CS204426B1 - Method of determination of the metakrylamide,metakrylamide acid alfa-hydroxyizobutter in the metakrylamidsulphate - Google Patents
Method of determination of the metakrylamide,metakrylamide acid alfa-hydroxyizobutter in the metakrylamidsulphate Download PDFInfo
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Abstract
Predmetom vynálezu je efektivna analytická metoda, ktorá umožňuje pri dodrženi štandardnýoh pracovnýoh podmienok relativné rýohle a přesné stanovenie metakrylamidu aj viazaného vo formě solí a dalších prchavých komponentov, za přítomnosti koncentrovanéj lsyseliny sírovéj. Podstata vynálezu spočívá v tom, že vzorky reakčných zmesi sa upravujú vodným roztokom štavelanu draselného pre stanovenie lcyseliny metaJcrylovej a vodným roztokom octanu draselného pre stanovenie dalších prchavých komponentov, Sálej sa přidá dioxán v množstve, ktoré zabezpečí oddelenie organickej vrstvy od anorganickéj a organioká vrstva sa analyzuje plynovou ohromatografiou.The object of the invention is to be effective analytical method that allows for compliance standard working conditions the relative abundance and precise determination of methacrylamide and bound in the form of salts and other volatile components, in the presence concentrated sulfuric acid. The essence of the invention is that samples of the reaction mixtures are treated with aqueous potassium oxalate solution for. \ t determination of methacrylic acid and aqueous potassium acetate solution for determination other volatile components, Saly add dioxane in an amount to ensure separating the organic layer from the inorganic and organic layers are analyzed gas chromatography.
Description
Predmetom vynálezu je efektívna analytická metoda, ktorá umožňuje pri dodržaní štandardných praoovných podmienok relativné rýchle a přesné stanovenie metakrylamidu aj viazaného vo formě soli a dalších prchavých komponentov, za přítomnosti koncentrované j kyseliny sirovej.It is an object of the present invention to provide an efficient analytical method which, subject to standard operating conditions, allows a relatively rapid and accurate determination of both salt-bound methacrylamide and other volatile components in the presence of concentrated sulfuric acid.
Precizně sledovanie jednotlivých medziproduktov pri syntéze inetylmetakrylátu z acetonkyanhydřinu a pósobeníin kyseliny sirovej cez metakrylamidsulfát a jeho esterifiIcáciu vodným metanolom naráža na niekolko ťažkosti. iíeakčná zmes amidácie a esterifikácie obsahuje 20 až 40 ’β kyseliny sirovej a metakrylam.id je viazaný vo formě síranu, ktorý sa móže z roztoku vylučovat’. Z hladiska riadenia reakcie je dóležité reakciu sledovat’ už v 1. stupni (amidácia), ako aj v 2. stupni při esterifikácii. Pre analytiku týchto procesov sa používá metoda bromid-broiničnanová [j)SN 66 1975{ Takenchi T., J. Chem. Soc.,Precisely following the individual intermediates in the synthesis of ethyl methacrylate from acetone cyanohydrin and sulfonic acid via methacrylamide sulphate and its esterification with aqueous methanol encounters several difficulties. The reaction mixture of amidation and esterification comprises 20 to 40 ’of ovej sulfuric acid and methacrylamide. The bound is in the form of sulphate which can be separated from the solution. From the viewpoint of reaction control, it is important to monitor the reaction both in the 1st stage (amidation) and in the 2nd stage in the esterification. The bromide-broinate method [j) SN 66 1975 {Takenchi T., J. Chem. Soc.
Jap. Ind. Chem. Sec. 6^, 539 (196«í)J.Jap. Ind. Chem. Sec. 6, 539 (196), J.
Metoda stanovenia dvojných vaziob je použitelná len v prvých štádiách reakcie.The double bond method is applicable only in the first stages of the reaction.
