WO2005113468A1 - Traceur dans compositions cimentaires et méthode d’identification - Google Patents

Traceur dans compositions cimentaires et méthode d’identification Download PDF

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Publication number
WO2005113468A1
WO2005113468A1 PCT/EP2004/050890 EP2004050890W WO2005113468A1 WO 2005113468 A1 WO2005113468 A1 WO 2005113468A1 EP 2004050890 W EP2004050890 W EP 2004050890W WO 2005113468 A1 WO2005113468 A1 WO 2005113468A1
Authority
WO
WIPO (PCT)
Prior art keywords
tracer
cement
based composition
materials
residue
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/EP2004/050890
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English (en)
Inventor
Ferdi Erdogan
Beyhan Gozogul
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kalekim Kimyevi Maddeler Sanayi ve Ticaret AS
Original Assignee
Kalekim Kimyevi Maddeler Sanayi ve Ticaret AS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Kalekim Kimyevi Maddeler Sanayi ve Ticaret AS filed Critical Kalekim Kimyevi Maddeler Sanayi ve Ticaret AS
Priority to TR2006/06381T priority Critical patent/TR200606381T2/xx
Priority to EA200602069A priority patent/EA010150B1/ru
Priority to PCT/EP2004/050890 priority patent/WO2005113468A1/fr
Publication of WO2005113468A1 publication Critical patent/WO2005113468A1/fr
Priority to BG109736A priority patent/BG66198B1/bg
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0096—Provisions for indicating condition of the compositions or the final products, e.g. degree of homogeneous mixing, degree of wear
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00034—Physico-chemical characteristics of the mixtures
    • C04B2111/00189—Compositions or ingredients of the compositions characterised by analysis-spectra, e.g. NMR

