DEVICE AND METHOD FOR THE PREPARATION AND ANALYSIS OF A MULTIPLE OF SAMPLE MATERIALS

Description

[0001] The invention relates to a device and a method for the production and analysis of a plurality of test materials, which are samples of a hydraulic binder. State of the art

[0002] Inorganic binders are used in the construction industry at a rate of approximately 4 gigatons annually. The composition of these binders has changed significantly in recent decades. Traditional cements based on Portland cement clinker and sulfate carriers have largely been replaced by sustainable, cost-effectively produced composite cements made from clinker, additives, and sulfate carriers, optimized for specific application properties. Due to the increasing complexity of binder composition, the necessary adjustments to binder particle size, and the required application properties, the financial and time expenditure for product optimization and development has increased. Key performance indicators in product optimization and development include, for example, workability, setting behavior, and strength development.Finally, the performance of the binder in its main application, concrete, must be examined.

[0003] The high material requirements for concrete testing necessitate an early preselection of suitable binder compositions and appropriate binder particle size ranges. Due to the considerable material requirements, the physical analytical methods commonly used in the construction materials industry, as described in EN 196 and EN 206, only allow for the analysis of a small number of samples and are also very time-consuming, for example, due to test ages of up to 28 days. Determining the effect of various parameter variations on the reactivity of the binder is therefore very time-consuming.

[0004] A scientific paper on fly ash is known from KUMAR S ET AL: "Mechanical activation of fly ash: Effect on reaction, structure and properties of resulting geopolymer", CERAMICS INTERNATIONAL, ELSEVIER, AMSTERDAM, NL, Vol. 37, No. 2, 1 March 2011 (2011-03-01), pages 533-541, XP027558930, ISSN: 0272-8842 [found on 2010-10-28].

[0005] From LIU C ET AL: "Effects of the granularity of raw materials on the hydration and hardening process of calcium phosphate cement", BIOMATERIALS, ELSEVIER SCIENCE PUBLISHERS BV., BARKING, GB, Vol. 24, No. 23, 1 October 2003 (2003-10-01), pages 4103-4113, XP004436344, ISSN: 0142-9612, DOI: 10.1016 / S0142-9612(03)00238-2, a scientific paper investigating the effect of particle size on the hydration and hardening of calcium phosphate cement is known.

[0006] From BOHNER M ET AL: "Combining particle size distribution and isothermal calorimetry data to determine the reaction kinetics of alpha-tricalcium phosphatewater mixtures", ACTA BIOMATERIALIA, ELSEVIER, AMSTERDAM, NL, Vol. 2, No. 3, May 1, 2006 (2006-05-01), pages 343-348, XP028009588, ISSN: 1742-7061, DOI: 10.1016 / J.ACTBIO.2006.01.003 [accessed 2006-05-01], the combination of particle size distribution and calorimetry for determining the reaction kinetics of calcium phosphate-water mixtures is known.

[0007] The production of artificial bone material is known from E. FERNA'NDEZ* ET AL: "Production and characterization of new calcium phosphate bone cements in the CaHPO 4 a-Ca 3 (PO 4) 2 system: pH, workability and setting times", JOURNAL OF MATERIALS SCIENCE: MATERIALS IN MEDICINE, Vol. 10, No. 4, January 1, 1999 (1999-01-01), pages 223-230, XP055256369, United States ISSN: 0957-4530, DOI: 10.1023 / A:1008958112257.

[0008] A scientific paper on the rheological and calorimetric behavior of cement mixtures is known from MEDINA C ET AL: "Rheological and calorimetric behaviour of cements blended with containing ceramic sanitary ware and construction / demolition waste", CONSTRUCTION AND BUILDING MATERIALS, ELSEVIER, NETHERLANDS, Vol. 40, December 28, 2012 (2012-12-28), pages 822-831, XP028972565, ISSN: 0950-0618, DOI: 10.1016 / J.CONBUILDMAT.2012.11.112.

