FR2920226A1 - Bernard calcimetry method for analyzing calcium carbonate rate in soil sample, involves introducing soil samples and hydrochloric acid dose in pill jars, where pill jars are closed using sealed closure traversed by tube connected to sensor - Google Patents

Bernard calcimetry method for analyzing calcium carbonate rate in soil sample, involves introducing soil samples and hydrochloric acid dose in pill jars, where pill jars are closed using sealed closure traversed by tube connected to sensor Download PDF

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FR2920226A1
FR2920226A1 FR0705619A FR0705619A FR2920226A1 FR 2920226 A1 FR2920226 A1 FR 2920226A1 FR 0705619 A FR0705619 A FR 0705619A FR 0705619 A FR0705619 A FR 0705619A FR 2920226 A1 FR2920226 A1 FR 2920226A1
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pill
jars
hydrochloric acid
calcimetry
pressure sensor
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Yacine Sadallah
Pierre Marche
Bertrand Garel
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CRITT Z3T ASS LOI DE 1901
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CRITT Z3T ASS LOI DE 1901
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/24—Earth materials
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
    • G01N7/14—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference
    • G01N7/18—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference by allowing the material to react

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
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  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
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  • Food Science & Technology (AREA)
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Abstract

The method involves introducing soil samples in pill jars i.e. bottles, and introducing a hydrochloric acid dose in the pill jars, where the pill jars are closed using a sealed closure that is traversed by a tube i.e. pipe, connected to a pressure sensor. An assembly conveyor is controlled by stepping motors with passages materialized by stainless steel rods that serve as guides during progression of the pill jars. The pill jars are moved using rotating magnetic fields during analyzing of a calcium carbonate rate in the soil samples. An independent claim is also included for a calcimetry machine comprising an assembly conveyor.

Description

- 1 La présente invention concerne une machine spéciale de calcimétrieThe present invention relates to a special calcimetry machine

destinée à analyser le taux de calcium dans des échantillons de sol avec une grande cadence. Un calcimètre, comme celui connu sous l'appellation Calcimètre de Bernard , permet de mesure le volume de CO2 dégagé par action de l'acide chlorhydrique (HCI) sur le carbonate de calcium (CaCO3) d'un échantillon de sol ou de roche, ce principe est bien connu pour des essais en laboratoire, l'objectif de la présente invention est d'adapter ce principe à des mesures industrielles à de grandes cadences (de l'ordre de quelques centaines d'échantillons par heure). A ù Principe de la mesure (Figure N 1) Après avoir procédé à leur émottage afin d'en éliminer les objets solides (graviers, pierres, ...), les échantillons sont introduits dans des pilluliers, une dose d'acide chlorhydrique est ensuite introduite dans chaque pillulier qui est ensuite bouché à l'aide d'un bouchon étanche traversé par une tubulure (conduit) reliée à un capteur de pression qui peut être relié à une carte d'acquisition pilotée par un ordinateur (PC) permettant le stockage des données et de réaliser des tracés graphiques de la réaction. L'acide chlorhydrique réagit avec le carbonate de calcium contenu dans l'échantillon. Cette réaction entre le carbonate de calcium et l'acide chlorhydrique est une réaction totale et exothermique dégageant du dioxyde de carbone (CO2) comme décrit ci-20 dessous: Ca CO3 + 2 Hcl + H2O -* 02 + Ca Cl2 + 2H20 ^ Masse molaire du Ca CO3: MCaco3 = 100 g  designed to analyze calcium levels in soil samples at a high rate. A calcimeter, such as the one known under the name Bernard's Calcimeter, makes it possible to measure the volume of CO2 released by the action of hydrochloric acid (HCl) on the calcium carbonate (CaCO3) of a sample of soil or rock, this principle is well known for laboratory tests, the objective of the present invention is to adapt this principle to industrial measurements at high speeds (of the order of a few hundred samples per hour). A - Principle of the measurement (Figure N 1) After having proceeded to their crumbling in order to eliminate the solid objects (gravels, stones, ...), the samples are introduced in pilluliers, a dose of hydrochloric acid is then introduced into each pill that is then plugged with a sealed plug through a tubing (conduit) connected to a pressure sensor that can be connected to a computer-controlled acquisition card (PC) allowing the storing data and making graphical plots of the reaction. Hydrochloric acid reacts with the calcium carbonate contained in the sample. This reaction between calcium carbonate and hydrochloric acid is a total and exothermic reaction releasing carbon dioxide (CO2) as described below: CaCO3 + 2HCl + H2O - * 02 + CaCl2 + 2H20 ^ Mass Ca CO3 molar: MCaco3 = 100 g

