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Chloridazon


Information
Chloridazon technical
Chloridazon technical concentrates
Chloridazon wettable powders
Chloridazon water dispersible granules
Chloridazon suspension concentrates

5-amino-4-chloro-2-phenylpyridazin-3(2H)-one

AGP:CP/346

Information

COMMON NAME: chloridazon (ISO)

STRUCTURAL FORMULA

EMPIRICAL FORMULA: C10H8ClN3O

RMM: 221.6

CAS REGISTRY NUMBER: 1698-60-8

CIPAC CODE NUMBER: 111

CHEMICAL NAMES:

5-amino-4-chloro-2-phenylpyridazin-3(2H)-one (IUPAC)
5-amino-4-chloro-2-phenyl-3(2H)-pyridazone (CAS)

Chloridazon technical

FAO Specification 111/TC/S/F (1997)

1. DESCRIPTION

The material shall consist of chloridazon (Note 1) together with related manufacturing impurities and shall be a yellow to brown solid free from visible extraneous matter and added modifying agents (Note 2).

2. ACTIVE INGREDIENT

2.1 Identity tests

An identity test is required if the identity of the active ingredient is in doubt.

2.1.1 IR spectrum (111/TC/M/2.1, CIPAC D, p. 31).

2.1.2 HPLC (111/TC/M/2.2, CIPAC D, p. 35).

2.2 Chloridazon (111/TC/M/3, CIPAC D, p. 35)

The chloridazon content shall be declared (minimum 910 g/kg) and, when determined, the content obtained shall not differ from that declared by more than ± 25 g/kg.

3. IMPURITIES

3.1 4-Amino-5-chloro-isomer (111/TC/M/3, CIPAC D, p. 35)

Maximum: 60 g/kg.

3.2 Water (MT 30.1, CIPAC F, p. 91)

Maximum: 20 g/kg.

4. PHYSICAL PROPERTIES

4.1 Acidity, alkalinity (MT 31, CIPAC F, p. 96)

Maximum acidity: 1 g/kg calculated as H2SO4
Maximum alkalinity: 1 g/kg calculated as NaOH.

NOTES

1. The spelling in French is chloridazone.

In Canada, Denmark, Poland, USA a former proposal pyrazon has become effective. PAC is the common name in Japan.

2. If additives are present, then they shall be declared in g/kg in general terms. If they interfere with the methods of analysis for the active ingredient or give rise to hazards in processing etc., then their composition and suitable methods of analysis shall be supplied.

Chloridazon technical concentrates

FAO Provisional Specification 111/TK/S/F (1997)

1. DESCRIPTION

The material shall consist of chloridazon, complying with the requirements of FAO specification 111/TC/S/F (1997), together with related manufacturing impurities and shall be a solid of yellow to brown colour free from visible extraneous matter and added modifying agents except for the carrier and auxiliaries needed for the final formulation (Note 1).

2. ACTIVE INGREDIENT

2.1 Identity tests

An identity test is required if the identity of the active ingredient is in doubt.

2.1.1 IR spectrum (111/TC/M/2.1, CIPAC D, p. 31).

2.1.2 HPLC method (111/TC/M/2.2, CIPAC D, p. 35).

2.2 Chloridazon (cf. 111/WP/M/3, CIPAC D, p. 35)

The chloridazon content shall be declared and, when determined, the content shall not differ from that declared by more than the following amounts:

Declared content

Permitted tolerance

above 500 g/kg

± 25 g/kg

3. IMPURITIES

3.1 Water (MT 30.1, CIPAC F, p. 91)

Maximum: 50 g/kg.

4. PHYSICAL PROPERTIES

4.1 Acidity, alkalinity (MT 31, CIPAC F, p. 96)

Maximum acidity: 50 g/kg calculated as H2SO4

Maximum alkalinity: 50 g/kg calculated as NaOH.

4.2 pH range (MT 75, CIPAC F, p. 205)

pH range: 5.0 to 10.0.

5. STORAGE STABILITY

5.1 Stability at 54°C (MT 46.1, CIPAC F, p. 149)

After storage at 54 ± 2°C for 14 days, the determined average active ingredient content must not be lower than 97% relative to the determined average content before storage (Note 2) and the product shall continue to comply with 4.1 and 4.2.

NOTES

1. If additives are present, then they shall be declared in g/kg in general terms. If they interfere with the methods of analysis for the active ingredient or give rise to hazards in processing etc., then their composition and suitable methods of analysis shall be supplied.

