SU72251A1 - Method for quantitative determination of pyridine bases - Google Patents
Method for quantitative determination of pyridine basesInfo
- Publication number
- SU72251A1 SU72251A1 SU4916A SU4916A SU72251A1 SU 72251 A1 SU72251 A1 SU 72251A1 SU 4916 A SU4916 A SU 4916A SU 4916 A SU4916 A SU 4916A SU 72251 A1 SU72251 A1 SU 72251A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- pyridine bases
- solution
- quantitative determination
- ammonia
- pyridine
- Prior art date
Links
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 title description 22
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 title description 11
- 238000000034 method Methods 0.000 title description 5
- 239000002585 base Substances 0.000 description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- 229910021529 ammonia Inorganic materials 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 2
- 239000007853 buffer solution Substances 0.000 description 2
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 description 2
- 239000012047 saturated solution Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910021204 NaH2 PO4 Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- DLGYNVMUCSTYDQ-UHFFFAOYSA-N azane;pyridine Chemical compound N.C1=CC=NC=C1 DLGYNVMUCSTYDQ-UHFFFAOYSA-N 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229940045641 monobasic sodium phosphate Drugs 0.000 description 1
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 1
- 235000019799 monosodium phosphate Nutrition 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Description
В основу способа положено применение буфера - насыщенного раствора одноосновного фосфорнокислого натра, имеющего ,3- 4,6, достаточный дл удержани аммиака в растворе и дл полной отгонки пиридиновых оснований.The method is based on the use of a buffer — a saturated solution of monobasic sodium phosphate, having 3–4.6 sufficient to keep the ammonia in solution and to completely distill the pyridine bases.
Описываемый способ количественного определени пиридиновых оснований заключаетс в следующем .The described method for the quantitative determination of pyridine bases is as follows.
Берут навеску анализируемого продукта из расчета содержани в ней пиридиновых оснований около 0,15 S, разбавл ют водой до 200 мл, подщелачивают при индикаторе фенолфталеине до слабого порозовени и отгон ют в аппарате Кьельдал пиридиновые основани с примесью аммиака в приемник, содержащий 10%-ный раствор серной кислоты. Дестиллат нейтрализуют по смешанному индикатору (0,1% диметилгельба и 0,1% метиленовой сини), имеющему рН 3,25.A sample of the analyzed product is taken from the calculation of about 0.15 S of pyridine bases in it, diluted with water to 200 ml, made alkaline with phenolphthalein indicator until slightly rosy, and the Kjeldahl apparatus is distilled off into the receiver containing 10% ammonia. sulfuric acid solution. The distillate is neutralized by a mixed indicator (0.1% dimethylgel and 0.1% methylene blue) having a pH of 3.25.
Полученный дестиллат количественно перенос т в аппарат Кьельдал , добавл ют к нему буферный раствор (насыщенный раствор NaH2 РО4) и отгон ют свободные отThe obtained distillate is quantitatively transferred to a Kjeldahl apparatus, a buffer solution is added to it (saturated solution of NaH2 PO4) and the free
аммиака пиридиновые основани в приемник, содержащий 0,2 N раствор серной кислоты, подкрашенной смешанным индикатором.ammonia pyridine bases to a receiver containing a 0.2 N solution of sulfuric acid tinted with a mixed indicator.
Количество пиридиновых оснований определ етс обратным титрованием свободной кислоты 0,1 N раствором щелочи.The amount of pyridine bases is determined by back titration of the free acid with a 0.1 N alkali solution.
После первичной отгонки пиридиновых оснований в растворе содержитс 0,01 мол сульфатов пиридиновых оснований, по расчету имеющих рН 3,58 и 0,01 мол сульфатаммони - рН около 5,5. При кип чении такого раствора, нейтрализованного по смешанному индикатору, при добавлении к нему буферного раствора, который поддерживает рН раствора около 4, отгон ютс только пиридиновые основани , а аммиак удерживаетс в растворе.After the initial distillation of the pyridine bases, 0.01 mol of pyridine bases sulfates are contained in the solution, calculated to have a pH of 3.58 and 0.01 mol of ammonium sulfate - pH about 5.5. When such a solution, neutralized by a mixed indicator, is boiled, adding a buffer solution that maintains the pH of the solution to about 4, only pyridine bases are distilled off, and ammonia is kept in solution.
Метод дает точность до 1 % содержани пиридиновых оснований.The method gives an accuracy of up to 1% of the content of pyridine bases.
Предмет изобретени Subject invention
Способ количественного определени пиридиновых оснований в присутствии аммиака или аммоний219Method for quantitative determination of pyridine bases in the presence of ammonia or ammonium219
№ 72251 2 -72251 2 -
ных солей, отличающийс тем,н ют пиридиновые основани , нечто после добавлени к испытуемо-содержащие аммиака, и подверму раствору одноосновного фос-гают их ацидиметрическому титрофорнокислого натри от смеси отго-ванию.salts, characterized by the addition of pyridine bases, something after adding ammonia to the test substance, and exposing them to a solution of monobasic phos- phage of their acidimetric sodium titrophoric acid from the mixture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU4916A SU72251A1 (en) | 1943-01-25 | 1943-01-25 | Method for quantitative determination of pyridine bases |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU4916A SU72251A1 (en) | 1943-01-25 | 1943-01-25 | Method for quantitative determination of pyridine bases |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| SU69534A1 SU69534A1 (en) | 1947-10-31 |
| SU72251A1 true SU72251A1 (en) | 1947-11-30 |
Family
ID=48248840
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU4916A SU72251A1 (en) | 1943-01-25 | 1943-01-25 | Method for quantitative determination of pyridine bases |
Country Status (1)
| Country | Link |
|---|---|
| SU (1) | SU72251A1 (en) |
-
1943
- 1943-01-25 SU SU4916A patent/SU72251A1/en active
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