Principle of Wet Digestion
Principle of Wet Digestion
⮚ Wet ashing:
It’s also used for quantification of minerals. It is done by using strong acids or their
mixtures to oxidize sample or usually used for elemental analysis. (Flaming and Atomic
Absorption Spectrometry both are used for wet ashing).
Apparatus:
● Weighing balance
● Conical flask
● Hot plate
● Measuring cylinder of 50-100 ml
Reagents/Solvents:
-Mixture of diacids [Nitric acid HNO3] , [ Perchloric acid HClO4]
-Distilled water
Procedure:
1. Take 0.5 g of sample of interest in a conical flask.
2. Add 10ml of diacids in the ratio of 3:1 [Nitric acid HNO3], [ Perchloric acid HClO4]
in flash that contain sample and place it on hot plate for 10 hours.
3. Remove or pick up the sample when it turns transparent or when 1-2 ml of
sample remains behind in the flask.
4. Cool the sample and transfer it to 100 ml beaker/conical flask and make volume
with distilled water upto 100 ml.
1) Flame Spectrophotometer:
It is an equipment which works on the principle of emission.
Flame Spectrophotometer:
In flame, wet digested (ashed) sample is automised and electrons move to higher
energy state when these electrons return back to ground state emit energy of specific
wavelength. Amount determined by instrument called “Flame Spectrophotometer”. -----
-Amount of emitted energy of a specific wavelength for element of interest is measured.
-Emission is directly proportional to concentration of target food (amount of target
food).
Apparatus:
● Atomic, flame spectrophotometer
● Plastic bottle 100 ml
● Beaker 150 ml
● Crucible 30 ml
● Digestion apparatus
● Hot plate
● Dessicator
● Filter paper
● Pipette (2,4,10 ml)
● Volumetric flask (20,50,100 ml)
● Weighing balance
● Measuring cylinder
● Muffle furnace
Reagents:
● Distilled H2O
● Perchloric acid
● Nitric acid
● Stock solution of different minerals ( Ca, Cu, Fe, Mn, Zn, Cd, Se, Mg, Co, etc)
Procedure:
● Prepare or set up instrument (Atomic or Flame Spectrophotometer)
● Turn standard solution of each mineral element with minimum of 4 different
conc. (5,10,15,20 ppm). You can also use 3,6,9,12 ppm or 4,8,12,16 ppm as well,
it depends on requirements of mineral.
● Flush burner with distilled water between sample and reestablish zero
absorption point after eavh point.
● Preparation of calibration /standard curve from average of each standard.
● Read conc. of sample from plotted curve and compare it with standard curve.
Standard solution:
"It is made by specific amount of stock or mother solution if we want to identify mineral
element".
For standard solution of iron we pickup iron stock solution.