Manufacture, Homogeneity & Stability of PT samples

SPEX CertiPrep/Protocol Analytical

203 Norcross Ave, Metuchen, NJ 08840

vsivakumar@SPEXCSP.Com

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Studies Offered

Waste Water (WP) Drinking Water (WS) DMRQA Chem DMRQA WET Microbiology (WS) Microbiology (WP)

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Overview

Manufacture Analysis Assigned value Homogeneity Stability Reporting

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Follow EPA (NERL Ci0045) Criteria And NELAC Documents Provide Labs Equal Challenge Use Random Numbers to Select Concentrations

within Range Follow Historical Design Guidelines

Basis for Separation of Analytes Stability Spectral and chemical influences Regression Equations from Historical Data Rules for Number of Analytes Required to be Present

Sample Design

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Raw materials from certified source Analysis for impurities in the raw material Assay for analyte content Weigh out compound Dissolve Add matrix reagent Dilute to volume Flame seal in pre-cleaned glass ampules

Manufacture

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Verification Analysis

Manufacture as per design Verification Analysis NIST RULE: Quality Check: Prepared Value is within + 1/3 of acceptance

limit to a maximum of + 10% of the Prepared Value

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Verification Analysis

NELAC RULE:

Mean of the verification analysis shall be within 1.5 standard deviation as calculated for Laboratory acceptance.

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Method Repeatability

NIST RULE:

Method Repeatability expressed as standard deviation shall be within 1/6 acceptance limits as calculated for the laboratories ( to a maximum of 5% of the prepared value).

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Method Repeatability

NELAC RULE Repeatability limit is 0.5 sd

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Homogeneity

Done prior to sample shipment To establish all samples distributed to the

laboratories have the same assigned value for every parameter to be evaluated.

Done on final packaged samples Samples are selected randomly Number of samples depend on the total number of

ampules Samples are picked from the beginning, middle and

end of the packaging run

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Homogeneity

Samples may be considered homogenous if

Sx < 0.25C

When there is no apparent visual trend.

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Trace Metals LOT#: 21-108T1-PT aArsenic PASS? 0.9963True Value 50Units: ug/L b

49.29 -0.028049.5549.19 c49.31 0.059649.1249.54 d

0.0681

sigma 0.1778389average 49.333333 0Rule1: NIST Rule 1 49.787(TV - 1/3AL) < average < (TV + 1/3AL)

47.967933 < 49.333333 < 52.032067 YESRule 2: NIST Rule 2 s C (2s)Sigma <1/6 AL 3.0481 6.0962

0.1778389 < 1.0160333 YESRule 3: Repeatability Rulestd dev (Sx) < .167C

0.1778389 < 1.0180654 YESRule 4: Homogeneity Rule

Ss (Sx) </ = 0.25C0.1778389 < 1.52405 YES

Rule 5: Verification of Prepared Value (NELAC) Lower UpperTarget value - analyzed value < 1.5 * SD 43.7 55.9

0.67 < 4.57215 YES

Product is Verified and Homogeneious

Acceptance Limits

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UNCERTAINTY

Associated With Preparation Purity Of Raw Material Weighing Make Up To Volume

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Stability

Absolute difference between the mean of the homogeneity verification value (X)and stability verification value should be

|X – Y| < 0.2C

or

Stability value is within 1/3 acceptance limits given for the laboratories

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StabilityTrace Metals LOT#: 21-108T1-PT aArsenic PASS? 0.9963True Value 50Units: ug/L b

49.65 -0.028049.5849.48 c

0.0596

d0.0681

sigma 0.08544average 49.57 0

49.787

Homogeneity Average: 49.333333Stability Rule s C (2s)

(Hx - Sx) < 0.2C 3.0481 6.09620.24 < 1.21924 YES

NIST Stability Rule(TV - 1/3AL ) < average < (TV + 1/3 AL)

47.9679333 < 49.57000 < 52.032067 YES

Lower Upper43.7 55.9

Product Is Stable

Acceptance Limits

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Reports

Final assigned values Study Statistics Review of the Study for pass/fail rate Study Summary Study Discussion Study data Individual Laboratory Reports