^ Masse molaire du Hcl : MHc, = 36 g ^ Masse molaire du CO2: MCo2 = 44 g 25 Soit P c02 la pression du gaz CO2 dans le flacon du volume V : Pco2 Vco2 = mco2.rco2.Tco2 (1) ^ Vco2 volume occupé par le gaz carbonique CO2 VCO2 = V Flacon Flacon + V conduit capteur/flacon - V liquide ^ mco2 Masse du gaz carbonique 30 ^ rco2 = 188 iJ/kg K constante spécifique du dioxyde de carbone ^ Tco2 = température du gaz CO2 mco2 Pco2. Vcoz = On( a : rco2.'l'co2 2) Le principe de la mesure consiste à prendre toujours la même quantité massique (mo) d'échantillon de terre à analyser par rapport à la même masse (m) de Ca CO3 pur (étalon de mesure) dont on aura préalablement déterminée par la mesure la pression P002 (étalon) on a alors : mo= -2 PCO2 (étalon) . VCO2 rco2. T CO2 (étalon)  Molar mass of HCl: MHc = 36 g. Molar mass of CO2: MCo2 = 44 g. Let P CO2 be the pressure of the CO2 gas in the flask of volume V: Pco2 Vco2 = mco2.rco2.Tco2 (1) ^ Vco2 volume occupied by carbon dioxide CO2 VCO2 = V Bottle Bottle + V led sensor / flask - V liquid ^ mco2 Mass of carbon dioxide 30 ^ rco2 = 188 iJ / kg K specific constant of carbon dioxide ^ Tco2 = CO2 gas temperature mco2 pco2. Vcoz = On (a: rco2.'l'co2 2) The principle of the measurement consists in always taking the same mass quantity (mo) of soil sample to be analyzed with respect to the same mass (m) of pure Ca CO3 (measurement standard), the pressure P002 (standard) will have been previously determined by the measurement, and then: mo = -2 PCO2 (standard). VCO2 rco2. T CO2 (standard)

mCO2(échanti lion) = PCO2 (échantillon) . V CO2 rco2. T CO2 (échantillon) PCO2 (échantillon) TCO2 (étalon) D'où mCO2 (échantillon) = MO. -I CO2 (étalon) T CO2 (échantillon) En général : TCO2 (étalon) TCO2 (échantillon) dans un local isotherme PCO2 (échantillon) D'où mc02 (échantillon) = MO. ù t CO2 (étalon) B û Description technologique (Figure N 2) Cette machine spéciale de calcimétrie est destinée à analyser le taux de calcium 10 d'échantillons de sol avec une grande cadence de plus d'une centaine d'échantillons par heure. Elle est constituée principalement : ^ D'un tapis roulant muni de couloirs matérialisés par des tiges en acier inoxydables servant de guides lors de l'avancement des piluliers.  mCO2 (sample) = PCO2 (sample). V CO2 rco2. T CO2 (sample) PCO2 (sample) TCO2 (standard) From where mCO2 (sample) = MO. -I CO2 (standard) T CO2 (sample) In general: TCO2 (standard) TCO2 (sample) in an isothermal room PCO2 (sample) From where mc02 (sample) = MO. CO2 (standard) B - Technological description (Figure N 2) This special calcimetry machine is designed to analyze the calcium level of soil samples with a high rate of more than one hundred samples per hour. It consists mainly of: ^ A conveyor belt with corridors materialized by stainless steel rods serving as guides during the advancement of pillboxes.

15 L'avancement par intermittence du tapis est commandé par des moteurs pas à pas muni d'une régulation afin d'assurer la précision du positionnement des piluliers lors de la phase d'approche du bouchon muni du capteur de pression. ^ Les flacons ont une contenance de 250 ml environ et contiennent au maximum 2 g de terre et d'eau déminéralisée UHQ.The intermittent advancement of the belt is controlled by stepper motors provided with a regulation to ensure the accuracy of the positioning of the pillagers during the approach phase of the cap equipped with the pressure sensor. The flasks have a capacity of approximately 250 ml and contain a maximum of 2 g of soil and demineralized UHQ water.

