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  • PHYSICAL STABILITY OF AGROCHEMICAL FORMULATIONSFrom Suspension to emulsion

    Presented by: Dr. Martin Viertelhaus, BASF SE

    13th June 2017

    Brings to you the webinar on...

  • Your Speaker

    Dr. Martin Viertelhaus is Research Scientist Crystalline Materials and Polymorphism atBASF SE, Ludwigshafen, Germany.

    His expertise is in the field of solid state development and physicochemicalcharacterization of active ingredients: e.g. agrochemical, pharmaceutical andperformance chemicals. During his professional career, he worked for pharmaceuticaland chemical companies as well as for a service provider.

    Dr. Martin Viertelhaus

    The audience is muted and send the questions to info@crystallizationsystems.com

    This webinar will last 45 minutes

    This webinar is being recorded and will be made available

    mailto:info@crystallizationsystems.com

  • TECHNOBIS CRYSTALLIZATION SYSTEMS Privately owned company 50 employees Located in Alkmaar, The Netherlands Leader in 3 major markets: Pharma, Agro

    and Fine Chemicals

    Portfolio 3 products for: formulation,

    process optimization andcrystallization related research

    http://www.lilly.com/index.htmlhttp://www.lilly.com/index.htmlhttp://www.gsk.com/index.htmhttp://www.gsk.com/index.htmhttp://www.lilly.com/index.htmlhttp://www.gsk.com/index.htm

  • Products

    Discover Early stage salt, polymorph screening Single crystal growth

    Screen Solubility, MSZW Phase diagrams Selecting solvents Polymorphs, Salt and Co-crystals

    screening

    Optimize Form control Habit control Particle size Process optimization Formulation

    Working volume:0.5 1 ml

    16 reactors

    Working volume:2.5 5 ml8 reactors

    Working volume:0.06 0.1 ml32 reactors

  • 150 Jahre

    Dr. Martin Viertelhaus

    Physical Stability of Agrochemical FormulationsFrom Suspension to Emulsion

    5

  • Overview

    solid state properties

    agrochemicals and their formulations

    two active ingredients

    plus formulants

    re-crystallization

    Agrochemical Formulation, Suspension, Emulsion, M. Viertelhaus 6

  • Solid State Properties

    solid state properties depend on the crystal form

    knowledge about (meta)stable solid forms of active ingredients (AIs) is important for production formulation storage application

    Agrochemical Formulation, Suspension, Emulsion, M. Viertelhaus 7

    lead optimization development registration production

    marketing/ sales IP protection

    new generation products

  • Formulation and Solid State of Active Ingredient

    Agrochemical Formulation, Suspension, Emulsion, M. Viertelhaus 8

  • Agrochemicals

    indications fungicides (F)

    herbicides (H)

    insecticides (I)

    product application

    formulated concentrate

    dilution in water(compatibility with water)

    application to fields

    Agrochemical Formulation, Suspension, Emulsion, M. Viertelhaus 9

  • Agrochemical Formulation

    formulation development high active loading

    low viscosity (liquid)

    easy to dissolve/disperse (solid) storage stability 2 years at ambient temperature 2 weeks @ 54C (accelerated)

    application stability

    robustness in biological tests

    Agrochemical Formulation, Suspension, Emulsion, M. Viertelhaus 10

  • Formulation Stability

    production mixing properties viscosity

    storage sedimentation, re-suspension agglomeration, crystallization

    dilution and application mixing crystal growth

    Agrochemical Formulation, Suspension, Emulsion, M. Viertelhaus 11

    crystalline active on leaf surface

  • Agrochemical Formulation

    63 different classifications of formulations

    active is

    solid in solid mixture suspended in liquid dissolved in water or solvent

    solid state properties of active of interest in formulation

    after dilution

    during application on the plant

    Agrochemical Formulation, Suspension, Emulsion, M. Viertelhaus 12

    int. code description

    EC emulsifiable concentrateSL soluble concentrateDC dispersible concentrate

    SC suspension concentrate

    SE suspo-emulsion

    OD dispersion in oil

    EW emulsion, oil in water

    ME micro-emulsion

    CS capsule suspension

    WG water dispersible granule

    WP wettable powderCropLife International, Technical Monograph n2

  • Agrochemical FormulationActive x Active

    the majority of agrochemical formulations include more than one active ingredient

    up to four actives ingredients

    less resistance building

    broader application window

    cooperative effects

    stronger curative effect

    13Agrochemical Formulation, Suspension, Emulsion, M. Viertelhaus

    soybean rust

  • Two Active Ingredients

    2 solid actives:

