Page 40 - Application Handbook - Liquid Chromatography

33

 Analysis of Dicyandiamide in Fertilizers

Fig. 3 shows the sample preparation process
t
t
i
l
l
i
f
e (
e (
er
er
f
i
1.

00 g
00 g
1.
)
z
z
i
)
er
er
pl
pl
Sample (fertilizer) 1.00 g described in the fertilizer test method.
am
S S
am
Fertilizer certified reference materials A and
Met hanol 100 m B* were treated in accordance with the
Methanol 100 mL L
sample preparation procedure described in
Fig. 3. The final solutions from the sample
Shake
S hak e preparation were then spiked with
(10 minutes)
(10 minutes) dicyandiamide with the standard addition
technique so that the concentrations of
dicyandiamide reached 10 mg/L. Figures 4 &
5 show the chromatograms obtained. The
Residue
s
ut
S
Supernatant solution R es i due analysis conditions are the same as in Table
ol
i
on
nat
ant
uper
1. (In accordance with the sample
preparation procedure in Fig. 3, if 100 % of
F ilt r a t e w it h P T F E Waste the dicyandiamide was recovered, its
Filtrate with PTFE
Membrane Filter content would be calculated as equivalent to
Membrane Filter
(Pore size 0.2 µm)
(Pore size 0.2 µm) a 0.1 % mass fraction with respect to the
fertilizer.)
*Fertilizer certified reference material A
o H
t
LC
P
ec
nj
I Inject to HPLC (FAMIC-A-10) is a high-analysis compound
t
fertilizer containing urea. Fertilizer certified
reference material B (FAMIC-B-10) is a
Fig. 3: Sample Preparation
general-compound fertilizer not containing
urea. Both are commercially available from
FAMIC.

mAU mAU
40 Fertilizer Certified 1  Peak 40 Fertilizer Certified 1  Peak
Reference Material A 1. Dicyandiamide Reference Material B 1. Dicyandiamide
30 30
20 20
10 10
0 0
0.0 2.5 5.0 7.5 min 0.0 2.5 5.0 7.5 min
Fig. 4: Chromatogram of Fertilizer Certified Reference Fig. 5: Chromatogram of Fertilizer Certified Reference
Material A (spiked with 10 mg/L dicyandiamide) Material B (spiked with 10 mg/L dicyandiamide)
First Edition: April 2013
© Shimadzu Corporation, 2013