SU51866A1 - The method of quantitative determination of 4,4 dinitrostilbene 2,2-disulfonic acids mixed with 4,4-dinitrodibenzyl 2,2-disulfonic acid - Google Patents
The method of quantitative determination of 4,4 dinitrostilbene 2,2-disulfonic acids mixed with 4,4-dinitrodibenzyl 2,2-disulfonic acidInfo
- Publication number
- SU51866A1 SU51866A1 SU??-1705A SU1705A SU51866A1 SU 51866 A1 SU51866 A1 SU 51866A1 SU 1705 A SU1705 A SU 1705A SU 51866 A1 SU51866 A1 SU 51866A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- disulfonic
- dinitrostilbene
- dinitrodibenzyl
- quantitative determination
- disulfonic acid
- Prior art date
Links
- 238000000034 method Methods 0.000 title description 4
- 239000002253 acid Substances 0.000 title description 3
- KHYMHQBQSOPFBF-UHFFFAOYSA-N 5,5-dinitro-2-(2-phenylethenyl)cyclohex-3-ene-1,1-disulfonic acid Chemical class OS(=O)(=O)C1(S(O)(=O)=O)CC([N+]([O-])=O)([N+]([O-])=O)C=CC1C=CC1=CC=CC=C1 KHYMHQBQSOPFBF-UHFFFAOYSA-N 0.000 title description 2
- UETHPMGVZHBAFB-OWOJBTEDSA-N 4,4'-dinitro-trans-stilbene-2,2'-disulfonic acid Chemical compound OS(=O)(=O)C1=CC([N+]([O-])=O)=CC=C1\C=C\C1=CC=C([N+]([O-])=O)C=C1S(O)(=O)=O UETHPMGVZHBAFB-OWOJBTEDSA-N 0.000 description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- NQAQCAROZAAHGL-UHFFFAOYSA-N (1,2-dinitro-2-phenylethenyl)benzene Chemical compound C=1C=CC=CC=1C([N+](=O)[O-])=C([N+]([O-])=O)C1=CC=CC=C1 NQAQCAROZAAHGL-UHFFFAOYSA-N 0.000 description 1
- QWUWMCYKGHVNAV-UHFFFAOYSA-N 1,2-dihydrostilbene Chemical group C=1C=CC=CC=1CCC1=CC=CC=C1 QWUWMCYKGHVNAV-UHFFFAOYSA-N 0.000 description 1
- ZDTXQHVBLWYPHS-UHFFFAOYSA-N 4-nitrotoluene-2-sulfonic acid Chemical class CC1=CC=C([N+]([O-])=O)C=C1S(O)(=O)=O ZDTXQHVBLWYPHS-UHFFFAOYSA-N 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 1
- PJANXHGTPQOBST-VAWYXSNFSA-N Stilbene Natural products C=1C=CC=CC=1/C=C/C1=CC=CC=C1 PJANXHGTPQOBST-VAWYXSNFSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- IZJVVXCHJIQVOL-UHFFFAOYSA-N nitro(phenyl)methanesulfonic acid Chemical compound OS(=O)(=O)C([N+]([O-])=O)C1=CC=CC=C1 IZJVVXCHJIQVOL-UHFFFAOYSA-N 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- PJANXHGTPQOBST-UHFFFAOYSA-N stilbene Chemical compound C=1C=CC=CC=1C=CC1=CC=CC=C1 PJANXHGTPQOBST-UHFFFAOYSA-N 0.000 description 1
- 235000021286 stilbenes Nutrition 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Description
При синтезе 4,4 динитростильбен 2,2 дисульфокислоты окислением п-нитротолуол - о-сульфокислоты, количественное определение конечного продукта сильно затруднено наличием побочного продукта реакции - 4,4 динитродибензил 2,2 дисульфокислоты.During the synthesis of 4,4 dinitrostilbene 2,2 disulfonic acids by oxidation of p-nitrotoluene - o-sulfonic acids, the quantitative determination of the final product is greatly hampered by the presence of a reaction by-product - 4,4 dinitrodibenyl 2.2 disulfonic acids.
