Agilent 7700 Series ICP-MS

MassHunter Workstation
Quick Start Guide
This guide describes how to use the Agilent 7700 Series ICP- MS
MassHunter Workstation.

Agilent Technologies
 Startup 3
Preparing for Analysis 4
Things to check before analysis 4
Prepare tuning solutions 4
Ignite the plasma 5
Check tuning 6
Setting Quantitative Method Parameters 12
Set up a Quantitative Method 12
Access Method parameters directly 19
Use the Method Wizard to create a method 19
Running the Samples 21
Set up the Sequence 21
Analyze the samples 23
Quantitative Data Analysis 25
Typical scenarios for Data Analysis 25
Open an existing batch for data analysis 26
Creating a new batch for data acquisition 26
Create the Data Analysis (DA) method for Quantitative data analysis 28
Process the batch 32
View analysis results 33
Save analysis results 34
Generate a report 34
Semi-Quantitative Analysis 35
Prepare for SemiQuant Analysis 35
Create a SemiQuant acquisition method 35
Analyze the samples 37
Create a new batch or open a new batch for SQ data analysis 37
Create the Data Analysis (DA) method for Quantitative data analysis 28
Process the batch 40
Correcting the Semiquant Factors 41
Change the SemiQuant Factors 42

2 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide

Startup
To start the Agilent 7700 Series ICP- MS MassHunter Workstation software:
• Double- click the ICP MS Top desktop icon , or
• Select Programs > ICP- MS MassHunter Workstation > ICP- MS Top from
the Windows Start menu.
The ICP- MS Top window opens:

Toolbar The following shortcuts are available on the ICP- MS MassHunter Workstation
toolbar:

Button Action Button Action

Display Instrument Status Panel Display Data Acquisition Panel

Display Tuning Panel Display Data Analysis Panel

Run Current Method Run Current Sequence

Run Method Wizard Edit Sequence

Edit Method Load Sequence

Load Method Save Sequence

Save Method Display online help window

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 3

Preparing for Analysis
The following topics will help you prepare the instrument for analysis with
Agilent 7700 Series ICP- MS MassHunter Workstation.

Things to check before analysis

Utilities
• Argon gas pressure: 500 to 700 kPa
• Cell gas (Helium): 90 to 130 kPa
• Cell gas (Hydrogen): 20 to 60 kPa
• Exhaust duct (on)
• Cooling water (Chiller or heat exchanger on)
• Drain and rinse tank (not full)

Peristaltic pump tubing

• Sample, drain, and internal standard lines

Prepare tuning solutions

You will need the following standards and solutions for ICP- MS operation:
• Tuning solution (1ppb Li, Co, Y, Ce, Tl)
• Internal standard solution
• Dilute the P/A factor tune solutions 75x, then mix the two solutions 1:1 to
prepare a P/A factor tune solution for use in the lab. PA factor tuning is
used to achieve linear functionality across the detector’s pulse and analog
modes. Pulse mode is used to quantitate relatively low concentrations (ppb
range). Analog mode is used to quantitate relatively high concentrations
(ppm range).

4 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide

 Ignite the plasma
1 Open the Instrument Control panel in either of the following ways:
• Select Instrument Control from the Instrument menu, or
• Click the Instrument Control icon.
The ICP- MS Instrument Control panel opens:

2 Confirm that the instrument is in Standby mode by checking the title bar of
the Instrument Control panel.
3 Ignite the plasma by clicking the Ignite Plasma icon in the toolbar.
4 Once the plasma is on and the instrument goes from standby to analysis
mode, check tuning as described in the following section.

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 5

 Check tuning
The following diagram labels the parts of the ICP- MS instrument. You can
refer to this diagram during the discussion of tuning parameters in this
section.

Interface Octopole Reaction System (ORS)

Skimmer Cone Quadrupole Mass Analyzer

Octopole
Ion Source Ion Reaction Cell
Lens Hyperbolic Quadrupole Rod Assembly
RF Generator Reaction Gas
Sample Introduction Electron Multiplier

Detector

AMFC Turbo-
Molecular
Pump

Ar Gas Vacuum System

Sample
Sampling Cone Foreline
Pump

Open the Tuning panel by selecting Tune from the Instrument menu,
or by clicking the Tune icon on the ICP- Top toolbar.

6 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide

 Toolbar The following items (shortcuts) are available on the Tuning panel toolbar:

Button Action Button Action

Load tuning parameters from file Save tuning parameters to file

Generating tuning report Print current graph

Tune sensitivity Tune Oxide Ion

Tune Doubly Charged Ion Resolution and Axis

Select Mode & start Autotune Set Acquisition parameters for tuning

View meter control panel Display online help window

Tip See the “Tuning 7700” in online help for more information on individual
tuning parameters.

Plasma Correction
Execution of plasma correction is necessary in the following cases:
• When the instrument is installed
• When the nebulizer has been changed
(However, if the same nebulizer unit is reused repeatedly by detaching and
reattaching, it is not necessary to conduct the correction each time as long
as the nebulizer is installed correctly.)
• When the sampling cone is changed
• When the torch is changed
• When the matrix tolerance has changed after the instrument has been used
for 6- 12 months and normal maintenance procedures have been followed
Once plasma correction is performed, there is no need to conduct it again in
most cases, provided the instrument is used for normal measurement.

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 7

 Operating Method
When performing plasma adjustment, use a 1pbb tuning solution containing
Ce. The following explains the method, refer to the online help.