[0009] From LIU C ET AL: "Effects of the granularity of raw materials on the hydration and hardening process of calcium phosphate cement", BIOMATERIALS, ELSEVIER, AMSTERDAM, NL, Vol. 24, No. 23, October 1, 2003 (2003-10-01), pages 4103-4113, XP004436344, ISSN: 0142-9612, DOI: 10.1016 / S0142-9612(03)00238-2, a scientific paper on the effect of the granularity of raw materials on the hydration and hardening of calcium phosphate cement is known.

[0010] From CHEUNG J ET AL: "Impact of admixtures on the hydration kinetics of Portland cement", CEMENT AND CONCRETE RESEARCH, PERGAMON PRESS, ELMSFORD, NY, US, Vol. 41, No. 12, March 8, 2011 (2011-03-08), pages 1289-1309, XP028310002, ISSN: 0008-8846, DOI: 10.1016 / J.CEMCONRES.2011.03.005 [accessed 2011-03-10], a scientific paper on the influence of admixtures on the hydration kinetics of Portland cement is known.

[0011] From IRASSAR EF ET AL: "Influence of limestone content, gypsum content and fineness on early age properties of Portland limestone cement produced by inter-grinding", CEMENT AND CONCRETE COMPOSITES, ELSEVIER APPLIED SCIENCE, BARKING, GB, Vol. 33, No. 2, 1 February 2011 (2011-02-01), pages 192-200, XP027587153, ISSN: 0958-9465, a scientific paper investigating Portland cement mixtures of different compositions and degrees of grinding is known. Disclosure of the invention

[0012] Starting from this, the object of the present invention is to provide a device and a method for the production and analysis of a plurality of test materials, which represent samples of a hydraulic binder, whereby a simple and quick analysis of the effect of a variation of different parameters on the reactivity of the binder is made possible.

[0013] This problem is solved according to the invention by a device having the features of independent device claim 1 and by a method having the features of independent method claim 9. Advantageous embodiments are described in the dependent claims.

[0014] A device for producing and analyzing a plurality of test materials comprises, according to a first aspect, a grinding device for grinding material components, at least a first metering device for metering at least one material component into the grinding device, at least a second metering device for metering an excitation liquid to the at least one ground material component, and a homogenization device for homogenizing the material components and the excitation liquid to form a test material. The device further comprises a control device that is at least connected to the grinding device and is configured to vary at least one parameter characteristic of the grinding intensity of the grinding device, such that, in particular, the particle size of the material components is changed. Furthermore, the device comprises at least one measuring device for determining the reactivity of the test material.

[0015] The grinding device preferably comprises a fine mill, in particular a disc vibratory mill, whose rotational speed and grinding time are adjustable. For example, the fine mill is operated automatically and includes an automatic cleaning device. The grinding device further comprises, for example, a vibratory mill, a ball mill, a vertical roller mill, or a bed roller mill.

[0016] Sample materials are hydraulic binders that exhibit varying compositions of different material components, such as clinker, sulfate carriers, or additives. Examples of additives include blast furnace slag, fly ash, pozzolan, limestone, or calcined clay.

[0017] A dosing device for dispensing at least one material component into the grinding device preferably comprises a load cell that automatically feeds a specific quantity of the material component to the grinding device, for example, gravimetrically or volumetrically. The dosing device is connected to the grinding device directly or indirectly via an intermediate storage unit. According to the invention, a dosing device, or at least one dosing device for dispensing a plurality of material components, is arranged for each material component in the grinding device. For example, the dosing device is integrated into the sample feed area of ​​the grinding device. A dosing device for dispensing an excitation liquid to the at least one ground material component comprises, for example, a controllable pump, for example, in the form of a peristaltic pump or pipette. The excitation liquid is, for example, water or an alkaline solution.

[0018] A homogenization device for homogenizing the material components and the excitation liquid to form a test material preferably comprises a vibration device or a stirring device, wherein the homogenization is carried out by vibration or stirring.