20 Ces mêmes flacons contiennent un barreau aimanté pour l'agitation qui sera faite pendant la phase analyse grâce à un champ magnétique tournant (un pour chaque flacon). ^ Dès que les flacons sont dans la zone d'analyse, des doigts préhenseurs immobilisent les flacons pendant que les bouchons portant l'aiguille de la pompe 25 péristaltique et la tubulure du capteur de pression descendent grâce à un support métallique lui-même mobile grâce à un vérin régulé en vitesse et en effort. ^ Dès que les bouchons sont mis, l'acide chlorhydrique est envoyé dans les flacons grâce à 10 pompes péristaltiques (une pour chaque flacon) via 10 électrovannes. Les 10 capteurs de pression fournissent chacun un signal (4/20 mA), correspondant à la 30 pression de CO2 dans le flacon. La mesure de la pression CO2 est terminée dès que l'on atteint le palier de stabilisation (4p <_ 2%) le signal est enregistré en continu sur un PC via une liaison RS 232 pour la détermination du taux de CaCO3 des échantillons suivant le protocole détaillé du principe de la mesure. Les bouchons sont alors libérés par retrait vers le haut du support métallique ; une aspiration des effluves (CO2 + vapeur d'acide) est mise en action et évacuée via une 5 hotte vers un bac de neutralisation par barbotage. Les doigts de préhension sont alors libérés et le tapis peut avancer d'un cran pour renouveler le cycle. 10 15 20 25 30 35These same vials contain a magnetic bar for stirring which will be made during the analysis phase by means of a rotating magnetic field (one for each vial). As soon as the flasks are in the analysis zone, gripping fingers immobilize the flasks while the caps carrying the needle of the peristaltic pump and the tubing of the pressure sensor are lowered by means of a metal support which is itself mobile. to a cylinder regulated in speed and effort. As soon as the stoppers are put, the hydrochloric acid is sent into the flasks by means of 10 peristaltic pumps (one for each flask) via 10 solenoid valves. The pressure sensors each provide a signal (4/20 mA), corresponding to the CO2 pressure in the vial. The measurement of the CO2 pressure is completed as soon as the stabilization step is reached (4p <_ 2%) the signal is recorded continuously on a PC via an RS 232 link for the determination of the CaCO3 content of the samples following the detailed protocol of the principle of measurement. The plugs are then released by pulling up the metal support; an aspiration of the effluents (CO2 + acid vapor) is put into action and evacuated via a hood to a bubbling neutralization tank. The gripping fingers are then released and the carpet can advance a notch to renew the cycle. 10 15 20 25 30 35

Claims (7)

Revendicationsclaims 1. Procédé de calcimétrie destiné à analyser le taux de calcium dans N échantillons de sol avec une grande cadence caractérisée en ce que les échantillons sont introduits dans des pilluliers et qu'une dose d'acide chlorhydrique est ensuite introduite dans chaque pillulier qui est ensuite bouché à l'aide d'un bouchon étanche traversé par une tubulure (conduit) reliée à un capteur de pression.  Calcimetry method for analyzing the calcium level in N soil samples with a high rate characterized in that the samples are introduced into pilluliers and a dose of hydrochloric acid is then introduced into each pillulier which is then plugged with a leakproof plug through a tubing (conduit) connected to a pressure sensor. 2. Procédé, selon la revendication 1, caractérisé en ce que les piloliers avancent sur un tapis roulant, commandé par des moteurs pas à pas, muni de couloirs matérialisés par des tiges en acier inoxydable servant de guides lors de l'avancement des piluliers.  2. Method according to claim 1, characterized in that piloliers advance on a treadmill, controlled by stepper motors, provided with corridors materialized by stainless steel rods serving as guides during the advancement of pill-makers. 3. Procédé, selon la revendication 1, caractérisé en ce que pendant la phase d'analyse, on agite les piluliers qui contiennent un barreau aimanté pour l'agitation grâce à un champ magnétique tournant (un pour chaque pilulier).  3. Method according to claim 1, characterized in that during the analysis phase, the pill organizers which contain a stir bar for stirring are shaken by a rotating magnetic field (one for each pill). 4. Procédé, selon la revendication 1, caractérisé en ce que dès que les piluliers sont dans la zone d'analyse, des doigts préhenseurs (2N doigts) immobilisent les piluliers pendant que les bouchons (N bouchons) portant chacun l'aiguille de la pompe péristaltique et la tubulure du capteur de pression descendent grâce à un support métallique lui-même mobile grâce à un vérin régulé en vitesse et en effort.  4. Method according to claim 1, characterized in that as soon as the pillboxes are in the analysis zone, gripping fingers (2N fingers) immobilize the pill containers while the plugs (N plugs) each carrying the needle of the peristaltic pump and the tubing of the pressure sensor go down thanks to a metal support itself mobile thanks to a cylinder regulated in speed and effort. 5. Procédé, selon la revendication 1, caractérisé en ce que dès que les bouchons sont mis, l'acide chlorhydrique est envoyé dans les piluliers grâce à N pompes péristaltiques (une pour chaque pilulier) via N électrovannes, les N capteurs de pression fournissant chacun un signal (4/20 mA), correspondant à la pression de CO2 dans le flacon.  5. Method according to claim 1, characterized in that as soon as the caps are put, the hydrochloric acid is sent into the pilluliers with N peristaltic pumps (one for each pill) via N solenoid valves, the N pressure sensors providing each a signal (4/20 mA), corresponding to the CO2 pressure in the bottle. 6. Procédé, selon la revendication 1, caractérisé en ce que le signal de chaque capteur de pression (N capteurs) est enregistré en continu à l'aide d'une liaison RS232 permettant de remonter à la cinétique de la réaction en continu.  6. Method according to claim 1, characterized in that the signal of each pressure sensor (N sensors) is recorded continuously using an RS232 link to go back to the kinetics of the reaction continuously. 7. Machine de calcimétrie pour la mise en oeuvre du procédé selon l'une des revendications précédentes caractérisée en ce qu'elle comporte : des piluliers dans lesquels sont introduit les échantillons et l'acide chlorhydrique, bouchés par un bouchon étanche traversé par une tubulure reliée à un capteur de pression, un tapis roulant commandé par des moteurs pas à pas, muni de couloirs matérialisés par des tiges en acier inoxydable servant de guide lors de l'avancement des piluliers,- 5 des doigts préhenseurs pour immobiliser les piluliers, des capteurs de pression, un par pilulier, des pompes péristaltiques, une par pilulier, - des électrovannes.5  7. calcimetry machine for carrying out the method according to one of the preceding claims characterized in that it comprises: pilluliers in which are introduced samples and hydrochloric acid, sealed by a sealed cap through a tubing connected to a pressure sensor, a treadmill controlled by stepper motors, provided with corridors materialized by stainless steel rods serving as a guide during the advancement of the pill-makers, 5 gripping fingers to immobilize the pillboxes, pressure sensors, one per pillbox, peristaltic pumps, one per pillbox, - solenoid valves.
FR0705619A 2007-08-23 2007-08-23 Bernard calcimetry method for analyzing calcium carbonate rate in soil sample, involves introducing soil samples and hydrochloric acid dose in pill jars, where pill jars are closed using sealed closure traversed by tube connected to sensor Pending FR2920226A1 (en)

