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Analytics · Method validation · continued

Repeatability versus intermediate precision posts 121–135

This is a continuation of a long topic, addressed by post number rather than by page. Start at post 1 · go to the accepted answer.

CB
c.bakkerTL22 Jul 2025#121

Limits of detection and quantitation: LOD is the lowest concentration that produces a signal above background. LOQ is the lowest concentration at which the method meets precision and accuracy acceptance criteria. Both are determined empirically.

It reads as pedantry until the day it does not.

0 likes 13mo
MB
m.brobergTL22 Jul 2025#122

Clear enough that I do not think I have a follow-up, which is unusual.

3 likes 13mo
SL
s.leclercTL4 Moderator2 Jul 2025#123

Taking post #120 at face value and following it one step further.

Taking repeatability versus intermediate precision seriously for a moment rather than deflecting: the honest position is that the community has observations and no controlled comparison, and those two things support very different sentences.

11 likes 13mo
MI
m.ibarraTL22 Jul 2025#124
KTurkington, post #33: An observation about repeatability versus intermediate precision that I cannot explain and am posting anyway, on the principle that unexplained observations are more useful public than private. Go to post

Marking my uncertainty on repeatability versus intermediate precision explicitly. I am confident about the direction, much less confident about the size, and not confident at all that it generalises past the case in the first post.

24 likes in reply to #33 13mo
AF
a.friskTL22 Jul 2025 · edited#125

Post #124 answers the question as asked. The question underneath it is different.

The most useful single question about a method: what would it fail to detect? Every method has an answer and few documents state it.

This has been discussed before and I could not find the thread, so, again.

0 likes 13mo
PM
p.mbekiTL22 Jul 2025#126
NM
n.moreauTL23 Jul 2025#127

Precision has two levels worth distinguishing: repeatability within a run and intermediate precision across days, analysts and instruments. The second is where most methods lose the numbers people quote.

7 likes 13mo
JN
j.nascimentoTL23 Jul 2025#128
unit_conversion, post #47: On post #46 — agreed on the reasoning, with one qualification. Distinguishing three things in the repeatability versus intermediate precision discussion that keep getting used interchangeably: the observation, the proposed mechanism, and the recommendation that gets attached to both. Go to post

Reading back through the repeatability versus intermediate precision threads from last year, the same three questions come up every time and only one of them has ever been answered properly. That seems like a documentation gap rather than a knowledge gap.

17 likes in reply to #47 13mo
TH
TL4_HalvorsenTL4Leader · Journal club3 Jul 2025#129
a.frisk, post #36: Where I part company with post #33, and it is a narrow parting. Two sentences on repeatability versus intermediate precision and then I will stop, because the rest is speculation and the thread is better without mine. What is documented is narrow. What is inferred from it is broad. The gap between them is where every argument here lives. Go to post

That is the distinction I keep failing to hold on to. Written down now.

3 likes in reply to #36 13mo
CA
c.amankwahTL23 Jul 2025#130

On repeatability versus intermediate precision: the maintained page in the documentation commons covers the general case with citations and a review date, which is more reliable than any reply here including this one.

11 likes 13mo
RV
r.venkatesanTL3Wiki editor3 Jul 2025#131
unit_conversion, post #47: On post #46 — agreed on the reasoning, with one qualification. Distinguishing three things in the repeatability versus intermediate precision discussion that keep getting used interchangeably: the observation, the proposed mechanism, and the recommendation that gets attached to both. Go to post

Post #130 and I disagree about the size of the effect, not about the direction.

The limit of quantitation determines what the impurity table can honestly contain. Peaks below it can be reported as detected and cannot be reported as a number.

I would be interested in a counterexample if anyone has one.

0 likes in reply to #47 13mo
KP
k.pereiraTL23 Jul 2025#132
b.oyler, post #18: A note on scope: what I am saying about repeatability versus intermediate precision applies to the case in the first post and I would not extend it further without checking. Go to post

Source for the repeatability versus intermediate precision figure, since it was asked for. It is in the discussion rather than the abstract, which is why the version circulating is stronger than the paper is.

Reading the surrounding paragraph is worth the two minutes. The authors are more careful than their summarisers.

23 likes in reply to #18 13mo
MM
maintenance_modeTL3Regular3 Jul 2025 · edited#133

Repeatability versus intermediate precision is one of those subjects where the general answer and the answer for a specific case diverge, and the thread will go in circles until someone says which one is being asked for.

10 likes 13mo
AP
au.pereiraTL23 Jul 2025#134

System suitability is the ongoing evidence that a validated method is still performing. Validation is done once; suitability is done every run, and it is the one that appears on a certificate.

3 likes 13mo
TY
two_year_lineTL3Regular3 Jul 2025#135
s.bergstrom, post #34: Where a pharmacopoeial monograph exists, a method that follows it inherits a great deal of assurance. Almost nothing discussed here has one. Go to post

Post #133 put the caveat in the right place and I want to underline it.

Where a pharmacopoeial monograph exists, a method that follows it inherits a great deal of assurance. Almost nothing discussed here has one.

32 likes in reply to #34 13mo

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