SOP for Preparation and Standardization of Volumetric Solutions

The records of preparation and standardization details of volumetric solutions shall be maintained as per (Logbook Format). The volumetric solution bottles shall be labeled as per SOP for Labeling Policy.

The control no. shall be given to all volumetric solutions as VSXX-YYY, where VS stand for the volumetric solution, XX is code no. of volumetric solution and YYY is serial no. of volumetric solution Preparations and standardization of the various volumetric solutions are given below: Standardize the Volumetric Solutions in Triplicate set against the Primary Standard, chemical, equimolar/ Equi- normal solution as applicable.

The average of all three results will be treated as the actual strength of the solution. The individual value will be taken up to the 4^th decimal place and the mean of all three values will be taken up to the 3^rd decimal place.

{tocify} $title={Table of Contents}

AMMONIUM THIOCYANATE (0.1M)

(Code No. VS01)

PREPARATION

Weigh accurately 7.612gm of ammonium thiocyanate in a 1000 ml volumetric flask and add sufficient water to dissolve properly and dilute to 1000 ml with water. Standardize the solution in the following manner.

Zinc Nitrate Formula, Properties and Uses

STANDARDIZATION (TRIPLICATE)

Pipette 30 ml of 0.1 M silver nitrate standard solution in a glass stoppered flask and dilute with water to 50 ml, add 2 ml of nitric acid and 2 ml of ferric ammonium sulphate solution and titrate with 0.1M ammonium thiocyanate solution to the first appearance of a red-brown colour.

Calculation

Volume taken of 0.1Msilver nitrate (ml) x Molarity of 0.1Msilver nitrate

Molarity = --------------------------------------------------

Volume consumed (ml) of 0.1 M ammonium thiocyanate

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD^* of the triplicate results of standardization / re-standardization should not more

than 0.2 %

Reference In-House

Frequency

Preparation 1 Months

Standardization Initially after preparation

Re-standardization After 15 days

Storage conditions Store the solution in a well-stoppered glass bottle at ambient

temperature

Precautions (if any) None specific

BENZETHONIUM CHLORIDE (0.004 M)

(Code No. VS02)

PREPARATION

Weigh accurately 1.792gm of benzethonium chloride (dried to constant weight at 105˚C) in a 1000 ml volumetric flask and add sufficient water to dissolve properly and dilute to 1000 ml with water. Standardize the solution in the following manner.

STANDARDIZATION (TRIPLICATE)

Dissolve 0.35 gm of the dried substance (benzethonium chloride) in 30 ml of anhydrous glacial acetic acid, add 6ml of mercuric acetate solution and carry out the non-aqueous titration (appendix 3.45, IP), using 0.05 ml of crystal violet solution as indicator. Perform a blank determination and any necessary correction.

Each ml of 0.1M perchloric acid is equivalent to 0.04481gm of C₂₇H₄₂ClNO₂

Calculation

Molarity : (W) x (P)

---------------------

(W1) x 100

Where W = Actual Weight of benzethonium chloride used for preparing Volumetric Solution

W1= Molecular Weight of benzethonium chloride

P = Potency of benzethonium chloride

The potency of benzethonium Chloride (P): Vol. of HClO₄ x Molarity of HClO₄ ×100 × 44.81

----------------------------------------------------------------------

Weight of benzethonium Chloride × 0.1

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization / re-standardization should not be more than 0.2 %.

Reference I P/In-House (IP 2007, Vol. I, Page No. 548)

Frequency

Preparation 1 Month

Standardization Initially after preparation

Re-standardization After 15 days

Storage conditions Store the solution in a well-stoppered glass bottle at ambient temperature

Precautions (if any) None specific

CERRIC AMMONIUM SULPHATE (0.1M)

(Code No. VS03)

PREPARATION

Dissolve 65.0 gm of cerric ammonium sulphate with the aid of gentle/heat, in a mixture of 30 ml. of sulphuric acid and 500 ml. of water. Cool, filter the solution, if turbid, and dilute to 1000 ml with water. Standardize the solution in the following manner.

STANDARDISATION (TRIPLICATE)

Weigh accurately about 0.2 gm. of arsenic trioxide, previously dried at 105ºC for 1 hour, and transfer to a 500 ml. conical flask washes the inner walls of the flask with 25 ml. of an 8.0% w/v solution of sodium hydroxide, swirl to dissolve, add 100 ml. of water and mix. Add 30 ml. of dilute sulphuric acid, 0.15 ml. of osmic acid solution, 0.1 ml of ferroin sulphate solution and slowly titrate with 0.1M cerric ammonium sulphate solution until the pink colour is changed to a very pale blue, adding the titrant slowly towards the end-point.

Each 1ml of 0.1M ferric ammonium sulphate is equivalent to 0.004946 gm of As₂O_3.

Calculation

Wt. of arsenic trioxide (mg) x Potency of arsenic trioxide × 0.1

Molarity = ---------------------------------------------

Volume consumed (ml) x 4.946 x 100

Osmic acid solution

1 % w/v solution of osmic acid in water.

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/ re-standardization should not be more than 0.2%.

Reference I.P./In-House (IP 2007, Vol. I, Page No. 549)

Frequency :

Preparation 01 Month

Standardization Initially after preparation

Re- standardization After15 days

DISODIUM EDETATE (0.1M)

(Code No. VS04)

PREPARATION

Weigh accurately 37.2 g of disodium edetate in a 1000 ml volumetric flask and add sufficient water to dissolve properly and dilute to 1000 ml with water. Standardize the solution in the following manner.

