Precipitation forms

NH4)3Moi2PO40 H2O. The bright yellow precipitate formed from a phosphate, am monium molybdate and HNO3 in solution. Used as a test for phosphates. 

Mohr method Titration of Cl with Ag in the presence of added Cr04 ". A red precipitate forms at the end point. 

Nessler s reagent An alkaline solution of Hglj in KI used for detecting and estimating ammonia (brown colour or precipitate formed). 

To a few drops of formalin solution add a few drops of dinitro-phenylhydrazine reagent A (p. 263) a yellow precipitate is produced in the cold. Acetaldehyde and acetone give orange-coloured precipitates. Dissolve water-insoluble compounds e.g-y benzaldehyde, salicylalde-hyde, acetophenone and benzophenone) in a small volume of methanol before adding reagent B. With benzophenone the precipitate forms slowly. 

Reduction of ammoniacal silver nitrate. Place 2 ml. of dilute silver nitrate solution in a clean test-tube. Add 1 drop of NaOH solution and then add dil. ammonia drop by drop until the precipitate formed by the NaOH is just not redissolved. Now add 1-2 ml. of glucose solution and place the test-tube in a water-bath at 50-60° a silver mirror is produced in 1 - 2 minutes. 

Place about 1 g. of the nitro-hydrocarbon in a boiling-tube and add 5 ml. of cone. HCl and several pieces of granulated tin. Warm the mixture and shake continuously to break up the oily drops of the nitro-compound. When all the oil has disappeared (about 3 minutes heating) pour off the liquid from any undissolved tin into a 100 ml. conical flask. Cool and add cautiously 30% aqueous NaOH solution until the precipitate formed redissolves to give a dark-coloured solution. Cool the latter thoroughly and shake well with about 15 ml. of ether. Separate the ethereal layer in a separating-funnel, wash with water and evaporate the ether in a basin on a previously heated water-bath in a fume-cupboard atoay from all flames. The residue is either... 

In a 500 ml. wide-mouthed reagent bottle place a cold solution of 25 g. of sodium hydroxide in 250 ml. of water and 200 ml. of alcohol (1) equip the bottle with a mechanical stirrer and surround it with a bath of water. Maintain the temperature of the solution at 20-25°, stir vigorously and add one-half of a previously prepared mixture of 26-5 g. (25 -5 ml.) of purebenzaldehyde (Section IV,115) and 7 -3 g. (9-3 ml.) of A.R. acetone. A flocculent precipitate forms in 2-3 minutes. After 15 minutes add the remainder of the benzaldehyde - acetone mixture. Continue the stirring for a further 30 minutes. Filter at the pump and wash with cold water to eliminate the alkali as completely as possible. Dry the solid at room temperature upon filter paper to constant weight 27 g. of crude dibenzalacetone, m.p. 105-107°, are obtained. Recrystallise from hot ethyl acetate (2-5 ml. per gram) or from hot rectified spirit. The recovery of pure dibenzalacetone, m.p. 112°, is about 80 per cent. 

The acetonitrile and mercuric nitrate amounts remain the same except they are to be accompanied by 12.6g of fuming nitric acid (see chemicals section) in the reaction flask. Then, with cooling, the safrole or allylbenzene is added just like before. The reaction is immediate and takes no more than 20 minutes of stirring after which lOOmL ice cold dH20 is slowly added. Next, with vigorous stirring, saturated sodium chloride solution is slowly added until a pronounced precipitate forms. This yellowish mass is the chloride. 

Sodium metal (0.23 g, 10 mmol) was dissolved in abs. EtOH (30 ml), Gramine (1.74g, 10 mmol) and diethyl formamidoinalonate (2.03 g, 10 mmol) were added, followed by slow addition of dimethyl sulfate (2.52 g). The solution was allowed to stand at room temperature for 4h, during which a precipitate formed. The mixture was poured into water and the product collected by filtration (99% yield). 

The toluene solution from the previous step was treated with an ethanol solution of NaOEt (0.1 mol in 100 ml) at O C. When about a quarter of the solution had been added a thick precipitate formed and ether (100 ml) was added to maintain a fluid slurry. The remainder of the NaOEt was added and the slurry was stirred overnight. The solid was collected and w ashed with ether. It was then mixed with ether (200 ml) and 2NHC1 (75 ml) and shaken in a separatory funnel until the solid dissolved. The ether layer was washed with 2NHHC1 (2 X 50ml) and water and dried over MgS04. The solution was decolorized with Magnesol and evaporated to give the a-nitro ester as a red oil. 