[0019] The control unit is designed, for example, to vary the parameters characteristic of the grinding intensity electrically or mechanically. For instance, the desired parameter value is either entered manually at the control unit or determined by the control unit based on other parameters, such as the dosage quantity or particle size of the material components or the material composition.

[0020] A characteristic parameter for the grinding intensity of the grinding device is, for example, the rotational speed, the gap width, or the duration of grinding the material components. The grinding intensity influences the particle size of the material components ground by the grinding device, with a high grinding intensity producing a small particle size and a low grinding intensity producing a large particle size of the ground material components. Therefore, varying the grinding intensity also varies the particle size of the material components.

[0021] To produce a test material, a specific composition of the test material or several test materials is preferably set via the control unit, wherein the proportions of certain material components can be adjusted manually on the control unit or determined by the control unit. The dosing unit doses a predetermined quantity of material components into the grinding unit, in which the material components are ground, for example, individually or together. Preferably, the ground test material is filled into a preferably liquid-impermeable sample container, which is then fed into the homogenization unit. Following the dosing of the excitation liquid to the ground material components in the sample container, the homogenized test material is fed into the measuring unit to determine the reactivity.

[0022] A control device designed to vary at least one parameter characteristic of the grinding intensity of the grinding unit enables the production of a large number of test materials whose particle size varies in a known manner. A large number of test materials of varying fineness can be easily produced and analyzed in the measuring device. This allows for the straightforward determination of the reactivity of the test materials as a function of their particle size, resulting in a high data density with respect to the variation in particle size. A precise analysis, particularly of nonlinear relationships between the reactivity and the particle size of the test material, can be performed, thus enabling reliable optimization of these parameters.

[0023] According to a first embodiment, the measuring device is a calorimetric measuring device, in particular an isothermal heat flow calorimeter. A calorimetric measuring device determines the heat of reaction released by the test material. The released heat of reaction and the course of the heat release over time are characteristic of the reactivity of a test material, in particular a binder. The calorimetric measuring device enables a simple and rapid determination of the reactivity of the test material.

[0024] According to the invention, the control device is connected to the dosing device and is designed to control the dosing quantity of the material component. This allows the quantity of the material components and the particle size of the test material to be varied by means of the control device, whereby a large number of test materials with parameters varied in a known manner, such as particle size and composition of the test material, can be produced, thus enabling an analysis of the reactivity as a function of the composition of the test material.

[0025] According to a further embodiment, at least one dosing device is heatable. This enables the dosing of a sulfate carrier with simultaneous thermal dehydration, thus allowing the targeted adjustment and use of partial or complete sulfate carriers in the test materials.

[0026] The device also features a crushing unit located upstream of the grinding unit. This crushing unit enables the pre-crushing of material components, such as granules with a size of approximately 3-10 mm. Furthermore, the crushing unit increases the dosing accuracy of material components with a large particle size.

[0027] According to another embodiment, the device includes a rheometric measuring device for determining the rheological properties of the test material. Rheometric measuring methods enable a simple determination of the dependence of the rheometric properties of the test material on parameters such as grain size and composition.

[0028] According to a further embodiment, the device has a sample storage unit with a plurality of sample containers for holding a sample material. Such a sample storage unit enables the simultaneous analysis of a plurality of sample containers with sample materials in a measuring device, such as a calorimetric or rheological measuring device. This significantly reduces the time required for the analysis of a plurality of sample materials.

[0029] According to a further embodiment, the measuring device is designed in such a way that it determines the reactivity of a plurality of test materials simultaneously.

[0030] According to a further embodiment, the device also includes a metering device downstream of the grinding unit for dosing at least one cement additive to the at least one ground material component. Preferably, the control unit is connected to the metering unit so that the amount of cement additive can be adjusted via the control unit. Cement additives include, for example, grinding aids such as DEG (diethylene glycol) or TEA (triethanolamine), or organic or inorganic additives that modify cement properties (e.g., TIPA, CaCl₂).

