CS268572B1 - The method of analysis of the cationic components in the substrate and the preparation of the enrichment accelerator - Google Patents

Abstract

RieXenie aa refers to the use of the analysis of cationic components in materials from the preparation of rubber accelerators based on 2-mercaptobenzothiazole. The analyzed cationic components aa are separated in an isotaohophorothioke column at the intensity of the electric parade from 7 to 400 ΛίΑ. Vodiaoi electrolyte contains 0.001 to Ο.ΟΙί^βοΙ . 1 cation and einimite with the same mobility as the analyzed components and protons and a oxidizing acid property in the range of pH 2.0 to 10.5. The conducting electrolyte contains a cation with a maximum mobility equal to that of the analyzed components, or is neutralized by the counterion of the conducting electrolyte to a pH approximately equal to the pH of the conducting electrolyte. After the detection of the analyzed components in their zones, the measured signal of the detector or the lengths of the analyzed components is used to identify or determine the content of the components in the analyzed sample.

Description

The invention relates to a process for the analysis of cationic components in thermoforms from the preparation of rubber scavengers based on 2-mercaptobenzothional (nnpr, N-morpholinyl-2-benzothiazolesulfone, N-cyclohexyl-2-benzothiazolesulfenamide, 2-mercaptin benzothobenzothenzoate), o linseed, aniline, die ton o lamin, λ o thanks, calcium ap, isotaophoresis.

Rubber chemicals based on 2-metaptaptobenzothiazole have the first application in the rubber industry in the processing of rubber compounds of natural or synthetic rubbers used in the manufacture of tires, rubber wool, conveyor belts, wedge belts, cables, latex compounds, rubber bands. ea is also used in the pharmaceutical industry in the manufacture of ointments and has. also used as a chemical analytical reagent. The rubber chemical N-morpholinyl-2-benzothiazolylsulfenamide and N-cycchexyl-2-benzotiazolylsulfanilide is most often prepared by the oxidation-condensation reaction of 2-mercaptobenzotlazole and morpholine reap, cyclohexylamine using sodium peroxides or oxidizing reagents such as oxidizing reagents. The basic raw materials for the production of 2-mercaptobenzothiazole are aniline, carbon disulfide and sodium bromide. For the determination of morpholine, cyclohexylamine, aniline and most commonly, it uses azidobasic titration methods (Sippia, S,: Quantitative Orpanio Analysis, 3 θύ * New, York and London, John VILEY and Sons, 1963) Šafařík, L, - Stránský, Z ,: Odmčrná analysis in organic expanded tádlooh, Prague, SNTL 1982 / and possibly also used gas chromatography / Takaschi Hamuro, J, Chromatoí? Z, Anal, Chen ,, 3θ2 (ΐ9θθ) 203 /, Acid-base determination or photometric motors.

Torna ea found that the analysis of cationic components in materials from the preparation of rubber additives based on 2-roercaptobonzothiazole (in starting materials, intermediates and final products) such as morpholine, cyclooxylamine, butterfly morpholine, diethanolamine, aniline, calcium sodium and calcium. in their zones of conductivity, spectrophotometry, gradient-potonial, thermal, high-frequency-conductivity, pH or radar detector, can be carried out according to the process of the invention, which is based on novelty and differs from the methods hitherto used.

Summary of the invention lies in the fact that the analyzed sepaxáoia katloniokýoh components e and place on a column of izotachofore ticksJ the electric current of 7 to 00 ^ / u, e vodlaoim obeahujáoira electrolyte ion konoentráoli of 0.001 to 0.012 mol - dm ^J or at least as the eye pohyblivé®tou have analyzed the cationic components and the proton b of the buffer with an aidobasic property in the cloud at 2.1 to 10.5, e.g. -2-hydroxy®tylpiperazine-N-2-tansulfonic acid, arginine, valine,

The separation of the analytes is carried out with the electrolyte terminating the cation b by at most the same moving eye of the analytes cationic components, e.g. , which may have been neutralized by the lead electrolyte to a pH approximately equal to the pH of the water electrolyte and after detection! of the analyzed components in ioh zones from the measured signal by the detector or the lengths of the zones of the components are performed ioh Identification or determination of the content of the components in the analyzed component.

