ICP-MS USER GUIDE

FOR X-SERIES UNIT

IN LAB 236

THIS DOCUMENT IS A
WORK IN PROGRESS MAY
CHANGE OFTEN. - DON

Table of Contents
Starting and Stopping the ICP-MS...................................................................................... 2
INSTALL TUBING ON PERISTALTIC PUMP........................................................... 4
RESOLVING PROBLEMS.................................................................................................7
PLASMA LIGHTS, BUT DOES NOT STAY ON FOR SOMETIME..........................9
SHUTTING DOWN..................................................................................................... 10
SHUTTING DOWN THE VACUUM PUMP FOR ICP-MS........................................... 11
MAKING A NITRIC ACID DILUTION.......................................................................... 12
MIXING A 10 ppb TUNE A DILUTION......................................................................... 14
CLEANING THE CONES WITH ULTRASOUND.........................................................16
TAKING THE COVER OFF OF THE INSTRUMENT...................................................17
OTHER GENERAL TIPS AND GUIDELINES ..............................................................18

1
 STARTING AND STOPPING THE ICP-MS
TURN ON THE ARGON
1. Turn the Argon gas valve on. The pressure on the secondary lower
pressure regulator will need to maintain at ≥85 psi to light the plasma.

Note: To check whether the pressure is correct, turn off the argon to the
regulator if it is connected. Loosen the nut holding the hose to the regulator
to relieve any left over pressure in the regulator; tighten after releasing gas.
Turn the knob to “Decrease” several turns. Turn the gas on again and adjust
to the 80 psi or so pressure by turning the knob in the direction of
“Increase”. If the tank has adequate pressure, it should be ready for use.

Figure 1: Use the side labeled GAS on the liquid argon tank to attach the
regulator. Use a CGA 580 adapter.

2
TURN ON THE CHILLER

2. Turn on the chiller. The chiller is set for a water temperature of 20°C.
If operating properly, the chiller should reach its target temperature in
less than 3 minutes. Otherwise, when trying to ignite the plasma, an
error message will appear.

Again wait until the chiller reaches a temperature of 20°C before trying to
ignite the plasma.

The chiller requires that enough water in the tank for operations. Never put
DI water into the chiller or this will hasten corrosion. Mix the DI water with
a 50/50 mix of tap water and DI Water. Fill the tank to the point indicated.

Figure 2: The water chiller.

If fresh water, add about a gram of chloramine to inhibit bacterial growth.

If chiller is not cooling, open backside to check if radiator fan is moving.

This model has been known to have a stuck solenoid valve; to dislodge stuck
valve, lift front of instrument about 3 inches from floor and drop it. Yes, that
is right, actual solution from tech support for a stuck valve.

3
INSTALL TUBING ON PERISTALTIC PUMP

3. Tighten the tubing on the peristaltic pump on the ICP-MS. The tubing
sections around the pump should be replaced after 40 hours of use.
This is a peristaltic pump, so make sure to align the tubing so that the
liquid from the samples will uptake by the pump.

Figure 3: Proper configuration for tubing to be mounted onto peristaltic

pump. Tighten the tubing with screws on top. Make firm, but not too tight.

From the Practical Guide to ICP-MS, page 167:

• Manually stretch new tubing before use.

• Maintain the proper tension on tubing.
• Ensure tubing is placed correctly in channel of the peristaltic pump.
• Periodically check flow of sample delivery-throw away tubing if in
doubt.
• Replace tubing in there is any sign of wear-do not wait until it breaks.
• With a high sample workload, change tubing every day or every other
day.

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 • Release pressure on pump when not in use.
• Pump and capillary tubing can be a source of contamination.
• Pump tubing is a consumable-keep a large supply on hand.

Connect sample tubing from auto-diluter or auto-sampler and check the

configuration.

NOTE: For most of our purposes, there are two types of tubing. One is
Black-White/Orange-White and another is Black-White/Black-White. The
latter is 1-mm diameter tubing and this should go after the nebulizer since it
has a large diameter. The tubing is PVC material and that is fine for most of
the acid/water solutions. If using the HPLC and organic compounds are
used, check the tubing for compatibility with organic materials.

