LU86253A1 - Determn. of polychlorinated bi:phenol(s) in oils - by decomposition and determn. of chloride by mercurimetry - Google Patents

Determn. of polychlorinated bi:phenol(s) in oils - by decomposition and determn. of chloride by mercurimetry Download PDF

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Publication number
LU86253A1
LU86253A1 LU86253A LU86253A LU86253A1 LU 86253 A1 LU86253 A1 LU 86253A1 LU 86253 A LU86253 A LU 86253A LU 86253 A LU86253 A LU 86253A LU 86253 A1 LU86253 A1 LU 86253A1
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LU
Luxembourg
Prior art keywords
content
pcb
oil
ions
determn
Prior art date
Application number
LU86253A
Other languages
French (fr)
Inventor
Nelis Philippe
Original Assignee
Labofina Sa
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 Labofina Sa filed Critical Labofina Sa
Priority to LU86253A priority Critical patent/LU86253A1/en
Priority to IT20787/86A priority patent/IT1190345B/en
Priority to FR8609327A priority patent/FR2584821B3/en
Priority to GB8616003A priority patent/GB2177794B/en
Priority to BE1/011514A priority patent/BE905031A/en
Priority to NO862756A priority patent/NO169312C/en
Priority to DE19863622928 priority patent/DE3622928A1/en
Priority to ES8600215A priority patent/ES2000484A6/en
Priority to TNTNSN86104A priority patent/TNSN86104A1/en
Publication of LU86253A1 publication Critical patent/LU86253A1/en

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
    • 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
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
    • G01N33/0036—Specially adapted to detect a particular component
    • G01N33/0047—Specially adapted to detect a particular component for organic compounds
    • G01N33/0049—Specially adapted to detect a particular component for organic compounds for halogenated organic compounds
    • 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
    • G01N33/26—Oils; viscous liquids; paints; inks
    • G01N33/28—Oils, i.e. hydrocarbon liquids
    • G01N33/2835—Oils, i.e. hydrocarbon liquids specific substances contained in the oil or fuel

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Pathology (AREA)
  • Physics & Mathematics (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Medicinal Chemistry (AREA)
  • Food Science & Technology (AREA)
  • Combustion & Propulsion (AREA)
  • Molecular Biology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The polychlorinated biphenyl (PCB) content of oils is measured by decomposing the PCB to form Cl ions, extracting the Cl ions, determining the Cl ion concn. by mercurimetry, and calculating the PCB content from the Cl ion concn. and the Cl content of PCB. Pref. the oil is diluted with a paraffinic or naphthenic hydrocarbon treated with a soln. of a polycyclic aromatic hydrocarbon in an inert polar solvent, treated with excess alkali metal dispersed in a paraffinic or naphthenic hydrocarbon, treated with a Cl-free aq. acid to remove excess alkali metal, and then decanted. The aq. phase is titrated with an aq. Hg(NO3)2 soln. at pH 1-4 in the presence of an indicator, and the resulting Cl ion concn. (in ppm) is multiplied by 100/T, where T is the estimated Cl content of PCB. Interference from reducing agents in the titration is eliminated by pretreating the aq. phase with an oxidising agent, esp. H2O2. The Cl content due to PCB may be determined by chromatography, the oil on a polar adsorbent, eluting the oil with a 5-10C aliphatic hydrocarbon, removing the solvent from the eluate, and measuring the Cl content of the eluate.

Description

i - ! ‘ ! '<r MEMOIRE DESCRIPTIF déposé à 1'appui d'une DEMANDE DE BREVET DE PREMIERE ADDITION au brevet principal n° 85992 formée par la Société dite : LABOFINA S.A.i -! ‘! '<r DESCRIPTIVE MEMORY filed in support of a FIRST ADDITION PATENT APPLICATION to main patent n ° 85992 formed by the so-called Company: LABOFINA S.A.

pour Méthode de traitement d'huiles contenant des biphényles chlorés.for Method of treatment of oils containing chlorinated biphenyls.

