Determination of highly polar compounds in water samples around former ammunition plants

Lewin, U.; Wennrich, Luise; Efer, J.; Engewald, W.

doi:10.1007/bf02505543

Cited by 23 publications

(14 citation statements)

References 8 publications

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“…Among them, GC is the most commonly employed besides HPLC [14]. However, these compounds are thermolabile and polar compounds, and a derivatization step is often required to obtain good GC performance [15 -19].…”

Section: Introductionmentioning

confidence: 99%

Determination of four aromatic amines in water samples using dispersive liquid–liquid microextraction combined with HPLC

Wang¹,

Wei

et al. 2008

J of Separation Science

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A new method for the determination of four aromatic amines in water samples was developed by using dispersive liquid-liquid microextraction (DLLME) technique combined with HPLC-variable wavelength detection (HPLC-VWD). In this extraction method, 0.50 mL methanol (as dispersive solvent) containing 25.0 microL tetrachloroethane (as extraction solvent) was rapidly injected by a syringe into 5.00 mL water sample. Accordingly, a cloudy solution was formed. After centrifugation for 2 min at 4000 rpm, the fine droplets of the tetrachloroethane containing the analytes were sedimented in the bottom of the conical test tube (7+/-0.2 microL). Then, 5.0 microL of the settled phase was determined by HPLC-VWD. Parameters such as the kind and volume of extraction solvent and dispersive solvent, extraction time, and salt concentration were optimized. Under the optimum conditions, the enrichment factors ranged from 41.3 to 94.5. Linearity was observed in the range of 5-5000 ng/mL. The LODs based on S/N of 3 ranged from 0.8 to 1.8 ng/mL. The RSDs (for 400 ng/mL of p-toluidine and o-chloroaniline, 100 ng/mL of p-chloroaniline and p-bromoaniline) varied from 4.1 to 5.3% (n=6). The water samples collected from rivers and lakes were successfully analyzed by the proposed method and the relative recoveries were in the range of 85.4-111.7% and 90.2-101.3%, respectively.

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Section: Introductionmentioning

confidence: 99%

Determination of four aromatic amines in water samples using dispersive liquid–liquid microextraction combined with HPLC

Wang¹,

Wei

et al. 2008

J of Separation Science

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“…Additionally, a methanol eluate from a purification system used for the treatment of groundwater in the area of a former ammunition plant was investigated. This sample contained a variety of explosives and related compounds among which 2-A-4,6 DNT, 4-A-2,6-DNT and 2-A-6-NT were determined at concentrations of 1334, 1761 and 237 ng/mL, respectively, using HPLC [21]. Figure 6C shows the electropherogram for this rather complex sample and Fig.…”

Section: Performance Characteristics and Practical Applicationmentioning

confidence: 99%

Determination of hydrazine, monomethylhydrazine, 1,1‐dimethylhydrazine, and 1,2‐dimethylhydrazine by nonaqueous capillary electrophoresis with amperometric detection

et al. 2005

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The present study is concerned with the application of nonaqueous capillary electrophoresis (NACE) with electrochemical detection (ED) to the separation and quantitative determination of hydrazine (Hy) and its methyl derivatives. The best performance of NACE-ED was found when using 4 mM sodium acetate/10 mM acetic acid/methanol: acetonitrile = 1:2 as the running buffer, with a bare platinum working electrode set at +1.0 V in an end-column amperometric detection cell. The choice and ratio of suitable solvents for the separation and injection media played an essential role for the performance characteristics of the method. The limits of detection for Hy, methylhydrazine, symmetrical dimethylhydrazine, and unsymmetrical dimethylhydrazine were 5, 2, 12, and 1 ng/mL, respectively. This is between one and two orders of magnitude lower than that achieved by previously reported CE-ED methods in aqueous buffer systems in conjunction with various types of chemically modified electrodes. The practical utility of the new NACE-ED methodology is demonstrated in terms of the determination of traces of Hys in spiked environmental samples containing a wide range of explosives and related compounds.

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“…For the separation of eight nitrobenzoic acids (see Table 3) that were recently found or proposed to be present in ammunition wastewater [3,4,5], TBAHS was used as the IPR for HPLC-DAD with the following gradient program: 20% MeOH/80% TBAHS (v/v) to 95/5 in 30 min. To enable hyphenation with an MS, we tested the separation of these acids with the four volatile IPRs given in Table 2.…”

Section: Separationmentioning

confidence: 99%

“…However, in the last few years it has become obvious that more polar metabolites of NACs need to be considered, such as environmental oxidation products like nitrobenzoic acids [3,4,5] and by-products from 2,4,6-trinitrotoluene (TNT) production, like sulfonated nitrotoluenes [5,6]. For such polar, acidic compounds, ionpairing chromatography with tetrabutylammonium hydrogensulfate (TBAHS) is frequently used, and we recently developed a separation system for 12 abundant compounds using HPLC with diode array detection (HPLC-DAD) [7].…”

Section: Introductionmentioning

confidence: 99%

HPLC-MS investigations of acidic contaminants in ammunition wastes using volatile ion-pairing reagents (VIP-LC-MS)

Schmidt

Buetehorn

Steinbach

2004

Analytical and Bioanalytical Chemistry

148

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In order to hyphenate ion pairing chromatography and MS detection we used several types of formates as volatile ion pairing reagents (IPRs) instead of common tetraalkylammonium salts, as these salts tend to precipitate in the ion source. The formates were prepared by mixing formic acid with the corresponding amine. Both tributyl- and trihexylammonium formate proved to be valuable IPRs for the separation of acidic compounds like nitrobenzoic acids, nitrobenzenesulfonic acids and nitrated phenols. Due to the weaker retention of the ion-pairs with trialkylammonium formates compared with tetraalkylammonium compounds, either less organic modifier or a higher concentration of the IPR had to be used. With negative atmospheric pressure chemical ionization mass spectrometry and electrospray ionization mass spectrometry it was possible to unambiguously identify several acidic oxidation products of 2,4,6-trinitrotoluene (TNT) in ammunition wastewater and soil extracts. 2-amino-4,6-dinitrobenzoic acid was often found to be the main metabolite of TNT in such water samples.

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Determination of highly polar compounds in water samples around former ammunition plants

Cited by 23 publications

References 8 publications

Determination of four aromatic amines in water samples using dispersive liquid–liquid microextraction combined with HPLC

Determination of four aromatic amines in water samples using dispersive liquid–liquid microextraction combined with HPLC

Determination of hydrazine, monomethylhydrazine, 1,1‐dimethylhydrazine, and 1,2‐dimethylhydrazine by nonaqueous capillary electrophoresis with amperometric detection

HPLC-MS investigations of acidic contaminants in ammunition wastes using volatile ion-pairing reagents (VIP-LC-MS)

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