Při esterifikácii je přítomný metylmetakrylát, kyselina inetakrylová a oligoméry týchto látok. Vhodnejšia je metoda, ktorá využívá princip hydrolýzy metakrylamidu a vydestilovanie čpavku, ktorý sa v ďalsom postupe stanoví pfakenchi Ts. , J. Chem. Soc. Jap., Ind. Chem. Sec. 60, 1448 (1957)J· Aj druhá metoda je poměrně zložitá, pracná a nie za každých okolností přesná.Methyl methacrylate, inetacrylic acid and oligomers thereof are present during esterification. A method which uses the principle of methacrylamide hydrolysis and distillation of ammonia, which is determined in the next process by pfakenchi Ts, is preferable. J. Chem. Soc. Jap., Ind. Chem. Sec. 60, 1448 (1957) J The second method is also quite complex, laborious and not accurate at all times.
Pri sledovaní postupu esterifikácie je potřebné sledovat’ konverziu metanolu a výťažok metylmetakrylátu. Pro stanovenie čistoty metylmetakrylátu existuje viac práč s postupní i polarografickými JjPasciak J., Chem. Anal. (Varšava) 6, 411 (1 961)J, plynovou ohromatografiou pKosek Li., Chem. prám. 15 . 16Ο (1963)J, stanovenie dvojných vázieb [Ťurusawa M., J. Chem. Soc. Jap., Ind. Chem. Sec. ňý , 539 (19Ó2)J, kolorimetricky j^Poležajev W. G. , Iíuznecova L. V., Anal. Abstr. 12, 4973 (19Ó6)J a IČ spektrami jLlnon., Anal, Chem. 30, 1441 (1958)J. Vo všetkých případech sa tu přesné výsledky dosiahnu hlavně po vydělení - izolácii metylmetakrylátu, ked už v reakčnotn prostředí nie je přítomná kyselina sírová, alebo síran.In monitoring the esterification process, it is necessary to monitor methanol conversion and methyl methacrylate yield. For the determination of the purity of methyl methacrylate, there is more work with both sequential and polarographic Jj Pasciak J., Chem. Anal. (Warsaw) 6, 411 (1961) J, by gas chromatography pKosek Li., Chem. raft. 15 Dec 16Ο (1963) J, determination of double bonds [[urusawa M., J. Chem. Soc. Jap., Ind. Chem. Sec. 53, 539 (19), colorimetrically. Poljayev W.G., Iuznecova L.V., Anal. Abstr. 12, 4973 (1966) and IR spectra, Inc., Anal, Chem. 30, 1441 (1958). In all cases, accurate results are obtained here mainly after separation - isolation of methyl methacrylate, when sulfuric acid or sulphate is no longer present in the reaction medium.
Podl’a tohto vynálezu sa spósob stanovenia metakrylamidu, kyseliny metakrylovej, amidu kyseliny «/ý-hydroxyizomaslovej v metakrylamidsulfáte a v zmesiach esterifikácie metakrylamidsulfátu pri výrobě metylmetakrylátu z acetonkyanhydrinu, kyseliny sirovej a metanolu metodou plynovéj ohromatografie uskutočňuje tak, že vzorky reakčných zmesi sa upravujá vodným roztokom šťavelanu draselného o koncentraci! 10 až 30 hm., v množstvo najmenej molámom vzhladom na přítomná volná a viazaná kyselinu sírová, pre stanovenie kyseliny metakrylovej a vodným roztokom octanu draselného o koncentraci! 23 až 70 hmotn. pre stanovenie ostatných uvedených zložiek, dalej sa přidá dioxán v množstva, ktoré zabezpečí oddelenie organickéj vrstvy od anorganickéj a organická vrstva sa analyzuje plynovou ohromatografiou.According to the present invention, a method for determining methacrylamide, methacrylic acid, N-hydroxyisobutyric acid amide in methacrylamide sulfate and esterification mixtures of methacrylamide sulfate in the production of methyl methacrylate from acetone cyanohydrin, sulfuric acid and methanol is carried out Potassium oxalate concentration! 10 to 30 wt.%, In an amount of at least molar relative to the free and bound sulfuric acid present, for the determination of methacrylic acid and an aqueous solution of potassium acetate at a concentration of 10 to 30 wt. 23 to 70 wt. To determine the other components listed above, dioxane is added in an amount to separate the organic layer from the inorganic layer and the organic layer is analyzed by gas chromatography.
