Determination of Pd and Co as Their Dithiocarbamate Complexes by Liquid Chromatography without Solvent Extraction

Mueller, B. J.; Lovett, R. J.

doi:10.1080/00032718508082581

Cited by 16 publications

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“…A third approach involves forming the complexes directly in a solvent system similar to the chromatographic mobile phase, usually acetonitrile and/or water (5,6,18). External formation, or direct reaction, procedures are far less timeconsuming than solvent extraction procedures and can be utilized for metal species that require a longer time for metal-complex formation than in situ methods allow.…”

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Salt-induced phase separation for the determination of metals as their diethyldithiocarbamate complexes by high-performance liquid chromatography

Mueller¹,

Lovett²

1987

Anal. Chem.

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R e vMgh-perfonnance liquid Chromatography wlth ultraviolet detection can be used to determine trace levels of Pt(II), Pd(II), Rh(III), Co(III), Ru(III), and I r in aqueous solution following complexation with dlethyidithlocarbamate. The metal Complexes are extracted into acetonitrile from aqueous solution by the addition of a saturated salt solution. Quantitative metal recovery from aqueous solution is achievable for most metals for a wide solution pH range. Detection limits for the metals are <3 ng of metaMmL of original aqueous sample. Analyses of real samples are highly reprodudbile and sensitive. I r can interfere in the determination of Pt(1I) and Rh( I I I). A general protocol for chromatographic separation and determination of Pt( I I), Pd( I I ) , Rh( I I I), Ru( I I I), and I r in aqueous solution Is presented.The use of dithiocarbamates for the determination of trace-level amounts of metals by chromatographic techniques has become popular in recent years. The ability to separate metal-dithiocarbamate complexes by high-performance liquid chromatography (HPLC) has been well documented (1-3). The actual application of dithiocarbamates for real sample analysis by chromatographic methods has also been addressedThe formation of metal-dithiocarbamate complexes for chromatographic separation has been carried out in three different ways. Solvent extraction for the preconcentration of trace metals from aqueous solution using dithiocarbamates has been used extensively in metal determinations by atomic absorption spectroscopy (14). 4-Methyl-2-pentanone has generally been used as the extracting solvent and is nebulized directly into a flame (15,16) or injected into a graphite furnace (17). A similar application of these solvent extraction techniques has been used to determine trace metals by liquid chromatography (4,9,10,18), generally extracting the complex into chloroform. The ultraviolet absorption spectrum of chloroform interferes with the UV detection of the complexes by HPLC and chloroform also presents solubility problems in certain reversed-phase applications; thus chloroform is usually removed by a slow vacuum evaporation and the sample is reconstituted into an appropriate solvent which can be injected into the chromatographic system.A number of workers (6, 7,18-22) add the dithiocarbamate ligand to their chromatographic mobile phase, allowing the metal-dithiocarbamate complexes to form in situ, which speeds up the analyses by avoiding solvent extraction. In situ methods have no capacity for preconcentrating the metal and are only applicable to metal species which rapidly form stable complexes in the mobile phase. The method also requires large amounts of complexing agent and the devotion of the (4-1 3).'Present address: E. I. Present address:HPLC system to metal determinations. Dithiocarbamates absorb in the ultraviolet region; thus visible detection wavelengths (which have smaller absorptivity coefficients than ultraviolet wavelengths) are required or electrochemical detection is needed.A third approach ...

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Salt-induced phase separation for the determination of metals as their diethyldithiocarbamate complexes by high-performance liquid chromatography

Mueller¹,

Lovett²

1987

Anal. Chem.

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“…1. The chelation of DEDTC and Pd(II) has been well characterized in the literature [11,12]. Near complete chelation was achieved by adding an excess amount of DEDTC.…”

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“…Near complete chelation was achieved by adding an excess amount of DEDTC. UV detection of the resulting complex at the maximum absorption of 297 nm was used for analysis [11]. However, the detection of Pd-DEDTC complex by DART-MS does not provide the optimum sensitivity due to the lack of basic nitrogen(s).…”

Section: Resultsmentioning

confidence: 99%

“…Adequate mixing was achieved by pipeting the mixture solution up and down several times immediately before DART-MS analysis. According to the literature [11], the concentration of the chelating agent must be at least 4 fold in excess of chelating reaction ratio. Therefore the final chelating agent concentration was chosen to be approximately 1 mM for all the samples used in this study with a concentration range from 0 M (blank) to 90 M.…”

Section: Sample Preparationmentioning

confidence: 99%

“…The separation and detection of metal chelates by LC-UV and LC-MS have been achieved for many metal species such as Pt, Rh, Pd, Os, Ni, Co, V, Cu, Fe and Ni [9][10][11][12][13]. Recently studies have investigated the detection of organometallic compound by DART-MS [14].…”

Section: Introductionmentioning

confidence: 99%

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