LU86285A1 - 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 PDFInfo
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- LU86285A1 LU86285A1 LU86285A LU86285A LU86285A1 LU 86285 A1 LU86285 A1 LU 86285A1 LU 86285 A LU86285 A LU 86285A LU 86285 A LU86285 A LU 86285A LU 86285 A1 LU86285 A1 LU 86285A1
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- 239000003921 oil Substances 0.000 title claims abstract description 46
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 title 1
- 238000000354 decomposition reaction Methods 0.000 title 1
- 239000002904 solvent Substances 0.000 claims abstract description 22
- 239000003463 adsorbent Substances 0.000 claims abstract description 6
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 claims abstract description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 28
- 239000000460 chlorine Substances 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 21
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 15
- 229910052801 chlorine Inorganic materials 0.000 claims description 15
- 150000001491 aromatic compounds Chemical class 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000002480 mineral oil Substances 0.000 claims description 8
- 238000010828 elution Methods 0.000 claims description 7
- 238000013375 chromatographic separation Methods 0.000 claims description 6
- QWTDNUCVQCZILF-UHFFFAOYSA-N isopentane Chemical compound CCC(C)C QWTDNUCVQCZILF-UHFFFAOYSA-N 0.000 claims description 6
- 125000004432 carbon atom Chemical group C* 0.000 claims description 3
- AFABGHUZZDYHJO-UHFFFAOYSA-N dimethyl butane Natural products CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 claims description 2
- JVSWJIKNEAIKJW-UHFFFAOYSA-N dimethyl-hexane Natural products CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 claims description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims 2
- 150000003071 polychlorinated biphenyls Chemical group 0.000 abstract description 26
- 150000002500 ions Chemical class 0.000 abstract description 6
- 238000004448 titration Methods 0.000 abstract description 3
- 239000004215 Carbon black (E152) Substances 0.000 abstract 2
- 229910052783 alkali metal Inorganic materials 0.000 abstract 2
- 150000001340 alkali metals Chemical class 0.000 abstract 2
- 229930195733 hydrocarbon Natural products 0.000 abstract 2
- 150000002430 hydrocarbons Chemical class 0.000 abstract 2
- 239000002253 acid Substances 0.000 abstract 1
- 239000003638 chemical reducing agent Substances 0.000 abstract 1
- 238000004587 chromatography analysis Methods 0.000 abstract 1
- ORMNPSYMZOGSSV-UHFFFAOYSA-N mercury(II) nitrate Inorganic materials [Hg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ORMNPSYMZOGSSV-UHFFFAOYSA-N 0.000 abstract 1
- 239000007800 oxidant agent Substances 0.000 abstract 1
- 239000002798 polar solvent Substances 0.000 abstract 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000012530 fluid Substances 0.000 description 6
- 235000010446 mineral oil Nutrition 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
- 239000003085 diluting agent Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000008030 elimination Effects 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- BTAGRXWGMYTPBY-UHFFFAOYSA-N 1,2,3-trichloro-4-(2,3,4-trichlorophenyl)benzene Chemical compound ClC1=C(Cl)C(Cl)=CC=C1C1=CC=C(Cl)C(Cl)=C1Cl BTAGRXWGMYTPBY-UHFFFAOYSA-N 0.000 description 1
- XKEFYDZQGKAQCN-UHFFFAOYSA-N 1,3,5-trichlorobenzene Chemical compound ClC1=CC(Cl)=CC(Cl)=C1 XKEFYDZQGKAQCN-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000002477 conductometry Methods 0.000 description 1
- 238000003869 coulometry Methods 0.000 description 1
- 230000005264 electron capture Effects 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 150000001911 terphenyls Chemical class 0.000 description 1
Classifications
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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—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
- G01N33/0047—Organic compounds
- G01N33/0049—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—Specific substances contained in the oils or fuels
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Pathology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Physics & Mathematics (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)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
Description
MEMOIRE DESCRIPTIF déposé à 1 * appui d1 uneDESCRIPTIVE MEMORY filed at the press of a
DEMANDE DE BREVET D'INVENTIONPATENT INVENTION APPLICATION
formée par la Société dite : LABOFINA S.A.formed by the so-called Company: LABOFINA S.A.
pour Méthode de traitement d'huiles contenant des composés aromatiques polyhalogénés.for Method of treatment of oils containing polyhalogenated aromatic compounds.
