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Maintaining and Assuring the Performance of an ICP Spectrometer: A QC Approach

Presented by: Art Ross, Director of Research and Development SCP SCIENCE
Authors: David Smith, Quality Assurance Manager, and Art Ross, Director of Research and Development SCP SCIENCE Member of CRMMA

Abstract
Todays need for continuous accuracy and demonstration of analytical competence has created the need for the periodic checking of ICP spectrometer performance. Monitoring selected critical instrument parameters and taking appropriate corrective action can prevent operational and mechanical problems that will lead to analytical errors and instrument downtime.
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References
Jean-Michel Mermet and Emanuelle Poussel ICP Emission Spectrometers: 1995 Analytical Figures of Merit. Goal was to establish performance criteria to select the best ICP instrument for the analytical requirements. We adapted the criteria to provide a Quality Control tool for ICP spectrometers.
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Quality Control Tests

Monitoring critical instrument parameters like;

Warm up time Long term stability Resolution Repeatability Plasma robustness Signal to noise ratio Raw count verification

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General
ICP Spectrometer used:

Model: Spectro Ciros Vision EOP (2004) Software: Smart Analyzer ver. 1.50.0534

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General
Operating Conditions:

Power of Plasma: 1400w Argon flow rates:

Coolant: 14 l/min Auxiliary: 1 l/min Nebulizer flow: 0.99 l/min

Nebulizer type: Spectro Cross flow Spray chamber: Scott Sample introduction: Peristaltic pump

Note: It is important to maintain the same instrument operating conditions from one test to the other to permit comparison between results. If changes occur, they are to be noted. SCP SCIENCE
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Warm-up time (Short-term stability)

Purpose: Time required for ICP to become sufficiently stable for quantitative analysis. Method: Relative Standard Deviation (RSD) of 5 integrations on 4 sets of data

Ar (I) 404.442 10 ppm Ba (II) 455.403 10 ppm Zn(II) 206.200 difference in intensity between subsequent sets is within +/-1% for all three lines.
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Warm-up time (Short-term stability)

Frequency: Quarterly Possible causes for poor or varying results:

Sample introduction sytem; Environmental conditions; Recirulating cooling system Possible electronic instablity
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Warm-up time (Short-term stability)

Results

<15 minutes is excellent 15 to 20 Very Good 20 to 30 Good 30 to 60 poor >60 very poor

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Warm-up time (Short-term stability)

Corrective Action:

Verify sample introduction system

Cleanilness of sample introduction system Pump tubing, Draining of spray chamber, Pulsation of nebulizer,

Monitor room temperature for fluctuations; Verify chiller is working correctly

Clogged fliters on cooling system

Cooling filters on instrument

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Warm-up time ( <15 minutes)

Warm-Up Time (minutes)
16 14

TIme (Minutes)

12 10 8 6 4 2 0

Action taken: Cleaned torch, changed tubing and cleaned nebulizer.

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06 b-

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Long-term stability
Purpose: To monitor analytical drift over time to minimize required recalibration or restandardization. Method: Comparison of RSD on 5 sets of 10 integrations at 0, 30, 60, 180, 300 and 480 minutes.
Ar (I) 404.442 10 ppm Ba (II) 455.403 10 ppm Zn(II) 206.200

Frequency: Quarterly
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Long-term stability
Results

<1% excellent 1-2% very good 2-3% good 3-5% poor >5% very poor

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Long-term stability
Corrective Action:

Verify sample introduction system - specifically the nebulizer:

Worn out pump tubing Salting on the tip of injector; Devitrefication of torch

Temperature fluctuations in room temperature for non heated optics If argon RSD values are unstable, verify Argon supply

Pressure variations; Purity; Faulty regulator; Freezing of liquid cylinder.

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Long-term stability (2 to 3 %)
Long-term stability
5.0 4.5 4.0 3.5 3.0 Ar (I) Ba (II) Zn (II)

Leak detected in valve on argon supply line which caused inconsistent pressure. Valve replaced.

%RSD

2.5 2.0 1.5 1.0 0.5 0.0 Dec-05 Jan-06 Month Feb-06 Mar-06

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Resolution
Purpose: To determine wavelength resolution. Better resolution means less spectral interference and better Signal to Background Ratio (SBR). Frequency: Yearly Method: Profile analysis of Ba(II) 230.424 nm. Width of the peak at 1/2 its height in nanometers.