Uvedený postup je relativné rýohly, pričom umožňuje v konečnej fáze použitie moderných a rýohlyoh metod pre stanovenie látok důležitých z hladiska vyhodnotenia priebehuThis procedure is relative to the soil and allows, in the final phase, the use of modern and soil-based methods for the determination of substances important for the evaluation of the
204 420 reakcie, a to na zariadení, ktoré sa bežne používá pri kvantitativných a kvalitatívnyoh analytiokýoh metódaoh prohavých látok. Efektivně rieši oddelenie minerálnych látok od organických zložiek, pričom metoda je z hladiska pracnosti a požiadaviek na pomooné látky velmi nenáročná.204 420 on a device that is commonly used in quantitative and qualitative analytical methods. It effectively solves the separation of minerals from organic constituents, while the method is very unpretentious in terms of laboriousness and requirements for the auxiliary substances.
Podlá popísanej ohromatografickeJ metody je možné stanovit’ vo vzorkáoh z reakčnej zmesi z amidáoie metakrylamid, z esterifikáoie metakrylamidu, kyseliny metakrylovej, metanol, amid kyseliny <£-hydroxyizomaslovej a pri úpravě režimu tiež metylmetakrylát. Stanovenie je rýchle, spolehlivé, operativně a je vhodné pre aplikáoiu na prevádzkovú kontrolu.According to the described chromatographic method, samples from the reaction mixture of amide methacrylamide, esterification of methacrylamide, methacrylic acid, methanol, β-hydroxyisobutyric acid amide and methyl methacrylate can be determined in the sample. The assay is fast, reliable, operative and suitable for field inspection applications.
Podstata stanovenia spočívá v úpravo vzorky, napr. reakčnej zmesi. Metakrylamid sa uvolňuje zo sulfátu, anorganické zložky sa vyzrážajú za přítomnosti vhodného rozpúšťadla a do prístroja sa dávkuje výlučné zmes organickýoh látok. Pre stanovenie metakrylamidu, metanolu a metylmetakrylátu sa ako činidlo používajú alkalické soli mono- alebo dikarboxylových kyselin v nadbytku na prítomnú kyselinu sírovú volnú a v metakrylamidsulfáte. Chemizmus dejov prebiehajúoich po přidaní alkaliokej soli možno popisať následovně:The essence of the assay consists in treating the sample, e.g. of the reaction mixture. The methacrylamide is released from the sulfate, the inorganic components are precipitated in the presence of a suitable solvent, and an exclusive mixture of organic substances is metered into the apparatus. For the determination of methacrylamide, methanol and methyl methacrylate, alkali salts of mono- or dicarboxylic acids in excess of the free sulfuric acid present and in methacrylamide sulphate are used as reagents. The chemistry of the events taking place after the addition of the alkali metal salt can be described as follows:
ZFROM
CIí2 a C - CO - NH2 «HgSO^ + 2 RCOOMe -> CH2 a C - C^ +2 RCOOH + Me^O^ ch3 ca3 nh2 Cl 2 and C - CO - NH 2 · H 2 SO 4 + 2 RCOOMe -> CH 2 and C - C 2 +2 RCOOH + Me ^ O ^ ch 3 ca 3 nh 2
HgSO^ + 2 RCOOMe -> MOgSO^ + 2 RCOOH, kde Me představuje alkalioký kov alebo amóniový ion. Po proběhnuti reakoie sa vzorok riedi dioxánom, na zvolenú strednú konoentráciu metakrylamidu (metanol, metyImetakrylát) vzhladom na závislost’ konoentráoie - odozva detektoru. Anorganické soli vzniknuté úpravou vzorku sa prakticky usadia na dne nádobky a vzorkuje sa organická vrstva.HgSO4 + 2 RCOOMe → MOgSO4 + 2 RCOOH, wherein Me represents an alkali metal or ammonium ion. After the reaction has taken place, the sample is diluted with dioxane, to the chosen mean concentration of methacrylamide (methanol, methyl methacrylate), depending on the dependence of the conoentration - detector response. The inorganic salts formed by the treatment of the sample are practically deposited at the bottom of the vessel and the organic layer is sampled.
