Classifications

• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
  • C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
  • C07C227/38—Separation; Purification; Stabilisation; Use of additives
  • C07C227/44—Stabilisation; Use of additives
• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
  • C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
  • C07C227/38—Separation; Purification; Stabilisation; Use of additives
  • C07C227/40—Separation; Purification
  • C07C227/42—Crystallisation
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/16—Organic compounds
  • C11D3/26—Organic compounds containing nitrogen
  • C11D3/33—Amino carboxylic acids
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
  • C11D7/22—Organic compounds
  • C11D7/32—Organic compounds containing nitrogen
  • C11D7/3254—Esters or carbonates thereof

Definitions

• the present invention deals with a process for preparing a solid, preferably storage stable, composition comprising at least one aminocarboxylate complexing agent, comprising the follow- ing steps: a) Providing an initial aminocarboxylate composition with a content of 0.1 and 50 % by weight, preferably 1 to 25 % by weight, solid particles of aminocarboxylates of orthorhom- bic crystal system, relative to the total initial solid composition, b) Increasing the relative humidity (rH) to at least 50% and/or adding at least 1 % by weight of water or of an aqueous solution (SO) or slurry (SL) with a water content of at least 10 % by weight, preferably at least 30% by weight, relative to the total weight of the aqueous solution or slurry, c) keeping the obtained composition at a temperature of 20 to 95 °C over a period of 1 mi- nute to 5 months, d) optionally drying the resulting solid composition, preferably to a residual moisture content of less than 20 %,
• MGDA methyl glycine diacetic acid
• GLDA glutamic acid diacetic acid
• ADW automatic dishwashing
• phosphate-free laundry detergents and phosphate-free ADW formulations For shipping such complexing agents, in most cases either solids such as granules are being ap- plied or aqueous solutions.
• Solid compositions e. g. granules and powders
• solid have the advantage of being essentially water- free. That means that in case of shipping, no water has to be shipped, and costs for extra weight can be avoided.
• the term “solid” has its usual meaning, i. e. refers to the state of a compound or composition at room temperature, i. e. at 20 °C).
• EP 0 845 456 A2 describes a process for preparing a crystalline solid consisting essentially of certain glycine-N,N-diacetic acid derivatives by adjusting the water content of the initial mass containing glycine-N,N-diacetic acid derivatives to a range of 10 to 30 % by weight and subsequently inducing crystallisation.
• MGDA powder and MGDA solution are mixed and heated, then a crystalline solid resulted.
• inorganic peroxides which are, together with complexing agents like MGDA, frequently used in detergent formulations, for example dishwashing detergent formulations, e.g. ADW formulations.
• Exam- ples of inorganic peroxides are sodium perborate, sodium persulfate and in particular sodium percarbonate.
• One way known in the art to improve the storage stability e. g. of MGDA is an increase of the degree of crystallinity of the complexing agent, as well as an increase of amount of MGDA in orthorhombic crystal form.
• the inventive process for preparing a solid, preferably storage stable, composition comprising at least one aminocarboxylate complexing agent comprises the following steps: a) Providing an initial aminocarboxylate composition with a content of 0.1 and 50 % by weight, preferably 1 to 25 % by weight, solid particles of aminocarboxylates of orthorhom- bic crystal system, relative to the total initial solid composition, b) Increasing the relative humidity (rH) to at least 50% and/or adding at least 1 % by weight of water or of an aqueous solution (SO) or slurry (SL) with a water content of at least 10 % by weight, preferably at least 30% by weight, relative to the total weight of the aqueous solution or slurry, c) keeping the obtained composition at a temperature of 20 to 95 °C over a period of 1 mi- nute to 5 months, preferably 2 minutes to 1 month, optionally, d) drying the resulting solid composition, preferably to a residual moisture content of less than 20 %,
• water is added by setting the relative humidity to a range of 50 to 90%, preferably 60 to 85%, and/or by adding at least 1% by weight, preferably 2 to 10 % by weight, of water or of an aqueous solution (SO) or slurry (SL), optionally by spraying the water or aqueous solution (SO) or slurry (SL) onto the initial solid composition.