STANDARDIZATION (TRIPLICATE)

Weigh accurately 0.2 g of calcium carbonate, previously dried at 110°C for 2 hours and cooled in a desiccator and transferred in a 250 ml conical flask and add 10 ml of water, and swirl to form a slurry. Cover the flask with a watch glass and introduce 2 ml of dilute hydrochloric acid from a pipette. Swirl the content of the flask to dissolve the calcium carbonate properly. Wash down the sides of the flask, the outer surface of the pipette and the watch glass with water to dilute 100 ml. Add 30 ml of disodium edetate solution from a 50 ml burette 15 ml of 1 M sodium hydroxide solution and 300 mg of hydroxy naphthol blue, and continue the titration with 0.1M disodium edetate solution to a blue endpoint.

Every 1 ml of 0.1M disodium edetate is equivalent to 0.010009gm of CaCO₃

Calculation

Wt. of Calcium Carbonate (mg) x Potency of CaCO₃ × 0.1

Molarity = -------------------------------------------

Volume consumed (ml) x 10.009 × 100

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10 % of the theoretical concentration.

2) RSD* of the triplicate results of standardization/ re-standardization should not be more than

0.2 %.

Reference IP/In-House (IP 2007, Vol. I, Page No. 549)

Frequency

Preparation 1 Month

Standardization Initially after preparation

Re- standardization After15 days

Storage conditions Store the solution in a well-stoppered glass bottle at ambient

temperature.

Precautions (if any) Non specific

DISODIUM EDETATE (0.05 M)

(Code No. VS05)

PREPARATION

Weigh accurately 18.6 gm of disodium edetate in a 1000 ml volumetric flask and add sufficient water to dissolve properly and dilute to 1000 ml with water. Standardize the solution in the following manner.

STANDARDISATION (TRIPLICATE)

Weigh accurately 0.2 g of calcium carbonate, previously dried at 110°C for 2 hours and cooled in a desiccator and transfer in a 250 ml conical flask and add 10 ml of water, and swirl to form a slurry. Cover the flask with a watch glass and introduce 2 ml of dilute hydrochloric acid from a pipette. Swirl the content of the flask to dissolve the calcium carbonate properly. Wash down the sides of the flask, the outer surface of the pipette and the watch glass with water to dilute 100 ml. Add 15 ml of disodium edetate solution from a 50 ml burette and 15 ml of 1 M sodium hydroxide solution and 300 mg hydroxyl naphthol blue, and continue the titration with 0.05M disodium edetate solution to a blue endpoint.

Each 1 ml of 0.05M disodium edetate is equivalent to 0.0050045gm of CaCO₃

Calculation

Wt. of Calcium Carbonate (mg) x Potency of CaCO₃× 0.05

Molarity = --------------------------------------

Volume consumed (ml) x 5.0045 × 100

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization / re-standardization should not more

than 0.2 %.

Reference In-House

Frequency

Preparation 1 Month

Standardization Initially after preparation

Re- standardization After 15 days

Storage conditions Store the solution in a well-stoppered glass bottle at ambient

temperature.

Precautions (if any) None specific

FERROUS AMMONIUM SULPHATE (0.1 M)

(Code No. VS06)

PREPARATION

Dissolve 40.0 gm of ferrous ammonium sulphate in a previously cooled mixture of 40 ml. of sulphuric acid and 200 ml. of water, dilute with sufficient boiled and cooled water to produce1000 ml. Standardize the solution in the following manner

STANDARDIZATION (TRIPLICATE)

Measure accurately 25.0 ml. of solution into a flask, add 2 drops of 1,10-phenanthroline solution and titrate with 0.1M ferric ammonium sulphate until the red colour changed to pale blue.

Calculation

M2 x V2

Molarity = ----------------------

Where M2 = molarity of 0.1M ferric ammonium sulphate solution.

V2 = volume of 0.1 M ferric ammonium sulphate consumed in

V1 = volume of 0.1 M ferrous ammonium sulphate taken in ml.

1,10-phenanthroline

Dissolve 1.5 gm. Of 1,10-phenanthroline in sufficient water to produce 100 ml.

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/ re-standardization should not be more

than 0.2%.

Reference I.P./In-House (IP 2007, Vol. I, Page No. 549)

Frequency :

Preparation 01 Month

Standardization Initially after preparation

Re- standardization After 15 days

Storage conditions Store the solution in a light-resistant container at ambient temperature

Precautions (if any) None specific

HYDROCHLORIC ACID (1M)

(Code No. VS07)

PREPARATION

Dilute 85 ml. of hydrochloric acid with water to produce 1000 ml. Standardize the solution in the following manner.

STANDARDISATION (TRIPLICATE)

Weigh accurately about 1.5 gm. of anhydrous sodium carbonate, previously dried at about 270°C for 1 hour. Dissolve it in 100 ml. of water and add 0.1ml. of methyl red solution. Add the acid slowly from a burette, with constant stirring, until the solution becomes faintly pink. Heat the solution to boiling, cool and continue the titration. Heat again to boiling and titrate further as necessary until the faint pink colour is no longer affected by continued boiling.

Every 1 ml of 1M hydrochloric acid is equivalent to 0.05299gm of Na₂CO₃

Calculation

Wt. of sodium carbonate (mg) x Potency of Na₂Co₃× 1

Molarity = ---------------------------------

Volume consumed (ml) x 52.99 × 100

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/ re-standardization should not be more than 0.2%.

