- Description:White to off white free flowing powder with a faint odor or is odorless
- Solubility : Transfer 0.01 gm of sample in a beaker and add 100 ml of water. Mix properly.It should be insoluble in water. Repeat the process for other common solvent like isopropyl alcohol and methylene dichloride.
3.0) Identification Test:
- A. Infrared Absorption (197K)
Triturate 1 to 2 mg of the substance (Dried at 1050C for 6 hrs) with the 0.3 gm to 0.4 gm of dried, finely powdered potassium bromide. These quantities are usually suitable for a discl3 mm in diameter and a spectrum of suitable intensity. Grind the mixture carefully, spread it uniformly in a suitable die and compress vacuum at a pressure of about 800 Mpa. Place the disc in disc holder and place the in FTIR. Measure the spectrum in the range of 400 to 4000 nm
- B. 1) Shake about l g with l0 ml of water: the aqueous phase does not produce white precipitate with sodium bitarlarate solulion (1 g in 10 ml of water).
2) Shake about 1 g with l0 ml of O.1N hydrochloric phase and the sodium- bitartrate TS (1 gm in l0 ml of water) produces a white crystalline precipitate that is soluble in 6N ammonium hydroxide and in solutions of alkali hydroxides and carbonates. The formation of the precipitates , which is usually slow, is accelerated by stirring or rubbing the inside of the test tube with a glass rod. The addition of a small amount of glacial acetic acetic acid or alcohol also promotes the precipitation.
4.0) Iron:
Standard Iron solution:
Dissolve 863.4 mg of ferric ammonium sulfate in water add l0 ml of 2 N sulfuric acid, and dilute with water to 100 ml. Pipet l0 ml of this solution into a 1000 ml volumetric flask, add l0 ml of 2N sulfuric acid, dilute with water to volume, and mix. This solution contains the equivalent of 0.01 mg (l0ug) of iron per ml.
Ammonium Thiocynate solution:
Dissolve 30 g of ammonium thiocynate in water to make 100 ml
Standard preparation:
Into a 50 ml color comparison tube pipet l mr of standard iron solution (10ug of Fe), dilute with water to 45 ml, add 2 ml of hydrochloric acid, and mix.
Test preparation:
Transfer 0.1 gm to a suitable crucible and ignite at a low heat until thoroughly ashed. Add to the carbonized mass 2 ml of nitric acid and 5 drops of sulfuric acid, and heat cautiously until white fumes are no longer evorved. Ignite, preferably in a muffle furnace, at 500oC to 600oC, until the carbon is completely burned off. Cool, add 4 ml of 6 n HCl, cover , digest on a steam bath for 15 min. Uncover and slowly evaporate on a steam bath to dryness. Moisten the residue with 1 drop of HCl. Add 10 ml of hot water , and digest for 2 min. dilute with water to about 25 ml. Filter if necessary , rinse the cruicle and the filter with 10 ml of water, combining the filtrate and rinsing in a 50 ml color comparison tube, add 2 ml of HCl, dilute with water to 45 ml and mix.
Procedure:
To each of the tubes containing the standard preparation and the test preparation add 50 mg of the ammonium peroxydisulfate crystals and 3 ml of ammonium thiocynate solution, and mix, the color of the solution from the test preparation is not darker than that of the solution from the standard solution.
5.0) Limit of Sodium
Test solution: Transfer about 2 gm, accurately weighed, to a 400 ml borosilicate beaker, add 20 ml of sulfuric acid, cover with a borosilicate watch glass, and heat until charring is complete. While continuing to heat the beaker, add 20 ml of nitric acid drop wise. Continue to heat and add nitric acid until all of the organic material has been destroyed as indicated by the content of the beaker turning from brown to a very pale straw coloured or colourless solution. Continue to evaporate the solution, and if it turns brown during the evaporation, add nitric acid drop wise until the brown colour disappears. Evaporate just to dryness, cool, and dissolve the residue in 40 ml of water and 10 ml of 6 N hydrochloric acid . Heat to boiling , cool, transfer to a 100 ml volumetric flask. Dilute with water to volume and mix.
Standard solution : To three separate 100 ml volumetric flask add, respectively , 1.00, 2.00 and 3.00 ml of a solution containing 254.2 mg of sodium chloride in 1000 ml of water. Add water to volume , and mix to obtain sodium chloride solutions having concentrations equivalent to 1,2 and 3 µg/ ml of Na , respectively.
Instrumental condition: Flame photometry
Analytical wavelength : 589 nm
Procedure : Adjust the settings of a suitable flame photometer so that determination of the solution containing 3µg/ml of the sodium solution reads close to 100 % at 589 nm. Determine the readings of the three solutions at 589 nm. Readjust the wavelength setting to 580 nm , and determine the background emission reading for one of these standard solutions. Pipet 5 ml of the sample solution into a 100 ml volumetric flasks, add water to volume, and mix. Observe the emission reading of this solution and 589 nm, using the same instrument settings, then readjust the wavelength setting to 580 nm, and observe the back ground emission readings. Prepare a standard curve by plotting the corrected standard readings versus the square root of the sodium concentration. From this standard curve, determine the sodium content of the test specimen. It is not greater than 0.20%
6.0) Powder Fineness
Transfer about 4 gm accurately weighed to a no. 100 standard sieve placed on top of a no. 200 standard sieve and pan. Using soft 2 cm brush, brush the sample lightly across the no. 100 sieve until no more particle pass through by brushing and tapping. Dust off the particles on the underside of the no. 100 sieve into the no. 200 sieve. Obtain the weight of the material retained on the no. 100 sieve. Similarly determine the weight of material retained by the no. 200 sieve.
7.0) Loss on Drying
Weight an appropriate glass- stoppered, shallow weighing bottle that has been dried for about 30 minutes under the same conditions to be employed in the determination ( at 1050C) and cooled to room temperature in a desiccators. Put the test specimen about 1 to 2 gm in the bottle, replace the cover, and accurately weigh the bottle and the contents. Place the loaded bottle in the drying chamber, removing the stopper and leaving it also in the chamber. Dry the test specimen at the temperature 1050C and for 6 hours in the monograph. Upon opening the chamber, close the bottle promptly, and allow it to come to room temperatuire in a desiccators before weighing . Weigh the bottle and the contents.
Weight of empty bottle : ………. gm
Weight of bottle + sample :………… gm
Weight of only sample :………..gm
After drying weight of bottle :………. gm
Weight of loss :………..gm
Calculation : Weight of loss X 100
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Weight of sample
