Classifications

• • G—PHYSICS
  • G01—MEASURING; TESTING
  • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
  • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
  • G01N30/96—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange
• • G—PHYSICS
  • G01—MEASURING; TESTING
  • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
  • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
• • 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
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T436/00—Chemistry: analytical and immunological testing
  • Y10T436/18—Sulfur containing
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T436/00—Chemistry: analytical and immunological testing
  • Y10T436/19—Halogen containing
  • Y10T436/193333—In aqueous solution
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T436/00—Chemistry: analytical and immunological testing
  • Y10T436/20—Oxygen containing
  • Y10T436/200833—Carbonyl, ether, aldehyde or ketone containing
  • Y10T436/201666—Carboxylic acid
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T436/00—Chemistry: analytical and immunological testing
  • Y10T436/25—Chemistry: analytical and immunological testing including sample preparation
  • Y10T436/25375—Liberation or purification of sample or separation of material from a sample [e.g., filtering, centrifuging, etc.]
  • Y10T436/255—Liberation or purification of sample or separation of material from a sample [e.g., filtering, centrifuging, etc.] including use of a solid sorbent, semipermeable membrane, or liquid extraction

Definitions

• a method for the determination of anions in solution by means of ion exchange comprising adding to a solution, preferably an aqueous solution containing an anion in unknown quantity to be analyzed, a compound selected from the group consisting of quaternary aliphatic ammonium picrates having a total of at least 30 carbon atoms, preferably dissolved in an immiscible organic solvent, thereby to form by ion exchange the corresponding quaternary ammonium compound of said anion to be analyzed and to release a corresponding amount of picrate anion.
• two layers are formed upon mixing and the quaternary ammonium compound of said unknown anion becomes dissolved in the organic solvent, while said released picrate ion becomes dissolved in the aqueous phase.
• Known techniques such as optical methods are employed to determine the amount of released picrate ion, which is a measure of the amount of original unknown anion to be analyzed.
• the present invention relates to a method for quantitative determination of anions by means of liquid ion exchange.
• the object of the present invention is to determine anions quantitatively with precision.
• the present invention comprises using at least one compound 3,725,006 Patented Apr. 3, 1973 selected from the group consisting of quaternary aliphatic ammonium picrates having a total of at least 30 carbon atoms as anion exchange compound.
• the total number of carbon atoms is 38, and preferably the aliphatic groups are alkyl, suitably alkyl chains having 6 to 8 carbons, and most preferably identical alkyl chains.
• n-tetrahexylammonium picrate has been found to be especially suitable but also n-tetraheptyl and n-tetraoctylammonium picrate can be used.
• X- is an ion P- is a picrate ion
• Q+ is a quaternary ammonium ion
• concentration E is extraction constant
• aq is aqueous phase
• org is organic phase Addition of the reactions 1 and 3 give aq+Q or aq. +Q org which corresponds to the equation given above.
• the concentration of picrate ions is equal to the sum of the concentration of free quaternary ammonium ions and the concentration of ion pairs between the quaternary ammonium ion and X.
• this ion reaction is used for analytical purposes the analytical error is zero when the concentration of picrate ions is equal to the initial concentration of the anion X; which is equal to the sum of the concentration 0f the free anion X" and the concentration of (R NX in the organic phase.
• a basis for the determination of the experimental conditions is optical properties, such as the light absorption or fluorimetric characteristics of the anion (C6H2N307)
• the molar absorptivity of the picrate ion in an aqueous solution is 1.4 10 at the absorbance maximum, 355 III/L.
• the most suitable concentration range for a sample is easily calculated to about 10 to 10* moles per litre when a 1 cm. photometric cell is used.
• the choice of reagent concentration is determined by the magnitude of the extraction constant for (R NX.
• the quaternary ammonium picrate is preferably used in at least about 50 times excess, suitably at least about 100 times excess in comparison with the amount of anion which is to be determined.
