The term “SAP” in the context of acetic acid glacial testing likely refers to the “Saponification Value” or “Saponification Acid Value.” The Acetic Acid Glacial Testing Procedure (SAP) saponification value is a measure of the average molecular weight of all the fatty acids present in a substance. It is often used in the analysis of fats and oils. Here’s a general procedure for determining the saponification value of acetic acid glacial:
PURPOSE
To ensure the quality of incoming Raw Material.
SCOPE
It is applicable to the Quality Control Department.
RESPONSIBILITY
- Quality Control Manager
- Asst. Quality Control Manager
- Analyst
- Lab Assistant
PROCEDURE
Machinery/Equipment/Apparatus
- Analytical balance
- Glass Wares
- Silica crucible
- Hot plate
- Desiccator
- Burette
- Hot plate
Chemicals/Reagents
Sr. # |
Name |
| Chemicals | |
| 1 | Distilled Water |
| 2 | Ethanol 96% |
| 3 | Chloroform |
| Reagents | |
| 1 | Lead standard solution 1 ppm |
| 2 | Acetate buffer pH 3.5 |
| 3 | Thioacetamide reagent |
| 4 | Chloride standard solution 5 ppm |
| 5 | Nitric acid 2M |
| 6 | Silver nitrate R2 solution |
| 7 | Barium chloride solution 25 % |
| 8 | Sulphate standard solution 10 ppm |
| 9 | Acetic acid 5M |
| 10 | Citric acid 20 % w/v |
| 11 | Ammonia 10 M |
| 12 | Iron standard solution 1 ppm |
| 13 | Sulphuric acid 6M |
| 14 | Potassium dichromate VS 0.0167 M |
| 15 | Potassium iodide (freshly prepared solution) |
| 16 | Sodium thiosulphate VS 0.1M |
| 17 | Starch mucilage solution |
| 18 | Sodium hydroxide VS 1M0 |
| 19 | Phenolphthalein solution |
Physical Analysis
This analysis is done by Analytical supervisor with the help of Quality Control Assistant.
Test of Physical Form:
Check the sample and confirm its physical form; it should be translucent, crystalline mass or clear volatile liquid.
Test of Colour:
Confirm the colour of the material by comparing with reference sample; It should be colourless.
Test of odour:
Note its odour. It should be pungent.
Test of solubility:
Miscible with water, ethanol (96%) chloroform and most of fixed and volatile oils.
Test of Residue on evaporation:
Weigh about 20 g of substance in a pre-weighed crucible and evaporate to dryness. Then dry it to 105oC and weight
Observation and calculation:
Wt. of crucible = X g
Wt. of crucible + substance = Y g
Wt. of crucible + residue = Z g
Wt. of substance = Y – X = A g
Wt. of residue = Z – X = B g
B
% age = ———– x 100
A
It should be not more than 0.01 % w/w.
Record the results of Physical Analysis on Raw Material Analysis Sheet.
Limit Tests:
This analysis is done by Analytical supervisor with the help of Quality Control Assistant.
Chlorides:
Sample:
- a) Dilute 5 ml of liquid to produce 100 ml with water.
- b) To 15 ml above solution add 1 ml of 2M nitric acid.
- c) Pour 1 ml of silver nitrate R2 solution in (a).
- d) Allow to stand for 5 minutes.
Standard preparation:
- Mix 10 ml chloride standard solution (5 ppm) with 5 ml of distilled water.
- Add 1 mL of silver nitrate to the mixture as an addition to R2.
- Allow to stand for 5 minutes
Observation
None of the examples produced in the sample are more severe than standard when viewed compared to black backgrounds.
Heavy Metals:
Sample Preparation
- Evaporate 3.4 gm of sample to dryness and dissolve the residue in 20 ml of water.
- Take 12 ml of above solution and add 2 ml of Acetate buffer pH 3. 5 and mix.
- Add 1.2 ml of thioacetamide reagent mix immediately and allow to stand for two minutes.
Standard Preparation
- Mix 10 ml of 1 ppm lead standard solution with 2 ml of above sample solution being examined.
- Add 2 ml of acetate buffer pH 3.5 and mix.