2. Analysis of the product before and after storage stability test should be carried out at the same time (i.e. after storage) to reduce analytical error.

Chloridazon wettable powders

FAO Provisional Specification 111/WP/S/F (1997)

1. DESCRIPTION

The material shall consist of a homogeneous mixture of technical chloridazon, complying with the requirements of FAO specification 111/TC/S/F (1997), together with the filler(s) and other necessary formulants. It shall be in the form of a fine powder free from visible extraneous matter and hard lumps.

2. ACTIVE INGREDIENT

2.1 Identity test (111/WP/M/2, CIPAC D, p. 37)

An identity test is required if the identity of the active ingredient is in doubt.

2.2 Chloridazon (111/WP/M/3, CIPAC D, p. 37)

The chloridazon content shall be declared (g/kg) and, when determined, the content obtained shall not differ from that declared by more than the following amounts.

Declared content

Permitted tolerance

above 100 up to 250 g/kg

± 6 % of declared content

above 250 up to 500 g/kg

± 5 % of declared content

above 500 g/kg

± 25 g/kg

3. IMPURITIES

3.1 Water (MT 30.1, CIPAC F, p. 91)

Maximum: 50 g/kg.

4. PHYSICAL PROPERTIES

4.1 pH range (MT 75.2, CIPAC F, p. 206)

pH range: 7.0 to 10.0.

4.2 Wet sieve test (MT 59.3, CIPAC F, p. 179)

Maximum: 0.5 % retained on a 75 m m test sieve.

4.3 Suspensibility (MT 15.1, CIPAC F, p. 45) (Notes 1 and 2)

A minimum of 70 % of the chloridazon content found under 2.2 shall be in suspension (Note 3) after 30 minutes in CIPAC Standard Water D at 30°C ± 2°C (Notes 4 and 5).

4.4 Persistent foam (MT 47.1, CIPAC F, p. 152)

Maximum: 20 ml after 1 minute (Note 6).

4.5 Wetting of the product (MT 53.3.1, CIPAC F, p. 164)

It shall be completely wetted in 3 minutes without swirling (Note 7).

5. STORAGE STABILITY

5.1 Stability at 54°C (MT 46.1.1, CIPAC F, p. 149)

After storage at 54 ± 2°C for 14 days, the determined average active ingredient content must not be lower than 97 % relative to the determined average content before storage (Note 8) and the product shall continue to comply with 4.1, 4.2, 4.3 and 4.5.

NOTES

1. The product should be tested at the highest and lowest rates of use recommended by the supplier, provided this does not exceed the conditions given in Method MT 15.1, CIPAC F, p. 45.

2. This test will normally only be carried out after the heat stability test 5.1.

3. Chemical assay is the only fully reliable method to measure the mass of active ingredient still in suspension. However, simpler methods such as gravimetric and solvent extraction determination may be used on a routine basis provided that the methods have been shown to give results equal to those of the chemical assay. In case of dispute the chemical method shall be the "Referee method".

4. Alternatively, if the buyer requires other CIPAC Standard Waters to be used, then this shall be specified when ordering.

5. Unless another temperature is specified.

6. The mass of sample to be used in the test should be at the highest rate of use recommended by the supplier.

7. The properties of chloridazon and the low bulk weight of chloridazon WPs may cause wettabilities that exceed the 1 min. time frame usual for WPs.

8. Analysis of the product before and after storage stability test should be carried out at the same time (i.e. after storage) to reduce analytical error.

Chloridazon water dispersible granules

FAO Provisional Specification 111/WG/S/F (1997)

1. DESCRIPTION

The material shall consist of a homogeneous mixture of technical chloridazon, complying with the requirements of FAO specification 111/TC/S/F (1997), together with carriers and any other necessary formulants. It shall be in the form of granules (Note 1) for application after disintegration and dispersion in water. The product shall be dry, free flowing and free from visible extraneous matter and hard lumps.

2. ACTIVE INGREDIENT

2.1 Identity test (111/WP/M/2, CIPAC D, p. 37)

An identity test is required if the identity of the active ingredient is in doubt.

2.2 Chloridazon (111/WP/M/3, CIPAC D, p. 37) (Notes 2 and 3)

The chloridazon content shall be declared (g/kg) and, when determined (Note 4), the content shall not differ from that declared by more than the following amounts:

Declared content

Permitted tolerance

above 250 up to 500 g/kg

± 5 % of declared content

above 500 g/kg

± 25 g/kg

3. IMPURITIES

3.1 Water (MT 30.1, CIPAC F, p. 91)

Maximum: 50 g/kg.

