Fluoride compounds analysis

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. 

The synthesis of tantalum and niobium fluoride compounds is, above all, related to the fluorination of metals or oxides. Table 3 presents a thermodynamic analysis of fluorination processes at ambient temperature as performed by Rakov [51, 52]. It is obvious that the fluorination of both metals and oxides of niobium and tantalum can take place even at low temperatures, whereas fluorination using ammonium fluoride and ammonium hydrofluoride can be performed only at higher temperatures. 

Vibration spectra of fluoride and oxyfuoride compounds correspond to X Me ratios, especially in the case of island-type structure compounds. Analysis of IR absorption spectra provides additional indication of the coordination number of the central atom. Fig. 45 shows the dependence on the X Me ratio of the most intensive IR bands, which correspond to asymmetric Me-F modes in fluoride complexes, as well as v(Me=0) and v(Me-F) in oxyfluoride complexes. Wave numbers of TaF5, NbF5 and NbOF3 IR spectra were taken from [283-286]. 

Ceric ammonium sulfate, 5 674 Ceric fluoride, 5 674 Ceric hydroxide, 5 676 Ceric oxide, 5 670, 675 Ceric rare earths (RE), 74 631 Ceric sulfate, 5 674 Ceric sulfate method, for tellurium determination, 24 415 Cerium (Ce), 5 670-692 74 630, 63 It, 634t. See also Cerium compounds analysis, 5 679-680 color, 7 335... 

U. Grummisch, C. Kurowski, D. Timm, H. Grunewald, U. Meyhack, Rapid analysis of organic fluoride compounds for production control by diffuse reflectance near infrared spectroscopy, J. Near Infrared Spectrosc. 6 (1998) A239-A241. 

Direct analysis of the sulfonyl chlorides formed by reaction of phosphorus pen-tachloride with LAS is possible (2). The sulfonyl chlorides may also be formed by reaction with thionyl chloride or phosgene (3). Reaction with thionyl chloride is not recommended for LAS because of the superiority of PClj (4). The more volatile sulfonyl fluoride compounds may be produced by further reacting the sulfonyl chlorides with aque-... 

Oxides (Ln Oj), fluorides (LnF ), sulfides (Ln S, LnS), sulfofluorides (LnSF) of lanthanides are bases of different functional materials. Analytical control of such materials must include non-destructive methods for the identification of compound s chemical forms and quantitative detenuination methods which does not require analytical standards. The main difficulties of this analysis by chemical methods are that it is necessary to transform weakly soluble samples in solution. 

Compounds of the same stoichiometry type usually have the same type crystal structure within the row of alkali metals K - Rb - Cs rarely the same type structure with sodium-containing analogues and never ciystallize similarly with lithium-containing compounds. The crystal structure analysis of different fluoride and oxyfluoride compounds clearly indicates that the steric similarity between all cations and tantalum or niobium must be taken into account when calculating the X Me ratio. 

Fluoride ion, and weak acids and bases do not interfere, but nitrate, nitrite, perchlorate, thiocyanate, chromate, chlorate, iodide, and bromide do. Since analysis of almost all boron-containing compounds requires a preliminary treatment which ultimately results in an aqueous boric acid sample, this procedure may be regarded as a gravimetric determination of boron. 

Dermal Effects. Skin irritation was noted in wildlife officers at the RMA after they handled sick or dead ducks without gloves (NIOSH 1981). Although the investigators concluded that diisopropyl methylphosphonate contributed to the local effects, a number of other compounds were present. Analysis of the pond water indicated the presence of a number of organic and inorganic contaminants, including diisopropyl methylphosphonate (11.3 ppm) aldrin (0.368 ppm) dieldrin (0.0744 ppm) dicyclo-pentadiene, bicycloheptadiene, diethyl benzene, dimethyl disulfide, methyl acetate, methyl isobutyl ketone, toluene, and sodium (49,500 ppm) chloride (52,000 ppm) arsenic (1,470 ppm) potassium (180 ppm) fluoride (63 ppm) copper (2.4 ppm) and chromium (0.27 ppm). Because of the presence of numerous compounds, it is unclear whether diisopropyl methylphosphonate was related to the irritation. 

Analysis and mass spectrometry showed it to have the molecular formula C HeBrFa. This could have been formed by the addition of magnesium bromide to tetrafluorobenzyne followed by the elimination of magnesium bromide-fluoride to give bromotrifluorobenzyne (30) and hence the compound (31). Analysis of the 19F n.m.r. spectrum and more particularly the preparation of (31) from o-bromotetrafluorophenyl-magnesium bromide and benzene confirmed the suggested mechanism. In this latter reaction the ratio of (31) to (24) was 99 1 54>. 

Blood samples for analysis of volatile organic compounds (VOCs) including hexachloroethane should be collected into containers from which VOC contamination has been reduced (Ashley et al. 1992). Potassium oxalate/sodium fluoride is the recommended anti-coagulant. Blood samples should be placed on ice or refrigerated shortly after collection, and Ashley et al. (1992) recommend that analysis for VOCs be completed within 14 days. 

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