• SO aqueous solution
• SL slurry
• the solid composition is kept at a temperature of 30 to 95 °C over a period of 30 minutes to 1 month, preferably at 30 to 70°C over a period of 30 minutes to 2 weeks, preferably 30 minutes to 48 h.
• the drying may be done at a temperature in the range from 40° to 240°C, preferably 60° to 150°C, more preferably 60° to 120 °C, and/or until a residual moisture content of less than 18 % by weight, relative to the total weight of the solid composition, is reached.
• the solids content may be determined by Karl-Fischer titration (with regard to water content), Fe-titration (with regard to content of chelating agent, e. g. MGDA) and calculation of the re- maining content (with regard to content of optional polymer).
• the discoloration - which is a yellowing in this case - of the stored mixtures was determined by measuring the b-value of the CIELAB color space (Mach5 measurement device).
• providing solid particles (step a) ) and addition of water (step b) ) may be done simultaneously or consecutively.
• the solid particles (step a) ) are in the form of a powder, granule, crystal, compactate, flake, or agglomerate.
• the inventive process may at least partially be performed in a mixer, belt dryer, kneader, fluid- ized bed dryer, paddle dryer and/or cone dryer.
• the aminocarboxylate complexing agent may be selected from methylglycinediacetic acid (MGDA), (N,N)-Dicarboxymethyl glutamic acid (GLDA), nitrilotriacetic acid (NTA), ethylendia- mine tetraacetic acid (EDTA), ethylenediamine disuccinic acid (EDDS), and their respective alkali salts, preferably sodium salts, more preferably sodium salt of MGDA.
• MGDA methylglycinediacetic acid
• GLDA nitrilotriacetic acid
• EDTA ethylendia- mine tetraacetic acid
• EDDS ethylenediamine disuccinic acid
• the initial solid composition may further comprise up to 40 % by weight, preferably up to 30% by weight, of at least one organic or inorganic compound or mixtures thereof, relative to the total weight of the initial solid composition.
• the aqueous solution (SO) or slurry (SL) further comprises up to 40 % by weight, preferably up to 30% by weight, of at least one organic or inor- ganic compound or mixtures thereof, relative to the total weight of the aqueous solution (SO) or slurry (SL).
• the initial solid composition and/or the aqueous solution (SO) or slurry (SL) may also comprise at least one compound selected from the list consisting of polymers, preferably sulfonated pol- ymers, anti-oxidants, surfactants, colorants, pigments, further complexing agents, organic and inorganic acids and their salts.
• the initial solid composition may contain at least one polymer, e. g. homo-polymer and/or co- polymer.
• the polymer may be selected from homo- and co-polymers of (meth)acrylic acid.
• the initial solid composition may contain at least one anti-oxidant.
• the initial solid composition may contain at least one surfactant which may be selected from non-ionic, zwitterionic, cationic, and anionic surfactants.
• the initial solid composition may contain at least one colorant.
• the initial solid composition may contain one or more complexing agents other than MGDA or GLDA, for example IDS, citrate, EDDS and/or phosphonic acid derivatives.
• complexing agents other than MGDA or GLDA, for example IDS, citrate, EDDS and/or phosphonic acid derivatives.
• the initial solid composition may contain at least one organic acid (or its salt) with a molecular weight of less than 500 g/mol, e. g. formic acid, acetic acid and/or citric acid.
• the term “storage stable” solid composition refers to a solid composition (comprising at least one aminocarboxylate complexing agent) in combina- tion with a bleaching agent (e.g. percarbonate) which shows an improved or no yellowing upon storage at elevated temperature (e.g. 35°C) and humidity (e.g. 75% r.H.).
• a bleaching agent e.g. percarbonate
• the yellowing is de- termined by a change in b-value (CIELAB color space, Mach5 measurement device).
• inventive solid compositions exhibit overall advantageous proper- ties including but not limited to an excellent yellowing behavior, especially in the presence of bleaching agents. They are therefore excellently suitable for the manufacture of cleaning agents that contain at least one bleaching agent, such cleaning agent hereinafter also being referred to as bleach.
• inventive solid compositions are suitable for the manufacture cleaning agent for fibers or hard surfaces wherein said cleaning agent contains at least one peroxy com- pound.
