Page 73 - Application Notebook - Solution for Food Safety

Application No.L513
News

Q Analysis of Nitrous Acid and Ammonium mAU
Thiocyanate in Fertilizers 50
(ᶗ) 1 ˙Peaks
The method used to prepare fertilizer samples is shown Powdered fertilizer A 1. Nitrous acid
2. Ammonium
in Fig. 3. The method of pretreatment differed thiocyanate
depending on whether the sample was a powder or
liquid, and on extraction liquid pH. Standard additions 25
of nitrous acid and ammonium thiocyanate were made
to the samples for analysis (fertilizer) before being
further prepared according to the procedure shown in 2
Fig. 3 3), 4) . The results of analysis are shown in Fig. 4. 0
Testing Methods for Fertilizers (2016) describes a method
20
that uses ion chromatography for the analysis of 0 5 10 15 min
ammonium thiocyanate (5.8.a). However, because this mAU
method produces a complex eluent, it takes some time 200 (ᶘ) 1 ˙Peaks
for the baseline to stabilize. Another problem with the Powdered fertilizer B 1. Nitrous acid
method is that it has resulted in multiple system peaks 2. Ammonium
thiocyanate
and peaks close to the elution position of ammonium
thiocyanate. Nevertheless, on this occasion, the results 100
show that good separation was achieved, including for
contaminating constituents in the fertilizer.
2
1.00 g
Analytical sample (powder) 0
Spike 0 5 10 15 20
min
Leaving to stand For 18 hours
mAU
100 mL of water 50
(ᶙ) ˙Peaks
Extraction Stir to mix, for 10 minutes Liquid fertilizer A 1. Nitrous acid
2. Ammonium
thiocyanate
1.00 g 25 1
Analytical sample (liquid) 100 mL volumetric flask
Spike
50 mL of water
Extraction Stir to mix 2
0
Water (up to the marked line)
0 5 10 15 20
pH value confirmation min
pH 5 or more mAU
pH 4 or less 200 (ᶚ) ˙Peaks
Liquid fertilizer B 1. Nitrous acid
Aliquot (40 mL) 2. Ammonium
thiocyanate
Sodium hydroxide solution 1
pH adjustment (pH 5-7)
(5 mg/mL)
100
Transfer 100 mL volumetric flask
Water (up to the marked line)
2
filtration
0
0 5 10 15 20
min
Measurement
Fig. 4 Chromatograms of Fertilizer Sample Solutions
Fig. 3 Pretreatment (ᶗ) Powdered fertilizer A, (ᶘ) Powdered fertilizer B,
(ᶙ) Liquid fertilizer A, ( ᶚ ) Liquid fertilizer B
References
1) Ministry of Agriculture, Forestry and Fisheries notification: Establishment of official specifications for commercial fertilizers according to the Fertilizer
Control Law, dated February 22, 1986. Ministry of Agriculture, Forestry and Fisheries notification no. 284: Final revision, dated March 30, 2016.
Ministry of Agriculture, Forestry and Fisheries notification no. 884: Enactment, dated April 1, 2016. [In Japanese]
2) Testing Methods for Fertilizers (2016), Food and Agricultural Materials Inspection Center (FAMIC): http://www.famic.go.jp/ffis/fert/obj/
shikenho_2016.pdf [In Japanese]
3) Masanori Hasegawa, Yasuharu Kimura: Determination of Nitrous Acid and Ammonium Thiocyanate in Fertilizer by High Performance Liquid
Chromatography (HPLC): A Collaborative Study, Research Report of Fertilizer, vol. 8, 70-78 (2015) [in Japanese]
4) Kohei Ito, Yasuharu Kimura, Masanori Hasegawa, Yuji Shirai: Simultaneous determination of nitrous acid and thiocyanate in fertilizer by HPLC,
Japanese Journal of Soil Science and Plant Nutrition, 87 (3), 120-124 (2016) [In Japanese]

First Edition: Jan. 2017

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