1.0 PURPOSE
The purpose of the document is to establish a general and uniform method for the determination of moisture in milk powder.2.0 SCOPE
This standard testing procedure is suitable for the determination of moisture in milk powder.
3.0 RESPONSIBILITY
The expert and trained chemist are responsible for following this procedure. The technical manager is responsible for implementing this procedure.
4.0 REQUIREMENTS
4.1 Apparatus
4.1.1 Analytical balance, capable of weighing to the nearest 1 mg, with a readability of 0.1 mg.
4.1.2 Drying oven, capable of being maintained at 87°C ± 1°C throughout the working space, with forced Ventilation, thermostatically controlled.
4.3.2.1 Metal block, provided with channels of diameter 4.3 mm for holding the column in the drying oven.
4.3.2.2 Copper tubes, of lenght1500 mm, of internal diameter 2 mm, connected to the metal block in the drying oven.
4.3.2.3 Tube, made of polycarbonate, of length 350 mm, of diameter 40 mm filled with silica gel with hygrometer indicator.
4.3.2.4 The silica gel should have dried at 150°C for more than 12 h before use. Using the dry compressed air, no color change of the hygrometric indicator.
4.1.3 Desiccator, containing freshly dried silica gel with hydrometric indicator.
4.1.4 Columns, made of hard polypropylene, of length 90 mm, of internal diameter 20 mm, provided with two polyethylene filters, narrowed towards one end to fit onto the block.
4.1.5 Synthetic stoppers, made of soft polyethylene
4.1.6 Container, suitable for holding the columns.
4.1.7 Container, suitable for holding the synthetic stoppers.
4.1.8 Rod, made of polyvinyl chloride (PVC), of length 120 mm, of diameter 18 mm, suitable for placing the Polyethylene filters in the column.
4.1.9 Tweezers, suitable for removing the polyethylene filters from the column
4.1.10 Soap-film meter, suitable for measuring a flow of 33 ml/min.
4.1.11 Dry compressed air, minimum pressure of 200 kPa, moisture content of ≤ 0, 01 mg H2O per Iitre at Atmospheric pressure, free of any organic material. Use metal tubes only to connect the source of compressed air to the equipment in the drying oven. The container is made of glass and provided with an airtight lid.
4.1.12 Container, made of glass, provided with an airtight lid.
4.2 Glassware: NA
4.3 Reagent: NA
5.0 PROCEDURE
5.1 Preparation of Sample
Transfer the test sample to a dry close container of capacity twice the volume of the sample. Mix intensively by rotating & shaking the sample.
5.2 Preparation of column
5.2.1 Set the constant pressure regulator, appropriately. Measure, using the soap-film meter, the airflow of each channel.
5.2.2 Calculate the average flow per channel. Adjust the pressure, if necessary, to obtain an average airflow of 33 ml/min per channel.
5.1.2 Remove both synthetic stoppers from the column, Place the stoppers in the container and store at room temperature.
5.2.1 Place the column, provided with filters placed in position in the metal block, in the oven set at 87 °C for at least 1 hr. (Use slight pressure when placing the column in position to create an airtight connection).
5.2.2 Take the column out of the oven and close it with the synthetic stoppers. Place the closed column in the container with the other prepared columns.
5.2.3 Place the container and the columns in the desiccators. Close the desiccators and allow the whole to cool for 60 min ± 5 min.
5.3 Preparation of test portion
5.3.1 After cooling take one closed column at a time out of the container while leaving the container in the desiccator. Close the desiccators immediately after taking out a column weight. The closed column to the nearest 1 mg, recording the mass to four decimal places.
5.3.2 Remove the synthetic stoppers from the pre-weighed column. Using tweezers also remove the upper filter from the column; Keep the stoppers and the filter in a dry place in the weighing Room.
5.3.3 Add 5.0 g ± 0.3 g of the prepared test sample to the column. Using the rod, place the upper filter back in position in the column. Remove any dried milk above the filter with a clean tissue.
5.3.4 Close the Column with both synthetic stoppers.
5.3.5 Immediately weigh the closed column to the nearest 1 mg, recording the mass to four decimal places.
5.3.6 Open the desiccators place the closed column back into the container and close it again.
5.3.7 When the analysis involves more than one test sample, prepare all test portions by repeating the procedure for each separate test portion. Handle only one column at a time.
5.4 Determination
5.4.1 Open the desiccators.
5.4.2 Take one closed column with the prepared test portion at a time out of the container.
5.4.3 Remove both synthetic stoppers from each column.
5.4.4 Place the stoppers in the container and store them at room temperature.
5.4.5 Place each column and its contents in the metal block, which is placed in the drying oven.
5.4.6 As Soon As ready, close the oven, dry the columns and their contents in the oven set at 87°C for 5 h.
5.4.7 After drying, remove each column from the metal block. Replace both synthetic stoppers.
5.4.8 Open the desiccators and place the dried columns and their contents back into the container.
5.4.9 Immediately close the desiccators after placing the last column into the container, and allow the whole to cool for 60 min±5 min.
5.4.10 After cooling, open the desiccators and, in case of more than one test sample.
5.4.11 Take one closed column at a time out of the container leaving the container in the desiccators.
5.4.12 Close the desiccators immediately after taking out a column.
5.4.13 Weigh the closed column to the nearest 1 mg, recording the mass to four decimal places.
6.0 CALCULATION
Calculate the mass fraction of moisture in the
sample,
m1- m2
W, % by mass
= ---------- x 100
m1 -m0
Where,
m0 = Numerical value of the mass of the
column, filters, and stoppers, in grams.
m1 = Numerical value of the mass of the test
portion, the column, filters, and stoppers before drying in grams.
m2 = Numerical value of the mass of the test
portion, column, filters, and stoppers after drying in grams.
The calculation for Total
solid: Total Solid= 100-Moisture
7.0 REVISION/CHANGE HISTORY: NA
8.0 ATTACHMENTS
· Appendix-1: FLOW CHART FOR MOISTURE CONTENT (REFERENCE METHOD)
9.0 REFERENCES
· IS 11623:2008
Hi. I’m Writer of Researchsop.com. ’ ’ Please share these SOPs to all concern pharma people for their development. I like to fullfill the need of curious people. These things inspire me to make things looks better.
0 comments:
Post a Comment