Instrument will give reliable data only if regular maintenance is preformed.
Before Starting the instrument insure the check list has been successfully completed. 1. Turn on the gases and the chiller. There is no on/off switch for the auto sampler. 2. If the Main Instrument switch has been turned off, turn it on. Usually, this switch should remain on to avoid a waiting period for instrument startup. 3. Close the doors to the sample compartment. Be sure that the front door is fully closed and secured. 4. Turn on the autosampler and any other accessories.
Starting the Computer and Software -- To start the computer and software 1. Switch on the computer, monitor, and printer.
2. Click on the Start button. Select Programs PerkinElmer WinLab32, WinLab32 and WinLab32 software starts. To verify instrument configuration 1. Check that the autosampler type and tray are correct. Change, if required. To change the autosampler, exit the software and run the Reconfigure utility. To run the Reconfigure utility, click on Start Programs PerkinElmer WinLab32 Reconfigure. To change the tray, use the Autosampler... command in the Options menu.
2. For all instruments: Check that the peristaltic pump and tubing type are correct. Change if required, using the Pump... command in the Options menu. 3. For the Dual View (DV) instruments: In the Spectrometer Control window, check that the correct plasma viewing mode (axial or radial) is set. Change the viewing mode if required, using the options in the Spectrometer Control window Setting Up and Starting the Peristaltic Pump -- Before setting up the pump do a daily check of the system, started the instrument and accessories, and started the computer and software.
To set up the peristaltic pump 1. Check that the sample tubing and the drain tubing leading from the spray chamber are properly set up on the pump. 2. If the pump tubing is new, gently stretch it. Position the clips on the tubing in front of the tubing stops. 3. Replace the tubing clamps for each channel and swing the cam levers over to apply tension to the clamps. To start the pump 1. Place the sample capillary tubing in a container of a solution whose matrix matches that of the samples (for example: deionized water, diluted acid, or organic solvents). 2. In the Toolbar, click on the Plasma icon or in the Tools menu click on Plasma Control to Display the Plasma Control window. Click on the Pump button to turn on the pump.
3. Adjust the flow rate to 1.5 mL/min for aqueous analysis. (The aqueous analysis default value is 1.5 mL/min.) For organic analysis adjust the flow rate to 0.8 mL/min. (The organic analysis default value is 0.8 mL/min.) 4. If necessary, adjust the tension on the pump tubing, one channel at a time. For the sample tubing, gradually tighten the adjustment screw until the liquid flows smoothly without bubbles. The drain tubing should have a segmented flow of liquid leading to the drain bottle. Bubbles in the drain tubing are normal. Preparing to Ignite the Plasma
(Before beginning this step, be sure the system, instrument, computer, and pump are ready.) Before igniting the plasma Check that a method with the appropriate plasma conditions has been selected. Use the Method button on the toolbar to open a different method. Close and secure the doors to the sample compartment. An interlock will prevent from igniting the torch if the doors are not fully closed. To avoid ignition problems when switching from organic to aqueous solutions, purge organic vapors that may remain in the torch. When the humidity is high (>75%), water can condense on the RF coil of the torch when the torch is not in operation. To prevent damage to the RF coil, use a soft cloth to dry the coil before igniting the torch. If wavelengths below 190 nm will be measured, use the Spectrometer Control window to purge the optical system with nitrogen. A high purge time of approximately 15 minutes is usually sufficient if the instrument has been purging for a long time. Additional purge time may be necessary if the intensity readings are not satisfactory. Before running samples, return the purge rate to normal and take a measurement to insure a steady-state signal, indicating that the high purge time was sufficient. Igniting the Plasma Before beginning this step, be sure the system, instrument, computer, and pump are ready, and that the correct preparations to ignite the plasma. The Ignition Process -- During the ignition process, argon gas flows through the torch and spray chamber, purging the sample introduction system of air. With the argon continuing to flow, power is applied to the RF coil. Then, a high voltage spark is injected into the argon flow causing the argon to ionize. The free electrons that are created then interact with the applied RF field to cause further argon ionization and form a plasma. Messages appear in the Plasma Status display the ignition status. The system sets the plasma gas flows. Then a message reads “Initial Purge” and the system counts down in seconds. The plasma is ignited, the plasma gas flows are then set to the starting plasma conditions of the active method in the Plasma Control Window, or if the override method is selected to those specific set points. At the end of this process, a message reads “Plasma has been ignited.” Viewing the Plasma During Ignition -- When the plasma is ignited, observe it closely through the viewing window. If the plasma is unstable, immediately click the Plasma switch to Off in the Plasma Control window (or press F9) to turn off the plasma; or, press the red Emergency Plasma Off button above the sample compartment. An unstable plasma, as shown in the diagram, can cause the end of the torch to become overheated and to deform. If the deformity is severe, the argon gas flow patterns will be altered, and the torch must be replaced.Pressing the red Emergency Plasma Off button shuts off the plasma directly and bypasses the software. This button can be used if the software hangs up or if communication between the instrument and the computer is interrupted. Using this button does not harm the instrument. When this button is used, reset the system before reignition of the torch. Be sure that the red button is in the “out” position, and select the Reset RF Emergency Off command in the System menu.
