Iodine Standard Materials: Preparation and Inter-Laboratory Comparisons
Notice bibliographique
Résumé
The Idaho National Laboratory is preparing to enter the community of AMS practioners who analyze for 129Iodine. We expect to take delivery of a 0.5 MV compact accelerator mass spectrometry system, built by NEC, in the early summer of 2014. The primary mission for this instrument is iodine; it is designed to analyze iodine in the +3 charge state. As part of the acceptance testing for this instrument, both at NEC and on-site in our laboratory, some sort of standard or reference material is needed to verify performance. Appropriate standard materials are not readily available in the commercial marketplace. Small quantities can sometimes be acquired from other laboratories already engaged in iodine analyses. In the longer-term, meaningful quantities of standard materials are needed for routine use in analyses, and for quality control functions1. We have prepared some standard materials, starting with elemental Woodward iodine and NIST SRM 3231 [Iodine-129 Isotopic Standard (high level)] 10-6 solution. The goal was to make mixtures at the 5x10-10, 5x10-11, 5x10-12 ratio levels, along with some unmodified Woodward, in the chemical form of silver iodide. Approximately twenty grams of each of these mixtures were prepared. The elemental Woodward iodine was dissolved in chloroform, then reduced to iodide using sodium bisulfite in water. At this point the NIST spike material was added, in the form of sodium iodide. The mixed iodides were oxidized back to iodine in chloroform using hydrogen peroxide. This oxidation step was essential for isotopic equilibration of the 127 and 129 atoms. The iodine was reduced to iodide using sodium bisulfite as before. Excess sulfites and sulfates were precipitated with barium nitrate. After decanting, silver nitrate was used to precipitate the desired silver iodide. Once the silver iodide was produced, the material was kept in darkness as much as possible to minimize photo-oxidation. The various mixtures were synthesized independently of each other; there were no serial dilutions involved. Aliquots of these four materials have been submitted to five established AMS laboratories where iodine analyses are routinely performed: ETH (Zurich), CNA (Seville), PRIME (Purdue), LLNL (California), and Isotrace (Toronto.) Results from four of these laboratories have been received; in general they indicate that the desired 129/127 ratios have been achieved. We will discuss the results of this informal round-robin exercise. If the installation of the instrument in Idaho goes well, we may have some very preliminary results from the new system. An integral part of data reporting is the approach to data reduction. Accordingly, there will also be some discussion of various philosophies of data handling in regard to the use of standards to adjust data, and background subtraction.
Récupéré en direct depuis OpenAlex et désinversé. Les résumés ne sont pas conservés dans cette base de données : les index inversés représentent 8,6 Go des 9,3 Go de texte de la base, et le serveur dispose de 13 Go libres.
Comment cette classification a été obtenuedéplier
Prédiction machine sur la base complète
Imitation des enseignantsNi prévalence calibrée, ni vérité terrain. Validation humaine à venir. Le volet Gemma est une étiquette directe du modèle pour chaque travail de la base, lue sur la notice réduite au titre. Le volet Codex est un classifieur appris des 10 348 étiquettes directes de Codex et calibré sur les taux pondérés de l'échantillon; les champs sans appui suffisant ne portent aucun appel Codex. Le mode candidate est l'union des deux volets; le consensus est leur intersection. Ces sorties portent le statut machine_predicted_unvalidated et ne sont pas des étiquettes humaines.
Scores du classifieur distillé par catégorie (deux têtes)
| Catégorie | Codex | Gemma |
|---|---|---|
| Métarecherche | 0,034 | 0,032 |
| Méta-épidémiologie (sens strict) | 0,002 | 0,001 |
| Méta-épidémiologie (sens large) | 0,001 | 0,001 |
| Bibliométrie | 0,007 | 0,005 |
| Études des sciences et des technologies | 0,004 | 0,002 |
| Communication savante | 0,003 | 0,001 |
| Science ouverte | 0,004 | 0,003 |
| Intégrité de la recherche | 0,002 | 0,001 |
| Charge utile insuffisante (le modèle a refusé de juger) | 0,009 | 0,008 |
Scores machine (provisoires)
Les deux têtes enseignantes du modèle étudiant, lues sur ce travail. Un score ordonne la base pour la relecture; il n'affirme jamais une catégorie, et le statut de validation accompagne chaque rangée tel quel.
Scores de référence d'un modèle non mature (critères de maturité non atteints, 7 itérations). Un score ordonne; il n'affirme jamais une catégorie.
score_only:v0-immature-baseline · tel quel depuis la passe de notation : score_only signifie que le nombre peut ordonner les travaux, et qu'aucune étiquette de catégorie n'en découleClassification
machine, non validéePrédiction automatique; un appel candidat d’une seule source (Gemma direct ou Codex distillé), pas un consensus.
Le détail, modèle par modèle et score par score, se trouve en fin de page sous « Comment cette classification a été obtenue ».