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Resolution
Result Compare to manufacture specification Possible causes for poor or varying results: Problems with system optics; Ambient temperature variations in lab. Corrective Action: Verify optical viewing position. Monitor room temperature

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Repeatability
Purpose: To monitor instrument precision. Method: RSD of 15 consecutive readings of Mg(I) 285.213 nm. Frequency: Monthly

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Repeatability
Results

Simultanously

<0.2% Excellent 0.2 to 0.5% very good 0.5 t0 0.8% good 0.8 to 1.2% poor < 0.5% Excellent 0.5 to 1.0% very good 1.0 to 1.5% good 1.5 to 2.0% poor
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Sequential

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Repeatability
Corrective Action: Verify sample introduction
blockages in nebulizer; Worn-out pump tubing.

Voltage line stabilizer.

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Repeatability (0.5 to 0.8%)

Repeatability
0.800 0.700 0.600

%RSD

0.500 0.400 0.300 0.200 0.100 0.000

Verification and replacement of pump tubing.

05

05

06

06

06

05

20 0

06

06

00

00

20

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20

20

20

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/2 0

/2 0

/2 0

/2

/2

1/ 2/

2/

9/

6/

9/

6/

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2/ 20

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30

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Plasma Robustness
Purpose: To monitor sensitivity to matrix effects. Method: Net line intensity ratio of Mg(II) 280.270 nm and Mg(I) 285.213 nm. Frequency: Quarterly

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Plasma Robustness
Results

> 10 Excellent (low sensitivity to matrix effects) 10 to 8 Very Good 8 to 6 Good 6-4 poor <4 very poor (high sensitivity to matrix effects)
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Plasma Robustness
Possible causes for poor or varying results:

Plasma power; Optical viewing position. Optimize plasma power; Position of torch in load coil; Check for load coil deformation.
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Corrective Action:

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Plasma Robustness (6.0 to 8.0)

Plasma Robustness
9.0 8.5 8.0 7.5 7.0 6.5 6.0 5.5 5.0 Nov-05 Dec-05 Jan-06 Feb-06 Mar-06

Results very stable. No action required.

Ratio

Date

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Signal to Background Ratio

Purpose: To verify total instrument optimization and ensure detection limits are optimal. Method: Ratio of 15 readings taken of blank at 231.604 nm and Ni(II) at 231.604 nm Frequency: Monthly
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Signal-Background Ratio
Results

>30 Excellent 30 to 20 very good 20 to 10 good 10 to 2 poor <2 very poor

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Signal-Background Ratio
Possible causes for poor or varying results:

Improper torch alignment with optical interface; Nebulizer flow. Optimization of torch with the optical interface; Optimize nebulizer flow.

Corrective Action:

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Signal to Background Ratio (10 to 20)

Signal to Background Ratio
22.0 20.0 18.0

Adjust torch position.

Ratio

16.0 14.0 12.0 10.0 8.0

20 05

20 05

05

05

06

00 6

20 0

20 0

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12

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1/

2/

2/

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/2

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Raw Count Verification

Purpose: To monitor intensity stability. Method: 10 intensity readings taken of 26 elements at specified wavelengths. 10 ppm for all except K (100 ppm) and Si (5 ppm). Frequency: Monthly
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Raw Count Verification

Possible causes for poor or varying results: Degradation of torch and/or injector; Clouding over of optical interface; Torch position; Nebulizer flow rate

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Raw Count Verification

Corrective Action: Clean or replace torch and/or injector; Clean optical interface; Optimize torch position; Optimize nebulizer flow.

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Raw Count Verification (results)

Mg 1.4E+08 1.3E+08 1.2E+08 1.1E+08 1.0E+08 9.0E+07 8.0E+07
Clean torch and injector.

/0 5

05

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22 /0 5

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05

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2/

2/

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2/

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22

10 /2

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1/

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9/

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2/
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22

/0

Conclusion
Easily self-managed by any lab technician Allows lab manager to predict when routine maintenance is required. Tests take between 5 and 30 minutes

Long term stability requires 90 minutes over 8 hours

Good ROI for preventing down time Predicts when system is ready to use

i.e. Warm up time

Can be use to suggest frequency of Preventative Maintenance Non specific to manufacture of instrument Also available for ICP-MS

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Conclusion
SCP SCIENCE offers necessary documentation and solutions with PlasmaTEST. PlasmaTEST is available for both ICP-AES and ICP-MS.

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Questions?

Thank You! Please come visit us at -

Booth # 3345
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