• compositions e. g. powders or granules
• Inventive solid compositions may easily be converted into compac- tates and into agglomerates.
• Another aspect of the present invention is therefore the use of a solid composition for the manu- facture of a cleaning agent that contains at least one bleaching agent, and in particular for the manufacture of cleaning agent for fibers or hard surfaces, wherein said cleaning agent contains at least one peroxy compound.
• Another aspect of the present invention is a process for making at a cleaning agent by combining at least one inventive solid composition with at least one bleaching agent, preferably at least one peroxy compound.
• Another aspect of the present inven- tion is a cleaning agent, hereinafter also being referred to as inventive cleaning agent.
• inventive cleaning agents contain at least one bleaching agent and at least one inventive solid composi- tion (e. g. granule or powder). Inventive cleaning agents show a reduced tendency for yellowing and therefore have an extended shelve-life.
• suitable peroxy compounds are sodium perborate, anhydrous or for example as monohydrate or as tetrahydrate or so-called dihydrate, sodium percarbonate, anhydrous or, for example, as monohydrate, hydrogen peroxide, persulfates, organic peracids such as peroxylau- ric acid, peroxystearic acid, peroxy-a-naphthoic acid, 1 ,12-diperoxydodecanedioic acid, per- benzoic acid, peroxylauric acid, 1 ,9-diperoxyazelaic acid, diperoxyisophthalic acid, in each case as free acid or as alkali metal salt, in particular as sodium salt, also sulfonylperoxy acids and cationic peroxy acids.
• organic peracids such as peroxylau- ric acid, peroxystearic acid, peroxy-a-naphthoic acid, 1 ,12-diperoxydodecanedioic acid, per- be
• peroxy compound is selected from inorganic percarbonates, persul- fates and perborates.
• sodium percarbonates are 2 Na 2 CO 3 .3 H 2 O 2 .
• sodium perborate are ( Na 2 [B(OH) 2 ( O 2 )] 2 ), sometimes written as NaBO2-O2'3H2O instead.
• cleaning agents includes compositions for dishwashing, especially hand dishwash and automatic dishwashing and ware-washing, and compositions for hard surface cleaning such as, but not limited to compositions for bathroom cleaning, kitchen cleaning, floor cleaning, de- scaling of pipes, window cleaning, car cleaning including truck cleaning, furthermore, open plant cleaning, cleaning-in-place, metal cleaning, disinfectant cleaning, farm cleaning, high pressure cleaning, and in addition, laundry detergent compositions.
• Such cleaning agents may be liquids, gels or preferably solids at ambient temperature, solids cleaning agents being preferred. They may be in the form of a powder or in the form of a unit dose, for example as a tablet or pouch.
• inventive cleaning agents may contain in the range of from 2 to 50 % by weight of inventive solid composition and in the range of from 0.5 to 15 % by weight of bleach.
• Percentages are based on the solids content of the respective inventive cleaning agent.
• Inventive solid compositions are excellently suited for the manufacture of laundry detergents or cleaners.
• inventive cleaning agents may contain further ingredients such as one or more surfactants that may be selected from non-ionic, zwitterionic, cationic, and anionic surfactants.
• Other ingredients that may be contained in inventive cleaning agents may be selected from bleach activators, bleach catalysts, corrosion inhibitors, sequestering agents other than chelating agent (A), en- zymes, fragrances, dyestuffs, antifoams, and builders.
• Particularly advantageous inventive cleaning agents may contain one or more complexing agents other than MGDA or GLDA.
• Advantageous detergent compositions for cleaners and ad- vantageous laundry detergent compositions may contain one or more sequestrant (chelating agent) other than a mixture according to the present invention.
• sequestrants other than a mixture according to the present invention are IDS (iminodisuccinate), citrate, phosphon- ic acid derivatives, for example the disodium salt of hydroxyethane-1,1-diphosphonic acid (“HEDP”), and polymers with complexing groups like, for example, polyethyleneimine in which 20 to 90 mole-% of the N-atoms bear at least one CH2COO' group, and their respective alkali metal salts, especially their sodium salts, for example IDS-Na4, and trisodium citrate, and phos- phates such as STPP (sodium tripolyphosphate).
