Q U A L I T Y R E C O R D S / F O R M S

Doc. Level:IV Doc. Version: I

Doc. No: ZRK-QC-F.13 w.e.f: 1st Oct. 2013
Analysis Method of Formalin

Apparatus & Glass ware Requirements:

Name of Apparatus Capacity Quantity Grade
Conical Flask 250 ml 3 Pyrex/Borosil “A”
Beaker 1000 ml 2 Pyrex/Borosil “A”
Measuring Cylinder 50 ml, 250ml 2,2 Pyrex/Borosil “A”
Volumetric Flask 500, 1000 ml 1,2 Pyrex/Borosil “A”
Burette Graduated 50 ml 50 ml 2 Pyrex/Borosil “A”
Hydrometer 1.00 – 1.200 Range 1.0 -1.1 – 1.2 2 Glass Germeny
Thermometer Zeal 100 ⁰ C 1 Zeal
Weighing Scale 210 g 1 GF Series or Sartorius d=0.1mg
Magnetic Stirrer Medium Speed Rev 1 Teflon Coated Surface
Butter Paper 50 mm dia 6 Paper
Dropper 5 ml 4 Glass
Pipettes Graduated 5 , 50 ml 1,1 Pyrex/Borosil “A”
Micropippete 1000 µl 1 Micolit

Reagents & Chemicals:

Reagents & Chemicals Stock Grade Volumetric Solutions
Sodium Thiosulphite A.R Grade 0.75 M
Sulphuric Acid A.R Grade 1.0 N
Sodium Hydroxide A.R Grade 0.1 N
Bromo Thymol Blue indicator A.R Grade TS
Thymol Phthalien indicator A.R Grade TS
Methyl Orange indicator A.R Grade TS
Phenolphthalien indicator A.R Grade TS
Sodium Carbonate A.R Grade A.R Grade
Oxalic Acid A.R Grade A.R Grade
Water Distilled Distilled

Volumetric Solution Preparation:

Preparation of 1 N H2SO4 Solution:
Pipette out 27 ml of H2SO4 Concentrated A.R Grade & transfer into a 1000 ml volumetric flask add a sufficient quantity
of distilled water in it stir to mix & make up volume to mark with distilled water & stir to mix well. Preserve in a reagent
bottle of 1000 ml capacity.
Standardization of 1 N H2SO4 Solution:
Weigh accurately about 0.500 g of Sodium carbonate anhydrous A.R Grade & transfer into a 250 ml conical flask add a
sufficient quantity of distilled water in it & stir to dissolve, add 2 to 3 drops of methyl orange as an indicator. Yellow Color
develops. Titrate with 1 N Sulphuric acid along constant stirring. The end point would be orange red color.
Calculate the Normality of H2SO4 Solution With the help of following formula:

Weight of sodium carbonate anhydrous in grams x 1000

Normality of H2SO4 = ------------------------------------------------------------------------- =
Consumed volume of H2SO4 Solution x 53

Where 53 conversion factor of sodium carbonate.

Written BY: Reviewed By: Verified By: Approved By:

___________ ___________ ______________ ______________

Q.C. Incharge Q.C. Manager General Manager Director Technical
 Q U A L I T Y R E C O R D S / F O R M S
Doc. Level:IV Doc. Version: I
Doc. No: ZRK-QC-F.13 w.e.f: 1st Oct. 2013
Analysis Method of Formalin

Preparation of Sodium Sulphite 0.75 M:

Weigh accurately about 95.0 g of Sodium Sulphite A.R Grade & transfer into a 1000 ml volumetric flask add a sufficient
quantity of distilled water in it stir to mix & make up volume to mark with distilled water & stir to mix well. Preserve in a
reagent bottle of 1000 ml capacity.
Precautions:
1- Use clean & Dry glass apparatus
2- Wipe the exterior of pipettes with soft tissue paper while transferring liquid.
3- Accurately make up volume upto mark with diluents.
4- Rinse each glass ware well with distilled water & once rinse with diluents.
5- Weigh accurately upto 3 decimal.
6- Keep all solutions in well closed & tight sealed containers.
7- Avoid sniffing formalin solution.

