End Group Analysis of Polyisobutylene Succinic Anhydride (PIBSA) Carried Out with Pyrene Excimer Fluorescence
Bibliographic record
Abstract
A procedure is established to determine the molar fraction ( f doubly ) of doubly-maleated polyisobutylene (PIBSA 2 ) in a PIBSA sample mainly constituted of mono-maleated polyisobutylene (PIBSA 1 ), where the succinic anhydride (SA) groups are located at the end of the PIB chain. To this end, a PIBSA sample was labeled with 1-pyrenemethylamine (PyMA) to generate PIB-PySI, where the 1-pyrenemethyl group was linked to the PIB chain via a succinimide group. Depending on the procedure applied to purify the PIB-PySI samples, different regions of the molecular weight distribution (MWD) representing the PIBSA samples could be isolated and characterized by a combination of GPC, FTIR, and UV–vis absorption analysis to yield its MWD, number of isobutylene units per succinic anhydride ( N IB / N SA ), and pyrene content (λ Py, in μmol of pyrene per gram of sample). These analyses were consistent with the expected size and chemical composition of the different PIB-PySI samples. f doubly was calculated from the molar fraction ( f agg ) of pyrene labels attached onto the PIBSA 2 species. f agg was determined through the global model free analysis (MFA) of the fluorescence decays of the pyrene monomer and excimer acquired for solutions of the PIB-PySI samples in THF. The different fractions of the MWD of the PIBSA sample yielded similar f doubly values across the MWD, implying an even distribution of PIBSA 2 species across a PIBSA MWD. The constancy of f doubly across the MWD enabled the determination of the number average molecular weight ( M n ) of the PIB-PySI samples from λ Py . An analysis combining the GPC traces obtained with a differential refractive index and UV–vis absorption detector yielded the MWD of the original PIBSA sample. These experiments demonstrated that the proposed PEF-based methodology can be applied to characterize the SA end groups of PIBSA samples and could be further extended to characterize the end groups of other end-functionalized polymers.
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How this classification was reachedexpand
Full frame machine prediction
Teacher imitationNot calibrated prevalence, not ground truth. Human validation pending. The Gemma side is a direct model label for every work in the frame, read from the title-only record. The Codex side is a classifier learned from the 10,348 direct Codex labels and calibrated to design-weighted sample rates; fields without enough sample support carry no Codex call. Candidate is the union of the two sides; consensus is their intersection. These outputs are machine_predicted_unvalidated and are not human labels.
Distilled classifier scores by category (both heads)
| Category | Codex | Gemma |
|---|---|---|
| Metaresearch | 0.000 | 0.000 |
| Meta-epidemiology (narrow) | 0.001 | 0.000 |
| Meta-epidemiology (broad) | 0.000 | 0.000 |
| Bibliometrics | 0.001 | 0.000 |
| Science and technology studies | 0.000 | 0.000 |
| Scholarly communication | 0.000 | 0.000 |
| Open science | 0.000 | 0.000 |
| Research integrity | 0.000 | 0.001 |
| Insufficient payload (model declined to judge) | 0.002 | 0.001 |
Machine scores (provisional)
The two teacher heads of the student model, read on this work. A score orders the frame for review; it never asserts a category, and the validation status ships verbatim with every row.
Baseline scores from an immature model (maturity gate not passed, 7 training rounds). Scores rank; they never assert a category.
score_only:v0-immature-baseline · verbatim from the scoring run: score_only means the number may rank works, and no category label ships from itClassification
machine, unvalidatedMachine predicted; a candidate call from one source (direct Gemma or distilled Codex), not a consensus.
How this classification was reached, model by model and score by score, is at the end of the page under "How this classification was reached".