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REAGENTS
1. 2N ethanolic KOH .
Add 35 grams of KOH in 25 ml of demineralized water and cool to room temperature.
After cooling, dilute with ethanol to the volume of 250 ml in the 250ml volumetric flask .
2. Washing solution : ethanol / demineralised water = 1 : 1 ( v / v ) .
Measure 1 part ethanol and 1 part distilled water and add them together .
3. Saturated sodium chloride solution .
Add a quantity of sodium chloride in a sample bottle of 100 ml and add distilled water
and shake vigorously . At the bottom of the container should be have excess sodium
chloride .
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A: Toluene
B : Hexane
C : Ethyl acetate
D: 3 % aqueous formic acid solution in toluene
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4. The air bubbles should be removed by purge the solution approximately one
minute away in the suction.
5. When this is done, the solutions need to be in order to rinse the column.
STANDARDS
1. DAK stock solution 250 mg / l .
Weigh 25 mg of pure DAK to 0.1 mg and place it into a 100 mL volumetric flask . Fill the
volumetric flask with hexane solution / toluene up to the mark. Record the weight of the
solvent.
2. DAk standard 1 50 mg / l .
Weigh the DAK stock solution 2 ml to 0.1 mg into a 10 mL volumetric flask and then fill it
with solution of hexane / toluene. Record the weight of the solvent.
3. DAK standard solution 2 10 mg / l.
Weigh the standard DAK 1 2 ml to 0.1 mg into a 10 mL volumetric flask and then fill it
with solution of hexane / toluene. Note the weight.
4. Hexane / toluene solution (1:1)
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INJECTION
( UL)
blank
VOLUME
20
10
20
10
40
10
60
10
80
50
20
50
40
50
60
50
80
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AUTOSAMPLER
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*In the chromatogram , the peak from the DAK is around 3.5 minutes.
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DAK content
DAK mass 4
10 sample weight
Content
DAK
DAK
Concentration in the
=
sample
( mg / kg )
DAK mass
= Mass DAK
(ng)
Dissolution Volume = Volume in which sample is dissolved (ml )
Injection volume = Volume injected ( ul)
Sample weight
= Sample test portion weighed sample ( g )
4. Reporting
Report the final result. If more than one test is carried out on the same sample ,
report the average income and the number of repetitions . Round off results in an
integer.
5. Datastorage
All results are in the database put in the corresponding sample number
Validation:
Reproducibility is measured by different analysts on different days. This is done by using DAK control
standard from LCW and PH216E sample (this sample will be use as IOI LCA QC control standard).
LCW control standard (CLSP 555) :
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Mean
SD
Max
+2SD
+1SD
-1SD
-2SD
Min
N
666.27
25.25
713.68
716.77
691.52
641.03
615.78
635.04
15
PH216E sample (this sample will be use as IOI LCA QC control standard) :
Mean
SD
Max
+2SD
+1SD
-1SD
-2SD
Min
N
689.17
35.08
756.02
759.33
724.25
654.10
619.02
631.42
26
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