Preparation Of 0.1N Perchloric Acid (in Glacial Acetic Acid)

Preparation Of 0.1N Perchloric Acid (in Glacial Acetic Acid)
Molecular Formula:  HClO4			Molecular weight: 100.46
Preparation	:	Mix 8.5 mL of perchloric acid with 500 mL of glacial acetic acid and 21 mL of acetic anhydride, cool, and add glacial acetic acid to make 1000 mL. Alternatively, the solution may be prepared as follows. Mix 11 mL of 60 percent perchloric acid with 500 mL of glacial acetic acid and 30 mL of acetic anhydride, cool, and add glacial acetic acid to make 1000 mL. Allow the prepared solution to stand for 1 day for the excess acetic anhydride to be combined
Standardization	:	Accurately weigh about 700 mg of potassium biphthalate, previously crushed lightly and dried at  120ºC for 2 hours, and dissolve it in 50 mL of glacial acetic acid in a 250-mL flask. Add 2 drops of crystal violet TS, and titrate with the perchloric acid solution until the violet color changes to blue- green. Deduct the volume of the perchloric acid consumed by 50 mL of the glacial acetic acid.   Each 20.42 mg of potassium biphthalate is equivalent to 1 mL of 0.1 N perchloric acid.     Preserve in glass-stoppered bottles, protected from light
Calculation	:	N = g KHC3H4O4 0.20423 X mL HClO4 Solution
Water Determination	:	Determine the water content by Method I (see Water Determination        921  ), except to use a test specimen of about 5 g of the 0.1 N perchloric acid that is expected to contain approximately 1 mg   of water and the Reagent (see Reagent under Method Ia in Water Determination   921  ) diluted such that 1 mL is equivalent to about 1 to 2 mg of water. If the water content exceeds 0.5%, add more acetic anhydride. If the solution contains no titratable water, add sufficient water to obtain a content of between 0.02% and 0.5% of water. Allow the solution to stand for 1 day, and again   titrate the water content. The solution so obtained contains between 0.02% and 0.5% of water, indicating freedom from acetic anhydride.
Reference	:	USP

 

0.1N Perchloric Acid

Preparation Of 0.1N Potassium Bromate

Preparation Of 0.1N Potassium Bromate
Molecular Formula:  KBrO3			Molecular weight: 167.00
Preparation	:	2.784 g in 1000 mL Dissolve 2.784 g of potassium bromate in water to make 1000 mL
Standardization	:	Transfer an accurately measured volume of about 40 mL of the solution to a glass-stoppered flask, add 3 g of potassium iodide, and follow with 3 mL of hydrochloric acid. Allow to stand for 5    minutes, then titrate the liberated iodine with 0.1 N sodium thiosulfate VS, adding 3 mL of starch TS as the endpoint is approached. Correct for a blank run on the same quantities of the same reagents, and calculate the normality.     Preserve in glass-stoppered bottles, protected from light
Calculation	:	N = ml Na2S2O3 x N Na2S2O3 mL KBrO3 Solution
Reference	:	USP

Preparation Of 0.1N Oxalic Acid

 

Preparation Of 0.1N Oxalic Acid
Molecular Formula:  H2C2O4·2H2O			Molecular weight: 126.07
Preparation	:	6.303 g in 1000 mL Dissolve 6.45 g of oxalic acid in water to make 1000 mL
Standardization	:	Standardize by titration against freshly standardized 0.1 N potassium permanganate VS as directed under Potassium Permanganate, Tenth-Normal (0.1 N).   Preserve in glass-stoppered bottles, protected from light
Calculation	:	M = ml KMnO4 x N KMnO4 mL H2C2O4·2H2O
Reference	:	USP

