NITRR

ORGANIC PROCESS TECHNOLOGY

LAB FILE
VIRENDRA BHAGAT (09113055)

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Moisture content determination in Soaps

AIM - To determine the moisture content in given soap sample. RequirementsChina dish, oven, weighing machine and soap scraps.
TheorySoap is a salt of fatty-acid. Soap is produced by process saponification, where fats( from plants or animal) is first hydrolyzed into free fatty acids, which the combine with alkali to form crude soap and glycerol often called glycerin is liberated and is either left or washed out & recovered. Fats of plants or animals also contain some water content. Water is used to dilute lye crystals & act as a carrier for the lye. The less water in the recipe, the faster would be the saponification. Soap with high water content will take longer to unmold and longer to dry presence of water also prevents cracking and absence of water also causes the recipe to become too thick to flow.

Procedure1) Weigh accurately 5 gm of soap scraps and put it into china dish.
2) This china dish is now put into oven maintaining at temperature around 70 to 80 .

3) After 45 minutes of heating, the china dish was taken out and measures the weight of soap scraps again. 4) Note this reading. 5) Then again put these scraps back into the oven for at least 15 minutes. 6) After that again measuring the weight.

Observations Initial weight of soap scraps = 5.002 gm. Weight of china dish =40.5 gm.

After 45 minWeight of soap scraps = ____________ gm. After 1 hourFinal weight of soap scraps = ____________gm

Calculations-

% moisture content =

100

= ________________________________ 100

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= Result- moisture content present in given soap scraps is ________%. Precautions1) Heating should be done carefully. 2) Soap scraps must be dried within specified range of temperature.

Moisture content determination in Detergents

AIM - To determine the moisture content in given detergent sample.
RequirementsChina dish, oven, weighing machine and detergent sample. TheoryDetergent is a cleansing agent. In that sense soap is also a detergent. But the word detergent usually refers to a synthetic substance other than soap. A detergent contains an active agent called surfactant, which wets the fabric, emulsifies oily matter, solublizes grime and keeps the soil in suspension. This active agent contains two groups, one oil loving lipophilic and the other water loving hydrophilic.

Procedure7) Weigh accurately 5 gm of detergent sample and put it into china dish. 8) This china dish is now put into oven maintaining at temperature around 70 to 80 .

9) After 45 minutes of heating, the china dish was taken out and measures the weight of detergent sample again. 10) Note this reading.

11) Then again put this sample back into the oven for at least 15 minutes. 12) After that again measuring the weight.

ObservationsInitial weight of detergent sample = 5.002 gm. Weight of china dish =40.5 gm.

After 45 minWeight of detergent sample = ____________ gm.

Page |4 / /2012 Final weight of detergent sample = ____________gm CalculationsAfter 1 hour-

% moisture content

100

= ________________________________ 100 = Result- moisture content present in given detergent sample is ________%. Precautions1) Heating should be done carefully. 2) Detergent must be dried within specified range of temperature.

Estimation of total alkali content of Soap

Aim- To analyze the given soap sample and to determine the total alkali
content.

Apparatus Required
Beaker, Stirrer, Glass plate, conical flask, Pipette, Burette, Standard flask, Separating funnel, Bunsen Burner, Funnel.

Chemicals Required
Soap scraps, water, chloroform, 0.5 N NaOH, Methyl orange, Sodium carbonate, conc. H2SO4 .

Theory
Since soap is made from saponification process, which is the combination of free fatty acids and alkali, there is a presence of alkali matter in the soap. The types of alkali metal used determine the kind of soap produced. Sodium soaps are firm; potassium soaps are soft and often liquid. The stronger the alkali solution the faster would be saponification and faster would be tracing out of soap. Also, high presence of alkali can damage the body tissue.

Procedure
1) 5 gm of soap was weighed accurately in a glass plate and transferred into a 250 ml beaker. 2) 100 ml of water was added to completely dissolve the soap.

