Vacuum filtration, water

After 3 hours the stirring is stopped and the solution allowed to settle. By this time just about all the foil will have turned to dust, which is going to make the next step of vacuum filtration very difficult because it will plug up the filter paper in a second. So the chemist lets it settle, then pours off the liquid through the vacuum filtration setup (see methodology section). The flask is rinsed with lOOmL methanol, the methanol poured through the grey filter cake and the filter cake discarded. All of the filtrate is placed in a flask and vacuum distilled to remove all the methanol, isopropyl alcohol and water which will leave the chemist with oil and junk in the bottom of the flask. 

METHOD 2 [128, 129]--To make dibromodioxane one stirs 500g dioxane in a flask which is in an ice bath, all of which is in the hood. 990g of liquid Bra is rapidly added, causing the solution to get hot (one can also bubble in an approximate amount of bromine from a gas canister). The solution is dumped into a bucket containing 2L of ice water, causing the immediate formation of a large mass of orange dibromodioxane crystals which are separated by vacuum filtration and dried. 

The ammonium sulfate and sodium chloride are simultaneously dissolved, preferably ia a heel of ammonium chloride solution. The sodium chloride is typically ia excess of about 5%. The pasty mixture is kept hot and agitated vigorously. When the mixture is separated by vacuum filtration, the filter and all connections are heated to avoid cmst formation. The crystalline sodium sulfate is washed to remove essentially all of the ammonium chloride and the washings recycled to the process. The ammonium chloride filtrate is transferred to acid resistant crystallising pans, concentrated, and cooled to effect crystallisation. The crystalline NH Cl is washed with water to remove sulfate and dried to yield a product of high purity. No attempt is made to recover ammonium chloride remaining ia solution. The mother Hquor remaining after crystallisation is reused as a heel. 

Subsequently, the reaction mixture was stirred for 5 hours on an ice bath and was then allowed to stand overnight at -2°C. Thereafter, the reaction solution was admixed with water, the precipitate formed thereby was separated by vacuum-filtration, the filtrate was admixed with more water, and the aqueous solution was acidified with 2N hydrochloric acid. A greasy substance precipitated out which crystallized after a brief period of contact with boiling methanol. 2.6 grams (85% of theory) of 1,2,3,4-tetrahydro-2-[p-(N -cyclo-... 

The filtrate was adjusted to a pH of 9 by adding concentrated ammonia, and than a 1 N aqueous iodine-potassium iodide solution was added dropwise, whereby the tetrahydro-pyrimido-[5,4-d] pyrimidine obtained by hydrogenation with zinc in formic acid was converted by oxidation into 2,6-bis-(diethanolamino)-8-piperidino-pyrimido-[5/4-d]-pyrimidine. The completion of the oxidation was checked by means of a starch solution. The major amount of the oxidation product already separated out as a deep yellow crystalline precipitate during the addition of the iodine solution. After the oxidation reaction was complete, the reaction mixture was allowed to stand for a short period of time, and than the precipitate was separated by vacuum filtration, washed with water and dried. It had a malting point of 157°C to 158°C. The yield was 8.0 g, which corresponds to 95% theory. 

Cultures of G. polyedra (L. polyedrum) are grown at 20 5°C in a supplemented sea water medium (Hastings and Sweeney, 1957 Hastings and Dunlap, 1986), under cool-white fluorescent lighting of a 12-hr light/12-hr dark cycle. The cultures are inoculated at densities of 100 to 500 cells/ml. After 2-4 weeks, cells are harvested by vacuum filtration on a filter paper at cell densities of 7,000-15,000 cells/ml, yielding 0.3-0.7 g wet cells per liter of culture. 

Prepn. Dissolve 2.4g of Pb nitrate in 50ml w at 90—95°, and add with stirring a coned soln of Na benzoate (prepd by neutralizing 2g of benzoic acid with 0.6g NaOH). Evaporate the mixt on a w bath to a small vol while the liq still remains clear. Cool and add 50ml of 95% ethanol. This results in a very fine, light yel ppt, which is separated by vacuum filtration. After drying at 50°, analysis gave 41.82% Pb and 3.40% water... 

The precipitate is collected on filter paper (Note 7) in a Buchner funnel by vacuum filtration and is washed with 100 ml. of absolute ethanol. The solid is slurried in three 75-ml. portions of distilled water (Note 8), 100 ml. of absolute ethanol, two 100-ml. portions of reagent-grade acetone, and two 100-ml. portions of anhydrous ethyl ether. The filter cake is pressed dry in the funnel with suction by means of a piece of rubber dam, transferred to a tared, 500-ml., round-bottomed flask, and dried under reduced pressure (0.01 mm.) at room temperature for 24 hours (Note 9). The weight of the dry silver salt of succinimide is 51-54 g. (88-94%). 

