GB 437-2009Copper sulfate (For crops use) (English PDF)

3.1 Appearance

Blue or blue-green crystals, with no visible foreign matter.

3.2 Technical Specifications

Copper sulfate should meet the requirements of Table 1.

Table 1 copper sulfate Control Project Index

Item Index

Copper sulfate (CuSO4 · 5H2O) content /% >= 98.0

Arsenic mass fraction a/(mg/kg) <= 25

Pb mass fraction a/(mg/kg) <= 125

Cadmium mass fraction a/(mg/kg) <= 25

Water insoluble /% <= 0.2

Acidity (H2SO4 basis) /% <= 0.2

When a normal production, the mass fraction of arsenic, lead and cadmium content mass fraction was measured at least once every three months.

Test Method 4

4.1 Sampling

In accordance with GB/T 1605-2001 of "original drug product sampling" approach. Determining Sample packages with random number table method, the final sample

The amount should be less than 100g.

4.2 Identification Test

4.2.1 heating

After heating, the color should be blue to white, water was added to restore the color blue after cooling.

4.2.2 Precipitation

It was added dropwise a solution of barium chloride in the presence of hydrochloric acid, a white precipitate.

Determination of the mass fraction of copper sulfate 4.3

4.3.1 Method summary

Samples dissolved in water, under acidic conditions, adding an appropriate amount of potassium iodide was reacted with divalent copper, iodine precipitates equimolar to indicate starch

Agent, sodium thiosulfate standard titration solution precipitated iodine titration. From the volume of consumption of sodium thiosulfate standard titration solution, the sample is calculated sulfur

Acid copper content.

The following reaction formula.

2S2O32- + I2 = S4O62- + 2I-

4.3.2 Reagents and solutions

Potassium iodide;

Nitric acid;

Glacial acetic acid;

NaF. saturated solution;

Sodium carbonate. saturated solution;

Acetic acid. phi (CH3COOH) = 36%;

Starch indicator solution. rho (starch) = 5g/L;

Sodium thiosulfate standard titration solution. Ba (Na2S2O3) = 0.2mol/L, according to GB/T 601 and calibration formulations.

4.3.3 Determination Step

About 1g sample was weighed (accurate to 0.0002g) in 250mL Erlenmeyer flask, 100mL of water was added to dissolve, plus three drops of concentrated nitric acid, boiling,

Cooling, saturated sodium carbonate solution was added dropwise until a trace precipitate appears, then 4mL acetic acid solution was added, the solution was slightly acidic

Resistance, plus 10mL saturated sodium fluoride solution, 5g of potassium iodide titration with standard sodium thiosulfate solution titrated to a pale yellow solution. plus

Starch indicator solution 3mL, continue titration to the disappearance of the blue.

4.3.4 computing

The mass fraction of copper sulfate in the sample 1 (%) according to equation (1).

4.3.5 allows poor

The measurement results of the two parallel error should not exceed 0.6%.

4.4 Determination of arsenic, lead and cadmium content

4.4.1 Determination of arsenic content of

4.4.1.1 Method summary

In the presence of potassium iodide and stannous chloride, the high arsenic in the sample solution is reduced to trivalent arsenic, trivalent arsenic and zinc particles under acidic conditions

Hydrogen generation generates arsine gas, removing hydrogen sulfide, then with yellow mercuric bromide formed by lead acetate test paper to orange stain cotton, and

Gutzeit standard quantitative comparison.

4.4.1.2 Reagents and solutions

hydrochloric acid.

Potassium iodide solution. rho (KI) = 150g/L, stored in brown bottle (prepared before use).

Sodium hydroxide solution. rho (NaOH) = 200g/L.

Sulfuric acid. Ba (H2SO4) = 1mol/L.

Stannous chloride solution. rho (SnCl2 · 2H2O) = 400g/L, weigh 20g of stannous chloride (SnCl2 · 2H2O), was dissolved in 50mL salt

Acid; (0 °C stored at a refrigerator).

Lead acetate cotton. absorbent cotton immersed in a solution of lead acetate, dry out after 2h.

Arsenic metallic zinc.

Water. freshly distilled twice-distilled water.

Arsenic trioxide (As2O3). drying to constant weight stored in a sulfuric acid desiccator.

Arsenic standard solution A. Weigh 0.1320g trioxide in 1000mL volumetric flask, dissolve sodium hydroxide solution was added 5mL,

Was added a solution of 25mL sulfuric acid, diluted with water to the mark [solution rho (As) = 0.100mg/mL].

Arsenic standard solution B. pipette to take the above solution 1mL in 100mL volumetric flask, was added a solution of sulfuric acid 1mL, diluted with water

Scale, shake [solution rho (As) = 1.0µg/mL].

4.4.1.3 Instruments

Arsenic measuring apparatus. see Figure 1.

