Rapid determination of hexavalent chromium in textiles by a novel ammonium pyrrolidine dithiocarbamate derivatization combined with UHPLC–MS/MS
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Abstract Hexavalent chromium is mainly determined by traditional spectrophotometry, atomic absorption spectrometry, and ion chromatography methods. In the present work, a reliable ultra high performance liquid chromatography with tandem mass spectrometry method was firstly developed for the determination of hexavalent chromium in textiles. The sample was extracted by acetic acid/sodium acetate buffer solution and followed by derivatization with ammonium pyrrolidine dithiocarbamate. The resulting derivative product was extracted by ethyl acetate, separated on a C18 column, and detected through electrospray ionization source in the positive mode with multiple reaction monitoring conditions. The derivatization reaction conditions were investigated and optimized. The developed method was validated in terms of the sensitivity, linearity range, matrix effects, recovery, accuracy, intra‐ and interday precision. Results showed that the calibration curves of pure solvent and matrix were linear over the selected concentration ranges of 0.1–20.0 μg/L. The achieved instrument and method limit of quantification were 0.1 and 40.0 μg/kg, respectively. Recoveries were calculated at three spiked concentrations and the values were between 92.2 and 103% with relative standard deviation values of 2.7–4.9% for intra‐day precision and 6.1% for inter‐day precision. Successful analysis of hexavalent chromium in practical textiles indicated that there was hexavalent chromium contamination in textiles.Keywords:
Hexavalent Chromium
Matrix (chemical analysis)
Simultaneous Determination and Selective Determination of Trivalent Chromium and Hexavalent Chromium
In this paper,simultaneous determination and selective determination of trivalent chromium and hexavalent chromium were reviewed,the advantages and disadvantages of different measurement methods were analyzed,which had important significance for the research of trivalent chromium and hexavalent chromium.
Hexavalent Chromium
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Hexavalent Chromium
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Basic chromium sulphate is the most versatile and common tanning agent in the leather industry. Under certain circumstances, the oxidation of the trivalent chromium salts into the hexavalent compounds, which are used in leather manufacture, is a crucial issue. In this study, different proportions of basic chromium sulphate were used in tanning and re-tanning processes according to a commonly used recipe, and levels of chromium oxide and hexavalent chromium were studied stratigraphically in the cross-section of the leather. It was observed that the levels of chromium oxide and hexavalent chromium in the skins increased in relation to the proportions of basic chromium sulphate used in the process, and that the amounts added in the tanning process had a greater effect on the levels of hexavalent chromium formed in the layers of the skins than did the amounts added in re-tanning.
Hexavalent Chromium
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Chromium exists at various valences, including elemental, trivalent, and hexavalent chromium, and undergoes reduction-oxidation reactions in the environment. Since hexavalent chromium is known as a human carcinogen, it is most important to evaluate the oxidation-reduction characteristics of the hexavalent chromium species. Although hexavalent chromium can be reduced to trivalent state, the detailed information on this in workplace environments is limited. The purpose of this study was to investigate hexavalent chromium reduction in time in various conditions. A pilot chrome plating operation was prepared and operated in a laboratory for this study. There was evidence that the hexavalent chromium was reduced by time after mist generation. The percentage ratio (with 95% confidence intervals in parentheses) of hexavalent chromium to total chromium was almost 100% (99.1 approximately 102.3) immediately after mist generation, and was reduced to 87.4% (84.8 approximately 89.9) at 1 hour and 81.0% (78.3 approximately 83.5) at 2 hours, respectively. Another test indicated that hexavalent chromium collected on PVC filters was also reduced by time after sampling. Hexavalent chromium was reduced to 90.8% (88.2 approximately 93.3) at 2 hours after sampling. It also was found that hexavalent chromium was reduced during storage in air. It is recommended that air samples of hexavalent chromium be protected against reduction during storage.
Hexavalent Chromium
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Pollution by hexavalent chromium is a growing, global problem. Its presence in public water systems is often the result of industrial activities, both past and present. In this study, tricalcium aluminate (C3A, Ca3Al2O6) is added to solutions of varying concentrations of potassium chromate (K2CrO4) and samples of both the solid and liquid are taken at various time intervals to monitor the removal of chromium from the solutions. Solution concentrations of 0.2 M, 0.1 M, 0.02 M, and 0.01 M are used, and the chromium concentration is found to reduce in all cases. For the 0.02 M solution the chromium concentration is reduced from 1040 ppm to 3.1 ppm in 1 week, and the chromium concentration of the 0.01 M solution is reduced from 520 ppm to 0.26 ppm in only one day of reaction with the C3A. The chromium removed from solution is identified in the solid products, which were fully characterised as being a mixture of ettringite (Ca6[Al(OH)6]2(CrO4)3·26H2O) and monochromate (Ca4[Al(OH)6]2CrO4·8H2O) phases from analysis of Powder X-ray Diffraction and Fourier Transform Infrared Spectroscopy data. The work presented here is a proof of concept study to investigate C3A as a potential material for the removal of hexavalent chromium from solution. The results from this study are initial steps towards development of this as a technology for hexavalent chromium remediation.
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A new and rapid microwave assisted derivatization method for the determination of fatty acids in edible oil by GC MS was developed. The optimum conditions for derivatization, such as the derivatization solvent composition, microwave assisted derivatization pressure and time were studied for KOH methanol and H 2SO 4 methanol systems. The experimental results were compared with those obtained by traditional method of normal temperature derivatization .The applied range of the two derivatization systems was also discussed in detail. The derivatization was accomplished in 1 minute. Heptane was used as extraction solvent. The method is rapid, efficient, accurate and solvent saving.
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This paper established the simultaneous determination of trivalent chromium and hexavalent chromium in leather extract by ion chromatographic analysis method. Using IonPac CS5A chromatographic column can finishing two valent chromiums analysis in 8 min. Trivalent chromium and hexavalent chromium were chelated respectively by PDCA and DPC, and were detected respectively in ultraviolet and visible wavelength by UV-Vis detector. The possible presence of dyes and organic pollutants in leather extract were pretreated by On Guard RP column. The detection limit of trivalent chromium and hexavalent chromium were 31.0 μg/L and 0.41 μg/L respectively. This method is of high sensitivity, low disturbance, hign accuracy and efficiency.
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