SOP For Operation and Calibration of ICP-MS

This document details the procedure for operation and calibration of ICP-MS. It is the policy of XYZ Pharmaceuticals Limited that a written procedure shall be followed for the operation and calibration of ICP-MS.

This procedure is to be applied at the time of operating and calibration of ICP-MS (Inductively coupled plasma mass spectrometry). 

RESPONSIBILITY & Accountability

Persons along with their responsibilities are given below:

Executive   – Corporate Quality Assurance:- To prepare the SOP

Trainee Analyst/ Jr. Analyst/ Analyst/ Sr. Analyst:- To follow the SOP accordingly

Manager-Quality Control:- To ensure implementation of SOP


Check and ensure that:

5.0.1  The instrument is clean and free from dust. If not, then clean the instrument using a lint-free duster.

5.0.2  Switch on the blower and recirculater. It will circulate the coolant into the instrument to minimize the temperature of the instrument.

5.0.3 Before the ignition of the plasma, Vacuum pressure should be 10-4 torr.

5.0.4  Open software.

>Operation and Calibration of GC with FID & ECD


5.1.1    Argon gas cylinder should not be used below 100 psi in terms of gas quantity.

5.1.2     Release gas pressure should be between 60-80 psi.

5.1.3     Ensure that laboratory temperature is between 20 to 25 oC.

5.1.4     Ensure that humidity of the laboratory is between 40 to 60 % RH.





Sample waste container level


Check the level of the waste solution in the container.

Quartz torch


Visually check the torch condition and measure for proper alignment.

Peristaltic Pump


Visually check for the acceptable roller pressure, condition of the sample tubing and the drain tubing, and correct pump rotation.

Roughing Pump Oil


Visually check the condition and level of the oil.

Sampler and skimmer cones

Weekly or as necessary

Visually check the condition of each cone for cleanliness and proper orifice size.



Check and replace as needed.

Pump Oil

Every 3 months

Change pump oil.


As necessary

Check and adjust to the proper voltage.

Mist Eliminator


Visually check the sight glass. It should be clear of oil.


5.3.1    Disconnect the Instrument from the main power supply.

5.3.2    Clean the instrument externally with a clean and lint-free cloth daily.

SOP For Operation and Calibration of ICP-MS


5.4.1    Switch on the blower and recirculater.

5.4.2    Before the ignition of the plasma, Vacuum pressure should be 10-4 torr.

5.4.3    Open software.

5.4.4     Open “Workspace”-------quantitative analysis .wrk.

5.4.5    Open “Method”---“File” ---- Select a file or create “New File “ according to the requirement.

5.4.6    Set the parameters of analytics. (If “New File” is being selected)

5.4.7    Feed “Calibration Values” ---- Decide “Report format”.

5.4.8    Analyze ---“Blank” --- “Standard” ---- “Sample”.

5.4.9       If one wants to check the old data: Go to “Data set” --- Select the row ---“Reprocess report---See”” Summary. report”

5.4.10 Save calibration curve before shutting down of the computer.(Tuning file should not be   changed.)

5.4.11 Before switching off “Plasma” ---- Flush with wash solution at least for 15 minutes so that no memory is left.

5.4.12 Close the software: Switch off the blower and the recirculater. Close the gas supply from the cylinder keeping the flow in the pipeline.

5.4.13   Daily performance check: Instrument shall be calibrated on daily basis before analysis. calibration of instrument and selection of elements depends upon the sample for analysis on that day. for the daily calibration should not be less than 0.99. Data of calibration shall be preserved in hard copy as well as soft copy.


6.0.1 Linearity at Different Concentrations   Dilute the standard solution (Make: Plasma Cal SCP Science) containing 1000 ppm of arsenic (As), Lead (Pb), Mercury (Hg), and Cadmium(Cd) in the following way:

1000 ppm         100 ppm               10 ppm          1 ppm            100 ppb

20 ppb

10 ppb

 5 ppb

2 ppb Aspirate each concentration i.e. 20 ppb, 10 ppb, 5 ppb, and 2 ppb four times into the instrument.   Acceptance Criteria: Concentration mean of each aspiration should come the same as the dilution concentration. Linearity of different elements of different concentrations should not be less than 0.99.


7.0.1     Standardizations of the instrument are done once a month.

7.0.2     Switch on the blower & recirculates.

7.0.3     Before the ignition of the plasma, vacuum pressure should be 10-6 torr.

7.0.4     Open Software.

7.0.5     Open “Instrument “---------Start Plasma

7.0.6     Leave the plasma for 30 minutes or more (minimum 25 minutes).

7.0.7     Open ----“Workspace” ----------“Daily Performance .wrk”

7.0.8      Place the tuning solution( Make : Setup/Stab/Masscal Solution PE# N8125030.) containing 10 ppb of Magnesium(Mg), Indium(In) , Barium (Ba), Cerium (Ce)  and Uranium (U).

7.0.9  Analyze the above solution as “Sample “. 

7.0.10 Do  Quarterly Performance Check

Mg intensity > 40,000 cps/10 ppb

In Intensity > 250, 000 cps/10 ppb

U intensity > 200,000 cps/10 ppb

CeO/Ce ;Ba++/Ba < 3 %

Background 220 <2 cps

7.0.11    Observed intensity is acceptable up to 20% below from actual value; if it is below the 20% of the above-stated values then re-optimization is required.

7.0.12 Following parameters should be considered for re-optimization.

Nebulizer Gas Flow (NEB)

Auxiliary Gas Flow

Plasma Gas Flow

Lens Voltage

Inductively Coupled Plasma Radio-frequency (Rf) power

Analog Stage voltage

Pulse Stage voltage

Quadrupole Rod Offset (QRD)

Cell Path Voltage (CPV)

7.0.13     Click on get Analyte list Icon & select Analyte from Analyte Icon i.e.Mg

7.0.14     Select optimization criteria & select maximum intensity.

7.0.15     Click on optimize icon.

7.0.16     Repeat the steps 7.4.8, 7.4.9 & 7.4.10 for the above-mentioned parameters individually i.e. Nebuliser

Gas Flow, Auxiliary Gas Flow, and Plasma Gas flow

SOP For Operation and Calibration of ICP-MS


Generate Instrument Calibration number on calibration datasheet as INSCALXXYYZZZ

Where INS denotes Instrument, CAL denotes Calibration, XX denotes the year, YY denotes Month ZZZ denotes sequence number.


INS CAL:           Instrument Calibration

RPM:           Rotation per minute

USPRS:           United State Pharmacopoeia Reference Standard

A. R. No. :           Analytical report number          


Working Instructions (Inductively Coupled Plasma Mass Spectrometer); Issue Date: Jan 2006

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