[0031] The control unit is preferably connected to the dosing unit for dispensing the excitation fluid, so that the amount of excitation fluid can be controlled via the control unit and the reactivity of the sample material can be determined as a function of the amount of excitation fluid. Dosing is carried out, for example, via peristalsis or a pipette.

[0032] The device is preferably arranged in a temperature-controlled isothermal environment, such as a laboratory. This allows, for example, if the measuring device includes an isothermal heat flow calorimeter, the thermostat of the measuring device to be relieved of some of its load, whereby the temperature required for optimal measurement is maintained throughout the entire device.

[0033] The claimed invention includes a method for producing and analyzing a plurality of sample materials which are samples of a hydraulic binder, according to claim 9.

[0034] The advantages described above with reference to the device apply in a procedurally equivalent manner to the method for the production and analysis of a plurality of test materials.

[0035] According to a first embodiment, in step b) the rotational speed of the grinding device and / or the grinding time of at least one material component is varied.

[0036] Furthermore, according to another embodiment, the rheological properties of the majority of test materials are determined.

[0037] According to a further embodiment, at least one material component is broken before step b).

[0038] According to a further embodiment, step a) includes heating at least one material component.

[0039] Before step d), according to a further embodiment, the particle size of at least some of the ground material components is determined. Determining the fineness or particle size distribution of the sample, for example using sieves or a laser granulometer, allows the measurement results to be correlated with a particle size parameter and facilitates the easy implementation of the newly developed material in industrial production. Preferred embodiments of the invention

[0040] The invention is explained in more detail below with reference to several exemplary embodiments and the accompanying figures. Fig. 1 shows a schematic representation of a device for analyzing a test material according to one embodiment. Fig. 2 shows a schematic representation of a device for analyzing a test material according to another embodiment.

[0041] Fig. 1 Figure 1 shows a schematic representation of a device 10 for analyzing a sample material. The analysis device 10 has, by way of example, three containers 12, 14, and 16, each containing a material component. The representation of three containers 12, 14, and 16 is only exemplary; it is conceivable to provide a plurality of containers, each containing a material component, in the analysis device 10.

[0042] The material components are primarily components of a binder, such as cement. For example, clinker, such as Portland cement clinker or sulfoaluminate clinker, is used with a sulfate carrier and additives to produce binders. A sulfate carrier can be, for example, gypsum, hemihydrate, anhydrite, or other substances with an elevated SO₃ content. Additives include, for example, latent hydraulic materials, granulated blast furnace slag, lignite fly ash, silica dust, or pozzolans, such as bituminous coal fly ash, natural pozzolans, synthetic pozzolans, or filler materials such as limestone. The material components are stored in containers 12, 14, and 16, preferably as crushed material with a particle size of up to 3 mm, as powder with a particle size of up to approximately 0.09 mm, or as granules with a particle size of approximately 3 to 10 mm.

[0043] The analytical device 10 further comprises a first dosing device 18, which is connected to the containers 12, 14, and 16. The dosing device 18 is, for example, a load cell, a balance, or a volumetric measuring device. The dosing device dispenses a specific quantity of the material components from the respective container 12, 14, or 16. The dosing accuracy of the dosing device, based on the total sample weight, is approximately 0.01–1%, preferably 0.007–0.25%, and most preferably approximately 0.5%.

[0044] A grinding unit 20 is connected downstream of the dosing unit 18. The grinding unit 20 is, for example, a disc mill or a vibratory mill. The dosing unit 18 doses a specific quantity of a material component from one of the containers 12, 14, and 16 into the grinding unit 20. The material components are fed, for example, directly from one of the containers 12, 14, or 16 to the grinding unit 20 via the dosing unit 18, or they are combined in an intermediate storage area (not shown) and then fed together to the grinding unit 20.

[0045] The grinding device 20 is connected to a further optional dosing device 22 as well as a homogenization device 24, a second dosing device 26 for dosing an excitation liquid and a sample storage 30 with a plurality of sample containers 28.