Under certain conditions of analysis, which the EU expressed the so-called operating system of analysis (composition and conoentréoia vodiaoohoho electrolyte, intensity of electric current, geometric

CS 268 572 B1 ^!

The rotor is used with an isothophorotar knee, etc., The size of the measured signal is detected. rom in the corresponding zones of the eparon substance constant & characteristic for a certain substance. Té i <> «J <t» t οΛϊιολΙ nn vynlíva hlnvno pri kvn11tnt {vneJ nnulýz · lAtok, kd · s suffice · moral wave height to 1 from taohof oroograrae _t regie trovaxiú eapleovaóon, and compared Ju with the wave height assumed by J 3 t ,

The length of the zone of the analyte is again the quantum of the quantity in the isotaohoforetlo analysis.

A supporting analysis atom which can and advantageously be used in the analysis of the subject cathlonic components of the stage of the invention is given in Table I.

The analysis of the subject catalyst components according to the invention has a number of advantages. It allows both quantitative eye and qualitative analysis of the subject cathlonic components in a mixture of one analyzed solution (solution of analyzed components in water, solution after extraction of components and organic solvent in water) without chemical derivatization of the analyzed components, .

Other advantages are selectivity, speed and simplicity,

Some of the components in the rubber materials, in the raw materials and in the intermediate products for the production of the non-ionic substance cannot interfere with the analysis of the ionic components in question, unlike, for example, gas or liquid chromatography, which can be used to analyze ion-free components. The charge of the components is known and, in the case of multiple occurrences of the components in the analyzed samples, undesired overlaps of the concentration elution bands of the two components may occur during their separation.

BACKGROUND OF THE INVENTION It is possible to perform an analysis of the subject cationic components after separation from undesired non-polar impurities. in the analyzed samples, which would number the isotaohoforetio columns, by simple extraction of the analyzed components 2 of the organic solvent into an acidified or alkaline aqueous solution, which at the same time increases the selectivity of the analysis,

Process according to the invention It is also possible to carry out the analysis of nonionic components such as N-cyclooxy-2-benzothiazolylsulfenamide, N-morpholinyl-2-benzothiazolylsulfonates, which are reduced with

Izotaohoforetioká analysis present the components may be conducted for 10 to 20 minutes using a capillary column j (length 15 ^om »internal diameter of 0.8 or 0.3 mm), appropriate selection of the intensity of electric current analysis time can be further shortened. Concentration range sufficient millet stanovonia question components is 0.0001 to 100 hmotnoatných, detection limit is very low, to full quantitative tinfoil qualitative analysis of ingredients just injoktoval to izotaohoforetlokej column molar amount of 1θθ to 1θ ^"11 3 moles of analyte in 1 nu» solution.

The above advantages, as well as the fact that the analysis method according to the invention allows simultaneous, fast, simple and difficult to quantitatively and qualitatively stonovenio all cationic components present in the sample, provides wide possibilities of its application in complex modular control of technological process 2-mercaptobenzotlazole base.

The following examples illustrate but do not limit the scope of the invention.

CS 268 572 B1

Example 1

Determination of morpholine and cycloherylamine in the mother liquor from the production of N-morpholinyl-2-borohydride.

00a to odmornej Brník 250 om ^J e and weighed AAL 0.5 The sample and the volume of the solution and on scoring with water, from the solution to the injoktovalo lzetachoferotiokeJ of Cologne ram ^ 5 and held. is isotachophoretic. The length of the zones of the individual components of the reap was read on the isotachophorogram, the concentration of the components in the analyzed solution was calculated and the content in the sample was calculated.