(Inventeur : Monsieur Ph. Nélis).(Inventor: Mister Ph. Nélis).

Le brevet principal n° 85992 concerne une méthode permettant d'évaluer la teneur en biphényles chlorés (en abrégé : PCB) d'huiles, par dosage du chlore provenant de la destruction chimique des PCB. Cette méthode consiste essentiellement à : - détruire chimiquement les PCB contenus dans l'huile, avec formation d'ions de chlore, - extraire ces ions de chlore, λ.The main patent n ° 85992 relates to a method making it possible to evaluate the content of chlorinated biphenyls (abbreviated: PCB) of oils, by determination of the chlorine coming from the chemical destruction of PCBs. This method essentially consists in: - chemically destroying the PCBs contained in the oil, with the formation of chlorine ions, - extracting these chlorine ions, λ.

- 2 - '“ϊ - les doser par mercurimétrie pour obtenir la teneur en chlore de l'huile, et - calculer la teneur en PCB de l'huile à partir de cette teneur en chlore de l'huile et de la teneur estimée en chlore des PCB contenus dans cette huile.- 2 - '“ϊ - measure them by mercurimetry to obtain the chlorine content of the oil, and - calculate the PCB content of the oil from this chlorine content of the oil and the estimated content of chlorine of PCBs contained in this oil.

A cet effet, on met l'huile contenant des PCB, Ä exempte d'autres dérivés chlorés, en contact avec un excès de métal alcalin qui réagit avec les PCB en formant du chlorure de métal alcalin. Lorsque cette réaction est terminée, on élimine l'excès de métal alcalin en utilisant une solution aqueuse acide qui permet également d'extraire les ions de chlore. On laisse ensuite décanter le mélange, on soutire la phase aqueuse, qui contient les ions de chlore, puis on soumet cette phase aqueuse au titrage par une solution de nitate mercurique.To this end, the oil containing PCBs, free from other chlorinated derivatives, is brought into contact with an excess of alkali metal which reacts with the PCBs to form alkali metal chloride. When this reaction is complete, the excess alkali metal is removed using an acidic aqueous solution which also extracts the chlorine ions. The mixture is then allowed to settle, the aqueous phase, which contains the chlorine ions, is drawn off, then this aqueous phase is subjected to titration with a solution of mercuric nitate.

Toutefois, il a été observé que certaines substances réductrices minérales ou organiques, éventuellement présentes dans l'huile traitée, "étaient susceptibles de perturber le dosage par mercurimétrie.However, it has been observed that certain mineral or organic reducing substances, possibly present in the treated oil, "were capable of disturbing the determination by mercurimetry.

Le mode d'exécution faisant l'objet de la présente demande de brevet permet de remédier à cet inconvénient.The embodiment which is the subject of this patent application overcomes this drawback.

Il consiste à extraire les ions de chlore par une solution aqueuse acide et à soumettre la phase aqueuse décantée à un traitement oxydant, avant d'effectuer le dosage par mercurimétrie .It consists in extracting the chlorine ions with an acidic aqueous solution and in subjecting the decanted aqueous phase to an oxidizing treatment, before carrying out the dosage by mercurimetry.

On peut effectuer ce traitement oxydant à l'aide de peroxyde d'hydrogène. On a notamment porté à ébullition la solution aqueuse contenant les ions de chlore en présence d'une solution aqueuse de HjOj à 30 % en poids pen-9 dant environ 10 minutes. Après refroidissement, la phase aqueuse a été filtrée pour séparer toute couche huileuse restante et le filtre a été lavé à l'eau. On a ensuite effectué le dosage mercurimétrique sur l'ensemble du filtrat et des eaux de lavage.This oxidizing treatment can be carried out using hydrogen peroxide. In particular, the aqueous solution containing the chlorine ions was brought to the boil in the presence of an aqueous solution of HjOj at 30% by weight for approximately 10 minutes. After cooling, the aqueous phase was filtered to separate any remaining oily layers and the filter was washed with water. The mercurimetric determination was then carried out on all of the filtrate and of the washing water.

