Solid-phase Microextraction Method Research Articles

Evaluation of Malolactic Starters in White and Rosé Winemaking of Moschofilero Wines

The aim of the present study was to induce malolactic fermentation (MLF) after alcoholic fermentation (AF) of must of the Moschofilero cultivar, the only ‘gris’ native grape variety that is cultivated in Greece. For this purpose, Oenococcus oeni strains Viniflora® CH16, Viniflora® Oenos and Viniflora® CiNe were inoculated after the completion of AF driven by the Saccharomyces cerevisiae strain UCLM S325. Growth of the aforementioned starter cultures was assessed during fermentation by classical microbiological techniques, and verification of their dominance was performed by (GTG)5 fingerprinting. Assessment of standard enological parameters and colorimetric analysis were performed by established approaches. Identification and quantification of organic acids, ethanol and glycerol was performed by high performance liquid chromatography (HPLC), while the solid-phase microextraction method (SPME), coupled with gas chromatography/mass spectrometry (GC/MS), was employed for the identification and quantification of volatile compounds. Finally, sensory analysis took place according to ISO 13299:2016. The suitability of the starter cultures employed to drive AF and MLF was exhibited; AF and MLF of the white and rosé wines were completed after 15 days. Upon completion of AF, substantial differences were observed in the chemical characteristics of the white and rosé wines, which were also reflected in the balance descriptor. MLF also resulted in significant changes. In all cases total acidity decreased and volatile acidity and pH value increased, while the vanilla and butter descriptors increased. Interestingly, the color intensity of the rosé wines also increased. A series of strain-dependent changes in the chemical composition and sensory analysis of both white and rosé wines was also observed.

Volatile Organic Compounds of Streptomyces sp. TOR3209 Stimulated Tobacco Growth by Up-Regulating the Expression of Genes Related to Plant Growth and Development.

To investigate the mechanism underlying the plant growth-promoting (PGP) effects of strain Streptomyces sp. TOR3209, PGP traits responsible for indoleacetic acid production, siderophore production, and phosphate solubilization were tested by culturing the strain TOR3209 in the corresponding media. The effects of volatile organic compounds (VOCs) produced by the strain TOR3209 on plant growth were observed by co-culturing this strain with tobacco seedlings in I-plates. Meanwhile, the effects of VOCs on tobacco gene expression were estimated by performing a transcriptome analysis, and VOCs were identified by the solid-phase micro-extraction (SPME) method. The results showed positive reactions for the three tested PGP traits in the culture of strain TOR3209, while the tobacco seedlings co-cultured with strain TOR3209 revealed an increase in the fresh weight by up to 100% when compared to that of the control plants, demonstrating that the production VOCs was also a PGP trait. In transcriptome analysis, plants co-cultured with strain TOR3209 presented the highest up-regulated expression of the genes involved in plant growth and development processes, implying that the bacterial VOCs played a role as a regulator of plant gene expression. Among the VOCs produced by the strain TOR3209, two antifungal molecules, 2,4-bis(1,1-dimethylethyl)-phenol and hexanedioic acid dibutyl ester, were found as the main compounds. Conclusively, up-regulation in the expression of growth- and development-related genes via VOCs production is an important PGP mechanism in strain TOR3209. Further efforts to explore the effective VOCs and investigate the effects of the two main VOCs in the future are recommended.

Looking beyond the Active Substance: Comprehensive Dissipation Study of Myclobutanil-Based Plant Protection Products in Tomatoes and Grapes Using Chromatographic Techniques Coupled to High-Resolution Mass Spectrometry.

A comprehensive evaluation of the dissipation of a myclobutanil plant protection product was performed in tomato and grape samples. Different temperature conditions (3 and 22 °C) were evaluated. A biphasic kinetic model provided a suitable adjustment (R2 > 0.95), with persistence (residual level, RL50) lower than 24 days in all cases. Solid-liquid extraction and ultra-high-performance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC-Q-Orbitrap-HRMS) were used for metabolites' elucidation, identifying six myclobutanil metabolites, four out of them described for the first time and one of them confirmed using 1H, 13C, (1H-1H)-COSY, (1H-13C)-HMQC, and (1H-13C)-HMBC nuclear magnetic resonance (NMR). Their degradation curves were also evaluated, increasing their concentrations when the myclobutanil concentration decreases. Additionally, coformulants present in the commercial formulation were monitored employing headspace solid-phase microextraction method (HS-SPME)-gas chromatography coupled to HRMS (GC-Q-Orbitrap-HRMS). Seven coformulants were quantified in tomato samples. Their dissipation curves were studied, and it was observed that they were almost degraded 12 days after application.

