NY/T 3598-2020 English PDF (NY/T3598-2020)

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NY/T 3598-2020: Fosetyl-aluminium wettable powder
NY/T 3598-2020
NY
AGRICULTURAL INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 65.100.30
G 25
Replacing HG/T 3297-2001
Fosetyl-aluminium wettable powder
三乙膦酸铝可湿性粉剂
ISSUED ON: MARCH 20, 2020
IMPLEMENTED ON: JULY 01, 2020
Issued by: Ministry of Agriculture and Rural Affairs of the People's Republic of
China
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Requirements ... 5
4 Test methods ... 5
5 Acceptance and quality assurance periods ... 12
6 Marks, labels, packaging, storage and transportation... 13
Annex A (informative) Other names, structural formulas and basic physical and
chemical parameters for fosetyl-aluminium ... 14
Annex B (informative) Aluminum ion complex titration method ... 15
Annex C (informative) Determination for mass fraction of fosetyl-aluminium (chemical
titration) ... 18
Fosetyl-aluminium wettable powder
1 Scope
This Standard specifies the requirements, test methods, acceptance and quality
assurance periods, as well as marks, labels, packaging, storage and transportation for
fosetyl-aluminium wettable powder.
This Standard applies to fosetyl-aluminium wettable powder processed from fosetyl-
aluminium original drug, additives and fillers.
NOTE: Please refer to Annex A for other names, structural formulas and basic physical and
chemical parameters of fosetyl-aluminium.
2 Normative references
The following referenced documents are indispensable for the application of this
document. For dated references, only the edition cited applies. For undated references,
the latest edition of the referenced document (including any amendments) applies.
GB/T 601, Chemical reagent -- Preparations of reference titration solutions
GB/T 603, Chemical reagent - Preparations of reagent solutions for use in test
methods
GB/T 1600, Testing method of water for pesticides
GB/T 1601, Determination method of pH value for pesticides
GB/T 1604, Commodity pesticide regulations for acceptance
GB/T 1605-2001, Sampling method for commodity pesticides
GB 3796, General rule for packing of pesticides
GB/T 5451, Testing method for the wettability of dispersible powders of pesticides
GB/T 6682, Water for analytical laboratory use -- Specification and test methods
GB/T 8170-2008, Rules of rounding off for numerical values and expression and
judgement of limiting values
GB/T 14825-2006, Determination method of suspensibility for pesticides
method to determine the packages to be sampled. The final sample size shall be no less
than 300 g.
4.3 Identification test
4.3.1 Ion chromatography
This identification test can be carried out simultaneously with the determination of the
mass fraction of fosetyl-aluminium. Under the same chromatographic operating
conditions, the relative difference between the retention time of the main
chromatographic peak in the specimen solution and the retention time of the
ethyphosphonate chromatographic peak in the standard solution shall be within 1.5%.
4.3.2 Aluminum ion identification
Please refer to Annex B for qualitative identification of aluminum ions.
4.4 Determination of the mass fraction of fosetyl-aluminium
4.4.1 Method summary
The specimen is dissolved in mobile phase. Sodium carbonate and sodium bicarbonate
solutions are used as mobile phases. Use anion chromatography column and
conductivity detector to perform ion chromatography separation of ethyphosphonate in
the specimen. Use the external standard method for quantification (chemical titration
method can also be used to determine the mass fraction of aluminum triacetate. See
Annex C for details).
4.4.2 Reagents and solutions
Water: ultrapure.
Sodium carbonate: guaranteed pure.
Sodium bicarbonate: guaranteed pure.
Standard sample of fosetyl-aluminium: known mass fraction of fosetyl-aluminium,
ω≥97.0%.
4.4.3 Instruments
Ion chromatograph: equipped with conductivity detector and suppressor.
Integrator or electronic data acquisition system.
Chromatographic column: 250 mm × 4 mm (inner diameter) anion separation column
(filled with polyvinylbenzene/ethylvinylbenzene/polyvinyl alcohol matrix, with alkyl
quaternary ammonium or alkanol quaternary ammonium functional groups) and anion
protection column; particle size is 6 µm (or an equivalent chromatographic column).
Weigh 0.05 g (accurate to 0. 0001 g) of fosetyl-aluminium standard sample into a 100
mL volumetric flask. Add 20 mL of water. Place in an ultrasonic cleaner and sonicate
for 30 min. Cool to room temperature. Use mobile phase to dilute to volume. Shake
well. Use a pipette to transfer 1 mL of the above solution into another 100 mL
volumetric flask. Dilute to the graduation with mobile phase. Shake well. Filter.
4.4.5.2 Preparation of specimen solution
Weigh a specimen containing 0.05 g (accurate to 0.0001 g) of fosetyl-aluminium into a
100 mL volumetric flask. Add 20 mL of water. Place in an ultrasonic cleaner and
sonicate for 30 min. Cool to room temperature. Dilute to the graduation with mobile
phase. Shake well. Use a pipette to transfer 1 mL of the above solution into another 100
mL volumetric flask. Dilute to the graduation with mobile phase. Shake well. Filter.
4.4.5.3 Determination
Under the above operating conditions, after the instrument is stable, continuously inject
several needles of the standard solution until the relative change in the peak area of two
adjacent ethyphosphonate peaks is less than 1.5%. Measure in the order of standard
sample solution, specimen solution, specimen solution, and standard sample solution.
4.4.5.4 Calculation
Average the ethosphonate peak areas in the measured two injections of sample solution
and the two injections of standard solution before and after the specimen. The mass
fraction of fosetyl-aluminium in the specimen is calculated according to formula (1).
Where,
ω1 - the mass fraction of fosetyl-aluminium in the specimen, in percent (%);
A2 - the average value of the ethyphosphonate peak area in the specimen solution;
m1 - the mass of the standard sample, in grams (g);
ω - the mass fraction of fosetyl-aluminium in the fosetyl-aluminium standard sample,
in percent (%);
A1 - the average value of the ethyphosphonate peak area in the standard sample solution;
m2 - the mass of the specimen, in grams (g).
4.4.6 Allowable difference
The difference between the two parallel determination results of the mass fraction of
fosetyl-aluminium shall be no more than 0.6% for 40% and no more than 1.0% for 80%.
Take the arithmetic mean as the measurement result.
4.5 Determination of phosphite
4.5.1 Method summary
The specimen is dissolved in mobile phase. Sodium carbonate and sodium bicarbonate
solutions are used as mobile phases. Using an anion chromatography column and a
conductivity detector, the phosphite in the specimen is separated by ion chromatography.
Conduct quantification by external standard method.
4.5.2 Reagents and solutions
Water: ultrapure.
Sodium carbonate: guaranteed pure.
Sodium bicarbonate: guaranteed pure.
Sodium phosphite pentahydrate standard: known mass fraction ω≥98.0%.
4.5.3 Instruments
Ion chromatograph: equipped with conductivity detector and suppressor.
Integrator or electronic data acquisition system.
Chromatographic column: 250 mm × 4 mm (inner diameter) anion separation column
(filled with polyvinylbenzene/ethylvinylbenzene/polyvinyl alcohol matrix with alkyl
quaternary ammonium or al...