Filter IL of water sample through a filter paper. Place an Empore extraction disk in a Millipore extraction funnel. Rinse the disk with 10 mL of ethyl acetate, dichloromethane, and acetonitrile, successively. Dry the disk under vacuum and then rinse the disk with 10 mL of methanol and 20 mL of deionized water by vacuum filtration. Pass the prefiltered sample through the disk and elute alanycarb with two portions of 10 mL of acetonitrile. Transfer the eluates through anhydrous sodium sulfate into a 50-mL flask. Remove acetonitrile by rotary evaporation. Dissolve the residue in 1 mL of acetonitrile. 

Shipboard analysis for the sampling of trace metals in seawater has been discussed by Schuessler and Kremling [2] and Dunn et al. [3]. Teasdale et al. have reviewed methods for collection of sediment pore-waters using in situ dialysis samples [4]. Bufflap and Allen [5] compared centrifugation, squeezing, vacuum filtration, and dialysis methods for sediment pore-water sampling. 

Sometimes you ll need a vacuum for special work like vacuum distillation and vacuum filtration as with the Buchner funnel. An inexpensive source of vacuum is the water aspirator (Fig. 47). 

Every year I run a chem lab and when someone is doing a vacuum filtration, suddenly I ll hear a scream and a moan of anguish, as water backs up into someone s filtration system. Usually there s not much damage, since the filtrate in the suction flask is generally thrown out. For vacuum distillations, however, this suck-back is disaster. It happens whenever there s a pressure drop on the water line big enough to cause the flow to decrease so that there is a greater vacuum in the system than in the aspirator. Water, being water, flows into the system. Disaster. 

Pressure driven membrane process, 78 507 Pressure-driven membranes, in water treatment, 26 111 Pressure drop, 77 804 from area change, 73 261-262 in cake filtration, 77 330-332, 333-335 flow maldistribution and, 73 270 from flow turning, 73 262 frictional, 73 260-261 in gas adsorption, 7 657-658 in hyperbar vacuum filtration, 77 377 shellside tube bundle, 73 262-263 in vacuum filtration, 77 349-350 Pressure drop calculations, in heat exchanger design, 73 259-260 Pressure drop information, for resins, 74 399... 

One place where soil solution from saturated soils is routinely used is in the determination of salts in soil. Salts can build up in soil in low-rainfall areas. A measure of the salt content is essential for these soils. Typically, a saturated paste of soil is made and the water filtered by vacuum filtration. The filtrate can then be analyzed for electrical conductivity and this measurement, together with calcium, magnesium, and sodium content, can be used to calculate various measures of salt content and potential detrimental effects of salts on crops and water quality. 

C. (R,R)-N,N -Bis(3,5-di-tert-butylsalicylidene)-1,2-cyclohexanediamine. A 2-L, three-necked, round-bottomed flask equipped with a mechanical overhead stirrer, reflux condenser, and an addition funnel is charged with 29.7 g of (R,R)-1,2-diammoniumcyclohexane mono-(+)-tartrate salt (0.112 mol), 31.2 g of potassium carbonate (0.225 mol, 2 eq), and 150 mL of water. The mixture is stirred until dissolution is achieved, and 600 mL of ethanol is added. The cloudy mixture is heated to reflux with a heating mantle and a solution of 53.7 g (0.229 mol, 2.0 eq) of 3,5-di-tert-butylsalicylaldehyde in 250 mL of ethanol is then added in a slow stream over 30 min (Note 19). The addition funnel is rinsed with 50 mL of ethanol and the mixture is stirred at reflux for 2 hr before heating is discontinued. Water, 150 mL, is added and the stirred mixture is cooled to <5°C over 2 hr and maintained at that temperature for another hour. The yellow solid is collected by vacuum filtration and washed with 100 mL of ethanol. After the solid is air dried, it is dissolved in 500 mL of methylene chloride. The organic solution is washed with 2 x 300 mL of water, followed by 300 mL of saturated aqueous sodium chloride. The organic layer is dried over sodium sulfate, and filtered to remove the drying agent. The solvent is removed by rotary evaporation to yield the product as a yellow solid, mp 200-203°C (Notes 20 and 21). 

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