Reference I.P./In- House (IP 2007, Vol. I, Page No. 550)

Frequency :

Preparation 01Month

Standardization Initially after preparation

Re- standardization After 15 days

Storage conditions Store the solution in a stoppered glass bottle at ambient

temperature

Precautions (if any) 1) Handle with care under the fuming cupboard.

2) Wear hand gloves & nose mask during preparation

3) Never add water to the acid.

HYDROCHLORIC ACID (0.5 M)

(Code No. VS08)

PREPARATION

Dilute 42.5 ml. of hydrochloric acid with water to produce 1000 ml. Standardize the solution in the following manner.

STANDARDIZATION (TRIPLICATE)

Weigh accurately 0.750 gm. of anhydrous sodium carbonate, previously dried at about 270°C for 1 hour. Dissolve it in 100 ml. of water and add 0.1ml. of methyl red solution. Add the acid slowly from a burette, with constant stirring, until the solution becomes faintly pink. Heat the solution to boiling, cool and continue the titration. Heat again to boiling and titrate further as necessary until the faint pink colour is no longer affected by continued boiling.

Each 1 ml of 0.5M hydrochloric acid is equivalent to 0.026495gm of Na₂CO₃

Calculation

Wt. sodium carbonate (mg) x Potency of Na₂Co₃× 0.5

Molarity = ------------------------------------

Volume consumed (ml) x 26.495 × 100

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/ re-standardization should not be more

than 0.2%.

Reference In-House

Frequency:

Preparation 01 Month

Standardization Initially after preparation

Re- standardization After 15 days

Storage conditions Store the solution in a stoppered glass bottle at ambient temperature.

Precautions (if any) 1) Handle with care under the fuming cupboard.

2) Wear hand gloves & nose mask during preparation

3) Never add water to the acid.

HYDROCHLORIC ACID (0.1M)

(Code No. VS09)

PREPARATION

Dilute 8.5 ml. of hydrochloric acid with water to produce 1000 ml. Standardize the solution in the following manner.

STANDARDISATION (TRIPLICATE)

Weigh accurately 0.150 gm of anhydrous sodium carbonate previously dried at about 270°C for 1 hour. Dissolve it in 100 ml. of water and add 0.1ml.of methyl red solution. Add the acid slowly from a burette, with constant stirring, until the solution becomes faintly pink. Heat the solution to boiling, cool and continue the titration, heat again to boiling and titrate further as necessary until the faint pink colour is no longer affected by continued boiling.

Each 1 ml of 0.1M hydrochloric acid is equivalent to 0.005299gm of Na₂CO₃

Calculation

Wt. of sodium carbonate (mg) x Potency of Na₂Co₃ × 0.1

Molarity = -----------------------------------------

Volume consumed (ml) x 5.299 × 100

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/re-standardization should not be more

than 0.2%.

Reference In-House

Frequency :

Preparation 01 Months

Standardization Initially after preparation

Re- standardization After15 days

Storage conditions Store the solution in a stoppered glass bottle at ambient temperature

Precautions (if any) 1) Handle with care under a fuming cupboard.

2) Wear hand gloves & nose mask during preparation

3) Never add water to the acid.

HYDROCHLORIC ACID (0.02M)

(Code No. VS10)

PREPARATION

Dilute 1.7 ml. of hydrochloric acid with water to produce 1000 ml. Standardize the solution in the following manner.

STANDARDISATION (TRIPLICATE)

Weigh accurately 0.030 gm. of anhydrous sodium carbonate previous heated at about 270°C for 1 hour. Dissolve it in 100 ml. of water and add 0.1ml.of methyl red solution. Add the acid slowly from a burette, with constant stirring, until the solution becomes faintly pink. Heat the solution to boiling, cool and continue the titration. Heat again to boiling and titrate further as necessary until the faint pink colour is no longer affected by continued boiling.

Every 1 ml of 0.02M hydrochloric acid is equivalent to 0.0010598gm of Na₂CO₃

Calculation

Wt. of sodium carbonate (mg) x Purity of Na₂Co₃× 0.02

Molarity = --------------------------------

Volume consumed (ml) x 1.0598 × 100

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/re-standardization should not be more

than 0.2%.

Reference In-House

Frequency :

Preparation 01 Month

Standardization Initially after preparation

Re- standardization After 15 days

Storage conditions Store the solution in a stoppered glass bottle at ambient

temperature

Precautions (if any) 1) Handle with care under the fuming cupboard.

2) Wear hand gloves & nose mask during preparation

3) Never add water to the acid.

IODINE (0.05 M)

(Code No. VS11)

PREPARATION

Dissolve 14 gm of iodine in a solution of 36 gm of potassium iodide in 100 ml of water, add 3 drops of hydrochloric acid and dilute with water to 1000 ml. Standardize the solution in the following manner.

STANDARDISATION (TRIPLICATE)

Weigh accurately 0.150 gm of arsenic trioxide previously dried at 105⁰C for 1 hour and cooled in desiccators, dissolve in 20 ml of 1 M sodium hydroxide by warming (if necessary ) dilute with 40 ml of water, add 0.1 ml of methyl orange solution and add dropwise dilute hydrochloric acid until the yellow colour is changed to pink. Add 2 gm of sodium carbonate dilute with 50 ml of water and add 3 ml of starch solution. Titrate with 0.05M iodine solution until a permanent blue colour is produced.

