CS201835B1 - Method of indirect concentrated radio-nuclide roentgen-ffluorescence analysis - Google Patents
Method of indirect concentrated radio-nuclide roentgen-ffluorescence analysis Download PDFInfo
- Publication number
- CS201835B1 CS201835B1 CS682378A CS682378A CS201835B1 CS 201835 B1 CS201835 B1 CS 201835B1 CS 682378 A CS682378 A CS 682378A CS 682378 A CS682378 A CS 682378A CS 201835 B1 CS201835 B1 CS 201835B1
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- CS
- Czechoslovakia
- Prior art keywords
- analysis
- radionuclide
- ray fluorescence
- nuclide
- indirect
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims description 14
- 238000004458 analytical method Methods 0.000 title claims description 12
- 238000004876 x-ray fluorescence Methods 0.000 claims description 9
- 239000003153 chemical reaction reagent Substances 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- NTYJJOPFIAHURM-UHFFFAOYSA-N Histamine Chemical compound NCCC1=CN=CN1 NTYJJOPFIAHURM-UHFFFAOYSA-N 0.000 claims description 4
- KWGRBVOPPLSCSI-WPRPVWTQSA-N (-)-ephedrine Chemical compound CN[C@@H](C)[C@H](O)C1=CC=CC=C1 KWGRBVOPPLSCSI-WPRPVWTQSA-N 0.000 claims description 2
- MBYXEBXZARTUSS-QLWBXOBMSA-N Emetamine Natural products O(C)c1c(OC)cc2c(c(C[C@@H]3[C@H](CC)CN4[C@H](c5c(cc(OC)c(OC)c5)CC4)C3)ncc2)c1 MBYXEBXZARTUSS-QLWBXOBMSA-N 0.000 claims description 2
- AUVVAXYIELKVAI-UHFFFAOYSA-N SJ000285215 Natural products N1CCC2=CC(OC)=C(OC)C=C2C1CC1CC2C3=CC(OC)=C(OC)C=C3CCN2CC1CC AUVVAXYIELKVAI-UHFFFAOYSA-N 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- KWGRBVOPPLSCSI-UHFFFAOYSA-N d-ephedrine Natural products CNC(C)C(O)C1=CC=CC=C1 KWGRBVOPPLSCSI-UHFFFAOYSA-N 0.000 claims description 2
- AUVVAXYIELKVAI-CKBKHPSWSA-N emetine Chemical compound N1CCC2=CC(OC)=C(OC)C=C2[C@H]1C[C@H]1C[C@H]2C3=CC(OC)=C(OC)C=C3CCN2C[C@@H]1CC AUVVAXYIELKVAI-CKBKHPSWSA-N 0.000 claims description 2
- 229960002694 emetine Drugs 0.000 claims description 2
- AUVVAXYIELKVAI-UWBTVBNJSA-N emetine Natural products N1CCC2=CC(OC)=C(OC)C=C2[C@H]1C[C@H]1C[C@H]2C3=CC(OC)=C(OC)C=C3CCN2C[C@H]1CC AUVVAXYIELKVAI-UWBTVBNJSA-N 0.000 claims description 2
- 229960002179 ephedrine Drugs 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 229960001340 histamine Drugs 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims description 2
- 238000002795 fluorescence method Methods 0.000 claims 1
- 239000002090 nanochannel Substances 0.000 claims 1
- 230000006641 stabilisation Effects 0.000 claims 1
- 238000011105 stabilization Methods 0.000 claims 1
- 238000004448 titration Methods 0.000 description 6
- 230000005855 radiation Effects 0.000 description 5
- 238000003556 assay Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000002285 radioactive effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- CGFYHILWFSGVJS-UHFFFAOYSA-N silicic acid;trioxotungsten Chemical compound O[Si](O)(O)O.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 CGFYHILWFSGVJS-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
Description
Vynález sa týká stanovenia anorganických i organických látok, ktoré po převedení do roztoku reagujú s odmerným činidlom za tvorby ťažko rozpustných, připadne málo disociovaných zlúčenin. Odmerný roztok alebo stanovovaná látka musí obsahovat prvky stanovitelné metodou rádionuklidovej róntgenofluorescenčnej analýzy. Po oddělení nerozpustného podielu chemickéj reakcie centrifugáciou alebo inou vhodnou separačnou technikou sa definovaný objem roztoku nanesie na nosič, ktorý tvoří napr. pruh chromatogňafického papiera, a obsah sa stanoví metodou rádionuklidovej róntgenofluorescenčnej analýzy buď priamo alebo nepriamo z nadbytku odmerného činidla metodou štandardnej analytickej křivky alebo porovnáním s vhodné zvoleným štandardom. Metoda umožňuje i stanovenie látky po jej izolácii zo zmesi látok chemickou reakciou s činidlom a možno ju využit i na určenie ekvivalenčného bodu pri zrážacích titráciách.The invention relates to the determination of inorganic and organic substances which, after being dissolved, react with a volumetric reagent to form poorly soluble or low-dissociated compounds. The volumetric solution or the substance to be examined shall contain elements determined by the method of radionuclide X-ray fluorescence analysis. After separation of the insoluble fraction of the chemical reaction by centrifugation or other suitable separation technique, a defined volume of the solution is applied to a carrier, e.g. the chromathogenic paper band, and the content is determined by a radionuclide X-ray fluorescence analysis method either directly or indirectly from an excess of the reagent, using a standard analytical curve method or by comparison with an appropriate standard of choice. The method also allows the determination of a substance after its isolation from a mixture of substances by chemical reaction with a reagent and can also be used to determine the equivalence point in precipitation titrations.