Claims (2)

1. Méthode d'évaluation de la teneur en biphényles chlorés (PCB) d'une huile contaminée par des PCB, par destruction chimique des PCB contenus dans l'huile, avec formation d'ions de chlore, extraction de ces ions de chlo- * re, dosage de ces ions par mercurimétrie pour obtenir la * teneur en chlore de l'huile, puis calcul de la teneur en PCB de l'huile à partir de cette teneur en chlore de l'huile et de la teneur estimée en chlore des PCB contenus dans cette huile, suivant le brevet principal ne 85992, cette méthode étant caractérisée en ce que la - 4 - i. ‘ *- s phase aqueuse décantée, obtenue après extraction des ions de chlore, est soumise à un traitement oxydant, avant dosage de ces ions de chlore.1. Method for evaluating the chlorinated biphenyls (PCB) content of an oil contaminated with PCBs, by chemical destruction of the PCBs contained in the oil, with formation of chlorine ions, extraction of these chlorine ions * re, dosage of these ions by mercurimetry to obtain the * chlorine content of the oil, then calculation of the PCB content of the oil from this chlorine content of the oil and the estimated chlorine content of PCBs contained in this oil, according to main patent no 85992, this method being characterized in that the - 4 - i. ‘* - s decanted aqueous phase, obtained after extraction of the chlorine ions, is subjected to an oxidizing treatment, before dosing of these chlorine ions. 2. Méthode selon la revendication 1, caractérisée en ce que le traitement oxydant consiste à porter la phase aqueuse decantée à température d'ébullition en présence d'une solution aqueuse de t^C^·2. Method according to claim 1, characterized in that the oxidizing treatment consists in bringing the decanted aqueous phase to boiling temperature in the presence of an aqueous solution of t ^ C ^ ·
LU86253A 1985-07-09 1986-01-16 Determn. of polychlorinated bi:phenol(s) in oils - by decomposition and determn. of chloride by mercurimetry LU86253A1 (en)

Priority Applications (9)

Application Number Priority Date Filing Date Title
LU86253A LU86253A1 (en) 1986-01-16 1986-01-16 Determn. of polychlorinated bi:phenol(s) in oils - by decomposition and determn. of chloride by mercurimetry
IT20787/86A IT1190345B (en) 1985-07-09 1986-06-13 PROCEDURE FOR THE TREATMENT OF CHLORINATED BIPHENYL OILS
FR8609327A FR2584821B3 (en) 1985-07-09 1986-06-27 PROCESS FOR THE TREATMENT OF OILS CONTAINING CHLORINATED BIPHENYLES
GB8616003A GB2177794B (en) 1985-07-09 1986-07-01 Method for treating oils containing polychlorinated biphenyls
BE1/011514A BE905031A (en) 1985-07-09 1986-07-02 METHOD OF TREATING OILS CONTAINING CHLORINATED BIPHENYLES.
NO862756A NO169312C (en) 1985-07-09 1986-07-08 PROCEDURE FOR AA DETERMINING THE CONTENT OF POLYCLORATED BIFENYL COMPOUNDS IN AN OIL.
DE19863622928 DE3622928A1 (en) 1985-07-09 1986-07-08 METHOD FOR TREATING OILS CONTAINING POLYCHLORINE BIPHENYLE
ES8600215A ES2000484A6 (en) 1985-07-09 1986-07-09 Method for treating oils containing polychlorinated biphenyls
TNTNSN86104A TNSN86104A1 (en) 1985-07-09 1986-07-09 METHOD OF TREATING OILS CONTAINING CHLORINATED BIPHENYLS

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
LU86253 1986-01-16
LU86253A LU86253A1 (en) 1986-01-16 1986-01-16 Determn. of polychlorinated bi:phenol(s) in oils - by decomposition and determn. of chloride by mercurimetry

Publications (1)

Publication Number Publication Date
LU86253A1 true LU86253A1 (en) 1987-03-06

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