Each 1ml of 0.05M iodine is equivalent to 0.004946gm of As₂O₃.

Calculation

Wt. of Arsenic trioxide (mg) x Potency of Arsenic trioxide × 0.05

Molarity = ---------------------------------------

Volume Consumed (ml) x 4.946 × 100

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/ re-standardization should not be more

than 0.2%.

Reference I.P./In-House (IP 2007, Vol. I, Page No. 550)

Frequency :

Preparation 01 Months

Standardization Initially after preparation

Re- standardization After15 days

Storage conditions Store the solution in well stoppered light-resistant amber

coloured glass bottle.

Precautions (if any) 1) Handle with care.

2) Use hand gloves and a nose mask during preparation

MERCURIC NITRATE (0.02M)

(Code No. VS12)

PREPARATION

Dissolve 6.85 gm of mercuric nitrate in 20 ml of 1M nitric acid and add sufficient water to produce 1000 ml. Standardize the solution in the following manner.

STANDARDISATION (TRIPLICATE)

Dissolve 15 mg of sodium chloride in 50ml of water and titrate with the 0.02M mercuric nitrate solution determining the end-point potentiometrically using a platinum or mercury mercurous sulphate reference electrode.

Each 1 ml of 0.02M mercuric nitrate is equivalent to 0.002338gm of NaCl.

Calculation

Wt. of sodium chloride (mg) x Potency of sodium chloride× 0.02

Molarity = ---------------------------------

Volume Consumed (ml) x 2.338 × 100

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/ re-standardization should not be more

than 0.2%.

Reference I.P./In-House (IP 2007, Vol. I, Page No. 550)

Frequency

Preparation 01 Months

Standardization Initially after preparation

Re- standardization After 15 days

Storage conditions ore the solution in a well stoppered light-resistant amber coloured glass bottle.

Precautions (if any) None Specific

PERCHLORIC ACID (0.1M)

(Code No. VS13)

PREPARATION

Mix 8.5 ml. of perchloric acid with 500 ml. of anhydrous glacial acetic acid and 25 ml. of acetic anhydride, cool and add anhydrous glacial acetic acid to produce 1000 ml. Allow the prepared solution to stand for 1 day for the excess acetic anhydride to be combined and carry out the determination of water. If the water content exceeds 0.05%, add more acetic anhydride. If the solution contains no titrable water, add sufficient water to obtain a content of water between 0.02% and 0.05%. Allow the solution to stand for one day and again titrate the water content. The solution so obtained should contain between 0.02% and 0.05% of water. Standardize the solution in the following manner.

STANDARDISATION (TRIPLICATE)

Weigh accurately about 0.350 gm. of potassium hydrogen phthalate (KHP) previously dried at 120°C for 2 hours and dissolve it in 50 ml. of anhydrous glacial acetic acid add 0.1ml crystal violet solution as an indicator and titrate with the 0.1M perchloric acid solution until the violet colour changes to emerald-green. Perform a blank determination and make any necessary corrections.

Each 1ml of 0.1M perchloric acid is equivalent to 0.02042gm of C₈H₅KO₄

Calculation

Wt. of potassium hydrogen phthalate (mg) x Potency of KHP×0.1

Molarity = ------------------------------------

Volume consumed (ml) x 20.42 × 100

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/ re-standardization should not be more

than 0.2%.

Reference I.P./In-House (IP 2007, Vol. I, Page No. 550)

Frequency

Preparation 01 Month

Standardization Initially after preparation

Re- standardization After 15 days

Storage conditions Store the solution in a light-resistant airtight container at

ambient temperature

Precautions (if any) 1) Handle with care under a fuming cupboard.

2) Handle with care, wear hand gloves and nose mask

PERCHLORIC ACID (0.05M)

(Code No. VS14)

PREPARATION

Mix 4.25 ml. of perchloric acid with 500 ml. of anhydrous glacial acetic acid and 12.5ml.of acetic anhydride, cool and add anhydrous glacial acetic acid to produce 1000 ml. Allow the prepared solution to stand for 1 day for the excess acetic anhydride to be combined and carry out the determination of water. If the water content exceeds 0.05 %, add more acetic anhydride. If the solution contains no titrable water, add sufficient water to obtain the content of water between 0.02% and 0.05%. Allow the solution to stand one day and again titrate the water content. The solution so obtained should contain between 0.02% and 0.05% water content. Standardize the solution in the following manner.

STANDARDISATION (TRIPLICATE)

Weigh accurately about 0.1750 gm. of potassium hydrogen phthalate (KHP), previously powdered lightly and heated at about 120°C for 2 hours and dissolve it in 50 ml. of anhydrous glacial acetic acid. Add 0.1ml.of crystal violet solution as an indicator and titrate with 0.05M perchloric acid solution until the violet colour changes to emerald-green. Perform a blank determination and make any necessary corrections.

Each 1ml of 0.05M perchloric acid is equivalent to 0.01021gm of C₈H₅KO₄

Calculation

Wt. of potassium hydrogen phthalate (mg) x Potency of KHP×0.05

Molarity = ----------------------------------

Volume consumed (ml) x 10.21 × 100

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/ re-standardization should not be more

than 0.2%.

Reference In-House

Frequency

Preparation 01 Month

Standardization Initially after 24 hours of preparation

Re- standardization After15 days

Storage conditions Store the solution in a light-resistant airtight container at

ambient temperature

Precautions (if any) 1) Handle with care under a fuming cupboard.