    pre-formulation

    active 1+

    active 2

    mixtureof AIs

    eutecticmelt co-crystal

    Agrochemical Formulation, Suspension, Emulsion, M. Viertelhaus 14

  • Active I Active IIEutectic

    15Agrochemical Formulation, Suspension, Emulsion, M. Viertelhaus

    40.00

    50.00

    60.00

    70.00

    80.00

    90.00

    100.00

    110.00

    120.00

    40

    50

    60

    70

    80

    90

    100

    110

    120

    0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

    T / CT / C

    x Active II

    Tm/CTm(AI form II)/CTm(AII)/CTm(AI form I)/C

    melting points of separate actives above 80C

    mixed actives: eutectic melting at 62.6C

  • Suspension Stability Experiment

    pre-formulation or final formulation

    further reduction of melting pointconversion point from suspension to emulsion

    mixture of active ingredients and solvents/blank formulations stirring temperature rise pictures

    Agrochemical Formulation, Suspension, Emulsion, M. Viertelhaus 16

    Photos taken with Crystalline PV

  • Active I Active IIFormulation Development

    AI I : AI II (g/g)

    Crystalline PV: T ramp 20C/h, bottom stirred

    17

    54.1C 54.2C 54.3C 54.4C 54.5C 54.6C 54.7C 54.8C 54.9C 55.0C 55.1C 55.2C

    58.2C 58.4C 58.6C 58.8C 59.0C 59.2C 59.4C 59.6C 59.8C 60.0C 60.0C 60.0C

    solvent A

    solvent B

    Agrochemical Formulation, Suspension, Emulsion, M. Viertelhaus

    Photos taken with Crystalline PV

  • Final Formulation

    solids: eutectic melting at 62.6C

    eutectic melting temperature reduced to 59C in solvent A 55C in solvent B

    formulation physically not stableagglomeration, sedimentation

    decision:no suspension concentrate

    18Agrochemical Formulation, Suspension, Emulsion, M. Viertelhaus

  • Two Active Ingredientsplus Liquid Formulants

    Agrochemical Formulation, Suspension, Emulsion, M. Viertelhaus 19

    active 1+

    active 2mixtureof AIs

    liquid plus solid(e.g. eutectic +excess solid)

    eutecticmelt co-crystal

    active 1+ active 2

    + formulants

    mixture of AIsin formulation

    (SC)

    liquid plus solid(excess solid

    active) emulsion

    co-crystalin liquid

    formulation (SC)

    solution

  • Re-Crystallization

    temperature cycling to enhance the chance to crystallize

    crystal size

    crystal morphology

    individual experiments and temperature programs

    20Agrochemical Formulation, Suspension, Emulsion, M. Viertelhaus

    experiment: Crystalline PV, T ramp -7.5C/h, bottom stirred

    28.3C 28.0C 27.8C 27.6C 27.3C 27.0C 26.9C 26.5C 26.3C 26.0C

    Photos taken with Crystalline PV

  • Physical Stability of Agro Formulations

    investigation regarding solid state properties of actives model formulations final formulation

    can explain observation of farmers/users in final formulation

    can avoid running for the wrong formulation type

    21Agrochemical Formulation, Suspension, Emulsion, M. Viertelhaus

    dissolution

    re-crystallization

    phase transformation

  • Acknowledgement

    Agrochemical Formulation, Suspension, Emulsion, M. Viertelhaus 22

    Martin ViertelhausBASF SE

    Ludwigshafen

    Christian Sowa

    Rolf Hellmann

    +

    +

  • Any follow up questions or other enquiries: info@crystallizationsystems.com

    Participants will be sent details of how to access a recording of this webinar

    QUESTIONS?

    Webinar organized by

    www.crystallizationsystems.com

    mailto:info@crystallizationsystems.com

    PHYSICAL STABILITY OF AGROCHEMICAL FORMULATIONS From Suspension to emulsionYour SpeakerTECHNOBIS CRYSTALLIZATION SYSTEMSProductsPhysical Stability of Agrochemical FormulationsFrom Suspension to EmulsionOverviewSolid State PropertiesFormulation and Solid State of Active IngredientAgrochemicalsAgrochemical FormulationFormulation StabilityAgrochemical FormulationAgrochemical FormulationActive x ActiveTwo Active IngredientsActive I Active IIEutecticSuspension Stability ExperimentActive I Active IIFormulation DevelopmentFinal FormulationTwo Active Ingredientsplus Liquid FormulantsRe-Crystallization Physical Stability of Agro FormulationsAcknowledgementSlide Number 23

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