Appendix 3 — Method Verification Record

Parent procedure: 10 – Test and Calibration Methods

Purpose

To document objective evidence that a standard or published method can be performed by this laboratory with the performance characteristics required for its intended use. A verification record is required before any standard method is used for the first time, and following significant changes to equipment, personnel, or method edition.

Instructions

1. Complete one record per verification study. Where a standard method covers multiple analytes and all are verified in a single study, one record covering all analytes is acceptable.
2. Define all acceptance criteria in Section 3 before beginning experimental work.
3. Attach raw data and instrument output as annexes.
4. The completed record is reviewed and authorized by the Technical Manager before the method is released for routine use.
5. File as a controlled document per Procedure 00.

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Section 1 — Method Identification

Field	Entry
Verification record number	VER-[NNN]
Method name	[e.g., Karl Fischer coulometric titration for moisture determination]
Method ID (from Method Register)	[e.g., M-002]
Reference standard	[e.g., ISO 760:2020]
SOP number	[e.g., SOP-10-002 Rev. 01]
Reason for verification	☐ First use of method in laboratory · ☐ New instrument / significant instrument change · ☐ Method inactive >12 months · ☐ New edition of referenced standard · ☐ Other: [specify]
Scope of this verification	[Analytes, matrices, and concentration range covered by this verification — must fall within the published scope of the standard method]
Verification conducted by	[Analyst name and role]
Date(s) of study	[Date or range]

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Section 2 — Equipment and Materials Used

Item	Description	Equipment ID / Lot number	Calibration / expiry status
[Primary instrument]	[e.g., Karl Fischer coulometric titrator]	[e.g., AI-003]	[Calibrated — cert. ref.]
[Balance]	[e.g., Analytical balance, 0.1 mg]	[e.g., BA-001]	[Calibrated — cert. ref.]
[CRM / Reference material]	[e.g., Certified water standard, 1 mg/g H₂O]	Lot: [number] · Exp: [date]	[ISO 17034 certified]
[Reagents / titrant]	[e.g., Hydranal Composite 5, Karl Fischer reagent]	Lot: [number] · Exp: [date]	—
[Matrix sample for method check]	[e.g., In-house NMC cathode material, homogeneity confirmed]	[Internal ref.]	—
[Add rows]

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Section 3 — Acceptance Criteria (completed before experiments begin)

Enter criteria before beginning work. Source of criterion (method document, customer spec, laboratory requirement) must be stated.

Parameter	Acceptance criterion	Source of criterion
Trueness (CRM recovery)	[e.g., Recovery 97–103% of certified value]	[e.g., ISO 760 performance data / Technical Manager requirement]
Repeatability (RSD)	[e.g., RSD ≤ 1.5% for n = 10 replicates at working level]
Blank / background	[e.g., Blank titration < 0.01 mg H₂O equivalent]
LOQ confirmation (if applicable)	[e.g., RSD ≤ 10% and recovery 80–120% at LOQ]
Measurement range check (if applicable)	[e.g., Recovery within ±5% at low and high range limits]
[Add parameters as appropriate]

Technical Manager pre-approval of criteria: [Name] — Date: [Date]

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Section 4 — Trueness Study

4.1 CRM analysis

Analyze the CRM under the same conditions as routine samples. Minimum 6 replicates recommended.

Replicate	Measured value	Unit
1		[e.g., mg H₂O / g]
2
3
4
5
6
[Add rows if n > 6]
Mean
SD
RSD (%)

CRM certified value	[Value ± expanded uncertainty U, k=2]
Recovery (%)	[Mean measured / certified value × 100]
Within acceptance criterion?	☐ Yes · ☐ No

4.2 Spike recovery (if applicable)

Complete if CRM recovery alone is insufficient to confirm trueness in the target matrix.

Sample	Spike added	Native level	Expected total	Measured	Recovery (%)	Within criterion?
Matrix spike 1	[Value]	[Value]	[Value]	[Value]	[Value]	☐ Yes · ☐ No
Matrix spike 2	[Value]	[Value]	[Value]	[Value]	[Value]	☐ Yes · ☐ No
Matrix spike 3	[Value]	[Value]	[Value]	[Value]	[Value]	☐ Yes · ☐ No

Trueness conclusion: ☐ Pass · ☐ Fail — [Brief comment]

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Section 5 — Repeatability Study

If the trueness study used ≥ 6 replicates of the same material, this data may serve for both trueness and repeatability. If a separate repeatability study is conducted (e.g., using a stable in-house sample rather than a CRM), record it here.

Sample used: [Description] · Date: [Date] · Analyst: [Name]

Replicate	Result	Unit
1
2
3
4
5
6
[Add rows if n > 6]
Mean
SD
RSD (%)
Within acceptance criterion?	☐ Yes · ☐ No

Repeatability conclusion: ☐ Pass · ☐ Fail

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Section 6 — Additional Parameters (complete as applicable)

6.1 Blank / background

Blank type	Result	Unit	Within criterion?
[e.g., Reagent blank (no sample, full titration sequence)]	[Value]	[e.g., mg H₂O equivalent]	☐ Yes · ☐ No
[e.g., Method blank (empty vessel through full procedure)]			☐ Yes · ☐ No

6.2 Measurement range check

If the method is verified across a concentration range (not just at a single working level), record results at range limits.

Range limit	Nominal level	Measured result	Recovery (%)	Within criterion?
Low end	[Value]	[Value]	[Value]	☐ Yes · ☐ No
High end	[Value]	[Value]	[Value]	☐ Yes · ☐ No

6.3 LOQ confirmation (if applicable)

Analysis at or near the claimed limit of quantification.

Replicate	Result at LOQ level	Unit
1
2
3
4
5
6
Mean
RSD (%)
Recovery (%)
Within acceptance criterion?	☐ Yes · ☐ No

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Section 7 — Summary

Parameter	Result summary	Conclusion
Trueness	[e.g., CRM recovery 99.2%, RSD 0.8%, n=10]	☐ Pass · ☐ Fail
Repeatability	[e.g., RSD 0.9%, n=10]	☐ Pass · ☐ Fail
Blank	[e.g., < 0.005 mg H₂O equivalent]	☐ Pass · ☐ Fail
Range check	[e.g., Recovery 98–101% at both ends]	☐ Pass · ☐ Fail · ☐ N/A
LOQ confirmation	[e.g., RSD 6.2%, recovery 94%]	☐ Pass · ☐ Fail · ☐ N/A

Overall verification conclusion:

☐ Verified — method approved for routine use within the scope defined in Section 1.

☐ Verification failed — the laboratory was unable to achieve the required performance. The method may not be used until the cause is identified, resolved, and a successful verification study is completed. Required actions: [Specify]

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Section 8 — Annexes

Annex	Description	File name / Location
A	CRM certificate (current)	[File name / archive ref.]
B	Raw data — CRM replicates	[File name]
C	Raw data — repeatability study	[File name]
D	Raw data — blank measurements	[File name]
E	Instrument output files	[File name / folder ref.]
[Add rows]

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Authorization

Role	Name	Signature	Date
Study conducted by	[Analyst]		[Date]
Reviewed and authorized	[Technical Manager]		[Date]

By authorizing this record, the Technical Manager confirms that the verification study demonstrates that the laboratory can perform the method with the required performance characteristics, and that the method is approved for routine use within the stated scope.