RU2086961C1 - Method of photometric determination of cobalt - Google Patents
Method of photometric determination of cobalt Download PDFInfo
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- RU2086961C1 RU2086961C1 RU95108530A RU95108530A RU2086961C1 RU 2086961 C1 RU2086961 C1 RU 2086961C1 RU 95108530 A RU95108530 A RU 95108530A RU 95108530 A RU95108530 A RU 95108530A RU 2086961 C1 RU2086961 C1 RU 2086961C1
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- Prior art keywords
- cobalt
- solution
- determination
- quinolinazo
- nickel
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- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 15
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 14
- 239000010941 cobalt Substances 0.000 title claims abstract description 14
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 7
- 238000010521 absorption reaction Methods 0.000 claims abstract description 3
- -1 citric Chemical compound 0.000 claims abstract 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 11
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052721 tungsten Inorganic materials 0.000 abstract description 7
- 239000010937 tungsten Substances 0.000 abstract description 7
- 229910052759 nickel Inorganic materials 0.000 abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 abstract description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 abstract description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 abstract description 2
- 239000008139 complexing agent Substances 0.000 abstract description 2
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 2
- 239000011733 molybdenum Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
- 150000003870 salicylic acids Chemical class 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 7
- 239000012141 concentrate Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000010668 complexation reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- RJNYNDHYSJRRDW-UHFFFAOYSA-N 4-(pyridin-2-yldiazenyl)benzene-1,3-diol Chemical compound OC1=CC(O)=CC=C1N=NC1=CC=CC=N1 RJNYNDHYSJRRDW-UHFFFAOYSA-N 0.000 description 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000009918 complex formation Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000011089 mechanical engineering Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- OVARTBFNCCXQKS-UHFFFAOYSA-N propan-2-one;hydrate Chemical compound O.CC(C)=O OVARTBFNCCXQKS-UHFFFAOYSA-N 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
Изобретение относится к области аналитической химии, в частности к фотометрическим методам и может быть использовано для определения кобальта в различных объектах технологического производства. The invention relates to the field of analytical chemistry, in particular to photometric methods and can be used to determine cobalt in various objects of technological production.
Известен способ определения кобальта [1] Способ заключается в том, что кобальт переводят в окрашенное комплексное соединение, а фотометрирование ведут в 0,58-0,79 M растворе фосфорной кислоты при концентрации 4-(2-пиридилазо)-резорцина 1,0-1,1•10-3 M в присутствии катализатора железа при его концентрации 0,9-3,6•10-4 M.A known method for the determination of cobalt [1] the Method consists in the fact that cobalt is converted into a colored complex compound, and photometry is carried out in a 0.58-0.79 M solution of phosphoric acid at a concentration of 4- (2-pyridylazo) -
Известен также способ одновременного спектрофотометрического определения никеля и кобальта [2]
Для определения используют в качестве аналитического реагента 1,3,5,7-третрафенил-1,5-диазо-3,7-дифосфациклооктан, который в кислой водно-ацетоновой среде образует окрашенное комплексное соединение с солями никеля.There is also a method of simultaneous spectrophotometric determination of Nickel and cobalt [2]
For determination, 1,3,5,7-tertraphenyl-1,5-diazo-3,7-diphosphacyclooctane is used as an analytical reagent, which forms a colored complex with nickel salts in an acidic water-acetone environment.
Наиболее близким является метод определения кобальта [3] который состоит в том, что кобальт переводят в комплексное соединение с нитрозо-P-солью и определение проводят при pH 8,0. Молярный коэффициент светопоглощения ε15000 при l520 нм. The closest is the method for determination of cobalt [3] which consists in the fact that cobalt is converted into a complex compound with a nitroso-P salt and the determination is carried out at pH 8.0. The molar coefficient of light absorption ε15000 at l520 nm.
Недостатками всех известных способов является то, что многие ионы мешают определению: Fe (III), Mn, Zn, Co, Pb, Sn (IV), часто приходится проводить предварительное разделение, чтобы избежать осаждения гидроксидов различных металлов, определение ведут в цитратной среде. The disadvantages of all known methods is that many ions interfere with the determination of: Fe (III), Mn, Zn, Co, Pb, Sn (IV), often it is necessary to carry out preliminary separation in order to avoid the precipitation of hydroxides of various metals, the determination is carried out in a citrate medium.
Метод трудоемок и требует больших затрат времени, малоспецифичен. Мешают окислители и восстановители, включая железо (II). The method is time-consuming and time-consuming, not very specific. Oxidizing agents and reducing agents, including iron (II), interfere.
Предлагаемый способ фотометрического определения кобальта позволяет определять малые количества кобальта в присутствии больших содержаний никеля, вольфрама, молибдена и многих комплексообразователей: лимонная, винная, аскорбиновая, салициловая кислоты, тиомочевина в сильнокислой среде. The proposed method for photometric determination of cobalt allows to determine small amounts of cobalt in the presence of high contents of nickel, tungsten, molybdenum and many complexing agents: citric, tartaric, ascorbic, salicylic acid, thiourea in a strongly acidic environment.
Сущность метода заключается в том, что в качестве цветореагента используют хинолиназо P, при этом обработку проводят при pH 1, а фотометрируют раствор в области полосы поглощения с максимумом при 590 нм без предварительного отделения основы. Изучение реакции комплексообразования никеля с хинолиназо P показало на различие оптимальных условий по сравнению с кобальтом (табл.1). The essence of the method is that quinolinazo P is used as a color reagent, while the treatment is carried out at
Далее проводили определение кобальта в различных образцах (сталях, вольфрамовых концентратах). Next, cobalt was determined in various samples (steels, tungsten concentrates).
