Organic Solvent Analysis Workflow

The following describes the differences in organic solvent analyses on the instrument

based on the general elemental analysis workflow on MassHunter Workstation.

Operation Procedure Overview

Usually, start the operation of the instrument in Standby mode. The procedure for putting the instrument in Standby mode when the power is off is the same as the general procedure. In addition to the standard preparation, make sure that 20% oxygen/argon is supplied to the optional gas for the instrument.

Startup for Organic Solvent Analysis

In a startup for analysis of organic solvents, as in the case of aqueous solutions, the torch axis and mass axis are adjusted after plasma ignition to optimize the basic performance of the instrument. Isopropyl alcohol is used when the plasma is ignited.

Note that EM adjustment is not performed for organic solvent analyses, but it is for aqueous solutions. For more information on startup settings, refer to the startup for general aqueous solutions in Executing Startup.

Conditions for Performing a Startup

In organic solvent analyses, the operation procedure varies depending on whether a Startup is performed or not. Refer to Executing Startup for more information. To perform Startup, the instrument must meet the following conditions:

• x-lens
• Torch: internal diameter 1.5 mm, G3280-80004
• Nebulizer: MicroMist Nebulizer　G3266-65003

  Use the nebulizer with self-aspiration.

• Sample tube: internal diameter 0.25 mm, length 700 mm, with a connector, G3266-80010
• Platinum sampling cone G3280-67036
• Platinum skimmer cone G3280-67060
• Brass skimmer base G3280-60621

 

Part numbers are subject to change.

 

A startup cannot be performed for other conditions (e.g., s-lens is used). In such a case, refer to "When No Startup Is Performed" below and also "Operation Procedure When No Startup Is Performed."

When a Startup Is Performed

In this case, perform a startup after introducing isopropyl alcohol and igniting the plasma. Next, load a batch suitable for the solvent to be analyzed and perform lens tuning. After that, introduce the sample and start the analysis. You can adjust plasma conditions manually.

For details on the operation, refer to "Operation Procedure When a Startup Is Performed"

When No Startup Is Performed

In this case, perform tuning manually after introducing isopropyl alcohol and igniting the plasma. Perform lens tuning and start the sample analysis. You can adjust plasma conditions manually.

For details on the operation, refer to "Operation Procedure When No Startup Is Performed."

Solutions to Be Prepared

When you perform a Startup, prepare the following solutions in advance:

• Rinse solution

  Before starting the analysis, use isopropyl alcohol. During the analysis, use the target solvent.

• Tuning solution

  Prepare a tuning solution by diluting a standard solution of an aqueous solvent with isopropyl alcohol.

Solvent: Isopropyl alcohol. Li, Co, Y, Ce, and Tl at 10 mg/L

Operation Procedure When a Startup Is Performed

Start MassHunter Workstation

• Start the MassHunter Workstation software.

Configure Hardware

• Set an O ring for the connector of the sample tube used for the nebulizer for organic solvents (if the connector is used), a sample introduction tube, and a torch. Set a drain tube for organic solvents that is suitable for the target solvent. (For other conditions on the instrument, refer to "Conditions for Performing a Startup.")
• The peripump is used only for drainage and is not used for introducing liquids to the nebulizer.
• Configure the hardware settings on the MassHunter Workstation. On [System] - [Hardware] in the [Settings] dialog box, specify [Organic Solvent] for Ignition Mode, [MicroMist] for Nebulizer, and [PeriPump] for Sample Introduction. Select [x-Lens] for Ion Lenses.

Configure User Tune

Follow the steps below to configure User Tune.

1. Click [User Tune Configuration] from the [Startup] group in the Task Navigator.

 

To display the [Startup] group, click [Configuration] from the [Startup] group on the [Home] tab.

 

The User Tune Pane appears.

2. Select [IPA] from the [Organic Solvent Parameters] pull-down menu.
3. Select [No Gas] for [Set Base Tune for Startup].
4. Click [Startup Configuration] from the [Startup] group in the Task Navigator.
5. Click [Configure Ignition Sequence] on the Startup Pane toolbar.

   The [Configure Ignition Sequence] dialog box is displayed.

6. Select [User Tune], and then click [OK].

Configure Startup

• After enabling Custom Settings (click [Select Custom Settings] on the Startup Pane taskbar), configure as follows. Do not configure Plasma Correction, EM or P/A factor.

 

• In the standard settings, the rinse port is specified to be used. For some autosamplers, no organic solvent can be used as a rinse solution for the rinse port. In such a case, change the setting of [Set] in [PeriPump] so that the rinse port is not used. Be sure to allow sufficient Sample Uptake and Stabilization time. For details, refer to the instruction manual for each autosampler.

Turn Plasma ON / Execute Startup

• Click the [Plasma] from the [Startup] group in the [Home] tab. When the message "Do you want to perform a startup after plasma ignition?" is displayed, select [Yes].
• After Startup is complete, introduce the tuning solution.

Replace Solvent

• If the solvent used for the analysis is not isopropyl alcohol, introduce the target solvent.
• Select the rinse solution suitable for the target solvent.