4. PHYSICAL PROPERTIES

4.1 pH range (MT 75.2, CIPAC F, p. 206)

pH range: 7.0 to 10.0.

4.2 Wetting of the material (MT 53.3.1, CIPAC F, p. 164)

It shall be completely wetted in 30 sec. without swirling (Note 3).

4.3 Wet sieve test (MT 167, CIPAC F, p. 416)

Maximum: 0.5 % retained on a 75 m m test sieve.

4.4 Suspensibility (MT 168, CIPAC F, p. 41) (Notes 5 and 6)

A minimum of 75% of the chloridazon content found under 2.2 shall be in suspension after 30 min. in CIPAC Standard Water D at 30°C ± 2°C (Notes 7 and 8).

4.5 Degree of dispersion (MT 174, CIPAC F, p. 435)

Minimum: 80%.

4.6 Persistent foam (MT 47.1, CIPAC F, p. 152) (Note 9)

Maximum: 20 ml after 1 min.

4.7 Dustiness (MT 171.1, CIPAC F, p. 425) (Note 10)

Maximum: 12 mg collected dust.

4.8 Flowability (MT 172, CIPAC, p. 430)

At least 99 % of the product shall pass through a 5 mm test sieve after 20 liftings of the sieve.

5. STORAGE STABILITY

5.1 Stability at 54°C (MT 46.1.1, CIPAC F, p. 149) (Note 11)

After storage at 54 ± 2°C for 14 days, the determined average active ingredient content must not be lower than 97% relative to the determined average content before storage (Note 12) and the product shall continue to comply with 4.1, 4.3, 4.4, 4.5, 4.7 and 4.8.

NOTES

1. Depending on manufacturing conditions WG may have different forms and particle size ranges. To describe specific products it is recommended to add information about the form (e.g. irregular shape, nearly spherical, cylindrical) and the nominal size range.

2. If the upper limit was exceeded due to excessive desiccation, the material may be acceptable after moisture equilibration under appropriate storage conditions.

3. The method has been developed for water dispersible powder. It was proven suitable for water dispersible granules as well.

4. If additives interfere with the CIPAC method for chloridazon WPs, then the composition of the additives and suitable methods for chloridazon analysis shall be supplied.

5. Chemical assay is the only fully reliable method to measure the mass of active ingredient still in suspension. However, simpler methods such as gravimetric and solvent extraction determination may be used on a routine basis provided that these methods have been shown to give results equal to those of the chemical assay. In case of dispute the chemical method shall be the "Referee method".

6. The product should be tested at the highest and lowest use concentration recommended by the supplier, provided this does not exceed the conditions given in method MT 168.

7. Alternatively, if the buyers require other CIPAC Standard Waters to he used, then this shall be specified when ordering.

8. Unless another temperature is specified.

9. The mass of sample to be used in the test should be specified at the highest rate of use recommended by the supplier.

10. The optical method (MT 171.2) usually shows good correlation to the gravimetric method (MT 171.1) and can therefore be used as an alternative where the equipment is available. Where the correlation is in doubt, it must be checked with the product to be tested. In case of dispute, the gravimetric method shall be used. The dustiness of a chloridazon WG should not be more than 12 mg collected dust with the gravimetric method. This corresponds to a dust value of approximately 10 resulting from the optical method.

11. CIPAC MT 46.1.1 was meant originally for water dispersible powders. It was proven suitable for water dispersible granules, as well. Excessive desiccation can impair the active ingredient content range and the properties of the product. It may he necessary to seal the beaker in metal foil.

12. Analysis of the product before and after storage stability test should be carried out at the same time (i.e. after storage) to reduce analytical error.

Chloridazon suspension concentrates

FAO Provisional Specification 111/SC/S/F (1997)

1. DESCRIPTION

The material shall consist of a suspension of fine particles of technical chloridazon, complying with the requirements of the FAO specification 111/TC/S/F (1997) in an aqueous phase together with suitable formulants. After gentle agitation the material shall be homogeneous (Note 1) and suitable for further dilution in water.

2. ACTIVE INGREDIENT

2.1 Identity test (111/SC/M/2, CIPAC D, p. 38)

An identity test is required if the identity of the active ingredient is in doubt.

