PL53146B1 - - Google Patents

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Publication number
PL53146B1
PL53146B1 PL112839A PL11283966A PL53146B1 PL 53146 B1 PL53146 B1 PL 53146B1 PL 112839 A PL112839 A PL 112839A PL 11283966 A PL11283966 A PL 11283966A PL 53146 B1 PL53146 B1 PL 53146B1
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PL
Poland
Prior art keywords
halogen
combustion products
air
bromate
iodate
Prior art date
Application number
PL112839A
Other languages
Polish (pl)
Inventor
inz. Jerzy Waclawik mgr
inz. StefanWaszak mgr
Original Assignee
Instytut Chemii Ogólnej
Filing date
Publication date
Application filed by Instytut Chemii Ogólnej filed Critical Instytut Chemii Ogólnej
Priority to DE19671598641 priority Critical patent/DE1598641A1/en
Priority to GB5708/67A priority patent/GB1172262A/en
Priority to NL6701901A priority patent/NL6701901A/xx
Priority to FR94148A priority patent/FR1510628A/en
Priority to US614537A priority patent/US3546079A/en
Publication of PL53146B1 publication Critical patent/PL53146B1/pl

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Description

Pierwszenstwo: Opublikowano: 23. III. 1967 53146 KI. 42 1, 4/16 MKP G 01 n i£ C1YTELHIAI •i| mr»w**u Wspóltwórcy wynalazku: mgr inz. Jerzy Waclawik, mgr inz. Stefan Waszak Wlasciciel patentu: Instytut Chemii Ogólnej, Warszawa (Polska) Ciagly sposób oznaczania niewielkich stezen par chlorowcopochod¬ nych zwiazków organicznych i/albo chlorowcowodorów w po¬ wietrzu i innych gazach Wynalazek dotyczy ciaglego sposobu oznaczania par chlorowcopochodnych zwiazków organicznych np. trójchloroetylenu, czterochloroetylenu, chloro¬ formu, bromku metylu, fosgenu i chlorowcowodo¬ rów np. HCL, HBr, HF znajdujacych sie w bada¬ nym powietrzu lub innym gazie w postaci zanie¬ czyszczen w bardzo malych ilosciach rzedu do 0,02 ppm. Sposób ten polega na przeprowadzeniu chlorowca znajdujacego sie w zwiazkach w po¬ staci zwiazanej w wolny chlorowiec, który naste¬ pnie mozna oznaczac znanymi metodami, np. we¬ dlug opisu patentowego nr 50 961.Znane dotychczas sposoby polegaly badz na kolo¬ rymetrycznym oznaczaniu poszczególnych zwiaz¬ ków, badz na absorpcji ich w odpowiednim medium i nastepnie oznaczaniu róznymi metodami perio¬ dycznymi. Metody te jednak nie zapewniaja doklad¬ nego oznaczenia ilosciowego; sa one przewaznie jakosciowe lub pólilosciowe, a poza tym sa bardzo pracochlonne i czasochlonne.Z kolei istniejace ciagle metody oznaczania, zwlaszcza sposoby absorpcji w podczerwieni lub w ultrafiolecie wymagaja bardzo kosztownej apa¬ ratury.Znany jest takze sposób polegajacy na spaleniu wymienionych zwiazków w naczyniu kwarcowym wypelnionym ksztaltkami kwarcowymi lub meta¬ liczna platyna w postaci drutu lub folii. Otrzymana po spaleniu mieszanine chlorowca i chlorowcowodo¬ ru absorbowano w odpowiednim medium a nastep- 10 15 20 25 30 nie kolejno oznaczano poszczególne skladniki. Spo¬ sób ten wymaga stosowania do spalania chlorowco¬ pochodnych bardzo wysokich temperatur rzedu 950—1100°C i nie zapewnia równiez dokladnosci oznaczania.Wad tych mozna uniknac jesli zwiazany w zwiaz¬ kach organicznych chlorowiec przeprowadzi sie w wolna postac sposobem wedlug wynalazku.W tym celu powietrze lub gaz zanieczyszczone chlorowcopochodnymi i/albo chlorowcowodorami przepuszcza sie w sposób ciagly przez piec o tem¬ peraturze okolo 800°C wypelniony katalizatorem palladowym. W piecu nastepuje ilosciowe spalanie zanieczyszczen do wlasciwego chlorowcowodoru lub chlorowca, albo obu jednoczesnie. Produkty spa¬ lania przechodza nastepnie przez rurke wypelniona mieszanina bromku i bromianu, badz jodku i jo¬ danu, lub przez pluczke z ich wodnymi roztwo¬ rami. Podczas tej operacji produkty spalania prze¬ chodza ilosciowo w chlorowiec, który nastepnie oznacza sie sposobem i w urzadzeniu wedlug pa¬ tentu nr 50961, badz znanymi innymi metodami.Korzystnie jest jednakze stosowac do dalszego oznaczania metode elektrochemiczna podana w opi¬ sie patentu nr 50961.Jest to metoda prosta, czula i bardzo dokladna, która nie wymaga stosowania dodatkowo zródla energii elektrycznej a poza tym nadaje sie do wy¬ korzystania w ukladach sygnalizacyjnych.W przypadku stosowania metody galwanicznej 5314653146 3 4 produkty spalania uzyskane sposobem wedlug wy¬ nalazku mozna przeprowadzac bezposrednio do roztworu elektrolitu, który zawiera bromek i bro¬ mian lub jodek i jodan.Przyklad. Powietrze zanieczyszczone parami 5 trójchloroetylenu w ilosci do 3,0 ppm przeplywalo ze stala szybkoscia przez piec o temperaturze 800°C wypelniony katalizatorem palladowym. W piecu tym nastapilo ilosciowe spalanie trójchloroetylenu do dwutlenku wegla, chloru i do chlorowodoru, io „ Produkty spalania przepuszczano nastepnie przez \ugke wypelniona mieszanina bromku i bromianu wydzielajac równowazna ilosc bromu, która naste¬ pnie • oznaczono sposobem i w urzadzeniu wedlug opisu patentowego nr 50961. 