Simple, fast and inexpensive large “whole water” volume sample SPE-loading using compressed air and finely ground sand

2019 ◽  
Vol 11 (7) ◽  
pp. 894-896 ◽  
Author(s):  
Ola Svahn ◽  
Erland Björklund
Keyword(s):  
Solid Phase Extraction ◽  
Solid Phase ◽  
Standard Technique ◽  
Sample Volume ◽  
Compressed Air ◽  
Water Volume ◽  
Phase Extraction ◽  
Environmental Trace Analysis ◽  
Large Sample Volume ◽  
Whole Water

In environmental trace analysis there is often a need to enrich the compounds of interest from a large sample volume, where the use of solid phase extraction (SPE) is more or less the standard technique.

Adsorption of Organic Pollutants in Wastewater using Solid Phase Extraction Absorbent from Agro-Waste

2019 ◽  
Vol 7 (2) ◽  
pp. 245-253 ◽  
Author(s):  
Wan Norfazilah Wan Ismail ◽  
Dzul Iskandar Muhammad Fauzi ◽  
Nurlin Abu Samah
Keyword(s):  
Solid Phase Extraction ◽  
Organic Pollutants ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Sample Volume ◽  
Wastewater Sample ◽  
Phase Extraction ◽  
Nano Powder ◽  
Optimum Parameters ◽  
Limit Of Quantitation

A rapid solid phase extraction (SPE) combined with gas chromatography equipped with mass spectrometry (GC-MS) method was developed and validated for the determination of acenaphthylene, acenaphthene and naphthalene in wastewater sample collected from petroleum industry’s drainage. Important SPE parameters, namely absorbent amount, sample volume, type of elution solvent and its volume were optimized. The optimum parameters obtained are: 200 mg silica nano-powder, 2.0 mL sample volume and 2.0 mL n-hexane as elution solvent. The method showed good linearity in the range of 0.1-10.0 mg/L with satisfactory limit of detection (≤1.0 mg/L) and limit of quantitation (≤3.2 mg/L) under the optimized conditions. Good relative recoveries (94.7-99.9%) and intra- and inter-day precisions (≤2.8%, n=3) for acenaphthene, acenaphthylene and naphthalene were obtained. Toxicity study has revealed that it is a non-toxic absorbent and safe to be used for the removal of organic pollutants in water which is advantageous for routine wastewater analysis.

scholarly journals Atrazine and 2, 4-D determination in corn samples using microwave assisted extraction and on-line solid-phase extraction coupled to liquid chromatography.

2018 ◽  
Vol 62 (2) ◽  
Author(s):  
Ana Susana Santos-Hernández ◽  
Laura Hinojosa-Reyes ◽  
Isabel del Carmen Sáenz-Tavera ◽  
Aracely Hernández-Ramírez ◽  
Jorge Luis Guzmán-Mar
Keyword(s):  
Solid Phase Extraction ◽  
Solid Phase ◽  
Monolithic Column ◽  
Correlation Coefficients ◽  
Sample Pretreatment ◽  
Enrichment Factors ◽  
Sample Volume ◽  
Phase Extraction ◽  
Microwave Assisted ◽  
On Line

<p>On-line sample pretreatment (clean-up and analyte preconcentration) was coupled to sequential injection chromatography for the determination of 2, 4-D (2,4-dichlorophenoxyacetic acid) and atrazine in corn samples. Prior to their analysis, microwave-assisted approach was evaluated and optimized for the extraction of 2,4-D and atrazine in corn samples. Extraction was carried out using MeOH:water (30:70 v/v) solvent at 50°C for 15 min. The on-line SPE-HPLC/UV approach combined reversed solid-phase extraction using strata X sorbent with MeOH:H<sub>2</sub>O (80:20 v/v) at 1 mL min<sup>-1</sup> as eluent for the enrichment of the analytes. C18 monolithic column with acetonitrile:10 mM acetate buffer pH 4 (20:80, v/v) was employed as mobile phase at 2 mL min<sup>-1</sup> flow rate for separation of the compounds before UV detection. Enrichment factors up to 13.4 were achieved with a 10 mL sample volume. The developed procedure showed linear response ranges from 0.07–0.70 mg kg<sup>−1 </sup>for 2,4-D and atrazine with correlation coefficients &gt;0.993. The LODs were 0.03 and 0.02 mg kg<sup>-1 </sup>for 2,4-D and atrazine, respectively with RSD ranged from 4.0 to 7.2 % at 0.07 and 0.30 mg kg<sup>-1</sup>. The recoveries of 2,4-D and atrazine in corn samples were from 82.6 and 98.2%. The proposed method showed good recoveries and reasonable precision for herbicide analysis in corn samples avoiding the time-consuming batch sample pretreatment step, thus minimizing risks of sample contamination and analyte losses.</p>