• IDS aminodisuccinate
• citrate citrate
• phosphon- ic acid derivatives for example the disodium salt of hydroxyethane-1,1-diphosphonic acid (“HEDP”)
• HEDP hydroxyethane-1,1-diphosphonic acid
• polymers with complexing groups like, for example, polyethyleneimine in which 20 to
• the sum a + b + d is preferably in the range of from 5 to 100, even more preferably in the range of from 9 to 50.
• R 6 is -(CH 2 ) 2 -R 5 ,
• Mixtures of two or more different nonionic surfactants may also be present.
• surfactants that may be present are selected from amphoteric (zwitterionic) surfactants and anionic surfactants and mixtures thereof.
• amphoteric surfactants are those that bear a positive and a negative charge in the same molecule under use conditions.
• Preferred examples of amphoteric surfactants are so- called betaine-surfactants.
• Many examples of betaine-surfactants bear one quaternized nitrogen atom and one carboxylic acid group per molecule.
• a particularly preferred example of amphoter- ic surfactants is cocam idopropyl betaine (lauramidopropyl betaine).
• Suitable anionic surfactants are alkali metal and ammonium salts of C 8 -C 18 -alkyl sulfates, of C 8 -C 18 -fatty alcohol polyether sulfates, of sulfuric acid half-esters of ethoxylated C4- Ci2-alkylphenols (ethoxylation: 1 to 50 mol of ethylene oxide/mol), C 12 -C 18 sulfo fatty acid alkyl esters, for example of C 12 -C 18 sulfo fatty acid methyl esters, furthermore of Ci2-Ci8-alkylsulfonic acids and of C 10 -Cis-alkylarylsulfonic acids.
• Suitable anionic surfactants are soaps, for example the sodium or potassi- um salts of stearoic acid, oleic acid, palmitic acid, ether carboxylates, and alkylether phos- phates.
• laundry detergent compositions contain at least one anionic surfactant.
• inventive cleaning agents that are determined to be used for hard surface cleaning may contain 0.1 to 60 % by weight of at least one surfactant, selected from anionic surfactants, amphoteric surfactants and amine oxide surfactants.
• inventive cleaning agents do not contain any anionic detergent.
• Inventive cleaning agents may comprise one or more corrosion inhibitors.
• corrosion inhibitors include those compounds which inhibit the corrosion of metal.
• suitable corrosion inhibitors are triazoles, in particular benzotriazoles, bisbenzotria- zoles, aminotriazoles, alkylaminotriazoles, also phenol derivatives such as, for example, hydro- quinone, pyrocatechol, hydroxyhydroquinone, gallic acid, phloroglucinol or pyrogallol.
• inventive cleaning agents comprise in total in the range from 0.1 to 1 .5% by weight of corrosion inhibitor.
• Inventive cleaning agents may comprise one or more builders, selected from organic and inor- ganic builders.
• suitable inorganic builders are sodium sulfate or sodium carbonate or silicates, in particular sodium disilicate and sodium metasilicate, zeolites, sheet silicates, in particular those of the formula ⁇ -Na 2 Si 2 O 5 , ⁇ -Na 2 Si 2 O 5 , and ⁇ -Na 2 Si 2 O 5 , also fatty acid sul- fonates, a-hydroxypropionic acid, alkali metal malonates, fatty acid sulfonates, alkyl and alkenyl disuccinates, tartaric acid diacetate, tartaric acid monoacetate, oxidized starch, and polymeric builders, for example polycarboxylates and polyaspartic acid.
• organic builders are especially polymers and copolymers other such as (co)polymers (B) and include polymers and copolymers than (co)polymer (B), or one additional (co)polymer (B).
• organic builders are selected from polycarboxylates, for example alkali metal salts of (meth)acrylic acid homopolymers or (meth)acrylic acid copolymers, partially or completely neutralized with alkali.
• Suitable comonomers for (meth)acrylic acid are monoethylenically unsaturated dicarboxylic ac- ids such as maleic acid, fumaric acid, maleic anhydride, itaconic acid and citraconic acid.
