Determination of palladium and platinum trace content in wastes and tailings of chemical industry

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DETERMINATION OF PALLADIUM

AND PLATINUM TRACE CONTENT IN

WASTES AND TAILINGS OF

CHEMICAL INDUSTRY

Institute of Nuclear Physics,

Institute of Nuclear Physics, Uzbekistan Academy of Science,Uzbekistan Academy of Science, Tashkent

Tashkent

Laboratory Activation analysis of pure materials Laboratory Activation analysis of pure materials

I

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Objective

:

_:



Development of high-sensitivity

techniques for radiochemical

neutron activation determination

of palladium and platinum in a

wastes and

slimes

_slimes

of the chemical

_{of the chemical}

industry

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Conditions and characteristics of

techniques

Pd

m_sam = 150 mg, t_irr = 10 h, f = 1014 neut.sm2/s.

Analytical radionuclide

109Pd (T

1/2 = 13.5 h)

( 9 gamma-lines 40-780 keV)

Pt

m_sam = 150 mg, t_irr = 10 h, f = 1014_neut.sm2_/s.

Analytical radionuclide

197_{Pt (T}

1/2 = 20 h)

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Distribution coefficient of Pd and Pt in the

Dowex

Dowex--1 1 -- H HClCl andand Н Н₃₃РОРО₄₄ ion exchange systemion exchange system

Ions Concentration of HCl Concentration of H₃PO₄

1,2 М 3 М 6 М 9 М 12 М 1 М 3 М 5 М 7 М 12 М Pd(II) 1300 500 120 50 32 800 690 730 540 350 Pd(IV) 1600 350 80 55 33

Pt(II) 104 5000 2800 710 480

Pt(IV) 104 ₃₆₀₀ _{1900 870} ₄₃₀ _{3000 3000} ₃₀₀₀ _{1400 460}

 From HCl Dowex-1 except Pd and Pt are absorbes about From HCl Dowex-1 except Pd and Pt are absorbes about

15, from H

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Distribution coefficient of Pd and Pt in the

Dowex

Dowex-_-1 ₁-_- HNO_HNO₃₃ ion exchange_{ion exchange}system_system Element Concentration HNO₃

0,1 М 1 М 5 М 10 М 14 М

Pd 35 100 60 10 6

Pt 500 150 80 10

--- Except Pd and PtExcept Pd and Pt are absorbed Au, Re and Hgare absorbed Au, Re and Hg. .

 Distribution coefficient of more than 25 elements less Distribution coefficient of more than 25 elements less

1, and of more than 10 elements less than 5

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Eluation curve of the impurity elements in the

system of Dowex-1 - 1 M HNO

system of Dowex-1 - 1 M HNO₃₃

5 10 15 20 25 30 35 40 0 0.2 0.4 0.6

/

A_i A₀ V, ml

Ba, K, Na, Cs, Cd, Ga, Ir, Mn; Ag, Cr, Ni(Co), Cu, Zn, Fe, Sb; As, In, Se, Te, Sc, U, Th, La-Lu;

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Distribution profile of

Distribution profile of Pt_Pt (1) and _{(1) and}Pd_Pd (2) on the _{(2) on the}

chromatographic column. h= 5 sm, d = 0,5 sm chromatographic column. h= 5 sm, d = 0,5 sm 0.5 1.0 1.5 2.0 2.5 3.0 0 0.05 0.10 0.15 0.20 2 1 L, см

/

A_i A₀

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Procedure of analysis

The 150 mg of sample together with standards of Pd The 150 mg of sample together with standards of Pd

and Pt was irradiated in the channel of WWR-SM

reactor for 10 h. In a day after irradiation the sample

was dissolved in HCl+HNO

was dissolved in HCl+HNO₃₃ (3:1). The obtained (3:1). The obtained

solution was evaporated to damp salts, the residue was

dissolved in 1M HNO

dissolved in 1M HNO3₃ and transferred into and transferred into

chromatographic column filled with Dowex-1. Then

matrix elements were eluated from column with 25-30

ml of 1M HNO

ml of 1M HNO3₃. The Dowex-1 was transferred into the . The Dowex-1 was transferred into the

bottle for counting and

bottle for counting and -activity of Pd and Pt was -activity of Pd and Pt was

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The measuring equipment

 Gamma-spectrometer consisting from HPGe Gamma-spectrometer consisting from HPGe

the detector (efficiency 20 %, resolution 1,7 keV

for 1332,5 keV

for 1332,5 keV 6060Co) and multichannel analyzer Co) and multichannel analyzer

InSpector-1000 (Canberra, USA).

 Spectra processed with use of software package Spectra processed with use of software package

Genie-2000.

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Conclusion

 On the basis of the carried out investigations, On the basis of the carried out investigations,

RNAA techniques for determination of trace

contents of Pd and Pt in a industrial wastes and

tailings of chemical industries were developed

tailings of chemical industries were developed. .

These techniques are based on ion exchange

chromatographic concentration of Pd and Pt.

 LD 1.10LD 1.10-5-5 % for Pd and 2.10 % for Pd and 2.10-4-4 % mass for Pt. % mass for Pt. S

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Determination of palladium and platinum trace content in wastes and tailings of chemical industry

Objective

Objective

:

_:

Development of high-sensitivity

Development of high-sensitivity

techniques for radiochemical

techniques for radiochemical

neutron activation determination

neutron activation determination

of palladium and platinum in a

of palladium and platinum in a

wastes and

wastes and

slimes

_slimes

of the chemical

_{of the chemical}

industry

Conditions and characteristics of

Conditions and characteristics of

techniques

techniques

/

/

Procedure of analysis

Procedure of analysis

The measuring equipment

The measuring equipment

Conclusion

Conclusion

Thank you for your

Thank you for your

attention!