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Primary methods Primary methods Primary methods Primary methods Determination of the analyte mass concentration in single element water calibration solutions Martin Vlasák, Zuzana Luxemburková, Václav Sychra www.analytika.net www.analytika.net ; ; [email protected] [email protected] Analytika ® spol. s r.o., Ke Klíčovu 2a/816, 190 00 Praha 9

Primary methods - Analytika

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Page 1: Primary methods - Analytika

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

Gravimetric preparation of water calibration solutionsand analyte mass concentration determination

Page 3: Primary methods - Analytika

Sodium calibration solution in 2% (v/v) nitric acid(Kragten spreadsheet)

Page 4: Primary methods - Analytika

Antimony calibration solution in 1%HF+5%HNO3 (v/v)

Page 5: Primary methods - Analytika

Bismut standard solution in 2% (v/v) nitric acid

Page 6: Primary methods - Analytika

Chelatometric (complexometric) determinations

Page 7: Primary methods - Analytika

Chelatometric (complexometric) determinationsHuge amount of single element calibration solutions

Page 8: Primary methods - Analytika

Other titrimetric determinationsAlkalimetry, argentometry, manganometry, bromatometry

Page 9: Primary methods - Analytika

Alkali metals calibration solutionsDetermination in the form of alkali metal sulfates

Page 10: Primary methods - Analytika

Gold in 5% (v/v) hydrochloric acid solutionDetermination using hydroquinone reduction

Page 11: Primary methods - Analytika

Baryum in 2% (v/v) nitric acid solutionDetermination in the form of baryum chromate

Page 12: Primary methods - Analytika

Niobium in 1% (v/v) HF and 5% HNO3 (v/v) solutionDetermination using cupferron as precipitating agent

Page 13: Primary methods - Analytika

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

Nitrate, perrhenate and wolframate in water solutionDetermination using nitrone as precipitating agent

Page 15: Primary methods - Analytika

Ta and Ti in 1% (v/v) HF and 5% HNO3 (v/v) solutionDetermination using ammonia solution hydrolysis

Page 16: Primary methods - Analytika

Standard calibration solutions analysed

Page 17: Primary methods - Analytika

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

Literature

Page 19: Primary methods - Analytika

Acknowledgement