Procedure:
% age Determination of Formalin:
Weigh accurately upto 3 decimal 0.8 g of formalin solution directly in a conical flask, add about 50 ml of sodium
Thiosulphite 0.75 molar solution in it stir to homogenize, add 2 to 3 drops of thymol phthalin as an indicator. Blue Color
appears Check the pH of the resulting solution and maintain pH 9.1 to 9.3 with 1N Sulphuric acid or 1 N NaOH solution.
Titrate with 1 N Sulphuric acid along constant stirring. The end point would be colorless.
Calculate the concentration With the help of following formula:

Consumed volume of 1 N H2SO4 x 30.03 x Factor of H2SO4

% formaldehyde = ----------------------------------------------------------------------------- x 100
Sample Weight in grams x 1000

Where 30.03 is the conversion factor of formaldehyde.

% Free Formic Acid Determination in Formalin:

Weigh accurately upto 3 decimal about 50 g of formalin solution directly in a conical flask, add about 50 ml of Distilled
Water in it stir to homogenize, add few drops of BromoThymol Blue as an indicator. Titrate with 0.1 N NaOH solution
along constant stirring. Yellow Color changes into Green then Blue End point.
Calculate the concentration With the help of following formula:

Consumed volume of NaOH solution x 46.02 x Factor of NaOH solution

% Free Formic Acid = ----------------------------------------------------------------------------------------------- x 100
Sample Weight in grams x 1000

Where 46.02 is the conversion factor of formic Acid.

% Free Methanol Determination in Formalin:

Put Formalin Sample in a 250 ml Cylinder Insert an hydrometer of (1.00-1.200) in it, also insert a 100°C Thermometer in
it, Note Reading of Both Thermometer and Hydrometer & Determine the density of Formalin at 20°C by putting data in
following formula.
Density of Formalin at 20°C = (T1 - 20°C) x 0.00058 + density at T1 = ………………. g/cm3

Now Calculate the % free methanol by putting data in following formula.

% Free MeOH = % FA x 0.003 + 1.00171 – Density of formalin at 20°C = …………………. %

0.00253

Written BY: Reviewed By: Verified By: Approved By:

___________ ___________ ______________ ______________

Q.C. Incharge Q.C. Manager General Manager Director Technical
 Q U A L I T Y R E C O R D S / F O R M S
Doc. Level:IV Doc. Version: I
Doc. No: ZRK-QC-F.13 w.e.f: 1st Oct. 2013
Analysis Method of Formalin

Determination of Conversion Constant of Density at Different Temperatures

Constant(k) = Density of sample at at working temperature(D1) – Density of sample at chilled Temperature (D2)
Sample temperature at working (T1) – chilled temperature (T2)

1- For Example Formalin Density Constant 0.00058= D1 – D2 = 1.134 -1.114 = 0.020 = 0.00058
T1 – T2 54.5 – 20 34.5

2- For Example Methanol Density Constant 0.00093= D1 – D2 = 0.790 – 0.777 = 0.0130 = 0.00093
T1 – T2 34 – 20 14

Alternate Testing Method

Apparatus & Glass ware Requirements:

Name of Apparatus Quantity Name of Apparatus Quantity

Conical Flask 250 ml 3 Dropper Glass 4
Glass sytoppered 500 ml Flask 2 Reagent Bottles Transparent 100 ml 2
Beaker 250 ml 4 Reagent Bottles Transparent 1000 ml 4
Beaker 1000 ml 2 Reagent Bottles Amber 100 ml 1
Funnel 50 mm dia 4 Reagent Bottles Amber 1000 ml 1
Measuring Cylinder 100 ml 2 Weighing Scale d= 0.1 mg 1
Volumetric Flask 1000 ml 5 Magnetic Stirrer 1
Volumetric Flask 250 ml 2 Oven 200º C 1
Volumetric Flask 100 ml 4 Hot plate Heater 200º C 1
Burette Graduated 50 ml 4 Calculator 1
Pipette 25 ml Graduated 2
Pipette 10 ml volumetric 4
Pipette 1 ml Graduated 2