대체당 알룰로스를 이용한 고추장 양념장의 주요 방향 화합물 특성

Purpose: This study aimed to investigate the flavor characteristics of the Gochujang condiment and its flavor compounds when it was heated with the addition of allulose. Methods: The Gochujang condiment samples were prepared with the addition of 0%, 25%, 50%, 75%, 100% allulose, and sugar for sweetness and heated for 30 minutes. The solid-phase micro-extraction (SPME) method was used to capture the flavor aroma, gas chromatography-mass spectrometry (GC-MS), and gas chromatography-olfactometry (GC-O) were used for the analysis. Results: The volatile flavor components were analyzed to evaluate the flavor characteristics of the processed Gochujang condiment. A total of 43 volatile flavor components were identified with the heat treatment, among which diallyl trisulfide showed the highest peak, and diallyl disulfide, methyl-2-propenyl trisulfide, β-phellandrene, and β-caryophyllene also had high peaks. These five high-peak ingredients play an important role in determining the taste of the Gochujang condiment. It was confirmed that the volatile component was diallyl trisulfide, which increased as the allulose content increased. A total of 16 flavoring active ingredients of the condiment were identified. Also, most sulfur compounds and terpene were identified. Allyl methyl disulfide, dimethyl trisulfide, diallyl disulfide, β-phellandrene, and methyl 2-propenyl trisulfide played an important role in the flavoring of the Gochujang condiment. Conclusion: The main volatile components of the flavor compounds generated by the heat treatment included diallyl trisulfide, diallyl disulfide, methyl-2-propenyl trisulfide, β-phellandrene, and β-caryophyllene with high peak areas. The quantum of diallyl trisulfide increased as the allulose content increased. Allyl methyl disulfide, dimethyl trisulfide, diallyl disulfide, β-phellandrene, and methyl 2-propenyl trisulfide were identified as flavoring active compounds, and each of these contributed to the flavor of the Gochujang condiment.

Packed in‐tube SPME–LC–MS/MS for fast and straightforward analysis of cannabinoids and metabolites in human urine

Cannabinoids are pharmacologically active compounds present in cannabis plants, which have become important research topics in the modern toxicological and medical research fields. Not only is cannabis the most used drug globally, but also cannabinoids have a growing use to treat a series of diseases. Therefore, new, fast, and efficient analytical methods for analyzing these substances in different matrices are demanded. This study developed a new packed-in-tube solid-phase microextraction (IT-SPME) method coupled to liquid chromatography with tandem mass spectrometry (LC-MS/MS), for the automated microextraction of seven cannabinoids from human urine. Packed IT-SPME microcolumns were prepared in (508µm i.d.×50mm) stainless-steel hardware; each one required only 12mg of sorbent phase. Different sorbents were evaluated; fractional factorial design 24-1 and a central composite design were employed for microextraction optimization. Under optimized conditions, the developed method was a fast and straightforward approach. Only 250µl of urine sample was needed, and no hydrolysis was required. The sample pretreatment included only dilution and centrifugation steps (8min), whereas the complete IT-SPME-LC-MS/MS method took another 12 min, with a sample throughput of 3 samplesh-1 . The developed method presented adequate precision, accuracy and linearity; R2 values ranged from 0.990 to 0.997, in the range of 10-1000ngml-1 . The lower limits of quantification varied from 10 to 25ngml-1 . Finally, the method was successfully applied to analyze 20 actual urine samples, and the IT-SPME microcolumn was reused over 150 times.

Deep Eutectic Solvent-Based Coating Sorbent for Preconcentration of Formaldehyde by Thin-Film Solid-Phase Microextraction Technique

A thin-film solid-phase microextraction method with a sorbent composed of a deep eutectic solvent was developed for the preconcentration of formaldehyde from river and lake water samples. Four new deep eutectic solvents (DESs) were synthesized, each in molar ratios 1:1, 1:2, and 1:3. Among prepared compounds, the greatest efficiency in the proposed method of preconcentration of formaldehyde derivatized with Nash reagent was demonstrated by DES-3 consisting of benzyldimethylhexadecylammonium chloride and lauric acid, in a molar ratio of 1:3. For the proposed method, the parameters affecting the extraction efficiency of formaldehyde were optimized (including the choice of DES-based sorbent and desorption solvent as well as the sample volume and pH, the salting-out effect, the extraction time, and the desorption time). Under optimal conditions, the proposed method achieved good precision between 3.3% (for single sorbent) and 4.8% (for sorbent-to-sorbent) as well as good recovery ranging from 78.0 to 99.1%. The limits of detection and quantitation were 0.15 ng mL−1 and 0.50 ng mL−1, respectively. The enrichment factor was equal to 178. The developed method was successfully applied to determine formaldehyde in environmental water samples.

