Determination of trace fluoride in water samples by silylation and gas chromatography/mass spectrometry analysis

Du, Jian; Chen, Sheng; Wang, Yan; Zhang, Huarong; Jiang, Kezhi

doi:10.1002/rcm.9089

Cited by 9 publications

(7 citation statements)

References 26 publications

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“…Since COF 2 and phosgene yield the same derivatization product after reaction with 3,4-DMT (Figure 1), a confirmatory test to identify remains of the corresponding halide (F -) from COF 2 was explored. It was hypothesized that halide ions on the adsorbent would become volatile and suitable for detection with TD-GC/MS after reaction with a suitable derivatization reagent [26,27]. A number of tests using small postsampling additions of chlorotriethylsilane, both as liquid (1 µl) and in the vapor phase (≤250 µl headspace from the chemical bottle), demonstrated the production of fluorotriethylsilane.…”

Section: Tests Investigating the Discrimination Between Carbonyl Fluo...mentioning

confidence: 99%

The potential of thermal desorption‐GC/MS‐based analytical methods for the unambiguous identification and quantification of perfluoroisobutene and carbonyl fluoride in air samples

Wingfors

Mörén

Wiktelius

et al. 2022

J of Separation Science

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The reactive gases perfluoroisobutene and carbonyl fluoride are highly toxic and difficult to analyze in air. For this paper, the available sampling and analysis methods involving gas chromatography/mass spectrometry were investigated for their potential to give unambiguous identification and quantification of perfluoroisobutene and carbonyl fluoride, for which no such methods exist. Although high concentrations of perfluoroisobutene could be analyzed directly by manual split injection, sorbent sampling followed by thermal desorption GC/MS allowed lower concentrations to be analyzed. However, a significant degradation of perfluoroisobutene observed after thermal desorption analysis inspired the use of derivatization of perfluoroisobutene with 3,4‐dimercaptotoluene. The use of Tenax TA sorbent tubes spiked with 3,4‐dimercaptotoluene and trimethylamine in a molar ratio of 1:8 proved successful for the quantification of a unique perfluoroisobutene derivative, and the method was validated for atmospheres in the range of 0.13–152 ppb with a relative standard deviation of less than 20% and an accuracy of 90%. Although carbonyl fluoride was less stable than perfluoroisobutene, direct analysis was possible at high concentrations but the response was not linear. The 3,4‐dimercaptotoluene derivatization method developed was also applicable for quantification of carbonyl fluoride atmospheres.

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Section: Tests Investigating the Discrimination Between Carbonyl Fluo...mentioning

confidence: 99%

The potential of thermal desorption‐GC/MS‐based analytical methods for the unambiguous identification and quantification of perfluoroisobutene and carbonyl fluoride in air samples

Wingfors

Mörén

Wiktelius

et al. 2022

J of Separation Science

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“…7 Determination of fluoride concentration has been one of the important issues researched by analytical chemists because of the concentration range limitation in drinking water in terms of human health. 8 The traditional analytical methods for the determination of fluoride ions in water are ion chromatography (IC), 9 gas chromatography (GC), 10 ICP-MS, 11 AAS (i.e., by depression of Mg absorption), 12 and ion-selective electrode-based potentiometry (ISE). 13,14 Among these methods of F − determination, ISE and spectrophotometry stand out to give satisfactory results.…”

Section: Introductionmentioning

confidence: 99%

“…The traditional analytical methods for the determination of fluoride ions in water are ion chromatography (IC), gas chromatography (GC), ICP-MS, AAS (i.e., by depression of Mg absorption), and ion-selective electrode-based potentiometry (ISE). , Among these methods of F – determination, ISE and spectrophotometry stand out to give satisfactory results . The disadvantages of the ISE method were reported as limited selectivity, poor precision, long equilibration time, electrode drifting, and low solubility of the lanthanum fluoride membrane crystal − when determining fluoride at low concentrations.…”

Section: Introductionmentioning

confidence: 99%

“…The traditional analytical methods for the determination of fluoride ions in water are ion chromatography (IC), 9 gas chromatography (GC), 10 ICP-MS, 11 AAS (i.e., by depression of Mg absorption), 12 and ion-selective electrode-based potentiometry (ISE). 13 , 14 Among these methods of F – determination, ISE and spectrophotometry stand out to give satisfactory results.…”

