CS240359B1 - A method for determining carbon disulphide - Google Patents

A method for determining carbon disulphide Download PDF

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CS240359B1
CS240359B1 CS823609A CS360982A CS240359B1 CS 240359 B1 CS240359 B1 CS 240359B1 CS 823609 A CS823609 A CS 823609A CS 360982 A CS360982 A CS 360982A CS 240359 B1 CS240359 B1 CS 240359B1
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determination
carbon disulfide
carbon
carbon disulphide
dialkylamine
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CS823609A
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Slovak (sk)
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CS360982A1 (en
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Peter Hauskrecht
Jozef Bocko
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Peter Hauskrecht
Jozef Bocko
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Publication of CS240359B1 publication Critical patent/CS240359B1/en

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Abstract

Vynález rieši stanovenie sírouhlíka merkurimetrickou titráciou. Sírouhlík zreaguje s dialkylamínom na diálkylamínovú sol' dialkylditiokarmamínovej kyseliny, ktorá sa ztitruje odmerným roztokom octanu ortuťnatého na indikátor difenylkarbazid alebo difenylkarbazon do intenzívneho fialovomodrého sfarbenia. • Vynález nájde uplatnenie při stanovení sírouhlíka v ovzduší, vo vodách i v tuhých látkách.The invention solves the determination of carbon disulfide by mercurimetric titration. Carbon disulfide reacts with dialkylamine to form the dialkylamine salt of dialkyldithiocarbamic acid, which is titrated with a volumetric solution of mercuric acetate against the indicator diphenylcarbazide or diphenylcarbazone to an intense violet-blue color. • The invention finds application in the determination of carbon disulfide in air, water and solids.

Description

240 3240 3

Vynález sa týká stanoy^jig fír^h^kg np;chádzajúceho sa v plynněj, ^yapglng] | ty„-he] fáze.The present invention relates to a tentoylig yfluconil in the gas stream. those "-he] phases.

Bežne je známých vjacero metód pre sta-,novenle sírouhlíka. V záýíjgpýph ipetódáchstanovenia a kontroly emisií látok zňe8i§ťu-júcich ovzdušie, MLVH CSR a ŠSŘ, Praha(1978) sp popísané stanovenia, sírouhlíkaabsorpciou v roztoku dimetylamínu pódiarovnice (I)Normally, many methods for carbonated carbon black are known. In the case of the method of determination and control of airborne emissions, MLVH CSR and ŠSŘ, Prague (1978), the determination of sulfur dioxide and absorption in a solution of dimethylamine (I)

(CHsCHžjzNH + CS2 - (CH3CH2)2NCS2H (I)(CH3CH2j2NH + CS2 - (CH3CH2) 2NCS2H (I)

Kyseliha dietylditiokarbaminová sa stano-vuje potenciometrickou titráciou odmernýmroztokom dusičnanu sťrieborného vo vodno-alkoholickoum prostředí. Ďalěj sa tu popi-suje absorpcia sírouhlíka zo vzduchu v alko-holickom roztoku hydroxidu draselného po-dlá rovnice (2). Vzniknutý etylxantogenátdraselný sa stanoví odmerným roztokom jó-du na škrob. CO2H5/ ’Diethyldithiocarbamic acid is determined by potentiometric titration with a volumetric nitrate solution in a water-alcoholic medium. Hereinafter, the absorption of carbon disulphide from air in an alcoholic potassium hydroxide solution according to equation (2) is described. The resulting ethyl xanthate potassium is determined by volumetric solution of starch. CO2H5 / ’

C2H5OH + CS2 + KOH -> S=C + H2O \C2H5OH + CS2 + KOH -> S = C + H2O \ t

SKSK

(HJ V Μ. V. Alexejeva a kol. Stanovení škodli-vých látek ve vzduchu výrobních místností,SNTL Praha (1953) je popísané stanoveniesírouhlíka podlá rovnice (I), (III, IV) (C2H5)2NCS2H + NH(C2H5)2-> - (C2H5)2NCS2H . NH(C2H5)2 (ΠΙ) 2 (C2H5)2NCS2H.'NH(C2H5)2 + + C.u(CH5COO),2-[(C2H5)2NCS2jCu + + 2 CHsCOOH + 2 NH(C2’H5)2 - (IV)(HJ V V. V. Alexejeva et al. Determination of harmful substances in the air of production rooms, SNTL Prague (1953) describes the determination of the carbon according to equation (I), (III, IV) (C2H5) 2NCS2H + NH (C2H5) 2 NH (C2H5) 2 (C2H5) 2 (C2H5) 2NCS2H.NH (C2H5) 2 + Cu (CH5COO), 2 - [(C2H5) 2NCS2jCu + + 2 CH3COOH + 2 NH ( C2'H5) 2 - (IV)