V případe stanovenia kyseliny metakry1ověj je výhodné použit' pre úpravu vzorky alkaliokú sol kyseliny s vyšSou hodnotou pKa (napr. šťavelan draselný), nakolko pri použití kyseliny s nižšou hodnotou pKa dochádza k ustáleniu rovnováhy:In the case of methacrylic acid determination, it is preferable to use an alkali metal salt of an acid with a higher pKa (e.g. potassium oxalate) for treatment of the sample, since the use of an acid with a lower pKa results in equilibrium:
R - COOIC + CH„ = C - COOH > R COOH + CHO = C - COOKR - COOIC-CH "= C - COOH> R CH COOH + O = C - COOK
I | ch3 ch3 a výsledky sú nereprodukovatelné. Prehlad hodndt pKa u niektorýoh kyselin udává tabulka:I | ch 3 ch 3 and the results are not reproducible. An overview of the pKa values for some acids is given in the table:
204 428204 428
Postup pri stanovení metakrylamidu a kyseliny metakrylovej v reakčnej zmesi je obvykle nasledujáci:The procedure for determining methacrylamide and methacrylic acid in the reaction mixture is usually as follows:
K navážke 0,4 až 0,5 g sa přidá 1 ml destilovanej vody a 1 ml činidla (200 g oetan draselný alebo primeranó množstvo soli silnejšej kyseliny v 100 ml vody) a riedi sa dioxánom podl’a vopred zvolených štandardných podmienok, vzhladom na linearitu detektoru x.G pre stanovovaná látku. Obsah metakrylamidu sa vypočítá: % metakrylamidu = -....... -g g = navážka vzorky povodněj výrobyTo the 0,4-0,5 g portion, add 1 ml of distilled water and 1 ml of reagent (200 g of potassium oethane or an equivalent amount of stronger acid salt in 100 ml of water) and dilute with dioxane according to pre-selected standard conditions, the linearity of the xG detector for the analyte. The methacrylamide content shall be calculated:% methacrylamide = -....... -g g = sample of flood production
G = hmotnost’ upravenoj vzorky (po přidaní všetkých komponent) x = $i> hmot. metakrylamidu získaného analýzou upraveného vzorku.G = sample weight (after all components have been added) x = $ i> mass methacrylamide obtained by analysis of the treated sample.
Pod pojmom čtandardné podmienky sa pri postupe podlá vynálezu berá predovšetkým teplota, množstvo odoberanej p&vodnej vzorky, přidávané množstvo roztoku solí organických kyselin, množstvo dioxánu, doba pósobenia alkalickéj soli, doba rozdelovania fáz, množstvo odoberanej vzorky pre plynová ohromatografiu a podobné. Pri stanovovaní raetakryl amidu v réznyoh produktooh sa niňžu Standardně podmienky navzájom odlišovat', a to buď sčasti alebo úplné.The standard conditions in the process according to the invention are in particular temperature, the amount of the original sample taken, the amount of the organic acid salt solution added, the amount of dioxane, the duration of the alkaline salt exposure, the phase separation time, the sample amount for gas chromatography. In the determination of racetacryl amide in various products, the standard conditions will differ from each other, either in part or in full.