Determination of benzimidazoles in beef by molecularly imprinted boron nitride composite based dispersive solid phase microextraction and ultra performance liquid chromatography

The main objective of this study was to synthesize the molecularly imprinted boron nitride material and develop a high efficient method for extraction of the residue of veterinary drug in food sample. During the experiments, the molecularly imprinted microspheres with 2-aminobenzimidazole as the template were polymerize on boron nitride to synthesize a type of new composite. Then it was used as absorbent to develop a dispersive solid phase microextraction method for purification of benzimidazole drugs in beef followed by determination with ultra performance liquid chromatography. This composite could simultaneously recognize 7 benzimidazoles with high absorption capacity (36.23–38.88 μg/mg) and high recovery (92.3%-97.1%), and could be reused for 5 times. This sample extraction method achieved high enrichment factors (21.5–37.9), so the limits of detection for determination of the 7 drugs in beef were in the range of 0.2–0.5 ng/g. This is the first study reporting the use of boron nitride based material for the extraction of residual veterinary drug in food sample.

Determination of ultra-trace gold in cosmetics using aluminum-magnesium layered double hydroxide/graphene oxide nanocomposite

A new solid-phase microextraction method for preconcentration and determination of ultra-trace Au(III) and AuNPs was developed. For this purpose, a nanosized aluminum-magnesium layered double hydroxide (AlMg-LDH)/graphene oxide (GO) nanocomposite was synthesized. X-ray diffraction, Raman spectroscopy, and scanning electron microscopy confirmed the successful synthesis of the nanocomposite AlMg-LDH/GO with a well-crystallized hexagonal structure. The synthesized nanomaterial allows sorption with 100% recovery of AuNPs at pH 1–5 or AuNPs and Au(III) ions at pH 1–2. Therefore, gold ions and corresponding gold nanoparticles can be together or separately determined. The maximum sorption capacity of the nanocomposite is 12 mg g−1 for Au(III). After adsorption, gold was directly determined on the AlMg-LDH/GO by energy-dispersive X-ray fluorescence spectrometry with a detection limit of 0.06 ng mL−1, precision ca. 4%, and recovery >90%. According to the Green Chemistry rule, the method has significant advantages, such as reducing the amount of sorbent required and eliminating solvent. The elution of analytes from the nanosorbent is completely eliminated in the developed method. The developed method was successfully used to extract and determine ultra-trace gold in cosmetics products.

Elucidation of Analytical-Compositional Fingerprinting of Three Different Species of Chili Pepper by Using Headspace Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry Analysis, and Sensory Profile Evaluation.

The aim of the present study was to determine the volatile compounds of three different species of chili peppers, using solid-phase microextraction (SPME) methods in combination with gas chromatography–mass spectrometry (GC-MS). The detection of marker aroma compounds could be used as a parameter to differentiate between species of chili peppers for their detection and traceability in chili pepper food. The sensorial contribution was also investigated to identify the predominant notes in each species and to evaluate how they can influence the overall aroma. Three different pepper species belonging to the Capsicum genus were analyzed: Chinense, Annuum, and Baccatum. A total of 269 volatile compounds were identified in these species of chili peppers. The Capsicum annum species were characterized by a high number of acids and ketones, while the Capsicum chinense and Capsicum baccatum were characterized by esters and aldehydes, respectively. The volatile profile of extra virgin olive oils (EVOOs) flavored with chili peppers was also investigated, and principal component analysis (PCA) and hierarchical cluster analysis (HCA) of the volatile profiles were demonstrated to be a powerful analytical strategy for building a model that highlights the potential of a volatile characterization approach for use in evaluating food traceability and authenticity.

Evaluation of fresh, frozen, and lyophilized fecal samples by SPME and derivatization methods using GC×GC-TOFMS.