1. Before started the pump, place the sample capillary tubing in a container of a solution whose matrix matches that of the samples for the application (for example: deionized water, diluted acid, or organic solvents). The pump automatically shuts off at the beginning of the ignition sequence and is restarted at the end of the ignition sequence. 2. Click the Plasma switch to On in the Plasma Control window (or press F9) to turn on the plasma.
The Plasma Status display indicates when the plasma has been ignited. 3. Immediately examine the plasma through the viewing window. Viewing the Plasma During Ignition. After ignition of the plasma, be sure to observe it closely through the viewing window. If the plasma is unstable, immediately click the Plasma switch to Off in the Plasma Control window (or press F9) to turn off the plasma; or, press the red Emergency Plasma Off button above the sample compartment. An unstable plasma, as shown in the diagram, can cause the end of the torch to become overheated and to deform. If the deformity is severe, the argon gas flow patterns will be altered, and the torch must be replaced.
Note Pressing the red Emergency Plasma Off button shuts off the plasma directly and bypasses the software.
This button can be used if the software hangs up or if communication between the instrument and the computer is interrupted. Using this button does not harm the instrument. After use of this button, reset the system before reignition of the torch. Be sure that the red button is in the “out” position, and select the Reset RF Emergency Off command in the System menu.
To proceed if the plasma is stable 1. Wait one hour before running samples. This ensures accurate results, as it allows the temperature of the sample introduction system to fully stabilize. 2. Proceed to Optimizing and Verifying Performance.
To shut off the plasma if the plasma is unstable 1. Click the Plasma switch to Off in the Plasma Control window (or press F9) to turn off the plasma, or press the red Emergency Plasma Off button that is located above the sample compartment. 2. Proceed to Correcting Unsuccessful Ignition. To reignite the plasma after the plasma has been shut off An unstable plasma is usually caused by air leaking into the system. To correct this problem, do the following: 1. Check the torch gas connections.
2. Repeat the ignition procedure. Click the Plasma switch to On in the Plasma Control window (or press F9). The Plasma Status window indicates the ignition status. 3. Immediately examine the plasma as before.
To correct unsuccessful ignition Check this list of possible reasons for unsuccessful ignition. Review the Instrument Message history which is found on the Plasma Tab of the Diagnostics window. Correct the problem if possible, and then try to ignite the plasma again. Plasma Conditions Using the correct plasma conditions for the application. Check the Sampler: Plasma page in the Method Editor. Ignitor Cable or Contact On instruments with an ignitor cable, check to make sure that the cable is plugged in. On instruments with an ignitor contact, check that the copper strip on the torch is in close proximity to the ignitor contact finger. Exhaust vent -- Be certain the exhaust vent is operating properly and is not blocked. Operation of the exhaust vent is required to establish proper argon gas flow patterns as well as for safety reasons. Air leaks -- An unstable plasma is usually caused by air leaking into any part of the torch, nebulizer, or spray chamber. To correct this problem, do the following: Check the torch gas connections. Check that the torch O-rings are in good condition. Replace cracked or worn O-rings. Drain -- Check that the fitting on the spray chamber drain is secure. Be sure that the pump is properly draining the spray chamber and that the drain liquid is not backing up into the spray chamber. Nebulizer end cap -- Check that it is tightly secured to the spray chamber. Sample capillary and tubing -- Check that one end is attached to the nebulizer and that the other end is immersed in solution.