Settings for Preset Mode

Select the nebulizer and tuning type, and set to the Preset mode. Under the
Preset mode, parameters such as RF power, sampling position, carrier gas flow
rate, makeup gas flow rate, and nebulizer pump speed are fixed to the preset
values.
1 In the Tuning window, select Preset Plasma >> Select Plasma.
The Plasma Select dialog appears.
2 Check the Preset Mode box.
3 Select the type of nebulizer to be used from the drop- down menu (For
7700x).
4 Select Robust or one of the 3 levels of Ultra Robust (For 7700x). Select Hot
Plasma (For 7700s).
If the matrix concentration exceeds 1%, select Ultra Robust- Level: High (if
the desired sensitivity is not achieved, select Level Medium or Low).
5 Click OK.
The Tuning window becomes active.

Checking the Tuning

Check the tuning as follows:
1 Check the each parameters:
• Open the last- used tuning file (typically nogas.u, h2.u or he.u).
• Select Acquisition Parameters from the Acq. Params menu. Set the mass
numbers to be measured as 7 (Li), 89 (Y), 205 (Tl), and 156/140 (Ce oxide
formation rate) and click OK.
• Check the following values displayed on the Tuning window:

8 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide

 Table 1 Typical Sensitivity Values (For 7700x)

Mass Sensitivity (cps/ppb)

No Gas Mode He Gas Mode H2 Gas Mode
(3.6ml/min) (4.0ml/min)
7Li 30,000 --- ---
59
Co --- 24,000 ---
89Y 100,000 --- 60,000
205Tl 60,000 --- ---
Oxide ratio ≤ 1.5% (≤2% for MicroFlow Nebulizer)

2 If the desired sensitivity is not achieved, select Autotune from Tume menu.
Refer to the Help and execute Autotune.
3 After completing autotune, check the sensitivity parameters on the ICP- MS
Tuning - Sensitivity window.
4 Save the tune file by selecting Save from the File menu. In general you will
want to overwrite the tune file that was open, so that it has the updated
values.
5 (optional) Generate a tune report by selecting Generate Report from the
File menu. Enter optional comments if desired and click OK. A report
showing the following information is sent to your printer:
• Sensitivity data
• Resolution/Axis data
• Lens parameter settings
Depending on how your system is configured, tuning results will also be
recorded in the maintenance log.
Tip You can also get a hard copy of current tune parameters by clicking the
Stop button and selecting Print from the File menu.

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 9

 Reference: For 7700x
The recommended tuning parameter values for 7700x are shown below.

Table 2 Recommended Values for 7700x (When Using a MicroMist Nebulizer)

Parameter No Gas Mode Cell Gas Mode High Energy Collision Mode *2
Recommended Recommended Recommended Recommended Recommended Recommended
Value Range Value Range Value Range
RF Power [W] 1550 Fixed 1550 Fixed 1550 Fixed
Smpl Depth [mm] 8.0 Fixed 8.0 Fixed 8.0 Fixed
Carrier Gas [L/min] 1.05 1.01 to 1.11 1.05 1.01 to 1.11 1.05 1.01 to 1.11
Makeup Gas [L/min] 0 0 to 1.11 0 0 to 1.11 0 0 to 1.11
Dilution Gas [L/min] 0 Fixed 0 Fixed 0 Fixed
Neb Pump [rps] 0.1 Fixed 0.1 Fixed 0.1 Fixed
S/C Temp [degC] 2 Fixed 2 Fixed 2 Fixed
He or H2 gas [ml/min] 0 Fixed 3.6 (He) 3.2 to 4.0 (He) 10 (He) 7 to 10 (He)
4.0 (H2) 3.6 to 4.4 (H2)
Extract 1 [V] 0 Fixed 0 Fixed 0 Fixed
Extract 2 [V] -180 -200 to -160 -180 -200 to -160 -180 -200 to -160
Omega Bias [V] -80 -110 to -70 -80 -110 to -70 -80 -110 to -70
Omega Lens [V] 10 7 to 12 10 7 to 12 10 7 to 12
Cell Entrance [V] -30 -40 to -30 -40 -40 to -30 -130 -150 to -110
Cell Exit [V] -50 -60 to -40 -60 -60 to -40 -150 Fixed
Deflect [V] 10 8 to 15 0 -5 to 4 -80 -90 to-70
Plate Bias [V] -40 -50 to -30 -60 Fixed -150 Fixed
OctP RF [V] 180 150 to 200 180 150 to 200 190 180 to 200
*1
OctP Bias [V] -8 -10 to -6 -18 Fixed -100 Fixed
*1
QP Bias [V] -3 -7 to -3 -15 Fixed -96 -97 to -90

*1 Generally, set the QP Bias at least 2 to 3V higher than OctP Bias.

*2 High-Energy Collision mode allows for enhanced reduction of interference under the Helium mode.
However, as it will also result in reduced low-mass sensitivity, it should be used in accordance with
the purpose of the analysis.

10 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide

 Reference: For 7700s
The recommended tuning parameter values for 7700s are shown below.