Preparation of 0.1M mercuric nitrate

Preparation of 0.1M mercuric nitrate
Molecular Formula:  Hg(NO3)2			Molecular weight: 324.60
Preparation	:	32.46 g in 1000 mL Dissolve about 35 g of mercuric nitrate in a mixture of 5 mL of nitric acid and 500 mL of water, and dilute with water to 1000 mL.
Standardization	:	Transfer an accurately measured volume of about 20 mL of the solution to a conical flask, and add 2 mL of nitric acid and 2 mL of ferric ammonium sulfate TS. Cool to below 20 , and titrate with 0.1  N ammonium thiocyanate VS to the first appearance of a permanent brownish color.
Calculation	:	M = ml NH4SCN x N NH4SCN mL Hg(NO3)2
Reference	:	USP

 

Preparation of 1.0 N or normal Hydrochloric Acid solution

Preparation of 1.0 N or normal Hydrochloric Acid solution

Description		Hydrochloric Acid, Normal (1.0 N)
Molecular Formula	:	HCl	Molecular weight: 36.46
Instrument List	:	Balance, Volumetric flask 1000ml
Reagent	:	Hydrochloric Acid , water
Procedure	:	Dilute 85 mL of hydrochloric acid with water to 1000 mL
Standardization	:	Accurately weigh about 5.0 g of tromethamine, previously dried at 105 for 3 hours. Dissolve in 50 mL of water, and add 2 drops of bromocresol green TS. Titrate with 1 N hydrochloric acid to a pale yellow endpoint. Each 121.14 mg of tromethamine is equivalent to 1 mL of 1 N hydrochloric acid.
Calculation	:	N = Mg tromethamine 121.14 x ml HCl

  

Preparation of 0.05 N or Twentieth-Normal of Ceric Ammonium Nitrate solution

Preparation of 0.05 N or Twentieth-Normal of Ceric Ammonium Nitrate solution

Description	:	Ceric Ammonium Nitrate, Twentieth-Normal (0.05 N)
Molecular Formula	:	Ce(NO3)4·2NH4NO3	Molecular weight: 548.22
Instrument List	:	Balance, Beaker 1000ml, Filter paper
Reagent	:	ceric ammonium nitrate, Nitric acid
Procedure	:	Dissolve 2.741 g of ceric ammonium nitrate in 1 N nitric acid to obtain 100 mL of solution, and filter
Standardize	:	Accurately measure 10 mL of freshly standardized 0.1 N ferrous ammonium sulfate VS into a   flask, and dilute with water to about 100 mL. Add 1 drop of nitrophenanthroline TS, and titrate with the ceric ammonium nitrate solution to a colorless endpoint.

Preparation of 2.0 N or Double-normal acetic acid solution

Preparation of 2.0 N or Double-normal acetic acid solution

Molecular Formula	:	C2H4O2	Molecular weight: 60.05
Instrument List	:	Balance, Beaker 1000ml
Reagent	:	Glacial acetic acid, Water
Procedure	:	120.10 g glacial acetic acid into in a 1000 mL of Beaker. Add 116 mL of glacial acetic acid to sufficient water to make 1000 mL after cooling to room temperature
Reference	:	USP

 

Preparation of 0.1M Potassium Dichromate

 

Preparation of 0.1M Potassium Dichromate
Molecular Formula:  K2Cr2O7			Molecular weight: 294.18
Preparation	:	Dissolve 4.903 g of Potassium Dichromate transfer into a 1000ml volumetric flask then volume up to 1000 ml with Deionize water.
Standardization	:	·         Transfer 25.0 mL of this solution to a glass-stoppered into a 500-mL flask ·         add 2 g of potassium iodide (free from iodate) ·         dilute with 200 mL of water, ·         add 5 mL of hydrochloric acid, ·         allow to stand for 10 minutes in a dark place ·         adding 3 mL of starch TS as the endpoint is approached ·         titrate the liberated iodine with 0.1 N sodium thiosulfate VS ·         Carry out a blank determination.
Calculation	:	N = ml Na2S2O3 x N Na2S2O3 25.0
Reference	:	USP