ICP-MS (CAL-0117) – Calibration Documents

Calibration Documents: ICP-MS (CAL-0117)

Asset ID CAL-0117
Equipment ICP-MS
Equipment Type ICP-MS
Department QC
Area/Location Instrument Room
Process Use Elemental
Parameter Mass accuracy
Units amu
Range Min 0
Range Max 300
Acceptance Criteria ±0.1
Calibration Frequency (days) 365
Calibration Type External
Traceability ISO17025

Table of Contents

  1. Calibration SOP
  2. Calibration Protocol
  3. Calibration Checklist
  4. Deviation Impact Assessment
  5. Calibration Certificate

Calibration SOP

1. Purpose

The calibration of the ICP-MS (Asset ID: CAL-0117) is performed to ensure the accuracy of mass measurements, which is critical for maintaining patient safety, ensuring batch quality, and preserving data integrity. Accurate elemental analysis is essential in the QC department to prevent erroneous results that could impact product safety and efficacy.

2. Scope

  • Asset ID: CAL-0117
  • Equipment Name/Type: ICP-MS
  • Department/Area: QC / Instrument Room
  • Process Use: Elemental
  • Parameter: Mass accuracy
  • Range: 0 – 300 amu
  • Units: amu
  • Calibration Frequency: 365 days

3. Definitions

  • Calibration: The process of comparing a measurement instrument to a known standard to ensure accuracy.
  • Verification: The confirmation that a measurement instrument meets specified requirements.
  • Adjustment: The process of modifying a measurement instrument to bring it into compliance with specifications.
  • As Found: The condition of the instrument prior to any adjustments made during calibration.
  • As Left: The condition of the instrument after adjustments have been made and verified.
  • OOT (Out of Tolerance): A condition where the measurement falls outside the defined acceptance criteria.
  • Drift: The gradual change in the measurement accuracy of an instrument over time.
  • Traceability: The ability to verify the history, location, or application of an item by means of documented recorded identification.
  • Measurement Uncertainty: A parameter that characterizes the range of values within which the true value is expected to lie.
  • Intermediate Check: A verification process performed between calibrations to ensure ongoing accuracy.

4. References

  • Company Metrology SOP [TBD]
  • ISO/IEC 17025 traceability via calibration certificates
  • ALCOA+ principles

5. Responsibilities

  • Technician/Metrology: Perform calibration and document results.
  • QC/QA Reviewer: Review calibration documentation and results for compliance.
  • Owner Department: Ensure equipment is available and maintained.
  • External Service Provider: Conduct calibration as per external calibration type.

6. Safety & Preconditions

  • Ensure environmental controls are in place (temperature, humidity).
  • Allow for warm-up/stabilization of the ICP-MS as per manufacturer guidelines.
  • Maintain cleanliness of the instrument and surrounding area.
  • Check leveling of the instrument.
  • Verify power supply stability.
See also  Skid pH Sensor (CAL-0314) - Calibration Documents

7. Standards & Tools

  • Reference Standards Required: [TBD]
  • Traceability Statement: ISO17025
  • Certificate Validity Check: Ensure all certificates are current and valid.
  • Standard ID Placeholders: [TBD]

8. Calibration Strategy

The calibration will follow the As Found and As Left logic. The minimum number of test points will be five, including endpoints and midpoints within the specified range (0 – 300 amu). It is recommended to take three replicate readings at each point to ensure accuracy.

9. Step-by-Step Procedure

  1. Preparation: Gather all necessary tools and reference standards.
  2. Stabilization: Allow the ICP-MS to warm up for the specified time.
  3. As Found checks and data capture: Record initial measurements before any adjustments.
  4. Adjustment rules: If OOT is detected, follow the adjustment protocol; if not allowed, escalate to QA.
  5. As Left verification: Confirm that the instrument is within tolerance after adjustments.
  6. Labeling + documentation completion: Ensure all records are filled out accurately and contemporaneously (ALCOA+).