[0046] The analysis device 10 also includes a calorimetric measuring device 32 for determining the reactivity of a sample material and a rheometric measuring device 34 for determining the processing properties of the sample material.

[0047] Furthermore, the analysis device 10 has a control device 38 which is connected to the first dosing device 18, the grinding device 20, the excitation liquid dosing device 26, the homogenizing device 24 and the measuring devices 32 and 34.

[0048] In an analytical procedure using the analytical device 10, a specific composition of the sample material can be set via the control unit 38. The proportions of the material components from the containers 12, 14, 16 in the sample material can, for example, be set manually at the control unit 38 or calculated by the control unit 38 at a predefined interval, so that a plurality of sample materials with a proportion of a material component varying over a specific quantity interval can be analyzed. The control unit 38 is connected to the dosing unit 18 such that the dosing quantity of material components set at the control unit 38 is dosed from the containers 12, 14, 16 to the grinding unit via the dosing unit 18. The material components are then ground individually or together in the grinding unit 20.When the material components are milled together, the material components are processed one after the other in a . Fig. 1 The sample was dosed into the sample container (not shown) and then fed to the grinding device.

[0049] The control unit 38 allows, for example, adjustment of the rotational speed or vibration speed of the grinding unit 20, as well as the duration of the grinding process and thus the grinding intensity. A specific fineness of the sample material can therefore be set at the grinding unit 20 via the control unit 38.

[0050] Following the grinding unit 20, the test material is dosed into a sample container 28 via a dosing device 22. The dosing device 22 determines, for example, the net weight of the test material filled into the sample container 28. For example, the dosing device determines the net weight of the sample container 28, the total weight of the sample container 28 with the test material, and / or the net weight of the test material filled into the sample container 28.

[0051] The sample container is arranged in a sample storage area 30, which has a plurality of sample containers 28, each containing, for example, different sample materials. In the Fig. 1 In the illustrated embodiment, the sample storage comprises sixteen sample containers 28, which are arranged in four rows.

[0052] The steps described above are preferably repeated by varying the parameters controllable by the control device 38, so that a plurality of different sample compositions are arranged in different sample containers 28 in the sample storage 30.

[0053] An excitation liquid is supplied to the sample container 28 via the excitation liquid metering device 26. If one of the material components is Portland cement clinker or sulfoaluminate clinker, water is metered into the sample container 28 as the excitation liquid. If one of the material components is a geopolymer, an alkaline solution is metered into the sample container 28 as the excitation liquid. The excitation liquid metering device 26 includes, for example, a heating device for heating the excitation liquid, in particular to the temperature of the calorimetric measuring device 32. The metering accuracy of the metering device 26 is at most approximately 0.001 to 1%, preferably 0.007 to 0.25%, and most preferably approximately 0.5% of the desired metering quantity.

[0054] In particular, an excitation liquid is dosed to the material components in the sample container 28 via the excitation liquid metering device 26, such that the ratio of liquid to sample material is approximately 0.25 - 1.2, in particular 0.4 - 0.6, particularly preferably 0.45 - 0.55.

[0055] In the homogenization device 24, the excitation liquid and the material components in the sample container are homogenized to form a sample material. The homogenization device 24 includes, for example, a vibration device by which the sample container is subjected to vibration. Homogenization 24 can also be carried out by mechanical mixing, such as stirring or beating.

[0056] The sample container 28 in the sample storage unit 30 is then fed to the calorimetric measuring device 32. It is also conceivable to feed the sample container to the calorimetric measuring device 32 individually, without using the sample storage unit 30.

[0057] The addition of the excitation liquid to the material components initiates the hydration process, releasing the energy stored in the material components in the form of heat of reaction. The sample container 28 is therefore fed to the measuring device 32 immediately after the addition of the excitation liquid and subsequent homogenization, so that preferably all of the released heat of reaction can be measured. For example, the heat of reaction consists of energy previously stored in the clinker during cooling in a clinker cooler. This heat of reaction is characteristic of the reactivity of the mixture of material components. The energy released cumulatively during hydration at any given time corresponds to the weighted average of the contribution of the individual material components.The degree and rate of hydration are determined by the mineralogical composition of the material components, particularly the clinker, the added sulfate carriers, and the surface area generated during the milling of the material components. The hydration reaction proceeds isochemically, with the newly formed hydrate phases being largely X-ray amorphous.