Page |5 / /2012 3) The mixture was heated directly till the fatty-matter comes floating above. (Approximately 20-30 minutes) 4) Then concentrated H2SO4 was added to the beaker using a pipette carefully to the sides of the container until fatty acids were floating as a layer above the solution. The volume of H2SO4 was noted. 5) 50 ml of chloroform was added to the remaining solution and transferred to the separating funnel. 6) The solution was shaken thoroughly until it separates into 2 layers. 7) Separate fatty acid dissolved chloroform layer again from the aqueous solution. 8) The aqueous solution volume was measured accurately in a measuring cylinder and 10 ml of it was taken into conical flask. 9) 2 or 3 drops of methyl orange indicator was added and titrated against NaOH from the burette. 10) 11) Yellow to pale pink color indicates end point. Then the total alkali content was calculated.

Calculations
Total volume of the aqueous solution, V=__________ml

TITRATION
Standard NaOH vs soap sample. Volume of Soap Sample (ml) Burette Readings(ml) Initial Final Volume of NaOH (ml) Concorda nt Titration value(t) Indicator

Methyl Orange

10 ml of aqueous solution required

of NaOH.

Page |6 / /2012 ml of aqueous solution requires = V1

Amount of NaOH required by acid in aqueous solution ,V 1 = Normality of NaOH= 0.5N Volume of H2SO4 required V2 = ______ Normality of H2SO4, N2 = 46 N Weight of Soap taken = 5 % of Alkalinity = --------------------------------Result The total alkali content of the given soap sample was found to be__________ Precautions1) Heating should be done carefully. 2) Soap scraps must be dissolved thoroughly. 3) Acids and other chemicals should be handled carefully. 4) Separation must be done properly.

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Estimation of Total Fatty Matter (TFM) Content of Soap

AIM- To analyze the sample of the given soap and to determine the total fatty matter content.

Page |7 / /2012 Apparatus Required Beaker, Stirrer, Glass plate, conical flask, Pipette, Burette, Standard flask, separating funnel, Bunsen Burner, Funnel, China dish. Chemicals Required Given sample of soap, Water, Chloroform, Sodium carbonate, 0.5 N HNO 3. Theory Total Fatty Matter (TFM) is one of the most important characteristics describing the quality of soap. It is defined as the total amount of fatty matter, mostly fatty acids, that can be separated from a sample after splitting with mineral acid, usually hydrochloric acid. The fatty acids most commonly present in soap are oleic, stearic and palmitic and pure, dry, sodium oleate has TFM 92.8%. Besides moisture, finished commercial soap, especially laundry soap, also contains fillers used to lower its cost or confer special properties, plus emollients, preservatives, etc. and then the TFM can be as low as 50%. Fillers, which are usually dry powders, also make the soap harder, harsher on the skin and with greater tendency to become 'mushy' in water and so low TFM matter is usually associated with hardness and lower quality. Procedure 1) 5 gm of soap was weighed accurately in a glass plate and transferred into a 250 ml beaker. 2) 100 ml of water was added to completely dissolve the soap. 3) The mixture was heated directly till the fatty matter comes floating above. (Approx 20 to 30 minutes) 4) Then concentrated H2SO4 was added to the beaker using a pipette carefully to the sides of the container until the fatty acids were floating as a layer above the solution. The volume of H2SO4 was noted. 5) The fatty matter collected was filtered using a filter paper and transferred to a pre-weighed china dish. 6) The contents were allowed to evaporate in an electric oven and the residue was weighed. 7) From the difference in weight, the % of fatty matter in the given soap sample was calculated. Calculation Weight of the soap sample = 5 gm = _____________ =______________

{Weight of the china dish+ Soap before drying} { Weight of china dish + Soap after drying } % of fatty mater = % of fatty matter = ___________

/ Weight of soap sample

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Result The percentage of total fatty matter present in the given sample of soap was found to be__________

Precautions1) Heating should be done carefully. 2) Soap scraps must be dissolved thoroughly. 3) Acids and other chemicals should be handled carefully. 4) Separation must be done properly.