Make sure that the tubing connections stay together, otherwise any exposure
to air from an unconnected tubing setup will kill the plasma.

Before sampling, pay attention to the nebulizer pressure on the status bar; it
should be between 1.5 mbar to 2.0 mbar. Too little pressure and there is leak
somewhere; too much and the nebulizer may be plugged.

If running no more samples for the day, always make sure to relieve the
tension on the tubing.

5
COLLECT EXCESS SAMPLE

4. Make sure to have container ready for the excess sample and DI water
rinse. The container may be laboratory glassware or any container that
is made of HDPE (high density poly ethylene). Even a small amount
of diluted nitric acid will lower the pH to around 2 or below.
Neutralize the acid and water solution with ordinary before
pouring down the drain.
5. Turn on auto-sampler.

Once these items are in place, start Plasma Lab and press “ON” to ignite the
plasma.

Figure 4: Ice build up on a tank of argon. The hose popped off of the
regulator and the valve on the tank was not closed. The argon vented at low
pressure for several hours and because of the rapid escape of gas, the ice
formed.

6
RESOLVING PROBLEMS

On occasion, there will be problems igniting the plasma. The errors

displayed by Plasmalab are at times not directly related to the problem at
hand.

First, check that the gas is at the required 90-lbs or so. Remove the air pipe
from the ICP-MS and check whether there is any flow or suction through the
air pipe. Make sure the chiller is at operating temperature. Check the tubing
connected to the nebulizer and make sure there are no leaks.

Check that PlasmaLabService has started. Restart if necessary. The

computer typically stays on to monitor for errors from the ICP-MS. It may
be good to reboot the computer and make sure PlasmaLabService has
started. To find the service, click the “Gears” that are on the task bar.
Try again.

If this still does not work, call Thermo-Fisher technical support at

1-800-642-6538 and describe the problem. The serial number X0448 is
written on the instrument. Write down the reference number. Log the
problem in the MS-Word “Logbook-ICPMS.doc” located on the desktop.

7
It is possible under certain circumstances, for the plasma to not light because
the cone hole is too big. The increased hole size will not allow the plasma to
light because the proper vacuum is not obtainable.

Another trick that helps, and this from Thermo tech support, is to disconnect
the multi-pin cable on the backside of the instrument near the hose to the
output vent. Disconnect this cable and re-connect leaving it disconnected for
several seconds; repeat about 3 to 5 times and try starting plasma again.

Pages 130 to 131 from the X Series ICP-MS Getting Started Guide start-
up guide has a flowchart for troubleshooting plasma start issues.

OTHER PARAMETERS FOR PLASMA

The Load can range from 0 to 255, but should be greater than 90. The Tune
value can range from 0 to 255, but should be AROUND 200.

8
PLASMA LIGHTS, BUT DOES NOT STAY ON FOR SOMETIME
Sometimes the plasma will run for a few minutes and then turn off. First,
make sure that the all the tubing to the nebulizer and from pump is
connected correctly. Any substantial amount of air will interfere with the
plasma staying on for a period of time.

Check to make sure that the silver screen is touching the grounding pin on
the teflon torch holder (inside the cage).

Check the Event Log under the instrument guy icon (the person wearing a
lab coat) to see what errors may have occurred.

Sometimes, after several attempts, the problem will work itself out and the
plasma will stay on for the duration of the available argon.

9
SHUTTING DOWN

Once the samples are run, turn off plasma, loosen tubing from peristaltic
pump, turn off the chiller, turn off the argon gas. Leave the desktop
computer on and the vacuum pump on.

Figure : After using, loosen guides from tubing and loosen the tubing.

Sometimes, the Plasmalab software loses contact while the plasma is

operating. Close Plasmalab, and check to see the status of Plasmaservices.
Restart the services and try Plasmalab again. If this still does not work,
restart the computer and try again. Usually, this should allow a regaining of
control to the ICP-MS.

