Abstract
A technique for analysis of surfacing materials (cast cobalt-based carbide alloys) using by ICP-AES in combination with microwave autoclave sample preparation is developed. Composition of the acid mixture, temperature and time parameters of the sample preparation under microwave heating in an autoclave are specified, thus ensuring complete quantitative transfer of the sample into a convenient analytical form without losses of volatile components for the subsequent ICP-AES analysis. Analytic lines of the elements free from spectral interference were chosen to determine all the rated components in the casting materials from cast carbide alloys. Study of surfacing materials was carried out using alloys Pr-B3K-PrH-U10Kh63B5, Pr-B3K-P-PrN-U20Kh57B10 and TsN-2-E-190K62X29B5C2, containing the alloying elements (% wt.): Co (up to 65); Cr (28.0 – 32.0); W (4.0 – 11.0); Si (1.0 to 3.0); C (1.0 – 2.0); Ni (0.1 – 2.0); Mn (0.3 – 0.6) and Fe (up to 2.0). The correctness of determining rated element was confirmed in analysis of standard samples using sample weight variation. The developed technique was tested on industrial prototypes of surfacing materials made of cobalt-based cast carbide alloys of tested grades. The method is rapid (11-fold reduction in the time of analysis) and reagent-saving (by 12.5 times) procedure compared to single-element methods by 11 times and reduction of the volume of applied reagents. Combination of the multielement ICP-AES method with microwave sample preparation provides an increase in the accuracy of Si, Cr, Mn, Fe, Ni, and W determination in surfacing materials of cast carbide alloys within a range of rated concentrations.
Highlights
Ðàçðàáîòàíà ìåòîäèêà àíàëèçà íàïëàâî÷íûõ ìàòåðèàëîâ èç ëèòûõ òâåðäûõ ñïëàâîâ íà îñíîâå êîáàëüòà ìåòîäîì àòîìíî-ýìèññèîííîé ñïåêòðîìåòðèè ñ èíäóêòèâíî-ñâÿçàííîé ïëàçìîé (ÀÝÑ-ÈÑÏ) â ñî÷åòàíèè ñ ìèêðîâîëíîâîé àâòîêëàâíîé ïðîáîïîäãîòîâêîé
Îáîñíîâàíû ñîñòàâ êèñëîòíîé ñìåñè è òåìïåðàòóðíî-âðåìåííûå ïàðàìåòðû ïðîáîïîäãîòîâêè â óñëîâèÿõ ìèêðîâîëíîâîãî íàãðåâà â àâòîêëàâå, îáåñïå÷èâàþùèå êîëè÷åñòâåííîå ïåðåâåäåíèå ïðîáû â óäîáíóþ àíàëèòè÷åñêóþ ôîðìó áåç ïîòåðü ëåòó÷èõ êîìïîíåíòîâ äëÿ ïîñëåäóþùåãî ÀÝÑ-ÈÑÏ àíàëèçà
The developed technique was tested on industrial prototypes of surfacing materials made of cobalt-based cast carbide alloys of tested grades
Summary
© Àëåêñàíäð Âàëåðüåâè÷ Âÿ÷åñëàâîâ, Âàëåðèÿ Âàëåðüåâíà Öåïêîâà, Àííà Äåíèñîâíà Òèòîâà, Òàòüÿíà Íèêîëàåâíà Åðìîëàåâà. Ðàçðàáîòàíà ìåòîäèêà àíàëèçà íàïëàâî÷íûõ ìàòåðèàëîâ èç ëèòûõ òâåðäûõ ñïëàâîâ íà îñíîâå êîáàëüòà ìåòîäîì àòîìíî-ýìèññèîííîé ñïåêòðîìåòðèè ñ èíäóêòèâíî-ñâÿçàííîé ïëàçìîé (ÀÝÑ-ÈÑÏ) â ñî÷åòàíèè ñ ìèêðîâîëíîâîé àâòîêëàâíîé ïðîáîïîäãîòîâêîé. Îáîñíîâàíû ñîñòàâ êèñëîòíîé ñìåñè è òåìïåðàòóðíî-âðåìåííûå ïàðàìåòðû ïðîáîïîäãîòîâêè â óñëîâèÿõ ìèêðîâîëíîâîãî íàãðåâà â àâòîêëàâå, îáåñïå÷èâàþùèå êîëè÷åñòâåííîå ïåðåâåäåíèå ïðîáû â óäîáíóþ àíàëèòè÷åñêóþ ôîðìó áåç ïîòåðü ëåòó÷èõ êîìïîíåíòîâ äëÿ ïîñëåäóþùåãî ÀÝÑ-ÈÑÏ àíàëèçà. A technique for analysis of surfacing materials (cast cobalt-based carbide alloys) using by ICP-AES in combination with microwave autoclave sample preparation is developed. Äëÿ ðàñòâîðåíèÿ òðóäíîðàñòâîðèìûõ êàðáèäîâ è ñèëèöèäîâ õðîìà è âîëüôðàìà â ñîñòàâ ðåàêöèîííîé ñìåñè [13] áûëî ðåêîìåíäîâàíî âêëþ÷àòü ñëåäóþùèå êèñëîòû: HF, HNO3 è HCl. Ïðèñóòñòâèå â ñìåñè HF ñâÿçàíî ñ åå ñïîñîáíîñòüþ â ïðèñóòñòâèè îêèñëèòåëÿ îáåñïå÷èâàòü ïåðåâåäåíèå â ðàñòâîð êàðáèäîâ è ñèëèöèäîâ Cr è W è óäåðæèâàòü â ðàñòâîðå âîëüôðàì çà ñ÷åò ðåàêöèé êîìïëåêñîîáðàçîâàíèÿ, ïðåäóïðåæäàÿ âûïàäåíèå â îñàäîê âîëüôðàìîâîé êèñëîòû; HNO3 õîðîøî ðàñòâîðÿåò Mn, Fe, Co è Ni, à HCl — Cr. Âûáîð ñîñòàâà ðåàêöèîííîé ñìåñè è òåìïåðàòóðíî-âðåìåííîãî ðåæèìà, îáåñïå÷èâàþùèõ ïîëíîå ðàçëîæåíèå èññëåäóåìûõ ïðîá ÍÌ, îñóùåñòâëÿëè ýêñïåðèìåíòàëüíî ïðè íåïðåðûâíîì íàãðåâå äî òåìïåðàòóð 140, 170 è 220 °C, ïîëíîòó ðàçëîæåíèÿ êîíòðîëèðîâàëè âèçóàëüíî. Óñëîâèÿ îïðåäåëåíèÿ Si, Cr, Mn, Fe, Ni, W â ÍÌ ìåòîäîì ÀÝÑ-ÈÑÏ
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