Предлагаемое изобретение основано на известном из литературы различном отношении перманганата к стильбеновым и дибензильным производным.The present invention is based on the known ratio of permanganate to stilbene and dibenzyl derivatives known from the literature.
Способ состоит в том, что сначала определ ют общее содержание нитрогруппы смеси динитростильбен и динитродибензил дисульфокислот. Определение производ т обычными методами , например, восстанавливают пробу цинком и полученные амины титруют нитритом. Далее в отдельной навеске определ ют количество динитростильбен дисульфокислоты непосредственным титрованием перманганатом . Общее содержание нитропродуктов определ етс дл того, чтобы можно было выразить содержание динитростильбен дисульфокислоты в процентах от общего содержани The method consists in first determining the total nitro group content of the mixture of dinitrostilbene and dinitrodibenzyl disulfonic acids. The determination is made by conventional methods, for example, the sample is reduced with zinc and the resulting amines are titrated with nitrite. Next, in a separate sample, the amount of dinitrostilbene disulfonic acid is determined by direct titration with permanganate. The total content of nitroproducts is determined so that the content of dinitrostilbene disulfonic acid can be expressed as a percentage of the total content
нитропродуктов.nitroproducts.
Пользу сь предлагаемым методом, можно весьма точно проводить контроль процесса окислени нитротолуолсульфокислоты в динитростильбен дисульфокислоту.Using the proposed method, one can very accurately control the process of nitrotoluene sulfonic acid oxidation to dinitrostilbene disulfonic acid.
Пример. 10 г технической пасты динитростильбен дисульфокислоты размешивают в 500 см теплой воды и добавл ют небольшое количество серной кислоты до полного растворени пасты. Далее раствор нейтрализуют углекислым натром и довод т до 1 литра.Example. 10 g of technical paste dinitrostilbene disulfonic acid is stirred in 500 cm of warm water and a small amount of sulfuric acid is added until the paste is completely dissolved. The solution is then neutralized with sodium carbonate and adjusted to 1 liter.
К 500 см этого раствора прибавл ют 50 см сол ной кислоты (уд. веса 1,19) и нагревают до кипени . При температуре 90 - 95° осторожно внос т 30 г цинковой пыли. Через 5-10 минут раствор декантируют через воронку Бюхнера, осадок промывают 2 раза по 100 см гор чей воды, затем 100 см 25%-го аммиака и снова 100 см гор чей воды. Промывные воды все врем декантируют с осадка цинковой пыли через воронку и фильтраты соедин ют вместе. Наконец цинковую пыльTo 500 cm of this solution was added 50 cm of hydrochloric acid (specific weight 1.19) and heated to boiling. At a temperature of 90-95 °, 30 g of zinc dust are carefully introduced. After 5-10 minutes, the solution is decanted through a Buchner funnel, the precipitate is washed with 2 times 100 cm of hot water, then 100 cm of 25% ammonia and again 100 cm of hot water. The washings are decanted all the time from the zinc dust precipitate through a funnel and the filtrates are combined. Finally zinc dust
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU??-1705A SU51866A1 (en) | 1936-10-31 | 1936-10-31 | The method of quantitative determination of 4,4 dinitrostilbene 2,2-disulfonic acids mixed with 4,4-dinitrodibenzyl 2,2-disulfonic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU??-1705A SU51866A1 (en) | 1936-10-31 | 1936-10-31 | The method of quantitative determination of 4,4 dinitrostilbene 2,2-disulfonic acids mixed with 4,4-dinitrodibenzyl 2,2-disulfonic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU51866A1 true SU51866A1 (en) | 1936-11-30 |
Family
ID=52017909
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU??-1705A SU51866A1 (en) | 1936-10-31 | 1936-10-31 | The method of quantitative determination of 4,4 dinitrostilbene 2,2-disulfonic acids mixed with 4,4-dinitrodibenzyl 2,2-disulfonic acid |
Country Status (1)
| Country | Link |
|---|---|
| SU (1) | SU51866A1 (en) |
-
1936
- 1936-10-31 SU SU??-1705A patent/SU51866A1/en active
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