ASSAy Dissolve 0.250 g in water R and R and dilute to 100.0 ml with the same solvent. To 20.0 20.0 ml of the solution add 100 ml of water of water R , 20 ml of hydrochloric of hydrochloric acid R , 0.2 g of potassium of potassium bromide R and R and 0.05 ml of methyl red solution R . Titrate dropwise with 0.0167 M potassium bromate, bromate , shaking continuously, until the red colour disappears. 1 ml of 0.0167 of 0.0167 M potassium bromate is equivalent to 3.429 mg of C 6H7N3O.
Methyl Red Solution Dissolve 50 mg of methyl of methyl red in red in a mixture of 1.86 ml of 0.1M sodium hydroxide and 50 ml of ethanol (96%) and add sufficient water to produce 100 ml. Complies with the following test. Sensitivity A mixture of 0.1 ml of the solution, 100 ml of carbon dioxide-free water and 0.05 ml of 0.02 M hydrochloric acid VS is VS is red. Not more than 0.1 ml of 0.02 M sodium hydroxide VS is VS is required to change the colour of the solution to yellow. Colour change
pH 4.4 (red) to pH 6.0 (yellow).
Hydrochloric Acid VS
Hydrochloric Acid VS For a 0.1M solution
HCl = 36.46
Dilute 8.5 ml of hydrochloric of hydrochloric acid with acid with sufficient water to produce 1000 ml.
Ascertain its exact concentration concentration in the following following manner. Dissolve 0.1 g of anhydrous of anhydrous sodium carbonate in 20 ml of water , water , add 0.1 ml of methyl of methyl orange solution and titrate titrate with the hydrochloric hydrochloric acid until the solution becomes becomes reddish yellow. Boil for 2 minutes and continue the titration until the reddish yellow colour is restored. Each ml of 0.1M hydrochloric acid VS VS is is equivalent to 5.30 mg of Na2CO3. For a 1M solution
Dilute 103.0 g of hydrochloric of hydrochloric acid to acid to 1000 ml with water . water .
Ascertain its exact concentration as described for the 0.1 M solution using 1.000 g of anhydrous of anhydrous sodium carbonate dissolved in 50 ml of of water water .. Each ml of 1M hydrochloric hydrochloric acid VS is VS is equivalent to 53.00 mg of Na2CO3. For a 2 M M solution
Dilute 206.0 g of hydrochloric of hydrochloric acid to acid to 1000 ml with water . water .
For a 3M solution
Dilute 309.0 g of hydrochloric of hydrochloric acid to acid to 1000 ml with water . water .
For a 6 M M solution
Dilute 618.0 g of hydrochloric of hydrochloric acid to acid to 1000 ml with water . water .
Sodium Hydroxide VS
Sodium Hydroxide VS For a 0.1M solution produce 1000 ml.
NaOH = 40.00
Dissolve 4.2 g of sodium of sodium hydroxide in sufficient carbon dioxide-free water to
Ascertain its exact concentration immediately immediately before use in the following manner. manner. Titrate 20 ml of the solution with 0.1M hydrochloric acid VS VS using using the indicator indicator prescribed prescribed in the assay in which the the solution is to be used. Each ml of 0.1 M hydrochloric acid VS VS is is equivalent to 4.00 mg of NaOH. When a carbonate-free solution solution is specified it is prepared using the following method. method. Dissolve sodium hydroxide in an equal weight of water of water and allow to stand overnight. overnight. Taking precautions to avoid absorption of carbon dioxide, siphon off or decant the clear supernatant liquid and dilute with carbon dioxide-free water to the desired molarity. molarity. The solution complies with the following following test.
Titrate 20 ml of hydrochloric acid VS of the same molarity as the solution being examined with the sodium hydroxide solution using 0.5 ml of phenolphthalein solution as indicator. At the end point add just sufficient of the acid to discharge the pink colour and boil to reduce the volume to 20 ml. Add, whilst boiling, sufficient of the acid again to discharge the pink colour which does not reappear after prolonged boiling. Not more than 0.1 ml of the acid is required. For a 1M solution produce 1000 ml.