Inventeur : Monsieur Ph. NélisInventor: Monsieur Ph. Nélis
La présente invention se rapporte à une méthode de traitement d'huiles minérales contenant des composés aromatiques polyhalogénés. Elle concerne plus spécialement une méthode permettant d'éliminer sélectivement les paraffines chlorées utilisées fréquemment dans la formulation d'huiles industrielles contenant des composés aromatiques polyhalogénés, notamment des composés aromatiques polychlorés, tels que biphényles polychlorés et terphényles polychlorés.The present invention relates to a method for treating mineral oils containing polyhalogenated aromatic compounds. More particularly, it relates to a method making it possible to selectively remove the chlorinated paraffins frequently used in the formulation of industrial oils containing polyhalogenated aromatic compounds, in particular polychlorinated aromatic compounds, such as polychlorinated biphenyls and polychlorinated terphenyls.
- 2 -- 2 -
Ces composés aromatiques polyhalogénés, dont les biphényles polychlorés (désignés ci-après par PCB) sont les représentants les plus utilisés, se trouvent, en combinaisons variées, dans des fluides industriels dont les appli-a cations sont nombreuses : fluides diélectriques pour trans formateurs, fluides caloporteurs, fluides hydrauliques, etc «. «These polyhalogenated aromatic compounds, of which polychlorinated biphenyls (hereinafter referred to as PCBs) are the most used representatives, are found, in various combinations, in industrial fluids whose applications are numerous: dielectric fluids for transformers, heat transfer fluids, hydraulic fluids, etc. ". "
Depuis que les PCB ont été classés comme polluants, des critères ont été établis pour classer les fluides en fonction de leur teneur en PCB. C'est ainsi que d'après 1'Environmental Protection Agency aux Etats-Unis d'Amérique, les fluides contenant moins de 50 ppm (parties par million) de PCB sont considérés comme étant exempts de PCB, ceux avec une teneur de 50 à 500 ppm sont estimés contaminés, tandis que ceux à plus de 500 ppm sont classés PCB.Since PCBs have been classified as pollutants, criteria have been established to classify fluids according to their PCB content. For example, according to the Environmental Protection Agency in the United States of America, fluids containing less than 50 ppm (parts per million) of PCBs are considered to be free of PCBs, those with a content of 50 to 500 ppm are considered contaminated, while those above 500 ppm are classified as PCB.
Les réglementations actuellement appliquées dans un pays peuvent être modifiées. De plus, elles varient d'un pays à l'autre. D'autre part, les industriels traitant des huiles contaminées pour en réduire la teneur en PCB ainsi que les utilisateurs achetant des huiles régénérées désirent connaître la teneur en PCB avec plus de précision .The regulations currently applied in a country are subject to change. In addition, they vary from country to country. On the other hand, manufacturers treating contaminated oils to reduce their PCB content as well as users purchasing regenerated oils want to know the PCB content more precisely.
Les méthodes qui permettent de déterminer la teneur en PCB d'une huile font appel à des appareillages très coûteux tels que la chromatographie gazeuse couplée à un détecteur à capture d'électrons, à un spectromètre de masse, à un spectromètre infra-rouge à transformée de Fourier ou encore à la chromatographie liquide à haute performance. Toutes ces techniques sont compliquées et nécessitent une infrastructure fixe ainsi qu'un personnel-hautement qualifié .Methods for determining the PCB content of an oil use very expensive equipment such as gas chromatography coupled with an electron capture detector, a mass spectrometer, an infrared transform spectrometer. Fourier or high performance liquid chromatography. All these techniques are complicated and require a fixed infrastructure as well as highly qualified personnel.
De nombreux utilisateurs préfèrent des méthodes plus simples et moins coûteuses basées sur la détermination du Cl. Parmi ces méthodes, nous pouvons citer : la - coulométrie, les rayons X, l'analyse élémentaire par miné- - 3 - ralisation et dosage des ions Cl par titrimétrie, conducti-métrie, électrode spécifique, etc ... Certains de ces tests ne nécessitent que très peu de matériel et peuvent être considérés comme des méthodes de terrain. Cependant, avec ces méthodes analytiques basées sur la détermination du Cl, les valeurs trouvées ne résultent pas toujours de la seule présence des PCB dans les huiles minérales examinées. En effet, dans certaines formulations d'huiles industrielles, on utilise fréquemment des paraffines chlorées. Si un échantillon d'huile contient à la fois des paraffines chlorées et des PCB, la teneur en Cl mesurée ne peut être transformée en teneur en PCB.Many users prefer simpler and less costly methods based on the determination of Cl. Among these methods, we can cite: - coulometry, X-rays, elemental analysis by mineralization - 3 - realization and determination of Cl ions by titrimetry, conductometry, specific electrode, etc. Some of these tests require very little equipment and can be considered as field methods. However, with these analytical methods based on the determination of Cl, the values found do not always result from the mere presence of PCBs in the mineral oils examined. In fact, in certain formulations of industrial oils, chlorinated paraffins are frequently used. If an oil sample contains both chlorinated paraffins and PCBs, the Cl content measured cannot be transformed into PCB content.
