 'Calibrationsummarylog.txt' located in the following directory:
C:\ProgramData\Agilent\ICPExpert\Log\Instrument serial number\Result.txt
 

Tip If the calibration fails, check the sample introduction system components. If the system components seem fine, prepare a new instrument calibration solution and try again. If the calibration failure is with the low UV wavelengths such as Al it is most likely that a longer polychromator (optics) purge time is required or the Polychromator boost is off and/or the snout purge is off. If the failures are more wide spread, prepare a new wavelength calibration solution and try again. You can also examine the Calibrationdetaillog.txt or Calibrationsummarylog.txt file and determine which elements failed the calibration.

Performing a wavelength calibration with an AVS 4 and an autosampler

1. Fill an appropriate sample tube with wavelength calibration solution and load it into a vacant rack position on the autosampler.
2. Click Autosampler on the toolbar.
3. On the rack image, click on the tube position that the wavelength calibration solution was placed in and then click Move and Lower Probe.
4. Turn on the pump to begin aspirating the solution.
5. Adjust the peristaltic pump pressure bars for even sample flow (if needed). See Adjusting the pressure on the pump tubing.
6. Click Instrument in the top toolbar and then click Calibration on the left navigation bar.
7. Select Use axial configuration during calibration ONLY if you plan to perform the instrument calibration in axial view (for VDV/SVDV instruments only). If this option is not selected, the instrument calibration will be performed in radial view.
8. Select Organic wavelength calibration ONLY if you plan to perform a calibration using wavelengths and settings specific to organic analysis.
9. Once the instrument calibration solution is aspirating, click Calibrate.
10. When the calibration is complete, move the autosampler probe to the rinse position.
11. Rinse thoroughly before beginning an analysis.

After a short while, an indication of the success or failure of the calibration will appear, as well as an indication of the wavelength offsets.

The results of the wavelength calibration are stored as text files and are saved to text files entitled 'Calibrationdetaillog.txt' and 'Calibrationsummarylog.txt' located in the following directory:
C:\ProgramData\Agilent\ICPExpert\Log\Instrument serial number\Result.txt
 

Tip If the calibration fails, check the sample introduction system components. If the system components seem fine, prepare a new instrument calibration solution and try again. If the calibration failure is with the low UV wavelengths such as Al it is most likely that a longer polychromator (optics) purge time is required or the Polychromator boost is off and/or the snout purge is off. If the failures are more wide spread, prepare a new wavelength calibration solution and try again. You can also examine the Calibrationdetaillog.txt or Calibrationsummarylog.txt file and determine which elements failed the calibration.

Performing a wavelength calibration manually with an AVS 4

1. Disconnect the autosampler probe capillary tube from the inlet end of the peristaltic pump tubing.
2. Connect appropriate tubing (if required) and place it into wavelength calibration solution.
3. Turn on the pump to begin aspirating the solution.
4. Adjust the peristaltic pump pressure bars for even sample flow (if needed). See Adjusting the pressure on the pump tubing.
5. Click Instrument in the top toolbar and then click Calibration on the left navigation bar.
6. Select Use axial configuration during calibration ONLY if you plan to perform the instrument calibration in axial view (for VDV/SVDV instruments only). If this option is not selected, the instrument calibration will be performed in radial view.
7. Select Organic wavelength calibration ONLY if you plan to perform a calibration using wavelengths and settings specific to organic analysis.
8. Once the instrument calibration solution is aspirating, click Calibrate.
9. When the calibration is complete, reconnect the autosampler probe capillary tube.
10. Move the autosampler probe to the rinse position if required.
11. Rinse thoroughly before beginning an analysis.

After a short while, an indication of the success or failure of the calibration will appear, as well as an indication of the wavelength offsets.

The results of the wavelength calibration are stored as text files and are saved to text files entitled 'Calibrationdetaillog.txt' and 'Calibrationsummarylog.txt' located in the following directory:
C:\ProgramData\Agilent\ICPExpert\Log\Instrument serial number\Result.txt
 

Tip If the calibration fails, check the sample introduction system components. If the system components seem fine, prepare a new instrument calibration solution and try again. If the calibration failure is with the low UV wavelengths such as Al it is most likely that a longer polychromator (optics) purge time is required or the Polychromator boost is off and/or the snout purge is off. If the failures are more wide spread, prepare a new wavelength calibration solution and try again. You can also examine the Calibrationdetaillog.txt or Calibrationsummarylog.txt file and determine which elements failed the calibration.

 

See also:

• Status
• Tests