This specification, which is PART ONE of this publication, is based on an evaluation of data submitted by the manufacturer whose name is listed in the evaluation report (636/2005). It should be applicable to relevant products of this manufacturer, and those of any other formulators who use only TC from the evaluated source. The specification is not an endorsement of those products, nor a guarantee that they comply with the specification. The specification may not be appropriate for the products of other manufacturers who use TC from other sources. The evaluation report (636/2005), as PART TWO, forms an integral part of this publication.

1 Description

The material shall consist of a suspension of fine particles of technical spinosad complying with the requirements of WHO specification 636/TC (February 2007), 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 tests (636/SC/M/2, CIPAC Handbook L, p.121, 2006) The active ingredient shall comply with an identity test and, where the identity remains in doubt, shall comply with at least one additional test.

2.2 Spinosad content (636/SC/M/3, CIPAC Handbook L, p.121, 2006)

The spinosad (spinosyn A + spinosyn D) content shall be declared (g/kg or g/l at 20 ± 2ºC, Note 2) and, when determined, the average content measured shall not differ from that declared by more than the following tolerance:

Declared content, g/kg or g/l at 20 ± 2ºC Tolerance

above 100 up to 250

above 250 up to 500

Note: the upper limit is included in each range

± 6% of the declared content

± 5% of the declared content

3 Physical properties

3.1 pH range (MT 75.3, CIPAC Handbook J, p.131, 2000)

pH range: 6.5 to 8.5.

3.2 Pourability (MT 148.1, CIPAC Handbook J, p.133, 2000)

Maximum "residue": 5%.

3.3 Spontaneity of dispersion (MT 160, CIPAC Handbook F, p.391, 1995)

(Note 3)

A minimum of 75% of the spinosad content found under 2.2 shall be in suspension after 5 min in CIPAC Standard Water D at 30 ± 2°C.

3.4 Suspensibility (MT 184, CIPAC Handbook K, p.142, 2003) (Note 3) A minimum of 70% of the spinosad content found under 2.2 shall be in suspension after 30 min in CIPAC Standard Water D at 30 ± 2°C.

3.5 Wet sieve test (MT 185, CIPAC Handbook K, p.148, 2003) (Note 4)

Maximum: 0.5% of the formulation shall be retained on a 75 Nm test sieve.

3.6 Persistent foam (MT 47.2, CIPAC Handbook F, p.152, 1995) (Note 5)

Maximum: 20 ml after 1 min.

4 Storage stability

4.1 Stability at 0°C (MT 39.3, CIPAC Handbook J, p.126, 2000)

After storage at 0 ± 2°C for 7 days, the formulation shall continue to comply with the clauses for:

– suspensibility (3.4);

– wet sieve test (3.5).

4.2 Stability at elevated temperature (MT 46.3, CIPAC Handbook J, p.128, 2000)

After storage at 54 ± 2°C for 14 days, the determined average active

ingredient content must not be lower than 95% relative to the determined average content found before storage (Note 6) and the formulation shall continue to comply with the clauses for:

– pH range (3.1),

– pourability (3.2),

– spontaneity of dispersion (3.3),

– suspensibility (3.4),

– wet sieve test (3.5).

Note 1 Before sampling to verify the formulation 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 formulation 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 nondispersed matter at the bottom. A suitable and simple method of checking for a nondispersed sticky layer "cake" is by probing with a glass rod or 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.

Note 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 mass per millilitre and in calculation of the active ingredient content (in g/l) if methods other than CIPAC MT 3.3 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.

Note 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 these methods have been shown to give equal results to those of the chemical assay method. In case of dispute, the chemical method shall be the referee method.

Note 4 This test detects coarse particles (e.g. caused by crystal growth) or agglomerates (crust formation) or extraneous materials which could cause blockage of spray nozzles or filters in the spray tank.

Note 5 The mass of sample to be used in the test should be specified at the application rate of use recommended by the supplier.

Note 6 Samples of the formulation taken before and after the storage stability test should be analyzed concurrently after the test in order to reduce the analytical error.