Section: Introductionmentioning

confidence: 99%

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Spectrophotometric Fluoride Determination Using St. John’s Wort Extract as a Green Chromogenic Complexant for Al(III)

2022

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In this study, we applied an innovative approach of green analytical chemistry to develop a novel and eco-friendly chromogenic agent for fluoride determination by making use of the nontoxic Al(III)-flavonoid complex in a natural extract from St. John’s wort plant. The initial intensely yellow-colored Al(III)-flavonoid complex formed in the plant extract was converted to a colorless AlF6 3– complex with increasing amounts of fluoride, and color bleaching of the Al-flavonoid chromophore (measured as absorbance decrement) was proportional to fluoride concentration. The developed method gave a linear response within the F– concentration range of 0.11–1.32 mM with the LOD and LOQ values of 0.026 mM (0.5 mg L–1) and 0.079 mM (1.5 mg L–1), respectively. The LOD value for fluoride was below the WHO-permissible limit (1.5 mg L–1) and the US-EPA-enforceable limit (4 mg L–1) in water. The possible interference effects of common anions (Cl–, Br–, I–, NO3 –, HCO3 –, SO4 2–, and PO4 3–) and cations (K+, NH4 +, Ag+, Ca2+, Mg2+, Mn2+, Fe2+, and Fe3+) were investigated; the observed interferences from Fe2+, Fe3+, and PO4 3– were easily eliminated by masking iron with the necessary amount of Na2EDTA without affecting the blank absorbance of the Al(III)-flavonoid complex, precipitating phosphate with Ag(I) salt, and partly neutralizing alkaline water samples to pH 4 with acetic acid. The developed method was applied to real water samples and also validated against a reference spectroscopic method at the 95% confidence level.

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“…The interest of the scientific community and the importance of fluoride determination is best illustrated (besides the number of existing [13][14][15][16][17][18][19]) by the development and publication of instrumental methods in recent years based on the following techniques: Gas chromatography-mass spectrometry [20], inductively coupled plasma mass spectrometry [21,22], molecular absorption spectrometry [23,24], spectrophotometry [25], ion chromatography [26], high-resolution continuum source graphite furnace atomic absorption spectrometry [27], etc. Unlike these enumerated techniques, potentiometry (one of the nondestructive techniques of electrochemical analysis based on the measurement of the potential difference under equilibrium conditions between the reference and the indicator electrodes) does not require expensive equipment, elaborate and complex sample pretreatment steps, and authorized skilled personnel.…”

Section: Introductionmentioning

confidence: 99%

Potentiometric Determination of Free Fluoride Content in Wines from Dalmatia Region (Croatia)—A Comparative Study of Direct Potentiometry and Standard Addition Method

et al. 2022

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The aim of this study was to investigate 30 different types of Dalmatian wines as a potential source of fluoride. A fluoride ion selective electrode was used to measure the fluoride concentration in each sample. The direct potentiometric method and the standard addition method were evaluated, the latter being suggested as more accurate and precise. Measurements were performed in two buffers, acetate buffer and total ionic strength adjustment buffer (TISAB), to compare their influence on fluoride determination. The obtained results show that TISAB is a better choice than acetate buffer as a medium for fluoride determination. According to the proposed method, mass concentrations of fluoride of 0.19 and 0.18 mg/L were found in the studied red and white wines, with standard deviations of 0.04 and 0.03 mg/L, respectively. All determined fluorine levels in the tested wines were within the recommended limits and do not pose a risk to human health. No significant difference was found between the fluorine content in white and red wines, but there was a difference depending on the place of origin of the wine. The measured pH values for all the wines studied (except one sample) are very similar and show no significant correlation with the fluoride content.

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Determination of trace fluoride in water samples by silylation and gas chromatography/mass spectrometry analysis

Cited by 9 publications

References 26 publications

The potential of thermal desorption‐GC/MS‐based analytical methods for the unambiguous identification and quantification of perfluoroisobutene and carbonyl fluoride in air samples

The potential of thermal desorption‐GC/MS‐based analytical methods for the unambiguous identification and quantification of perfluoroisobutene and carbonyl fluoride in air samples

Spectrophotometric Fluoride Determination Using St. John’s Wort Extract as a Green Chromogenic Complexant for Al(III)

Potentiometric Determination of Free Fluoride Content in Wines from Dalmatia Region (Croatia)—A Comparative Study of Direct Potentiometry and Standard Addition Method

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