Phosphorus hydrochloric acid extractable

Ammonium Fluoride-hydrochloric Acid Extractable Phosphorus of Soils Bray s 1 Method Bray and Kurtz, 1945 (For soils with pH around 5.5 or less)... 

Organic phosphorus is determined by the difference in phosphorus content of the 1M hydrochloric acid extract measured before and after ignition of the dry sediments at 550°C. In all instances the orthophosphate is determined by using standard Technicon AutoAnalyzer II techniques. Silica does not interfere. 

Phosphorus extracted from sediment by NaOH has been related to non-occluded, surface-exchangeable, bioavailable forms (22). Hydrochloric acid extraction yields occluded phosphorus incorporated in hydrous metal oxides, carbonate and phosphate minerals of sediment. Hydroxylamine reagent specifically removes hydrous manganese oxides, while amorphous hydrous oxides of iron and aluminijm are removed by the oxalate reagent. Total available sediment phosphorus analyses includes sediment organic phosphorus components in addition to the inorganic portion determined by the selective extraction procedures. 

In the lower reaches of the Genesee River, the results of the extractions suggest that substances other than hydrous oxides are phosphorus sinks. This is evident where the amount of sediment phosphorus extracted by hydrochloric acid steadily increases down river, while the oxalate extractable phosphorus remains relatively constant. Schwertmann (2 ) emphasized that the results of such procedures are best considered as a measure of the relative amount of a phase or, more generally, a measure of an element s reactivity in a sediment under carefully controlled conditions. Laboratory experiments (Figure 8) show that phosphorus uptake by calcium carbonate, under simulated natural conditions, proceeds slowly. The large hydrochloric acid extractable component observed at Rochester may arise from slow uptake and subsequent mineralization of dissolved inorganic phosphorus by carbonate minerals. 

Studies in the tropics have reported organic phosphorus in the supernatant after resin extraction, in the sodium bicarbonate extract, in the sodium hydroxide extract before sonication, in the sodium hydroxide extract after sonication, and in the concentrated hydrochloric acid extract. Sodium bicarbonate recovers easily hydrolysable organic phosphorus (Bowman and Cole, 1978), while sodium hydroxide recovers organic phosphorus associated with humic and fulvic acids. Concentrated hydrochloric acid recovers organic phosphorus from more stable pools, although it may also extract bioavailable organic phosphorus from particulate organic matter (Tiessen and... 

A mixture of 10 g of the above piperazine carboxylate ester, 8 g of phosphorus pentoxide and 20 ml of phosphorus oxychloride is heated under reflux for about 1 day, diluted with 100 ml each of chloroform and benzene and quenched with 200 g of ice. The mixture is made basic with 10% sodium hydroxide. Theorganic layer is Isolated and extracted with 150 ml of dilute hydrochloric acid. The product is precipitated from the aqueous layer by addition of 10% sodium hydroxide, extracted with benzene and dried over potassium carbonate. Recrystallization from benzene-petroleum ether gives 2[Pg.77]

The mixture is taken up with water and the base is extracted from the toluene with dilute hydrochloric acid. The hydrochloric solution is rendered alkaline with caustic soda, the base is separated with ether, dried, and after distillation of the ether fractionated in vacuo, BP at 0.05 mm Hg, 150° to 153°C. The basic ether is then dissolved in dry ether, and ether saturated with dry hydrogen chloride is added dropwise with stirring. An excess of hydrogen chloride must be avoided as it may produce decomposition to the corresponding diphenyl ethylene. The ether-moist hydrochloride is preferably dried at once in vacuo and subsequently reprecipitated from acetone-ether and then again dried in vacuo over phosphorus pentoxide. Hydrochloride, MP 12B°C. 

This crude product is dissolved in 100 ml of dilute hydrochloric acid, the acid solution is extracted with ether, and the aqueous layer is made basic with sodium hydroxide solution (3N) in the presence of ether (approximately 250 ml). The ether layer Is separated, dried over potassium hydroxide and evaporated to a white solid. Additional purification by repeating the formation of the hydrochloric acid salt and reprecipitation of the base is carried out. When purified in this manner, followed by drying at 80°C in vacuo over phosphorus pentoxide, 2-chloro-11-(4-methyl-1-piperazinyl)dibenz[b,f] [1,4]oxazepine, li/IP 109° to 111°C, is obtained. 