- Add 1.2 ml of thioacetamide reagent. Mixed immediate then allow stand for two minute.
Blank
- Mix 10 ml of distilled water with 2 ml of prescribed solution.
- Mix 10 ml of 10 ppm lead standard solution with 2 ml of prescribed solution being examined.
- Add 2 ml of acetate buffer pH 3.5 and mix.
- Add 1.2 ml of thioacetamide reagent. Mixed immediate then allow stand for two minute.
Observations
- None of the brown colors produced in the sample are more severe than the standard
- The standard solution exhibits slightly brown colour when compared to blank.
Sulphate
Sample Preparation
- Take 12.5 ml of solution S used in diluted to 15 ml with water chloride.
- Add 1 ml of 25 % W/V solution of barium chloride to 1.5 ml of sulphate standard solution (10 PPM SO4) Shake and allow to stand for one minute.
- Add 15 ml of solution prepared in Step (a) to the solution obtained in Step (b).
- Add 0.5 ml of 5M Acetic Acid in and allow to stand for 5 minutes.
Standard Preparation
Take 15 ml of sulphate standard solution (10 ppm S04) and proceed from (2) to (4).
Observation
Any opalescence produced in sample solution is not more intense than that of standard solution (10 ppm)
Acetic Acid Glacial Testing Procedure (SAP)
Reducing Substance:
Mix 5 ml with 10 ml of water. To 5 ml add 6 ml of 6M sulphuric acid cool, add 2 ml of 0.0167M potassium dichromate VS, allow to stand 1 minute add 25 ml of water and 1 ml of freshly prepared potassium iodide solution and titrate the liberated iodine with 0.1M sodium thiosulphate VS using starch mucilage as indicator.
Not less than 1 ml of 0.1M sodium thiosulphate should require.
Record the results of Limit Test on Raw Material Analysis Sheet.
Acetic Acid Glacial Testing Procedure (SAP)
Chemical Analysis:
Identification Test of Glacial Acetic Acid:
- Strongly acidic, even when diluted free. (can be tested by using pH meter).
- When diluted with water and neutralized, Heat the substance being examined with an equal quantity of oxalic acid acidic vapous with the characteristic odour of acidic acid are evolved.
Contents of Glacial Acetic Acid:
Acetic Acid Glacial Testing Procedure (SAP)
Sample Preparation:
Accurately weigh a conical flask with a ground glass stopper containing 25 ml of water R. Add 1.0 ml of the substance to be examined and weigh again accurately. Add 0.5 ml of phenolphthalein solution R and titrate with 1 M sodium hydroxide.
1 ml of 1 M sodium hydroxide is equivalent to 60.1 mg of C2H4O2.
Observation:
- Volume of 1M sodium hydroxide used = P ml
- Volume consumed = Q ml
- Exact molarity of sodium hydroxide after standardization = M
- Note the readings.
Calculations:
Calculate the contents of Glacial Acetic acid as follows:
Factor: 1 ml of 1 M sodium hydroxide is equivalent to 60.1 mg of C2H4O2.
Q x Factor
——————- x 100 = S
2
S =Contents of acetic acid in % age.
Limit:
The contents of Glacial Acetic acid should be 99 – 100.5 %.
Record the results of Chemical Test on Raw Material Analysis Sheet.
Quality Record(s)/Form(s)
The following quality records will be prepared and managed according to the company’s quality records control procedures.
| Required Record | Form Reference No. |
| GIR Acetic Acid Glacial Testing Procedure (SAP) | PPC/IV/000 |
| GRN Acetic Acid Glacial Testing Procedure (SAP) | PPC/IV/000 |
| Raw Material Analysis Sheet | SOR/QCD/RM/00 |
| Raw Material Q. C. No Register | SOR/QC/RM/0 |
- It’s crucial to handle chemicals with care, follow safety protocols, and work in a well-ventilated area.
- The equipment used should be clean and free of contaminants.
- Calibration of the burette and accurate measurement of the sample are essential for precise results.
Always refer to specific laboratory procedures, protocols, and safety guidelines provided by your institution or organization, as they may have specific requirements or variations for this type of analysis Acetic Acid Glacial Testing Procedure (SAP)