Podmienky pre plynová ohromatografiu sá následovně: detektor PID teplota kolony l6o °C teplota dávkovača 200 °C dlžka kolony 1,2 m priemer kolony 3 mni náplň kolony 5 $ hmot. PBGA na CHEZASORBB o zrnění 0,1 až 0,5 mm. Prietok nosného plynu (Ng) 30 ml/min ,prietok vodílca 30 ml Il^/min, prietok vzduchu 0,6 l/min, citlivost’ : 1 000 (použitý přistroj Chrom 4l).The conditions for gas chromatography are as follows: PID detector Column temperature 16 ° C Dispenser temperature 200 ° C Column length 1.2 m Column diameter 3 m Column charge 5 $ wt. PBGA on CHEZASORBB with a grain size of 0.1 to 0.5 mm. Carrier gas flow (Ng) 30 ml / min, conductor flow 30 ml / min, air flow 0.6 l / min, sensitivity: 1000 (used 4l instrument).
Blučné Časy (min) 1-dioxán + kyselina octová - prvá fázaBluetong times (min) 1-dioxane + acetic acid - first phase
2- kyselina metakrylová (i min 30 s)2-methacrylic acid (i min 30 s)
3- raetakrylamid (4 min 30 s)3-methacrylamide (4 min 30 sec)
4- amid kyseliny ,£-hydroxyizomaslovej (10 min 6 s).4-hydroxy-butyric acid 4-amide (10 min 6 sec).
Relativná chyba opakovatelnosti a směrodatná odchylka <r = ± 0,58 =1,89% relat.Relative repeatability error and standard deviation <r = ± 0.58 = 1.89% relative.
Pri stanovení kyseliny metakrylovej sa k navážke 0,4 až 0,5 g přidá 1,5 ml roztoku oxalátu draselného a dioxán pre vyzrážanie solí. Postupuje sa podobné ako pri stanovení metakrylamidu, včítane výpočtu. Podl’a obsahu kyseliny metakrylovej sa citlivost’ reguluje v rozpatí 1 : 500 až 1 : 1 000.For the methacrylic acid determination, add 1.5 ml of potassium oxalate solution and dioxane for the precipitation of salts to the weight of 0,4 to 0,5 g. The procedure is similar to that for methacrylamide, including calculation. Depending on the methacrylic acid content, the sensitivity is regulated between 1: 500 and 1: 1000.
Směrodatná odchýlit a a relativná chyba opakovatelnosti sá (Τ' = - 0,47, °^= 3,02 7» relatStandard deviation a and relative repeatability error s (Τ '= - 0,47, ° ^ = 3,02 7 »relat
Pri stanovení metanolu v reakčnej zmesi esterifikácie sa postupuje podobné ako v případe metakrylamidu, včítane výpočtu. Směrodatná odchylka a relativná chyba opakovatelnosti v případe metanolu je i 0,26, cT= 3,78 % relat. Použité podmienky: PIU,The determination of methanol in the esterification reaction mixture is similar to that of methacrylamide, including calculation. The standard deviation and the relative repeatability error in the case of methanol are also 0.26, cT = 3.78% relative. Conditions used: PIU,
204 428 dlžka kolony 1,2 m, prlemer kolony 4 mm, náplň 15 λ hmot. Z3.S -oxydiproploultril na Chro matone N-AN, zmenie 0,12 až 0,16 mra. Teplota kolony 70 °C, teplota dávkováča 130 °C, prietok nosného plynu 120 ml/mln, prietok - 0,038 MPa, prietok vzduchu - 0,111 MPa, oltllvosť 1,10^0. Elušnó Sasy: metanol - 2 min, metylmetakrylét - 3 min 48 s, dioxán (rozp.) - 9 min 18 s, posun papieru 6 mm/min.204 428 column length 1.2 m, column diameter 4 mm, packing 15 λ wt. Z 3 S -oxydiproploultil on Chro matone N-AN, changes 0.12 to 0.16 mra. Column temperature 70 ° C, batch temperature 130 ° C, carrier gas flow 120 ml / mln, flow rate - 0.038 MPa, air flow rate - 0.111 MPa, flow rate 1.10. Elušnó Sases: methanol - 2 min, methyl methacrylate - 3 min 48 s, dioxane (sol) - 9 min 18 s, paper feed 6 mm / min.
