primary methods - analytika
TRANSCRIPT
![Page 1: Primary methods - Analytika](https://reader031.vdocuments.pub/reader031/viewer/2022021713/620b67a1be201a3bab332c4d/html5/thumbnails/1.jpg)
Primary methodsPrimary methodsPrimary methodsPrimary methodsDetermination of the analyte
mass concentrationin single element water calibration solutions
Martin Vlasák, Zuzana Luxemburková, Václav Sychra
www.analytika.netwww.analytika.net;; [email protected]@analytika.net
Analytika® spol. s r.o., Ke Klíčovu 2a/816, 190 00 Praha 9
![Page 2: Primary methods - Analytika](https://reader031.vdocuments.pub/reader031/viewer/2022021713/620b67a1be201a3bab332c4d/html5/thumbnails/2.jpg)
Gravimetric preparation of water calibration solutionsand analyte mass concentration determination
![Page 3: Primary methods - Analytika](https://reader031.vdocuments.pub/reader031/viewer/2022021713/620b67a1be201a3bab332c4d/html5/thumbnails/3.jpg)
Sodium calibration solution in 2% (v/v) nitric acid(Kragten spreadsheet)
![Page 4: Primary methods - Analytika](https://reader031.vdocuments.pub/reader031/viewer/2022021713/620b67a1be201a3bab332c4d/html5/thumbnails/4.jpg)
Antimony calibration solution in 1%HF+5%HNO3 (v/v)
![Page 5: Primary methods - Analytika](https://reader031.vdocuments.pub/reader031/viewer/2022021713/620b67a1be201a3bab332c4d/html5/thumbnails/5.jpg)
Bismut standard solution in 2% (v/v) nitric acid
![Page 6: Primary methods - Analytika](https://reader031.vdocuments.pub/reader031/viewer/2022021713/620b67a1be201a3bab332c4d/html5/thumbnails/6.jpg)
Chelatometric (complexometric) determinations
![Page 7: Primary methods - Analytika](https://reader031.vdocuments.pub/reader031/viewer/2022021713/620b67a1be201a3bab332c4d/html5/thumbnails/7.jpg)
Chelatometric (complexometric) determinationsHuge amount of single element calibration solutions
![Page 8: Primary methods - Analytika](https://reader031.vdocuments.pub/reader031/viewer/2022021713/620b67a1be201a3bab332c4d/html5/thumbnails/8.jpg)
Other titrimetric determinationsAlkalimetry, argentometry, manganometry, bromatometry
![Page 9: Primary methods - Analytika](https://reader031.vdocuments.pub/reader031/viewer/2022021713/620b67a1be201a3bab332c4d/html5/thumbnails/9.jpg)
Alkali metals calibration solutionsDetermination in the form of alkali metal sulfates
![Page 10: Primary methods - Analytika](https://reader031.vdocuments.pub/reader031/viewer/2022021713/620b67a1be201a3bab332c4d/html5/thumbnails/10.jpg)
Gold in 5% (v/v) hydrochloric acid solutionDetermination using hydroquinone reduction
![Page 11: Primary methods - Analytika](https://reader031.vdocuments.pub/reader031/viewer/2022021713/620b67a1be201a3bab332c4d/html5/thumbnails/11.jpg)
Baryum in 2% (v/v) nitric acid solutionDetermination in the form of baryum chromate
![Page 12: Primary methods - Analytika](https://reader031.vdocuments.pub/reader031/viewer/2022021713/620b67a1be201a3bab332c4d/html5/thumbnails/12.jpg)
Niobium in 1% (v/v) HF and 5% HNO3 (v/v) solutionDetermination using cupferron as precipitating agent
![Page 13: Primary methods - Analytika](https://reader031.vdocuments.pub/reader031/viewer/2022021713/620b67a1be201a3bab332c4d/html5/thumbnails/13.jpg)
Ni in 2% (v/v) HNO3 and Pd in 5% (v/v) HCl solutionDetermination using dimethylglyoxime as precipitant
Ni2++
N
N
OH
OH
2OH
-
N
N
Ni2+
N
N
O O
O O
H
H
+ 2H+
![Page 14: Primary methods - Analytika](https://reader031.vdocuments.pub/reader031/viewer/2022021713/620b67a1be201a3bab332c4d/html5/thumbnails/14.jpg)
Nitrate, perrhenate and wolframate in water solutionDetermination using nitrone as precipitating agent
![Page 15: Primary methods - Analytika](https://reader031.vdocuments.pub/reader031/viewer/2022021713/620b67a1be201a3bab332c4d/html5/thumbnails/15.jpg)
Ta and Ti in 1% (v/v) HF and 5% HNO3 (v/v) solutionDetermination using ammonia solution hydrolysis
![Page 16: Primary methods - Analytika](https://reader031.vdocuments.pub/reader031/viewer/2022021713/620b67a1be201a3bab332c4d/html5/thumbnails/16.jpg)
Standard calibration solutions analysed
![Page 17: Primary methods - Analytika](https://reader031.vdocuments.pub/reader031/viewer/2022021713/620b67a1be201a3bab332c4d/html5/thumbnails/17.jpg)
Conclusion
� primary methods (gravimetry and titrimetry)
are capable for the determination of a nominal
value of the analyte mass concentration with
acceptable uncertainty below 0,2% (rel.)
� metrological compatibility between analyte
mass concentration value found and certified
was for more than 60 solutions fulfilled
![Page 18: Primary methods - Analytika](https://reader031.vdocuments.pub/reader031/viewer/2022021713/620b67a1be201a3bab332c4d/html5/thumbnails/18.jpg)
Literature
![Page 19: Primary methods - Analytika](https://reader031.vdocuments.pub/reader031/viewer/2022021713/620b67a1be201a3bab332c4d/html5/thumbnails/19.jpg)
Acknowledgement