Table 3 Recommended Values for 7700s (When Using a MicroFlow Nebulizer)

Parameter High Sensitivity Cell Gas Mode High Energy Collision Cool Plasma
Mode*2
Recom- Recom- Recom- Recom- Recom- Recom- Recom- Recom-
mended mended mended mended mended mended mended mended
Value Range Value Range Value Range Value Range
RF Power [W] 1500 fixed 1500 fixed 1500 fixed 600 fixed
Smpl Depth [mm] 8 7 to 10 8 7 to 10 8 7 to 10 18 fixed
Carrier Gas [L/min] 0.7 fixed 0.7 fixed 0.7 fixed 0.7 fixed
Makeup Gas [L/min] 0.5 0.3 to 0.7 0.5 0.3 to 0.7 0.5 0.3 to 0.7 0.75 0.6 to 1.2
Dilution Gas [L/min] 0 fixed 0 fixed 0 fixed 0 fixed
Neb Pump [rps] 0.1 fixed 0.1 fixed 0.1 fixed 0.1 fixed
S/C Temp [degC] 2 fixed 2 fixed 2 fixed 2 fixed
He or H2 gas [ml/min] 0 fixed 3.6(He) 3.2 to 4.0(He) 10(He) 7 to 10(He) 0 fixed
4.0(H2) 3.6 to 4.4(H2)
Extract 1 [V] 4.5 3 to 7 4.5 3 to 7 4.5 3 to 7 -120 -200 to -40
Extract 2 [V] -100 -170 to -60 -100 -170 to -60 -100 -170 to -60 -5 -30 to 5
Omega Bias [V] -70 -100 to -30 -70 -100 to -30 -70 -100 to -30 -70 -120 to -30
Omega Lens [V] 11 5 to 15 11 5 to 15 11 5 to 15 6 3 to 10
Cell Entrance [V] -30 -40 to -30 -40 -40 to -30 -130 -150 to -110 -30 -40 to -30
Cell Exit [V] -50 -60 to -40 -60 -60 to -40 -150 fixed -60 fixed
Deflect [V] 12 8 to 15 0 -5 to 4 -80 -90 to -70 9 5 to 13
Plate Bias [V] -40 -50 to -30 -60 fixed -150 fixed -60 fixed
OctP RF [V] 180 150 to 200 180 150 to 200 -190 180 to 200 150 100 to 200
OctP Bias [V] *1 -8 -12 to -6 -18 fixed -100 fixed -18 -30 to -10
QP Bias [V] *1 -3 -5 to -3 -15 fixed -96 -97 to -90 -5 -5 to -3

*1 Generally, set the QP Bias at least 2 to 3V higher than OctP Bias.

*2 High-Energy Collision mode allows for enhanced reduction of interference under the Helium mode.
However, as it will also result in reduced low-mass sensitivity, it should be used in accordance with
the purpose of the analysis.

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 11

Setting Quantitative Method Parameters
The following topics will help you create an acquisition method for
quantitative analysis with the Agilent 7700 Series ICP- MS MassHunter
Workstation.

Set up a Quantitative Method

Create a quantitative method for environmental analysis as described below:
1 Select Edit Entire Method from the Methods menu. This initiates a series
of dialog boxes, so you can set the parameters for your method. See the
online help for a full description of the items on these dialog boxes.
Tip See also “Use the Method Wizard to create a method” on page 19.
2 On the Edit Method dialog box, mark the following options, then click OK.

3 On the Method Information dialog box:

a Enter a comment
b Mark the Data Analysis check box to run the data analysis automatically
after data acquisition. For instructions on setting up a Data Analysis
method, see “Open an existing batch for data analysis” on page 26.
c Click OK.

12 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide

 4 On the Select Sample Types (or Select QC Items, if the Intelligent Sequence
software is installed) dialog box:
a Configure the list of Selected QC Items on the right to contain CalStd
and Sample only.
b Depending on the method you started with, you may have to use the
Add- > and <- Remove buttons to create the desired list.
c Click OK.
5 On the Interference Equations dialog box:
a Display interference correction equations in one of the following ways:
• Mark Show All Masses to display all interference correction equations.
• From the pull- down menu at the bottom right, select Interference
Equation Library, to display interference correction equations in the
selected library.
b To edit the interference equation for a mass:
• Click on the desired mass number in the list.
• Click the Edit button to open the Edit Equation dialog box.
• Edit the equation as described in online help and click OK to close the
Edit Equation dialog box.
c Repeat Step 5b for all masses you want to edit.
d (optional) Click the Save button on the Interference Equation dialog box
to save the edited equations for use with other methods.
e When finished, click OK.
6 On the Acquisition Mode dialog box:
a Check the Spectrum (Multi Tune) option.
b Click OK. Multi Tune allows you to use different tuning modes (e.g.
Hydrogen and Helium modes) for different elements in a single run.

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 13

 7 Specify the masses and element to analyze as follows:
a On the Spectrum (Multi Tune) Acquisition Parameters dialog box, click
the Periodic Table button as shown below:

7a

This opens the Masses dialog box shown below:

14 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide

 b Using Table 4 on page 18 as a guide, click to select the masses to
monitor for each element. Selected masses appear in red in the
dialog box.
Double- click on a element to open the Select Isotopes dialog box.
Click the buttons for the isotopes you want to monitor. You can
select one or more isotopes per element. Red check marks indicate
the selected isotopes. To clear an isotope, click the right mouse
button. Click OK when you are finished selecting isotopes for that
mass.
c Repeat Step 7b to set up each mass as shown in Table 4.
d When you are finished, click the Mass Table button. The Mass Table
dialog box opens to display the masses to be monitored for each element.
Check that the masses listed in the Mass Table dialog box match those
shown in Table 4 and adjust them if necessary. This is the list of
masses that will be monitored in the method.
e When finished setting up all the required elements and masses, click OK
on the Mass Table and Masses dialog boxes.
8 Set the Tune File and Stabilization time for each step in the upper right
area of the Spectrum (Multi Tune) Acquisition Parameters dialog box:

Step Tune File Stabilization Time

1 Hydrogen mode 30 sec

2 Helium mode 30-50 sec

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 15

 9 Set the Integration time per Point for each mass:
a Click on the row for the mass in the column for the appropriate step (i.e.
Step 1 for Hydrogen mode, Step 2 for Helium mode) as specified in the
Reaction Gas column in the Table 4 on page 18. You can select
multiple masses by <Ctrl>+clicking on them.
b Enter the Integration time per Point as specified in Table 4. The
integration times in the table are generally relatively short, and can
be extended as necessary.
c Click the Enter button. The per Point integration time and calculated
per Mass integration time will be updated in the table.