10. Acceptance Criteria & Calculations

The acceptance criteria for mass accuracy is ±0.1 amu. The error calculation formula is:

Error = (Observed Value – True Value)

Pass/Fail Logic: If the absolute value of the error is less than or equal to 0.1 amu, the calibration passes; otherwise, it fails.

Rounding rule: [TBD]

11. Handling OOT / Failures

  • Immediate containment: Tag the equipment and stop use.
  • Notification & deviation initiation: Notify QA and document the deviation.
  • Impact assessment trigger: Define the impact window and review affected results/batches.
  • Recalibration after repair/adjustment: Ensure recalibration is performed before returning to service.
  • QA disposition placeholders: [TBD]

12. Records & Retention

  • Logbook entries: Document all calibration activities.
  • Calibration report/certificate filing: Maintain records as per company policy.
  • e-Records if applicable: [TBD]
  • Label content requirements: Include calibrated date, due date, technician name, and status.

13. Annexures

Annexure A: Calibration Data Sheet

Test Point Reference Observed Error Acceptance Pass/Fail As Found As Left
[TBD] [TBD] [TBD] [TBD] [TBD] [TBD] [TBD] [TBD]

Annexure B: Quick Checklist

  • Environmental controls verified
  • Instrument warm-up completed
  • Calibration standards prepared
  • Documentation ready
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Annexure C: Example Label Text

Calibration Date: [TBD]

Due Date: [TBD]

Calibrated By: [TBD]

Status: [TBD]

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Calibration Protocol

Calibration Protocol

Protocol ID Asset ID Equipment Name Equipment Type Dept Area Process Use Parameter Units Range Acceptance Criteria Frequency Calibration Type Traceability
[TBD] CAL-0117 ICP-MS ICP-MS QC Instrument Room Elemental Mass accuracy amu 0 – 300 ±0.1 365 days External ISO17025

Environmental Conditions

Temperature: [TBD]

Relative Humidity: [TBD]

Vibration: [TBD]

Drafts: [TBD]

Test Point Selection

  • Minimum: 0 amu
  • 25%: 75 amu
  • 50%: 150 amu
  • 75%: 225 amu
  • Maximum: 300 amu

Results Table

Test Point Ref Value Observed (As Found) Error Limit Pass/Fail Observed (As Left) Error Pass/Fail
0 amu [TBD] [TBD] [TBD] ±0.1 [TBD] [TBD] [TBD] [TBD]
75 amu [TBD] [TBD] [TBD] ±0.1 [TBD] [TBD] [TBD] [TBD]
150 amu [TBD] [TBD] [TBD] ±0.1 [TBD] [TBD] [TBD] [TBD]
225 amu [TBD] [TBD] [TBD] ±0.1 [TBD] [TBD] [TBD] [TBD]
300 amu [TBD] [TBD] [TBD] ±0.1 [TBD] [TBD] [TBD] [TBD]

Stepwise Instructions

  1. Preparation: Ensure the ICP-MS is clean and properly set up in the Instrument Room.
  2. Stabilization: Allow the instrument to stabilize for [TBD] minutes before calibration.
  3. Performing Readings: Take three replicate readings at each test point.
  4. Calculating Error: Calculate the error for each test point using the formula: Error = Observed – Ref Value.
  5. Evaluation: Compare the calculated error against the acceptance criteria of ±0.1 amu.
  6. Documentation: Record all observations in the results table and ensure data integrity (ALCOA+).

Deviation Instruction for OOT

  • Stop use of the ICP-MS immediately.
  • Notify the QA department of the out-of-tolerance condition.
  • Open a deviation report for the OOT findings.
  • Quarantine impacted results window: [TBD]
  • Await QA decision on further actions.