Potassium hydride (1 eq.) was washed with hexanes and suspended in anhydrous ether at 0°C. 7-Bromoindole was added as a solution in ether. After 15 min, the solution was cooled to — 78°C and t-butyllithium (2 eq.) which had been precooled to — 78°C was added by cannula. A white precipitate formed. After 10 min DMF (2 eq.) was added as a solution in ether. The reaction mixture was allowed to warm slowly to room temperature and when reaction was complete (TLC) the suspension was poured into cold 1 M H3PO4. The product was extracted with EtOAc and the extract washed with sat. NaHCOj and dried (MgS04). The product was obtained by evaporation of the solvent and purified by chromatography on silica gel (61% yield). 

Treatment of phenol with excess aqueous bromine is actually more complicated than expected A white precipitate forms rapidly which on closer examination is not 2 4 6 tribro mophenol but is instead 2 4 4 6 tetrabromocyclohexadienone Explain the formation of this product... 

Solubility losses are minimized by carefully controlling the composition of the solution in which the precipitate forms. This, in turn, requires an understanding of the relevant equilibrium reactions affecting the precipitate s solubility. Eor example, Ag+ can be determined gravimetrically by adding Ch as a precipitant, forming a precipitate of AgCl. 

Another important parameter that may affect a precipitate s solubility is the pH of the solution in which the precipitate forms. For example, hydroxide precipitates, such as Fe(OH)3, are more soluble at lower pH levels at which the concentration of OH is small. The effect of pH on solubility is not limited to hydroxide precipitates, but also affects precipitates containing basic or acidic ions. The solubility of Ca3(P04)2 is pH-dependent because phosphate is a weak base. The following four reactions, therefore, govern the solubility of Ca3(P04)2. 

In some situations the rate at which a precipitate forms can be used to separate an analyte from a potential interferent. For example, due to similarities in their chemistry, a gravimetric analysis for Ca + may be adversely affected by the presence of Mg +. Precipitates of Ca(01T)2, however, form more rapidly than precipitates of Mg(01T)2. If Ca(01T)2 is filtered before Mg(01T)2 begins to precipitate, then a quantitative analysis for Ca + is feasible. 

An increase in the time required to form a visible precipitate under conditions of low RSS is a consequence of both a slow rate of nucleation and a steady decrease in RSS as the precipitate forms. One solution to the latter problem is to chemically generate the precipitant in solution as the product of a slow chemical reaction. This maintains the RSS at an effectively constant level. The precipitate initially forms under conditions of low RSS, leading to the nucleation of a limited number of particles. As additional precipitant is created, nucleation is eventually superseded by particle growth. This process is called homogeneous precipitation. ... 

Color Plate 5 shows the difference between a precipitate formed by direct precipitation and a precipitate formed by a homogeneous precipitation. 

The solution that remains after a precipitate forms. 

Analyte Precipitant Precipitate Formed Precipitate Weighed... 

The reaction of a positively charged polyelectrolyte with a negatively charged polyelectrolyte produces a precipitate, forming the basis for a precipitation titration. This paper provides an overview of colloid titrations, discussing... 

Fig. 20. A hoUow-fiber solution-spinning system. The fiber is spun into a coagulation bath, where the polymer spinning solution precipitates forming the...

Niobic Acid. Niobic acid, Nb20 XH2O, includes all hydrated forms of niobium pentoxide, where the degree of hydration depends on the method of preparation, age, etc. It is a white insoluble precipitate formed by acid hydrolysis of niobates that are prepared by alkaH pyrosulfate, carbonate, or hydroxide fusion base hydrolysis of niobium fluoride solutions or aqueous hydrolysis of chlorides or bromides. When it is formed in the presence of tannin, a volurninous red complex forms. Freshly precipitated niobic acid usually is coUoidal and is peptized by water washing, thus it is difficult to free from traces of electrolyte. Its properties vary with age and reactivity is noticeably diminished on standing for even a few days. It is soluble in concentrated hydrochloric and sulfuric acids but is reprecipitated on dilution and boiling and can be complexed when it is freshly made with oxaHc or tartaric acid. It is soluble in hydrofluoric acid of any concentration. 