10
SHUTTING DOWN THE VACUUM PUMP FOR ICP-MS

There are times when it is necessary to totally shutdown the ICP-MS. The
only acceptable times for this is when maintenance is required on the
vacuum pump like changing the oil or to replace the detector that is located
inside the vacuum chamber.

Another acceptable time is if a known power outage to the building is

scheduled.

After the maintenance is completed or the power is back on, return the pump
to a vacuum state.

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 MAKING A NITRIC ACID DILUTION

The guidelines for diluting samples requires a 2% to 5% nitric acid solution.

To make it, one needs ultra-pure nitric acid (Nitric Acid-TraceMetal, Fisher
Chemical , 2.5L Catalog #: A509-212-or equivalent) and DI water.

To mix it, a 1-L volumetric flask, and a graduated cylinder is needed. A

beaker might be good to pour the acid into initially before pouring into the
graduated cylinder.

WARNING: When pouring a concentrated acid directly from the container,

this must be done under a fume hood.

Safety Note: When pouring a strong acid, wear laboratory nitrile or latex
gloves, goggles, and a lab coat or apron. Pour under a fume hood!

Start with the following equation:

V1 C1 = V2 C2

In this example, a 2% solution of HNO3 will be mixed from an

approximately 68% concentrated solution of nitric acid in a 1-L volumetric
flask. The label on the jar of acid should indicate a percentage concentration
of acid or a range. Choose the lower range and up the percentage. Again, the
HNO3 should work out to between 1% to 5%.

V1(68-%) = (1-L) (2-%)

V1 = 0.0294-L

V1 = 29.4-mL

To mix, pour water in a 1-L volumetric flask until it is about ¾ full. Pour 30-
mL of the nitric acid into a clean beaker (do this under the fume hood and
wear goggles, nitrile or latex gloves and a lab coat or apron).

12
Slowly mix the DI water into the flask and mix contents; a bit of heat will be
released. Mix and swish contents until the line is reached on the volumetric
flask.

This is the base for mixing calibration standards and diluting prepared
samples. It is recommended to prepare much since it will be used in other
sample preparations.

The HNO3 dilution does not need to be poured into other containers under a
fume hood.

Most nitric acid purchased is around 68% to 70% concentrated. The

following table is provided for the volumes of nitric acid to mix different
percent solutions. The numbers based on a weight/weight ratio of nitric acid
and water.

Diluting 68% HNO3 with 1-L of DI Water

Percent Volume Required
1% 14.7 - mL
2% 29.4 - mL
3% 44.1 - mL
4% 58.8 - mL
5% 73.5 - mL
Note: Since the HNO3 solution is for preparing a sample or calibration solution to
improve the solubility of metal ions, the volumes can be rounded up to make preparation
easier.

Suggested References: Any MSDS on Nitric Acid.

13
 MIXING A 10 ppb TUNE A DILUTION

Materials necessary: Tune A Solution, a 1% to 5% nitric acid dilution,

volumetric flasks of appropriate volumes to mix the desired ranges, transfer
pipettes, DI water.

A 10 ppb Tune A solution is required for the calibration of the ICP-MS and
obtaining the performance reports. The Tune A solution can be mixed to
other concentration values either higher or lower depending upon the
samples for analysis.

The Tune A Solution from Thermo is at a concentration of 10 mg/L in 5 %

HNO3. The concentration is equivalent to 10 ppm (1 mg/L = 1 ppm) or
10,000 ppb. If purchasing Tune A standard from another vendor, make sure
to beware of the concentration on the label and adjust calculation
accordingly.

How many millilieters of Tune A at 10 mg/L (10, 000) are needed to prepare
1 L (1000 mL) of 10 ppb Tune A?

Ci Vi = Cf Vf

(10,000 ppb) Vi = (1000 mL) (10 ppb)

After rearranging and dividing out the ppb units, the final result is:

Vi = 1 mL

Take 1 L volumetric flask and put the 1 mL first; file to the line with the 1%
to 3% nitric acid solution. Repeat the mathematic and procedure for other
concentrations of Tune A or other necessary standards. Since Tune A is used
to autotune and for the daily performance report, 1L is not too much.