Feces is a highly complex matrix containing thousands of metabolites. It also contains live bacteria and enzymes, and does not have a static chemistry. Consequently, proper control of pre-analytical parameters is critical to minimize unwanted variations in the samples. However, no consensus currently exists on how fecal samples should be stored/processed prior to analysis. The effects of sample handling conditions on fecal metabolite profiles and abundances were examined using comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC×GC-TOFMS). Solid-phase microextraction (SPME) and derivatization via trimethylsilylation (TMS) were employed as complementary techniques to evaluate fresh, frozen, and lyophilized fecal samples with expanded coverage of the fecal metabolome. The total number of detected peaks and the signal intensities were compared among the different handling conditions. Our analysis revealed that the metabolic profiles of fecal samples depend greatly on sample handling and processing conditions, which had a more pronounced effect on results obtained by SPME than by TMS derivatization. Overall, lyophilization resulted in a greater amount of total and class-specific metabolites, which may be attributed to cell lysis and/or membrane disintegration. A comprehensive comparison of the sample handling conditions provides a deeper understanding of the physicochemical changes that occur within the samples during freezing and lyophilization. Based on our results, snap-freezing at -80°C would be preferred over lyophilization for handling samples in the field of fecal metabolomics as this imparts the least change from the fresh condition.

Preparation of bamboo‐derived magnetic biochar for solid‐phase microextraction of fentanyls from urine

In this study, a biochar-based magnetic solid-phase microextraction method, coupled with liquid chromatography-mass spectrometry, was developed for analyzing fentanyl analogs from urine sample. Magnetic biochar was fabricated through a one-step pyrolysis carbonization and magnetization process, followed by an alkali treatment. In order to achieve desired extraction efficiency, feed stocks (wood and bamboo) and different pyrolysis temperatures (300-700°C) were optimized. The magnetic bamboo biochar pyrolyzed at 400°C was found to have the greatest potential for extraction of fentanyls, with enrichment factors ranging from 58.9 to 93.7, presumably due to H-bonding and π-π interactions between biochar and fentanyls. Various extraction parameters, such as type and volume of desorption solvent, pH, and extraction time, were optimized, respectively, to achieve the highest extraction efficiency for the target fentanyls. Under optimized conditions, the developed method was found to have detection limits of 3.0-9.4ng/L, a linear range of 0.05-10 μg/L, good precisions (1.9-9.4% for intrabatch, 2.9-9.9% for interbatch), and satisfactory recoveries (82.0-111.3%). The developed method by using magnetic bamboo biochar as adsorbent exhibited to be an efficient and promising pretreatment procedure and could potentially be applied for drug analysis in biological samples.

Rapidly covalent immobilization of β-ketoenamine-linked covalent organic framework on fibers for efficient solid-phase microextraction of phthalic acid esters

Rapid and convenient preparation of covalent organic framework (COF) coated fibers is of great significance to solid-phase microextraction (SPME) technology. In this work, a novel chemical preparation strategy was established for rapid fabrication of β-ketoenamine-linked COF coatings, in which clay-like starting materials of COFs were first wrapped on the fiber surface through self-viscosity and further fixed on the fiber in an oven via chemical bonding. Based on this strategy, four different COF (TpTph, TpPa-1, TpBD and TpTpb) coated fibers was fabricated within 1 h, which is very rapid compared to the recently reported research. Moreover, the strategy also demonstrates the good general applicability for COF fiber preparation. Subsequently, the TpTph coated fiber was used to develop a new SPME method for gas chromatography-tandem mass spectrometry (GC-MS/MS) of trace phthalic acid esters (PAEs) in environmental water. The developed analytical method compared to the previous SPME methods for PAEs based on other sorbents possesses low limits of detection (LODs, 0.02–0.08 ng L−1), and better or comparable precision (RSD ≤9.4%, n = 6), and relatively short extraction time. Furthermore, the trace PAEs (0.27–11.62 ng L−1) in the real water samples were successfully detected with recoveries of 82.2–117.5%. The above results indicates that the proposed fiber preparation strategy is reliable and opens a potential avenue for rapid and facile fabrication of COF coated fibers.

