FR2498332A2 - Tracing of drilling mud by acetate addn. - with titration method for selective estimation of acetate in later mud samples - Google Patents

Tracing of drilling mud by acetate addn. - with titration method for selective estimation of acetate in later mud samples Download PDF

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FR2498332A2
FR2498332A2 FR8101134A FR8101134A FR2498332A2 FR 2498332 A2 FR2498332 A2 FR 2498332A2 FR 8101134 A FR8101134 A FR 8101134A FR 8101134 A FR8101134 A FR 8101134A FR 2498332 A2 FR2498332 A2 FR 2498332A2
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iodine
volume
mud
excess
acetate
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FR8101134A
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FR2498332B2 (en
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Jean-Jacques Fery
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Total Compagnie Francaise des Petroles SA
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Compagnie Francaise des Petroles SA
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    • EFIXED CONSTRUCTIONS
    • E21EARTH OR ROCK DRILLING; MINING
    • E21BEARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
    • E21B49/00Testing the nature of borehole walls; Formation testing; Methods or apparatus for obtaining samples of soil or well fluids, specially adapted to earth drilling or wells
    • E21B49/005Testing the nature of borehole walls or the formation by using drilling mud or cutting data
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/26Oils; Viscous liquids; Paints; Inks
    • G01N33/28Oils, i.e. hydrocarbon liquids
    • G01N33/2823Raw oil, drilling fluid or polyphasic mixtures

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  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Mining & Mineral Resources (AREA)
  • Geology (AREA)
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  • Analytical Chemistry (AREA)
  • Immunology (AREA)
  • Food Science & Technology (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Medicinal Chemistry (AREA)
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  • Environmental & Geological Engineering (AREA)
  • Fluid Mechanics (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

Drilling muds are traced by addn. of acetate ion at a concn. of 0.001-0.05 M. The tracer is estimated in the filtrate of mud samples by addn. of dil. strong acid, distn. of the acetic acid and titration of the distillation with alkali. Modifications to the titration are now claimed, chiefly in order to eliminate interference by other weak acids present in the distillate. The mud filtrate is treated e.g. with dil. HCl or H2SO4 and distn. is at a temp. of 105-130 deg.C. Oxidisable weak acids in the distillate are then oxidised by I2 soln. and the excess of I2 then neutralised before adding a known excess of I2 soln. (vol. V2) of known normality, N1. The excess acid is then titrated with dil. strong alkali (normality N), (a) to pH 4.65, requiring vol. V3 and semi-neutralising the acetic acid, and (b) to pH 8.0, requiring vol. V4 and fully neutralising the acetic acid. Finally, the remaining I2 is titrated by thiosulphate of normality N1, requiring vol. V5. If V6 is the vol. of mud filtrate sample, given that the mol. wt. of CH3COONa.3H2O is 136, the concn. (C1) (g/l.) of this salt in the filtrate is given by: C1 = 272 x (N(V4V3)-N1(V2-V5))/V6.

Description

"PIETHODE DE TRrZCAGE DE LA BOUE DE FORAGE
PAR DETERINATlON DE LA CONCENTRATION D'UN ION SOLUBLE".
"DRILLING MUD TRrZCING PIETHODE
BY DETERINATION OF THE CONCENTRATION OF A SOLUBLE ION ".

Le brevet principal a pour objet une méthode de traçage de la boue de forage au moyen d'un ion traceur qui est l'ion acétate CH3 COO a une concentration comprise entre 1.10-3 et 5,10-2 ion par litre de boue. The main patent relates to a method of tracing drilling mud using a tracer ion which is the acetate ion CH3 COO at a concentration between 1.10-3 and 5.10-2 ion per liter of mud.

On peut déterminer la concentration de l'ion acétate dans le filtrat de l'échantillon recueilli en traitant préalablement le filtrat à doser par de l'acide sulfurique dilué et en distillant l'acide acétique ainsi libéré à une température de l'ordre de 120 à 130 C.  The concentration of the acetate ion in the filtrate of the collected sample can be determined by treating the filtrate to be determined beforehand with dilute sulfuric acid and distilling the acetic acid thus released at a temperature of the order of 120 at 130 C.

Au lieu d'acide sulfurique, on peut utiliser un autre acide fort tel que l'acide chlorhvydrique et la distillation de l'acide acétique peut s'effectuer à une température comprise entre 1050C et 1300C. Instead of sulfuric acid, another strong acid can be used such as hydrochloric acid and the distillation of acetic acid can be carried out at a temperature between 1050C and 1300C.