Definitions

  • the present invention relates to a method of identification of a cement-based material for determining whether it is of a particular type or belonging to a certain producer and a cement based composition comprising the tracer materials of said method.
  • the method incorporates use of specific tracer materials, admixed to various types of cementitious products such as; adhesives, filling materials, insulation mortars, repair mortars, grouts etc.
  • the novel method allows determination of the source and type of the product before/after the usage through a rapid and reliable way of analysis comprising a pre-treatment step followed by a X-Ray Diffractometric analysis which provides the capability of identifying the product both in powder form i.e. prior to application and in hardened form i.e. after application on a building structure.
  • the present invention refers to cement-based materials comprising very fine trace materials as an additive and a novel method for determining the producer and the kind of cement based product comprising the tracer materials of said method.
  • the product which failed to meet with the requirements is the product of concerned producer, but the type of the product was inappropriate for application on the building structure for which the consumer demands compensation.
  • a third possibility is that the defective product was produced by concerned producer and the type of the product was appropriate for the structure on which it was applied. In all three cases, it is important to the concerned producer to reliably identify at low cost whether the cement based material used in the pieces of cementitious product in hand was his own product and if yes, was it of the correct type for applying on the structure at which damage occurred.
  • a cementitious material includes a number of chemical admixtures depending on their functions, such as; air-entraining, water-retaining, retarding, accelerating and plasticizer additives.
  • the present invention proposes use of tracer materials within the cementitious composition, the tracer particles being invisible or hardly visible to the human eye under normal conditions.
  • the present methods offer some tracer particles characterized in their physical properties. These include using tracer particles having colors or sizes which are different to those of the cementitious composition and the detection method being based on distinguishing particles based on their physical properties using simple techniques such as screening.
  • One such method is disclosed in US 5,324,356 granted to Goodwin et al. Goodwin basically suggested pulverizing and screening a building material e.g.
  • any such component is likely to confuse the test staff as it is almost impossible to determine whether such particles are reinforcement fibers or flakes of a third party product or alternatively, the tracer materials of the concerned producer.
  • the identification method is the most primitive and thus most questionable approach that could be employed. It is practically inappropriate to add a tracer material which does not have near sizes to the filler. Under such cases, it is generally not possible to obtain a trustworthy identification result.
  • producing an imitation product is an extremely easy process in all three aforementioned assumptions.
  • the identification process would be more reliable compared to above mentioned assumptions whereas the process would require use of generally very expensive materials as the tracers.
  • the tracer materials are identified using their insolubility, then the identification method is again very questionable. Any natural or foreign content which is found e.g. in a hardened sample collected from a failed site and which is insoluble, may lead the identification process in an erroneous result. Under such a case, one should assume that all cement based products comprising non-dissolving agent should certainly belong to the concerned producer, which is no- doubt an erroneous.
  • the present invention aims to provide a method in which detection of tracer materials are conducted in the molecular level rather than in the macro level of physical properties. None of the present methods offer such reliable and efficient tracer materials and/or detection methods thereof applicable to cement-based compositions.
  • the present invention offers an extremely reliable combination of specific tracer materials and their detection method including an XRD (X-Ray Diffraction) analysis in which specific identification parameters, namely the distance between atom row planes of crystal lattices (d) and the intensity of diffracted light (I) are determined with a precision not open to debate.
  • XRD X-Ray Diffraction
  • One of the objects of the present invention is to provide an efficient method which enables a producer of cement based materials to identify reliably his product and its type before or after use on a structure.
  • Another object of the present invention is to provide a tracer material identification method, in which very fine tracer materials admixed in a cement based composition can be identified, such identification taking place in the molecular level.
  • Another object of the present invention is to provide novel process for identifying tracer materials in a cement based composition, in which tracer materials show particle size, shape and color characteristics which are substantially similar to those of said cement- based composition.
  • a further object of the present invention is to provide a tracer material identification method in which the tracer materials admixed in a cement based composition are identified using their crystal structure.
  • a further object of the present invention is to provide a tracer material identification method in which the tracer materials to be admixed to the product can be selected from a group of elements which can not be naturally encountered in the products of other producers.
  • a further object of the present invention is to provide cement based material comprising at least one tracer material which is identifiable by the method of the present invention.
  • the objects of the invention are achieved through use of specifically determined tracer materials such as talc, albite, orthoclase, chloride, zeolite, mica, vollastonite, barite, profillite, bentonite, serpentine, chromite, borax, kolemanite etc.
  • tracer materials such as talc, albite, orthoclase, chloride, zeolite, mica, vollastonite, barite, profillite, bentonite, serpentine, chromite, borax, kolemanite etc.
  • XRD X-Ray Diffractometry
  • the type of the tracer material shall be appropriate for use within the cementitious composition and be detectable either in powder form prior to use or after setting.
  • the method may be applied to both powdered and already hardened structures, comprising a number of pre-treatment steps such as removing foreign materials (soil, stone, dust, mortar etc.), washing the residue with a concentrated acid, filtration, drying, burning and finally analyzing in an X- Ray Diffractometer.
  • pre-treatments applied before the XRD analysis serve to the purpose of obtaining precise results in the diffractometer.
  • XRD detection is conducted by subjecting the residue in an X-ray field, measuring the distance (d) between the atom row planes of the crystal lattices and the intensity (I) of the diffracted light using the rays diffracted from the residue.