• a suitable polymer is in particular polyacrylic acid, which preferably has an average molecular weight M w in the range from 2000 to 40 000 g/mol, preferably 2000 to 10 000 g/mol, in particular 3000 to 8000 g/mol.
• copolymeric polycarboxylates in particular those of acrylic acid with methacrylic acid and of acrylic acid or methacrylic acid with maleic acid and/or fumaric acid, and in the same range of molecular weight.
• Suitable hydrophobic monomers are, for example, isobutene, diisobutene, butene, pentene, hexene and styrene, olefins with 10 or more carbon atoms or mixtures thereof, such as, for ex- ample, 1 -decene, 1 -dodecene, 1 -tetradecene, 1 -hexadecene, 1 -octadecene, 1-eicosene, 1- docosene, 1-tetracosene and 1-hexacosene, C 22 - ⁇ -olefin, a mixture of C 20 -C 24 - ⁇ -olefins and polyisobutene having on average 12 to 100 carbon atoms per molecule.
• Suitable hydrophilic monomers are monomers with sulfonate or phosphonate groups, and also nonionic monomers with hydroxyl function or alkylene oxide groups.
• men- tion may be made of: allyl alcohol, isoprenol, methoxypolyethylene glycol (meth)acrylate, meth- oxypolypropylene glycol (meth)acrylate, methoxypolybutylene glycol (meth)acrylate, methoxy- poly(propylene oxide-co-ethylene oxide) (meth)acrylate, ethoxypolyethylene glycol (meth)acry- late, ethoxypolypropylene glycol (meth)acrylate, ethoxypolybutylene glycol (meth)acrylate and ethoxypoly(propylene oxide-co-ethylene oxide) (meth)acrylate.
• Polyalkylene glycols here may comprise 3 to 50, in particular 5 to 40 and especially 10 to 30 alkylene oxide units per molecule.
• Particularly preferred sulfonic-acid-group-containing monomers here are 1-acrylamido-1 -pro- panesulfonic acid, 2-acrylamido-2-propanesulfonic acid, 2-acrylamido-2-methylpropanesulfonic acid, 2-methacrylamido-2-methylpropanesulfonic acid, 3-methacrylamido-2-hydroxypropane- sulfonic acid, allylsulfonic acid, methallylsulfonic acid, allyloxybenzenesulfonic acid, methal- lyloxybenzenesulfonic acid, 2-hydroxy-3-(2-propenyloxy)propanesulfonic acid, 2-methyl-2-pro- pene-1 -sulfonic acid, styrenesulfonic acid, vinylsulfonic acid, 3-sulfopropyl acrylate, 2-sulfoethyl methacrylate, 3-sulfopropyl methacrylate, sulfome
• Particularly preferred phosphonate-group-containing monomers are vinylphosphonic acid and its salts.
• a further example of builders is carboxymethyl inulin.
• Inventive cleaning agents may comprise one or more antifoams, selected for example from sili- cone oils and paraffin oils.
• zinc salt is selected from ZnO, ZnO aq, Zn(OH)2 and ZnCO 3 . Preference is given to ZnO aq.
• zinc salt is selected from zinc oxides with an aver- age particle diameter (weight-average) in the range from 10 nm to 100 pm.
• inventive cleaning agents comprise in total in the range from 0.05 to 0.4% by weight of zinc salt, based in each case on the dry content of the cleaning agent in question.
• the fraction of zinc salt is given as zinc or zinc ions. From this, it is possible to calculate the counterion fraction.
• inventive cleaning agents are free from heavy met- als apart from zinc compounds.
• this may be understood as meaning that inventive cleaning agents are free from those heavy metal compounds which do not act as bleach catalysts, in particular of compounds of iron and of bismuth.
• "free from” in connection with heavy metal compounds is to be under- stood as meaning that the content of heavy metal compounds which do not act as bleach cata- lysts is in sum in the range from 0 to 100 ppm, determined by the leach method and based on the dry content.
• inventive cleaning agents has, apart from zinc, a heavy metal con- tent below 0.05 ppm, based on the dry content of the formulation in question. The fraction of zinc is thus not included.
• heavy metals are deemed to be all metals with a specific density of at least 6 g/cm 3 with the exception of zinc.