Edit Batch

• Specify the conditions for the acquisition method, data analysis method, and sample list, excluding the conditions for tuning.
• Subsequent steps are the same as in the general operation for aqueous solution analyses.

Execute Queue

• Add the created batch to the queue and start the acquisition.

Check Analysis Results

• The analysis results can be viewed on the panes in the ICP-MSICP-QQQ Data Analysis window.

Generate Reports

• Generate a sample report or quick batch report.

Save Analysis Results

• Save Analysis results.

Turn Plasma OFF

• Turn off the plasma.

Exit MassHunter Workstation

• Exit the MassHunter Workstation software.

Operation Procedure When No Startup Is Performed

Start MassHunter Workstation

• Start the MassHunter Workstation software.

Configure Hardware

• Select MicroMist Nebulizer or MicroFlow Nebulizer (PFA) as the nebulizer. Set a sample introduction tube suitable for the sample, a torch, a drain tube for organic solvents, and an O ring for the connector of the sample tube used for the nebulizer for organic solvents (if the connector is used). For more information on selecting a sample introduction tube and torch, refer to Appendix A in the Hardware Maintenance Manual.
• The peripump is used only for drainage and is not used for introducing liquids to the nebulizer.
• Configure the hardware settings on the MassHunter Workstation. On the Dashboard Pane, select [Organic Solvent] for Ignition Mode and your nebulizer for Nebulizer. Set [PeriPump] for Sample Introduction. Select the lens to use for Lens.

Configure User Tune

Follow the steps below to configure User Tune.

1. Click [User Tune Configuration] from the [Startup] group in the Task Navigator.

 

To display the [Startup] group, click [Configuration] from the [Startup] group on the [Home] tab.

 

The User Tune Pane appears.

2. Select [IPA] from the [Organic Solvent Parameters] pull-down menu.
3. Select [No Gas] for [Set Base Tune for Startup].
4. Click [Startup Configuration] from the [Startup] group in the Task Navigator.
5. Click [Configure Ignition Sequence] on the Startup Pane toolbar.

   The [Configure Ignition Sequence] dialog box is displayed.

6. Select [User Tune], and then click [OK].

Configure Startup

• In this case, you do not need to configure a startup.

Turn Plasma ON

• Click the [Plasma] from the [Startup] group in the [Home] tab. When the message "Do you want to perform a startup after plasma ignition?" is displayed, select [No].
• In Analysis Mode after ignition, you can adjust Torch Axis and Resolution/Axis in the user tune. You can also use the Dashboard Pane to adjust Torch Axis and Resolution/Axis.
• When you adjust them manually, introduce the tuning solution.

Replace Solvent

• If the solvent used for the analysis is not isopropyl alcohol, introduce the target solvent.
• Select the rinse solution suitable for the target solvent.

Edit Batch

• Specify the conditions for the acquisition method, data analysis method, and sample list, excluding the conditions for tuning.
• Subsequent steps are the same as in the case of When a Startup Is Performed and the general operation for aqueous solution analyses.

Execute Queue

• Add the created batch to the queue and start the acquisition.

Check Analysis Results

• The analysis results can be viewed on the panes in the ICP-MSICP-QQQ Data Analysis window.

Generate Reports

• Generate a sample report or quick batch report.

Save Analysis Results

• Save Analysis results.

Turn Plasma OFF

• Turn off the plasma.

Exit MassHunter Workstation

• Exit the MassHunter Workstation software.

Differences between Organic Solvents and Aqueous Solutions

When an organic solvent is used, the gas flow rate and control timing used when the plasma is ignited are different from those of an aqueous solution. This is because the volatility, the viscosity, and the amount of the solvent introduced to the plasma vary depending on each organic solvent.

After the plasma is ignited, set the tuning parameters used in Analysis Mode so that they are suitable for organic solvents. The biggest differences from the case of aqueous solutions are in the nebulizer gas (also called carrier gas) flow rate, optional gas flow rate, makeup gas flow rate, peripump, and spray chamber temperature.

These differences in parameters are due to the following factors:

• To prevent carbons from being deposited as soot on the interface when the (organic solvent) sample is decomposed by plasma, oxygen is introduced through the optional gas.
• If a large amount of the (organic solvent) sample is introduced, the plasma may not be maintained. Also, a large amount of oxygen is also required.
• Some (organic solvent) samples deteriorate a peripump tube. So, such a sample is introduced by self-aspiration instead of using a peripump.
• Because no peripump is used, the introduction amount of the sample is controlled by changing the nebulizer gas flow rate and the inner diameter of the sample introduction tube.
• The peripump is used only for draining liquids.
• To reduce the vapor pressure of the (organic solvent) sample, the temperature of the spray chamber is set to -5ºC.
• In MassHunter Workstation, the above parameters are set in the batches for organic solvents. The available batch types are IPA, Kerosene, and Xylene, and the difficulty of maintaining the plasma increases in this order. If you cannot find a batch with a relevant solvent name, select the one whose difficulty of maintaining the plasma is closest to that of your solvent.

 

When you select Xylene but the plasma cannot be maintained or soot is deposited, replace the introduction tube with a thinner one and reduce the introduction amount of the sample.