CS232133B1 - Electrochemical determination of sulphidity admixtures on fracture plates of steels - Google Patents
Electrochemical determination of sulphidity admixtures on fracture plates of steels Download PDFInfo
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- CS232133B1 CS232133B1 CS833642A CS364283A CS232133B1 CS 232133 B1 CS232133 B1 CS 232133B1 CS 833642 A CS833642 A CS 833642A CS 364283 A CS364283 A CS 364283A CS 232133 B1 CS232133 B1 CS 232133B1
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- fracture
- amount
- steels
- steel
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- 229910000831 Steel Inorganic materials 0.000 title claims description 16
- 239000010959 steel Substances 0.000 title claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 4
- 230000010287 polarization Effects 0.000 claims description 4
- 238000011835 investigation Methods 0.000 claims description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 2
- 229910052753 mercury Inorganic materials 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 claims 1
- 150000003568 thioethers Chemical class 0.000 claims 1
- 239000000243 solution Substances 0.000 description 15
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 6
- 238000002848 electrochemical method Methods 0.000 description 6
- 229910052709 silver Inorganic materials 0.000 description 6
- 239000004332 silver Substances 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 3
- 239000005337 ground glass Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000011144 upstream manufacturing Methods 0.000 description 2
- 238000004832 voltammetry Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000004922 lacquer Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000000399 orthopedic effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- 238000009865 steel metallurgy Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- CADICXFYUNYKGD-UHFFFAOYSA-N sulfanylidenemanganese Chemical compound [Mn]=S CADICXFYUNYKGD-UHFFFAOYSA-N 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 125000000101 thioether group Chemical group 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
Landscapes
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
Description
Vynález sa týká elektrochemického sposobu určenia množstva sulfidických vtrúsenín na lomových plochách ocelí pre vyhodno-tenie fraktograři-ckých skúšck ocelových vzoriek.The invention relates to an electrochemical method for determining the amount of sulphide inclusions on fracture surfaces of steels for the evaluation of fracture testing of steel samples.
Doteraz sa množstvo sulfidických vtrús-ento na tamovej ploché oceli (ocelověj vzorky) stanovuje pomocou mikroskopického obrazu mulej časti lomovej plochy, získaného napr. použitím rastiOvacieho- elektronového mikroskopu, určením plošného p-odielu obrazu týchto vtrúsenín z celkovej plochy zobrazenej časti lomovej plochy.Until now, the amount of sulfide injection on the flat steel there (the steel sample) is determined by microscopic image of a small portion of the fracture surface obtained e.g. using a growth-electron microscope, determining the area p-image of these inclusions from the total area of the fracture surface portion shown.
Nevýhodou doterajšieh-o sposobu určenia množstva sulildických vtrúsenín na lomovej ploché je jednak to, že plošný podiel supluje hmotnostnú koocentráciu, jednak aj to, že tento údaj sa potom extrapoluje z plochy mikuQSinímky na celú plochu lomu. Tým .je takto určené množstvo zatažené výraznou chybou. Ani použitie elektró,navěj mikrosondy alebo e-nergiovo-disperznej analýzy nepředstavuje zásadné přesnější postup.A disadvantage of the prior art method for determining the amount of sulildic inclusions on a fracture flat is that the surface area substitutes for mass co-concentration, and that this data is then extrapolated from the area of the microscope to the entire fracture area. Thus, the amount thus determined is affected by a significant error. Neither the use of electrons, in particular microsondes, or energy-dispersive analysis, is a fundamentally more precise procedure.