De plus, certains fabricants de PCB diluaient les PCB par des monoaromatiques polychlorés, comme le 1,3,5 trichlorobenzène pour réduire la viscosité du mélange. ASKAREL est d'ailleurs une appellation commerciale caractérisant des mélanges de PCB et de ces diluants.In addition, some PCB manufacturers diluted PCBs with polychlorinated monoaromatics, such as 1,3,5 trichlorobenzene to reduce the viscosity of the mixture. ASKAREL is also a trade name characterizing mixtures of PCBs and these diluents.
On voit donc qu'il est nécessaire de pouvoir disposer d'une méthode peu coûteuse, facilement applicable, assurant une élimination sélective des paraffines chlorées hors d'huiles industrielles et permettant, par conséquent, de déterminer avec précision la teneur en PCB de ces huiles .It is therefore seen that it is necessary to be able to have an inexpensive method, easily applicable, ensuring a selective elimination of chlorinated paraffins out of industrial oils and therefore making it possible to precisely determine the PCB content of these oils. .
A cet effet, la méthode de la présente invention consiste essentiellement à soumettre un échantillon de l'huile à examiner à une séparation chromatographique liquide-solide dans une colonne contenant un adsorbant polaire, à effectuer l'élution d'huile exempte de paraffines chlorées à l'aide d'un solvant consistant en un hydrocarbure aliphatique saturé, ramifié ou non, contenant de 5 à 10 atomes de carbone, à éliminer le solvant hors de l'éluat récupéré, puis à déterminer la teneur en PCB de cet éluat débarrassé du solvant.To this end, the method of the present invention essentially consists in subjecting a sample of the oil to be examined to a liquid-solid chromatographic separation in a column containing a polar adsorbent, in carrying out the elution of oil free of chlorinated paraffins to using a solvent consisting of a saturated aliphatic hydrocarbon, branched or not, containing from 5 to 10 carbon atoms, to remove the solvent out of the eluate recovered, then to determine the PCB content of this eluate freed from the solvent.
La séparation chromatographique s'effectue à l'ai->. de d'une colonne contenant un adsorbant polaire, notamment - 4 - un adsorbant avec sites hydroxyles, tel que silice. Les matériaux polaires sont retenus sur la colonne, les paraffines chlorées étant absorbées en tête de colonne et étant séparées du mélange d'huile minérale et de PCB.The chromatographic separation is carried out with a->. of a column containing a polar adsorbent, in particular an adsorbent with hydroxyl sites, such as silica. The polar materials are retained on the column, the chlorinated paraffins being absorbed at the head of the column and being separated from the mixture of mineral oil and PCB.
- On effectue ensuite l'élution de ce mélange en faisant passer dans la colonne un solvant consistant en un hydrocarbure aliphatique saturé, ramifié ou non, contenant de 5 à 10 atomes de carbone. A titre d'exemples, on peut citer 11isopentane, le n-hexane, le n-heptane et l'isooctane. On utilise de préférence un solvant à bas point d'ébullition, notamment l'hexane. La fraction ainsi récupérée consiste en solvant et huile traitée ne contenant plus que les PCB.The elution of this mixture is then carried out by passing through the column a solvent consisting of a saturated aliphatic hydrocarbon, branched or not, containing from 5 to 10 carbon atoms. By way of examples, mention may be made of isopentane, n-hexane, n-heptane and isooctane. Preferably, a solvent with a low boiling point is used, in particular hexane. The fraction thus recovered consists of solvent and treated oil containing only the PCBs.
