THE JOURNAL OF ANALYTICAL CHEMISTRY OF THE USSR
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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
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STAT
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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)
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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
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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
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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
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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
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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
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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
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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
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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
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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
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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
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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
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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
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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
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STAT
Sanitized Copy Approved for Release 2010/07/20 : CIA-RDP81-01043R000400050007-1