Obidva uvedené nedostatky odstraňuje vynález elektrochemického sposobu určenia množstva sulfidických vtrúsenín na lomových plochách oceli. Podstata tohto vynálezu spočívá; v .tom, žc, sudíldické vtrúse.niny, kitoiré sú tvořené predioivžetkým sulfidom mcnganatým, na povrchu lomu kovu sa rozpustia v roztoku zvíedenej kyseliny chlorovodíkové), pričom ale kov je zároveň aj výrazné katodicky polarizovaný.Both of these drawbacks are overcome by the invention of the electrochemical method of determining the amount of sulfide inclusions on fracture surfaces of steel. The essence of the present invention lies; in that the sudiddic inclusions, which consist of predominantly all manganese sulphide, dissolve on the surface of the metal in a solution of dilute hydrochloric acid), but the metal is also strongly cathodically polarized.
Elektrody tom je uvedený -roztok kyseliny a anodou je nějaký iný vhodný kov, napr. striebro. Za týchto podmienok sa kovová matrica vyšetřované) lomovej plochy nerozpúšťa, dochádza iba k vývinu vodíka elektrolytickým rozkládám roztoku kyseliny chlorovodíkové]' a mikrokvant sirovodíka chemickým rozkladom sulfidických vtrúsenín. Celý proces prebieha v inertnom a-naerobnom prostředí, vytvára-nom prúdoim argonu, ktorý unáša vzniklý sirovodík do roztoku hydroxidu sodného, kde dochádza k jeho kvantitativnému zachyteniu a finálnemu analytickému určeniu pomocou metody rozpúšťacej voltammetrie s použitím stacioinárinej ortuťoveij kvapkiovej elektrody.The electrode is said acid solution and the anode is any other suitable metal, e.g. silver. Under these conditions, the metal matrix of the fracture surface under investigation does not dissolve, only hydrogen evolution occurs through the electrolytic decomposition of the hydrochloric acid solution and the hydrogen sulfide microcquant by chemical decomposition of the sulfide inclusions. The whole process takes place in an inert and a-naerobic environment, generated by a stream of argon, which carries the hydrogen sulphide formed into the sodium hydroxide solution, where it is quantitatively captured and final analytically determined using a solution voltammetric method using a stationary mercury droplet electrode.
Vynález elektrochemického sposobu určenia množstva sulfidických vtrúsenín na lomioivej plocho oceli je podlá převedeného vyhladania odborinej a patentovej literatúry prvým sposobom umožňujúcim skutočne kvantitativné určenie úhrnného množstva sulfidov obsiahnntých na lomovej ploché oceli, pričom dosiahnutá přesnost je naj-menej +10 % výsledného množstva alebo lepšie. Tým vynález umožňuje podstatné pre-snejšie merať a hodnotit účinky sulfidických vtrúsenín na lámavosť ocelí.The invention of the electrochemical method for determining the amount of sulfide inclusions on a fracture flat steel is based on the prior art search and patent literature first method allowing a truly quantitative determination of the total amount of sulfides contained on a fracture flat steel, with better or less than + 10% accuracy. Thus, the invention makes it possible to measure and evaluate the effects of sulfide interactions on the brittleness of steel substantially more accurately.
Na připojenou! obrázku je znázorněná používaná experimentálna skleněná -aparatúra pre elektrochemický sposob určenia množstva sulfidických vtrúsenín na lomových plochách oceli:On connected! The figure shows the experimental glassware used for the electrochemical method of determining the amount of sulphide inclusions on fracture surfaces of steel:
Vo- vyvíjacej nádobko A sa vkládá lomová vzorka upevněná na silnom oceíovom drote prestrčeniom gumovou zátkou tesne uzatvárajúcou hrdlo- postranného tubusu nádobky. Do nádobky ústi skloněnou fritou ukonč-ený vývod vedlajsieho (anodického) priestoru 2 so- zábrusovým hrdlom prc· vloženie strieb-ornej elektrody 3 upevnenej tiež v gumo-vej zátfce. Trubkou 4 sa privádza do nádobky inertný plyn. Na dno nádobky sa vkládá miešadielko .pre magnetickú miešačku, umiestnenú pod vyvíjaclou nádobkou. Vyvijncia nádobka je hoře ukončená zábrusovým vývodom 5, pre nástavec 6, ktorý je spojený hadičkou 7 (z m-akčeného P7C] s přívodovou trubkou 8 ústiacou skleněnou fritou v zúžeuej časti eloktroanalytickej nádobky B.A fracture specimen, mounted on a thick steel wire, is inserted into the development vessel A by inserting a rubber stopper tightly closing the neck side tube of the vessel. The outlet of the adjacent (anodic) space 2 with a ground-glass throat opens into the container by an inclined frit, and the silver electrode 3 is also mounted in the rubber stopper. An inert gas is fed into the vessel through tube 4. A stirrer is placed on the bottom of the container for the magnetic stirrer located below the developing container. The developing vessel is terminated at the top with a ground joint 5, for the extension 6, which is connected by a hose 7 (of m-actuated P7C) to the inlet pipe 8 through a glass frit in the narrowed portion of the electroanalytical vessel B.