  • the distance (d) and the light intensity (I) values for each kind of the tracer material selected for use in the method of the present invention are known and shown on charts comprising such predetermined data as in the case of ASTM charts. Values obtained from the diffractometer are then compared with the values shown on the chart and used to determine whether the residue comprises or not and, if yes, the type of the tracer material used by the concerned producer.
  • Fig. 1 is a schematic 2-dimensional demonstration of an x-ray diffraction occurring on a residue material surface intended to simulate, by way of an example, an X ray being diffracted on plane surface of a residue and rebounded with a specific light intensity.
  • Cement-based materials are compositions generally comprising 30 to 60% Portland Cement, aggregates and additives like cement-based adhesives, filling materials, insulation mortars, repair mortars, grouts etc. which are used for different purposes in constructions through use of a setting or a hardening component, generally water. Hydrolysis occurs in the structure of the formulation as soon as the hardening agent contacts the cementitious material. At this stage the calcium aluminates, calcium silicates and other compounds are hydrolyzed and pH of the composition increases immediately to over 12 and a large amount of heat release occurs due to the release of alkaline hydroxide (OH ) ions. At this point said specifically selected tracer materials perform a highly resistant property against those highly alkaline pH values and against hard conditions having the ability to stay in the structure for many years and coinciding to micro level particles of cementitious and additive phases.
  • OH alkaline hydroxide
  • the present invention comprises a number of steps for precisely detecting the existence of a tracer material in a residue to provide an indication for the producer and type of the product. These steps include removing the solid bulk materials (soil, sand, stone etc.) around the residue, washing the same using any strong acid e.g. HCI, drying, burning and finally locating the residue in an X-Ray Diffractometer.
  • Preferred tracer materials of the present invention are talc, albite, orthoclase, chloride, zeolite, mica, vollastonite, barite, profillite, bentonite, serpentine, chromite, borax and kolemanite in very fine form.
  • Aforementioned pre-treatment steps are, selectively and as necessary, applied to a hardened composite sample, aiming to obtain a relatively pure material for a precise identification in the diffractometer step.
  • the sample is to be cleaned out from the rough materials and preferentially washed out in a strong acid, such as hydrochloric acid.
  • the acid-wash substantially provides removal of cement and filling materials from the sample.
  • the sample is optionally washed with water, filtrated and dried.
  • the tracer material sought in the sample should of a type insoluble and non-reactant to the materials involved in these treatments or shortly, the tracer material shall be capable of retaining its crystal structure during the pre-XRD treatments.
  • Organic materials are removed by optionally burning the sample for a preferred duration of 1 hour at an elevated temperature between 250 to 650 °C. It is found out during the tests that burning the sample is not an essential step of the identification process, but it is preferred due to the fact that the tracer materials are frequently surrounded by organic components which reduce the detectability of the tracers in the x-ray diffractometry. A clear tracer component which is free of organic materials can be more sharply detected in the XRD analysis while accompanying the additional benefit of adding a lower tracer content in the cement based composition.
  • the amount of organic compound content can be used in combination to existence of a tracer material to determine the type of a product.
  • the amount of organic material can be measured during the burning step. It is guaranteed by the pre-XRD treatments that all the minerals and other foreign materials which may inadvertently affect x-ray diffractometry are removed. It is further more stated that aforementioned pre-XRD treatments are found to be helping the tracer material concentration in the sample increase. In return, this feature provides the advantage of freedom to use a lower amount of tracer content in the final product while still remaining in the detectable limits.
  • X Rays can easily detect minerals and inorganic materials having formal crystal shapes.
  • X Rays are conventionally created in a vacuum tube and emitted from an anode electrode.
  • the regularly ordered atoms of the lattice structures of the minerals diffuse the X Rays causing interferences and consequently these indicate the proper constitution of the secondary dispersion of the emission.
  • Bragg Law is employed to understand the diffractometry behavior during the XRD analysis. According to the same, X Rays should come through a mineral with a definite angle and the difference of distance between the incoming and outgoing rays should be equal to a multiple of the wave length.
  • n ⁇ 2 d sin O in which n, is the diffraction coefficient ⁇ , is the diffraction angle ⁇ , is the X Ray wave length d, is the distance between the atom row planes in the crystal lattice.
  • the sample to be put under X-rays is preferentially brought into powder form in order to increase the intensity of the reflection.
  • Each mm 3 contains approximately 110 particles and their different locations provide intensive reflections.
  • the X Rays, generated in the generator part of the XRD equipment with high voltage, are directed towards the pulverized sample and the diffracted X Rays with definite angles are converted to electronic data by means of a sensor located on a mobile goniometry arm.
  • Each mineral and each crystallized material has a characteristic spectrum, which is also indicated in ASTM charts. Mineral identification is achieved through a brief comparison of experimental analysis results with the values e.g. indicated on ASTM charts.
  • Table-2 is a typical ASTM chart prepared upon XRD identification of a certain mineral, four conventional d and I values, exact diffraction list and surfaces and crystallographic-chemical-instrumental information used in the XRD.
  • the present invention proposes a very reliable identification method even in very low tracer material concentrations in the sample. Having the capability of reliably identifying tracer materials in very low concentrations, producers are able to reduce material costs while at the same time producing end products which comprise less foreign content to deteriorate desired features of a cement based composition. While prior art methods essentially adopt some simple approaches such as sieving, floating, coloring, sizing etc. of tracer materials for further detection, the present invention introduces instrumental analysis conducted in molecular level. The novel process of the present invention also allowed the producers to reliably identify their products before or after application in a building through use of specific tracer materials which are capable of retaining their crystal structure throughout the entire identification process.
  • the novel process of the present invention has also provided use of said tracer materials which show particle size, shape and color characteristics which are substantially similar to those of said cement-based composition in which they are added.
  • These highly efficient tracer materials include, but are not limited to talc, albite, orthoclase, chloride, zeolite, mica, vollastonite, barite, profillite, bentonite, serpentine, chromite, borax, kolemanite which are specifically selected for cementitious materials and which do not show an amorphous characteristics.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

