Metal Analysis

Sample dissolution for metal analysis (Wet oxidation of samples)
Reagents
1. Conc. Nitric acid (HNO3)AR

2. Perchloric acid (HClO4) AR (60 %)
3. Hydrochloric acid (HCl) AR
4. Digestion system
5. Digestion flasks
1g of well blended plant samples was weighed into the digestion flask. 10 ml of 2:1 by volume of
nitric-perchloric acid was added to the sample and digested until dense white fumes appeared
(usually takes about 1 hour 30 min maximumg). The digest was allowed to cool and some
quantity of distilled water was added to the digest. The solution was then filtered into a 50 ml
volumetric flask and diluted to volume (SSSA, 1996).
Analysis on AAS
The resultant digest was then determined on an Atomic Absorption Spectrophotometer (AAS) at
the specific wavelength of each metal. (Cu, Mg, Ca, Zn, Cr, Pb, and Fe) were analyzed using
Model 210 VGP of the Buck Scientific AAS series with air-acetylene gas mixture as oxidant.
Extracts from the above digestion were aspirated after calibrating the equipment for each
-1
element. The results were recorded as mg l of solution and were calculated to mg/kg/% of
sample using the weight of sample taken as a denominator of the digest volume (50 ml).
Calculation
mg kg-1 sample = digest conc. x dilution factor
digest conc = Analyte reading on AAS
DF = Vol of digest x aliquot

wt of sample
vol of digest = Final volume of digested or extracted sample
aliquot = ratio of sample to distilled water (when diluted further)

Potassium analysis on Flame Photometer
Potassium was analyzed using Model 410 Corning Clinical Flame Photometer with air-butane gas
mixture as oxidant. Extracts from the above digestion were aspirated and the equipment calibrated for the
element (K). The results were recorded as mg l -1 of solution and were calculated to mg kg -1 of sample
using the weight of sample taken (5g) as a denominator of the digest volume (50 ml).
Calculation
mg kg-1 sample = digest conc. X DF
digest conc = Analyte reading on the photometer
DF = Vol of digest x aliquot

wt of sample
vol of digest = Final volume of digested or extracted sample
aliquot = ratio of sample to distilled water (when diluted further)
weight of sample = wt of sample taken for digestion or extract

COLORIMETRIC DETERMINATION OF PHOSPHATE IN PLANT
MATERIAL
(Vanado-Molybdate Method)
Apparatus:
1. Colorimetre
2. Volumetric flask 100 ml
Reagents
a. Vanado-Molybdate reagent – dissolve 25 g ammonium molybdate (NH 4)6 MoO24·4H2O in 200 ml
hot water and cool. Dissolve separately in 1.25 g of NH 4 metavanadate in 120 ml hot water. Cool
and add 250ml of HNO3to the vanadate solution add dilute to 1 litre.
b. P standard solution: stock 1000 ppm P. Dissolve 0.4374 g dry anhydrous KH 2PO4 in distilled
water and dilute to 1 litre. Store the solution in a dark brown Pyrex glass bottle in a cool place.
Procedure
1. Pipette 10ml of samples solution (from wet digestion or dry ashing) into 50mly volumetric flask
and add 25 ml distilled water.
2. Within 5 minutes, add 10 ml of vanado molybdate reagent add dilute to volume mix and let stand
for 15 minutes.
3. Determine % transmittance
4. Standard curve for P – pipette 0, 1, 2, 3, 4 and 5ml of the 100 ppm P standard solution into a
series of 50 ml volumetric flasks and the colour is developed according to the same procedure as
stated in steps 1, 2 and 3.
5. Plot absorbance against concentration
6. Calculate % P content in plant sample
DETERMINATION OF NITROGEN
Samples were analyzed chemically according to the official methods of analysis described by the
Association of Official Analytical Chemist (A.O.A.C., 18th Edition, 2005).
This could be done in two ways which is the titrimetric and the colourimetric.
The Titrimetric
This consists of three techniques namely, Digestion, Distillation and Titration.
Digestion
10ml of each sample was taken carefully into the Kjeldahl digestion tubes to ensure that all sample
materials got to the bottom of the tubes. To this we added 1 Kjedahl catalyst tablet and 10 ml of conc.
H2SO4. These were set in the appropriate hole of the digestion block heaters in a fume cupboard. The
digestion was left on for 4 hours after which a clear colourless solution was left in the tube. The digest
was cooled and carefully transferred into 100 ml volumetric flask, thoroughly rinsing the digestion tube
with distilled water and the flask was made up to mark with distilled water.
ADAPTED AUTO-ANALYZER METHOD FOR NITROGEN

Sample preparation:
The samples are digested by the usual Kjeldhal method
Standard: 1000 ppm N
Standard is prepared from (NH4)2SO4 in 8 % conc.H2SO4
Weigh accurately 4.719 g of (NH4)2SO4 and dissolve to 1litre mark with 8 %
H2SO4 to make 1000 ppm of Nitrogen. Prepare 100 ppm from stock standard.
Working standards of 1, 15, 20 and 30 ppm are prepared from the 100 ppm.
Reagents:
1. Diluent – weigh accurately 200 g of NaCl and measure 15 ml cone. H 2SO4 and make up to 2 litres
with distilled water.
2. Sodium citrate tartrate: 40 g NaOH 50g sodium citrate and 150 g sodium tartrate and make up to
1litre with distilled water.
3. Alkaline phenate – Dissolve 100 g sodium hydroxide in distilled water cool and add 138 ml of
liquid phenol or 276 g of phenol crystal and make up to 1 litre store in a dark bottle.
4. Commercial bleach i.e. JIK
Procedure:
1. 1ml of either standard or sample
2. Add 4.0ml of diluent and mix
3. Add 1.5ml of potassium phosphate tartrate mix
4. Add 2.5ml of alkaline phenate, mix thoroughly
5. Add 1.5ml of the commercial bleach and also thoroughly
Leave for at least 30 minutes and read on Spectronic 20 at 630 nm. Blank should contain all reagents. Use
calibration curve to determine Nitrogen content.
pH DETERMINATION

Metal Analysis

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Sample dissolution for metal analysis (Wet oxidation of samples)

1. Conc. Nitric acid (HNO3)AR

mg kg-1 sample = digest conc. x dilution factor

digest conc = Analyte reading on AAS

DF = Vol of digest x aliquot

vol of digest = Final volume of digested or extracted sample

aliquot = ratio of sample to distilled water (when diluted further)

mg kg-1 sample = digest conc. X DF

digest conc = Analyte reading on the photometer

DF = Vol of digest x aliquot

vol of digest = Final volume of digested or extracted sample

aliquot = ratio of sample to distilled water (when diluted further)

weight of sample = wt of sample taken for digestion or extract

This consists of three techniques namely, Digestion, Distillation and Titration.

ADAPTED AUTO-ANALYZER METHOD FOR NITROGEN

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