CS265658B1 - Method of parallel quantitative determination of by-products in tetrabromodiade - Google Patents
Method of parallel quantitative determination of by-products in tetrabromodiade Download PDFInfo
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- CS265658B1 CS265658B1 CS86704A CS70486A CS265658B1 CS 265658 B1 CS265658 B1 CS 265658B1 CS 86704 A CS86704 A CS 86704A CS 70486 A CS70486 A CS 70486A CS 265658 B1 CS265658 B1 CS 265658B1
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Abstract
Byla vypracována metoda pro kvantitativní stanovení vedlejších produktů v tetrabromdianu po převedení na trimethyl- silyletftery. Analýza se provádí například na náplňové ohromatografické koloně délky 2,40 m a vnitřním průměru 2 mm při teplotě 250 °C a průtoku nosného plynu 22 ml/min. Kolona je smočena silikonem na bílém nosiči. Za podmínek analýzy je možno stanovit chlor- a bromderiváty fenolu, p-isopropenvlfenolu a dianu.A method was developed for the quantitative determination of by-products in tetrabromide after conversion to trimethylsilylethers. The analysis is carried out, for example, on a packed chromatography column with a length of 2.40 m and an internal diameter of 2 mm at a temperature of 250 ° C and a carrier gas flow of 22 ml / min. The column is wetted with silicone on a white support. Under the conditions of the analysis, the chloro- and bromo derivatives of phenol, p-isopropylene phenol and dian can be determined.
Description
(57)(57)
Byla vypracována metoda pro kvantitativní stanovení vedlejších produktů v tetrabromdianu po převedení na trimethylsilyletftery. Analýza se provádí například na náplňové ohromatografické koloně délky 2,40 m a vnitřním průměru 2 mm při teplotě 250 °C a průtoku nosného plynu 22 ml/min. Kolona je smočena silikonem na bílém nosiči. Za podmínek analýzy je možno stanovit chlor- a bromderiváty fenolu, p-isopropenvlfenolu a dianu.A method for the quantitative determination of by-products in tetrabromdian after conversion to trimethylsilyl ether was developed. The analysis is carried out, for example, on a 2.40 m long column chromatography column with an internal diameter of 2 mm at 250 ° C and a carrier gas flow rate of 22 ml / min. The column is wetted with silicone on a white support. Under the conditions of analysis, the chloro and bromo derivatives of phenol, p-isopropenylphenol and diane can be determined.
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Vynález se týká kvantitativního stanoveni vedlejších produktů v tetrabromdlanu metodou plynová chromatografie·The present invention relates to the quantitative determination of by-products in tetrabromdlan by gas chromatography.
Tetrabromdien, t.j. 2,2-bi8-(4-hydroxy-3,5-dibrom)-propan, který je významným retardérem hořeni, se vyrábí bromaci dlenu, t.j. 2,2-bis-(4-hydroxyfenyl)-propanu bromem za přítomnosti chloru. Vedle žádaného produktu vzniká řada vedlejších produktů typu substituovaných fenolů, izopropenylfenolů a dianů, např.Tetrabromadiene, ie 2,2-bis- (4-hydroxy-3,5-dibromo) -propane, which is an important flame retardant, is produced by bromination of dlen, ie 2,2-bis- (4-hydroxyphenyl) -propane with bromine, presence of chlorine. In addition to the desired product, a number of by-products of substituted phenols, isopropenylphenols and dianes, e.g.