Optimizing and Verifying Performance Before proceeding, insure the setup is completed. Performance checks Performance checks should be done regularly to help assure acceptable performance. The frequency of using these checks depends on how critical analytical the precision must be in each application. To help assure acceptable performance and to monitor instrument condition, it is suggested that a log be maintained. These tests include: • Sodium bullet test, where the aspiration of a solution of 1000 mg/L or more of sodium should produce a defined “bullet” in the center of the plasma discharge. This test allows the user to visualize the sample flow in the plasma, to evaluate proper sample introduction.
• Background Equivalent Concentration (BEC) test, which is a useful indicator of the relative sensitivity of the instrument for a particular emission line. The BEC value is the concentration of an element which would produce the same emission intensity as the plasma background measured at the analyte wavelength. The BEC checks torch alignment, plasma viewing height (only meaningful in radial view), nebulizer gas flow rate, and incident RF power. • Precision Test, which expresses the short-term precision for several measurements for a strong emission line. This test indicates the Relative Standard Deviation (RSD) of the instrument's analyte emission intensity or concentration measurements. The RSD may also be referred to as the CV (Coefficient of Variation). A high RSD or CV is usually indicative of a problem with the sample introduction system such as improper drainage, leaks, improper tension on the pump tubing, worn pump tubing, or nebulizer problems. • Detection Limit Test, which measures the noise of the baseline signal in concentration units to give an indication of the lowest concentration of an element which can be measured. The detection limit is calculated as three times the standard deviation of the blank. To make performance checks Use the following procedures in sequence or use the Browse buttons to move through each procedure. 1. Sodium Bullet Test 2. Creating a Method for the Performance Checks 3. Setting Up for the Performance Checks 4. Performing the Background Equivalent Concentration (BEC) Test 5. Performing the Precision Test 6. Performing the Detection Limit Test
Sodium Bullet Test To run the sodium bullet test: 1. For aqueous analyses, aspirate a 1000 mg/L solution of sodium. For organic analyses, aspirate an appropriate organic blank. 2. Examine the plasma through the viewing window in the sample compartment door. A yellow-orange bullet (or green, in the case of organic compounds) should be visible in the center of the discharge, and should extend from the base of the discharge to about 2-3 mm past the RF coil. If the bullet height is unsatisfactory, adjust the nebulizer argon flow in the Method Editor or Plasma Control windows. If no bullet appears or the bullet is faint: • Check the sample must contain sodium at the required concentration. • Check that sample is being pumped to the nebulizer. Make sure that the pump lever is engaged and that the pump tubes are connected appropriately. • Check that the drain is being pumped properly. There will be a segmented flow of bubbles through the tubing. If the above checks fail to make an improvement, turn off the plasma, then check the following: • Check that the nebulizer end cap is connected tightly.
• Check the nebulizer spray pattern: run deionized water for several minutes, then remove the nebulizer end cap. If the nebulizer spray is sputtering or uneven, inspect the nebulizer tips for clogging and clean or replace them as necessary. • Check that the injector is not clogged. Disassemble the torch if there is a clog.
