SU1647391A1 - Method for determining active oxygen in superconducting copper -containing ceramics - Google Patents
Method for determining active oxygen in superconducting copper -containing ceramics Download PDFInfo
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- SU1647391A1 SU1647391A1 SU894686125A SU4686125A SU1647391A1 SU 1647391 A1 SU1647391 A1 SU 1647391A1 SU 894686125 A SU894686125 A SU 894686125A SU 4686125 A SU4686125 A SU 4686125A SU 1647391 A1 SU1647391 A1 SU 1647391A1
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- solution
- active oxygen
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- sample
- superconducting
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 10
- 239000001301 oxygen Substances 0.000 title claims abstract description 10
- 239000000919 ceramic Substances 0.000 title claims abstract description 6
- 238000000034 method Methods 0.000 title claims abstract description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract 4
- 229910052802 copper Inorganic materials 0.000 title claims abstract 4
- 239000010949 copper Substances 0.000 title claims abstract 4
- 238000004448 titration Methods 0.000 claims abstract description 7
- 238000004458 analytical method Methods 0.000 claims abstract description 4
- 150000003839 salts Chemical class 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims abstract description 3
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract 6
- CKFMJXZQTNRXGX-UHFFFAOYSA-L iron(2+);diperchlorate Chemical compound [Fe+2].[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O CKFMJXZQTNRXGX-UHFFFAOYSA-L 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical class [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims 2
- GDDNTTHUKVNJRA-UHFFFAOYSA-N 3-bromo-3,3-difluoroprop-1-ene Chemical compound FC(F)(Br)C=C GDDNTTHUKVNJRA-UHFFFAOYSA-N 0.000 claims 1
- 150000007513 acids Chemical class 0.000 claims 1
- -1 phosphoric Chemical class 0.000 claims 1
- 239000012266 salt solution Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 26
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 abstract description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 abstract description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 abstract description 3
- 238000004364 calculation method Methods 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 239000012085 test solution Substances 0.000 abstract description 2
- LHOWRPZTCLUDOI-UHFFFAOYSA-K iron(3+);triperchlorate Chemical compound [Fe+3].[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O LHOWRPZTCLUDOI-UHFFFAOYSA-K 0.000 abstract 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 abstract 2
- 238000005516 engineering process Methods 0.000 abstract 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 abstract 2
- 239000002887 superconductor Substances 0.000 abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 2
- HYKDWGUFDOYDGV-UHFFFAOYSA-N 4-anilinobenzenesulfonic acid Chemical compound C1=CC(S(=O)(=O)O)=CC=C1NC1=CC=CC=C1 HYKDWGUFDOYDGV-UHFFFAOYSA-N 0.000 abstract 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract 1
- 238000009835 boiling Methods 0.000 abstract 1
- 239000001569 carbon dioxide Substances 0.000 abstract 1
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract 1
- 239000000460 chlorine Substances 0.000 abstract 1
- 229910052801 chlorine Inorganic materials 0.000 abstract 1
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 abstract 1
- 239000000706 filtrate Substances 0.000 abstract 1
- 238000005259 measurement Methods 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- 238000003908 quality control method Methods 0.000 abstract 1
- 239000004317 sodium nitrate Substances 0.000 abstract 1
- 235000010344 sodium nitrate Nutrition 0.000 abstract 1
- 238000004090 dissolution Methods 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 1
- ABGFJRRSVBIXEZ-UHFFFAOYSA-L disodium;n-phenylaniline;sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O.C=1C=CC=CC=1NC1=CC=CC=C1 ABGFJRRSVBIXEZ-UHFFFAOYSA-L 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- DGXTZMPQSMIFEC-UHFFFAOYSA-M sodium;4-anilinobenzenesulfonate Chemical compound [Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=CC=C1 DGXTZMPQSMIFEC-UHFFFAOYSA-M 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Изобретение относитс к способам определени активного кислорода в сверхпровод щей медьсодержащей керамике и может быть использовано при разработке технологии высокотемпературных сверхпроводников и при контроле их качества с целью повышени точности и сокращени времени анализа. Дл этого готов т 0,05 н. Изобретение относитс к аналитической химии, а именно к способам определени активного кислорода в сверхпровод щей медьсодержащей керамике, и может быть использовано при разработке технологии высокотемпературных сверхпроводников и контроле их качества. Целью изобретени вл етс повышение точности и сокращение времени анализа . Пример. Готов т 0.05 н.