X3 Xj X2 - Cl, X3 « Br (I) x2- OH χχ X2 · Br, X3 Cl (II) Χχ xi “ x2 * X3 * Br (I«)Xj X 3 X 2 - Cl, X 3 "Br (I) x 2 OH χ χ · X 2 are Br, X 3 Cl (II) Χ χ x i" * 2 * 3 * X Br (I ")
CH,CH,
0ΗΧ2Χχ X40 ΗΧ 2 Χ χ X 4
OHOH
Χχ X3 Cl, X2 « H, X4 - Br (IV) 3 χ X 3 Cl, X 2 H H, X 4 - Br (IV)
Χχ « X3 « Br, X2 H, X4 - Cl (V) χχ « X3 . X4 . Br, X2 « Η (VI) X1 x2 x3 · x4 “ Br (VII)Χ χ X X 3 Br Br, X 2 H, X 4 - Cl (V) χ χ X X 3 . X 4 . Br, X 2 Η (VI) X 1 x 2 x 3 · x 4 “ Br (VII)
b X4 Hb X 4 H
H, x4 · Br x4 - Br • Br, X4 HH, x 4 · Br x 4 - Br • Br, X 4 H
Cl, X4 Br χ2 β χ4 b BrCl, X 4 Br χ 2 β χ 4 b Br
Br, X. b cl • X4 - Br (VIII) (IX) (x) (xi) (xii) (xiii) (XIV) (xv)Br, X. b cl • X 4 - Br (VIII) (x) (xi) (xii) (xiii) (XIV) (xv)
Obsah vedlejších produktů zhoršuje vlastnosti tetrabromdlanu, takže je žádoucí jejich kvalitu i kvantitu analyticky zjistit.The content of by-products deteriorates the properties of tetrabromdlan, so it is desirable to analyze their quality and quantity.
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Metody určené k analýze směsí po bromaci dianu nejsou známy· Publikovány byly pouze metody pro stanoveni tetrabromdianu ve vzduchu» vodě a sedimentech metodami tenkovrstvá chromatografie* plynová chromatografie* kapalinové chromátografie* epektrofotometrie a plynové chromatografie ve spojeni 8 hmotnostní spektrometrii·Methods for analysis of mixtures after Dian bromination are not known · Only methods for determination of tetrabromate in air »water and sediments by thin layer chromatography * gas chromatography * liquid chromatography * epectrophotometry and gas chromatography in conjunction with 8 mass spectrometry have been published ·
Nyni byl nalezen způsob kvantitativního stanovení vedlejších produktů v tetrabromdianu* který je předmětem tohoto vynálezu a jehož podstata spočivá v tom, že se tetrabromdian silyluje Silylačním činidlem, s výhodou N*O-bis-(trimethyíeilyl)-trifluoroacetamidem a utvořené trimethylsilylethery tetrabromdianu a vedlejších produktů se podrobí plynové chromatografii na náplňové koloně smočené chlorfenylsilikonovým olejem·We have now found a method for the quantitative determination of byproducts in tetrabromodian * which is the object of the present invention, which comprises the silylation of tetrabromodian with a silylating agent, preferably N * O-bis- (trimethylsilyl) -trifluoroacetamide and tetrabromodian trimethylsilyl ethers and byproducts is subjected to gas chromatography on a packed column wetted with chlorophenyl silicone oil ·
Vzorek se silyluje vhodným silylačním činidlem, nejlépe N«0-bl8-(trlmethyleilyl)-trifluoroacetamidem* za zvýšené teploty a nepřistupu vzdušné vlhkosti· Silylovaný produkt se injektuje do odpeřovaciho prostoru plynového chromatografu a po separaci na náplňové koloně smočené chlorfenylovým silikonem se detekuji složky plamenoionizačnim detektorem· Odezvy detektoru se převedou na obsah složek v původním vzorku·The sample is silylated with a suitable silylating agent, preferably N-O-b18- (trlmethyleilyl) -trifluoroacetamide * at elevated temperature and no air humidity. · The silylated product is injected into the vaporization chamber of the gas chromatograph and after separation on a packed column wetted with chlorophenyl silicone Detector responses are converted to the contents of the components in the original sample.
Způsob stanoveni podle vynálezu umožňuje jednoduchým způsobem sledovat průběh reakce, tvorbu vedlejších produktů a hodnotit kvalitu tetrabromdianu·The assay method according to the invention makes it possible to monitor the reaction progress, the formation of by-products and the quality of tetrabromdian in a simple manner.
