Solvent Extraction of Beryllium with Trifluoroacetylacetone and Hexafluoroacetylacetone.

Scribner, William G.; Borchers, Mary J.; Treat, W. J.

doi:10.1021/ac60244a041

Cited by 25 publications

(6 citation statements)

References 14 publications

(13 reference statements)

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“…Such properties are exhibited by hexafluoroacetylacetone (HHFA), a ligand with a pKa of 4.63 and a KD of 6.8 X 10"3 at pH <3.88 in H20-cyclohexane (33). The poor extraction of rare earths (38), Be2+ (34), and the nonextraction of Al3+, Zr4~, and Hf4+ (35) with this reagent have been reported.…”

Section: Resultsmentioning

confidence: 95%

Substoichiometric extraction of cations with mixtures of hexafluoroacetylacetone and tri-n-octylphosphine oxide in cyclohexane

Mitchell¹,

Ganges²

1974

Anal. Chem.

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toxic levels are detectable. The limit of detectability is generally assumed to be three times the standard deviation of the background. Using our results, one can infer the detectability limits as a function of atomic number, and these results are shown in Figure 7. By increasing the bombarding time by a factor of four, the detectability limit will be improved by a factor of two.An important facet of any measuring technique is the Recently the utility of methods of separation in nuclear analyses has been enhanced by the development of sub-

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Section: Resultsmentioning

confidence: 95%

Substoichiometric extraction of cations with mixtures of hexafluoroacetylacetone and tri-n-octylphosphine oxide in cyclohexane

Mitchell¹,

Ganges²

1974

Anal. Chem.

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“…Iron present in samples interfered because of chelation with the ligand and the partial decomposition of the chelate in the gas chromatograph (Moshier and Sievers, 1965), as demonstrated in Figure 1. Scribner, Borchers, et al (1966) showed that the use of 0.05M EDTA added to the sample prior to extraction with 0.25M trifluoroacetylacetone resulted in a 90% decrease in the amount of ferric iron extracted from the aqueous layer, but in some samples (blood) the remaining iron still interfered. Therefore, we turned to the use of the magnetic cathode for the complete removal of iron.…”

Section: Resultsmentioning

confidence: 99%

Gas chromatographic determination of beryllium in biological materials and in air

Noweir¹,

Cholak²

1969

Environ. Sci. Technol.

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The gas chromatographic determination of ultratrace quantities of beryllium in urine, blood, tissue, and air-borne dust is described. Except for air-borne dust, the procedure involves a doiible extraction, first with acetylacetone in benzene and then with a benzene solution of trifluoroacetylacetone. Beryllium in air-borne dust is extracted only by trifluoroacetylacetone in benzene. Levels as low as 1 X 10"10 gram (0.0001 µg.) of beryllium per sample can be determined by this method. Except for Fe3+ and Al3+, none of the ions usually present in air-borne dust or biological material interferes with the analysis. Fe3+ is removed in a magnetic mercury cathode. Al3+ can be precipitated with 8-quinolinol in chloroform. Recovery of beryllium ranged from 70 to 90% at levels from 1 X 10-9 gram (0.001 µg.) to 1 X 10~7 gram (0.10 µg.) per sample. The method is reliable, as shown by the results of analysis of air-borne dust and lung tissues. Beryllium has been determined in air-borne dusts and biological materials using colorimetric, fluorometric, or spectrographic methods (Cholak, 1959; Smythe and

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“…The Co 2+ , Ni 2+ and Cu 2+ extractions all started around pH 2 but did not exceed 70%. Since an extractant of the β-diketone type extracts metal ions to an organic phase under weakly acidic conditions through a proton exchange reaction, 16,17 the pH-dependent extraction of metal ions observed here implies that perfluorocarbon could work as an extracting phase. It should be noted that the competitive extraction (more than 12 h) also gave the same results, meaning that the forward extraction of these metal ions was achieved within 3 h.…”

