Determination of Methyl- and Dimethylamine in Waste Water by HPLC

Lehotay, J.; Rattay, V.; Brandšteterová, Eva; Oktavec, D.

doi:10.1080/10826079208017171

Cited by 12 publications

(3 citation statements)

References 8 publications

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“…Phenyl isothiocyanate has been utilized for the determination of dimethylamine in waste waters but the method was reported to show poor linearity and a poor limit of detection. 29 In this work, phenyl isothiocyanate was used for the determination of ammonia and a number of aliphatic amines in environmental waters, involving their conversion into phenylthioureas and HPLC. Phenyl isothiocyanate is stable for long periods in aqueous medium over a wide range of pH and temperature and the resulting phenylthioureas have adequate retention on C 18 sorbent and strong UV absorption, making this reagent suitable for the determination of amines in water.…”

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confidence: 99%

Determination of ammonia and aliphatic amines in environmental aqueous samples utilizing pre-column derivatization to their phenylthioureas and high performance liquid chromatography

Sahasrabuddhey¹,

Jain²,

Verma³

1999

Analyst

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Pre-column conversion of ammonia and a number of aliphatic amines into phenylthiourea or its derivatives by reaction with phenyl isothiocyanate, followed by HPLC, has been used for their determination in environmental waters. Optimum conversion was found when the reaction was carried out in sodium hydrogencarbonatecarbonate medium at 40 °C for 15 min. Well separated peaks were obtained on a C 18 column with an acetonitrile-water gradient (1 ml min 21 ) of 30% acetonitrile for an initial 5 min which was increased linearly to 100% over 15 min and then maintained isocratic for 5 min, the acetonitrile ratio finally being returned to 30% in 5 min. The derivatized analytes were subjected to off-line solid phase extraction on C 18 sorbent. A linear calibration graph was obtained for 0.01-10 mg l 21 analytes with a correlation coefficient of 0.9954 for ammonia and in the range 0.9982-0.9996 for amines. The limit of detection for ammonia was 0.2 mg l 21 and for amines in the range 0.3-0.6 mg l 21 . The method was applied to tap, underground, river and aquarium waters, the recovery being in the range 97-106% (RSD 1.8-4.5%). Many of the samples were found to contain more than the permissible limit of ammonia. Phenyl isothiocyanate is stable for long periods in aqueous medium over wide ranges of pH and temperature, and the resulting phenylthioureas have adequate retention on C 18 sorbent and strong UV absorption, making this reagent suitable for the determination of amines in water.

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confidence: 99%

Determination of ammonia and aliphatic amines in environmental aqueous samples utilizing pre-column derivatization to their phenylthioureas and high performance liquid chromatography

Sahasrabuddhey¹,

Jain²,

Verma³

1999

Analyst

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“…It should be noted that most of the previously reported methods for DMA determination have some serious limitations. These are: the need for time consuming derivatization or pre‐concentration extraction steps , application at high temperatures (300–700 °C) , narrow range of measurement (less than one order of magnitude of concentration) short life time (60 hours) , high cost (US$ 400–800) not selective or not suitable for measuring concentrations above 5 μg mL −1 . The proposed potentiometric DMA sensors, however, offer several advantages compared with many of those previously published.…”

Section: Resultsmentioning

confidence: 99%

“…However, little is known about the methods used for the quantification of dimethylamine. Currently, some techniques have been used for the quantification of low‐molecular weight aliphatic amines including titrimetry, colorimetry , ion chromatography , high‐performance liquid chromatography (HPLC) , gas chromatography (GC) , and capillary electrophoresis (CE) . A liquid chromatographic method for determining dimethylamine after a prior micro‐extraction and two‐stage derivatization with o‐phthalaldialdehyde and 9‐fluorenylmethyl chloroformate has been advocated .…”

Section: Introductionmentioning

confidence: 98%

Novel Flow‐through Potentiometric System for Dimethyamine Assessment Using New Ion Exchangers Doped‐polymeric Membrane Sensors

2018

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New simple potentiometric sensing systems are described for the sensitive and selective monitoring of dimethylamine (DMA). These systems are based on using polymeric membranes doped in some ion exchangers such as dimethylamine/phosphomolybdate [(CH3)2NH3]22+[MP]2− (Sensor I), dimethylamine/tetraphenylborate [(CH3)2NH3]+[TPB]− (Sensor II) and dimethylamine/phosphotungstate [(CH3)2NH3]+[TP]− (sensor III). All the sensing systems are incorporated in poly(vinyl chloride) matrix plasticized with o‐NPOE. In a Trizma buffer solution of pH 7.1, the sensors exhibit a stable, fast and linear response for 5.0×10−6–1.0×10−2, 2.5×10−5–1.0×10−2, and 5.0×10−6–1.0×10−2 mol L−1 DMA+ with slopes of 53.2±0.4, 49.4±0.6, and 53.8±0.3 mV decade−1, and detection limits of 2.0×10−6 (0.16 μg mL−1), 1.6×10−5(1.3 μg mL−1), and 1.4×10−6 (0.11 μg mL−1) mol L−1 for sensors (I), (II), and (III), respectively. Potentiometric selectivity measurements of these sensors reveal negligible interferences from most common aliphatic and aromatic amines. Satisfactory results are obtained with an average accuracy of 99.5 % and a mean precision of ±0.5 %. Validation of the proposed assay methods are examined by measuring the limit of detection, linearity range, accuracy, precision, within‐day repeatability, between‐days reproducibility and method ruggedness. Good performance characteristics and applicability of these sensors for DMA assessment in different matrices under static and hydrodynamic modes of measurements are demonstrated. The proposed sensors are also prepared in a tubular form and used as DMA detector in a two‐channel flow injection setup for continuous monitoring. The frequency rate is 27–53 samples h−1. The sensors are satisfactory applied for DMA quantification in both biological matrices and environmental samples with recoveries ranging between 95.0 and 104.0 %.

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Determination of Aliphatic Amines by High Performance Liquid Chromatography with Amperometric Detection after Derivatization with Phenylisothiocyanate

2000

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Liquid chromatography with amperometric oxidative detection is proposed as a sensitive method for the determination of aliphatic amines previously converted in thioureido derivatives by reaction with phenylisothiocyanate (PIT). The phenylthioureas of four model amines, methylamine (MA), propylamine (PA), n-butylamine (BA) and isobutylamine (IBA) have been synthesized and isolated. Their electrochemical behavior on a glassy carbon electrode has been explored by cyclic voltammetry. The thioureido derivatives can be oxidized through two one-electron steps at acidic pH values, presumably involving the intermediacy of proton transfers. A mechanistic pathway is also proposed on the basis of experimental data. Liquid chromatographic parameters as mobile phase composition and¯ow rate, temperature and working electrode potential have been optimized. The method permits the simultaneous determination of the phenylthioureas of the selected amines with detection limits in the lower mgL 71 range.

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Determination of Methyl- and Dimethylamine in Waste Water by HPLC

Cited by 12 publications

References 8 publications

Determination of ammonia and aliphatic amines in environmental aqueous samples utilizing pre-column derivatization to their phenylthioureas and high performance liquid chromatography

Determination of ammonia and aliphatic amines in environmental aqueous samples utilizing pre-column derivatization to their phenylthioureas and high performance liquid chromatography

Novel Flow‐through Potentiometric System for Dimethyamine Assessment Using New Ion Exchangers Doped‐polymeric Membrane Sensors

Determination of Aliphatic Amines by High Performance Liquid Chromatography with Amperometric Detection after Derivatization with Phenylisothiocyanate

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