scholarly journals Simple and Fast Methods Based on Solid-Phase Extraction Coupled to Liquid Chromatography with UV Detection for the Monitoring of Caffeine in Natural, and Wastewater as Marker of Anthropogenic Impact

2012 ◽  
Vol 2012 ◽  
pp. 1-7 ◽  
Author(s):  
Sònia Moret ◽  
Manuela Hidalgo ◽  
Juan M. Sanchez
Keyword(s):  
Detection Limit ◽  
Solid Phase Extraction ◽  
Natural Waters ◽  
Wastewater Treatment Plants ◽  
Solid Phase ◽  
Sample Volume ◽  
Uv Detection ◽  
Phase Extraction ◽  
Method Detection Limit ◽  
Spe Method

Two concentration methods for fast and routine determination of caffeine (using HPLC-UV detection) in surface, and wastewater are evaluated. Both methods are based on solid-phase extraction (SPE) concentration with octadecyl silica sorbents. A common “offline” SPE procedure shows that quantitative recovery of caffeine is obtained with 2 mL of an elution mixture solvent methanol-water containing at least 60% methanol. The method detection limit is 0.1 μg L−1 when percolating 1 L samples through the cartridge. The development of an “online” SPE method based on a mini-SPE column, containing 100 mg of the same sorbent, directly connected to the HPLC system allows the method detection limit to be decreased to 10 ng L−1 with a sample volume of 100 mL. The “offline” SPE method is applied to the analysis of caffeine in wastewater samples, whereas the “on-line” method is used for analysis in natural waters from streams receiving significant water intakes from local wastewater treatment plants.

scholarly journals Dispersive Micro Solid-Phase Extraction Using Multiwalled Carbon Nanotubes for Simultaneous Determination of Trace Metal Ions by Energy-Dispersive X-ray Fluorescence Spectrometry

2013 ◽  
Vol 67 (2) ◽  
pp. 204-209 ◽  
Author(s):  
Robert Skorek ◽  
Beata Zawisza ◽  
Eva Marguí ◽  
Ignasi Queralt ◽  
Rafal Sitko
Keyword(s):  
Carbon Nanotubes ◽  
Solid Phase Extraction ◽  
Trace Metal ◽  
Solid Phase ◽  
Sample Volume ◽  
Phase Extraction ◽  
Multiwalled Carbon ◽  
X Ray ◽  
Trace Metal Ions

A methodology based on dispersive micro solid-phase extraction (DMSPE) using multiwalled carbon nanotubes (MWCNTs) as solid sorbent prior to measurement with energy-dispersive X-ray fluorescence (EDXRF) spectrometry is proposed. The procedure consists of chelating of nickel, cobalt, copper, and lead ions with ammonium pyrrolidinedi-thiocarbamate (APDC) and posterior adsorption of metal chelates on MWCNTs (1 mg) dispersed in the aqueous samples (100 mL). DMSPE promotes immediate interaction between the metal chelates and MWCNTs and shortens time of sample preparation in comparison with classical solid-phase extraction. After microextraction process, MWCNTs are collected onto filter and directly measured by EDXRF. With this technique, the direct quantification of metal species held in solid materials is possible and, therefore, the elution step can be avoided. The effects of various experimental parameters such as pH of the solution, amounts of MWCNTs and APDC, sample volume, and time of stirring were investigated. With the best analytical conditions (1 mg of MWCNTs, 2 mg of APDC, 100 mL sample volume, pH = 7, and 5 min time of stirring), Co(II), Ni(II), Cu(II), and Pb(II) can be simultaneously determined with very good recoveries (101%, 98%, 96%, 99%, respectively) and detection limits (0.43, 0.11, 0.46, 0.15 ng mL−1, respectively). The method was applied in determination of trace metal ions in tap water and wastewater samples.