Структурная формула хинолиназо P представлена в следующем виде:
Состав вольфрамового концентрата приведен в табл.2.The structural formula of quinolinazo P is as follows:
The composition of the tungsten concentrate is given in table.2.
Использование в качестве органического реагента хинолиназо-P и то, что определение ведут при значениях pH 1,0, способствует повышению избирательности, точности и экспрессности анализа. The use of quinolinazo-P as an organic reagent and the fact that the determination is carried out at pH 1.0 helps to increase the selectivity, accuracy and expressness of the analysis.
Не мешают комплексообразованию большие содержания никеля, вольфрама. High nickel and tungsten contents do not interfere with complex formation.
Метод освобождается от лишних операций, таких как отделение, кипячение. The method is freed from unnecessary operations, such as separation, boiling.
Пример. Example.
I. Реактивы: KOH, BK8 концентрат вольфрамовый, H2O дистиллированная, хинолиназо-P 1•10-3 M, стандартный раствор Co C=1•10-3 M.I. Reagents: KOH, BK 8 tungsten concentrate, H 2 O distilled, quinolinazo-P 1 • 10 -3 M, standard solution Co C = 1 • 10 -3 M.
II. Ход определения. Переводят пробу в раствор щелочной обработкой. 3 г KOH помещают в тигель и расплавляют на плитке, дают остыть. Добавляют навеску концентрата m= 1г, закрывают крышкой и нагревают до 800oC в муфели и прокаливают в течение 1 ч. Охлаждают, затем заливают горячей водой. Образец переводят в колбу на 100 мл и доводят до метки дистиллированной водой.II. The course of determination. Transfer the sample to the solution by alkaline treatment. 3 g of KOH are placed in a crucible and melted on a tile, allowed to cool. A portion of the concentrate m = 1 g was added, closed with a lid and heated to 800 ° C in muffles and calcined for 1 hour. Cool, then pour hot water. The sample is transferred to a 100 ml flask and adjusted to the mark with distilled water.
Для анализа отбирают аликвоты раствора в колбу на 100 мл и туда же вводят 3 мл 1•10-3 M раствора хинолиназо-P и создают pH 1,0 раствором соляной кислоты (1:1). Снимают оптическую плотность на фотометре ФЭК-56М при λ590 нм относительно раствора сравнения. Полученные данные контролируют методом добавок.Aliquots of the solution are taken for analysis into a 100 ml flask and 3 ml of 1 • 10 -3 M quinolinazo-P solution are added thereto and a pH of 1.0 is created with a hydrochloric acid solution (1: 1). Optical density is removed on an FEK-56M photometer at λ590 nm relative to the comparison solution. The data obtained is controlled by the additive method.
Полученные результаты приведены в табл.3. The results are shown in table.3.
Различие в значениях pH комплексообразования и lMeRNi и Co с хинолиназо-P позволяет определять кобальт в никелевых сплавах, вольфрамовых концентратах.The difference in pH values of complexation and l MeR Ni and Co with quinolinazo-P makes it possible to determine cobalt in nickel alloys and tungsten concentrates.
Предлагаемый способ можно успешно применить в области металлургии, приборостроения, судостроения, машиностроения, химической промышленности, медицины, а также в пищевой промышленности. The proposed method can be successfully applied in the field of metallurgy, instrumentation, shipbuilding, mechanical engineering, chemical industry, medicine, as well as in the food industry.
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Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| RU95108530A RU2086961C1 (en) | 1995-05-25 | 1995-05-25 | Method of photometric determination of cobalt |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| RU95108530A RU2086961C1 (en) | 1995-05-25 | 1995-05-25 | Method of photometric determination of cobalt |
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| Publication Number | Publication Date |
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| RU95108530A RU95108530A (en) | 1997-02-20 |
| RU2086961C1 true RU2086961C1 (en) | 1997-08-10 |
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| RU95108530A RU2086961C1 (en) | 1995-05-25 | 1995-05-25 | Method of photometric determination of cobalt |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2163372C1 (en) * | 1999-06-15 | 2001-02-20 | Чувашский государственный университет им. И.Н. Ульянова | Kinetic method for assessing copper and cobalt simultaneously present in media |
| RU2267778C1 (en) * | 2004-11-17 | 2006-01-10 | Красноярский государственный университет | Indicator composition for determination of cobalt (ii) in aqueous solution |
-
1995
- 1995-05-25 RU RU95108530A patent/RU2086961C1/en active
Non-Patent Citations (1)
| Title |
|---|
| 1. Авторское свидетельство СССР N 1276984, кл. G 01 N 21/78, 1986. 2. Авторское свидетельство СССР N 1451593, кл. G 01 N 31/22, 1989. 3. ГОСТ 15934. 11 - 80. Концентраты медные. Методы определения кобальта. * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2163372C1 (en) * | 1999-06-15 | 2001-02-20 | Чувашский государственный университет им. И.Н. Ульянова | Kinetic method for assessing copper and cobalt simultaneously present in media |
| RU2267778C1 (en) * | 2004-11-17 | 2006-01-10 | Красноярский государственный университет | Indicator composition for determination of cobalt (ii) in aqueous solution |
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| Publication number | Publication date |
|---|---|
| RU95108530A (en) | 1997-02-20 |
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