[0058] The calorimetric measuring device 32 is designed in such a way that it determines the heat emitted by the test material over a certain period of time.

[0059] Commercially available calorimeters, such as isothermal heat flow calorimeters, enable the parallel determination of the heat of hydration of several different sample materials over a specific period. Known calorimeters have multiple measuring channels in which different sample materials are analyzed simultaneously. The calorimetric measuring device 32 is designed such that small sample quantities, such as 1–10 g, preferably 3–8 g, and most preferably about 5 g, are sufficient to determine the reactivity of the sample material. The measuring device 32 determines the heat of hydration, for example, over a measurement period of about 1–8, in particular 4–6, and preferably 5 days at a temperature in the calorimeter of about 20–45 °C, particularly 20–27 °C. By increasing the temperature to about 45 °C, short measurement times of less than one day are also conceivable.

[0060] The calorimetric measuring device 32 transmits the measurement result to the control device 38. The control device 38 is further designed in such a way that it determines the reactivity of the test material by means of the heat emitted by the test material as determined by the calorimetric measuring device.

[0061] Between the elements of the analysis device 10, for example, transport devices such as conveyor belts, mobile robots or stationary robots with a long reach are arranged, which are in Fig. 1 and 2 are schematically represented as arrows.

[0062] Fig. 2 Figure 1 shows a schematic representation of a device 11 for analyzing a test material according to a further embodiment. The analysis device 11 has all the elements of the device described in relation to Fig. 1The described analysis device 10 is characterized in that the dosing device 18 of the analysis device 10 has been replaced by three dosing devices 40, 42, 44, the dosing device 40 additionally comprising a heating device 46. Furthermore, the analysis device 11 of the Fig. 2 a further crushing device 36 upstream of the grinding device 20 and a third further dosing device 48 for dosing solid or liquid additives, such as grinding aids (e.g. DEG, TEA) or cement additives (e.g. TIPA, CaCl2) into the sample container 28.

[0063] The analysis device 11 also includes a rheometric measuring device 34 for determining the rheological properties of the sample materials in the sample containers 28 of the sample storage 30.

[0064] The analytical method that can be carried out with the analytical device 11 essentially corresponds to that described above. Fig. 1The described analytical method, wherein each of the containers 12, 14, 16 is assigned a dosing device 40, 42, 44, which doses a quantity of material components, adjustable by means of the control device 38, to the crushing device 36. The dosing device 40, which is assigned to container 16, has a heating device 46 by which the material component from container 16 can be heated. The material component in container 16 is, for example, a sulfate carrier, which is heated by means of the heating device 46 and thus thermally dewatered.

[0065] The crushing device 36 crushes in particular material components of large grain size, such as granules with a grain size of about 3 to 10mm, before the material components are fed to the grinding device 20.

[0066] Furthermore, the analysis method using the analysis device 11 includes a rheometric measurement using the rheometric measuring device 34. The rheometric measuring device 34 determines the rheological properties, such as the yield strength, of at least a portion of the sample material in the sample containers 28 of the sample storage 30.

