CS238795B1 - Method of determining of 2,5-dialcoxy-4-morpholinylbendiazone compositions - Google Patents
Method of determining of 2,5-dialcoxy-4-morpholinylbendiazone compositions Download PDFInfo
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- CS238795B1 CS238795B1 CS84260A CS26084A CS238795B1 CS 238795 B1 CS238795 B1 CS 238795B1 CS 84260 A CS84260 A CS 84260A CS 26084 A CS26084 A CS 26084A CS 238795 B1 CS238795 B1 CS 238795B1
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- Czechoslovakia
- Prior art keywords
- diazonium
- determined
- electrode
- passive component
- excess
- Prior art date
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- 238000000034 method Methods 0.000 title claims abstract description 8
- 239000000203 mixture Substances 0.000 title 1
- 239000012954 diazonium Substances 0.000 claims abstract description 7
- -1 diazonium cation Chemical class 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 4
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 2
- 150000001989 diazonium salts Chemical class 0.000 abstract description 5
- DYRDKSSFIWVSNM-UHFFFAOYSA-N acetoacetanilide Chemical compound CC(=O)CC(=O)NC1=CC=CC=C1 DYRDKSSFIWVSNM-UHFFFAOYSA-N 0.000 abstract description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 abstract description 2
- 239000010931 gold Substances 0.000 abstract description 2
- 229910052737 gold Inorganic materials 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-O diazynium Chemical compound [NH+]#N IJGRMHOSHXDMSA-UHFFFAOYSA-O 0.000 abstract 2
- 230000015556 catabolic process Effects 0.000 abstract 1
- 238000006731 degradation reaction Methods 0.000 abstract 1
- 238000011835 investigation Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 7
- KAZMCIGKULUUMR-UHFFFAOYSA-N 6-methylpyridazin-3-amine Chemical compound CC1=CC=C(N)N=N1 KAZMCIGKULUUMR-UHFFFAOYSA-N 0.000 description 5
- 239000000126 substance Substances 0.000 description 3
- JJYPMNFTHPTTDI-UHFFFAOYSA-N 3-methylaniline Chemical compound CC1=CC=CC(N)=C1 JJYPMNFTHPTTDI-UHFFFAOYSA-N 0.000 description 2
- APRRQJCCBSJQOQ-UHFFFAOYSA-N 4-amino-5-hydroxynaphthalene-2,7-disulfonic acid Chemical compound OS(=O)(=O)C1=CC(O)=C2C(N)=CC(S(O)(=O)=O)=CC2=C1 APRRQJCCBSJQOQ-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- RZXMPPFPUUCRFN-UHFFFAOYSA-N p-toluidine Chemical compound CC1=CC=C(N)C=C1 RZXMPPFPUUCRFN-UHFFFAOYSA-N 0.000 description 2
- 238000003969 polarography Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- KOPFEFZSAMLEHK-UHFFFAOYSA-N 1h-pyrazole-5-carboxylic acid Chemical compound OC(=O)C=1C=CNN=1 KOPFEFZSAMLEHK-UHFFFAOYSA-N 0.000 description 1
- YOVXTCPXRNWWRF-UHFFFAOYSA-N 2,5-dibutoxy-4-morpholin-4-ylaniline Chemical compound C1=C(N)C(OCCCC)=CC(N2CCOCC2)=C1OCCCC YOVXTCPXRNWWRF-UHFFFAOYSA-N 0.000 description 1
- UIKUBYKUYUSRSM-UHFFFAOYSA-N 3-morpholinopropylamine Chemical compound NCCCN1CCOCC1 UIKUBYKUYUSRSM-UHFFFAOYSA-N 0.000 description 1
- XJCVRTZCHMZPBD-UHFFFAOYSA-N 3-nitroaniline Chemical compound NC1=CC=CC([N+]([O-])=O)=C1 XJCVRTZCHMZPBD-UHFFFAOYSA-N 0.000 description 1
- 239000006171 Britton–Robinson buffer Substances 0.000 description 1
- AFBPFSWMIHJQDM-UHFFFAOYSA-N N-methyl-N-phenylamine Natural products CNC1=CC=CC=C1 AFBPFSWMIHJQDM-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 229940075397 calomel Drugs 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 125000000664 diazo group Chemical group [N-]=[N+]=[*] 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000003891 environmental analysis Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Předmětem vynálezu je způsob stanovení 2,5-dialkoxy-4-morfolinylbenzen-diazoniovýoh sloučenin, jehož podstata spočívá v tom, že se stanovovaný diazoniový kationt zkopuluje přebytkem pasivní komponenty, například acetoacetanilidu při pH 8 až 9 na azosloučeninu a nezreagovaný přebytek