4.4.1.4 Determination Step

4.4.1.4.1 preparation of standard solution

Draw arsenic standard solution B1mL, 1.5mL, 2mL, 2.5mL, 3mL, were placed in a conical flask, add 5mL hydrochloric acid, water was added to the

30mL, 5mL plus potassium iodide solution, 5 drops of stannous chloride solution, mixed, room temperature for 10min.

4.4.1.4.2 prepared sample solution

0.1g sample was weighed (accurate to 0.0002g) placed in a conical flask, add 5mL hydrochloric acid, water was added to 30mL, 5mL plus potassium iodide

Solution, 5 drops of stannous chloride solution, mixed, placed in room temperature for 10min.

4.4.1.4.3 Determination

To the conical flask, 3g of each of the zinc arsenic, and now preloaded with plug cotton and mercury bromide lead acetate test paper of Arsenic

Tube placed 1h at 25 °C, taken Gutzeit comparing the sample mass to give arsenic, arsenic spot color if the sample in the standard color Gutzeit

In addition, increase or decrease the sample weight, the sample may be compared Gutzeit color standard of the color Gutzeit.

4.4.1.5 computing

Arsenic content in the sample 2 (mg/kg), according to formula (2).

(2)

Where.

--- [rho] concentration of arsenic standard solution B, in micrograms per milliliter (µg/mL);

Qiao --- Sample Gutzeit arsenic standard solution B corresponds to the volume in milliliters (mL).

4.4.2 Determination of the mass fraction of lead

4.4.2.1 Method summary

Samples with hydrochloric acid - nitric acid decomposition, cadmium sample solution in an air - acetylene flame atomization, vapor atomic absorption resulting from the lead

Hollow cathode lamp emitted light of a characteristic wavelength of 217.0nm, and the absorbance is directly proportional to the concentration of cadmium based atomic state.

4.4.2.2 Reagents and solutions

hydrochloric acid;

Nitric acid;

Water. secondary distilled water;

Lead standard stock solution. rho (Pb) = 1mg/mL;

Dissolved Acetylene.

4.4.2.3 Instruments

Atomic absorption spectrophotometer, with air - acetylene burner and lead hollow cathode lamp.

Heating plate. the temperature is adjustable at 250 °C.

4.4.2.4 Determination Step

Preparation of sample solution 4.4.2.4.1

Weigh the sample (2 ~ 4) g (accurate to 0.0002g), a 100mL beaker, wetted with a small amount of water, and hydrochloric acid was added 30mL

10mL nitrate, covered with a watch glass at (150 ~ 200) °C boil on a hot plate after 30min, removed heating was continued dish surface, evaporated to near dryness,

Remove. After cooling, 50mL of hydrochloric acid and 4mL water, mixed and filtered. The filtrate was collected in a 100mL flask, drained after a small amount of water will

The residue was washed three times, combined in the filtrate, adding water to the mark, the standby.

Draw standard curve 4.4.2.4.2

Pipette lead standard stock solution 0.1mL, 0.2mL, 0.3mL to three 100mL volumetric flask, was added 4mL hydrochloric acid, washed with water

Volume, and mix. This concentration of lead standard solution were 1mg/kg, 2mg/kg, 3mg/kg. At the same time the preparation of blank solution. In election

At a given optimum conditions, using air - acetylene flame at a wavelength of 217.0nm, the reference solution as the blank, absorbance measured for each standard solution

Light value. Mass fraction of lead standard solution (mg/kg) as the abscissa, the absorbance value corresponding to the ordinate, drawing working curve.

4.4.2.4.3 Determination

Sample solution (or after suitable dilution) under the same measurement conditions of the standard solution measured absorbance of the sample solution, on the working curve

Isolated respective lead concentration (mg/kg).

4.4.2.5 computing

Lead sample mass fraction 3 (mg/kg), according to equation (3) is calculated.

(3)

Where.

--- [rho] concentration measured absorbance value of the sample on the calibration curve corresponding to the lead in milligrams per liter (mg/L);

4.4.2.6 allow poor

This method of parallel measurement results of the difference between the two should be less than 10mg/kg.

4.4.3 Determination of the mass fraction of cadmium

4.4.3.1 Method summary

Samples with hydrochloric acid - nitric acid decomposition, cadmium sample in air - acetylene flame atomization, atomic vapor generated from the absorbed cadmium hollow

Cathode lamp emitted light of a characteristic wavelength of 228.8nm, and the absorbance is directly proportional to the concentration of cadmium based atomic state.

4.4.3.2 Reagents and solutions

hydrochloric acid;

Nitric acid;

Water. secondary distilled water;

Cadmium standard stock solution. rho (Cd) = 1mg/mL;

Dissolved Acetylene.