 

This specification, which is PART ONE of this publication, is based on an evaluation

of data submitted by the manufacturer whose name is listed in the evaluation reports

(636/2005, 636/2007). It should be applicable to relevant products of this

manufacturer, and those of any other formulators who use only TC from the

evaluated source. The specification is not an endorsement of those products, nor a

guarantee that they comply with the specification. The specification may not be

appropriate for the products of other manufacturers who use TC from other sources.

The evaluation reports (636/2005, 636/2007), as PART TWO, form an integral part of

this publication.

1 Description (Note 1)

The material shall consist of two homogeneous layers of technical spinosad

complying with the requirements of WHO specification 636/TC (February

2007) together with carriers and any other necessary formulants. It shall be in

the form of tablets for direct application. The formulation shall be of dry,

unbroken tablets, free from visible extraneous matter.

2 Active ingredient

2.1 Identity tests (636/DT/M/2, CIPAC Handbook, Notes 2 and 3)

The active ingredient shall comply with an identity test and, where the identity

remains in doubt, shall comply with at least one additional test.

2.2 Spinosad content (636/DT/M/3, CIPAC Handbook, Notes 2 and 3)

The spinosad (spinosyn A + spinosyn D) content shall be declared (74.8 g/kg)

and, when determined, the average measured content shall not differ from

that declared by more than ±10%.

2.3 Tablet dose uniformity (636/DT/M/3, CIPAC Handbook, Notes 2 and 3)

The spinosad (spinosyn A + spinosyn D) content, measured separately in 20

tablets shall have a relative standard deviation (RSD) of not more than 10%.

3 Physical properties

3.1 Tablet integrity (Notes 2, 4 and 5)

No broken tablets observed on inspection.

3.2 Attrition resistance (MT178.2, CIPAC Handbook H, p.304, 1998) (Notes 2

and 5)

Minimum: 98% attrition resistance.

_

4 Storage stability

4.1 Stability at elevated temperature (MT 46.3, CIPAC Handbook J, p.128,

2000)

After storage at 54 ± 2°C for 14 days without pressure (Note 6), the

determined average active ingredient content must not be lower than 95%

relative to the determined average content found before storage (Note 7) and

the formulation shall continue to comply with the clauses for:

– tablet integrity (3.1),

– attrition resistance (3.2).

Note 1 The tablets are round, 12 mm in diameter, approximately 6 mm in height, weighing approximately 1.34 g. The tablets consist of two layers, one contains an effervescent system with its water-soluble acid component present in excess, a combination intended to aid gentle dispersion in water after application and to provide a relatively quick initial release of the

active ingredient into the water. The other layer provides a slower release of spinosad to

maintain an appropriate concentration over an extended period of time. The tablets are not intended for dispersion in water prior to application.

Note 2 For determination of identity (2.1) and spinosad content (2.2), a sufficient quantity of entire tablets may be milled and thoroughly mixed to provide an homogeneous powder, prior to weighing portions for analysis. Alternatively, the spinosad content may be calculated as the average g/kg obtained from the analyses of 20 separate tablets (2.3) and identity may be confirmed using one or more individual tablets. Tablets to be analyzed individually must also be crushed or milled to a fine powder, prior to extraction.

To determine tablet integrity (3.1), carefully remove all 250 tablets from a pack and count

those that are broken. Unbroken tablets (from test 3.1) should be used in the tests for attritionresistance (3.2) and storage stability (4.1).

Note 3 Methods for the identification and determination of spinosad content in TC, SC and GR formulations were published in CIPAC Handbook L, pages 123-127 (2006). The method for analysis of tablet (DT) formulations was adopted as a full CIPAC method in 2007. Prior to publication of the Handbook, copies of the DT method may be obtained through the CIPAC website, http://www.cipac.org/prepubme.htm.

Note 4 Visual observation only. At least one pack of 250 tablets should be inspected.

Note 5 Prior to testing, tablets should be retained within the moisture-barrier packaging to preserve the integrity of the effervescent system within the tablets.

Note 6 Without pressure means that the test is done as specified by CIPAC method MT 46.3, submethod 2 for solid formulations (no pressure is applied to the sample during its ageing). Tablets are to be retained within the sealed moisture-barrier packaging throughout the 14 days storage at 54C.

Note 7 Analysis of the formulation before and after the storage stability test should be carried out concurrently (i.e. after storage), to minimize the analytical error.