Táto nádobka má v hornéj časti záhrusové hrdla pre vlioižeinfie Indikačmej (<stacionárně j, ortufovej, kvapkovej) elektrody 9, referentnej elektrody 10, a nádobky vedla; šleho priestoiru 11, ukončeného trubkou so zábrusqm a skleněnou fritou a zhora zábrusom pre vkládanie -str-iebornej anody 12. Na dno nádobky B sa opat vloží miešadielk-o pre magnetickú miosačku umiestnenú pod nádobkou.The receptacle has at its top a cone throat for the location of the indicator (<stationary, orthogonal, droplet) electrode 9, the reference electrode 10, and the receptacle overhead; The bottom part of the vessel 11 is terminated with a ground glass tube and a glass frit and a ground joint for inserting a silver anode 12. A magnetic stirrer stirrer is placed at the bottom of the vessel B under the vessel.
Okrem skleněněj apuratúry je na obrázku schematicky naznačené pripojenie potřebných prístrojov — zdroja Z rovnosmeirného prúdu p e vyvijaciu elektrolýzu a 3-elektródového polarografu P pre finálnu rozpúštaciu voltammetrickú analýzu.In addition to the glass apparatus, the diagram shows the schematic connection of the necessary devices - a source of equidirectional current for the development of electrolysis and a 3-electrode polarograph P for the final dissolution voltammetric analysis.
Na obrázku nie sú znázorněné obidve magnetické miešačky, preimývačky pre plyn s vodou, ktoré sú zairadené před nrívodaú trubku 4 a za vývod 13.The figure does not show both magnetic stirrers, gas-water scrubbers, which are connected upstream of the inlet pipe 4 and the outlet 13.
Vlastný postup elektrochemického sposobu určenia množstva sulfidických vtrúsonln na lomových plochách ocelí je objasněný ďalej na příklade 1.The actual procedure of the electrochemical method for determining the amount of sulphide in the fracture surfaces of steels is explained below in Example 1.
Příklad 1Example 1
Analyzovaná lemová vzorka sa -najskor mechanicky upraví tak, aby jej dížka nepřesahovala 8—10 mm (počínajúc od lomovej plochy), připevní sa k ocelovému, 1—2 mm silnému a asi 12—15 cm dlhému drotu prostrčenému gumovou zátkou. Vzdialenoisf zátky od vzorky sa upraví tak, aby vzorka sa nachádzala asi 10 mm odo dna vyvíjacej nádobky, ak gumová zátka tesne uzaviera zábirus-ové hrdlo postranného tubusu nádobky. Potom sa vzorka nalakuje rýchloacbmúcim vodovzdorným lakom okrem vyšetro.vanej lomovej plochy a lak sa nechá dobře zaschnúť po dobu dvoch hodin.The edge sample to be analyzed is mechanically adjusted so that its length does not exceed 8-10 mm (starting from the fracture surface), attached to a steel 1-2 mm thick and about 12-15 cm long wire pierced with a rubber stopper. The distance from the sample stopper is adjusted so that the sample is located about 10 mm from the bottom of the developing container when the rubber stopper tightly closes the side-neck of the container side tube. The sample is then varnished with a quick-absorbing waterproof varnish in addition to the investigated fracture surface and allowed to dry well for two hours.