2) Handle with care, wear hand gloves and nose mask

POTASSIUM PERMANGANATE (0.02M)

(Code No. VS15)

PREPARATION

Dissolve 3.2 gm of potassium permanganate in 1000 ml water, heat on the water bath, allow standing for 2 days and filter through glass wool. Standardize the solution in the following manner.

STANDARDISATION (TRIPLICATE)

To 25 ml of this solution in a glass stoppered flask add 2 gm of potassium iodide, followed by 10 ml of 1M sulphuric acid. Titrate the liberated iodine with 0.1 M sodium thiosulphate using 3 ml of starch solution, added towards the end of the titration, as the indicator. Perform the blank determination and any necessary correction.

Each 1ml of 0.1M sodium thiosulphate is equivalent to 0.00316 gm of KMnO₄.

Calculation

M2 x V2

Molarity = ----------------------

Where M2 = molarity of 0.1M sodium thiosulphate solution.

V2 = volume of 0.1 M sodium thiosulphate consumed in

V1 = volume of 0.1 M potassium permanganate taken in ml.

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization / re-standardization should not be more

than 0.2 %.

Reference I P/In-House (IP 2007, Vol. I, Page No. 551)

Frequency

Preparation 01 Months

Standardization Initially after preparation

Re-standardization After 15 days

Storage conditions Store the solution in a well-stoppered glass bottle at ambient

temperature

Precautions (if any) None specific

POTASSIUM IODATE (0.05M)

(Code No. VS16)

PREPARATION

Weigh accurately 10.70 gm of potassium iodate previously dried at 110°C to constant weight in sufficient water to produce 1000 ml. Standardise the solution in the following method.

STANDARDISATION (TRIPLICATE)

Weigh accurately 0.35 gm of potassium iodide, dissolve in about 10 ml of water, add 35 ml of hydrochloric acid and 5 ml of chloroform. Titrate with 0.05 M potassium iodate until the purple colour of iodine disappears from the chloroform. Add the last portion of the iodate solution dropwise and agitate vigorously and continuously. Allow standing for 5 minutes. If any colour develops in the chloroform layer continue the titration until the chloroform is decolourised.

Each 1ml of 0.05 M potassium iodate is equivalent to 0.0166gm of potassium iodide.

Calculation

Wt. of potassium iodide (mg) x Potency of potassium iodide× 0.05

Molarity = ---------------------------

Volume consumed (ml) x 16.6 × 100

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/ re-standardization should not be more

than 0.2%.

Reference I.P./In-House (IP 2007, Vol. I, Page No. 551)

Frequency

Preparation 01 Month

Standardization Initially after preparation

Re- standardization After 15 days

Storage conditions Store the solution in light-resistant container at ambient

temperature

Precautions (if any) None specific

POTASSIUM HYDROXIDE (0.1M)

(Code No. VS17)

PREPARATION

Dissolve 6 gm of potassium hydroxide in sufficient carbon dioxide-free water to produce 1000 ml. Standardize the solution in the following manner.

STANDARDISATION (TRIPLICATE)

Titrate 20.0 ml of the solution with 0.1 M hydrochloric acid using 0.5 ml of phenolphthalein solution as an indicator. Each ml of 0.1 M hydrochloric acid is equivalent to 0.005611 g of KOH.

Calculation

Vol. taken in ml. (0.1 M KOH) X Molarity of HCl (0.1M)

Molarity = -----------------------------

Volume consumed of 0.1M HCl (ml)

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/ re-standardization should not be more

than 0.2%.

Reference I.P./In-House (IP 2007, Vol. I, Page No. 551)

Frequency

Preparation 01 Months

Standardization Initially after preparation

Re- standardization After 15 days

Storage conditions Store the solution in a

light-resistant container at ambient temperature

Precautions (if any) None specific

POTASSIUM HYDROXIDE ETHANOLIC (0.5M)

(Code No.VS18)

PREPARATION

Dissolve 30 g of potassium hydroxide in 40 ml of water and then add sufficient ethanol (60 %) to produce 1000 ml.

STANDARDISATION (TRIPLICATE)

Titrate 20.0 ml of the solution with 0.5 M hydrochloric acid using 0.1 ml of phenolphthalein solution as indicator until the permanent pale-pink colour is produced.

Each ml of 0.5 M hydrochloric acid is equivalent to 0.02806 g of KOH.

Calculation

Vol. taken in ml. (0.5 M HCl) X Molarity of HCl (0.5M)

Molarity = -----------------------------------

Volume consumed of 0.5M Eth. KOH (ml)

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/ re-standardization should not be more

than 0.2%.

Reference I.P./In-House (IP 2007, Vol. I, Page No. 551)

Frequency

Preparation 01 Month

Standardization Initially after preparation

Re- standardization After 15 days

Storage conditions Store the solution in the light-resistant container at ambient

temperature

Precautions (if any) None specific

SILVER NITRATE (0.1M)

(Code No. VS19)

PREPARATION

Dissolve 17.0 gm of Silver Nitrate in sufficient water to produce 1000 ml. Standardize the solution in the following manner.

STANDARDISATION (TRIPLICATE)

Weigh accurately about 0.1 gm. of sodium chloride, (previously dried at 110°C for 2 hours) and dissolve in 5 ml. of water. Add 5 ml. of acetic acid, 50 ml. of methanol and 0.15 ml of eosin solution. Stir, preferably with a magnetic stirrer, and titrate with 0.1M silver nitrate solution.