Přiklad 1 mg tetrabromdianu se silyluje v mikrozkumavce uzavřené propichovací gumovou zátkou 0*25 ml N,O-bis-(trimethyleilyl)-trifluoroacetamidu v kovovém bloku zahřívaném na 80 °C po dobu 30 minut· Na konci silylace se k roztoku přidají 4 kapky chloroformu. Z tohoto roztoku se dávkuje injekční stříkačkou typu Hamilton s kapacitou 10 1 , 0,6 1 do injektoru plynového chromatografu vyhřátého na 280 °C při průtoku nosného plynu dusíku 22 ml/min· Separuje senBkleněné koloně délky 2,40 m a s vnitřním průměrem 2 mm, plněné bílým nosičem zrnění 80 až 100 mesh, smočeným 5 % chlorfenyleilikonového oleje při teplotě 250 °C· ,Example 1 mg of tetrabromodian is silylated in a microtube closed with 0 * 25 ml piercing rubber stopper of N, O-bis- (trimethyleilyl) -trifluoroacetamide in a metal block heated to 80 ° C for 30 minutes. . From this solution is metered Hamilton syringe with a capacity of 10 1 0.6 1 into the injector of the gas chromatograph-heated to 280 ° C with a nitrogen carrier gas flow of 22 ml / min · n Bkleněné separate a column inner diameter of 2.40 mas 2 mm, filled with a white grain carrier of 80 to 100 mesh, dipped with 5% chlorophenyleilicone oil at 250 ° C ·,
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Detekuje ee plamenoionizačnim detektorem, který je vyhřátý na 300 °C. Zastoupeni složek ve vzorku se vyhodnotí z odezev detektoru zpracovaných vyhodnocovacím zařízením přístroje nebo integrátorem.It is detected by a flame ionization detector that is heated to 300 ° C. The representation of the components in the sample is evaluated from the detector responses processed by the instrument evaluation device or the integrator.
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Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CS86704A CS265658B1 (en) | 1986-01-31 | 1986-01-31 | Method of parallel quantitative determination of by-products in tetrabromodiade |
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CS86704A CS265658B1 (en) | 1986-01-31 | 1986-01-31 | Method of parallel quantitative determination of by-products in tetrabromodiade |
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CS70486A1 CS70486A1 (en) | 1989-03-14 |
CS265658B1 true CS265658B1 (en) | 1989-11-14 |
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CS86704A CS265658B1 (en) | 1986-01-31 | 1986-01-31 | Method of parallel quantitative determination of by-products in tetrabromodiade |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2005085216A1 (en) * | 2004-03-05 | 2005-09-15 | Nissan Chemical Industries, Ltd. | Isoxazoline-substituted benzamide compound and noxious organism control agent |
-
1986
- 1986-01-31 CS CS86704A patent/CS265658B1/en unknown
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2005085216A1 (en) * | 2004-03-05 | 2005-09-15 | Nissan Chemical Industries, Ltd. | Isoxazoline-substituted benzamide compound and noxious organism control agent |
EA011764B1 (en) * | 2004-03-05 | 2009-06-30 | Ниссан Кемикал Индастриз, Лтд. | Isoxazoline-substituted benzamide compound and pesticide |
US7662972B2 (en) | 2004-03-05 | 2010-02-16 | Nissan Chemical Industries, Ltd. | Isoxazoline-substituted benzamide compound and pesticide |
AU2005219788B2 (en) * | 2004-03-05 | 2010-06-03 | Nissan Chemical Corporation | Isoxazoline-substituted benzamide compound and noxious organism control agent |
EA014881B1 (en) * | 2004-03-05 | 2011-02-28 | Ниссан Кемикал Индастриз, Лтд. | Substitited alkylbenzene derivatives |
US8022089B2 (en) | 2004-03-05 | 2011-09-20 | Nissan Chemical Industries, Ltd. | Isoxazoline-substituted benzamide compound and pesticide |
US8138213B2 (en) | 2004-03-05 | 2012-03-20 | Nissan Chemical Industries, Ltd. | Isoxazoline-substituted benzamide compound and pesticide |
US8492311B2 (en) | 2004-03-05 | 2013-07-23 | Nissan Chemical Industries, Ltd. | Isoxazoline-substituted benzamide compound and pesticide |
US10045969B2 (en) | 2004-03-05 | 2018-08-14 | Nissan Chemical Industries, Inc. | Isoxazoline-substituted benzamide compound and pesticide |
US10596157B2 (en) | 2004-03-05 | 2020-03-24 | Nissan Chemical Corporation | Isoxazoline-substituted benzamide compound and pesticide |
US10874645B2 (en) | 2004-03-05 | 2020-12-29 | Nissan Chemical Corporation | Isoxazoline-substituted benzamide compound and pesticide |
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Publication number | Publication date |
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CS70486A1 (en) | 1989-03-14 |
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