Calibration curves were plotted as the dependence of the measured zone length of a component on an isotachophorograft from its amount of material used for analysis, into an isotoohoforetio column and injected with 1.2 _f 3 _r U _t 5, a standard solution of components at a concentration of 0.01 mol, dm,

Calibration dependences in the form of linear equations were obtained by regression analysis,

Isotachophoretic analyzes were performed under the conditions of operating system No. 1,2, 3 »» 5t 7 »9» ¹⁰ > ¹¹ f ^{12 and} 13 avodenýoh in Table 1,

Example 2

Determination of morpholine, methylmorpholine, ethanolamine, diethanolamine, sodium and calcium in distillation residues from the production of N-morpholinyl-2-benzothiazole sulphonamide 3 3

Odxaarnoj to a 100-cm 5 charged with about 1 g of sample was added 25 e and ^J on hypochlorite and the dissolution of the sample was adjusted to volume Volume of chloroform, from the roz3 3 3 -3 flux was measured up to 25 cm per flask odmernoj 25Ο cm _° ⁵⁰⁰¹ was added θ »5 mol. dm ^J of the KOJI solution and the volume of the solution ea was adjusted to the mark with water. The contents were shaken for about 5 ", and the distribution of Inut vrstlev into izotaohoforetiokeJ injektovolo column 5 of the aqueous layer ^55, an evaluation of the place is the same as example the first

Isotachoferotic analysis was performed under operating conditions of operating conditions No. 5, 7 »and 8 listed in Table 1,

Example 3

Determination of © aniline in 2-mercaptobejisothiazole

About 1 g of the sample was weighed into a 100 .mu.m volumetric flask, 25 .mu.l of ethanol, 5 .mu.l of 0.1 mol .mu.l of HCl solution were added and the volume of the solution was adjusted to the mark with water. paper (red tape) and 25 solutions were injected from the filtrate into an isotachophoretic column,

Evaluation of the isotachoferotic analysis was performed as in Example 1,

Isotachophorotloc analysis of ea was performed under the conditions of operating system No. 8 listed in Table 1,

Example ¹ i

Determination of methylmorpholine and diethanolamine in teclmiocoa morpholine.

The preparation of the sample solution for the reaction analysis, the evaluation of the isothohoforetical analysis and the procedure carried out as in Example 1,

Isotaoferrophic analysis was performed under the conditions of the operating system δ, 7 and 8 given in Table 1,

CS 268 572 B1

Table 1, Some supported systems for ml of cationic components according to the invention

E Parameter Cí < ilo system 1 2 3 4 5 6 7 8 9 10 1 1 12 13 Water, ion H ⁺ H ⁺ H ⁺ K ⁺ K ⁺ Na ⁺ K * Na ⁺ K ⁺ K ⁺ K ⁺ K ⁺ Bo * 0 / mol, 1 ¹ / 0.01 0.01 0.005 0.001 Oh, O1 0.01 0.012 0.01 0.01 0.01 0.01 0.01 0.01 Proteon / - / Cl " KS AN KF KFUM KO KO KF KO MES MOPS HEPES ARG VAL pH 2.0 2.4 2.7 4.3 5.0 5.2 5.3 5.2 6.0 7, 1 8, 0 9.0 10.5 Finished Icy ion TRIS TBA BALA WHERE TRIS CLGL TBA h ₃ o ⁺ BALA TBA TRIS TRIS TRIS EU o / mol, 1 1 / 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.005 0.01 0.01 0.01 0.01 0.01 Proteon / - / KO KM KF KFUM KO KO KF KO Cl OH he " Cl Cl pH 5, ° 5.0 ^{í (} , 5 '•, 5 5.0 4.0 5.0 M 5.0 X M 8.5 8.5 I, // UA / 250 250 4 00 60 300 WHAT 250 250 200 200 150 150 150 Ι ₂ // ΟΛ / 50 50 60 7 40 10 50 40 45 45 50 30 30

E c electrolyte, VE b conducting electrolyte, UE e terminating electrolyte, Protion / - / s di a 00 i negated form of the component with negative charge, KS AN with acid, and uLf aniline, KF with acid, phthalic, KFUM π acid, fumaric , KO = kys. acetic acid, HES = acid, N-morpholinethanesulfonic acid, MOPS b acid. 3- (N-morpholino) prepanesulfane, HEPES, N-2-hydroxyethylpiperazine-N-2-ethanesulfonic acid, TRIS and triahydroxymethylaminomethane, TBA, tetrabutylamine, DALA = beta-alanine, KAM c acid, aminobutyrs, GLGLo-glyoyl, ARG = arginine, VAL · s valine, Ip = electric current intensity in an isotoohoforothioco column with an internal diameter of 0,8 reap. 0.3 mm, and the pH of the solution is not checked.