Vo všetkýoh prípadooh sa praoovalo metodou priamej kalibrácie.In all cases, direct calibration was performed.
Za podmienok použitých pro stanovenie metanolu, možno stanovit’ aj metylmetakrylét, ktorý sa stanoví s istým obmedzenim, nakolko sa tento mfiže separovat’. Směrodatná odehýlka a relativná chyba opakovatelnosti pre metylmetakrylét je (j= 0,058 a Λ 2,22 'β relot. V případe, že esterlfikéoia prebieha za přítomnosti rozpúšťadla v dvoch fázach je možné stanovovat’ metylmetakrylét v éasovom priebehu reakcie v jednotlivých fázach.Under the conditions used for the determination of methanol, methyl methacrylate may also be determined, which shall be determined subject to a certain limit to the extent to which it may be separated. The standard deviation and the relative repeatability error for methyl methacrylate is (j = 0.058 and Λ 2.22 relot. In the case where the ester is carried out in the presence of a solvent in two phases it is possible to determine methyl methacrylate over time in the individual phases.
Tento spfisob stanovenia metakrylamidu, kyseliny metakrylovej, metanolu alebo aj raetylmetakrylátu v reakšnýoh zmesiaoh pri syntéz© metylmetakrylátu z acetónkyarihydrínu má podl’a tohto vynálezu niekolko předností:This method of determining methacrylamide, methacrylic acid, methanol or even methyl methacrylate in a reaction mixture for the synthesis of methyl methacrylate from acetone cyanohydrin has several advantages according to the invention:
a/ umožňuje bilancovat’ reakšný proces v jednotlivých reakšnýoh stupňoch a sledovat’ kineticky jednotlivé medzistupne (amidáoia, esterlfikéoia), b/ vzhladom na klasické metody je metoda plynovej chromatografie operativnějala, rýchlejšia a spolehlivé jSia.a) it allows to balance the reaction process in individual reaction stages and to monitor the individual intermediate stages (amide, ester, b), b) with respect to classical methods, the gas chromatography method is more operative, faster and more reliable.
Aplikáoiu metody popisujú nasledujúoe příklady.The following examples describe the application of the method.
Příklad 1Example 1
Amidáoia aoetónkyanhydrínu sa uskutočňuje bežne používaným postupom. Pri 80 °C sa zmieša 60 g aoetónkyanbydrínu (94,95 $) , 103 β kyseliny sírovej (99,8 % hmot.), 0,16 g hydrochinonu. Teplota sa zvýši na 90 °C a odoberú sa příslušné vzorky:The amidation of the oetone cyanohydrin is carried out by a conventional method. At 80 ° C, 60 g of α-oetone cyanbydrin ($ 94.95), 103 β of sulfuric acid (99.8% by weight), 0.16 g of hydroquinone are mixed. The temperature is raised to 90 ° C and appropriate samples are taken:
V tomto případe sa reakcia uskutošnila pri nízkéj teplote, kde ešte neprebiehajú vo zvýšenej miere vedlajšle reakcie, všítane polymerizašnýoh.In this case, the reaction was carried out at a low temperature, where the side reactions, including the polymerization, still do not take place to an increased extent.
Příklad 2Example 2
Pre amidáoiu sa použije násada ako v příklade 1 a tým, že teplota amidáoie bude 150 °C. Po 3 hodináoh reakoie sa stanoví obsah metakrylamidu ohromatografloky 5,2 % hmot. Obsah dvojitýoh v&zieb bromid - bromišnanovou metodou podlá ČSN 66 1975 17,8 ?á hmot.For the amidation, the batch was used as in Example 1 and the temperature of the amidation was 150 ° C. After a reaction time of 3 hours, the methacrylamide content was determined in 5.2% by weight of the chromatograph. Content of double bonds by bromide - bromo-hypochlorite method according to ČSN 66 1975 17.8 wt.