9b

9a

9c

d Repeat for each mass in the table. For masses such as 71 that are
monitored in both steps, remember to enter integration times for both.

16 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide

 10 Make the following additional selections on the Spectrum (Multi Tune)
Acquisition Parameters dialog box:
a Select Full Quant (3) for the Peak Pattern.
b Set the Repetition count to 3.

10b

10a
c Mark the Return to First Tune Step option at the bottom of the screen,
and click OK.

10c

11 On the Peristaltic Pump Program dialog box, set the following parameters,
then click OK. See online help for more information on these parameters
and on the optional features: Intelligent Rinse and Execute Pre- emptive
Rinse.
• Before Acquisition
• After Acquisition (Rinse Port)
• After Acquisition (Rinse Vial)
12 (optional) Set up pre- emptive rinsing as follows:
a Select Set PeriPump Program from the PeriPump menu in the
Acquisition window.
b On the Peristaltic Pump Program dialog box, mark the Execute
Pre- emptive Rinse option at the bottom of the screen.
c Enter an initial time of 15 seconds, then click OK.
d Adjust the time so that the analysis is completed 5 seconds before the
rinse solution reaches the nebulizer.
13 To save the method:
a On the Method Save Options dialog box, mark all items, and click OK.
b On the Save Method As dialog box, enter a method name, and click OK.

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 17

 Table 4 Set up information for elements and masses for Environmental Analysis
Element Mass Confirmation Mode Internal Approx. Integration
Mass1 Standard2 Time (sec/Point)
6
Be 9 No gas Li 0.3
6
B 11 No gas Li 0.1
Na 23 He 45Sc 0.05
45Sc
Mg 24 He 0.05
45
Al 27 He Sc 0.3
P 31 No Gas 6Li (72Ge, 45Sc)3 0.1
K 39 He 9 or 71 0.05
Ca 44 43 He 9 or 71 0.1
45Sc
V 51 He 0.5
45Sc
Cr 52 53 He 1
45Sc
Mn 55 He 0.1
Fe 56 57 He 45Sc 0.1
45Sc
Co 59 He 0.1
45Sc
Ni 60 He 1
Cu 63 65 He 45Sc 0.1
72Ge
Zn 66 64 He 0.1
72Ge
As 75 He 1
Se 78 He or (H2)4 72Ge 5
72Ge
Br 79 No Gas 0.1
103Rh
Mo 95 98 He 0.1
Ag 107 109 No Gas 115In 0.1
115In, (209Bi)
Cd 111 114 No Gas 1
103Rh (115In, 209Bi)
Sn 118 No Gas 0.1
115In, (209Bi)
Sb 121 No Gas 0.1
103Rh (115In, 209Bi)
I 127 No Gas 0.1
115In, (209Bi)
Ba 137 135 No Gas 0.1
209Bi
Hg 201 202 No Gas 1
175Lu, (209Bi)
Tl 205 No Gas 0.1
175Lu, (209Bi)
Pb 208 No Gas 0.1
175Lu, (209Bi)
Th 232 No Gas 0.1
175Lu, (209Bi)
U 238 No Gas 1
1) Can be subject to interferences.
2) ISTD solution P/N is 5188-6525. See page 23 for more information.
3) Alternate internal standards are shown in parentheses.
4) When H2 option is installed (then better MDL can be achieved).

18 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide

 Access Method parameters directly
You can access some method panels directly, using the following menu items:

Method parameters Window Menu Menu item

Method Information ICP-MS Top Methods Edit Method Information

Select Sample Items, ICP-MS Top Methods Select QC Items

Select QC Items
(Intelligent Sequence
Software is installed)

Interference Equation ICP-MS Top Methods Edit Interference Equation

Acquisition Mode Acquisition EditParameters Set Mode

Spectrum Acquisition Acquisition EditParameters Set Parameters

Parameters

Peristaltic Pump Acquisition PeriPump Set Peripump Program

Program

Method Save Options ICP-MS Top Methods Save As

Use the Method Wizard to create a method

This way of creating a method makes it easy to create methods for
environmental analyses, since it supplies many of the parameters that are
appropriate for various sample types and regulations.
1 Select Run Method Wizard from the Methods menu in ICP- MS Top.
General Items 2 Enter name for the method and click the Next> button.
Sample 3 Select the sample as follows:
a Select Environmental as the Application Type.
b Select a Sample, such as Drinking Water or High TDS. A description of
the current selection is displayed in the lower part of the window.
c Select a Regulation, such as EPA200.8 or EPA6020. Only the guidelines
that apply to the selected sample are displayed.
d Click the Next> button.