pasivní komponenty se stanoví roztokem diazoniové soli aminolátky, přičemž se bod ekvivalence určí kapkovou zkouškou na výtok s pasivní komponentou, nebo potenciometričky na elektrodovém systému zlatá rotační elektroda - nasycená kalomelová elektroda. Zkoumaná diazoniová sloučenina je jednou z hlavních komponent diazoniových materiálů, citlivých na světlo a náchylných rozkladu.The subject of the invention is a method of determination 2,5-dialkoxy-4-morpholinylbenzene diazonium the compounds of which lies wherein the diazonium cation is determined copulates with excess passive component for example acetoacetanilide at pH 8 to 9 to an azo compound and an unreacted excess the passive components are determined by the solution the diazonium salt of the aminates, with the equivalence point is determined by a drop test a discharge with a passive component, or potentiometers on the electrode system gold rotating electrode - saturated calomel electrode. The diazonium compound under investigation is one from the main components of diazonium materials, sensitive to light and susceptible to degradation.
Description
Vynález řeší způsob stanovení 2,5-dialkoxy-4-morfolinylbenzendiazoniových sloučenin obecného vzorceThe present invention provides a method for the determination of 2,5-dialkoxy-4-morpholinylbenzenediazonium compounds of the general formula
CH,CH,
CH2' ch2 CH 2 'ch 2
RORO
OR kde R je alkyl s 1 až 5 atomy uhlíku.OR wherein R is alkyl of 1 to 5 carbon atoms.
Tyto látky jsou hlavní komponenty diazografických materiálů citlivých na světlo.These substances are the main components of light sensitive diazographic materials.
Výěe uvedené typy látek, které jsou náchylné k rozkladu jak pevné, tak ve vodném prostředí, zvláětě na světlo a v nepřítomnosti stabilizátorů jako kyselina citrónová, vinná aj.The above-mentioned types of substances which are susceptible to decomposition both in solid and aqueous environments, especially in light and in the absence of stabilizers such as citric, tartaric, etc.
V úvahu přicházející metody jako například polarografie, vystupuje diazoniovou sloučeninu během analýzy působení prostředí, kdy může pokračovat nedefinovaný stupeň rozkladu a za druhé je polarografie metoda relativní, vyžadující referentní standard, jehož příprava je z těchto typů látek prakticky nerealizovatelná.Considerable methods such as polarography, the diazonium compound exits during the environmental analysis, where an undefined degree of decomposition can continue, and secondly, the polarography is a relative method requiring a reference standard, the preparation of which is practically impracticable from these types of substances.
Nyní byl nalezen způsob stanovení 2,5-dialkoxy-4-morfolinylbenzendiazoniových sloučenin, který je předmětem tohoto vynálezu a jehož podstata spočívá v tom, že se stanovený kationt zkopuluje přebytkem pasivní komponenty, například acetoacetanilidu v alkalickém prostředí při pH 8 až 9 na azoaloučeninu a nezreagovaný přebytek pasivní komponenty ee stanoví roztokem diazoniové soli aminolátky například diaza-p-toluidinu, přičemž se bod ekvivalence určí kapkovou zkouškou na výtok s pasivní komponentou, nebo potenciometricky na elektrodovém systému zlatá rotační elektroda - nasycená kalomelová elektroda.We have now found a method for determining the 2,5-dialkoxy-4-morpholinylbenzenediazonium compounds of the present invention, which is characterized in that the determined cation is coupled with an excess of a passive component, e.g. the unreacted passive component ee is determined by a solution of the diazonium salt of an amino compound such as diaza-p-toluidine, wherein the equivalence point is determined by a drop test for passive component effluent or potentiometrically on the electrode system by a gold rotating electrode - saturated calomel electrode.