Anodický priestor vyvíjacej nádobky sa celkom naplní roztokom kyseliny chtonovodíkovej (1 M), vloží sa doňho strieboriná elektroda a pevne uzatvorí.The anodic chamber of the developing vessel is completely filled with hydrochloric acid solution (1 M), a silver electrode is inserted into it and tightly sealed.
Do vlastného priestoru vyvíjacej nádobky sa naleje cca 40 ml roztoku 2 M HC1, vloží sa doňho- malé magnetické miešadielko a na horný vývod nádobky sa nasadí zábrusový nástavec s PVC - hadičkou, ktorej druhý kioiniec je spojený s prívodnou trubicau elektneanalytickej nádobky. Vyvíjací a nádobka sa umlestni na plotnu elektromagnetickej mieš-ačky a upevní na laboratórmom stojane.About 40 ml of 2 M HCl solution is poured into the tank, a magnetic stirrer is inserted into it and a ground joint with a PVC tube is attached to the upper outlet of the vessel. The second tube is connected to the inlet tube of the electro-analytical vessel. Place the developing and container on the plate of the electromagnetic mixer and attach it to the laboratory rack.
Do elektrioanalytickej nádobky sa -odmerá presne 50 ml roztoku 2 M NaOH, vhodí sa magnetické miešadielko, vloží sa do příslušných zébrusových otvorov ireferentna elektroda, ďalej nádobka vedlajšieho -priestoiru naplněná r-oztokiom 0,1 M NaOH s upevnenou strieborno-u anodou, a namiesto indikačnej elektrody sa příslušný tubus těsna uzjatvnrí zábrusovou zátkou. Celá nádobka sa umiest-i na platňu magnetickej miešač< ky a upevní sa na stojane.Exactly 50 ml of 2 M NaOH solution is metered into the electrioanalytic vessel, the magnetic stirrer is discarded, an irreferent electrode is inserted into the respective serrated holes, a secondary vessel filled with a 0.1 M NaOH solution fixed with a silver anode, and instead of the indicating electrode, the respective tube is tightly closed with a ground-glass stopper. The entire container is placed on a magnetic stirrer plate and mounted on a rack.
Za vývod plynov sa připojí gumovou hadičkou premývačka pre plyn s vodou, drua há premývačka sa připojí před prívodnú trubku před vyvíjaciu nádobku.A gas-water scrubber is connected downstream of the gas outlet, and a second scrubber is connected upstream of the feed pipe before the feed vessel.
Celá zostavená aparatura sa potom dokladné odvzdušní živým prúdom čistého argonu po dobu aspoň 30 minút. Upravená lomová vzorka, po zaschnutí laku a odvzdušnení aparatúry, sa vloží postranným tubusom do roztoku kyseliny vo vyvíjacej nádobke a gumová zátka nosiča vzorky sa tesne upevní v hrdle tubusu. Vyčnievajúca časť drótu nosiča sa vodivo spojí s katodickým vývodom zdroja rovnosmerného prúdu, strieborná anoda sa spojí s jeho anodickým vývodom a na elektrodová dvojicu sa odvětví elektrické nápátie 1,5 až 2 V. Prúd inertného plynu sa přitom nepřeruší a ponechá ďalej prechádzať mierným prúdom. 0bidva roztoky, vyvíjací kyslý aj absorbujúci alkalický sa behom analýzy intenzívně miešajú magnetickými miešadielkami.The entire assembled apparatus is then evacuated with a live stream of pure argon for at least 30 minutes. The treated fracture specimen, after the lacquer has dried and the apparatus has been vented, is inserted through the side tube into the acid solution in the developing vessel, and the rubber stopper of the sample carrier is tightly fitted in the neck of the tube. The protruding portion of the carrier wire is conductively coupled to the cathodic outlet of the direct current source, the silver anode is coupled to its anodic outlet, and a 1.5 to 2 volt electrical patch sector is applied to the electrode pair while the inert gas flow is not interrupted. Both acidic and alkaline absorbing solutions are vigorously stirred with magnetic stirrers during analysis.