раствор перхлората железа (Н). Дл этого в колбу помераствор перхлората железа (It) путем растворени навески соли Мора в хлорной кислоте . Навеску образца сверхпровод щей керамики раствор ют в 10 мл 0,06 н.раствора Fe (CIO/i)2 в смеси с NH/iCI04 После полного растворени образца в раствор добавл ют 10 мл концентрированной НзР04 и 10 мл HCI04, 3 капли дифениламиносульфо- ната натри и титруют 0,04 н раствором КгСг20т. Расчет количества активного кислорода провод т по формуле Х-М а/(2т-16а). где М - молекул рна масса соединени без учета активного кислорода; m - масса навески Г, а - NK2O2O7 ( Vl - V2 ) 10 3 , rfleNK2Cr2O7 нормальность раствора бихро- мата кали , Vi и V2 - объемы раствора бих- ромата капи , идущие на титрование 10 мл раствора хлористого железа и исследуемого раствора соответственно, мл Погрешность определени индекса активного кислорода не превышает 2%, врем , затрачиваемое на проведение одного измерени , не более 10 мин. 1 табл сл с щают 0.2 М углекислого бари (ВаСОз) марки ч.д.а. и 300 мл воды и небольшими порци ми вливают хлорную кислоту НСЮд марки ч.д.а. (общее содержание кислоты - 0,5 мол ). По окончании бурного выделени углекислого газа раствор нагревают до начала кипени , в раствор небольшими порци ми при интенсивном перемешивании ввод т раствор соли Мора (0,1 моль в 200 мл воды) - (NH4)2Fe (804)2 марки ч.д.а. и оставл ют охлаждатьс . Хлорый раствор фильтруют . Осадок отбрасывают, а фильтрат о 4 sj CJ Ч)The invention relates to methods for determining active oxygen in superconducting copper-containing ceramics and can be used in the development of high-temperature superconductors technology and in controlling their quality in order to improve accuracy and reduce analysis time. To do this, prepare 0.05 n. The invention relates to analytical chemistry, in particular, to methods for determining active oxygen in superconducting copper-containing ceramics, and can be used in the development of high-temperature superconductors technology and their quality control. The aim of the invention is to improve the accuracy and reduce the analysis time. Example. Prepared 0.05 n solution of iron perchlorate (H). To do this, iron perchlorate (It) solution is dissolved in a flask by dissolving a portion of the Mora salt in perchloric acid. A portion of the sample of superconducting ceramics is dissolved in 10 ml of 0.06 n. Fe (CIO / i) 2 solution mixed with NH / iCl4. After the sample is completely dissolved, 10 ml of concentrated HzP04 and 10 ml of HCI04 are added to the solution, 3 drops of diphenylaminosulfonic acid. sodium nitrate and titrated with 0.04 N of the CrSg20t solution. The calculation of the amount of active oxygen is carried out according to the formula X-M a / (2m-16a). where M is the molecular weight of the compound, excluding active oxygen; m is the sample mass G, a is NK2O2O7 (Vl-V2) 10 3, rfleNK2Cr2O7 is normality of potassium bichromate solution, Vi and V2 are the volumes of dichromate solution capi, which are used for titration of 10 ml of ferric chloride solution and test solution, respectively, ml The error in determining the active oxygen index does not exceed 2%; the time taken to perform one measurement is not more than 10 minutes. 1 table sl with sch 0.2 m of barium carbonate (VaSO3) of grade ch.d. and 300 ml of water and pour in small portions of perchloric acid, grade HCSYD grade. (total acid content is 0.5 mol). After the end of the rapid evolution of carbon dioxide, the solution is heated to the beginning of boiling, a solution of Mohr salt (0.1 mol in 200 ml of water) - (NH4) 2Fe (804) 2 grade hp . and allowed to cool. Chlorine solution is filtered. The precipitate is discarded, and the filtrate is about 4 sj CJ h)
Description
разбавл ют в растворе НСЮ4(с содержанием кислоты 2 моль) и довод т обьем раствора до 2 л.diluted in a solution with HCL4 (with an acid content of 2 mol) and adjusted to a volume of 2 liters.
Приготовленный растворе рН 0 прозрачен , не имеет окраски, практически не окисл етс и устойчив в течение длительного времени. Точную концентрацию полученного раствора перхлората железа (II) определ ют титрованием бихроматом кали в кислой среде с дифениламинсульфонатом натри в качестве индикатора.The pH 0 prepared by the solution is transparent, has no color, is practically not oxidized, and is stable for a long time. The exact concentration of the resulting iron (II) perchlorate solution is determined by titration with potassium bichromate in an acidic medium with sodium diphenylamine sulfonate as an indicator.
