Zirconium crucible for melting analytical sample, method of preparing analytical sample and method of analysis
View Patent ↗Proposed is a zirconium crucible used for melting an analytical sample in the pretreatment of the analytical sample, wherein the purity of the zirconium crucible is 99.99 wt % or higher. In light of the recent analytical technology demanded of fast and accurate measurement of high purity materials, the present invention provides a zirconium crucible for melting an analytical sample, a method of preparing such analytical sample, and a method of analysis that enables the analysis of high purity materials by inhibiting the inclusion of impurities from the crucible regardless of difference in the analysts and their skill.
1. A zirconium crucible utilized for melting an analytical sample in the pretreatment of the analytical sample, wherein the zirconium crucible consists of zirconium metal having a purity of 99.99 wt % or higher.
2. The zirconium crucible utilized for melting an analytical sample according to claim 1 , wherein the melting of the analytical sample is performed by using a basic flux comprising one or more types of alkali chemicals selected from Na 2 CO 3 , K 2 CO 3 , H 3 BO 3 , NaOH, KOH, Na 2 B 2 O 7 , and Li 2 B 2 O 7 , or said basic flux added with one or more types of oxidizing agents selected from Na 2 O, Na 2 O 2 , K 2 O, K 2 O 2 , KNO 3 , and KClO 3 , or one or more types of acid flux selected from Na 2 S 2 O 7 , K 2 S 2 O 7 , and NaHSO 4 .
3. A zirconium crucible according to claim 1 , wherein said zirconium crucible provides lower limits of quantification for each of Mn, Al, Si, Mg, Co, Ti, Cu, Mo, Fe, Cr, W, Pb, and Ni of 10 wtppm or less.
4. A method of treating an analytical sample using a high purity zirconium crucible, including a step of preliminarily melting the analytical sample in a zirconium crucible to obtain the analytical sample, the zirconium crucible consisting of zirconium metal having a purity of 99.99 wt % or higher.
5. The method of treating an analytical sample according to claim 4 , further including steps of weighing and placing the analytical sample in the crucible, and during said preliminary melting step, melting the analytical sample using a basic flux comprising one or more types of alkali chemicals selected from Na 2 CO 3 , K 2 CO 3 , H 3 BO 3 , NaOH, KOH, Na 2 B 2 O 7 , and Li 2 B 2 O 7 , or said basic flux added with one or more types of oxidizing agents selected from Na 2 O, Na 2 O 2 , K 2 O, K 2 O 2 , KNO 3 , and KClO 3 , or one or more types of acid flux selected from Na 2 S 2 O 7 , K 2 S 2 O 7 , and NaHSO 4 .
6. A method according to claim 4 , further comprising the step of analyzing the analytical sample as melted during said preliminary melting step with lower limits of quantification for each of Mn, Al, Si, Mg, Co, Ti, Cu, Mo, Fe, Cr, W, Pb, and Ni of 10 wtppm or less.
7. A method of analysis, including the steps of melting an analytical sample by using a zirconium crucible consisting of zirconium metal having a purity of 99.99 wt % or higher, and performing analyses with the analytical sample melted during said melting step to obtain analytical results, in which lower limits of quantification for each of Mn, Al, Si, Mg, Co, Ti, Cu, Mo, Fe, Cr, W, Pb, and Ni is 10 wtppm or less.