Sur la thermogravimétrie des précipités analytiques

Duval, Thérèse; Duval, Clément

doi:10.1016/s0003-2670(01)93776-6

Cited by 8 publications

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“…To avoid loss of ammonia and water the hexahydrate should be precipitated in the cold and dried below 30°C. (68,129). The factors affecting the precipitation of the hexahydrate have also been studied by Lassieur (153).…”

Section: Nitrogenmentioning

confidence: 99%

“…According to Schuhecker (250) and Lustig (164) elimination of carbon during ignition of the hexahydrate to the pyrophosphate is facilitated by ashing with the aid of perchloric and nitric acids. The change to pyrophosphate occurs at 4770 C. (68).…”

Section: Nitrogenmentioning

confidence: 99%

“…A new procedure for magnesium involves its precipitation as magnesium ammonium arsenate hexahydrate and iodometrio determination of the arsenic (182). Pyrolysis curves for several of the most used magnesium precipitates have been determined (68). For quantitative separation of magnesium in a dense coarsely crystalline form and its subsequent determination by permanganate titration, Gordon and Caley (95) recommend precipitation with pure diethyl oxalate, in 85% acetic acid solution.…”

Section: Magnesiummentioning

confidence: 99%

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Fertilizers

Jacob¹

1949

Anal. Chem.

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Section: Nitrogenmentioning

confidence: 99%

Section: Nitrogenmentioning

confidence: 99%

Section: Magnesiummentioning

confidence: 99%

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Fertilizers

Jacob¹

1949

Anal. Chem.

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confidence: 99%

The thermal dissociation of sodium hexanitrocobaltate(III)

Wendlandt

Southern

1970

Journal of Thermal Analysis

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The stoichiometry of the thermal decomposition reaction of Naz[Co(NO~)nl was studied by TG, DTA and mass spectrometric analysis.The thermal properties of NazKz[Co(NO2)6] 2 9 n H20 and Kz[Co(NOz)~] have been investigated by Duval and co-workers [1,2]. For the latter compound, a TG curve plateau was found from 43 ~ to 160 ~ which was said to be suitable for the automatic determination of cobalt. Above 160 ~ the evolution of 3 moles of NOz per mole of complex took place to give the mixture, CoO + 3KNOz. The same type of dissociation reaction was reported for Csz[Co(NO2)6] [3] and Naa[Co(NOz)6] [4]. Since the above data did not give very much information on the decomposition reaction stoichiometry or analysis of the reaction products, the thermal dissociation of Naz[Co(NOz)6] was studied in somewhat greater detail by TG, DTA and mass spectrometric analysis (MSA). Experimental Preparation of Na3CCo(NO~) 6]This complex was prepared by the method of Cunningham and Perkin [5] Analysis of the compound gave % metal oxide: 23.3% found, 23.69~ calc. nitrogen: 21.2% found, 20.79% calc. ApparatusThe thermobalance, DTA apparatus, and mass spectrometer have all been previously described [6]. The heating rate for the TG and DTA experiments was 10 ~ Results and discussionThe mass-loss and DTA curves of Naz[Co(NOz)6] and the MSA data are shown in Fig. 1.The mass-loss curve was rather surprising for two reasons: first, the initial complex was thermally stable up to about 200~ and, second, it did not dissociate

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Beckmann Fragmentation and Rearrangement. Part VI thian‐3‐one oximes. Fragmentation reactions no. 26

Grob¹,

Ide²

1974

Helvetica Chimica Acta

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In 70% aqueous dioxane thian‐3‐one anti‐oxime p‐toluenesulfonate (tosylate) (8b) undergoes concerted fragmentation to the methylidenesulfonium ion 14, part of which recyclizes to 1,3‐thiazepin‐4‐one (11). With the syn‐isomer 8b rearrangement to 1,4‐thiazepin‐3‐one (10) and fragmentation to 14 occur in the ratio 4:1. Analysis of the rate data in 80% ethanol shows that anti fragmentation is 142 times as fast as syn fragmentation, but only 26 times as fast as rearrangement of the ‘homomorphous’ thian‐4‐one oxime tosylate (18b). A comparison of the rates of cyclohexanone oxime tosylate 20, thian‐3‐ and ‐4‐one oxime tosylates reveals the rate retarding influence of sulfur. – The configurations assigned to the stereoisomeric thian‐3‐one oximes (8a) in the literature have to be reversed in the light of present results.

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Sur la thermogravimétrie des précipités analytiques

Cited by 8 publications

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The thermal dissociation of sodium hexanitrocobaltate(III)

Beckmann Fragmentation and Rearrangement. Part VI thian‐3‐one oximes. Fragmentation reactions no. 26

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