Creating a Method for the Performance Checks
The following procedure describes how to create the method for the BEC, Detection Limit, and Precision tests. This method can be stored and recalled later for periodic performance checks at whatever interval is desired. To create the method for the tests: 1. In the File menu, click on New Method... 2. In the Create New Method dialog, select default conditions for an aqueous analysis. 3. When the Method Editor appears, click on Periodic Table. In the Periodic Table, select manganese using the 257.610 wavelength. Select other elements of interested in using for the performance checks. If available, cadmium or titanium (in addition to manganese) would be good choices to get an overall indication of the instrument's performance. For cadmium, select 226.502 nm; for titanium, select 334.940 nm. 4. Type a description for the method. In the File menu, select Save Method. Type a name for the method such as “perftest” and click on OK. If the plasma has been on, allow five minutes for the torch to cool before ! checking the following. 5. On the Spectrometer: Settings page, select: Read Time: Min 10 sec.; Max 20 sec. Read Delay: 60 sec. for manual sampling; approx. 120 sec. for an autosampler Replicates: 3 6. Click on the Sampler tab. On the Plasma page, select Same for all Elements and use the parameters listed below for axial viewing:
Plasma Flow: 15 L/min Aux Flow: 0.5 L/min Neb Flow: 0.75 L/min RF Power: 1450 W View Dist: 15 mm
7. Click on the Sampler tab. On the Peristaltic Pump page, select: Sample Flow Rate:1.50 mL/min 8. Click on the Process tab. On the Peak Processing page, select: Peak Algorithm: Peak Area Points/Peak: 3 9. Click on the Calibration tab. On the Define Standards page, with one Calibration Blank and one Calibration Standard. On the Calib Units and Concentration page, select 10 mg/L of Manganese. If there are other elements, select the standard concentrations for these elements. Typically, use a concentration 100 times greater than the expected detection limit.
10. Click on the Options tab. For the Results Display and Printed Log, select: Analytical Header, Replicate Data, Means and Statistics 11. In the File menu, select Save Method. Setting Up for the Performance Checks Solutions Do the performance checks with the following solutions:
• Manganese solution: 10 mg/L (in 1% HNO3 or an appropriate acid). Optionally, use a multielement solution containing other elements of interest (at a concentration 100 times greater than the recommended detection limit If available, cadmium or titanium (in addition to manganese) would be good choices to get an overall indication of the instrument's performance. • Blank solution containing deionized water and an appropriate acid to match the sample matrix. • Rinse solution containing deionized water and an appropriate acid. The acid concentration should match the standard and samples. Setting Up for the Tests
To run the tests, use a method. Refer to Creating a Method for the Performance Check. Before running the tests, complete the following procedures: • Detector Calibration • Wavelength Calibration • Torch View Optimization
Performing the Background Equivalent Concentration (BEC) Test How is the BEC Determined? The BEC test determines what concentration of analyte is equivalent to the plasma background at the analyte wavelength. This provides an indication of the sensitivity of the instrument. First perform a calibration by running a blank followed by a standard. The calibration establishes the relation between emission intensity and concentration. A calibration also takes into account the dark current noise. Once the calibration is complete, close the shutter, thereby blocking the light from the plasma source from reaching the detector. At this point, take a reading (at zero intensity). This extrapolates the calibration line backward until it intercepts the concentration axis. The resulting concentration value is negative. Changing the sign to positive, gives the BEC value.
Performing the BEC Test First set up the system for the tests. 1. Check that the method a created for the performance tests (for example,“perftest”, is open. If not, in the File menu, click on Open Method. 2. Click on the Manual icon to open the Manual Analysis Control window. 3. In the Manual Analysis Control window, select Print Log. In addition, to save results, click on Open... and select a Results Data Set Name. 4. Aspirate the blank and click on Analyze Blank. 5. Aspirate the manganese or multielement solution and click on Analyze Standard. This completes the calibration. 6. Aspirate the rinse solution. 7. In the Tools menu, click on Spectrometer Control. 8. In the Spectrometer Control window, close the shutter by selecting the“Closed” option. 9. Click on the Manual Analysis Control window to bring it to the front. For the Read Delay, select Override Method and set the Read Delay to 0. 10. While continuing to aspirate the rinse solution, click on Analyze Sample. (This will give results in concentration units.) 11. Click on the Spectrometer Control window to bring it to the front. Change the shutter from Closed to the Auto position, which returns it to instrument control. Check the results. By taking the negative value and making it a positive value, the BEC for Mn at 257.610 nm. It should be less than or equal to 0.04 mg/L.
Performing the Precision Test Before starting, run the set up the system for the tests. For convenience, run this test after the BEC test. Use a solution of 10 mg/L manganese for the test or, optionally, a multielement solution containing other elements of interest. 1. Be certain the method created for the performance tests (for example,“perftest”) is open. If not, in the File menu, click on Open Method. 2. After the BEC test, the Manual Analysis Control window should be displayed. If not, click on the Manual icon. 3. In the Method Editor, click on the Spectrometer: Settings page and specify 10 replicates. 4. In the Manual Analysis Control window, disable Override Method to use the Read Delay specified in the method. To disable it, click on the box to remove the check mark. 5. Aspirate the manganese or multielement solution. 6. In the Manual Analysis Control window, click on Analyze Sample. Check the results. The RSD should be less than 1.0%.