Dissolve 42 g of sodium hydroxide in sufficient carbon dioxide-free water to
Ascertain its exact concentration immediately before use in the following manner. Titrate 20 ml of the solution with 1M hydrochloric acid VS using the indicator prescribed in the assay in which the solution is to be used. Each ml of 1 M hydrochloric acid VS is equivalent to 40.00 mg of NaOH. When 0.1M sodium hydroxide VS is used in the assay of halide salts of organic bases, ascertain its exact concentration in the following manner. Dissolve 0.100 g of benzoic acid in a mixture of 5 ml of 0.01M hydrochloric acid and 50 ml of ethanol (96%). Titrate with the solution being examined and note the volume added between the two points of inflection. Each ml of 0.1 M sodium hydroxide VS is equivalent to 12.21 mg of C 7H6O.
Hydrochloric Acid
HCl = 36.46 (7647-01-0 )
Where no molarity is indicated use analytical reagent grade of commerce with a relative density of about 1.18, containing not less than 35% w/w and not more than 38% w/w of HCl and about 11.5 M in strength. A colourless, fuming liquid. Solutions of molarity x M should be prepared by diluting 85 x ml of hydrochloric acid to 1000 ml with water . Store in a container of polyethylene or other non-reacting material at a temperature not exceeding 30°.
Potassium Bromate
Potassium Bromate
KBrO3 = 167.0 (7758-01-2 )
Analytical reagent grade of commerce. White, granular powder or crystals.
Potassium Bromide
Potassium Bromide
KBr = 119.0 (7758-02-3)
Analytical reagent grade of commerce. Potassium bromide used for infrared absorption spectrophotometry complies with the following requirement. The infrared absorption spectrum, Appendix II A, of a disc 2 mm thick prepared from material previously dried at 250° for 1 hour has a substantially flat baseline over the range 4000 to 620 cm –1; it exhibits no maxima with an absorbance greater than 0.02 above the baseline with the exception of maxima due to water at 3440 and 1630 cm –1.
Merck index Absorption maximum: uv max (water): 266 nm (E1%1cm 378); (0.01N HCl): 265 nm (E1%1cm ~420) Toxicity data: LD50 in mice (mg/kg): 151 i.p., 149 i.v. (Jenney, Pfeiffer) Derivative Type: 4-Aminosalicylate CAS Registry Number: 2066-89-9 Additional Names: Pasiniazide Manufacturers' Codes: GEWO-399 Trademarks: Paraniazide (Hepatrol); Dipasic (Gewo) Molecular Formula: C13H14N4O4 Molecular Weight: 290.27. Percent Composition: C 53.79%, H 4.86%, N 19.30%, O 22.05% Literature References: An equimolecular salt produced by dissolving the components in hot dil alc, followed by cooling and evapn: Charonnat, Boime, Compt. Rend. 236, 2140 (1953). Prepn: CH 303085 (1955 to Hoffmann-La Roche). Properties: Yellow crystals from methanol or ethanol, mp 142-144°. Sparingly sol in water. uv max 272, 303 nm (E1%1cm 550, 445). Melting point: mp 142-144° Absorption maximum: uv max 272, 303 nm (E1%1cm 550, 445) Derivative Type: Methanesulfonate CAS Registry Number: 13447-95-5 CAS Name: 4-Pyridinecarboxylic acid 2-(sulfomethyl)hydrazide Additional Names: methaniazide Molecular Formula: C7H9N3O4S Molecular Weight: 231.23. Percent Composition: C 36.36%, H 3.92%, N 18.17%, O 27.68%, S 13.87% Literature References: Prepn: Logemann, US 2759944 (1956 to Carlo Erba). Properties: Crystals, dec 187-189°. Derivative Type: Methanesulfonate sodium CAS Registry Number: 3804-89-5 Additional Names: Sodium isonicotinylhydrazide methanesulfonate Trademarks: Neoiscotin (Daiichi) Molecular Formula: C7H8N3NaO4S Molecular Weight: 253.21. Percent Composition: C 33.20%, H 3.18%, N 16.60%, Na 9.08%, O 25.27%, S 12.66% Properties: Yellow crystals from water, dec 164-167°. Derivative Type: Methanesulfonate calcium CAS Registry Number: 6059-26-3 Trademarks: Neo-Tizide (Farmitalia Carlo Erba) Molecular Formula: C14H16CaN6O8S2 Molecular Weight: 500.52. Percent Composition: C 33.60%, H 3.22%, Ca 8.01%, N 16.79%, O 25.57%, S 12.81% Properties: Crystals, dec 215-220°. Therap-Cat: Antibacterial (tuberculostatic). Therap-Cat-Vet: Antibacterial (tuberculostatic); anti-actinomycotic agent.