Une méthode d’identification d’une composition cimentaire contenant au moins un traceur non amorphe est ici présentée. La méthode énumère les différentes étapes consistant à retirer le ciment et prélever un échantillon en utilisant un acide puissant, à laver le résidu et éventuellement le filtrer et le sécher. Le résidu est de préférence brûlé à une température élevée pour retirer tout contenu organique et placé dans un diffractomètre à rayons X. L’angle et l'intensité des rayons diffractés sont mesurés et comparés avec les données préétablies des traceurs spécifiques. Les matériaux des traceurs sont spécifiquement sélectionnés parmi le talc, l’albite, l’orthoclase, le chlorure, la zéolithe, le mica, la wollastonite, la barytine, la pyrophillite, la bentonite, la serpentine, la chromite, le borax et la colémanite, qui sont des substances adaptées aux compositions cimentaires avec leurs formes moléculaires cristallines et des caractéristiques d’inertie chimique favorables à l’analyse par diffraction de rayons X.
PCT/EP2004/050890 2004-05-21 2004-05-21 Traceur dans compositions cimentaires et méthode d’identification Ceased WO2005113468A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
TR2006/06381T TR200606381T2 (tr) 2004-05-21 2004-05-21 Çimento terkiplerinde belirteç malzemeler ve bunların tanımlanması için yöntem
EA200602069A EA010150B1 (ru) 2004-05-21 2004-05-21 Индикаторные материалы в цементных составах и способ их идентификации
PCT/EP2004/050890 WO2005113468A1 (fr) 2004-05-21 2004-05-21 Traceur dans compositions cimentaires et méthode d’identification
BG109736A BG66198B1 (bg) 2004-05-21 2006-11-10 Метод за идентифициране на циментиращ състав