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Application note: If using an Eppendorf, make sure to practice the manual
actions of taking a sample. The best method for checking whether the
pipette and one's technique is good by taking some DI water and pipette 1
mL; weigh this 1-mL of DI water on a 3 to 4 digit scale. If weighs close to
1 gram, then the equipment and technique are good. Remember that for DI
water, 1 mL = 1 gram = 1 cubic centimeter.

What if 250 mL of 5 ppb Tune A solution was necessary?

Ci Vi = Cf Vf

(10 ppb) Vi = (250 mL) (5 ppb)

After rearranging, 125 mL of 10 ppb Tune is necessary. Pour 125 mL of

Tune A into 250 mL volumetric flask and fill the rest with 1% to 5% nitric
acid solution to the fill mark on the flask.

Use this formula and procedure for making other concentrations of standard.

Reference:

Calculating Concentration
http://chemistry.about.com/library/weekly/aa081003a.htm

15
CLEANING THE CONES WITH ULTRASOUND

After some hours of sample analysis, the cones at the entry point of mass
spectrometer will become dirty.

Follow the instructions in the manual for removing the cones from the ICP-
MS.

Fill the ultrasonic unit pictured below with DI water to about an 1 inch to 1.5
inches of the top. Find a small beaker to put the cones in with some DI water
filling the beaker. Do each cone separately for about 15 minutes.

Rinse the cones a couple of times with DI water while in the beaker. Try to
minimize contact with the cones unless wearing gloves. Set the cones out to
dry. After drying, reinstall the cones.

After cleaning the cones or installing new ones, run some 300 ppm Ca+
conditioning solution to prepare cones. The Ca+ in a plasma deposits a
ceramic surface.

16
TAKING THE COVER OFF OF THE INSTRUMENT

Sometimes it is necessary to remove the cover from the ICP-MS to access

the circuit breakers, vacuum cage, or vacuum chamber.

If turning off the breakers to reset the instrument, leave them off for at least
30 seconds before turning back on. This should allow for most of the
electronics to discharge.

The breaker to the far right says “Electronics Embedded PC Rotary Pump
Turbo Pump”. This breaker also controls the roughing pump on sitting on
the floor beneath the table. If it does not come back on after resetting the
breaker, press the RED button on the board just to the right. The GRAY
button stops the roughing pump.

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OTHER GENERAL TIPS AND GUIDELINES

(TUNING, AUTOTUNES, PERFORMANCE REPORTS)

Most of this if from the class instruction provided by Thermo.

1. Before tuning, doing a performance report, or running samples, run

instrument for about 15 minutes.

2. Run a performance report at the beginning; unless there are problems,

no need to run again. The PlasmaLab software records every
performance report ever done.

3. Auto-tunes are only necessary after replacing the cone and torch, but
only do an autotune if it fails the performance reports.

4. Instrument requires a good Tune to acquire a good mass calibration,

but no required often.

5. Detector set-up: voltages set by cross calibration; should be done

regularly.

6. Must have >400,000 counts for analogue counting to be engaged.

7. Never use an AA standard for ICP-MS.

8. Calibration: (2) points are enough. A blank and an upper limit. Could
be validated by preparing a standard in between those values.

9. Boron, antimony, and molybdenum “stick” to tubing and glass. May

require an alkaline solution to wash out effectively.

10.If the elements are unknown, run sample with out the internal
standards and see what is in the sample. Then adjust or choose the
procedure depending upon elements that you are looking for.

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11.Pay attention to interferences when setting up experiment. To reduce
interferences, choose an isotope that is less abundant.

12.As the argon gas decreases in the tank, Kr (Krypton) does not bail off
as fast and that may generate interferences that require a correction for
certain analysis (like with arsenic and selenium).
13.If the plasma is flickering, this may indicate the flow is too high. Call
maintenance to have Siemens adjust the flow rate within an acceptable
range

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