Dosial’ používané radiometrické titračné metody využívali meranie jednak radioaktivity jednotlivých zložiek vstupujúcich do reakcie, jednak boli vypracované ďalšie metody ako beta-odrazové titrácie, beta-absorpčné titrácie, rádiocoulometrické titrácie a titrácie za použitia rádioaktívnych kryptonátov. Nevýhodou týchto metod bola spotřeba velkého množstva vzorky, malá selektivita stanovenia i vyššia rizikovost práce, spojená s otvorenými zdrojmi rádioaktívneho žiarenia. Tieto nevýhody odstraňuje nepriamia koncentračná rádionuklidová rontgenofluorescenčná analýza, ktorej podstata spočívá v tom, že stanovená látka sa nechá chemicky reagovat s nadbytkom zodpovedajúceho činidla, ktorého nezreagované množstvo sa oddělí od reakčného produktu a stanoví rádionuklidovou róntgenofluorescenčnou analýzou v roztoku nanesenom na nosič, například papierový filter alebo sklenenú membránu.The radiometric titration methods used so far have utilized both the radioactivity measurement of the individual components of the reaction and other methods such as beta-reflection titration, beta-absorption titration, radiocoulometric titration and titration using radioactive cryptonate. The disadvantage of these methods was the consumption of large quantities of samples, low selectivity of the assay and higher risk of work associated with open sources of radioactive radiation. These disadvantages are overcome by indirect concentration radionuclide X-ray fluorescence analysis, which consists in allowing the substance to be chemically reacted with an excess of the corresponding reagent, the unreacted amount of which is separated from the reaction product and determined by a radionuclide X-ray fluorescence analysis glass membrane.
Výhodou navrhovanej metody je vysoká selektivita, vyplývajúca z vlastněj podstaty charakteristického žiarenia stanovovaného prvku, značená citlivost stanovenia, dobrá reprodukovatefnosť, malé množstvo vzorky potřebné k analýze. Stanovovanie je možné previest v množstve vzorky řádové desatiny ml i menšie. Na stanovenie sa nanáša 20 μϊ roztoku. Dosahovaná medza stanoviteTnosti opísanej metody je 10'6g látky. Na excitáciu charakteristického žiarenia sa používajú uzatvorené rádionuklidové zdroje nízkoenergetiokého gama alebo X žiarenia o aktivitě řádové desiatky mCi. Energia zvoleného rádionuklidového zdroj a musí byť o ňiečo váčšia ako je vazbová energia elektrónov na K, připadne L vrstvě. Vzniknuté charakteristické žiarenie, vysielané prvkom odmerného činidla alebo stanovovanej látky sa deteguje scintilačným alebo polovodičovým detektorom, napojeným na vyhodnooovaciu jednotku — jed201835 nokanálový, připadne mnohokanálový analyzátor.The advantage of the proposed method is the high selectivity resulting from the intrinsic nature of the characteristic radiation of the assay element, the labeled sensitivity of the assay, good reproducibility, the small amount of sample needed for analysis. The determination can be carried out in a sample amount of the order of tenths of ml or less. Apply 20 μϊ of solution for the determination. The achieved yield stanoviteTnosti-described method was 10 -6 g of the product. Enclosed radionuclide sources of low energy gamma or X radiation of the order of tens of mCi are used to excite characteristic radiation. The energy of the selected radionuclide source a must be somewhat greater than the binding energy of the electrons on the K or L layer. The characteristic radiation produced by the element of the measuring reagent or the analyte is detected by a scintillation or semiconductor detector connected to an evaluation unit - a poison 201835 or a multi-channel analyzer.
Príkladom použitia vo vynáleze opísanej metody je analýza ephedrinu, emetinu, histaminu, procairau pomocou kyseliny silikowolfrámovej alebo fosfomolybdénovej ako činidla. Metoda teda umožňuje rozšírenie rádionuklidovej róntgenofluorescenčnej analýzy i na stenovenie organických látok, pre ktoré nemožno použiť konvenčnú rádionuklidovú r óntgenof luoresceněnú metodu.An example of use of the method described in the invention is the analysis of ephedrin, emetine, histamine, procaira using silicotungstic acid or phosphomolybdenic acid as reagent. Thus, the method allows the extension of the radionuclide x-ray fluorescence analysis to the screening of organic substances for which the conventional radionuclide x-ray fluorescence method cannot be used.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS682378A CS201835B1 (en) | 1978-10-20 | 1978-10-20 | Method of indirect concentrated radio-nuclide roentgen-ffluorescence analysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS682378A CS201835B1 (en) | 1978-10-20 | 1978-10-20 | Method of indirect concentrated radio-nuclide roentgen-ffluorescence analysis |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CS201835B1 true CS201835B1 (en) | 1980-11-28 |
Family
ID=5416141
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS682378A CS201835B1 (en) | 1978-10-20 | 1978-10-20 | Method of indirect concentrated radio-nuclide roentgen-ffluorescence analysis |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS201835B1 (en) |
-
1978
- 1978-10-20 CS CS682378A patent/CS201835B1/en unknown
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