Performing the Detection Limit Test First have the set up the system for the tests. For convenience, run this test after the BEC or Precision test. Use a solution of 10 mg/L manganese for the test or, optionally, a multielement solution containing other elements of interest. 1. Check that the method created for the performance tests (for example,“perftest”, is open. If not, in the File menu, click on Open Method. Make the following changes to the method: On the Spectrometer: Settings page, select: Read Time: Min 50 sec.; Max 50 sec. Replicates: 20 2. After running the BEC or Precision test, the Manual Analysis Control window should be displayed. If not, click on the Manual icon. 3. Aspirate the rinse solution and rinse sufficiently, after a Precision test (rinse for two minutes). 4. The BEC test, included a calibration so skip to Step 5. Otherwide make a calibration curve: • Aspirate the blank and click on Analyze Blank. • Aspirate the manganese or multielement solution and click on Analyze Standard. Rinse for at least 2 minutes after the standard is analyzed. A full 5-minute rinse is recommended. 5. Aspirate the blank solution. 6. While continuing to aspirate the blank, press Analyze Sample. (This will give results in concentration units.) Note Increasing the Read Time in the method to 50 seconds will provide better detection limits. Check the results. To determine the detection limit, multiply the standard deviation of the blank by three. Compare the results with the required detection limits for the elements. Detection limits for the three elements we suggested for the test are:
Selecting a Workspace, Method, and Sample Information File Before analysis of samples, check the following: windows suitable for the analysis; one or more methods; and a sample information file. To select these items for automated analyses 1. In the File menu, click on Open Workspace... and select the workspace desired. The group of windows (a workspace) that appears to carry out analysis. The Automated Analysis Control window must appear in this workspace. For example, set up a workspace using the following windows; Spectra Display, Results Display, Calibration Display, and Plasma Control or any other windows of choice. If a workspace is not selected it can be selected from individually from the Windows and Tools menus. The selected windows can be saved as a workspace by using Save As Workspace... in the File menu. 2. Select a method on the Automated Analysis Control window Set Up page by double-clicking on the first empty cell in the Method column. In the Open Method dialog, select the method that to be used. 3. To select more than one method, first select Open Methods in List on the Setup page. This option is located below the Methods and Sample Locations table. Repeat Step 2 to select additional methods. 4. Select a sample information file if desired. By using a sample information file, information entered about the samples (for example, sample weights or dilutions) is used in the analysis. In the Automated Analysis Control window Set Up page, click on Open… and select a sample information file in the Open Sample Information dialog.
5. To run samples from a sample information file, first select the check box for Use Sample Information. In the table, under the Sample Info File column, three options appear in a drop-down list. To analyze all of the samples in the sample information file, select All Defined from the dropdown list. To select only certain autosampler locations, select Locations. When the sample numbers listed in the sample information file, select Sample Nos. When selecting Locations or Sample Nos., be sure to enter the autosampler locations or sample numbers in the appropriate columns. Example: 10-15,18,20,22,25-30 - or - If a sample information file is not used deselect the check box for Use Sample Information below the name of the sample information file. Then enter the autosampler locations in the Locations column. Type individual locations or a range of locations. Use commas to separate the locations and ranges. It is not necessary to enter the locations of blanks, QC’s, check or calibration solutions. Enter locations for these to be treated as a sample within the analysis. Example: 10-15,18,20,22,25-30 6. The settings can be saved in a workspace by using Save As Workspace... in the File menu. If a workspace is not selected, select these windows individually from the Windows and Tools menus. The selected windows can be saved as a workspace by using Save As Workspace... in the File menu.