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Cited By (6)

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Publication number Priority date Publication date Assignee Title
EP2605010A1 (en) 2011-12-14 2013-06-19 Geoservices Equipements Method for determining the relative content of a fist rock species and of a second rock species in a rock sample extracted from a wellbore, and associated device
WO2014060782A1 (en) * 2012-10-19 2014-04-24 Barouchas Pantelis Automatic portable and digital soil calcimeter
FR3015038A1 (en) * 2013-12-16 2015-06-19 Sominex METHOD FOR DETERMINING THE CONTENT IN DIFFERENT MINERALS OF A ROCK, PORTABLE DEVICE THEREFOR
RU171554U1 (en) * 2017-02-07 2017-06-06 Общество С Ограниченной Ответственностью "Тауруслаб" CALCIMETER
US20170199109A1 (en) * 2014-09-23 2017-07-13 Halliburton Energy Services, Inc. Automated Calcimeter Systems
RU2701868C1 (en) * 2019-01-15 2019-10-02 Общество С Ограниченной Ответственностью Научно-Производственное Предприятие "Экохимприбор" Nitrate chalk pulp analyzer

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2605010A1 (en) 2011-12-14 2013-06-19 Geoservices Equipements Method for determining the relative content of a fist rock species and of a second rock species in a rock sample extracted from a wellbore, and associated device
WO2013088415A1 (en) 2011-12-14 2013-06-20 Geoservices Equipements Method for determining the relative content of a first rock species and of a second rock species in a rock sample extracted from a wellbore, and associated device
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AU2012354105B2 (en) * 2011-12-14 2016-01-28 Geoservices Equipements Method for determining the relative content of a first rock species and of a second rock species in a rock sample extracted from a wellbore, and associated device
WO2014060782A1 (en) * 2012-10-19 2014-04-24 Barouchas Pantelis Automatic portable and digital soil calcimeter
FR3015038A1 (en) * 2013-12-16 2015-06-19 Sominex METHOD FOR DETERMINING THE CONTENT IN DIFFERENT MINERALS OF A ROCK, PORTABLE DEVICE THEREFOR
FR3015037A1 (en) * 2013-12-16 2015-06-19 Sominex METHOD FOR DETERMINING THE CONTENT IN DIFFERENT MINERALS OF A ROCK, PORTABLE DEVICE THEREFOR
WO2015092247A1 (en) * 2013-12-16 2015-06-25 Sominex Method of determining amounts of different minerals of a rock, associated portable device
US20170199109A1 (en) * 2014-09-23 2017-07-13 Halliburton Energy Services, Inc. Automated Calcimeter Systems
US9939361B2 (en) * 2014-09-23 2018-04-10 Halliburton Energy Services, Inc. Automated calcimeter systems
RU171554U1 (en) * 2017-02-07 2017-06-06 Общество С Ограниченной Ответственностью "Тауруслаб" CALCIMETER
RU2701868C1 (en) * 2019-01-15 2019-10-02 Общество С Ограниченной Ответственностью Научно-Производственное Предприятие "Экохимприбор" Nitrate chalk pulp analyzer

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