Pokus sa nechá prebiehať po dobu 2 hodin. Potom sa zastaví miešanie roztokov, do elektroanalytíckej nádobky sa vloží indikačná elektroda, preruší sa prietok plynu a vykoná sa finálně určenie množstva absorbovaného sírovodíka v roztoku alkalického hydroxidu metodou rozpúšťacej voltammetrie.The experiment is allowed to proceed for 2 hours. Stirring of the solutions is then stopped, an indicator electrode is inserted into the electroanalytic vessel, the gas flow is interrupted and the amount of absorbed hydrogen sulfide in the alkaline hydroxide solution is finally determined by the solution voltammetric method.
Potom sa v pokuse pokračuje po dobu 30 minút a prevedie sa dalšia analýza, po pr. aj ešte sa viackrát opakuje pokial' hodnota velikosti voilitiamimetriLcikiej vlny neinaid-obudn-e, svojej maximálnej a konštantnej hodnoty. Podmienky finálnej rozpúšťacej voltammetrickej analýzy sa doporučujú (v zhode s literárnymi prameňmlj: elektrodový potenciál zhromaždovacej fázy —0,30 V až —0,50 voltov, doba zhromaždovacej fázy 50 sekund až 5 minút, potenciálové rozmedzie spatnej polarizácie a registrácie kriviek —0,3 (—0,5) V až —1,0 V pri rýchlosti polarizácie 5 V/min. Každá voltammetrická křivka sa registruje na novej ortufovej kvapke.The experiment is then continued for 30 minutes and further analysis is performed, after pr. it is repeated several times as long as the value of the neilidic wave size of its maximum and constant value. Final dissolution voltammetric analysis conditions are recommended (in accordance with literary sources: pool electrode potential of –0,30 V to –0,50 volts, pool phase time of 50 seconds to 5 minutes, potential polarization polarization potential and curve registration –0,3 (00.5) V to 11.0 V at a polarization rate of 5 V / min Each voltammetric curve is registered on a new orthopedic drop.
Kalibrácia metody sa vykoná pomocou roztokov sulfidu sodného (tiež připravených za anaerobných podmienok a najskór faktorizovaných jódometrickyj. Zo získanéj kalibračnej závislosti sa potom odčítá množstvo zachyteného sírovodíka a tým aj množstvo rozpuštěných sulfidov na vyšetrovanej lomovej ploché.The calibration of the method is carried out using sodium sulphide solutions (also prepared under anaerobic conditions and most iodometrically scored).
Elektrochemický spósob určenia množstva sulfidických vtrúsenín na lomových plochách je možné využit v skúšobníctve hutnického priemyslu ako aj vo výskumných a vývojových laboratóriach zabývajúcich sa problematikou metalurgie železa a oceli.Electrochemical method of determination of amount of sulphide inclusions on quarry surfaces can be used in testing of metallurgical industry as well as in research and development laboratories dealing with problems of iron and steel metallurgy.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS833642A CS232133B1 (en) | 1983-05-23 | 1983-05-23 | Electrochemical determination of sulphidity admixtures on fracture plates of steels |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS833642A CS232133B1 (en) | 1983-05-23 | 1983-05-23 | Electrochemical determination of sulphidity admixtures on fracture plates of steels |
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| Publication Number | Publication Date |
|---|---|
| CS364283A1 CS364283A1 (en) | 1984-05-14 |
| CS232133B1 true CS232133B1 (en) | 1985-01-16 |
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| CS833642A CS232133B1 (en) | 1983-05-23 | 1983-05-23 | Electrochemical determination of sulphidity admixtures on fracture plates of steels |
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| CS364283A1 (en) | 1984-05-14 |
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