OIL PARAMETER ANALYSIS

5.7 Phosporus
5.7.1 Principle
 The test portion is ignited, the ashes then digested with nitric acid. A yellow
phosphovanadomolybdic complex is then formed between phosphoric, vanadic
and molybdic ions. The resulting color is determined by a spectrophotometer.
5.7.2 Apparatus &Chemicals

 5 and 10 ml graduated pipettes

 20 and 25 ml burettes
 50 ml quartz crucible, low form, Jurgens Cat. No. 683-9825
 Spectrophotometer suitable for observations at 400 nm (Perkin Elmer Lambda
12)
 Furnace for temperatures up to 1000ºC
 Nitric acid, approx. 6 N aqueous solution (420 ml conc. HNO3 (65%) is diluted
with distilled water to 1 liter)
 Ammonium molybdate ((NH4)6Mo7O24.4H2O), AR grade, 50 g/l aqueous solution
 Ammonium vanadate (NH4VO3), acid aqueous solution: dissolve about 2.5 g of
ammonium vanadate in about 500 ml of hot water. Cool and then add about 20
ml conc. nitric acid ( = 1.4 g/ml). Make up to 1 liter with distilled water.
 Standardized phosphate stock solution containing 0.1 mg of phosphorus per ml:
dissolve 1.156 g of disodium hydrogen phosphate (Na2HPO4.12H2O) or 0.4393
g of monopotassium hydrogen phosphate (KH2PO4) in 1 liter of water.

5.7.3 Working Stage

1. Calibration
Prepare 0.2, 0.4, 0.8, 1.6, 3.2, 4.0, 8.0 g/ml solutions by pipetting 0.05, 0.1,
0.2, 0.4, 0.8, 1.0, 2.0 ml of the phosphate stock solution, followed by 20 ml of
the ammonium molybdate-vanadate mixture and make up to 25 ml with 6 N
nitric acid. Utilize these solutions in order to plot the calibration curve in such a
way that this curve expresses the calibration factor as:
abs
CF =
ppm

Typically, the CF  9.76 x 10-2

2. Determination

PUBLISHER Author Approved ISSUE

PT CLARIANT ADSORBENTS INDONESIA Ahmad Zaki Nuzulia Andria 18-June-2014
Anshori Classification
INTERNAL
The printout is a working copy of this document – For the latest valid revision please refer to the GMS database Page 11 of 15
OIL PARAMETER ANALYSIS

Weigh (exactly to within 1 mg) about 5.000 ± 0.5 g (event. more or less
according to its presumed phosphorus content ) of fat into the same crucible.
Put it to the furnace with setting:
T1 = 400OC ----- time 1a= 3 hour

time 1b= 4hour

T2 = 800OC ----- time 2a= 1hour
time 2b= 30 minutes
T3 = 900OC ----- time 3a= 30 minutes
time 3b= 2 hour
After finish and cool off, add exactly 5 ml of aqueous-nitric solution, homogenized.
Add 10 ml of aqueous ammonium vanadate solution and 10 ml of the acidic
aqueous ammonium molybdate solution.
Mixed thoroughly with the help of small beaker, and then allow standing for 20
minutes on the crucibles.
Prepare a blank test, not containing fat, under exactly the same conditions.
Mix carefully, transfer the test solutions into the spectrophotometric cell of the
apparatus.
Measure the absorbance at 400 nm against the blank solution.
5.7.4 Calculation
P (ppm) = A x 25
CF x G

Where:
CF= calibration factor (determined from the calibration curve)
A= absorbance
G = weight of the fat sample (in g)

5.8 Chlorophyll
5.8.1 Principle
 The chlorophyll is determined by measuring the absorbance at a highest
absorption of chlorophyll.

PUBLISHER Author Approved ISSUE

PT CLARIANT ADSORBENTS INDONESIA Ahmad Zaki Nuzulia Andria 18-June-2014
Anshori Classification
INTERNAL
The printout is a working copy of this document – For the latest valid revision please refer to the GMS database Page 12 of 15