2. In the File menu, click on Open Method... to select a method, If an appropriate method is not there, Create a Method. To select these items for manual analyses 1. In the File menu, click on Open Workspace... to select the workspace. The group of windows (a workspace) that appears enables analysis to be performed. The Manual Analysis Control window must appear in this workspace. Optional windows include: Spectra Display, Results Display, Calibration Display, and Plasma Control.3. A sample information file is optional. Make a sample information file to enter all the sample information before an analysis begins. Create a Sample Information File. If a sample information file is not selected, the software uses the default file called “Untitled.” Be sure to open the Sample Information Editor and check that entries in the “Untitled” file for the appropriate analysis. If some entries are completed, but others are not, the sample concentration may not be reported in sample units. 4. Settings can be saved in a workspace by using Save As Workspace... in the File menu.
Setting Options in Control Window Before analyze of samples, set certain options in the control window. These options are not specified in the method and include: specifying the results data set where data is saved; specifying whether if the results are printed during the analysis; specifying special automatic startup and shutdown options; and specifying automatic export of data.
For all analyses, to select options for the analyses 1. In the Automated Analysis Control window Set Up page or the Manual Analysis Control window, click on Open... next to the Results Data Set Name information field. Select the name of the data set where the results will be saved. If this data set already exists, new data will be added to it. After selecting a results data set name, the Save Data box is selected automatically (a checkmark appears), confirming that data will be saved.
2. To print a log of intensity counts, analytical results, and other information about the analysis, select the Print Log During Analyses box. For automated analyses only, to select other options 1. To be automatically switched off componets when the analysis is finished, first select the Automatic Shutdown box, then click on Set... to open the Automatic Shutdown/Startup dialog. Complete this dialog, and click on OK. 2. For Automatic Startup, use the above dialog to schedule an automatic startup. Also specify whether the plasma is to be ignited and if the pump is to begin operating upon startup. 3. During the analyses, it is possible to automatically export data contained in the results data set and write it into a file that can be read by many other programs, including spreadsheet and database management programs. To do this, select Auto Export, then click on Set... and select the Export Designs. First create the Export Design(s) in the WinLab32 Data Manager. An export design defines a subset of data items that to be exported from a data set.
4. On simultaneous ICP instruments only, select automatic wavelength realignment to occur at regular intervals. Select the Auto Wavelength Realign box on the Automated Analysis Control window Set Up page and, then click on Set... to set a time interval. To view the wavelengths for one element 1. Select an element. 2. Click on All Wavelengths or Recommended Wavelengths to specify the values. The On Arrays option will narrow down the search to just those wavelengths that appear on the subarray.
3. If the Center Wavelength entry field is not clear, double-click on this box and press Delete to clear it. 4. Click on Search. The specified wavelengths for that element appear in the table.
Define Elements Page Use this page to define the symbol, wavelength, name, and function of an element. In the Method Editor, an “element” represents a combination of parameters associated with a measurement at a particular wavelength. When measuring an element at more than one wavelength, repeat the element on this page for each separate wavelength, see the double listing for two chromium wavelengths at the left.
5. Save the menu settings in a workspace by using Save As Workspace... in the File menu.
Arranging Samples Before arranging samples in the autosampler using the autosampler loading list, first entered all information for the samples and solutions in the method or methods and in the sample information file if one exists. To get samples and solutions ready for analyses first Prepare the required samples and solutions according to standard laboratory procedures. To load samples and solutions in the autosampler using the Automated Analysis Control window 1. In the Automated Analysis Control window, click on the Analyze tab. 2. In the System menu, click on Autosampler Loading List to see a list of the locations of the samples and solutions. 3. Load samples and solutions in an empty tray. 4. Click on Load Tray. 5. Place the loaded tray in the autosampler. 6. In the Analysis menu, click on Autosampler Go to Wash.
To load samples and solutions in the autosampler when the Manual Analysis window is open 1. In the System menu, click on Autosampler Loading List to see a list of the locations of the samples and solutions. 2. Load samples and solutions in an empty tray. 3. In the Analysis menu, click on Autosampler Load Autosampler Tray or press Shift-F11. 4. Place the loaded tray in the autosampler. 5. Click on Go to Wash Loc. in the Manual Analysis Control window.
Analyzing Samples Three types of analyses Select a method of analysis from the options below.
Automated Analyses, using an autosampler to analyze all samples and solutions.
Manual Analyses, manually presenting samples and solutions to the instrument
Manual Analyses -- Using the Autosampler, requiring both manual operations and an autosampler to analyze samples and solutions. In this case, often used for method development, direct control of the autosampler, to holding samples for analysis.