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 19

 Elements 4 The list of masses and elements that will be monitored is displayed. The
information in this list is based on the sample and regulation selected
above. Review the element information and make any changes as follows:
a Right- click on the element of interest in the Element List Information.
b Select one of the following options from the shortcut menu:
• Add - see Step 4c below
• Delete - removes the selected mass from the list
• Edit - see Step 4c below
c If you are adding or editing an element, enter the following information
on the Add (or Edit) Elements dialog box, then click OK.
• Mass
• Element Name
• Integration time (sec/Point)
• Tune step number
d (optional) Click the Edit/View Equation button to view or edit an
interference correction equation. See online help for more information.
e Click the Next> button.
Finish 5 Review the method information, then click the Finish button.
Tip You can edit the method later by selecting Edit Entire Method from the
Methods menu and marking the parts of the method to edit, or from the menus
items shown in the previous section.

20 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide

Running the Samples
The following topics will help you prepare a sequence, and run your samples
with the Agilent 7700 Series ICP- MS MassHunter Workstation.

Set up the Sequence

Set up a sequence for your analysis as follows:
1 Select Edit Sample Log Table from the Sequence menu in the ICP- MS Top
window. The samples you enter will be injected in the order they are listed
in the table.
2 Enter the following information for the first sample (Row 1) of the table:
a Method: Double- click in the Method column of Row 1 to open the Select
Method dialog box. Select the desired method and click OK.
b Type: Click in the Type column of Row 1 to open a list of types.
• Select CalBlk for calibration blanks.
• Select CalStd for calibration standards.
• Select Sample for unknown samples.
c Vial: Click in the Vial column of Row 1 and enter the vial number of the
first sample or standard.
• The large bottles for cleaning solutions are positioned at 1, 2, and 3.
• The small vials on the rack are positioned at 1001, 1002, 1003... etc.
d Data File: Leave this cell blank to assign a file name automatically at run
time.
e Sample: Enter a name for the sample in the Sample column.
f Comment: Enter a comment for the sample in the Comment column.
g Dil/Lvl: Specify a Dilution factor or Level.
• For standard solutions: click in the Dil/Lvl column of Row 1 and select
the desired level from the list.
• For samples: click in the Dil/Lvl column of Row 1 and type in the
dilution factor (1 for undiluted), or double- click to open the Calculate
Dilution Factor dialog box. See online help for more information.
h ISTD Conc: Double- click in the ISTD Conc column of Row 1 to open the
Set ISTD Conc dialog box. Select the desired calibration level or set a
ISTD Conc value, then click OK.

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 21

 3 Fill in values for the rest of your samples as follows:
a Select the first row and the subsequent rows by dragging the mouse.
b Right- click in the highlighted rows and select Fill Down from the
shortcut menu.
c The values for Method, Type, Dil/LVL and ISTD Conc are copied from
Row 1 to the selected blank rows. Sequential Vial numbers are assigned.
4 Modify the information for the sample rows added in Step 3 to match your
analyses.
5 (optional) To turn off the plasma automatically at the end of the sequence,
append the following row to the end of the sequence:
• Type: Keyword
• Data File: StandBy
• Leave all other cells blank
6 (optional) Select the Import DA Method from Existing Batch check box to
import an existing data analysis method from the specified data batch
directory. You can import the DA Method Only or the DA method and Std
Data. You can also apply a data analysis method after data acquisition.
7 Click OK to close the Edit Sample Log Table dialog box.
8 If errors are found in the table, a message appears.
a Click OK and the offending cell will be highlighted in the table.
b Fix the problem in the highlighted cell.
9 Repeat Steps 7 & 8 until no errors are detected.
10 (optional) Select Save from the Sequence menu in the ICP- MS Top window.
Enter a name for the sequence you just created, and click OK. You don’t
need to save a sequence to run it, but doing so allows you to open it later
and use it as a starting point for creating a new sequence more quickly.

22 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide

 Analyze the samples
1 Prepare the following standards, samples, and each solutions to use for
analysis. The solutions should contain 0.5% HCl as well as nitric acid.
• Make up the following calibration standards by diluting SPEX
XSTC- 760A with nitric acid to approx. 1%. The concentration of the
undiluted solution is 100x that of drinking water quality standard.

Calibration SPEX XSTC-760A Na Mg, K, Ca

curve ranges (ppm) (ppm)

Level 1 Blank HNO3 0 0

Level 2 1/1000 dilution (1/10 of standard) 10 5

Level 3 1/200 dilution (1/2 of standard) 50 25

Level 4 1/100 dilution (standard concentration) 100 50

For high-concentration Na, Mg, K, and Ca, it is safer to prepare their mixed standard
solutions separately instead of mixing with the SPEX mixed standard solution, so as to
prevent contamination with the reagent, particularly if the required concentration level is
1/100 of the standard.

• Dilute samples with nitric acid to approx. 1%

• Dilute Internal standard solution (P/N 5188- 6525) 200 times (for on- line
internal standard)
• Use of nitric acid (1 to 5%) is recommended for the cleaning solution, as
it will clean the introduction system better than pure water. If pure
water is used, residual memory may be washed out while introducing
acidic samples, affecting the quantitative measurement.
2 Select Run from the Sequence menu or click the icon on the toolbar to
open the Start Sequence dialog box.
3 Set the parameters to the desired values.