Every 1 ml of 0.1M silver nitrate is equivalent to 0.005844gm of NaCl.

Calculation

Wt. of sodium chloride (mg) x Potency of NaCl × 0.1

Molarity = --------------------------------------

Volume consumed (ml) x 5.844 × 100

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/ re-standardization should not be more

than 0.2%.

Reference I.P./In-House (IP 2007, Vol. I, Page No. 551)

Frequency

Preparation 01 Month

Standardization Initially after preparation

Re- standardization After 15 days

Storage conditions Store the solution in tightly stoppered amber coloured

glass bottles at ambient temperature.

Precautions (if any) 1) Avoid direct contact during weighing and its spillage.

2) Use hand gloves.

SILVER NITRATE (0.1M) POTENTIOMETRIC

(Code No. VS20)

PREPARATION

Dissolve 17.0 gm of silver nitrate in sufficient water to produce 1000 ml. Standardize the solution in the following manner.

STANDARDISATION (TRIPLICATE)

Weigh accurately about 0.1 gm. of sodium chloride in a 100 ml beaker and dissolve in it 50 ml. of water. Carry out the titration potentiometrically.

Every 1 ml of 0.1M silver nitrate is equivalent to 0.005844gm of NaCl.

Calculation

Wt. of sodium chloride (mg) x Potency of NaCl × 0.1

Molarity = --------------------------------

Volume consumed (ml) x 5.844 × 100

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/ re-standardization should not be more

than 0.2%.

Reference In-House

Frequency

Preparation 01 Month

Standardization Initially after preparation

Re- standardization After 15 days

Storage conditions Store the solution in tightly stoppered amber coloured

glass bottles at ambient temperature.

Precautions (if any) 1) Avoid direct contact during weighing and its spillage.

2) Use hand gloves.

SODIUM HYDROXIDE (1M)

(Code No. VS21)

PREPARATION

Dissolve 42.0 gm of Sodium hydroxide in sufficient carbon dioxide-free to produce 1000 ml. Standardize the solution in the following manner.

STANDARDISATION (TRIPLICATE)

Weigh accurately 5.0 gm. of potassium hydrogen phthalate (KHP), previously powdered and dried at 120°C for 2 hours and dissolved in 75 ml. of carbon dioxide-free water. Add 0.1 ml. of phenolphthalein solution and titrate with 1M sodium hydroxide solution until a permanent pink colour is produced.

Each 1ml of 1M sodium hydroxide is equivalent to 0.2042 gm of C₈H₅KO₄

Calculation

Wt. of potassium hydrogen phthalate (mg) x Potency of KHP× 1

Molarity = -----------------------------------------

Volume consumed (ml) x 204.2 × 100

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/ re-standardization should not be more

than 0.2%.

Reference IP/In-House (IP- 2007, Vol. I. Page No. 552)

Frequency

Preparation 01 Month

Standardization Initially after preparation

Re- standardization After 15 days

Storage conditions Store the solution in a well-stoppered light-resistant HDPE bottle,

which prevent access to atmospheric Carbon Dioxide at ambient temperature.

Precautions (if any) 1) Handle with care.

2) Use hand gloves and a nose mask during preparation.

SODIUM HYDROXIDE (0.1M)

(Code No. VS22)

PREPARATION

Dissolve 4.2 gm of sodium hydroxide in sufficient carbon dioxide-free water to produce 1000 ml. Standardize the solution in the following manner.

STANDARDISATION (TRIPLICATE)

Weigh accurately about 0.5 gm. of potassium hydrogen phthalate (KHP), previously powdered and dried at 120°C for 2 hours and dissolve in 75 ml of carbon dioxide-free water. Add 0.1 ml. of phenolphthalein solution and titrate with the 0.1M sodium hydroxide solution until a permanent pink colour is produced.

Each 1ml of 0.1M sodium hydroxide is equivalent to 0.02042 gm of C₈H₅KO₄

Calculation

Wt. of potassium hydrogen phthalate (mg) x Potency of KHP × 0.1

Molarity = --------------------------------------

Volume consumed (ml) x 20.42 × 100

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/ re-standardization should not be more

than 0.2%.

Reference In-House

Frequency

Preparation 01 Month

Standardization Initially after preparation

Re- standardization After 15 days

Storage conditions Store the solution in well-stoppered light-resistant HDPE bottle

which prevent access to atmospheric carbon dioxide at ambient

temperature

Precautions (if any) 1) Handle with care.

2) Use hand gloves and a nose mask during preparation.

SODIUM HYDROXIDE (0.05M)

(Code No. VS23)

PREPARATION

Dissolve 2.1gm of sodium hydroxide in sufficient carbon dioxide-free water to produce 1000 ml. Standardize the solution in the following manner.

STANDARDISATION (TRIPLICATE)

Weigh accurately about 0.25 gm. of potassium hydrogen phthalate (KHP), previously powdered and dried at 120°C for 2 hours and dissolve in 75 ml. of carbon dioxide-free water. Add 0.1 ml. of phenolphthalein solution and titrate with 0.05M sodium hydroxide solution until a permanent pink colour is produced.

Each 1ml of 0.05M sodium hydroxide is equivalent to 0.01021gm of C₈H₅KO₄

Calculation

Wt. of potassium hydrogen phthalate (mg) x Potency of KHP×0.05

Molarity = ------------------------------------

Volume consumed (ml) x 10.21 × 100

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/ re-standardization should not be more

than 0.2%.

