manufacture, homogeneity & stability of pt samples
DESCRIPTION
Manufacture, Homogeneity & Stability of PT samples. SPEX CertiPrep/Protocol Analytical 203 Norcross Ave, Metuchen, NJ 08840 [email protected]. Studies Offered. Waste Water (WP) Drinking Water (WS) DMRQA Chem DMRQA WET Microbiology (WS) Microbiology (WP). Overview. Manufacture - PowerPoint PPT PresentationTRANSCRIPT
Manufacture, Homogeneity & Stability of PT samples
SPEX CertiPrep/Protocol Analytical
203 Norcross Ave, Metuchen, NJ 08840
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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