4.4.3.3 Instruments

Atomic absorption spectrophotometer, with air - acetylene burner and cadmium hollow cathode lamp;

Heating plate. the temperature is adjustable at 250 °C.

4.4.3.4 Determination Step

Preparation of sample solution 4.4.3.4.1

Weigh the sample (2 ~ 4) g (accurate to 0.0002g), a 100mL beaker, wetted with a small amount of water, and hydrochloric acid was added 30mL

10mL nitrate, covered with a watch glass at (150 ~ 200) °C boil on a hot plate after 30min, removed heating was continued dish surface, evaporated to near dryness,

Remove. After cooling, 50mL of hydrochloric acid and 4mL water, mixed and filtered. The filtrate was collected in a 100mL flask, the residue was rinsed with a small amount of water

4.4.3.4.3 Determination

Sample solution (or after suitable dilution) under the same measuring conditions as the standard solution, measuring absorbance of the sample solution, on the working curve

Isolated corresponding cadmium content (mg/kg).

4.4.3.5 computing

Cadmium content in the sample 4 (mg/kg), according to equation (4) is calculated.

(4)

Where.

--- [rho] concentration measured absorbance value of the sample on the working curve corresponding cadmium, in units of milligrams per liter (mg/L);

4.4.3.6 allow poor

This method of parallel measurement results of the difference between the two should be less than 1mg/kg.

4.5 Determination of insoluble matter

4.5.1 Method summary

Sample was dissolved by heating an appropriate amount of water, dried, and insolubles were filtered hot, water-insoluble solid content of insoluble matter mass fraction of the sample

Calculation.

4.5.2 Reagents

water.

4.5.3 Instruments

Standard ground-stoppered Erlenmeyer flask. 250mL;

Fritted glass funnel crucible. G4 type;

Suction conical flask. 500mL;

Oven;

Glass dryer;

Water bath.

4.5.4 Determination Step

The glass fritted funnel crucible drying (110 °C about 1h) to a constant weight (to the nearest 0.0002g), cooled in a desiccator until use. Call

10g sample was taken (accurate to 0.0002g), placed in a conical flask, 100mL of water and 2 drops of concentrated sulfuric acid, heated to dissolve, while hot

Constant weight G4 filter crucible was filtered, the filter residue was washed with hot water with 20mL (co washed five times). The filter cake filled with G4 filter crucible, put

Into an oven at 105 °C ~ 110 °C in drying to constant weight.

4.5.5 computing

4.6 Determination of acidity

4.6.1 Reagents and solutions

Water. New boiled, pH value of 6 to 8;

Potassium hydrogen tartrate. saturated solution, pH = 3.56 (25 °C); pH = 3.55 (30 °C);

Glacial acetic acid;

Sodium hydroxide standard titration solution. Ba (NaOH) = 0.02mol/L, according to GB/T 601 and calibration formulations.

4.6.2 Instruments

pH meter (with magnetic stirrer);

Glass electrode;

Saturated calomel electrode;

Burette. 10mL, having 0.05mL indexing.

4.6.3 Determination Step

After stabilizing the instrument, the electrode is placed in standard buffer solution [pH of saturated potassium hydrogen tartrate, pH = 3.56 (25 °C), pH =

3.55 (30 °C)], the instrument reading position readings adjusted to pH standard buffer solution at this temperature, when reading standard buffer solution unchanged

When this instrument can be used.

4.6.3.2 Determination

About 2g sample was weighed (accurate to 0.002 g of), a 100mL beaker was added 50mL of water, under magnetic stirring to dissolve the sample,

Titration solution is then titrated with standard sodium hydroxide to a pH meter reading of 4.00, is the end.

4.6.4 computing

Acidity content of Sample 6 (%) according to equation (6) is calculated.

4.7 product testing and acceptance

Shall comply with the provisions of GB/T 1604's. Limit values rounding processing using the value comparison method.

5.1 copper sulfate marking, labeling, packaging, should comply with the provisions of GB 3796.

5.2 packaging material can be iron sulfate, nonflammable plastic drum, fiber drum lined with double plastic bags, tightly sealed to prevent moisture absorption, but also

It may take other forms of packaging according to user requirements or ordering agreement, subject to the provisions of GB 3796.

5.3 sulfate package airiness, dry place.

5.4 storage and transportation to prevent moisture and sunlight, no food, seed, feed mix, avoid contact with skin, eyes, nose and mouth to prevent inhalation.

5.5 Security. copper sulfate is low toxicity fungicides, can be swallowed or inhaled toxic. When used, should wear protective gloves, masks, protective wear clean

clothes. Immediately after use with soap and water wash. Such as poisoning occurs, it is timely examination and treatment.

5.6 Warranty. Under the provisions of storage and transportation conditions, copper sulfate guarantee period from the date of manufacture 2 years.

END: Draft Version (GB 437-2009)