Reference In-House

Frequency

Preparation 01 Month

Standardization Initially after preparation

Re- standardization After15 days

Storage conditions Store the solution in well-stoppered light-resistant HDPE

the bottle which prevents access to atmospheric carbon dioxide at

ambient temperature.

Precautions (if any) 1) Handle with care.

2) Use hand gloves and a nose mask during preparation.

SODIUM THIOSULPHATE (0.1M)

(Code No. VS24)

PREPARATION

Dissolve 25 gm of sodium thiosulphate and 200 mg. of sodium carbonate in carbon dioxide-free water to produce 1000 ml. Standardize the solution in the following manner

STANDARDISATION (TRIPLICATE)

Weigh accurately about 0.2 gm. of potassium bromate and dissolve sufficient water to produce 250 ml. To 50 ml. of this solution add 2 gm. of Potassium Iodide and 3 ml. of 2M Hydrochloric acid and titrate with 0.1M sodium thiosulphate solution using starch solution added towards the end of the titration, as indicator until the blue colour is discharged to end-point

Every 1 ml of 0.1M sodium thiosulphate is equivalent to 0.002784gm of KBrO₃

Calculation

Wt. of potassium bromate(mg) × 50 x Potency of potassium bromate× 0.1

Molarity = ------------------------------------

Volume consumed (ml) x 2.784 x 250 × 100

SODIUM THIOSULPHATE (0.001M)

(Code No. VS25)

PREPARATION

Take 10 ml 0.1M of sodium thiosulphate in a 1000 ml volumetric flask and produce 1000 ml with carbon dioxide-free water. Standardize the solution in the following manner

STANDARDISATION (TRIPLICATE)

Weigh accurately about 0.05 gm. of potassium bromate and dissolve sufficient water to produce 500 ml. To 10 ml. of this solution add 2 gm of Potassium Iodide and 3 ml. of 2M hydrochloric acid and titrate with 0.001M sodium thiosulphate solution using starch solution added towards the end of the titration, as indicator until the blue colour is discharged to a blue coloured end-point

Each 1 ml of 0.001M sodium thiosulphate is equivalent to 0.00002784gm of KBrO_3.

Calculation

Wt. of potassium bromate(mg) x 10 x Potency of potassium bromate ×0.001

Molarity = -----------------------------------

Volume consumed (ml) x 0.02784 x 500 × 10

SODIUM NITRITE (0.1M)

(Code No.VS26)

PREPARATION

Dissolve 7.5 gm of sodium nitrite insufficient water to produce 1000 ml of water. Standardize the solution in the following manner

STANDARDISATION (TRIPLICATE)

Dissolve 0.3 gm of sulphanilic acid in 50 ml of 2M hydrochloric acid, add 3 gm of potassium bromide, cool in ice and titrate with the 0.1M sodium nitrite solution determining the end-point potentiometrically.

Each 1ml of 0.1M sodium nitrite is equivalent to 0.01732gm of C₆H₇NO₃S.

Calculation

Wt. of sulphanilic acid (mg) x Potency of sulphanilic acid × 0.1

Molarity = -------------------------------------

Volume consumed (ml) x 17.32 ×100

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/ re-standardization should not be more than 0. 2%.

Reference I.P./In-House (IP 2007, Vol. I, Page No. 552)

Frequency

Preparation 01 Month

Standardization Initially after preparation

Re- standardization After 15 days

Storage conditions Store the solution in a well-stoppered light-resistant HDPE bottle

which prevent access to atmospheric carbon dioxide at ambient

temperature.

Precautions (if any) None specific

SODIUM LAURYL SULPHATE (0.004M)

(Code No. VS27)

PREPARATION

Dissolve 0.2884gm of sodium decyl sulphate, calculated in reference to the substance at 105˚C for 2 hrs, in sufficient water to produce 1000ml. Standardise the solution in the following manner.

STANDARDISATION (TRIPLICATE)

To 50 ml of the solution add 15ml of chloroform, 10 ml of sulphuric acid and 1ml of dimethyl yellow–orate blue solution. Titrate with 0.004M benzethonium chloride, shaking vigorously and allowing the layer to separate after each addition until the chloroform layer acquires a permanent clear green colour.

Each 1ml of 0.004M benzethonium chloride is equivalent to 0.001154gm of C12H25NaO4S.

Calculation

M2 x V2

Molarity = ----------------------

Where M2 = molarity of 0.004M benzethonium chloride solution.

V2 = volume of 0.004Mbenzethonium chloride consumed in

V1 = volume of 0.004M sodium lauryl sulphate taken in ml.

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization / re-standardization should not be more than 0.2 %.

Reference In-House

Frequency

Preparation 1 Months

Standardization Initially after preparation

Re-standardization After 15 days

Storage conditions Store the solution in a well-stoppered glass bottle at ambient

temperature

Precautions (if any) None specific

SULPHURIC ACID (1M)

(Code No. VS28)

PREPARATION

Add slowly, with stirring, 60 ml. of sulphuric acid to produce 1000 ml with water, allowing cooling to 25°C. Standardise the solution in the following manner.

STANDARDISATION (TRIPLICATE)

Weigh accurately about 1.5 gm of anhydrous sodium carbonate (previously heated at about 270°C for 1 hour). Dissolve it in 100 ml. of water and add 0.1 ml. of methyl red solution. Add the acid slowly from a burette, with constant stirring, until the solution becomes faintly pink. Heat the solution to boiling, cool and continue the titration, Heat again to boiling and titrate further as necessary until the faint pink colour is no longer affected by continued boiling.