Calcium carbonate, available both from natural sources and as precipitated forms (see Calcium compounds), is most useful in coating because of purity and high brightness, ie, 90—95%. Ground carbonates from marble deposits have high purity levels as do the carbonates from some chalk deposits. 

Analysis for Poly(Ethylene Oxide). Another special analytical method takes advantage of the fact that poly(ethylene oxide) forms a water-insoluble association compound with poly(acryhc acid). This reaction can be used in the analysis of the concentration of poly(ethylene oxide) in a dilute aqueous solution. Ereshly prepared poly(acryhc acid) is added to a solution of unknown poly(ethylene oxide) concentration. A precipitate forms, and its concentration can be measured turbidimetricaHy. Using appropriate caUbration standards, the precipitate concentration can then be converted to concentration of poly(ethylene oxide). The optimum resin concentration in the unknown sample is 0.2—0.4 ppm. Therefore, it is necessary to dilute more concentrated solutions to this range before analysis (97). Low concentrations of poly(ethylene oxide) in water may also be determined by viscometry (98) or by complexation with KI and then titration with Na2S202 (99). 

This PAG contains 1—2% sulfate as soluble calcium sulfate. Sulfate has been found to make PAG products unstable precipitate forms in less than one week at 50°G. Sulfate, however, has also been seen to increase PAG activity in water clarification and is thus intentionally added in one preparation (24). Precipitated calcium sulfate creates a sludge disposal problem. Typical Al content as AI2O2 of PAG products made from alum is 6 —8%. 

Silver Thiosulfate. Silver thiosulfate [23149-52-2], Ag 2 y is an insoluble precipitate formed when a soluble thiosulfate reacts with an excess of silver nitrate. In order to minimize the formation of silver sulfide, the silver ion can be complexed by haUdes before the addition of the thiosulfate solution. In the presence of excess thiosulfate, the very soluble Ag2(S203) 3 and Ag2(S203) 3 complexes form. These soluble thiosulfate complexes, which are very stable, are the basis of photographic fixers. Silver thiosulfate complexes are oxidized to form silver sulfide, sulfate, and elemental sulfur (see Thiosulfates). 

Tantalic Acid and Tantalates. Tantahc acid [75397-94-3] Ta20 is the name of the white insoluble precipitate formed by hydrolysis... 

In the field, cassiterite ore is usually recognized by its high density (7.04 g/cm ), low solubiUty in acid and alkaline solutions, and extreme hardness. Tin in solution is detected by the white precipitate formed with mercuric chloride. Stannous tin in solution gives a red precipitate with toluene-3,4-dithiol. 

Hydrolysis of solutions of Ti(IV) salts leads to precipitation of a hydrated titanium dioxide. The composition and properties of this product depend critically on the precipitation conditions, including the reactant concentration, temperature, pH, and choice of the salt (46—49). At room temperature, a voluminous and gelatinous precipitate forms. This has been referred to as orthotitanic acid [20338-08-3] and has been represented by the nominal formula Ti02 2H20 (Ti(OH). The gelatinous precipitate either redissolves or peptizes to a colloidal suspension ia dilute hydrochloric or nitric acids. If the suspension is boiled, or if precipitation is from hot solutions, a less-hydrated oxide forms. This has been referred to as metatitanic acid [12026-28-7] nominal formula Ti02 H2O (TiO(OH)2). The latter precipitate is more difficult to dissolve ia acid and is only soluble ia concentrated sulfuric acid or hydrofluoric acid. 

Identification. When a solution of ferric chloride is added to a cold, saturated vanillin solution, a blue color appears that changes to brown upon warming to 20°C for a few minutes. On cooling, a white to off-white precipitate (dehydrodivanillin) of silky needles is formed. Vanillin can also be identified by the white to slightly yellow precipitate formed by the addition of lead acetate to a cold aqueous solution of vanillin. 

The first report concerning barium compounds occurred in the early part of the seventeenth century when it was noted that the ignition of heavy spar gave a peculiar green light. A century later, Scheele reported that a precipitate formed when sulfuric acid was added to a solution of barium salts. The presence of natural barium carbonate, witherite [14941-39-0] BaCO, was noted in Scodand by Withering. 

In general, hydrated borates of heavy metals ate prepared by mixing aqueous solutions or suspensions of the metal oxides, sulfates, or halides and boric acid or alkali metal borates such as borax. The precipitates formed from basic solutions are often sparingly-soluble amorphous soHds having variable compositions. Crystalline products are generally obtained from slightly acidic solutions. 

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