Superficially capped amino metal-organic framework for efficient solid-phase microextraction of perfluorinated alkyl substances

Perfluorinated alkyl substances (PFASs) were ubiquitously in the surface and groundwater. It is crucial and urgent to develop a rapid and ultrasensitive analysis method for the quantification of trace-level PFASs. Herein, a highly hydrophobic sorbent by capping phenylsilane groups on the surfaces of NH2-UiO-66(Zr) nanocrystals was used for efficient solid-phase microextraction (SPME) of PFASs in water samples. It was found that the superficially capped nanocrystals (NH2-UiO-66(Zr)-hp) exhibited both faster extraction kinetics and higher enrichment capacity than the non-capped nanocrystals. The extraction of eleven kinds of PFASs by NH2-UiO-66(Zr)-hp fiber reached equilibrium in 20 min. The enrichment factors of the NH2-UiO-66(Zr)-hp fiber ranged from 6.5 to 48, with a preference for long-chain PFASs over short-chain PFASs. It was proposed that superficial capping eliminated competitive moisture adsorption on the surfaces of the non-capped nanocrystals, thus facilitating the adsorption of PFASs through hydrophobic interaction. By using this new sorbent, the limits of detection of the SPME method as low as 0.035 to 0.616 ng·L−1 were achieved for the target PFASs. The recoveries of PFASs in the environmental water samples were 80.9%-120%. This study presents a new strategy for developing an efficient sorbent for PFASs by surface hydrophobic modification.

Efficient entrapment of inorganic Se species in water and beer samples with functional groups-rich monolith-based adsorbent.

An efficient multiple fibers solid-phase microextraction method based on porous monolith was established for Se(IV) and Se(VI) analysis. Poly(4-vinylphenylboronic acid/styrene-co-ethylene dimethacrylate/divinylbenzene) monolith was fabricated and employed as the extraction phase for efficient entrapment of Se(IV) complexed with o-phenylenediamine, followed by elution with a methanol/formic acid (99/1.0, v/v) mixture and quantification by high-performance liquid chromatography with diode array detector. The Se(VI) species was measured by the difference between total inorganic Se and Se(IV) after pre-reduction. Different characterization techniques were employed to inspect the structure and morphology of prepared adsorbent. A series of key extraction factors were optimized so as to achieve the expected extraction performance. Under the optimized separation and capture parameters, the linear range and limit of detection for Se(IV) in water sample were 0.050-200 and 0.013 μg/L, respectively. For beer sample, the corresponding values were 0.010-300 and 0.032 μg/L. The developed microextraction approach was successfully utilized to detect trace Se(IV) and Se(VI) in environmental water and beer samples with satisfactory fortified recovery and repeatability. Results well reveal the attractive merits of the established method in the analysis of Se species, including simple preparation of adsorbent, convenient extraction procedure, good sensitivity, high cost-effectiveness, and eco-friendliness.

Headspace solid-phase microextraction method for extracting volatile constituents from the different parts of Saudi Anethum graveolens L. and their antimicrobial activity

Anethum graveolens L. is a famous aromatic herb that is widely used as a spice and has been applied in folk medicine to cure many diseases. The current work was carried out to compare the chemical composition and antimicrobial potency of essential oils obtained from the different parts of Saudi Arabia. graveolens. The oil constituents were extracted by headspace solid-phase microextraction and were quantified and qualitatively identified using GC/MS. As a result, essential oil isolated from A. graveolens seeds exhibited the highest antimicrobial activity compared to oils isolated from other parts, followed by flowers, leaves and stems. All tested A. graveolens essential oil samples exhibited stronger antifungal activities against Aspergillus parasiticus when compared to itraconazole. To the best of our knowledge, the current work is the first report comparing different parts of Saudi A. graveolens plant with respect to their essential oil chemical composition and antimicrobial potentials. The essential oil of A. graveolens seeds have the highest contents of carvone and limonene and show superior antimicrobial activities compared to other parts of the plant.

A polydimethylsiloxane/deep eutectic solvent sol-gel thin film sorbent and its application to solid-phase microextraction of parabens

A novel, efficient and reproducible thin-film solid-phase microextraction method using the polydimethylsiloxane/deep eutectic solvent sol-gel as coating material was developed for preconcentration of parabens from environmental samples.New sorbent materials consisting of polydimethylsiloxane with nine new synthesized deep eutectic solvents were prepared by the sol-gel method, and these materials were used to prepare thin film coatings on a mesh support. Among obtained compounds, the highest efficiency in the extraction of parabens was demonstrated by a sorbent consisting of trihexyltetradecylphosphonium chloride and n-docosanol in a molar ratio 1:2 mixed with polydimethylsiloxane.For the proposed method, the parameters affecting the extraction efficiency of parabens were optimized, including the coating material type based on polydimethylsiloxane/deep eutectic solvent, the sample volume, the salting-out effect, the pH of the sample, the extraction time, the desorption solvent and time. The limits of detection and quantitation were from 0.023 to 0.062 ng mL−1 and 0.076–0.201 ng mL−1, respectively, and the enrichment factors ranged from 174 to 186. Under optimal conditions, the proposed method based on measurements for river and lake water achieved good precision between 2.7 and 5.9% and recovery ranging from 79.1 to 88.1%. The developed method was successfully applied to determine trace levels of parabens in the samples of surface waters collected from rivers and lakes.