Automated Analyses, using an autosampler to analyze all samples and solutions Manual Analyses, manually presenting samples and solutions to the instrument.
Automated Analyses Automated analyses are performed using the Automated Analysis Control window. Other windows such as the Results window are optional.
To perform automated analyses
NOTE: During an analysis, the shutter automatically opens and closes for each sample. If there is an extensive number of samples to analyze, however, set the shutter to the open position manually to increase analytical throughput. Select this in the Spectrometer Control Window. Close the shutter when the analysis is complete. Leaving the shutter in the open position with the plasma on could lead to deterioration of the optics and eventual degradation of UV performance. It is recommended that the shutter be closed when analyses are not being performed.
Examining the Run List To examine the run list before analyzing samples 1. Examine the list of solutions in the run list on the Analyze page of the Automated Analysis Control window. If the method or sample information file is changed, click on Rebuild List to view an updated run list. Verify the run list is correct. If it is correct, skip steps 2 and 3 below.
A sample run list is shown at the right.
2. To make changes to the run list for unknown samples, go to the Sample Information Editor and make the changes in the Sample Information file. To make changes to QC samples, go to the Method Editor and make changes in. the QC section of the method. For matrix-check samples make changes for these samples as defined in the method and scheduled in the sample information file. 3. To make changes to the run list for calibration solutions, go to the Method Editor Calibration: Define Standards Page and make the changes.
4. To analyze a selected group of samples that are a subset of samples in the sample information file, type the locations or sample numbers on the Automated Analysis Control window Set Up page. Example: 10- 15,18,20,22,25-30 Calibrating and Analyzing Samples According to the calibration choices, select the appropriate steps below. All controls (Analyze All, Calibrate, and Analyze Samples) are located on the Automated Analysis Control Analyze page. Select the calibration parameters in the Method Editor Calibration pages and view the calibration curves in the Calibration Display window. View a summary of the calibration data in the Results Display Window.
NOTE: Directly before analyzing aqueous solutions, we recommend that aspirate a solution of deionized water with an acid concentration that matches the calibration blank and standards for at least 10 minutes. This procedure stabilizes the sample introduction system.
Select a calibration option and analyze mode
.
Stopping and Restarting (When an analysis is stopped, the autosampler probe automatically goes back to the wash.)
To stop an analysis -- In the Automated Analysis Control window Analyze page, click on the button used to start the analysis, press F8 (Cancel), or select Cancel Analysis... from the Analysis menu. In the Stopping an Analytical Sequence dialog select the option that indicates how to stop.
To change Set Up options after an analysis has begun. -- Click on the tab for the Set Up page. Change any available set up option. For example, select whether or not to save data, change the sample information file or program an automatic shutdown. On simultaneous ICP instruments, select an auto wavelength realign. Some options are locked. To change any locked option, first click on the tab for the Analysis page and then click on Reset Sequence. For example, change a data set after click on Reset Sequence.
To restart an analysis from a selected solution -- In the Automated Analysis Control window Analyze page, click on the button the originally used to start the analysis. The other buttons will be disabled. In the Continuing an Analytical Sequence dialog, select where the analysis will continue. Tip: The Run List on the Analyze page of the Automated Analysis Control window shows the sample, highlighted in yellow, that was being run when the analysis stopped.
To restart an analysis from the beginning -- In the Automated Analysis Control window Analyze page, click on Reset Sequence and then on a button (Analyze All, Calibrate, or Analyze Samples) that starts an analysis.