• Tetrahexylammonium picrate was prepared by shaking 1.5 moles (721.5 g.) of tetrahexylammonium iodide in methylene chloride with a first aqueous solution of 1.65 moles (343.5 g.) of picric acid adjusted to pH 8 with NaOH. When the phases had separated the aqueous phase was removed and a new aqueous solution containing 0.175 mole (40 g.) of picric acid adjusted to pH 8 with NaOH was added to the methylene chloride solution. The phases were shaken and allowed to separate. The aqueous phase was removed and the methylene chloride phase was washed with distilled water. Then the methylene chloride phase was evaporated and the residue, 800 g. of tetrahexylammonium picrate, was recrystallized from acetonitrile. Yield 92%. MP. 25-35 C.
• EXAMPLE 2 The determination of the anion dioctylsulphosuccinate was made by shaking first 10.0 ml. of sodium dioctylsulphosuccinate dissolved in a phosphate buffer having pH 6.5 and the concentration of 10" moles per litre with regard of Na-dioctylsulphosuccinate (10- moles of Nadioctylsulphosuccinate) in a 30 ml. centrifuge tube with a glass stopper with 10.0 ml. of a solution of tetrahexylammonium picrate in methylene chloride having the concentration of 10- moles per litre, that is moles of tetrahexylammonium picrate. Then the tube was centrifuged to separate the two phases and the absorption of the aqueous phase at 355 my. was measured.
• the standard curve is obtained from the following data:
• EXAMPLE 3 The determination of an anion having a small extraction constant was also carried out. As anion the perchlorate ion, C10 1 was selected.
• EXAMPLE 4 The same test as in Example 3 was carried out with lauryl sulphate, at first a standard curve being obtained which was similar to the one for the perchlorate ion.
• the present invention is useful for the determination of anions, which together with the quaternary ammonium ion have an extraction constant exceeding about 10
• examples of such anions which can be determined are the anions of aliphatic and aromatic sulphonic acids, dialkylsulphosuccinates and higher aliphatic and aromatic carboxylic acids.
• the extraction constant of tetrahexylammonium perchlorate is 10 which gives a satisfactorily high reaction yield for quantitative estimations, while iodide, the extraction constant of which is 10 has a too low reaction yield for quantitative use.
• the present method is industrially useful as mentioned above, for example, for the stability control of sodium dioctylsulphosuccinate, but can in general be used for the determination of anions in waste water, for purity control in chemical synthesis operations and for quality control of pharmaceuticals.
• a method for the determination of anions by means of liquid ion exchange characterized in that a compound selected from the group consisting of quaternary aliphatic ammonium picrates having at least 30 carbon atoms in total is used as anion exchanging compound.
• a method for the determination of anions in solution by means of ion exchange comprising adding to a solution containing an anion in unknown quantity to be analyzed, a compound selected from the group consisting of quaternary aliphatic ammonium picrates having a total of at least 30 carbon atoms, thereby to form by ion exchange the corresponding quaternary ammonium compound of said anion to be analyzed and release a corresponding amount of picrate anion, and measuring the amount of picrate anion so released, said unknown anion being such that its said quaternary ammonium compound so formed has an extraction constant exceeding about 10 7.
• alkyl groups have 6 to 8 carbon atoms.
• alkyl groups are identical and have 6 to 8 carbon atoms.
• Su1fur1'c shou1d be Su1phonic Co1umn 2, 11'ne 30 "ion shou1d be anion Co1umn 2, 11'ne 39, "0rd” shou1d be org Co1umn 3, 11"ne 45, "455 nm” shou1d be 355 nm Signed and ⁇ sealed this 18th day of December 1973.

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• Health & Medical Sciences (AREA)
• Life Sciences & Earth Sciences (AREA)
• Physics & Mathematics (AREA)
• Chemical & Material Sciences (AREA)
• Analytical Chemistry (AREA)
• Biochemistry (AREA)
• General Health & Medical Sciences (AREA)
• General Physics & Mathematics (AREA)
• Immunology (AREA)
• Pathology (AREA)
• Molecular Biology (AREA)
• Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

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Family Applications (1)

Country Status (7)

Cited By (6)

• 1970
  • 1970-06-04 SE SE7790/70A patent/SE342510B/xx unknown
• 1971
  • 1971-05-26 CH CH769171A patent/CH555541A/xx not_active IP Right Cessation
  • 1971-05-27 DE DE19712126291 patent/DE2126291A1/de active Pending
  • 1971-05-28 GB GB1813171A patent/GB1332043A/en not_active Expired
  • 1971-06-01 CA CA114470A patent/CA931055A/en not_active Expired
  • 1971-06-02 FR FR7119994A patent/FR2095820A5/fr not_active Expired
  • 1971-06-03 US US00149766A patent/US3725006A/en not_active Expired - Lifetime

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