THE JOURNAL OF ANALYTICAL CHEMISTRY OF THE USSR

Document Type: 
Collection: 
Document Number (FOIA) /ESDN (CREST): 
CIA-RDP81-01043R000400050007-1
Release Decision: 
RIPPUB
Original Classification: 
K
Document Page Count: 
65
Document Creation Date: 
December 22, 2016
Document Release Date: 
July 20, 2010
Sequence Number: 
7
Case Number: 
Publication Date: 
June 1, 1956
Content Type: 
REPORT
File: 
AttachmentSize
PDF icon CIA-RDP81-01043R000400050007-1.pdf11.3 MB
Body: 
Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 11 THE JOURNAL OF ANALYTICAL CHEMISTRY . OF THE USSR Volume XI, No. 3 (May-June, 1966) IN ENGLISH TRANSLATION Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 STAT Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 TI-IE JOURNAL OF ANALYTICAL'CHEMISTRY OF THE USSR IN ENGLISH TRANSLATION May-June, 1956 TABLE OFCONTENTS 1. A New Gravimetric Method for the Determination of the Nitrite Ion Using Nitriton-B . (o-Aminoanilide of Benzene Sulfonic Acid). N.P.. Komar and I.U. Martynchenko. 2. A Microflotation Method of Analyzing Heavy Water. I.P. Gragerov ........... 3. Separation of Niobium, Tantalum and Titanium by Extraction. F.V. Zaikovsky... . Russ. Page Page 265 259 271 264 277 269 4. Separation of Magnesium, Aluminum, Chromium, Manganese, Iron, Nickel and Cop- per by an Ion-Exchange Method. D.I. Ryabchikov and V.F. Osipova ......... 285 278 5. Colorimetric Determination of Traces of Copper in Metallic Nickel and Its Compounds in the Ultra-Violet. K.P.. Stolyarov and F.B. Agrest .................... 293 286 6. Rapid Methods of Micro-Elemental Analysis. Part 12. Simultaneous Determination of Carbon, Hydrogen, Silicon and Halides. V.A. Klimova and E.G. Bereznitskaya... 299 292 7. ' Isolation and Separation of a Mixture of Formaldehyde and Acetaldehyde by Means of Dimedone. A.F. Lukovnikov..................................... 305 299 8..` Application of d-Hydroxynaphthoic Aldehyde in Analytical Chemistry. Part 2. A New Semi.-Micro Gravimetric Method for the Determination of Copper. S.I. Gusev and V.1. Kumov ....................................... 309 303 . Chromotropic Azo Dyes as Reagents for Trivalent Thallium. I.M. Korenman, V.G. . Potemkina and L.S. Fedorova .................................. 313 307 10. Polarographic Determination of Acrylonitrile in Aqueous-Alcohol Solutions. M.N. Platonova ............................................... 317 310 :ii. Polarographic Determination on Solid Electrodes of Heavy Metals in the Air of Indus- trial Establishments. I.B. Kbgan ............................... 321 313 12. Kinetic Methods of Quantitative Analysis. Part III. Determination of Small Amounts of Molybdenum. K.B. Yatsimirsky and L.P. Afanaseva . ........ 327 319 331 323 13. Cementation of Certain Metals by Zinc Amalgam. E.F. Speranskaya ........ . 14. " A Mercurimetric Method of Determining Iodides. R. Mi. Zamanov............ 339 329 15. A Method of Concentrating Traces of Copper by Means of Organic Reagents. V.T. Chuiko and A.U. Mamenko ......................... ... ...... . 343 332 16. The Precipitability of Strontium Oxalate in the Presence of Other Ions. M.P. Babkin 347 337 17. Systematic and Random Errors in Chemical Analysis. V.V. Nalimov......... 351 341 18. A Manostatoand Receiver for Vacuum Distillation in Columns. M.I. Rosengart, A.L. Liberman and D.M. Dubinin ..... .................... .. .. 361 351 Brief Communications 19. The Use of Chromatography in Qualitative Analysis. Stoiko Yankov. ........ 365 355 20. The Dichromate Method of Determining.Piperazine. A.A. Chemerisskaya . 367 356 (Continued on inside back cover) Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 THE JOURNAL OF ANALYTICAL CHEMISTRY OF THE U.S.S.R. Molume XI, No. 3 May?June, 1956 Editor in Chief: A. P. Vinogradov Editorial Board: I. P. Alimarin, A. M. 