Development of novel thin-film solid-phase microextraction materials based on deep eutectic solvents for preconcentration of trace amounts of parabens in surface waters.

A green and sensitive thin-film solid-phase microextraction method based on deep eutectic solvent was developed that enables simultaneous isolation, preconcentration, and determination of parabens in surface waters. Six new deep eutectic solvents were synthesized and used directly to prepare thin-film coatings on a stainless steel mesh support. Among the compounds obtained, the highest efficiency in the extraction of parabens was found for a material consisting of trihexyltetradecylphosphonium chloride and n-docosanol in a molar ratio of 1:2. For the proposed method, parameters affecting the extraction efficiency of parabens, such as the coating material, the desorption solvent, the volume of the sample, the pH of the sample, the extraction and desorption time, and the salting-out effect, were optimized. Under optimal conditions, the proposed method allowed us to achieve good precision between 3.6 and 6.5% and recovery ranging from 68.1 to 91.4%. The limits of detection range from 0.018 to 0.055ng/mL.

Determination of gold at trace levels in gold plating wastewater samples by vortex-assisted amidosulfonic acid-coated magnetic nanoparticle-based solid-phase microextraction method prior to slotted quartz tube flame atomic absorption spectrometric measurements

Determination of gold at trace levels in gold plating wastewater samples by vortex-assisted amidosulfonic acid-coated magnetic nanoparticle-based solid-phase microextraction method prior to slotted quartz tube flame atomic absorption spectrometric measurements

In-syringe dispersive micro-solid phase extraction method for the HPLC-fluorescence determination of aflatoxins in milk

The simultaneous determination of aflatoxins (B 1 , B 2 , M 1 and M 2 ) in milk using a new sample pretreatment technique, the in-syringe dispersive micro-solid phase extraction (ISDμSPE), coupled with high performance liquid chromatography with fluorescence detection is described. The separation of the aflatoxins were performed using C18 Hypersil gold (250 mm × 4.6 mm, 5 μm) column at 40 °C under gradient elution for 35 min. The excitation and emission wavelengths of the fluorescence detector were at 360 nm and 440 nm, respectively. On-line photo-chemical derivatization was used to enhance the detection of aflatoxin B 1. Several parameters such as type and amount of sorbent, vortex speed, vortex time and elution solvent were evaluated. Limits of detection (LOD) ranged from 0.003 to 0.005 ng mL −1 , limits of quantification (LOQ) ranged from 0.01 to 0.02 ng mL −1 , recoveries ranged from 73.0 to 109.6%, and relative standard deviations (RSDs) was less than 17.3%. The proposed method was succesfully applied to the analysis of aflatoxins in milk. • An alternative microextraction procedure for the simultaneous determination of aflatoxin M 1 , M 2 , B 1 and B 2 in milk. • Samples and sorbent are dispersed in the syringe allowing higher surface area for interaction. • Acetone was used to replace hazardous chlorinated solvents.

Empirical correlations for diffusivity and the partition coefficient for phthalates in PVC materials and modelling emissions of automotive sealants

Polyvinylchloride (PVC) based sealants commonly contain phthalate plasticizers that are emitted into the air over time. The low volatility classifies them as Semi-Volatile Organic Compounds (SVOCs). Empirical relationships are determined for estimation of the diffusion and solid/air partition coefficients for phthalates in PVC materials using data compiled from studies of phthalates in other PVC materials, such as vinyl flooring. The relationships are functions of vapor pressure of the compounds, which are determined from a Clausius-Clapeyron equation. A test chamber was constructed to continuously sample the air and measure the air concentration based on a Solid Phase MicroExtraction (SPME) method. The partition coefficient was tested with dioctyl terephthalate (DOTP) in a PVC-based sealant, in which the results fell within the reasonable error of the value predicted from the empirical relationship. The model is applied to outdoor and manufacturing scenarios to evaluate the effect of temperature and mass transfer coefficient.