Comparison of Solid Phase Extraction Techniques for Herbicides

Weed Science ◽  
1996 ◽  
Vol 44 (3) ◽  
pp. 689-693 ◽  
Author(s):  
Melissa B. Riley ◽  
Renee J. Keese
Keyword(s):  
Organic Solvent ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Fold Increase ◽  
Extraction Methods ◽  
Plant Production ◽  
Water Volume ◽  
Phase Extraction ◽  
Liquid Liquid Extraction ◽  
Selection Of

Solid phase extraction (SPE) procedures were used to determine the recoveries of herbicides typically used in containerized ornamental plant production from water samples. Recoveries from C18cartridges and disks were compared for each of 12 herbicides with variations in elution solvent and volume of elution solvent tested. Recoveries for nine of the herbicides from the cartridges and disks using acetone as an elution solvent were not affected by SPE matrix. Fluazifop recovery was greater with the disks, while napropamide and oxadiazon recoveries were greater with cartridges. Both cartridges and disks yielded low recoveries (23 to 47%) of benefin and prodiamine. Changing the elution solvent from acetone to acetonitrile resulted in 10% improvement for the recovery of benefin and a three- to four-fold increase in recovery of prodiamine. Acetonitrile decreased recoveries of napropamide, oryzalin, oxadiazon, oxyfluorfen, and pendimethalin from cartridges. For the disks, oxyfluorfen, prodiamine, and trifluralin had increased recovery, while fluazifop, oxadiazon, and simazine had decreased recovery with acetonitrile as the elution solvent. Increasing the amount of acetone eluting solvent increased the recovery of prodiamine and oxyfluorfen while decreasing the recovery of fluazifop, pendimethalin, simazine, and trifluralin. Binding capacities of oryzalin on cartridges and disks averaged 13.2 and 7.8 mg, respectively. The advantage of the disk lies in the greater volume of water that can be processed, while the higher cost and greater variability are disadvantages. Cartridge extraction yielded good recoveries with lower standard deviations, and used less organic solvent. Selection of an SPE extraction method depends upon the herbicides under evaluation, expected levels, and the water volume being processed. Both SPE techniques offer advantages over traditional liquid-liquid extraction methods such as reduced requirements for organic solvent and sample preparation.

Trace Determination of Rhodamine and Eosine in Oil-Water Reservoir Using Solid-Phase Extraction

2014 ◽  
Vol 880 ◽  
pp. 276-281 ◽  
Author(s):  
Mikhail A. Gavrilenko ◽  
Nataliya A. Gavrilenko ◽  
Shamshiya K. Amerkhanova ◽  
Aitolkyn S. Uali ◽  
Alisher A. Bilyalov
Keyword(s):  
Solid Phase Extraction ◽  
Solid Phase ◽  
Water Reservoir ◽  
Sample Volume ◽  
Batch Adsorption ◽  
Phase Extraction ◽  
Colorimetric Measurements ◽  
Oil Water ◽  
Polymethacrylate Matrix

A method for the trace analysis of rhodamine and eosine with colorimetric measurements based on solid-phase extraction (SPE) by transparent polymethacrylate matrix (PMM) is described. Solid-phase extraction on PMM allowed a 380-fold enrichment of the dyes if 10 mL sample volume is used with extraction efficiencies 98%. The method enables the determination of rhodamine to 0.06 mg/L and eosine to 1.2 mg/L combined with a fast and easy sample-preparation (pH-adjusting prior to SPE). Simultaneous extraction and determination of rhodamine and eosine in reservoir samples with high salinity confirmed the applicability and reproducibility of the method. Batch adsorption results indicated that Langmuir isotherm described the adsorption isotherms better.

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