Each 1ml of 1M sulphuric acid is equivalent to 0.10598gm of Na₂CO₃

Calculation

Wt. of sodium carbonate (mg) x Potency of Na₂Co₃×1

Molarity = -------------------------------------

Volume consumed (ml) x 105.98 × 100

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/ re-standardization should not be more than 0.2%.

Reference I.P./In-House (IP 2007, Vol. I, Page No. 552)

Frequency

Preparation 01 Month

Standardization Initially after preparation

Re- standardization After 15 days

Storage conditions Store the solution in a well-stoppered glass bottle at

ambient temperature.

Precautions (if any) 1) Handle with care in the fuming cupboard.

2) Use hand gloves and a nose mask during preparation.

3) Never add water to acid.

ZINC SULPHATE (0.1M)

(Code No. VS29)

PREPARATION

Dissolve 29 gm of zinc sulphate in sufficient water to produce 1000 ml. Standardise the solution in the following manner.

STANDARDISATION (TRIPLICATE)

Measure accurately 25 ml. of 0.1 M zinc sulphate into a 250 ml Conical flask and add 25 ml of ammonia ammonium chloride buffer TS. Titrate with 0.1M disodium edetate using erichrome black T as an indicator.

Calculation

Molarity of 0.1 M EDTA x Taken volume of 0.1 M EDTA (ml)

Molarity = -----------------------------------

The volume of 0.1 M zinc sulphate consumed (ml)

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/ re-standardization should not be more than 0.2%.

Reference In-House

Frequency

Preparation 01 Month

Standardization Initially after preparation

Re- standardization After 15 days

Storage conditions Store the solution in a light-resistant container at ambient

temperature

Precautions (if any) None specific

ZINC SULPHATE (0.05M)

(Code No. VS30)

PREPARATION

Dissolve 14 gm of zinc sulphate in sufficient water to produce 1000 ml. Standardise the solution in the following manner

STANDARDISATION (TRIPLICATE)

Measure accurately 25 ml. of 0.05 M zinc sulphate into a 250ml conical flask and add 25 ml of ammonia ammonium chloride buffer TS. Titrate with 0.05M disodium edetate using erichrome black T as an indicator.

Calculation

Molarity of 0.05 M EDTA x Taken volume of 0.05 M EDTA (ml)

Molarity = --------------------------------

The volume of 0.05 M zinc sulphate consumed (ml)

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/ re-standardization should not be more than 0.2%.

Reference In-House

Frequency

Preparation 01 Month

Standardization Initially after preparation

Re- standardization After15 days

Storage conditions Store the solution in light-resistant container at ambient

temperature

Precautions (if any) None specific

FERRIC AMMONIUM SULPHATE (0.1 M)

(Code No. VS31)

PREPARATION

Dissolve 50 gm of ferric ammonium sulphate in a mixture of 300 ml of water and 6 ml of sulphuric acid, dilute with water to 1000 ml and mix. Standardise the solution as follows.

STANDARDISATION (TRIPLICATE)

Accurately measure about 25 ml of the solution into a glass stoppered flask, add 3 ml of hydrochloric acid, mix and add a solution of 2 gm of potassium iodide in 10 ml of water. Insert the stopper, allow to stand for 10 minutes, then titrate the liberated iodine with 0.1 M sodium thiosulphate VS, adding 3 ml of starch TS as the endpoint is approached.

Each ml of 0.1 M sodium thiosulphate is equivalent to 0.004822g of FeNH₄(SO₄)₂12H₂O.

Calculation

M2 x V2

Molarity = ----------------------

Where M2 = molarity of 0.1M sodium thiosulphate solution.

V2 = volume of 0.1 M sodium thiosulphate consumed in

V1 = volume of 0.1 M ferric ammonium sulphate taken in ml.

ACCEPTANCE CRITERIA

1) Accuracy of the solution should be within ± 10% of the theoretical concentration.

2) RSD* of the triplicate results of standardization/ re-standardization should not be more

than 0.2%.

Reference I.P./In-House (IP 2007, Vol. I, Page No. 549)

Frequency :

Preparation 01 Month

Standardization Initially after preparation

Re- standardization After 15 days

Storage conditions Store the solution in a light-resistant container at ambient

&nbsp temperature

Precautions (if any) None specific

*RSD formula: 100 ( N (xi - X )² )^1/2

∑ N -1

&nbspX i =1

where N = set of measurement

xi = Individual measurement

x =mean of the set

SOP for Preparation and Standardization of Volumetric Solutions

AMMONIUM THIOCYANATE (0.1M)

BENZETHONIUM CHLORIDE (0.004 M)

CERRIC AMMONIUM SULPHATE (0.1M)

DISODIUM EDETATE (0.1M)

DISODIUM EDETATE (0.05 M)

FERROUS AMMONIUM SULPHATE (0.1 M)

HYDROCHLORIC ACID (1M)

HYDROCHLORIC ACID (0.5 M)

HYDROCHLORIC ACID (0.1M)

HYDROCHLORIC ACID (0.02M)

SODIUM THIOSULPHATE (0.001M)

SODIUM NITRITE (0.1M)

SODIUM LAURYL SULPHATE (0.004M)

SULPHURIC ACID (1M)

ZINC SULPHATE (0.1M)

ZINC SULPHATE (0.05M)

FERRIC AMMONIUM SULPHATE (0.1 M)

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