A solution of 100 g (1.7 mols) of isopropylamine in 60 cc of water was stirred into a solution of 4-hydroxyphenoxypropylene oxide. After the exothermic reaction has subsided, the reaction mixture was heated for two hours at 60Thereafter, the aqueous ethanol was distilled off, and the solid residue was dissolved in aqueous hydrochloric acid comprising more than the theoretical stoichiometric molar equivalent of hydrochloric acid. The aqueous acid solution was extracted with ether and was then made alkaline with sodium hydroxide, whereby a solid crystalline precipitate was formed which was filtered off and dried over phosphorus pentoxide. The product was 1,1 -(4 -hvdroxvphenoxv)-2-hvdroxv-3-isopropylamino-pro-pane. Its hydrochloride had a melting point of 166°Cto 169°C. 

B) /3-Methylglutaric Acid.—In a 5-1. flask are placed 400 g. of the amide and 11. of concentrated hydrochloric acid the mixture is warmed on a steam bath until solution is complete, after which it is diluted with 1 1. of water and refluxed for eight hours. The amber-colored solution is saturated with sodium chloride and extracted with five 600-cc. portions of ether. The combined ether extracts are dried for one hour over phosphorus pentoxide, and the solvent is removed by distillation. The residue, crude /3-methylglutaric acid, weighs 238-240 g. (80 per cent of the theoretical amount) and melts at 79-82° with previous softening. This product is recrystallized from about 250 cc. of 10 per cent hydrochloric acid. The recovery is about 90 per cent (Note 4), and the purified product melts at 85-86°. 

To a flame-dried, three-neck, 1-1 flask were added, in order, p-xylene (107 g, 1.0 mol), phosphorus trichloride (412 g, 3.0 mol), and anhydrous aluminum chloride (160 g, 1.2 mol). The reaction mixture was slowly heated to reflux with stirring. After 2.5 h at reflux, the reaction was allowed to cool to room temperature and the volatile components distilled at reduced pressure. The residual oil was slowly added to cold water (1 1) with stirring, and a white solid formed. The solid was removed by filtration, washed with water, and air dried. The solid was suspended in water (1 1) to which was added 50% sodium hydroxide solution (90 ml) to cause dissolution. The solution was saturated with carbon dioxide and filtered through Celite . The basic solution was washed with methylene chloride (200 ml) and acidified with concentrated hydrochloric acid (200 ml). The white solid that separated was isolated by extraction with methylene chloride (3 x 250 ml). The extracts were dried over magnesium sulfate, filtered, and evaporated under reduced pressure to give the pure 2,5-dimethylbenzenephosphinic acid (99 g, 60%) as an oil, which slowly crystallized to a solid of mp 77-79°C. 

Two typical acid extractants are the Bray (which has two forms, both of which are acidic) and the Mehlich-3. The Bray extractant is a dilute solution of hydrochloric acid and ammonium fluoride [11], The Mehlich-3 extractant is a dilute solution of acetic and nitric acids and also contains ammonium nitrate and EDTA [11], Both are designed to extract soluble, exchangeable, and easily dissolved nutrients, particularly phosphate. While the Bray extractant is designed to extract plant available phosphorus, the Mehlich-3 extractant also extracts potassium [10-12],... 

Aspila et al. [60] have described a semi-automated method for the determination of inorganic, organic and total phosphorus in river and lake sediments. Total phosphorus is extracted from sediments with 1M hydrochloric acid after ignition at a high temperature (550°C) (method 1) or by digestion with sulphuric acid-potassium persulphate at 135°C in a sealed PTFE-lined Parr bomb (method 2). 

Excess phosphorus oxychloride is removed as well as possible with a rotary evaporator under reduced pressure. The residue Is cooled to room temperature and 300 ml of diethyl ether Is added. The mixture is poured into a separatory funnel. Hexane is added until the two phases separate cleanly and the funnel is shaken vigorously. The phases are separated and the lower layer is extracted with three 250-mL portions of ether (Note 4). The combined organic layers are washed with 300 mL of cold aqueous 10% hydrochloric acid and 200 mL of aqueous 5% sodium hydroxide (Note 5) and then concentrated carefully with a rotary evaporator to give 136-156 g (70-87%) of crude diethyl 2-chloro-2-cyclopropylethene-l, 1-dicarboxyl ate ... 