Pro toto navrhované stanovení nepřímou kopulační metodou lze jako pasivní komponenty použít acetoacetanilid, hydroxyfenalmočovinu, morfolinopropýlamid oxynaftoové kyseliny a podobně.Acetoacetanilide, hydroxyphenal urea, morpholinopropylamine oxynaphthoic acid and the like can be used as passive components for this proposed indirect coupling method.
Pro retitraci nadbytku pasivní komponenty lze použít odměrného roztoku diazoniové soli p-toluidinu, m-toluidinu, p-nitrosnilinu, m-nitroanilinu aj. Způsob indikace lze zvolit jednak vizuální na výtok s H kyselinou, jednak potenciometrický na elektrodovém systému zlatá rotační elektroda - nasycená kalomelová elektroda.For retitration of excess passive component, a volumetric solution of diazonium salt of p-toluidine, m-toluidine, p-nitrosniline, m-nitroaniline, etc. can be used. The indication method can be visualized for H acid effluent or potentiometric on electrode calomel electrode.
Příklad provedeniExecution example
Příprava zásobního roztoku diaza 2,5-dibutoxy-4-morfolinyl anilinu. Do 100ml odměrné baňky se přesně neváží cca 4 g vzorku, rozpustí v destilovaná vodě a doplní po značku.Preparation of a 2,5-dibutoxy-4-morpholinyl aniline diaza stock solution. Do not weigh approximately 4 g of the sample into a 100 ml graduated flask, dissolve in distilled water and make up to the mark.
Do 150ml kádinky se nalije 50 ml Britton-Robinsonova pufru £.JBEp) = 0,4 mol/1 o hodnotě 8,5 pH. Připipetuje se 20 ml roztoku acetoacetanilidu £ (AAA) = 0,1 mol/1. Za míchání ee připipetuje 20 ml zásobního roztoku diazolátky. Po cca 5minutovém míchání se pH roztoku upraví na hodnotu 9,5. Nezkopulovaný přebytek acetoacetanilidu se titruje roztokem di-aza-p-toluidinu £ (dpT) = 0,1 mol/1. Bod ekvivalence a nadbytek diaza-p-toluidinu se zjistí na filtračním papíru na výtok s H kyselinou. Výpočet obsahu diazolátky:50 ml of Britton-Robinson buffer (pH = 0.4 mol / l, pH 8.5) is poured into a 150 ml beaker. Pipette 20 ml acetoacetanilide solution (AAA) = 0.1 mol / l. While stirring, ee is pipetted with 20 mL of the diazo reagent stock solution. After stirring for about 5 minutes, the pH of the solution was adjusted to 9.5. The uncoupled excess of acetoacetanilide is titrated with di-aza-p-toluidine solution δ (dpT) = 0.1 mol / l. The equivalence point and excess diaza-p-toluidine are determined on H-acid filter paper. Calculation of diazolate content:
(20 - ad.fd) . 0,0431502 . 5 . 100 % hmot. = ——...............-..... 11 — — kde a^ je spotřeba odměrného roztoku diaza-p-toluidinu v ml je faktor odměrného roztoku diaza-p-toluidinu, n je navážka vzorku v gramech(20 - and d .f d ). 0,0431502. 5. 100% wt. = ——...............-..... 11 - - where a ^ is the consumption in ml of the volumetric solution of diaza-p-toluidine is the factor of the volumetric solution of diaza-p-toluidine , n is the sample weight in grams
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Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS84260A CS238795B1 (en) | 1984-01-12 | 1984-01-12 | Method of determining of 2,5-dialcoxy-4-morpholinylbendiazone compositions |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS84260A CS238795B1 (en) | 1984-01-12 | 1984-01-12 | Method of determining of 2,5-dialcoxy-4-morpholinylbendiazone compositions |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CS26084A1 CS26084A1 (en) | 1985-05-15 |
| CS238795B1 true CS238795B1 (en) | 1985-12-16 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS84260A CS238795B1 (en) | 1984-01-12 | 1984-01-12 | Method of determining of 2,5-dialcoxy-4-morpholinylbendiazone compositions |
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| Country | Link |
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| CS (1) | CS238795B1 (en) |
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1984
- 1984-01-12 CS CS84260A patent/CS238795B1/en unknown
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| Publication number | Publication date |
|---|---|
| CS26084A1 (en) | 1985-05-15 |
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