204 428 (35,05 S Br/100 e)· Je zřejmé, že sa bróm vlaže na dvojité vazby večďajáíoh produktov (oligoméry), a preto této metoda nie je vhodná pre přesné stanovenie obsahu metakrylamidu.204 428 (35,05 S Br / 100 e) · It is obvious that bromine is wavering to double bonds of several products (oligomers) and therefore this method is not suitable for the accurate determination of methacrylamide content.
Přiklad 3Example 3
Esterifikácia metakrylamidsulfátu sa uslcutočňuje vodným metanolom za použitia 232 g metakrylamidsulfátu (i mól), 72 g vody (Ji moly), 53 g metanolu (1,6 molu), 1 g hydroohinónu. Teplota 90 °C, doba 150 min. Po 150 min reakcie sa stanovilo 2,9 $> hmot. nezreagovaného metakrylamidsulfátu. Výťažok metylmetakrylátu podl’a chroraatografiokej metody bol 78 % hmot., podl’a metody stanovenia dvojitých vázieb 83 % hmot. Z výsledku získaného pri esterifikácii vidno, že použitím klasickéj metody dochádza k nadhodnoteniu výsledkov dosahovaných pri esterif ikácii, v důsledku viazania brómu na různé vedTajšie produkty.The esterification of methacrylamide sulfate is carried out with aqueous methanol using 232 g of methacrylamide sulfate (1 mole), 72 g of water (1 mole), 53 g of methanol (1.6 mole), 1 g of hydroquinone. Temperature 90 ° C, time 150 min. After a reaction time of 150 min, 2.9% by weight was determined. unreacted methacrylamide sulfate. The methyl methacrylate yield according to the chromatographic method was 78% by weight, and according to the double bond method 83% by weight. From the result obtained in the esterification, it can be seen that the classical method results in an overestimation of the results obtained in the esterification due to the binding of bromine to various by-products.
Přiklad 4Example 4
Zmiešaním známého množstva metakrylamidu a amidu kyseliny jC-hydroxyizomaslovej a kyseliny sírovej sa připraví zmes, v ktorej sa stanoví obsah amidov podl’a vypracovaného postupu analýzy.By mixing a known amount of methacrylamide and β-hydroxyisobutyric acid amide and sulfuric acid, a mixture is prepared in which the amide content is determined according to the analysis procedure developed.
Stanovená zložka metakrylamid amid kyseliny Jj-iiydroxyizomaslovej teoret. obsah hmot.Determined component methacrylamide amide of β-hydroxyisobutyric acid theoret. weight content
29,029.0
3,5 stanov, obsah ýo hmot. 28,83.5 statutes, content ýo mass. 28.8
3,33.3
Takto bolo možné stanovit’ touto metodou vedl’a seba za přítomnosti kyseliny sírovej metakrylamid a amid kyseliny X -hydroxyizomaslovej.Thus it was possible to determine methacrylamide and X-hydroxyisobutyric acid amide by this method side by side in the presence of sulfuric acid.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS844378A CS204426B1 (en) | 1978-12-18 | 1978-12-18 | Method of determination of the metakrylamide,metakrylamide acid alfa-hydroxyizobutter in the metakrylamidsulphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS844378A CS204426B1 (en) | 1978-12-18 | 1978-12-18 | Method of determination of the metakrylamide,metakrylamide acid alfa-hydroxyizobutter in the metakrylamidsulphate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CS204426B1 true CS204426B1 (en) | 1981-04-30 |
Family
ID=5434938
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS844378A CS204426B1 (en) | 1978-12-18 | 1978-12-18 | Method of determination of the metakrylamide,metakrylamide acid alfa-hydroxyizobutter in the metakrylamidsulphate |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS204426B1 (en) |
-
1978
- 1978-12-18 CS CS844378A patent/CS204426B1/en unknown
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