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 23

 4 The Data Batch Directory is set to a unique name based on the current
date and time. The format is year, month, day, hour, and sequential
numbers. For example, 08H14K01.B is the second batch directory created
between 10AM and 11AM on August 14, 2008. The parts of the name are
derived as follows:
08 = 2008
H= August
(month - A through L corresponds to the 12 months, in order, so A = January, etc.)
14= the day of the month
K= the hour of the day
(A - X correspond to 0 - 23)
01= a sequential number for sequences run within the same hour, i.e. 00, 01, 02, and so on
.B= the file extension for a batch file

If you wish, you can type in a different directory name instead. The name
can be up to eight characters long. The batch folder will be created in
C:\ICPMH\1\DATA\.
5 (optional) Select the Import DA Method from Existing Batch check box to
import an existing data analysis method from the specified data batch
directory. You can import the DA Method Only or the DA method and Std.
Data.
6 Click the Edit DA Method button in the lower left of the dialog box, then
create a Data Analysis method as described on page 28.
7 Click the Run Sequence button to start the run. The Run Sequence Status
dialog box appears.

8 If desired, you can monitor acquisition as described in online help.

9 When the sequence is complete, analyze the data as described in the
following section.

24 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide

Quantitative Data Analysis
The following topics will help you perform data analysis on your samples with
the Agilent 7700 Series ICP- MS MassHunter Workstation.

Typical scenarios for Data Analysis

Description

To import an existing The data was acquired with reference to a Data Analysis (DA) method.
method (E.g. the “Edit DA Method” button was clicked or the “Import DA Method from Existing Batch”
option was selected when setting up the sequence).
In this scenario, the ICP-MS Data Analysis window opens automatically after acquiring the data.
Proceed in one of the following ways:
• If no changes are required to the DA method, then proceed to “View analysis results” on
page 33 and to “Generate a report” on page 34.
• If you wish to modify the existing DA method for this acquired data, then proceed to “Create
the Data Analysis (DA) method for Quantitative data analysis” on page 28 to open the Method
Editor and make changes to the DA method.

To create a method The data was acquired without reference to a DA method.

after completing data In this scenario, the ICP-MS Data Analysis window opens automatically after acquiring the data,
acquisition but only the file name is displayed, since no analysis method has yet been applied. Proceed as
follows:
a Open the method editor as described in “Create the Data Analysis (DA) method for Quantitative
data analysis” on page 28.
b Proceed to create a DA method for Quantitative data analysis.

To create a method You want to create a DA method without reference to any acquired data.
before performing data a Follow the steps in“Open an existing batch for data analysis” on page 26 to create a new batch
acquisition folder, since a data batch does not already exist.
b If desired, import samples as described in Step 3.
c Proceed to “Create the Data Analysis (DA) method for Quantitative data analysis” on page 28.

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 25

 Open an existing batch for data analysis
If the window is not already open, open the ICP- MS Data Analysis window in
either of the following ways:
• Select Main Panel from the DataAnalysis menu in the ICP- MS Top window,
or
• Click the button on the ICP- MS Top toolbar.

Tip To open an existing batch:

a Select Open Analysis File from the File menu to open the Open Batch
dialog box.
b Select the file of interest and click Open. This opens an Analysis file with
data that has been previously acquired.
c Then proceed to “Create the Data Analysis (DA) method for
Quantitative data analysis” on page 28 to create a Data Analysis
(DA) method (if a DA method was not applied at time of data
acquisition) or to modify the method, if needed (if the DA method
was already applied).

Creating a new batch for data acquisition

1 Create a new Batch Folder, which will be used to contain your data analysis
results:
a Open the New Batch Folder dialog box in either of the following ways:
• Click the New Batch Folder toolbar button , or
• Select New Batch Folder from the File menu.
b Type in a name for the new folder (you may select a different location if
desired).
c Click the Create button.

26 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide

 2 Import the samples as follows:
a Select Import Samples from the File menu.
b Navigate to the data file folder where the data files of interest are located
and click the Open button. The data files in that folder are displayed on
the Import Samples dialog box.
c To import samples from another folder, click the Browse button.
d Repeat Steps b and c until all samples of interest are displayed on the
Import Samples dialog box.
e Select the samples to import:
• <Ctrl>+click to select multiple samples from the list.
• Click the Select All button to select all samples in the list.
f Click OK.

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 27

 Create the Data Analysis (DA) method for Quantitative data analysis
1 Open the Method Editor window in either of the following ways:
• Click the Edit Method toolbar button , or
• Select Edit from the Method menu.
Tip To import existing DA method, click Import Method only or Import
Method and Standard Data and select an analysis file to import.

2 Select Data Analysis Method from Method Tasks section 2 (on the left side
of the screen) to display the Data Analysis Method pane
3 Set the options as follows:
a Mark the check box for FullQuant Analysis.
b Set the Analysis Mode to Spectrum.
c Select the correction method from the Interference Correction list.

3a

3b

3c

4 Select a Sample Template from the list.

28 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide

 5 Select Analyte List from Method Tasks section 3 to display the Analyte List
pane.
.

To open the analyte list from the existing data:

• Click the button, or
• Right- click in the pane and select Load list from acquired data.
Tip You can also create an analyte list in either of the following ways:
• To load an analyte list from an acquisition method that has already been
developed, click the button.
• To add new analyte lines, click the button, then designate the Tune
Step, Mass, Name and Analyte/ISTD for each new line as described in
Step 6.
6 Enter the following information for each analyte:
a Click the button at the right end of the Tune Step column, and select
a tune step number.
b Click the button at the right end of the Analyte/ISTD column and
select either analyte or ISTD.