Des essais comparatifs ont montré que cette méthode est particulièrement sélective et permet d'éliminer les paraffines chlorées initialement présentes dans une huile minérale contenant des PCB. Pour ces essais, on a préparé trois solutions à base d'huile minérale pour transformateurs :Comparative tests have shown that this method is particularly selective and makes it possible to remove the chlorinated paraffins initially present in a mineral oil containing PCBs. For these tests, three solutions based on mineral oil for transformers were prepared:
Solution I : huile + 5 % (en poids) de paraffines chlorées ;Solution I: oil + 5% (by weight) of chlorinated paraffins;
Solution II : huile + 5 % de PCB;Solution II: oil + 5% PCB;
Solution III : huile + 5 % de paraffines chlorées + 5 % de PCB.Solution III: oil + 5% chlorinated paraffins + 5% PCB.
Chaque solution a été soumise à une séparation chromatographique dans une colonne à garnissage de silice. On a ensuite soumis à élution en utilisant successivement les solvants suivants : hexane, toluène, dichlorométhane, éther éthylique, acétone et méthanol. L'analyse infrarouge a montré que le premier éluat, c'est-à-dire l'éluat à l'hexane, contenait : pour la solution I : uniquement de l'huile; pour la solution II : de l'huile ainsi que les PCB; pour la solution III : de l'huile ainsi que les PCB.Each solution was subjected to chromatographic separation in a column packed with silica. It was then subjected to elution using successively the following solvents: hexane, toluene, dichloromethane, ethyl ether, acetone and methanol. The infrared analysis showed that the first eluate, that is to say the hexane eluate, contained: for solution I: only oil; for solution II: oil and PCBs; for solution III: oil and PCBs.
- 5 -- 5 -
Dans l'éluat suivant, ou éluat au toluène, on a constaté la présence des paraffines chlorées pour les solutions I et III. Dans les autres éluats, on n'a remarqué par infra-rouge ni paraffines chlorées, ni PCB pour les 3 . solutions.In the following eluate, or toluene eluate, the presence of chlorinated paraffins was observed for solutions I and III. In the other eluates, no infrared chlorinated paraffins or PCBs were noted for the 3. solutions.
La méthode de la présente invention permet donc d'obtenir un éluat exempt de paraffines chlorées et comprenant le solvant, de l'huile minérale et les PCB. On élimine ensuite le solvant en chauffant doucement. Sur l'huile récupérée contenant les PCB, on détermine la teneur en chlore en utilisant toute méthode connue, notamment la méthode par titrimétrie décrite dans le brevet luxembourgeois n° 85992 de la Demanderesse.The method of the present invention therefore makes it possible to obtain an eluate free from chlorinated paraffins and comprising the solvent, mineral oil and PCBs. The solvent is then removed by gentle heating. On the recovered oil containing the PCBs, the chlorine content is determined using any known method, in particular the titrimetry method described in the Luxembourg patent No. 85992 of the Applicant.
Le teneur en chlore d'origine PCB de l'huile de départ se calcule d'après la formule IThe original chlorine PCB content of the starting oil is calculated according to formula I
Cl = C2.W2 (Formule I) W1 dans laquelleCl = C2.W2 (Formula I) W1 in which
Cl est la teneur en chlore d'origine PCB de l'huile de départ, C2 est la teneur en chlore de l'huile éluée et séparée du solvant, W2 est le poids d'huile éluée et séparée du solvant, W1 est le poids d'huile soumise à la séparation chromato-graphique.Cl is the original chlorine content PCB of the starting oil, C2 is the chlorine content of the oil eluted and separated from the solvent, W2 is the weight of oil eluted and separated from the solvent, W1 is the weight of oil subjected to chromatographic separation.
D'après un mode d'exécution de l'invention, on pèse une quantité Wl, généralement comprise entre 5 et 10 grammes, de l'huile à examiner. On dilue cet échantillon par une quantité équipondérale d'hexane ou solvant similaire et on le place en tête d'une colonne chromatographi-que (hauteur : 40 cm; diamètre : 1 cm) remplie de gel de silice ou d'alumine. On effectue ensuite l'élution par de l'hexane ou autre solvant similaire et on récupère une fraction comprenant le solvant et de l'huile contaminée par les PCB, mais exempte de paraffines chlorées. Lorsque » * - 6 - l'élution est terminée, on chauffe doucement pour éliminer le solvant- On pèse la quantité W2 d'huile récupérée. On détermine ensuite la teneur C2 en chlore de cette huile.According to an embodiment of the invention, an amount W1, generally between 5 and 10 grams, of the oil to be examined is weighed. This sample is diluted with an equal weight of hexane or similar solvent and placed at the head of a chromatographic column (height: 40 cm; diameter: 1 cm) filled with silica gel or alumina. The elution is then carried out with hexane or other similar solvent and a fraction comprising the solvent and oil contaminated with PCBs, but free of chlorinated paraffins, is recovered. When the elution is complete, the mixture is gently heated to remove the solvent. The quantity W2 of oil recovered is weighed. The C2 content of chlorine in this oil is then determined.
