Determination of residual (free) monomer in water based polymer emulsions by head space gas chromatography mass spectrometry

Petha, Narendra H.; Lokhande, R. S.; Patil, Raju M.; Seshadri, Devender T.

doi:10.1016/j.polymertesting.2017.09.002

Cited by 4 publications

(5 citation statements)

References 3 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…Hence, we developed a simple yet sensitive method to measure styrene in aqueous solutions. Compared with the GC and LC methods, the limit of detection of our UV method (limit of detection, 0.1 μg/mL) is in the same range as for the GC method 37 while higher than for the LC method. 39 , 40 …”

Section: Methodsmentioning

confidence: 86%

“…Styrene detection was traditionally measured by gas chromatography–mass spectrometry (GC–MS), − high-performance liquid chromatography with a UV detector (HP-LC), , or an electrochemical method . Back in 1951, UV–vis was used for styrene detection in solid PS samples .…”

Section: Methodsmentioning

confidence: 99%

“… 42 The ISO (ISO 2561:2015; 1974) issued the standard method of residual styrene determination in PS products by GC. Few studies used GC, 43 GC–MS 37 and HP-LC 39 , 40 to detect styrene in aqueous solutions. However, these techniques were either tedious or expensive because the columns are easily contaminated.…”

Section: Methodsmentioning

confidence: 99%

See 2 more Smart Citations

Role of Residual Monomers in the Manifestation of (Cyto)toxicity by Polystyrene Microplastic Model Particles

Zhang

Paul

Brehm

et al. 2023

Environ. Sci. Technol.

View full text Add to dashboard Cite

Polystyrene (PS) is an important model polymer for the investigation of effects of microplastic (MP) and nanoplastic (NP) particles on living systems. Aqueous dispersions of PS MP or NP contain residual monomers of styrene. In consequence, it is not clear if the effects observed in standard (cyto)toxicity studies are evoked by the polymer (MP/NP) particle or by residual monomers. We addressed that question by comparing standard PS model particle dispersions with in-house synthesized PS particle dispersions. We proposed a rapid purification method of PS particle dispersions by dialysis against mixed solvents and developed a simple method of UV–vis spectrometry to detect residual styrene in the dispersions. We found that standard PS model particle dispersions, which contain residual monomers, exerted a low but significant cytotoxicity on mammalian cells, while the in-house synthesized PS, after rigorous purification to reduce the styrene content, did not. However, the PS particles per se but not the residual styrene in both PS particle dispersions resulted in immobilization of Daphnia. Only by using freshly monomer-depleted particles, will it be possible in the future to assess the (cyto)toxicities of PS particles, avoiding an otherwise not controllable bias effect of the monomer.

show abstract

Section: Methodsmentioning

confidence: 86%

Section: Methodsmentioning

confidence: 99%

See 1 more Smart Citation

Role of Residual Monomers in the Manifestation of (Cyto)toxicity by Polystyrene Microplastic Model Particles

Zhang

Paul

Brehm

et al. 2023

Environ. Sci. Technol.

View full text Add to dashboard Cite

show abstract

“…As acrylonitrile is frequently used in the polymer manufacturing industry, a number of gas chromatography and liquid chromatography methods are available in the literature for the determination of residual acrylonitrile in polymer products as well as the liquid and solid waste stream. − Oligonucleotide manufacturing employs strongly basic conditions in the backbone deprotection and the subsequent ammonolysis reaction that can potentially convert acrylonitrile into 3-amino-propionitrile and bis(2-cyanoethyl)amine, which are not genotoxic (Figure B). − Because of the reactivity of acrylonitrile in the sample matrices generated under strongly basic reaction conditions, sample preparation is critical, and the available methods cannot be used directly to determine trace amounts of acrylonitrile in oligonucleotide intermediates.…”

Section: Introductionmentioning

confidence: 99%

Trace-Level Determination of Acrylonitrile Generated in the Manufacturing Process of Oligonucleotides by Static Headspace Gas Chromatography with an Electron Impact(+) Mass Detector

Guo

Stolee

Fillon

et al. 2021

Org. Process Res. Dev.

