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NY/T 3598-2020 PDF in English


NY/T 3598-2020 (NY/T3598-2020, NYT 3598-2020, NYT3598-2020)
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NY/T 3598-2020: PDF in English (NYT 3598-2020)

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 alkanol quaternary ammonium functional groups) and anion
protection column; particle size is 6 µm (or an equivalent chromatographic column).
Filter: the pore size of the filter membrane is approximately 0.45 µm.
Microsampler: 50 µL.
Quantitative injection tube: 5 µL.
Ultrasonic cleaner.
4.5.4 Ion chromatography operating conditions
Mobile phase: carbonate eluent [c(Na2CO3) = 4.5 mmol/L + c (NaHCO3) = 0.8 mmol/L].
Weigh 477 mg of sodium carbonate and 67.2 mg of sodium bicarbonate and dissolve
them in 1000 mL of water. Mix well.
Flow rate: 0. 8 mL/min.
4.6 Moisture
In accordance with the provisions of GB/T 1600.
4.7 pH
In accordance with the provisions of GB/T 1601.
4.8 Determination of suspension rate
Weigh a specimen containing 0.5 g of fosetyl-aluminium (accurate to 0.0001 g). Follow
the provisions of 4.1 in GB/T 14825-2006. Use mobile phase to transfer the remaining
1/10 of the suspension to a 200 mL volumetric flask. Determine the mass fraction of
fosetyl-aluminium according to 4.4. Calculate the suspension rate.
4.9 Determination of wetting time
Follow the provisions of GB/T 5451.
4.10 Wet screening test
Follow the provisions of 2.2 in GB/T 16150-1995.
4.11 Determination of persistent foaming properties
Follow the provisions of GB/T 28137.
4.12 Determination of thermal storage stability
Follow the provisions of 2.3 in GB/T 19136-2003. After thermal storage, the mass
fraction of fosetyl-aluminium shall not be lower than 95% of that before storage. The
pH, suspension rate, wetting time and wet screening test shall still meet the standard
requirements to be qualified.
5 Acceptance and quality assurance periods
5.1 Acceptance
It shall comply with the provisions of GB/T 1604.
5.2 Quality assurance periods
Under the specified storage and transportation conditions, the quality assurance period
for fosetyl-aluminium wettable powder is 2 years from the production date. During the
quality assurance period, all indicators shall comply with standard requirements.
Annex B
(informative)
Aluminum ion complex titration method
B.1 Principle
The determination of aluminum ions in fosetyl-aluminium samples adopts the
complexometric titration method. That is, the fosetyl-aluminium sample is decomposed
in an excess CDTA standard solution under acid and heating conditions; aluminum ions
form a complex with CDTA; the excess CDTA standard solution is back-titrated with a
zinc sulfate standard titration solution.
B.2 Reagents and solutions
Perchloric acid.
Xylenol orange.
Hexamethylenetetramine (HMTA).
1,2-Cyclohexanediaminetetraacetic acid (CDTA).
Sodium hydroxide.
Zinc sulfate standard titration solution: c(ZnSO4) = 0.05 mol/L.
Potassium nitrate.
Deionized water.
B.3 Instruments
150 mL beakers.
20 mL pipettes.
Automatic potentiometric titrator.
Magnetic stirrer with heating.
B.4 Operation steps
B.4.1 Preparation of CDTA standard solution
Weigh 8.5 g of sodium hydroxide into a 2 L volumetric flask. Add 500 mL of water to
dissolve. Weigh out another 36.4 g of CDTA. Dissolve with heat. After cooling to room
temperature, dilute to the graduation with water.
B.4.2 Preparation of perchloric acid solution
In a 500 mL beaker with 300 mL of water previously added, add 100 mL of perchloric
acid while stirring.
B.4.3 Preparation of grinding indicator
Weigh 0.1 g of xylenol orange and 9.9 g of potassium nitrate and grind in a mortar until
completely mixed.
B.4.4 Determination of blank CDTA standard solution
Use a pipette to transfer 20 mL of CDTA standard solution into a 250 mL Erlenmeyer
flask. Add 20 mL of water to dilute. Add 5 mL of perchloric acid solution. Heat to
boiling for about 1 min.
After cooling to room temperature, add 6.0 g of HMTA. Stir until completely dissolved.
Add 30 mg ~ 50 mg of grinding indicator. Titrate with zinc sulfate standard titration
solution until the solution changes from yellow to red as the end point.
Repeat the determination three times.
B.4.5 Determination of sample
Weigh a specimen containing 0.1 g of fosetyl-aluminium (accurate to 0. 0001 g) into a
250 mL beaker. Add 20 mL of water. Add 5 mL of perchloric acid solution. Heat to
boiling for about 1 min.
Add exactly 20 mL of CDTA standard solution. Heat to boiling for about 1 min. After
cooling to room temperature, add 6.0 g of HMTA. Stir until completely dissolved. Add
30 mg ~50 mg of grinding indicator. Titrate with zinc sulfate standard titration solution
until the solution changes from yellow to red as the end point.
B.5 Calculation of aluminum ions
The mass fraction of aluminum ions is calculated according to formula (B.1).
Where,
ω4 - the mass fraction of aluminum in the specimen, in percent (%);
V0 - the average value of the zinc sulfate standard titration solution volume consumed
Buffer solution: pH=7.3±0.2. Weigh 100 g of sodium hydroxide (accurate to 0. 0002 g)
into a 2000 mL beaker. Add 1.8 L of water to dissolve. Neutralize to pH=8.0 with
phosphoric acid solution. After cooling to room temperature, neutralize with phosphoric
acid solution to pH=7.3±0.2. Add 30 g of potassium iodide and 20 mL of iodine
standard titration solution. Stir to dissolve and transfer to a 2000 L volumetric flask.
Dilute to the graduation. Store in dark place at room temperature. Before use, titrate
with sodium thiosulfate standard titration solution until colorless.
C.3 Instruments
Potentiometric titrator.
Ultrasonic water bath.
pH meter.
Adjustable heating mantle.
Spherical condenser tube.
Iodine vial: 250 mL.
Burette: 25 mL, brown.
C.4 Determination steps
C.4.1 Specimen solution
Weigh a specimen containing 3 g of fosetyl-aluminium (accurate to 0. 0001 g) and place
it in a 500 mL volumetric flask. Add 200mL of sodium hydroxide B solution. Place the
volumetric flask in an ultrasonic water bath and sonicate for 10 min. After cooling to
room temperature, add sodium hydroxide A solution to the volume and mix well. Use
a pipette to transfer 10 mL of the specimen solution into a 250 mL iodine flask. Add 40
mL of sodium hydroxide A solution. Connect to condenser pipe. Heat to boil and reflux
for 1 h. Flush the condenser tube with a small amount of water. Cool to room
temperature. Neutralize with sulfuric acid solution. Add 2 drops of phenolic acid
indicator near the end point. Continue titration until the red color disappears.
C.4.2 Determination
Use a pipette to add 25 mL of buffer solution and 20 mL of iodine standard titration
solution. Cap the bottle and mix well. Seal with water. Place the iodine bottle in a dark
place for 30 min ~ 45 min. Add 3 mL of acetic acid to acidify. Titrate with sodium
thiosulfate standard titration solution. Add 3 mL of starch indicator near the end point.
Continue titrating until the blue color of the solution disappears as the end point (or use
a potentiometric titrator to determine the end point).
C.4.3 Blank determination
......
 
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.