Le chlore ainsi dosé étant uniquement d'origine PCB et/ou . de leurs diluants, on aura donc la teneur Cl en chlore d'origine PCB et/ou de leurs diluants de l'huile de départ en appliquant la formule I donnée ci-dessus.The chlorine thus dosed being only of PCB and / or origin. of their diluents, there will therefore be the Cl content of chlorine of PCB origin and / or of their diluents of the starting oil by applying formula I given above.
Les exemples suivants sont donnés à titre d'illustration et ne comportent aucun caractère limitatif.The following examples are given by way of illustration and are in no way limiting.
Exemple 1Example 1
Afin de vérifier le mode d'exécution décrit ci-dessus, on a préparé une composition à base d'huile minérale pour transformateur et contenant des paraffines chlorées et des PCB. La teneur en chlore de cette huile était de 451 ppm (parties par million), à savoir 151 ppm de chlore d'origine paraffines chlorées et 300 ppm d'origine PCB.In order to verify the embodiment described above, a composition based on mineral oil for transformer was prepared and containing chlorinated paraffins and PCBs. The chlorine content of this oil was 451 ppm (parts per million), namely 151 ppm of chlorine from chlorinated paraffins and 300 ppm from PCB.
On a utilisé une colonne chromatographique contenant du gel de silice et on a effectué la dilution de l'huile ainsi que l'élution à l'aide d'hexane.A chromatographic column containing silica gel was used and the oil was diluted as well as eluted with hexane.
La quantité de composition mise en oeuvre était de 5 grammes.The amount of composition used was 5 grams.
Après élution et évaporation de l'hexane, on a recueilli 4,75 grammes d'huile, dont la teneur en chlore était de 310 ppm.After elution and evaporation of the hexane, 4.75 grams of oil were collected, the chlorine content of which was 310 ppm.
En appliquant la formule I, on a trouvé que la teneur en chlore, qui est uniquement d'origine PCB, de la composition de départ était de 295 ppm, ce qui démontre que le procédé de l'invention assure l'élimination complète des paraffines chlorées.By applying formula I, it was found that the chlorine content, which is only of PCB origin, of the starting composition was 295 ppm, which demonstrates that the process of the invention ensures the complete elimination of paraffins chlorinated.
Exemple 2 :Example 2:
On a répété le mode opératoire décrit à l'exemple 1, mais en remplaçant le n-hexane par de 1'isopentane.The procedure described in Example 1 was repeated, but replacing the n-hexane with isopentane.
On a trouvé que la teneur en chlore d'origine PCBIt has been found that the chlorine content of PCB origin
Claims (4)
Priority Applications (9)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| LU86285A LU86285A1 (en) | 1986-01-31 | 1986-01-31 | 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. |
| DE19863622928 DE3622928A1 (en) | 1985-07-09 | 1986-07-08 | METHOD FOR TREATING OILS CONTAINING POLYCHLORINE BIPHENYLE |
| NO862756A NO169312C (en) | 1985-07-09 | 1986-07-08 | PROCEDURE FOR AA DETERMINING THE CONTENT OF POLYCLORATED BIFENYL COMPOUNDS IN AN OIL. |
| TNTNSN86104A TNSN86104A1 (en) | 1985-07-09 | 1986-07-09 | METHOD OF TREATING OILS CONTAINING CHLORINATED BIPHENYLS |
| ES8600215A ES2000484A6 (en) | 1985-07-09 | 1986-07-09 | Method for treating oils containing polychlorinated biphenyls |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| LU86285 | 1986-01-31 | ||
| LU86285A LU86285A1 (en) | 1986-01-31 | 1986-01-31 | Determn. of polychlorinated bi:phenol(s) in oils - by decomposition and determn. of chloride by mercurimetry |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| LU86285A1 true LU86285A1 (en) | 1987-09-03 |
Family
ID=19730632
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| LU86285A LU86285A1 (en) | 1985-07-09 | 1986-01-31 | Determn. of polychlorinated bi:phenol(s) in oils - by decomposition and determn. of chloride by mercurimetry |
Country Status (1)
| Country | Link |
|---|---|
| LU (1) | LU86285A1 (en) |
-
1986
- 1986-01-31 LU LU86285A patent/LU86285A1/en unknown
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