On peut déterminer ensuite l'acidité forte du distillat par l'addition d'une solution d'une base forte telle que la soude jusqu'à l'obtention d'un pH de 4,2 à 4,3, puis l'acidité faible par l'addition d'un volume mesuré de cette solution de base forte jusqu'à l'obtention d'un pli d'environ 8. The strong acidity of the distillate can then be determined by the addition of a solution of a strong base such as sodium hydroxide until a pH of 4.2 to 4.3 is obtained, then the acidity weak by adding a measured volume of this strong base solution until a fold of about 8 is obtained.

On a trouvé, selon la présente addition, que l'on pouvait utiliser une méthode de dosage plus perfectionnée, tenant compte du fait que l'evolution du pH lors du dosage provoque une redissociation d'acides forts en acides faibles, ce qui conduit à effectuer une neutralisation en milieu oxydant. It has been found, according to the present addition, that a more sophisticated assay method could be used, taking into account the fact that the change in pH during the assay causes a redissociation of strong acids into weak acids, which leads to neutralize in an oxidizing medium.

D'autre part, on peut limiter l'incertitude sur la valeur du pH rencontrée dans la neutralisation de l'acidité forte, en utilisant le pK de l'acide acétique reconnu à 4,65 (tampon acétique). Cette valeur n'est pratiquement pas affectée par la température ou le milieu dans lequel se trouve la solution. On the other hand, one can limit the uncertainty on the pH value encountered in the neutralization of strong acidity, by using the pK of recognized acetic acid at 4.65 (acetic buffer). This value is practically unaffected by the temperature or the environment in which the solution is found.

Un objet de la présente addition consiste ainsi en ce qu'apres avoir effectué une oxydation des acides faibles indésirables du distillat par l'iode et avoir neutralisé exactement l'exces d'iode, on ajoute un exces d'iode d'un volume V2 et d'une normalité N1 connus, on neutralise partiellement l'acidité du distillat par un volume mesuré V3 d'une base de normalite N jusqu'à l'obtention d'un pH 4,65.On poursuit la neutralisation de l'acidité jusqu'à l'obtention d'un pH 8, en mesurant le volume total V4 de la base utilisé, on évalue le volume V5 de l'excès final d'iode, notamment au moyen de thiosulfate de même normalité, et on détermine la concentration de l'ion traceur d'après la différence entre la quantité molaire de la base contenue dans le volume (V4 - V3) de base utilisé à la neutralisation de l'acidité entre les pH 4,65 et 8 et la quantité molaire d'iode contenue dans le volume d'iode (V2 - V5) utilisé à la réoxydation d'acides parasites faibles générés par la variation de pli au cours du dosage. An object of the present addition thus consists in that after having carried out an oxidation of the undesirable weak acids of the distillate by iodine and having neutralized exactly the excess of iodine, an excess of iodine of a volume V2 is added. and of a known normality N1, the acidity of the distillate is partially neutralized by a measured volume V3 of a base of normality N until a pH 4.65 is obtained. The acidity is further neutralized until a pH 8 is obtained, by measuring the total volume V4 of the base used, the volume V5 of the final excess of iodine is evaluated, in particular by means of thiosulfate of the same normality, and the concentration of the tracer ion according to the difference between the molar quantity of the base contained in the volume (V4 - V3) of base used for the neutralization of the acidity between pH 4.65 and 8 and the molar quantity d iodine contained in the volume of iodine (V2 - V5) used for the reoxidation of weak parasitic acids generated by the fold variation in during dosing.

La concentration C1 en grammes par litre d'acétate de sodium cristallisé CH3 C00 Na, 3H20 est alors donnée, pour une base monovalente telle que la soude et pour un volume V6 de prise d'essai de filtrat de boue, compte-tenu de la deniineutralisation de l'acide acétique à pli 4,65, par la formule

Figure img00020001
The concentration C1 in grams per liter of crystallized sodium acetate CH3 C00 Na, 3H20 is then given, for a monovalent base such as sodium hydroxide and for a volume V6 of the mud filtrate test sample, taking into account the denineutralization of acetic acid at fold 4.65, by the formula
Figure img00020001

Claims (1)

