Agilent Technologies Agilent 7700 Series ICP-MS User manual

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

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

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

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

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 5
Ignite the plasma
1Open 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:
2Confirm that the instrument is in Standby mode by checking the title bar of
the Instrument Control panel.
3Ignite the plasma by clicking the Ignite Plasma icon in the toolbar.
4Once the plasma is on and the instrument goes from standby to analysis
mode, check tuning as described in the following section.

6 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide
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.
Open the Tuning panel by selecting Tune from the Instrument menu,
or by clicking the Tune icon on the ICP- Top toolbar.
Ion Source
Sample Introduction
Octopole
Reaction Cell
Electron Multiplier
Interface Octopole Reaction System (ORS)
Quadrupole Mass Analyzer
Detector
Vacuum System
Skimmer Cone
Ion
Lens Reaction Gas
RF Generator Hyperbolic Quadrupole Rod Assembly
Turbo-
Molecular
Pump
Foreline
Pump
Sampling Cone
Sample
Ar Gas
AMFC

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 7
Toolbar The following items (shortcuts) are available on the Tuning panel toolbar:
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.
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

8 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide
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.
1In the Tuning window, select Preset Plasma >> Select Plasma.
The Plasma Select dialog appears.
2Check the Preset Mode box.
3Select the type of nebulizer to be used from the drop- down menu (For
7700x).
4Select 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).
5Click OK.
The Tuning window becomes active.
Checking the Tuning
Check the tuning as follows:
1Check 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:

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 9
2If the desired sensitivity is not achieved, select Autotune from Tume menu.
Refer to the Help and execute Autotune.
3After completing autotune, check the sensitivity parameters on the ICP- MS
Tuning - Sensitivity window.
4Save 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.
Table 1 Typical Sensitivity Values (For 7700x)
Mass Sensitivity (cps/ppb)
No Gas Mode He Gas Mode
(3.6ml/min)
H2Gas Mode
(4.0ml/min)
7Li 30,000 --- ---
59Co --- 24,000 ---
89Y 100,000 --- 60,000
205Tl 60,000 --- ---
Oxide ratio ≤1.5% (≤2% for MicroFlow Nebulizer)

10 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide
Reference: For 7700x
The recommended tuning parameter values for 7700x are shown below.
*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.
Table 2 Recommended Values for 7700x (When Using a MicroMist Nebulizer)
Parameter No Gas Mode Cell Gas Mode High Energy Collision Mode *2
Recommended
Value
Recommended
Range
Recommended
Value
Recommended
Range
Recommended
Value
Recommended
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 H2gas [ml/min] 0 Fixed 3.6 (He)
4.0 (H2)
3.2 to 4.0 (He)
3.6 to 4.4 (H2)
10 (He) 7 to 10 (He)
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
OctP Bias [V] *1 -8 -10 to -6 -18 Fixed -100 Fixed
QP Bias [V] *1 -3 -7 to -3 -15 Fixed -96 -97 to -90

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 11
Reference: For 7700s
The recommended tuning parameter values for 7700s are shown below.
*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.
Table 3 Recommended Values for 7700s (When Using a MicroFlow Nebulizer)
Parameter High Sensitivity Cell Gas Mode High Energy Collision
Mode*2
Cool Plasma
Recom-
mended
Value
Recom-
mended
Range
Recom-
mended
Value
Recom-
mended
Range
Recom-
mended
Value
Recom-
mended
Range
Recom-
mended
Value
Recom-
mended
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 H2gas [ml/min] 0 fixed 3.6(He)
4.0(H2)
3.2 to 4.0(He)
3.6 to 4.4(H2)
10(He) 7 to 10(He) 0 fixed
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

12 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide
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:
1Select 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.
2On the Edit Method dialog box, mark the following options, then click OK.
3On the Method Information dialog box:
aEnter a comment
bMark 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.
cClick OK.

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 13
4On the Select Sample Types (or Select QC Items, if the Intelligent Sequence
software is installed) dialog box:
aConfigure the list of Selected QC Items on the right to contain CalStd
and Sample only.
bDepending on the method you started with, you may have to use the
Add- > and <- Remove buttons to create the desired list.
cClick OK.
5On the Interference Equations dialog box:
aDisplay 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.
bTo 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.
cRepeat 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.
eWhen finished, click OK.
6On the Acquisition Mode dialog box:
aCheck the Spectrum (Multi Tune) option.
bClick OK. Multi Tune allows you to use different tuning modes (e.g.
Hydrogen and Helium modes) for different elements in a single run.