Ditiokarbamát mednatý je hnedosfarbenázlt^čenina, ktorá sa stanoví kolorimetricky.Obdobné túťo metodu popisuje tiež V. Va-šák v Chemická analýza priemyslového 0-vzdušia SZN Praha (1962).Copper dithiocarbamate is a brown phospharbenase thioline which is determined by colorimetric methods. A similar method is also described by V. Va-shak in Chemical Analysis of Industrial O-Air SZN Prague (1962).

Moris B. Jakobs v Inorganic Poisons, JohnWiley and sons, New York (1967) popisujestanovenie sírouhlíka reakciou s etylamí-nom a octanom mednatým. Popisuje tu dá-le j modifikovaná dietylamínovú metódu, kdepoúžíva okrem dietylamínu a octanu hied-natého aj trietanolamín. Je tu popísaná tiežxantogenátová metóda stanovenia sírouhlí-ka, iba miestoi KOH sá používá NaOH. Ďa-lej sa tu spomína kolorimetrické stanoveniesírouhlíka xantogenátovou metodou. Etyl-xantogenát draselný po reakcii s octanommednatým tvoří žité sfarbenie, ktoré sa sta-noví kolorimetricky.Moris B. Jakobs in Inorganic Poisons, John Wiley and sons, New York (1967) describes the determination of carbon disulfide by reaction with ethylamine and copper acetate. Described herein is a modified diethylamine method, in addition to diethylamine, and triethanolamine. Also described herein is an xanthanate method for the determination of carbon disulfide, only NaOH is used in place of KOH. Hereinafter, the colorimetric determination of carbon by xanthogenate method is mentioned. Potassium ethyl xanthate, upon reaction with acetate, forms a lustrous color which is colorimetrically determined.

Postup podlá vynálezu umožňuje'stano-vit sírouhlík, ktorý sa nachádza v plynnej,kvapalnej alebo tuhej fáze. Podstata vynále-zu spočívá v tom, že sírouhlík .zreaguje s 35 9 • ' 4 £ djgJ^ylágjnpnj na diaj^ylamínovú sol dial-kyjditio^ard,aipípoyej kyseliny podl'a rovni-ce (III). Dialkyladitiokarbanánová sol' sastitruje odmerným roztokom octanu ortuť-n.atéhn na indikátor difenylkarbazidČeHs—NH—NII—CONH—NH—CsHs. Preby-točné Hg2+lóny zreagujú s difenylkarbázi-dom na intenzívně fialové sfarbenie, čím saindikuje koni.ec titrácie. Ako indikátor samóže použit tiež djf enyíkarbazón ' CeHsNH—NH -CO—N -N—CeHs. Výhodou nového sposobu stanovenia sí-rouhlíka merkurimetricky je jeho jednodu-chost a spolehlivost Sírouhlík možno sta-novit y množstváph, ktoré sa bežne stano-vujú titraČnými metódami. Přikladl.The process of the invention allows the carbon disulphide to be present in the gaseous, liquid or solid phase. SUMMARY OF THE INVENTION The present invention is based on the fact that the carbon disulfide is reacted with the alkali metal salt of the dialkylamine salt of the acid according to equation (III). Dialkyladithiocarbanane salt is sastitrated with a standard mercuric acetate solution to give diphenylcarbazide-H-NH-NII-CONH-NH-CsHs indicator. Excess Hg2 + lons react with diphenylcarbase to intensely violet color, indicating the end of titration. Also used is a diphenylcarbazone, C 6 H 5 NH-NH-CO-N -N-C 6 H 5, as a self-indicator. The advantage of the new method for the determination of sulfur hexafluoride is its simplicity and reliability. Carbon disulfide can be determined by amounts which are normally determined by titration methods. Přikladl.

