Fluoride detection

The reaction in neat CH,CN proceeded more slowly than in the "acid-catalysed cases. The initial, transient, prodnct was dark brown, which suggests, from Schmeisser s description, IF. This colour quickly disappeared IF5 was the sole iodine fluoride detected in the products. 

Conventional ISEs have been used as detectors for immunoassays. Antibody-binding measurements can be made with hapten-selective electrodes such as the trimethylphenylammonium ion electrode. Enzyme immunoassays, in which the enzyme label catalyzes the production of a product that is detected by an ISE, take advantage of the amplification effect of enzyme catalysis in order to reach lower detection limits. Systems for hepatitis B surface antigen and estradiol use horseradish peroxidase as the enzyme label and an iodide electrode as the detector. The horseradish peroxidase catalyzes the oxidation of p-fluoroanadine with the fluoride detected by the ISE. Biotin and cyclic have been determined... 

Recently, Fabre et al. [31] and Freund et al. [7, 8] used electro-chemically deposited, self-doped, boronic-acid-substituted, conducting polymers for saccharide and fluoride detection. Freund et al. prepared a potentiometric sensor for saccharides using self-doped PABA [7, 8]. The transduction mechanism in that system is reportedly the change in pKa of polyaniline that accompanies complexation, and the resulting change in the electrochemical potential. Sensors produced with this approach exhibit reversible responses with selectivity to various saccharides and 1,2-diols (Figure 3.22) that reflect their binding constants with phenylboronic acid observed in bulk solutions. The sensitivity... 

Rum, G. Lee, W-Y. Gardea-Torresdey, J. Apphcations of a U.S. EPA-Approved Method for Fluoride Determination in an Environmental Chemistry Laboratory Fluoride Detection in Drinking Water. J. Chem. Educ. 2000, 77, 1604-1606. 

Most fluorine-containing compounds can be reduced to the fluoride ion, F , which can be detected by the tests given below. 

Elemental fluorine and the fluoride ion are highly toxic. The free element has a characteristic pungent odor, detectable in concentrations as low as 20 ppb, which is below the safe working level. The recommended maximum allowable concentration for a daily 8-hour time-weighted exposure is 1 ppm. 

Figure 8.28 shows how the X-rays fall on the solid or liquid sample which then emits X-ray fluorescence in the region 0.2-20 A. The fluorescence is dispersed by a flat crystal, often of lithium fluoride, which acts as a diffraction grating (rather like the quartz crystal in the X-ray monochromator in Figure 8.3). The fluorescence may be detected by a scintillation counter, a semiconductor detector or a gas flow proportional detector in which the X-rays ionize a gas such as argon and the resulting ions are counted.

Significant vapor pressure of aluminum monofluoride [13595-82-9], AIF, has been observed when aluminum trifluoride [7784-18-1] is heated in the presence of reducing agents such as aluminum or magnesium metal, or is in contact with the cathode in the electrolysis of fused salt mixtures. AIF disproportionates into AIF. and aluminum at lower temperatures. The heat of formation at 25°C is —264 kJ/mol(—63.1 kcal/mol) and the free energy of formation is —290 kJ/mol(—69.3 kcal/mol) (1). Aluminum difluoride [13569-23-8] h.3.s been detected in the high temperature equihbrium between aluminum and its fluorides (2). 

Volatile impurities, eg, F2, HF, CIF, and CI2, in halogen fluoride compounds are most easily deterrnined by gas chromatography (109—111). The use of Ftoroplast adsorbents to determine certain volatile impurities to a detection limit of 0.01% has been described (112—114). Free halogen and haHde concentrations can be deterrnined by wet chemical analysis of hydrolyzed halogen fluoride compounds. 

Oxygen and nitrogen also are deterrnined by conductivity or chromatographic techniques following a hot vacuum extraction or inert-gas fusion of hafnium with a noble metal (25,26). Nitrogen also may be deterrnined by the Kjeldahl technique (19). Phosphoms is determined by phosphine evolution and flame-emission detection. Chloride is determined indirecdy by atomic absorption or x-ray spectroscopy, or at higher levels by a selective-ion electrode. Fluoride can be determined similarly (27,28). Uranium and U-235 have been determined by inductively coupled plasma mass spectroscopy (29). 

A reagent which is primarily of interest as a means of converting alcohols into fluorides has been used to dehydrate C-11 alcohols in high yields. 1 la-Alcohols dehydrate rapidly with 2-chloro-l-diethylamino-l,l,2-trifluoro-ethane reagent at low temperature, while 11 j5-alcohols require refluxing methylene chloride. Traces of fluoro compounds have been detected in the products. 

Apart from XeF, which is the light-emitting species in certain Xe/F2 lasers, there is no evidence for the existence of any odd-valent fluorides. Reports of XeFg have not been confirmed. Of the other halides, XeCl2, XeBr2 and XeCl4 have been detected by Mossbauer spectroscopy as products of the -decay of their... 

The proposed mechanism includes the production of HCl from the pyro-hydrolysis of the metal chlorides. Similar reactions are likely for bromides and iodides. Fluorides however are relatively stable and would not be expected to hydrolyse. It was considered that this might account for the inability of fluorides to cause cracking. Hydrogen absorption by titanium alloys exposed to chloride salts at elevated temperatures has been detected and found to be proportional to the amount of moisture participating in the reaction. 

Specific ion electrodes, similar in design to the glass electrode, have been developed to analyze for a variety of cations and anions. One of the first to be used extensively was a fluoride ion electrode that is sensitive to F- at concentrations as low as 0.1 part per million and hence is ideal for monitoring fluoridated water supplies. An electrode that is specific for Cl- ions is used to diagnose cystic fibrosis. Attached directly to the skin, it detects the abnormally high concentrations of sodium chloride in sweat that are a characteristic symptom of this disorder. Diagnoses that used to require an hour or more can now be carried out in a few minutes as a result, large numbers of children can be screened rapidly and routinely. 

The amount of reddish-purple acid-chloranilate ion liberated is proportional to the chloride ion concentration. Methyl cellosolve (2-methoxyethanol) is added to lower the solubility of mercury(II) chloranilate and to suppress the dissociation of the mercury(II) chloride nitric acid is added (concentration 0.05M) to give the maximum absorption. Measurements are made at 530nm in the visible or 305 nm in the ultraviolet region. Bromide, iodide, iodate, thiocyanate, fluoride, and phosphate interfere, but sulphate, acetate, oxalate, and citrate have little effect at the 25 mg L 1 level. The limit of detection is 0.2 mg L 1 of chloride ion the upper limit is about 120 mg L . Most cations, but not ammonium ion, interfere and must be removed. 

Disproportionation of Pu(IV). There are several needs associated witn the occurrence, detection, and mitigation of the disproportionation of Pu(IV) in applied plutonium recovery/ purification procedures. First, there is a great need for much more detailed information concerning the effect of typical process conditions [e.g., temperature, concentration of plutonium, hydrogen ion, nitrate ion, nitrite ion, fluoride ion, other metal ions (e.g., A13+, Fe3+, etc.), etc.] on the occurrence and extent of the reaction ... 

An interesting special application has been proposed by Schlichthorl and Peter.31,41 It aims at deconvolution of electrochemical impedance data to separate space charge and surface capacitance contributions. The method relies on detection of the conductivity change in the semiconductor associated with the depletion of majority carriers in the space charge region via potential-modulated microwave reflectivity measurements. The electrode samples were n-Si(lll) in contact with fluoride solution. 

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