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/EP2004/050890 WO2005113468A1 (fr) 2004-05-21 2004-05-21 Traceur dans compositions cimentaires et méthode d’identification

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TR (1) TR200606381T2 (fr)
WO (1) WO2005113468A1 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8596354B2 (en) 2010-04-02 2013-12-03 Schlumberger Technology Corporation Detection of tracers used in hydrocarbon wells
US8642346B2 (en) 2010-12-29 2014-02-04 United States Gypsum Company Tagged joint compound and method of identification
CN104535600A (zh) * 2014-12-12 2015-04-22 武汉钢铁(集团)公司 波长色散x射线荧光光谱法测定引流砂中三氧化二铬的方法
JP2019027889A (ja) * 2017-07-28 2019-02-21 三菱マテリアル株式会社 シリカフューム含有セメント組成物に含まれるシリカフュームの定量方法およびシリカフューム含有セメント組成物の製造方法
EP2513015B1 (fr) * 2009-12-18 2019-03-13 Construction Research & Technology GmbH Procédé d'identification qualitative et quantitative de marchandises pondéreuses

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Publication number Priority date Publication date Assignee Title
US2861636A (en) * 1952-04-18 1958-11-25 Socony Mobil Oil Co Inc Time setting clay cement and method of correcting lost circulation
CH453182A (de) * 1965-11-24 1968-06-14 Winteler Rudolf Verwendung von Chromoxyd oder oxydischen Chromerzen als Härter für Beton
US4354878A (en) * 1979-09-18 1982-10-19 Manville Service Corporation Mineral article such as thermal insulation containing visual identification means
EP0397963A1 (fr) * 1989-05-19 1990-11-22 Sika AG, vorm. Kaspar Winkler & Co. Liant hydraulique à haute réactivité pour la production de matériaux de construction
US5010301A (en) * 1989-08-22 1991-04-23 Exxon Production Research Company Method for determining the swelling clay content of cement mixtures by dielectric measurements
JPH061645A (ja) * 1992-06-22 1994-01-11 Ishikawajima Constr Materials Co Ltd 中性子遮蔽コンクリート
US5324356A (en) * 1991-05-29 1994-06-28 Chemrex Inc. Cement-based compositions containing tracer material
US5624489A (en) * 1995-01-23 1997-04-29 National Research Council Of Canada Conversion-preventing additive for high alumina cement products
US20020117090A1 (en) * 2001-02-20 2002-08-29 Richard Ku Super high strength concrete
JP2003035657A (ja) * 2001-07-25 2003-02-07 Sumitomo Kinzoku Kozan Siporex Kk 軽量気泡コンクリートパネルの劣化診断システム
DE10237764A1 (de) * 2002-08-17 2004-03-04 Economic Versicherungs-Vermittlung Gmbh Kennzeichnungsverfahren

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2861636A (en) * 1952-04-18 1958-11-25 Socony Mobil Oil Co Inc Time setting clay cement and method of correcting lost circulation
CH453182A (de) * 1965-11-24 1968-06-14 Winteler Rudolf Verwendung von Chromoxyd oder oxydischen Chromerzen als Härter für Beton
US4354878A (en) * 1979-09-18 1982-10-19 Manville Service Corporation Mineral article such as thermal insulation containing visual identification means
EP0397963A1 (fr) * 1989-05-19 1990-11-22 Sika AG, vorm. Kaspar Winkler & Co. Liant hydraulique à haute réactivité pour la production de matériaux de construction
US5010301A (en) * 1989-08-22 1991-04-23 Exxon Production Research Company Method for determining the swelling clay content of cement mixtures by dielectric measurements
US5324356A (en) * 1991-05-29 1994-06-28 Chemrex Inc. Cement-based compositions containing tracer material
JPH061645A (ja) * 1992-06-22 1994-01-11 Ishikawajima Constr Materials Co Ltd 中性子遮蔽コンクリート
US5624489A (en) * 1995-01-23 1997-04-29 National Research Council Of Canada Conversion-preventing additive for high alumina cement products
US20020117090A1 (en) * 2001-02-20 2002-08-29 Richard Ku Super high strength concrete
JP2003035657A (ja) * 2001-07-25 2003-02-07 Sumitomo Kinzoku Kozan Siporex Kk 軽量気泡コンクリートパネルの劣化診断システム
DE10237764A1 (de) * 2002-08-17 2004-03-04 Economic Versicherungs-Vermittlung Gmbh Kennzeichnungsverfahren

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PATENT ABSTRACTS OF JAPAN vol. 018, no. 198 (C - 1187) 7 April 1994 (1994-04-07) *
PATENT ABSTRACTS OF JAPAN vol. 2003, no. 06 3 June 2003 (2003-06-03) *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2513015B1 (fr) * 2009-12-18 2019-03-13 Construction Research & Technology GmbH Procédé d'identification qualitative et quantitative de marchandises pondéreuses
US8596354B2 (en) 2010-04-02 2013-12-03 Schlumberger Technology Corporation Detection of tracers used in hydrocarbon wells
US8642346B2 (en) 2010-12-29 2014-02-04 United States Gypsum Company Tagged joint compound and method of identification
CN104535600A (zh) * 2014-12-12 2015-04-22 武汉钢铁(集团)公司 波长色散x射线荧光光谱法测定引流砂中三氧化二铬的方法
JP2019027889A (ja) * 2017-07-28 2019-02-21 三菱マテリアル株式会社 シリカフューム含有セメント組成物に含まれるシリカフュームの定量方法およびシリカフューム含有セメント組成物の製造方法

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TR200606381T2 (tr) 2006-12-21
EA010150B1 (ru) 2008-06-30
EA200602069A1 (ru) 2007-08-31

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