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 29

 7 Select Full Quant from Method Tasks section 4 to display the FullQuant
Method Table pane:

8 Set the following calibration curve parameters:

• The calibration curve method (External Calibration / Standard Addition)
• Type of VIS correction for ISTD elements
• Curve fit type (Linear / Quadratic / Excluded)
• Handling of the origin (Ignore / Force / Blank offset)
• Calibration curve weight
• ISTD elements used for correction
• Concentration of the calibration curve level (Min Conc). For most
applications, enter 0.
• Concentration unit
• Concentration of the blank

30 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide

 9 The following Advanced Info method tasks are described in online help:
• FullQuant Outlier
• Edit Report Templates
10 Select Validate from Method Tasks section 5. Correct any method errors
before proceeding.
11 Select Return to Batch- at- a- Glance from Method Tasks section 5.
Click Yes to save the Data Analysis method.

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 31

 Process the batch
1 Initiate batch processing in either of the following ways:
• Click the Process Batch toolbar button , or
• Select Process Batch from the Process menu.
Analysis is performed on the samples you added to the batch in the
previous topic, using parameters set in the DA method. See “Create the
Data Analysis (DA) method for Quantitative data analysis” on page 28..
2 Review the analysis results that are displayed in the Batch Table and
Calibration Curve panes, as shown in the following examples.

Note The Process Batch button changes to black after processing: .

32 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide

 View analysis results
Batch Table 1 View the concentration and count for each element in the samples in the
pane Batch Table pane.
• Concentration and count for problematic data (Outlier) are displayed
with a color of each Outlier background.
• See online help for information if you want to change the way the data is
displayed, such as sorting or customizing the columns
• Also see online help for information on changing the layout or doing auto
review.
Spectrum 2 View mass spectra in the Spectrum pane. You can zoom in to identify
pane elements by right- clicking and dragging the mouse cursor around the
desired mass number. See online help for information on other ways to
display or process data in the Spectrum pane, such as:
• Switching between log and linear
• Switching between one- row and three- row
• Adding comments
• Identifying unknown spectra against an element database
• Subtracting background spectra
• Overlaying multiple spectra
• Tabulating the spectral information
Calibration Curve 3 View calibration curves for each element in the samples in the Calibration
pane Curve pane.
• Problematic calibration curves (Outliers) are displayed with a pink
background.
• See online help for information on other changes you can make to the
calibration curve, such as excluding a calibration curve level, changing
the concentration of a calibration curve level, changing the calibration
curve type, changing the handling of the origin, or changing the
weighting of calibration curve.
ISTD Stability 4 View the percent recovery of each ISTD element in the ISTD Stability Graph
Graph pane pane. See online help for more information.

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 33

 Save analysis results
Be sure to always save the analysis results in one of the following ways:

As a new file: Select Save Analysis File As from the File menu.

To overwrite an existing results file with the same name:

• Click the Save toolbar button , or
• Select Save from the File menu.

Generate a report
1 Select Generate from the Report menu in the MassHunter ICP- MS Analysis
window.
2 Mark the desired report options and click OK (see example below).

3 Click OK to generate the report.

34 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide

Semi-Quantitative Analysis
Semi- quantitative analysis allows you to quickly scan and obtain information
about the concentrations of all elements that are present in an unknown
sample. It is useful when you want to obtain concentration information for a
large number of elements (>70) without external calibration, such as screening
prior to quantitative analysis on target elements. Typically, semi- quantitative
analysis is accurate to +/- 30% or better on completely unknown samples.

Prepare for SemiQuant Analysis

Prepare the following samples and solutions for analysis:
• Samples (dilute with nitric acid to approx. 1%)
• Tuning solution (Li, Co, Y, Ce, Tl, 1ppb each, with approx. 1% nitric acid)
• Cleaning solution (1 to 5% nitric acid)

Create a SemiQuant acquisition method

1 Select Edit Entire Method from the Methods menu. This initiates a series
of dialog boxes, so you can set the parameters for your acquisition method.
See the online help for a full description of the items on these dialog boxes.
2 On the Edit Method dialog box, mark the following options, then click OK.

3 On the Method Information dialog box, set the following parameters, then
click OK:
a Enter a comment
b Be sure that the Data Analysis check box is checked; this is required to
run the data analysis automatically after data acquisition.

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 35

 4 On the Select Sample Types (or Select QC Items, if the Intelligent Sequence
software is installed) dialog box, set the following parameters, then click
OK:
a Configure the list of Selected QC Items on the right to contain Sample,
SQStd, SQBlk, and SQISTD.
b Depending on the method you started with, you may have to use the
Add- > and <- Remove buttons to create the desired list.
5 Set the Data Acquisition method parameters:
a On the Acquisition Mode dialog box, mark the Spectrum option and click
OK.
b On the Spectrum Acquisition Parameters dialog box, click the Mass
Scale button.
c On the Masses dialog box:
• Click the Clear All button.
• Select all mass numbers by double- clicking on the top, middle, and
bottom rows, then click OK.
d Make the following additional selections on the Spectrum Acquisition
Parameters dialog box, then click OK:
• Select Semi Quant (6) for the Peak Pattern.
• Clear the Set every Mass option, then set the per Point Integration
time to 0.05 or 0.1 sec.
• Set the Repetition count to 1.
e On the Peristaltic Pump Program dialog box, set the following
parameters, then click OK.
• Before Acquisition: Uptake Speed: 0 rps, Uptake Time: 0 sec,
Stabilization Time: 70 sec
• After Acquisition (Rinse Port): Rinse time: 30 sec
• After Acquisition (Rinse Vial)
See online help for more information on these parameters and on the
optional features: Intelligent Rinse and Execute Pre- emptive Rinse.
6 To save the method:
a On the Method Save Options dialog box, mark all items, and click OK.
b On the Save Method As dialog box, enter a name for the method, and
click OK.