Analyzing Additional Samples Several options are available when additional samples are to be analyzed when an analysis is in progress: To add samples to the sample sequence while an automated analysis is in progress, click on Priority... on the Analyze page of the Automated Analysis Control window. The Add Sample Dialog appears. To enter information on a new sample to be inserted in the analytical sequence, in the Analysis menu, click on Automated Analysis Append Samples to Analysis List while an automated analysis is in progress. The Append to Analysis List Dialog appears. To analyze additional samples at the end of an analysis, in the Analysis menu, click on the Automated Analysis Append Samples to Analysis List command to append samples from the sample information file to the end of the run list while an automated analysis is in progress. In the Append to Analysis List Dialog that appears, enter the sample numbers from the sample information file (do not enter autosampler locations). After an automated analysis is completed, to analyze additional samples, use the following procedure. 1. Check that the calibration curve still appears in the Calibration Display window. If not, select Recall Calibration... from the Analysis menu, then select the results data set that contains the calibration. 2. Using a Sample Information file, list the additional samples and autosampler locations. 3. In the Automated Analysis Control Set Up page, select the autosampler locations for the additional samples. 4. Click on the Analyze tab in the Automated Analysis Control window. 5. Click on Analyze Samples.
Generating Reports For saved data in a results data set (as requested in an analysis control window), use the WinLab32 Data Manager to generate reports in a wide variety of formats. To start the WinLab32 Data Manager In the File menu, click on Utilities Data Manager. or Click on the Start button in Windows. Select Programs P-E WinLab32 Data Manager.
Shutting Down the Instrument There are two ways to extinguish the plasma. Either extinguish the plasma manually or extinguish it automatically using Automatic Shutdown. Automatic Shutdown can be selected in the Automatic Shutdown/Startup dialog, which is accessed from the Automated Analysis Control Set Up page or using the Auto Shutdown/Startup command in the System menu. Another mode is Automatic Startup, which can also be selected in the Automatic Shutdown/Startup dialog. IWhen Automatic Startup is selected restart system, this affects the procedures for shut down.
For a scheduled an Automatic Shutdown or Startup, leave the WinLab32 software on. Do not exit the software.
To automatically extinguish the plasma and put the spectrometer on standby
If Automatic Shutdown is selected it indicated how the system will shut down, the system will automatically shut down and flush the sample introduction system according to the users choices. The system next extinguishes the plasma and puts the spectrometer into standby if that option was selected. The software remains on. To manually extinguish the plasma
1. Flush the sample introduction system for five minutes with the plasma on. During this five minutes, for analysis of aqueous solutions, either flush with deionized water only or flush with a dilute acid solution, followed by deionized water. After analyzing organic solutions, flush the system with an appropriate clean solvent. 2. Extinguish the plasma by clicking on the Plasma Off switch in the Plasma Control window. When the plasma is extinguished, the plasma off/on switch in the Plasma Control window changes from blue to white and the peristaltic pump stops pumping solution to the plasma.
Note: Pressing the red Emergency Plasma Off button on the instrument allows the plasma to be shut off directly and bypasses the software. This button can be used if the software hangs up or if communication between the instrument and the computer is interrupted. Using this button does not harm the instrument. If this button is used, reset the system before the plasma can be reignited. To reset the system, be sure that the red button is in the out position, and select the Reset Emergency Off command in the System menu.
3. Proceed with this step depending upon the conditions of Automatic Startup. If Automatic Startup is not being used -or- If Automatic Startup has been selected and does not include turning on the plasma and the pump Take the sample capillary out of the flush solution, and then run the pump for a few minutes to clear solvent from the sample capillary and pump the spray chamber. Release the clamp lever and remove the tubing. (This will increase the lifetime of the pump tubing.)
Caution: Always remove the sample capillary or the autosampler probe from the solution after finishing use of the pump. Otherwise, the solution can siphon into the spray chamber and flood it.
If Automatic Startup has been selected and includes turning on the plasma and the pump then Leave the sample capillary in the wash solution. If the level of the wash solution reservoir in the autosampler is above the spray chamber, leave the peristaltic pump tubing clamped. This prevents the wash solution from being siphoned into the spray chamber. -or- If the level of the wash solution reservoir in the autosampler is below the spray chamber, release the clamp lever on the pump tubing. This prevents the solution from being pumped when the system automatically starts up. 4. Manually put the spectrometer on standby as required, see below. To manually put the spectrometer on standby 1. In the System menu, click on Auto Shutdown/Startup. 2. In the dialog, select Enable shutdown... and Immediately on OK. Be sure Put Spectrometer into Standby is selected.
3. If the plasma has already been extinguished, be sure that the Wash before shutdown option is not selected and that Turn off Plasma and Pump is not selected. 4. Be sure Automatic Startup is enabled and set the date and time.