Reagents & Chemicals:

Reagents & Chemicals Grade Reagents & Chemicals Grade

Formalin standard 37 – 40 % Iodine A.R Grade
Sodium Hydroxide A.R Grade Potassium Iodide A.R Grade
Hydrochloric Acid A.R Grade Arsenic acid A.R Grade
Sulphuric Acid A.R Grade Oxalic Acid A.R Grade
Sodium Carbonate A.R Grade Potassium Dichromate A.R Grade
Sodium Bicarbonate A.R Grade Phenolphthalein A.R Grade
Sodium Thiosulphate A.R Grade Methyl Orange A.R Grade
Water Distilled Maize Starch A.R Grade

Written BY: Reviewed By: Verified By: Approved By:

___________ ___________ ______________ ______________

Q.C. Incharge Q.C. Manager General Manager Director Technical
 Q U A L I T Y R E C O R D S / F O R M S
Doc. Level:IV Doc. Version: I
Doc. No: ZRK-QC-F.13 w.e.f: 1st Oct. 2013
Analysis Method of Formalin

Volumetric Solution Preparation:

Preparation of 0.05M Iodine Solution:
Weigh accurately about 14 g iodine & dissolve in 36 g of Potassium Iodide solution in 100 ml water & add 2 to 3 drops of
HCl solution & transfer into a 1000 ml volumetric flask add a sufficient quantity of distilled water in it stir to mix & make
up volume to mark with distilled water & stir to mix well Stand Overnight for settlement. Preserve in a Brown glass
sytoppered reagent bottle of 1000 ml capacity protecting from light.
Methyl Orange Preparation:
Weigh accurately about 0.500 g of methyl orange A.R. Grade & dissolve in 100 ml of methanol A.R. Grade.
Standardization of 0.05M Iodine Solution:
Weigh accurately about 0.150 g of Arsenic trioxide previously dried at 105ºC for 1 hour & transfer into a 250 ml glass
sytoppered conical flask add a sufficient quantity of distilled water & 20 ml of 1 M NaOH Solution in it & stir to dissolve,
slightly heat to dissolve if necessary, add 0.1 ml methyl orange indicator, add Dilute HCl dropwise until yellow color
changes to pink, Add 2 g of sodium carbonate, 50 ml distilled water & 1 ml of starch solution as indicator. Titrate with
iodine solution until permanent blue color is produced, Also perform a blank analysis & Calculate the Molarity of iodine
Solution With the help of following formula:

Weight of AS2O3 in milligrams

Molarity of Iodine Solution = -------------------------------------------------------------- = ……….. M
4.946 x Consumed volume of Iodine Solution

Where 4.946 is the conversion factor o AS2O3.

Preparation of 1 M NaOH Solution:

Weigh accurately about 40.0 g of Sodium Hydroxide A.R Grade & transfer into a 1000 ml volumetric flask add a sufficient
quantity of distilled water in it stir to mix & make up volume to mark with distilled water & stir to mix well. Preserve in a
reagent bottle of 1000 ml capacity.
Standardization of 1 M NaOH Solution:
Weigh accurately about 0.700 g of Oxalic Acid A.R Grade & transfer into a 250 ml conical flask add a sufficient quantity
of distilled water in it & stir to dissolve, add 2 to 3 drops of phenolphthalein as an indicator. Start point will remain
colorless. Titrate with 1 M NaOH solution along constant stirring. The end point would be pink color.
Calculate the Molarity of NaOH Solution With the help of following formula:

Weight of Oxalic acid in grams x 1000

Normality of NaOH = ------------------------------------------------- =
Consumed volume of 1 M NaOH x 63
Where 63 conversion factor of oxalic acid.
Preparation of 1 N HCl Solution:
Transfer 85 ml of HCl Concentrated A.R Grade into a 1000 ml volumetric flask add a sufficient quantity of distilled water
in it stir to mix & make up volume to mark with distilled water & stir to mix well. Preserve in a reagent bottle of 1000 ml
capacity.
Standardization of 1 N HCl Solution:
Weigh accurately about 0.500 g of Sodium carbonate anhydrous A.R Grade & transfer into a 250 ml conical flask add a
sufficient quantity of distilled water in it & stir to dissolve, add 2 to 3 drops of methyl orange as an indicator. Yellow Color
develops. Titrate with 1 N HCl solution along constant stirring. The end point would be orange red color.
Calculate the Normality of HCl Solution With the help of following formula:

Written BY: Reviewed By: Verified By: Approved By:

___________ ___________ ______________ ______________

Q.C. Incharge Q.C. Manager General Manager Director Technical
 Q U A L I T Y R E C O R D S / F O R M S
Doc. Level:IV Doc. Version: I
Doc. No: ZRK-QC-F.13 w.e.f: 1st Oct. 2013
Analysis Method of Formalin

Weight of sodium carbonate anhydrous in grams x 1000

Normality of HCl = ------------------------------------------------------------------------- =
Consumed volume of 1 N HCl x 53

Where 53 conversion factor of sodium carbonate.

Preparation of 0.1 M Na2S2O3 Solution:

Weigh accurately about 25 g of Sodium thiosulphate & 0.2 g of sodium carbonate anhydrous A.R Grade & transfer into a
1000 ml volumetric flask add a sufficient quantity of distilled water in it stir to mix & make up volume to mark with
distilled water & stir to mix well. Preserve in a reagent bottle of 1000 ml capacity.
Standardization of 0.1 M Na2S2O3 Solution:
Weigh accurately about 0.200 g of potassium dichromate previously dried at 105ºC for 1 hour A.R Grade & transfer into a
500 ml glass sytoppered conical flask add a sufficient quantity of distilled water in it & stir to dissolve, add 3 g of
potassium iodide & 2 g of sodium bicarbonate, swirl to mix & allow to stand in dark for 15 minutes, Rinse inner walls of
flask & stopper with distilled water & Titrate the liberated iodine with sodium thiosulphate solution until yellow color
develops, add 1 ml of starch solution as an indicator blue color develops & continue your titration until blue color
discharged, Also perform a blank analysis & Calculate the Normality of H2SO4 Solution With the help of following
formula:

Weight of Potassium Dichromate in milligrams

Molarity of Na2S2O3 = -------------------------------------------------------------- =
49.04 x Consumed volume of Na2S2O3 Solution

Where 49.04 is the conversion factor of potassium dichromate.

Preparation of Starch Solution 1% w/v:

Weigh accurately about 1.0 g of water Soluble starch & Transfer into a 200 ml beaker with 100 ml previously boiling water
stir to homogenize & store in a reagent bottle of 100 ml capacity in a refrigerator for 1 week use only. Prepare fresh
solution when indicator response show lighter color.

% age Determination of Formalin:

Weigh accurately upto 3 decimal 1.0 g of formalin in 250 ml volumetric flask, make up volume to mark with water & mix
well to homogenize.
Pipette out 10 ml of this solution into a conical flask, add 25 ml of a 0.05 M Iodine solution and 10 ml of 1 M NaOH
solution in it. Allow to stand for 5 min. Acidify with 15 ml of 1M HCl Solution and determine the excess of iodine by
titration with a 0.1 M Na2S2O3 Solution.

Calculate the concentration With the help of following formula:

Consumed volume x Factor of 0.1 M Na2S2O3 Solution x 1.5

% formaldehyde = ----------------------------------------------------------------------------- x 100 = …………….. %
Content in mg of Sample dilution taken

1 ml of 0,1 N iodine consumed is equivalent to 1,5 mg formaldehyde.

Written BY: Reviewed By: Verified By: Approved By:

___________ ___________ ______________ ______________

Q.C. Incharge Q.C. Manager General Manager Director Technical