Determination of trimellitic anhydride(TMA) in factory atmospheres by high performance liquid chromatography

Purnell, C. J.; Warwick, C. J.

doi:10.1002/jhrc.1240030915

Cited by 11 publications

(5 citation statements)

References 4 publications

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“…This approach, which depends on routine TMA air monitoring of workers, has resulted in a significant reduction in TMA-induced occupational illness. 2 The most accurate methods for TMA detection presently involve batch air sampling followed by gas chromatography (GC) with flame ionization detection, 6,7 high performance liquid chromatography (HPLC), 8,9 or complex chemical derivatization schemes. 6,10 Unfortunately, such instrumentation and capability is rarely available on worksites and substantial time typically elapses from the time a sample is collected to the time when the results are reported back so that appropriate interventions could be implemented.…”

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confidence: 99%

“…The most accurate methods for TMA detection presently involve batch air sampling followed by gas chromatography (GC) with flame ionization detection, , high performance liquid chromatography (HPLC), , or complex chemical derivatization schemes. , Unfortunately, such instrumentation and capability is rarely available on worksites and substantial time typically elapses from the time a sample is collected to the time when the results are reported back so that appropriate interventions could be implemented. Furthermore, ambient air analysis is often found to poorly correlate with the actual personal exposure levels of highly exposed workers.…”

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confidence: 99%

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Perfluorosulfonic Acid Membrane Catalysts for Optical Sensing of Anhydrides in the Gas Phase

et al. 2010

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Continuous, on-site monitoring of personal exposure levels to occupational chemical hazards in ambient air is a long-standing analytical challenge. Such monitoring is required to institute appropriate health measures but is often limited by the time delays associated with batch air sampling and the need for off-site instrumental analyses. In this work, we report on the first attempt to use the catalytic properties of perfluorosulfonic acid (PSA) membranes to obtain a rapid, selective, and highly sensitive optical response to trimellitic anhydride (TMA) in the gas phase for portable sensor device application. TMA is used as starting material for various organic products and is recognized to be an extremely toxic agent by the National Institute for Occupational Safety and Health (NIOSH). Resorcinol dye is shown to become immobilized in PSA membranes and diffusionally constrain an orange brown product that results from acid-catalyzed reaction with more rapidly diffusing TMA molecules. FTIR, UV/vis, reaction selectivity to TMA versus trimellitic acid (TMLA), and homogeneous synthesis are used to infer 5,7- dihydroxyanthraquinone-2-carboxylic acid as the acylation product of the reaction. The color response has a sensitivity to at least 3 parts per billion (ppb) TMA exposure and, in addition to TMLA, excludes maleic anhydride (MA) and phthalic anhydride (PA). Solvent extraction at long times is used to determine that the resorcinol extinction coefficient in 1100 EW PSA membrane has a value of 1210 m(2)/g at 271.01 nm versus a value of 2010 m(2)/g at 275.22 nm in 50 vol% ethanol/water solution. The hypsochromic wavelength shift and reduced extinction coefficient suggest that the polar perfluorosulfonic acid groups in the membrane provide the thermodynamic driving force for diffusion and immobilization. At a resorcinol concentration of 0.376 g/L in the membrane, a partition coefficient of nearly unity is obtained between the membrane and solution concentrations and a maximum conversion rate of one ambient TMA molecule for every two membrane-immobilized resorcinol molecules is observed in 15 min.

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Perfluorosulfonic Acid Membrane Catalysts for Optical Sensing of Anhydrides in the Gas Phase

et al. 2010

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“…On the other hand, direct injection of unfunctionalized species gives rise to an overestimation of the anhydride, since the acid loses water at the injection temperature, condensing to the corresponding anhydride. − To bypass this problem, different analytical techniques were taken on account of performing the determination of anhydrides. Purnell and Warwick in 1980 proposed the use of LC for the determination of TMA: also in this case, authors had to hydrolyze TMA to trimellitic acid (TMAc) to be able to perform the analysis. To our knowledge, the only procedure present in the literature achieving simultaneous determination of TMA and TMAc (as impurity) was published in 1982 by Rushing et al: they derivatized the free carboxylic groups present in both molecules, without functionalizing the anhydride moiety, using diazomethane .…”

