1.0 PURPOSE
The purpose of the document is to establish a general and uniform method for the determination of total ash, acid-insoluble ash.
2.0 SCOPE
This standard testing procedure is suitable for the determination of a general and uniform method for the determination of total ash, acid insoluble ash.
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 Dish - Silica or platinum dish/crucible
4.1.2 Muffle Furnace - maintained at 550 ± 25oC
4.1.3 Ashless filter paper
4.1.4 Burner
4.1.5 Water bath
4.1.6 Drying Oven
4.2 Glassware
4.2.1 Desiccator
4.3 Reagent
4.3.1 Hydrochloric Acid-5N
5.0 PROCEDURE FOR TOTAL ASH
5.1 Weigh the nearest 0.001g, about 2 g of the prepared sample in general and 5g in case of herbs into the tared flat-bottomed dish.
5.2 Pour about 2 ml of ethanol on the material in the tared dish and ignite it.
5.3 Heat the dish carefully over a small flame to char the material.
5.4 Then ignite in the muffle furnace at 550 ± 25°C till the grey ash is obtained.
5.5 Cool and wet the ash with several drops of water, evaporate carefully to dryness, and heat in the muffle furnace for a further 1 hour at 550± 25°C.
5.6 If the wetting shows the ash to be carbon-free, remove the dish to a desiccator containing fresh, efficient desiccant, allow it to cool to room temperature, and weigh without delay.
5.7 If the wetting shows the presence of carbon, repeat the wetting and heating until no specks of carbon are visible and ignite in the muffle furnace for 1 hour after the disappearance of carbon.
5.8 If carbon is still visible, leach the ash with hot water, filter through the ashless filter paper, wash the filter paper thoroughly, transfer the filter paper and contents to the ashing dish, dry, and ignite in the muffle furnace at 5500C± 25°C until the ash is white. Cool the dish, add the filtrate, and evaporate it to dryness in a water bath.
5.9 Heat in the muffle furnace again at 5500C± 25°C, cool in the desiccators, and weigh as previously.
5.10 Repeat these operations until the difference in mass between two successive weighings is less than 0.002 g. Record the lowest mass. Retain the total ash for determining the acid-insoluble ash.
5.11 Calculation
Total
ash (on dry basis), % by mass = (W3-W1)
x100 x 100
(W2-W1) 100-M
Where,
W1 = Weigh of the empty
crucible, in g
W2 =Weigh of crucible+
sample (before ashing) in g
W3 = Weigh of crucible+
sample (after ashing) in g
M = Moisture
content of the sample (%)
6.0 PROCEDURE FOR ACID INSOLUBLE ASH
6.1 Refer to the total ash procedure till ashing.
6.2 To the ash contained in the porcelain and silica dish after total ash determination.
6.3 The dish was preserved containing the ash from the determination of total ash.
6.4 Add 25 ml of dilute hydrochloric acid. Cover with a watch glass.
6.5 Heat on a water bath for 10 minutes.
6.6 Allow to cool and filter the contents of the dish through a Whatman filter paper No. 42 or its equivalent.
6.7 Wash the filter paper with water until the washings are free from the acid.
6.8 After the filter paper is free from the acid, return the filter paper to the dish.
6.9 Keep it in an oven at 100 ± 2°C for 3 hours.
6.10 Ignite in a muffle furnace at 550 ± 25°C for one hour.
6.11 Cool the dish in desiccators and weigh it.
6.12 Repeat this process for heating for 30 minutes, cooling, and weighing until the difference between two successive weighings is less than one milligram. Record the lowest mass.
6.13
Calculation
Acid
insoluble ash, % by mass = (W4 –
W1 ) x100 x 100
W2-W1 (100-M)
Where,
W1 = Weigh of the empty
crucible, in g
W2 =Weigh of crucible+
sample (before ashing) in g
W3 = Weigh of crucible
i.e., acid insoluble ash, in g
M = Moisture
content of the sample (%)
7.0 REVISION/CHANGE HISTORY: NA
8.0 ATTACHMENTS
· Appendix-1: FLOW CHART FOR TOTAL ASH
· Appendix-2: FLOW CHART FOR ACID INSOLUBLE ASH
9.0 REFERENCES
TOTAL ASH
· Appendix 2.2.3 of A.P.I. Part II, Vol-1,2007
IS 1155 – 1968 (Reaff: 2010)
AOAC 20th Edn:2016 Chapter(32.1.05/923.03/p.2;32.2.01/945.38/p.46; 32.4.02/935.39/p.77 ;32.5.03/925.11/p.79)
· FSSAI Lab Manual for Cereal & Cereal Products-2016 – Sr.No 8.2
IS 1797-1985 (Reaff.2013);
AOAC 20th Edn:2016 Chapter (43.1.05/941.12/p.2)
FSSAI Lab Manual for Spice and condiments-2016 – Sr.No 4.0
Annex D of IS 4941:1994;RA 2008; Amendment -1,2011
Annex A of IS 1165:2002; RA 2013; Amendment -2,2014
Annex B of IS 14433:2007;RA 2012; Amendment -5,2016
ACID INSOLUBLE ASH
· Appendix 2.2.4 of A.P.I. Part II, Vol-1,2007
FSSAI Lab Manual for Cereal & Cereal Products-2016 – Sr.No 8.3
IS 13846:2009
Annex C of IS 1011-2002 (RA2009), Amd.-1, 2006
IS 1797-1985 (Reaff.2013) ;
AOAC 20th Edn:2016 Chapter (43.1.05/941.12/p.2 )
FSSAI Lab Manual for Spice and condiments-2016 – Sr.No 5.0
END OF THE DOCUMENT
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