Claims (1)

CS 268 572 B1 Table 1 Some of the cationic enzyme compositions of the present invention E Parameter number of the cyanide 1 2 3 5 6 7 8 9 10 1 1 12 13 Water, ion H + U + H + K + K * Na + K * Na + K + K + K + K + Bo * 0 / mol, 1 1 / 0.01 0.01 0.005 0.001 0.01 0.01 0.012 0.01 0.01 0.01 0.01 0.01 0.01 Protion / - / Cl "KSAN KF KFUH KO KO KF KO MES MOPS HEPES ARG VAL · pH 2.0 2.4 2.7 Ί.3 5.0 5.2 5.3 5.2 6.0 7, 1 8, 0 9.0 10.5 Ukonéu-Júci ion TRIS TRA BALA WHERE TO GLGL TBA u3o + BAIA TBA TOIS TOIS TOIS UE o / mol, 1 / 0.01 0.01 0.01 0 , 01 0,01 0,01 0,01 0,005 0,01 0,01 0,01 0,01 0,01 Protion / - / KO KM KFUM KO KO KF KO Cl "ou" OH "Cl" Cl "saw 5.0 5.0 '», 5'», 5 5.0 I |, 0 5.0 and 5.0 XX 0.5 8.5 I, // «A / 250 250 4 00 60 300 150 250 250 200 200 150 150 150 I2 // U'V '50 50 60 7 áo 10 50 áo ^ 5> t5 50 30 30 E c electrolyte, VE for electrolyte, UE c terminate electrolyte, Protion / - / 2 disooi negative charge, KSAN with acid, and ul-f aniline, KF with acid , phthalic, KFUM e acids, fumarate, KO 2 kye * acetic, MES = acid, N-morpholinetane sulfonic, MOPS and kye, 3- / N-morpholino / propane-aulionic, HEPES N-2-hydroxyl tylpiperazine N-2-ethanesulfonic, TRIS 2 triahydroxyme thylamine o methane, TBA 2 tetrabutylxunonium, DALA 2 beta-alanine, KAM c kye, U - aminomael, GLGL 2 glyoylglyoine, ARG = argin.in, VAL 2 valine, /, = the intensity of the electric current in the isotophorothiotic column having an internal diameter of 0.8 rosp, 0.3 mm, x and the pH of the solution aa does not control. DISCLOSURE OF THE INVENTION Spoeob analysis of cationic constituents in a material from the preparation of gum enriched urea compounds on a base of 2-mercaptobenzothiazole, e.g. trio, tri-titanium, gradient, thermo-thermal, electrophoretic-conductive, pU or radiation detector, characterized in that the analyzed cationic constituents and at the end of the isotophoretic column at an electrical current intensity of 7 to 100 [mu] A, and the lead olocolytes containing the cation of 0.001 to 0.012 mol, 1 1 1 and at least the same movable eye are analyzed by the components and protions and the buffer oxidobase in the pII2.1 and ,510.5 regions, e.g. , a solution of potassium hydroxide, sodium, barium in a mixture and fumarate, oot, violet, otorpholine tansulfene, morpholinopropane sulfonic acid, N-2 'hydroxyethylpiperazine-N-2-tansulfonic acid, argiuine, valine, and olefin terminating oleate and maximally equilibrium eye cationic components analyzed, for example, a solution of oothoic acid, a solution of trishydroxymethylaminoethane, tetrabutylammonium hydroxide, beta-alanine, 4-amino-naphthalic acid, glyoylglyoine, which is optionally neutralized with counter electrolytic counterions to pH equal to that of the water electrolyte, and after detection of the analyzed smears in ioh from the measured signal of the detector or the length of the zones of the component and performing the identification or treatment of the components in the analyzed component.