2.2 Chloridazon (111/SC/M/3, CIPAC D, p. 38)

The chloridazon content shall be declared (g/kg or g/l at 20°C) (Note 2) and, when determined, the content obtained shall not differ from that declared by more than the following amounts:

Declared content

Permitted tolerance

above 100 up to 250 g/l

± 6 % of the declared content

above 250 up to 500 g/l

± 5 % of the declared content

above 500 g/l

± 25 g/l

3. IMPURITIES

Not relevant

4. PROPERTIES

4.1 Mass per millilitre at 20°C (MT 3.3.2, CIPAC F, p. 19) (Note 3)

The range of the mass per millilitre (g/ml) at 20°C shall be declared. Usually 1.1 to 1.3 g/ml.

4.2 pH range (MT 75.2, CIPAC F, p. 206)

pH range: 5.0 to 9.0.

4.3 Pourability (MT 148, CIPAC F, p. 348)

Maximum "residue": 8.0%.

Maximum "rinsed residue": 0.6%.

4.4 Spontaneity of dispersion (MT 160, CIPAC F, p. 391)

A minimum of 75 % of the chloridazon content found under 2.2 shall be in suspension after 5 minutes in CIPAC Standard Water D at 25°C ± 2°C.

Alternatively, if the buyer requires other CIPAC Standard Waters or temperatures to be used, then this shall be specified when ordering.

4.5 Suspensibility (MT 161, CIPAC F, p. 394) (Notes 4 and 5)

A minimum of 75 % of the chloridazon content found under 2.2 shall be in suspension after 30 minutes in CIPAC Standard Water D at 30°C ± 2°C (Note 6).

Alternatively, if the buyers require other CIPAC Standard Waters or temperatures to be used, then this shall be specified when ordering.

4.6 Wet sieve test (MT 59.3, CIPAC F, p. 179)

Maximum: 0.2 % of the product shall be retained on a 75 m m test sieve.

4.7 Persistent foam (MT 47.2, CIPAC F, p. 152) (Note 6)

Maximum: 20 ml after 1 minute.

5. STORAGE STABILITY

5.1 Stability at 0°C (MT 39.1, CIPAC F, p. 128) (Note 7)

After storage at 0 ± 1°C for 7 days, the product shall continue to comply with 4.4, 4.5 and 4.6.

5.2 Stability at 54°C (MT 46.1 CIPAC F, p. 951)

After storage at 54 ± 2°C for 14 days, the determined average active ingredient content must not be lower than 97 % relative to the determined average content before storage (Note 8) and the product shall continue to comply with 4.3, 4.4, 4.5, 4.6 and, if required, with 4.2.

NOTES

1. Before sampling to verify the product quality, inspect the commercial container carefully. On standing, suspension concentrates usually develop a concentration gradient from the top to the bottom of the container. This may even result in the appearance of a clear liquid on the top and/or of sediment on the bottom. Therefore, before sampling, homogenize the product according to the instructions given by the manufacturer or, in the absence of such instructions, by gentle shaking of the commercial container (for example by inverting the closed container several times; large containers must be opened and stirred adequately). After this procedure, the container should not contain a sticky layer of non-dispersed product at the bottom. A suitable and simple method of checking for a non-dispersed sticky layer ("cake") is by probing with a glass rod or any similar device adapted to the size and shape of the container. All the physical and chemical tests must be carried out on a laboratory sample taken after the recommended homogenization procedure.

2. Unless homogenization is carried out carefully, it is possible for the sample to become aerated. This can lead to errors in the determination of the density and in the calculation of the active ingredient content in g/l, if methods other than MT 3.3, CIPAC F, p. 19, are used. If the buyer requires both g/kg and g/l at 20°C then, in case of dispute, the analytical results shall be calculated as g/kg.

3. Instead of using the delicate dilution method MT 3.3.2 for density determination direct measurement using the air comparison pyknometer is mostly preferable. With this alternate method air bubbles will not cause misleading results.

4. This test will normally only be carried out after the heal stability test 5.2.

5. Chemical assay is the only fully reliable method to measure the mass of active ingredient still in suspension. However, simpler methods such as gravimetric and solvent extraction determination may be used on a routine basis provided that these methods have been shown to give results equal to those of the chemical assay. In case of dispute the chemical method shall be the "Referee method".

6. The amount of sample to be used in the test should be specified at the highest rate of use recommended by the supplier.

7. The method has been developed for clear EC and SL formulations. For SCs the volume of visible deposit at the bottom and/or serum at the top of the cone shaped centrifuge tube shall be recorded omitting centrifugation.

8. Analysis of the product before and after storage stability test should be carried out at the same time (i.e. after storage) to reduce analytical error.


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