Do prebublávačky s fritou S2 sa dalo 20mililitrov dietylamínu a 5(3 ml etanolu. Rých-losťou 1,5 litra za minútu sa nechal cez fri-tu presávať vzduch, ktorý obsahoval síro-uhlík. Po přesátí vzduchu sa roztok kvanti-tativné prelial do 100 ml odmerky a doplniletanolom po značku. Odpipetovalo sa 25 mlzásobného roztoku, přidalo sa 3 kvapky di-fenylkarpazónu a titrovalo 0,05 N odmer-ným roztokom octanu ortuťnatého do fialo-. vomodrého sfarbenia. Hmotnostný' Obsah sí-rouhlíka vo vzduchu bol 0,127 °/o. Paralelnésg ťobilo stanovenie sírouhlíka z odmernejbanky tak, žé ša. přidal octan mednatý. Ob-sah sírouhlíka sa stanovil kolorimetricky.Podlá tejto metody bol hmotnostný obsah sírouhlíka 0,126 %. , P r i k 1 a d 220 ml of diethylamine and 5 (3 ml of ethanol were added to a S2 fritted tube), at a rate of 1.5 liters per minute, the air containing sulfur-carbon was passed through the filter. 100 ml volumetric flasks and supplementary ethanol are added by pipetting 25 ml of duplicate solution, 3 drops of diphenylcarpazone are added and titrated with a 0.05 N volumetric mercuric acetate solution to a violet blue color. The carbon disulphide content was determined by colorimetric analysis. According to this method, the carbon disulphide content was 0.126%, and the content of carbon disulphide was determined by colorimetric analysis.

Bp§tppqyalo sa pqdjd přikladl) 1, iba‘indikátor sp použij difenylkarbazid. Hmot-nostný obsah sírouhlíka hfll Q,127Příklad 3 po pdmcrky sa odyážjjp 5 § alkobflljcké-hq pqztoku sírpqhlíka. pájgj §a postupqya-' lo podlá příkladů 1. Hmotnostný obspjj §}-rouhlíka stanovený merkurimetricky na di-fenylkarbazón ako indikátor bol 2,54 %, a kolorimetricky 2,53 °/o. Přikládá 1 . ddvážilo sa 5 g pódy obsahujúcej síro-uhlík, z pódy sa sírouhlík vyextrahoval kvan-titativné'etanolom. palej sa postupovalo po-dlá příkladu 1. Hmotnostný obsah sírouhlí-ka stanovený merkurimetricky na difenyl-karbazón bol 0,241 %,'As used in Example 1 only, diphenylcarbazide is used. The carbon disulphide content of carbon monoxide, 127, Example 3, after the reaction, is stripped of alkali metal carbonate. pájgj §a postupqya- 'lo according to the examples 1. Mass obspjj §} -carbur determined merkurimetrically to diphenylcarbazone as an indicator was 2.54%, and colorimetrically 2.53 ° / o. Attaches 1. 5 g of sulfur-carbon-containing beer were weighed out, and carbon disulphide was extracted from the stage with quaternary ethanol. the palette was carried out as described in Example 1. The carbon disulphide content determined by mercury to diphenylcarbazone was 0.241%.

Stanovenie sírouhlíka podlá vynálezu mož-no použiť hlavně pri stanovení sírouhlíka vodpadných vodách a ovzduší. Obsah sírouhlí-ka v zásobnom roztoku sa musí pohybovat1v koncentráciach běžných pri ťitračných sta-noveniach. Z tohto dóvodu je metóda vhod-ná pre vyššie koncentrácie sírouhlíka.The carbon disulfide determination according to the invention can be used mainly in the determination of carbon disulphide in effluent and air. The carbon disulphide content of the stock solution must be in the concentrations common to the titration assay. For this reason, the method is suitable for higher carbon disulphide concentrations.

Claims (1)

240359 5/ 6 předmEt Spósob stanovenia sírouhlíka spočívajúciv reakcii sírouhlíka s prebytkom dialkylá-mínu na dialkylamínovú sol kyseliny dial-kylditiokarbamínovej vyznáčujúci sa tým, žévzniklá dialkylamínová sol' kyseliny diakyl- vynálezu . ditiokatbamínovej sa .stitruje odmerným roz-tokom octanu ortuťnatého na indikátor di-fenylkarbazid, lebo difenylkarbazon do fia-,lovomodrého sfarbeniaA method for the determination of carbon disulfide consists in reacting carbon disulfide with an excess of dialkylamine to dialkylamine salt of dialkyldithiocarbamic acid, characterized in that the dialkylamine salt of diacylic acid of the invention is formed. dithiocatbamine is titrated with the mercuric acetate titration to the diphenylcarbazide indicator, or diphenylcarbazone to the filament, blue color
CS823609A 1982-05-18 1982-05-18 A method for determining carbon disulphide CS240359B1 (en)

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