36 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide

 Analyze the samples
1 In the sequence table, set up a sequence with samples in the following
order:
a Tuning solution (1 ppb Li, Co, Y, Ce, Tl) - Sample Type is “SQStd”
b Blank (i.e. nitric acid) - Sample Type is “SQBlk”
c Sample 1 - > Sample 2 - > Sample 3 ... - Sample Type is “Sample”
2 Run the sequence:
a Select Run from the Sequence menu or click the icon on the toolbar
to open the Start Sequence dialog box.
b Click the Run Sequence button to start the run. The Run Sequence
Status dialog box appears.
c If desired, you can monitor acquisition as described in online help.

The same scenarios apply for offline Semi-quantitative data analysis as described in
NOTE “Typical scenarios for Data Analysis” on page 25.

Create a new batch or open a new batch for SQ data analysis

Refer to “Open an existing batch for data analysis” on page 26 and
“Creating a new batch for data acquisition” on page 26.

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 37

 Create the Data Analysis (DA) method for SemiQuant data analysis
1 Open the Method Editor window in either of the following ways:
• Click the Edit Method toolbar button , or
• Select Edit from the Method menu.
Tip To import existing DA method, click Import Method only or Import
Method and Standard Data and select an analysis file to import.

2 Select Data Analysis Method from Method Tasks section 2 (on the left side
of the screen) to display the Data Analysis Method pane.
3 Set the options as shown below:
a Mark the check box for SemiQuant Analysis.
b Set the Analysis Mode to Spectrum.
c Select the correction method from the Interference Correction list.

3a

3b

3c

4 Select a Sample Template from the list.

5 Select SemiQuant from Method Tasks section 3 to display the SemiQuant

pane.

38 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide

 Tip You can select elements to show in the pane by clicking Add/Remove
Standard Element.

6a

6 On the SemiQuant Method Table pane:

a Mark the check box for Advanced Parameters.
b Set the concentration of the elements in the standard sample being used
for the SemiQuant factor correction.
c Select the ISTD correction method.
For setting details, refer to “SemiQuant Pane” in the “Commands
Reference” section of online help.
7 Select Validate from Method Tasks section 5. Correct any method errors
before proceeding.
8 Select Return to Batch- at- a- Glance from Method Tasks section 5.
Click Yes to save the Data Analysis method.

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 39

 Process the batch
1 Initiate batch processing in either of the following ways:
• Click the Process Batch toolbar button , or
• Select Process Batch from the Process menu.
Analysis is performed on the samples you added to the batch in the
previous topic, using parameters set in the Data Analysis method, as
described in “Create the Data Analysis (DA) method for SemiQuant data
analysis” on page 38.
2 View/check the analysis results as follows:
a Batch Table pane- - Displays the concentration and count for each
element in the samples.
b Spectrum pane- - Displays mass spectra. You can zoom in to identify
elements by right- clicking and dragging the mouse cursor around the
desired mass number.
c Semiquant Factor pane- - Displays the SemiQuant factor graph for each
sample. Place the cursor near a point on a graph to display element
names and SemiQuant factor correction details. Use the arrow keys to
move between samples. If necessary, the factors can be changed as
described in “Change the SemiQuant Factors” on page 42.
If the SemiQuant Factor pane is not currently displayed, select
Calibration Curve from the View menu.
d ISTD Stability Graph pane- - Displays the percent recovery of each ISTD
element in the samples. See online help for more information.
3 Save results using Save Analysis File As or Save from the File menu.
4 Select Generate from the Report menu, select report options, and click OK.

40 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide

 Correcting the Semiquant Factors
On MassHunter Workstation, the SemiQuant factors are predefined for each
element. The greater the SemiQuant factor, the more efficiently that element is
ionized in the plasma, yielding a higher sensitivity. Use the following
procedure to correct the SemiQuant factors, as necessary.
1 Select and measure standard sample containing three or four elements
whose concentration are known. Make sure that the concentrations of the
elements in the standard sample cover the low, medium, and high ranges of
the mass spectrum, or use the tuning solution that contains Li, Co, Y, Ce
and TI as the standard sample.
2 In the ICM- MS Data Analysis window, load the data for the standard
sample into the batch folder.
3 Set the sample type of the loaded Standard Sample to SQStd as shown in
the example below:

4 Process the batch in either of the following ways:

• Click the Process Batch toolbar button , or
• Select Process Batch from the Process menu.
The SemiQuant factor for all elements will be corrected based on the
elements of known concentration in the standard sample (SQStd).

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 41

 Change the SemiQuant Factors
You can configure the SemiQuant factor, Base mass, and Reported mass
(isotopes).
1 Select SemiQuant Basic Parameters from the Global drop- down menu in
the ICP- Analysis window:

The SemiQuant Basic Parameters dialog box opens.

2 Make the change by either:

• Right- clicking within the table and selecting from the context menu; or
• Selecting a cell and directly editing its content.
Refer to the Help for more details.

42 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide

Notices
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www.agilent.com

In this Book
This Quick Start Guide
presents first steps to
using the Agilent 7700
Series ICP- MS MassHunter
Workstation.

© Agilent Technologies, Inc. 2009

Printed in USA
Rev. A, June 2009

*G7200-90210*
G7200-90210

Agilent Technologies