Approvals

Prepared Reviewed Approved
[Signature/Date] [Signature/Date] [Signature/Date]

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Calibration Checklist

Asset ID Equipment Dept Area Parameter Range Acceptance Frequency Traceability
CAL-0117 ICP-MS QC Instrument Room Mass accuracy 0 – 300 amu ±0.1 365 days ISO17025

Pre-calibration

  • [ ] Verify environmental conditions are within specifications
  • [ ] Ensure equipment has warmed up for the required duration
  • [ ] Clean the equipment as per SOP
  • [ ] Level the equipment if necessary
  • [ ] Check validity of reference standards
  • [ ] Ensure logbook is ready for recording
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As Found Execution

  • [ ] Set initial measurement setpoints
  • [ ] Perform repeat measurements as required
  • [ ] Record all raw data accurately
  • [ ] Perform necessary calculations

OOT Immediate Actions

  • [ ] Tag out the equipment
  • [ ] Stop use of the equipment
  • [ ] Notify appropriate personnel
  • [ ] Document deviation
  • [ ] Trigger impact review

As Left Verification

  • [ ] Conduct post-adjustment checks
  • [ ] Confirm results are within acceptance limits

Documentation & Closure

  • [ ] Update equipment label
  • [ ] Attach calibration certificate
  • [ ] Obtain reviewer sign-off
  • [ ] Update next due date in logbook

Data Integrity (ALCOA+): Ensure all data is Attributable, Legible, Contemporaneous, Original, and Accurate.

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Deviation Impact Assessment

Event Summary
Asset: ICP-MS
Date: [TBD]
Discovered By: [TBD]
Document References: [TBD]
As Found Results Summary: [TBD]

Immediate Containment Checklist

  • Stop use of the asset
  • Label/tag the asset as out of tolerance
  • Segregate impacted work

Define Impact Window

Last Known In-Tolerance Date Discovery Date
[TBD] [TBD]

Product/Batch/Test Impact Review

Batch/Study/Report ID Results Potentially Impacted Re-Test/Re-Weigh Decision
[TBD] [TBD] [TBD]

Data Integrity Review Prompts (ALCOA+)

  • Attributable: [TBD]
  • Legible: [TBD]
  • Contemporaneous: [TBD]
  • Original: [TBD]
  • Accurate: [TBD]
  • Complete: [TBD]
  • Consistent: [TBD]
  • Enduring: [TBD]
  • Available: [TBD]

Risk Assessment

Severity Probability Detectability Rationale Overall Risk
[TBD] [TBD] [TBD] [TBD] [TBD]

Investigation Summary

Root Cause: [TBD]

CAPA Plan

Action Owner Due Date Effectiveness Check
[TBD] [TBD] [TBD] [TBD]

QA Disposition

Release/Hold/Retest/Recall Triggers: [TBD]

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Calibration Certificate

Certificate No: [TBD]

Date: [TBD]

Next Due Date: [TBD]

Asset Details

Asset ID Equipment Name Equipment Type Dept Area Make/Model Serial No Location Parameter/Range/Units Acceptance Criteria
CAL-0117 ICP-MS ICP-MS QC Instrument Room [TBD] [TBD] [TBD] Mass accuracy (0 – 300 amu) ±0.1

Conditions

Environment: [TBD]

Reference Standards

Standard Name/ID Certificate No Due Date Traceability Statement
[TBD] [TBD] [TBD] Traceability to ISO17025

Results

As Found Results

Test Point Result (amu)
1 [TBD]
2 [TBD]
3 [TBD]
4 [TBD]
5 [TBD]

As Left Results

Test Point Result (amu)
1 [TBD]
2 [TBD]
3 [TBD]
4 [TBD]
5 [TBD]

Measurement Uncertainty Statement: [TBD]

Statement of Conformity: [Pass/Fail overall]

Remarks: [TBD]

Signatures

Performed by: ____________________ Date: ___________

Checked by: ____________________ Date: ___________

Approved by: ____________________ Date: ___________

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