• the heavy metals are metals such as bismuth, iron, copper, lead, tin, nickel, cadmium and chromium.
• inventive cleaning agents comprise no measurable fractions of bismuth compounds, for example less than 1 ppm.
• Inventive cleaning agents are excellent for cleaning hard surfaces and fibres.
• they may be used in dishwashing applications, preferably automatic dishwashing applications.
• inventive cleaning agents comprise one or more further ingredient such as fragrances, dyestuffs, organic solvents, buffers, disintegrants for tab- lets (“tabs”), and/or acids such as methylsulfonic acid.
• further ingredient such as fragrances, dyestuffs, organic solvents, buffers, disintegrants for tab- lets (“tabs”), and/or acids such as methylsulfonic acid.
• exemplary detergent composi- tions for automatic dishwashing detergents can be formulated by mixing the respective compo- nents according to the following Table F.
• Table F Example detergent compositions for automatic dishwashing
• Inventive tablets are preferably made with the help of a machine, for example a tablet press.
• the pelletizing process according to the invention can be carried out by mixing an inventive sol- id composition, e. g. granule or powder, with at least one non-ionic surfactant and optionally one or more further substance and then compressing the mixture to give tablets.
• inventive sol- id composition e. g. granule or powder
• non-ionic surfactant e. g. granule or powder
• optionally one or more further substance optionally one or more further substance
• (M.4) mixture of sodium salt of MGDA amorphous powder and sodium salt of MGDA ortho- rhombic powder;
• (M.4) is a mixture of 50 % by weight (M.2) and 50 % by weight (M.3). 10 g of each product were placed in a ceramic dish and then grinded together.
• the second part was added to a mixer. Then in summary 7% distilled water was sprayed on the samples at 70°C while the samples were stirred continuously. After adding the required amount water, the mixture was stirred for further 3 minutes. Then the mixture was compacted with 20 kN and milled to ⁇ 1 mm (V.2; V.4; V.6).
• V.4 sodium salt of MGDA agglomerate after re-crystallization (V.5) sodium salt of MGDA (94%) + sulfonated acrylic polymer (6%) agglomerate
• the humidity XRD experiments were performed using an Anton Paar CHC plus cryo and humid- ity chamber mounted on a Bruker D8 Advance.
• the data were collected using Cu Kai radiation using a primary Johansson type monochromator.
• the detector Li Kai, Bruker AXS
• the humidity and temperature were set and the first data were collected on reaching these set points.
• the data collection was performed for ten hours per experiment.
• the samples were prepared by taking phase pure samples of monoclinic form (Form I) and or- thorhombic form (Form II) and preparing these for XRD by light manual grinding. The samples were then carefully homogenized by shaking the weighed fractions in a closed sample bottle for 30 seconds. This mixture was then filled into the sample holder and flattened using a glass plate.
• the amorphous content was estimated using an internal standard method 2 . 10 mass% of Corundum was added to the sample and then the relative intensities of Corundum versus Form II used to analyze the recrystallization. The data collection was altered to the angular range of 23° to 26°(2 ⁇ ). Here two reflections are fit to the data. The first reflection at approxi- mately 23.6°(2 ⁇ ) is related to Form II whereas the reflection at 25.4°(2 ⁇ ) is related to Corundum. The temperature and humidity is set and data collected over the same time as the crystalline samples. The initial intensity ratio is used to calibrate the 50% Form II volume fraction. In the subsequent data sets the Form II fraction is determined usign the following ratio:
• I ill is the intensity of the first reflection of the first dataset related to the Form II and I iC or is the intensity of the second reflection of the first dataset related to the Corundum standard.
• the angular range is set to 2-80° (2 ⁇ ) with a step size of 0.02° (2 ⁇ ).
• the inci- dent divergent beam slit is set to 0.1 °.
• a Lynxeye detector is used with an opening angle of 3°.
• Data collection time is optimized to ensure a maximum peak height greater than 50'000 counts per step.
• the data are then analyzed using a Rietveld model containing the crystal structures of orthorhombic and monoclinic forms of Na 3 -MGDA-dihydrate.

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• 2023
  • 2023-08-18 EP EP23757640.0A patent/EP4581010A1/de active Pending
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