A solution of 13.8 gm (0.10 mole) of phosphorus trichloride in 30 ml of ethyl ether is added dropwise over a 3-4 hr period at —20°C to a stirred solution of 16.8 gm (0.3 mole) of propargyl alcohol, 30.0 gm (0.3 mole) of triethylamine, and 100 ml of ether. After the addition, the mixture is stirred for an additional hour at 0°-5°C, warmed slowly to room temperature overnight, water is added, the ether separated, and the resulting water layer extracted with two 100 ml portions of ether. The combined ether layer is washed with two 100 ml portions of dilute hydrochloric acid, two 100 ml portions of 10% aqueous sodium carbonate, dried, and concentrated under reduced pressure distillation of the residue affords 18.0 gm (92%), b.p. 115°-115°C (0.25 mm). 

It is recommended that the compound be fused with a mixture of sodium carbonate (2 parts) and sodium peroxide (1 part) as in the test for Phosphorus. Extract the fused mass with water, filter, and acidify with dilute hydrochloric acid. Pass hydrogen sulphide through the hot solution arsenic is precipitated as yellow arsenic sulphide. If antimony is present, it will be precipitated as orange antimony trisulphide. 

To 68 g. (0.5 mole) of phenylacetic acid (Org. Syn. 2, 63) (Note 1) in a i-l. flask fitted with a reflux condenser and a system for absorbing hydrogen chloride (Org. Syn. 8, 27) (Note 2), is added 35 g. (0.25 mole) of phosphorus trichloride. The mixture is heated on a steam bath for one hour. While the contents of the flask are still warm, 400 cc. of dry benzene is added. The benzene solution of phenylacetyl chloride is decanted from the residue of phosphorous acid on 75 g. (0.56 mole) of anhydrous aluminum chloride in a dry, i-l. flask which can be fitted to the same condenser. The reaction is vigorous at first and cooling is necessary. The mixture is refluxed for one hour on a steam bath, then cooled and poured into a mixture of 500 g. of cracked ice and 200 g. of concentrated hydrochloric acid. The benzene layer is separated, and the aqueous layer is extracted once with a mixture of 100 cc. of benzene and 100 cc. of ether (Note 2). The ether-benzene solution is washed once with 100 cc. of water (Note 3), and then dried over 40-50 g. of calcium chloride. The solution is filtered (Note 4) with suction into a i-l. Claiscn flask and the solvent is removed by distillation under reduced pressure (Note 5) the residue consists of a brown oil which solidifies on cooling. 

Concentrated hydrochloric acid also dissolves the trichloride, about 100 g. of the latter dissolving in 1 litre of acid at 100° C.7 Dissolution in hydriodic acid is accompanied by evolution of heat and the triiodide is formed.8 Ethyl iodide reacts similarly.9 Double decomposition reactions occur w hen arsenic trichloride is heated with phosphorus triiodide, stannic iodide or germanium iodide, the reactions being complete.10 Similarly, potassium iodide heated with arsenic trichloride in a sealed tube at 210° C., and potassium bromide at 180° to 200° C., form respectively arsenic triiodide and tribromide.11 Stannous chloride, added to the solution in hydrochloric acid, causes reduction to arsenic (see p. 29). Arsenic trichloride may be completely separated from germanium chloride by extraction with concentrated hydrochloric acid.12 Ammonium, sodium and cobaltic chlorides react with arsenic trichloride to form additive compounds with magnesium, zinc and chromic chlorides there is no reaction.13... 

A solution of 1 part of a,a -diethyl-4,4 -dihydroxystilbene in 5 parts of pyridine is added drop by drop to the strongly cooled solution of 2 parts of phosphorus-hydroxy chloride in 5 parts of pyridine. The mixture soon solidifies to a crystalline magma. It is allowed to stand in ice for A hour and then for an hour at room temperature. The mass is then poured into an excess of saturated sodium bicarbonate solution. Unconsumed parent material is removed by extraction with ether. The aqueous solution is then mixed with 2 N hydrochloric acid, whereupon the primary phosphoric acid ester of a,a -diethyl-4,4 -dihydroxystilbene of the formula is precipitated in the form of a voluminous white powder. By recrystallization or reprecipitation this ester may be further purified. 

---