'Dymov, E. S. Przhevalsky, D. I. R y a b c h i k o v (executive secretary), I . V . Tananaev (assistant t o the ediior in chief), Z . F. S h a k h o v a Collaborators: A. K. Babko, S. A. Borovik, A. M. Vasilyev (deceased), N. I. Vlodavets, S. I. Volfkovich, A. A. Grinberg, P. A. Kashinsky, A. S. Komarovsky, M. .'Konstantinova-Shlezinger, . I. M. Korenman, S. E. Krasikov, Yu. Yu. `Lurye, Yu. V. Moraehevsky, K. A. Nenadkevich, V. I. Petrashen, N. K. Pshenitsyn, A. K. Rusanov, S A., Strelkov,, N. A. Tananaev, A. N. Terenin, A. P. Terentyev, M. L. Chepelevetsky, Yu. A ` Chernikov, E, A. Shilov (A Publication of the .'.cademy of Sciences of the U.S.S.R.) STAT Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 A NEW GRAVIMETRIC METHOD FOR TIDE DETERMINATION OF THE NITRITE ION USING NITRITON-B (o-AMINOA.NILIDE OF BENZENESULFONIC ACID) N. P. Komar and I.yu. Martynchenko A.. M. Gorky Kharkov State University . During studies of the interaction of NOz ions with the o-amnoanilide of benzenesulfonic acid, which we tried to use instead of the less readily available o-anilide.of diphenic acid (Nitriton A. ) [1], it was found that the white turbidity, which appears on pouring the solutions together, very rapidly changes over into a coarse crystalline precipitate. In this sense, Nitriton B behaves like substances whose solubility changes considerably with crystal size, while the white turbidity which Nitriton A. forms with nitrite ions, does not possess this property. PreIi iif lry experiments showed that Nitriton B practically completely'precipitates NOz ions according to the reaction H HZN N = N (->- S - N?-~ \ HNO - SOa N -~ \ 2H20, leading to the form ation'of benzenesulfanyl-o-phenylenediazimide (atriazole). This precipitate, as indicated above, satisfies the requirements normally met in gravimetric analysis. This fact persuade~""us to study the possibility of using this reaction for the direct gravimetric determination of nitrite. This problem proved of particul~ t' interest in view of the fact that hitherto no method has been published for the gravimetric determination of nitrite ions. NaNOz Solution. The solution was prepared from?.cheniically pure grade material, which was given a preliminary wash with boiled water;it was isolated from air by means of two washers, one of which contained a solution of KOH 1: 2, while the other contained a mixture of one volume of KOH 1: 2 and one volume of pyrogallol 1: 5. NOZ concentration was checked by means of permanganate. Nitriton B Solution. 2.480 g of the o-aminoanilide of benzenesulfonic acid was dissolved in 1 liter of 0.2 M I-J S04. The solution can be stored. 0.2%. All the dilutions were carried out in calibrated measuring apparatus to ensure errors of not more thaq Preliminary tests were carried out over a wide pH range for 3.0 to 8.5. It was found that at a pH of 8,5, in general, no precipitate of the triazole was formed; neither was any formed at lower pH values until (o) 3,5 was reached, at which it was first detected. Within this pH range the reaction for NOi remained quite positive. Only at a pH of 3 was quantitative separation of NOx ions from solution achieved; at a pH of ~ 1.5 however, together with precipitate formation, the odor of nitrogen oxides could be detected, indicating the danger of loss of NOi ions. In this connection, further work was carried out in the pH range 1.5-2,8, with slow addition of reagent to the solution to be tested and efficient agitation. It was found, in addition, that complete 265 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 11 21. A Fractional Reaction for Cobalt. M.A. Popov. ............ . . Russ. Page Page 369 357 22. A New Indicator - Oxine Blue. LE. Lev ....... 371 359 23. Detection of Lead in Ores by the Trituration Method. E.P. Ozhigov, M.A. Rafienko and L.K. Ivanenka .... .......... .................... 373 361 24. Detection of Fluorine in Minerals and Ores by a Trituration Method. E.P. Ozh you . 375 . 363 Chronicle 25. ? Anatoly Kiprilovich Babko (On His Fiftieth Birthday) ...................... 3'77 365 26. Conference Held in Gorky State University on the Application of Labeled Atoms in Chemistry.......... . .................:............ 381 367 27. Announcement ................................................ , 383 368 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1 STAT Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1