[0067] In the analysis devices 10 and 11, parameters such as the mass fractions of the material components from containers 12, 14, and 16 in the sample material, the degree of milling of the material components, and the amount of excitation fluid and additives in the sample material can be adjusted via the control unit. This allows for the production of a large number of sample materials in which one or more parameters are varied in a known manner. Simultaneous analysis of the majority of sample materials from a sample storage facility 30 in the calorimetric measuring device 32 enables the simple determination of a material's reactivity as a function of specific parameters, such as grain size and material composition. Furthermore, the analysis devices 10 and 11 make it possible to easily produce a large number of sample materials and thus generate a high data density with respect to parameter variation.This allows for a precise analysis, especially of nonlinear relationships between the reactivity or rheological properties and the parameters of the test materials, such as composition and grain size. Reference symbol list

[0068] 10 Analysis device 11 Analysis device 12 Storage 14 Storage 16 Storage 18 First dosing device 20 Grinding device 22 Dosing device 24 Homogenizing device 26 Second dosing device for dosing an exciter liquid 28 Sample container 30 Sample storage 32 Measuring device 34 Measuring device 36 Crushing device 38 Control device 40 Dosing device 42 Dosing device 44 Dosing device 46 Heating device 48 Third dosing device

Claims

1. An apparatus (10, 11) for producing and analyzing a plurality of sample materials, wherein the sample materials are hydraulic binder and wherein the sample materials contain different compositions of various material components, which comprises a milling device (20) for milling material components, at least one first metering device (18; 40, 42, 44) for metering at least one material component into the milling device (20), at least one second metering device (26) for metering an activator liquid into the at least one milled material component, a homogenization device (24) for homogenizing the material components and the activator liquid to give a sample material, characterized in that the apparatus has a control device (38) which is connected at least to the milling device (20) and is configured in such a way that it varies at least one parameter characteristic for the milling intensity of the milling device (20) so that, in particular, the particle size of the material components is altered, wherein the control device (38) is connected to the at least one first metering device (18; 40, 42, 44) and is configured in such a way that it controls the metered amount of the material component and at least one measuring device (32) for determining the reactivity of the sample material is provided.

2. The apparatus (10; 11) as claimed in claim 1, wherein the measuring device (32) is a calorimetric measuring device.

3. The apparatus (10; 11) as claimed in any of the preceding claims, wherein the at least one first metering device (18; 40, 42, 44) is heatable.

4. The apparatus (10; 11) as claimed in any of the preceding claims, wherein the apparatus (10; 11) has a crushing device (36) which is located upstream of the milling device (20).

5. The apparatus (10; 11) as claimed in any of the preceding claims, wherein the apparatus (10; 11) has a rheometric measuring device (34) for determining the rheological properties of the sample material.

6. The apparatus (10; 11) as claimed in any of the preceding claims, wherein the apparatus (10; 11) has a sample store (30) having a plurality of sample containers (28) for accommodating a sample material.

7. The apparatus (10; 11) as claimed in any of the preceding claims, wherein the measuring device (32) is configured in such a way that it simultaneously determines the reactivity of a plurality of sample materials.

8. The apparatus (10; 11) as claimed in any of the preceding claims, comprising at least one third metering device (48) for metering at least one cement additive into the at least one milled material component located downstream of the milling device (20).

9. A process for producing and analyzing a plurality of sample materials, that are samples of a hydraulic binder, wherein the hydraulic binders contain different compositions of various material components, wherein the process comprises the steps: a) metering at least one material component into a milling device (20) b) milling the at least one material component in the milling device (20) c) metering an activator liquid into the at least one material component d) homogenizing the at least one material component and the activator liquid to give a sample material, characterized in that the steps a) to d) are repeated to produce a plurality of sample materials, with at least one parameter characteristic for the milling intensity being varied on the milling plant (20), where the process further comprises the step of determining the reactivity of the plurality of sample materials by means of a calorimetric measuring device (32).

10. The process as claimed in claim 9, wherein the speed of rotation of the milling device and / or the milling time of the at least one material component is varied in step b).

11. The process as claimed in claim 9 or 10, wherein the rheological properties of the plurality of sample materials are determined.

12. The process as claimed in any of claims 9 to 11, wherein the at least one material component is crushed before step b).

13. The process as claimed in any of claims 9 to 12, wherein step a) comprises heating of at least one material component.

14. The process as claimed in any of claims 9 to 13, wherein the particle size of at least part of the milled material components is determined before step d).