Навеску образца высокотемпературной сверхпровод щей керамики УВа2СизОб,5 массой 0,2 г раствор ют в 10 мл раствора Fe(CIO4)2 в смеси с МЩСЮч. Растворение происходит без нагревани в течение 5 мин. Легкость растворени св зана с достаточно высокой кислотностью раствора. После полного растворени образца в раствор добавл ют 10 мл концентрированной дл св зывани Fe3 и 10 мл НС1См, 3 капли дифениламиносульфата натри и титруют 0,04 н. раствором foCrsC, приготовленным из точной навески соли марки х.ч. Перед каждым определением проводитс контроль концентрации раствора Fe(CI04)2.A sample of the high-temperature superconducting ceramics UV-2CizOb, 5 with a weight of 0.2 g, is dissolved in 10 ml of a solution of Fe (CIO4) 2 in a mixture with MSW. Dissolution occurs without heating for 5 minutes. The ease of dissolution is due to the relatively high acidity of the solution. After the sample is completely dissolved, 10 ml of concentrated Fe3 and 10 ml of HC1Cm, 3 drops of sodium diphenylamine sulfate are added to the solution and titrated with 0.04N. a solution of foCrsC, prepared from an exact weight of salt brand h.ch. Before each determination, the concentration of the Fe (Cl04) 2 solution is monitored.
Расчет количества активного кислорода (X) провод т по формулеThe calculation of the amount of active oxygen (X) is carried out according to the formula
Х X
М.аMA
2т - 16а 2t - 16a
где М - молекул рный вес соединени без учета активного кислорода (дл УВа2СизОб,.19), m - масса навески, г;where M is the molecular weight of the compound excluding active oxygen (for HCa2CizOb, .19), m is the mass of the sample, g;
а NK2Cr20 ( Vt - V2 ) 10 3 , где NK2Cr2O7 нормальность раствора бихромата кали ;and NK2Cr20 (Vt - V2) 10 3, where NK2Cr2O7 is the normality of the potassium dichromate solution;
Vi - обьем раствора бихромата кали , идущий на титрование 10 мл раствора хлорного железа; мл;Vi is the volume of potassium dichromate solution, used for titration of 10 ml of ferric chloride solution; ml;
/2 - объем раствора бихромата кали , идущий на титрование исследуемого раствора , мл./ 2 - the volume of potassium dichromate solution going to the titration of the test solution, ml.
Обьем, пошедший на титрование 10 мл раствора Fe(CI04)2 и NH4CI04 (после добавлени 10мл НСЮ4И 10мл НзРСч) составл ет ,3.The volume that went to the titration of 10 ml of a solution of Fe (CI04) 2 and NH4CI04 (after adding 10 ml of NSU4I 10 ml NsRSch) is 3.
В таблице приведены массы навесок образца , объемы растворов бихромата кали , пошедшего на титровани растворов хлорного железа, в которых растворены навески и расчитанный индекс X.The table shows the weights of the sample, the volume of solutions of potassium dichromate, followed by titration of solutions of ferric chloride, in which the weights are dissolved and the calculated index X.
Предлагаемый способ позвол ет определ ть индекс активного кислорода с погрешностью менее 2%, тогда как дл прототипа эта величина не менее 5%. Врем . затрачиваемое на проведение одного анализа , не более 10 мин, а дл прототипа необходимо 1-2 ч из-за значительной продолжительности растворени образца.The proposed method allows to determine the active oxygen index with an error of less than 2%, whereas for the prototype this value is not less than 5%. Time spent for carrying out one analysis, no more than 10 minutes, and for a prototype 1-2 hours are necessary because of the considerable duration of sample dissolution.
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Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU894686125A SU1647391A1 (en) | 1989-05-03 | 1989-05-03 | Method for determining active oxygen in superconducting copper -containing ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU894686125A SU1647391A1 (en) | 1989-05-03 | 1989-05-03 | Method for determining active oxygen in superconducting copper -containing ceramics |
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| Publication Number | Publication Date |
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| SU1647391A1 true SU1647391A1 (en) | 1991-05-07 |
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| Application Number | Title | Priority Date | Filing Date |
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| SU894686125A SU1647391A1 (en) | 1989-05-03 | 1989-05-03 | Method for determining active oxygen in superconducting copper -containing ceramics |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103472059A (en) * | 2013-09-30 | 2013-12-25 | 武汉钢铁(集团)公司 | Method for measuring total iron content in fly ash |
-
1989
- 1989-05-03 SU SU894686125A patent/SU1647391A1/en active
Non-Patent Citations (1)
| Title |
|---|
| Y. Saito, Т. Noji, К. Hirokava, A. Endo et al. Determination of valence of copper and oxygen deficiency in superconducting SrxLa2-xCu04-y-lpn. I.AppI Phys., 1987, v. 26, № 5, p. L838-839. * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103472059A (en) * | 2013-09-30 | 2013-12-25 | 武汉钢铁(集团)公司 | Method for measuring total iron content in fly ash |
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