14 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide
7Specify the masses and element to analyze as follows:
aOn the Spectrum (Multi Tune) Acquisition Parameters dialog box, click
the Periodic Table button as shown below:
This opens the Masses dialog box shown below:
7a

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 15
bUsing 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.
cRepeat Step 7b to set up each mass as shown in Table 4.
dWhen 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.
eWhen finished setting up all the required elements and masses, click OK
on the Mass Table and Masses dialog boxes.
8Set 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

16 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide
9Set the Integration time per Point for each mass:
aClick 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.
bEnter 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.
cClick the Enter button. The per Point integration time and calculated
per Mass integration time will be updated in the table.
dRepeat for each mass in the table. For masses such as 71 that are
monitored in both steps, remember to enter integration times for both.
9a
9b
9c

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 17
10 Make the following additional selections on the Spectrum (Multi Tune)
Acquisition Parameters dialog box:
aSelect Full Quant (3) for the Peak Pattern.
bSet the Repetition count to 3.
cMark the Return to First Tune Step option at the bottom of the screen,
and click OK.
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:
aSelect Set PeriPump Program from the PeriPump menu in the
Acquisition window.
bOn the Peristaltic Pump Program dialog box, mark the Execute
Pre- emptive Rinse option at the bottom of the screen.
cEnter an initial time of 15 seconds, then click OK.
dAdjust the time so that the analysis is completed 5 seconds before the
rinse solution reaches the nebulizer.
13 To save the method:
aOn the Method Save Options dialog box, mark all items, and click OK.
bOn the Save Method As dialog box, enter a method name, and click OK.
10b
10a
10c

18 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide
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 H2option is installed (then better MDL can be achieved).
Table 4 Set up information for elements and masses for Environmental Analysis
Element Mass Confirmation
Mass1
Mode Internal
Standard2
Approx. Integration
Time (sec/Point)
Be 9 No gas 6Li 0.3
B11 N
o gas 6Li 0.1
Na 23 He 45Sc 0.05
Mg 24 He 45Sc 0.05
Al 27 He 45Sc 0.3
P 31 No Gas 6Li (72Ge, 45Sc)30.1
K 39 He 9 or 71 0.05
Ca 44 43 He 9 or 71 0.1
V51 He 45Sc 0.5
Cr 52 53 He 45Sc 1
Mn 55 He 45Sc 0.1
Fe 56 57 He 45Sc 0.1
Co 59 He 45Sc 0.1
Ni 60 He 45Sc 1
Cu 63 65 He 45Sc 0.1
Zn 66 64 He 72Ge 0.1
As 75 He 72Ge 1
Se 78 He or (H2)472Ge 5
Br 79 No Gas 72Ge 0.1
Mo 95 98 He 103Rh 0.1
Ag 107 109 No Gas 115In 0.1
Cd 111 114 No Gas 115In, (209Bi) 1
Sn 118 No Gas 103Rh (115In, 209Bi) 0.1
Sb 121 No Gas 115In, (209Bi) 0.1
I 127 No Gas 103Rh (115In, 209Bi) 0.1
Ba 137 135 No Gas 115In, (209Bi) 0.1
Hg 201 202 No Gas 209Bi 1
Tl 205 No Gas 175Lu, (209Bi) 0.1
Pb 208 No Gas 175Lu, (209Bi) 0.1
Th 232 No Gas 175Lu, (209Bi) 0.1
U 238 No Gas 175Lu, (209Bi) 1

G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide 19
Access Method parameters directly
You can access some method panels directly, using the following menu items:
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.
1Select 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:
aSelect Environmental as the Application Type.
bSelect a Sample, such as Drinking Water or High TDS. A description of
the current selection is displayed in the lower part of the window.
cSelect a Regulation, such as EPA200.8 or EPA6020. Only the guidelines
that apply to the selected sample are displayed.
dClick the Next> button.
Method parameters Window Menu Menu item
Method Information ICP-MS Top Methods Edit Method Information
Select Sample Items,
Select QC Items
(Intelligent Sequence
Software is installed)
ICP-MS Top Methods Select QC Items
Interference Equation ICP-MS Top Methods Edit Interference Equation
Acquisition Mode Acquisition EditParameters Set Mode
Spectrum Acquisition
Parameters
Acquisition EditParameters Set Parameters
Peristaltic Pump
Program
Acquisition PeriPump Set Peripump Program
Method Save Options ICP-MS Top Methods Save As

20 G7200-90210 (Rev. A) MassHunter Workstation Quick Start Guide
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:
aRight- click on the element of interest in the Element List Information.
bSelect 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
cIf 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.
eClick 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.