REVENDICATION CLAIM Méthode de traçage de boue de forage au moyen d'ions solubles, selon laquelle on étudie les variations de concentrations en ion du filtrat d'une boue de forage contenant une teneur prédéterminée d'un ion traceur constitué par l'ion acétate CH3 C00 à une concentration comprise entre 1.10~3 et 5.iO-2 ion par litre de boue et selon laquelle on a préalablement traité le filtrat à doser par un acide fort dilué et distillé l'acide acétique ainsi libéré à une température de l'ordre de 1050C à 1300C, caractérisé en ce qu'après avoir effectué une oxydation des acides faibles indésirables du distillat par l'iode et avoir neutralisé exactement l'excès d'iode, on ajoute un excès d'iode d'un volume V2 et d'une normalité connus, on neutralise partiellement l'acidité du distillat par un volume mesuré V3 d'une base forte jusqu'à l'obtention d'un pH 4,65, on poursuit la neutralisation de l'acidité jusqu'à l'obtention d'un pH 8, en mesurant le volume total V4 de la base utilisé, on évalue le volume Vs de l'excès final d'iode, et on détermine la concentration de l'ion traceur d'après la différence entre la quantité molaire de la base contenue dans le volume (V4 - V3) de la base utilisé à la neutralisation de l'acidité entre les pH 4,65 et 8 et la quantité molaire d'iode contenue dans le volume d'iode (V2 - V5) utilisé à la réoxydation d'acides parasites faibles générés par la variation de pH au cours du dosage.  Method of tracing drilling mud using soluble ions, according to which the ion concentration variations of the filtrate of a drilling mud containing a predetermined content of a tracer ion constituted by the acetate ion CH3 C00 are studied. a concentration between 1.10 ~ 3 and 5.iO-2 ion per liter of mud and according to which the filtrate to be assayed has been previously treated with a strong dilute acid and distilled the acetic acid thus released at a temperature of the order of 1050C to 1300C, characterized in that after having carried out an oxidation of the undesirable weak acids of the distillate by iodine and having exactly neutralized the excess of iodine, an excess of iodine of a volume V2 and of a known normality, the acidity of the distillate is partially neutralized by a measured volume V3 of a strong base until a pH 4.65 is obtained, the acidity is continued neutralization until the of a pH 8, by measuring the total volume V4 of the base used, the volume Vs is evaluated of the final excess of iodine, and the concentration of the tracer ion is determined according to the difference between the molar amount of the base contained in the volume (V4 - V3) of the base used to neutralize the acidity between pH 4.65 and 8 and the molar quantity of iodine contained in the volume of iodine (V2 - V5) used for the reoxidation of weak parasitic acids generated by the variation in pH during the assay.
FR8101134A 1980-01-08 1981-01-22 Tracing of drilling mud by acetate addn. - with titration method for selective estimation of acetate in later mud samples Granted FR2498332A2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
FR8101134A FR2498332A2 (en) 1980-01-08 1981-01-22 Tracing of drilling mud by acetate addn. - with titration method for selective estimation of acetate in later mud samples

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8000263A FR2473180A1 (en) 1980-01-08 1980-01-08 METHOD OF TRACING THE DRILLING MUD BY DETERMINING THE CONCENTRATION OF A SOLUBLE ION
FR8101134A FR2498332A2 (en) 1980-01-08 1981-01-22 Tracing of drilling mud by acetate addn. - with titration method for selective estimation of acetate in later mud samples

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FR2498332A2 true FR2498332A2 (en) 1982-07-23
FR2498332B2 FR2498332B2 (en) 1985-03-22

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2202048A (en) * 1987-03-09 1988-09-14 Forex Neptune Sa Monitoring drilling mud circulation
GB2202047A (en) * 1987-03-09 1988-09-14 Forex Neptune Sa Monitoring drilling mud
US5140527A (en) * 1988-12-15 1992-08-18 Schlumberger Technology Corporation Method for the determination of the ionic content of drilling mud

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2868625A (en) * 1955-07-22 1959-01-13 Jersey Prod Res Co Method of tracing the flow of water
US3623842A (en) * 1969-12-29 1971-11-30 Exxon Research Engineering Co Method of determining fluid saturations in reservoirs

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2868625A (en) * 1955-07-22 1959-01-13 Jersey Prod Res Co Method of tracing the flow of water
US3623842A (en) * 1969-12-29 1971-11-30 Exxon Research Engineering Co Method of determining fluid saturations in reservoirs

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2202048A (en) * 1987-03-09 1988-09-14 Forex Neptune Sa Monitoring drilling mud circulation
GB2202047A (en) * 1987-03-09 1988-09-14 Forex Neptune Sa Monitoring drilling mud
EP0282232A2 (en) * 1987-03-09 1988-09-14 Services Petroliers Schlumberger Monitoring drilling mud circulation
EP0282232A3 (en) * 1987-03-09 1989-08-16 Forex Neptune Sa Monitoring drilling mud circulation
US4904603A (en) * 1987-03-09 1990-02-27 Schlumberger Technology Corporation Monitoring drilling mud
US5140527A (en) * 1988-12-15 1992-08-18 Schlumberger Technology Corporation Method for the determination of the ionic content of drilling mud

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