15 PLPriority: Published: 23. III. 1967 53146 KI. 42 1, 4/16 MKP G 01 n i £ C1YTELHIAI • i | mr »w ** u Inventors: Jerzy Waclawik, MSc, Stefan Waszak, MSc. Patent owner: Institute of General Chemistry, Warsaw (Poland) Continuous method of determination of small concentrations of halogenated organic compounds and / or halogenated vapors in the air and other gases. The invention relates to a continuous method of determining the vapors of halogenated organic compounds, e.g., trichlorethylene, tetrachlorethylene, chloroform, methyl bromide, phosgene and halogenated hydrocarbons, e.g. HCl, HBr, HF, contained in the test air or other gas in the form of a vapor. ¬ cleanings in very small amounts, down to 0.02 ppm. This method consists in converting a halogen in a compound in a bound form into a free halogen, which can then be determined by known methods, e.g. according to the patent specification No. 50,961. The methods known so far consisted in the color-symmetric determination of individual compounds, or by absorbing them in a suitable medium and then determining them by various periodical methods. These methods, however, do not provide accurate quantification; they are usually qualitative or semi-quantitative, and besides, they are very laborious and time-consuming. In turn, the existing continuous methods of determination, especially methods of infrared or ultraviolet absorption, require very expensive equipment. There is also a known method involving the combustion of the above-mentioned compounds in a quartz vessel filled with quartz or metal platinum in the form of wire or foil. The mixture of halogen and hydrogen halide obtained after combustion was absorbed in a suitable medium, and then the individual components were successively determined. This method requires the use of very high temperatures, in the order of 950-1100 ° C, for the combustion of halogen derivatives, and also does not ensure the accuracy of the determination. These disadvantages can be avoided if the halogen bound in organic compounds is converted into free form according to the invention. For the purpose, air or gas contaminated with halogenated and / or hydrogen halides is continuously passed through a furnace at a temperature of about 800 ° C., filled with a palladium catalyst. The furnace quantitatively burns the pollutants to the appropriate hydrogen halide or halogen, or both. The combustion products then pass through a tube filled with a mixture of bromide and bromate or iodide and iodate, or through a rinse with their aqueous solutions. During this operation, the combustion products are converted quantitatively into halogen, which is then determined by the method and apparatus according to patent No. 50961, or by other methods. It is preferable, however, to use the electrochemical method for further determination, given in patent No. 50961. is a simple, sensitive and very accurate method, which does not require the use of an additional source of electricity and is also suitable for use in signaling systems. When using the galvanic method 5314653146 3 4 the combustion products obtained by the method according to the invention can be carried out directly to electrolyte solution, which contains bromide and bromine or iodide and iodate. Air contaminated with trichlorethylene vapors up to 3.0 ppm was passed at a constant rate through an oven at 800 ° C filled with palladium catalyst. In this furnace, the quantitative combustion of trichlorethylene to carbon dioxide, chlorine and hydrogen chloride took place, and the combustion products were then passed through a gulley filled with a mixture of bromide and bromate, giving off an equivalent amount of bromine, which was then determined by the method and apparatus according to patent description No. 50961. 15 PL