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confidence: 99%

Simultaneous Determination by Selective Esterification of Trimellitic, Phthalic, and Maleic Anhydrides in the Presence of Respective Acids

et al. 2023

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Trimellitic, phthalic, and maleic anhydrides are important building blocks to produce polymers and additives, such as plasticizers. In humans, the exposure to these compounds can cause several health issues. In European Union and USA, their presence in substances and mixtures is restricted by CLP Regulation (no. 1272/2008) and HCS/HazCom 2012, respectively, but no information about the corresponding acids is reported. For this reason, a selective method to determine anhydrides in mixtures, in the presence of acids, could be interesting. Nowadays, methods in the literature are either not selective or use explosive and toxic reagents (as diazomethane). In this work, an innovative, greener, and safer method for the simultaneous recognition and quantification of anhydrides and acids, via direct injection gas chromatography−mass spectrometry, is developed. The sample pretreatment consists in selective esterification with absolute ethanol on the anhydride, followed by a treatment with boron trifluoride-methanol for the methylation of remaining carboxylic groups. The optimization of the functionalization, a crucial step of the method, was optimized by experimental design. The limit of detection−limit of quantification (LOD−LOQ) values for trimellitic, phthalic, and maleic anhydrides are 0.31− 0.93, 0.47−1.41, and 0.06−0.18 μg/mL, respectively.

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“…[17][18][19][20] Solid sampling on Tenax, XAD-2, glass-fibre filters or PVC-filters have also been described. 9,10,[19][20][21][22][23][24][25][26][27][28][29][30][31][32][33] For analysis, GC 9,10,[19][20][21][22][23][24][25][26][27][28][29] using FID, ECD or MS detection and HPLC-UV 17,18,[29][30][31][32][33] have been used. A method for direct determination of hexahydrophthalic anhydride in air using a Fourier transform infrared spectrometer has also been developed.…”

Section: Introductionmentioning

confidence: 99%

Determination of airborne anhydrides using LC-MS monitoring negative ions of di-n-butylamine derivatives

Dahlin

Karlsson

Skarping

et al. 2004

J. Environ. Monitor.

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An air sampling method for simultaneous determination of organic acid anhydrides and isocyanates is presented. Air samples are collected in impinger flasks filled with 0.01 M di-n-butylamine (DBA) in a mixture of toluene-acetonitrile (7:3, v/v) with a 13 millimetre glass fibre filter in series. The amount of anhydrides and isocyanates are determined as their amide and urea derivatives using LC-MS. Four anhydrides, maleic anhydride (MA), phthalic anhydride (PA), tetrahydrophthalic anhydride (TA) and cis-hexahydrophthalic anhydride (HA) and 11 isocyanates could be separated in 9 minutes using gradient elution. Anhydride-DBA derivatives in standard solutions were quantified using LC with chemiluminescent nitrogen detection (CLND). Anhydride-DBA derivatives were found to be stable for at least two months when stored in acetonitrile or toluene in the freezer. The yield of DBA derivatives of anhydrides in the 0.01 M DBA in toluene-acetonitrile (7:3, v/v) was in the range of 70->95%. Using MS and negative electrospray ionisation (ES-) linear calibrations curves were obtained for the anhydrides with correlation coefficients ranging from 0.9970-0.9997. The instrumental detection limit for the anhydrides ranged from 10-30 fmol, based on a signal to noise root mean square (RMS) ratio of 3. Monitoring positive and negative ions simultaneously, both isocyanates and anhydrides could be determined as their DBA derivatives in the same chromatographic run. When air samples were collected during thermal degradation of different coated metal sheets both anhydrides and isocyanates were present in the same samples and all the studied anhydrides were found.

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Determination of trimellitic anhydride(TMA) in factory atmospheres by high performance liquid chromatography

Cited by 11 publications

References 4 publications

Perfluorosulfonic Acid Membrane Catalysts for Optical Sensing of Anhydrides in the Gas Phase

Perfluorosulfonic Acid Membrane Catalysts for Optical Sensing of Anhydrides in the Gas Phase

Simultaneous Determination by Selective Esterification of Trimellitic, Phthalic, and Maleic Anhydrides in the Presence of Respective Acids

Determination of airborne anhydrides using LC-MS monitoring negative ions of di-n-butylamine derivatives

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