View full text Add to dashboard Cite

A static headspace capillary gas chromatography (HS-GC) method featured with a short run time, a wide calibration range, and a diluent with strong buffering and stabilizing capability has been developed for the quantitative analysis of trace levels of acrylonitrile, a known genotoxic impurity and potential byproduct of oligonucleotide manufacturing. This GC method was achieved on a commercially available fused silica capillary column, and the total run time including GC oven temperature re-equilibration is 20 min. The method employs a split injection (5:1) and a programmed temperature ramp and was qualified in terms of specificity, accuracy, repeatability/precision, quadratic calibration range, limit of quantitation (0.40 ppm), limit of detection (0.10 ppm), solution stability, and robustness. The method was demonstrated to be quadratic over the range of four orders of magnitude from 0.40 to 4000 ppm with a correlation coefficient greater than 0.99 with average recoveries between 86 and 101%. Method performance was also evaluated using sample matrices of different pH values and compositions, and the method was demonstrated to be suitable as a platform test method for the determination of acrylonitrile in the manufacturing process of oligonucleotides. Finally, the degradation kinetics of acrylonitrile in backbone deprotection (1:1 acetonitrile/triethylamine) and ammonolysis (30% NH3 aqueous) matrices was assessed. Acrylonitrile was demonstrated to degrade quantitatively and quickly in the ammonolysis sample matrix.

show abstract

“…Emulsion Polymerization (EP) process has attained growing industrial interest for the preparation of polymer latexes compared to other polymerization techniques due to the use of water as the reaction medium which facilitate the agitation and mass transfer providing an inherently safe process compared to bulk polymerization or solvent‐based polymerization technique. It is also known to be more environment‐friendly due to the presence of almost negligible volatile organic content (VOC) at the end of the reaction especially for cases that the polymerization was let into completion …”

Section: Introductionmentioning

confidence: 99%

Batch‐to‐Batch Reproducibility Studies of Pilot‐Scale Emulsion Polymerization of Poly(styrene‐co‐butyl acrylate)

Harmain¹,

Chan

2018

Macromolecular Symposia

View full text Add to dashboard Cite

Studies on emulsion polymerization (EP) of poly(styrene‐co‐butyl acrylate) [P(S‐co‐BA)] can be accessed in open literature. However, these studies are mostly focusing on lab‐scale polymerization and subsequently characterization, of which discussion on pilot‐scale or mass‐production‐scale of the polymerization is scant. This paper focuses on the batch‐to‐batch reproducibility of P(S‐co‐BA) with 78.7 mol% of styrene and 21.3 mol% of butyl acrylate via EP in 3 metric‐ton (MT) pilot‐scale reactor. Polymerization efficiency, molecular, and physical characterization of the copolymers are examined using gravimetric analysis. Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance (NMR), gel permeation chromatography (GPC), thermal gravimetry analysis (TGA), differential scanning calorimeter (DSC), viscometer, capillary rheometer, particle size analyzer (including dynamic light scattering and laser diffraction techniques), and scanning electron microscope (SEM). The gravimetric analysis on the monomer conversion reveals that the polymerization in 3‐MT reactor is efficient with 100% conversion. Besides, 1H‐NMR results reveal that the styrene‐to‐butyl acrylate mole ratio of the copolymer is of close approximation of the monomer feed amount while FTIR is a rather convenient quality control (QC) tool for batch‐to‐batch reproducibility on the copolymer molecular structured. The physical characteristic of [P(S‐co‐BA)] for all five batches are considered reproducible.

show abstract

Determination of residual (free) monomer in water based polymer emulsions by head space gas chromatography mass spectrometry

Cited by 4 publications

References 3 publications

Role of Residual Monomers in the Manifestation of (Cyto)toxicity by Polystyrene Microplastic Model Particles

Role of Residual Monomers in the Manifestation of (Cyto)toxicity by Polystyrene Microplastic Model Particles

Trace-Level Determination of Acrylonitrile Generated in the Manufacturing Process of Oligonucleotides by Static Headspace Gas Chromatography with an Electron Impact(+) Mass Detector

Batch‐to‐Batch Reproducibility Studies of Pilot‐Scale Emulsion Polymerization of Poly(styrene‐co‐butyl acrylate)

Contact Info

Product

Resources

About