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confidence: 84%

“…In fact, β-diketone type derivatives are well-known as promising extractants for lanthanide and transition metal ions. 16,17 Next we inspected the competitive extraction of Fe 3+ , Co 2+ , Ni 2+ and Cu 2+ (0.1 mM each) from aqueous solutions (3 ml) at various pH values to FC-72 (3 ml) containing 1,1,1,5,5,6,6,6-octafluoro-2,4-hexanedione (10 mM) (Fig. 2a) We report a liquid-liquid extraction system based on perfluorocarbon (fluorous-solvent extraction) that allows selective extraction of metal ions from aqueous and organic phases to a perfluorocarbon phase (FC-72) with perfluorinated β-diketone (1,1,1,5,5,6,6,6-octafluoro-2,4-hexanedione), which can be followed by backward extraction using 1 M nitric acid.…”

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confidence: 99%

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Perfluorocarbon-based Liquid-Liquid Extraction for Separation of Transition Metal Ions

et al. 2007

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Fluorous chemistry has attracted a broad range of attention from chemists and engineers due to its unique properties. Remarkable progress on fluorous solvents has highlighted fluorocarbons, especially perfluorinated alkanes and ethers, as reaction and separation media. [1][2][3][4][5][6][7][8][9][10] Water solubility in perfluorocarbons is extremely low. Perfluorocarbons are usually immiscible with non-fluorinated organic solvents at ambient temperature. Perfluorocarbons selectively dissolve highly-fluorinated compounds. These characteristics make perfluorocarbons attractive as a separation phase (fluorousbiphasic and triphasic systems). 1-3 Since Zhu reported organic reactions in perfluorocarbons, several research groups have demonstrated the feasibility of fluorous solvents as alternative reaction and separation media to conventional organic solvents. [4][5][6][7][8] The fluorous biphasic system developed by Horvath and Rabai offers elegant integration of a homogeneous reaction and subsequent separation using a fluorous tag.1 Despite the outstanding studies on the separation of organic compounds based on fluorous multiphase systems, [1][2][3][11][12][13] there are few reports on the extraction of metal ions using perfluorocarbons. 1,7 Since metal ions are widely used as catalysts in a variety of reactions, their separation from the products or reaction media has great significance. In particular, the removal of metal ions from an organic solvent using a nonaqueous solvent would be very advantageous, because water-based separation techniques sometimes ruin water-sensitive products. 1 For example, organometallic catalysts are synthesized using another organometallic compound as a substrate or a catalyst. 14 After the synthesis, the remaining metals, as byproducts or substrates, sometimes affect the performance of the synthesized catalysts. This is why the very limited number of papers report fluorous extraction of metal catalysts only from an organic phase. 1,10 We think it more informative to study the feasibility of perfluorocarbon-based solvent extractions both from an aqueous phase and from an organic phase. Here we explore the solvent extraction of metal ions from an aqueous or organic phase to a perfluorocarbon phase using a highly fluorinated extractant (fluorous-solvent extraction).So far there is no report describing the extraction from an aqueous phase to a perfluorocarbon phase, to our knowledge. In a preliminary investigation, we studied the extraction of Cu 2+ (0.1 mM) from an aqueous phase (3 ml, 0.1 M acetate buffer at pH 4) to 3 ml perfluorohexane (FC-72, Sumitomo 3M) using 10 mM perfluorinated β-diketone (1,1,1,5,5,6,6,6-octafluoro-2,4-hexanedione, Aldrich; Fig. 1a) as an extractant. 15 After mixing the two phases using a rotatory mixer for 3 h at 25˚C, the Cu (Fig. 1b), suggesting that 1,1,1,5,5,6,6,6-octafluoro-2,4-hexanedione facilitated the Cu 2+ extraction to the FC-72 phase through complexing with Cu 2+ . In fact, β-diketone type derivatives are well-known as promising extractants for lan...

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Solvent Extraction of Beryllium with Trifluoroacetylacetone and Hexafluoroacetylacetone.

Cited by 25 publications

References 14 publications

Substoichiometric extraction of cations with mixtures of hexafluoroacetylacetone and tri-n-octylphosphine oxide in cyclohexane

Substoichiometric extraction of cations with mixtures of hexafluoroacetylacetone and tri-n-octylphosphine oxide in cyclohexane

Gas chromatographic determination of beryllium in biological materials and in air

Perfluorocarbon-based Liquid-Liquid Extraction for Separation of Transition Metal Ions

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