Claims (2)

Zastrzezenia patentowe 1. Ciagly sposób oznaczania niewielkich stezen par chlorowcopochodnych zwiazków organicznych i/albo chlorowcowodorów w powietrzu i innych 20 gazach, znamienny tym, ze powietrze lub gaz zanieczyszczone chlorowcopochodnymi, i/albo chlorowcowodorami przepuszcza sie w sposób ciagly przez piec o temperaturze okolo 800°C 5 wypelniony katalizatorem palladowym, gdzie na¬ stepuje spalanie zanieczyszczen do wlasciwego chlorowcowodoru lub chlorowca albo obu jedno¬ czesnie, a produkty spalania przechodza naste¬ pnie przez rurke wypelniona mieszanina bromku 10 i bromianu, badz jodku i jodanu lub przez plucz¬ ke z ich wodnymi roztworami, przy czym pro¬ dukty spalania przechodza ilosciowo w chloro¬ wiec, który nastepnie oznacza sie sposobem i w urzadzeniu wedlug patentu nr 50961, badz 15 innymi znanymi metodami.Claims 1. A continuous method of determining low concentrations of halogenated organic compounds and / or hydrogen halides in air and other gases, characterized in that air or gas contaminated with halogen derivatives and / or hydrogen halides is continuously passed through a furnace at a temperature of around 800 ° C C 5 filled with a palladium catalyst, where the pollutants are burned to the appropriate hydrogen halide or halogen or both, and the combustion products then pass through a tube filled with a mixture of bromide and bromate, or iodide and iodate, or by flushing with them. with aqueous solutions, the combustion products being converted quantitatively into chlorine, which is then determined by the method and apparatus according to patent No. 50961, or by other known methods. 2. Sposób wedlug zastrz. 1 znamienny tym, ze w przypadku oznaczania chlorowca sposobem wedlug patentu nr 50961 produkty spalania prze¬ prowadza sie bezposrednio do roztworu elektro¬ litu, który zawiera bromek i bromian lub jodek 20 i jodan. 10 15 KRAK 4, Sarego 7 — Zam. 73/67 — 340 PL2. The method according to claim The method of claim 1, characterized in that, in the case of the determination of halogen by the method of Patent No. 50,961, the combustion products are transferred directly to an electrolyte solution which contains bromide and bromate or iodide and iodate. 10 15 KRAK 4, Sarego 7 - Zam. 73/67 - 340 PL
PL112839A 1966-02-08 1966-02-08 PL53146B1 (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
DE19671598641 DE1598641A1 (en) 1966-02-08 1967-02-06 Continuous method for the determination of small amounts of fumes from halogen derivatives of organic compounds and hydrogen halides in air and other gases
GB5708/67A GB1172262A (en) 1966-02-08 1967-02-07 An Improved Method for Continuously Determining Concentrations of Gaseous Halogenated Organic Compounds and of Hydrogen Halide in Air or in Other Gases
NL6701901A NL6701901A (en) 1966-02-08 1967-02-08
FR94148A FR1510628A (en) 1966-02-08 1967-02-08 Method for continuously determining low concentrations of gaseous halogenated organic compounds and hydrogen halides in gases
US614537A US3546079A (en) 1966-02-08 1967-02-08 Method for determining continuously small concentrations of gaseous halogenated compounds and of hydrogen halides in air and in other gases

Publications (1)

Publication Number Publication Date
PL53146B1 true PL53146B1 (en) 1967-02-25

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