steffen full from anode slime to dore part1.ppt - lbma · the lbma assaying & refining seminar,...

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The LBMA Assaying & Refining Seminar, 24-25 March 2009 1 Norddeutsche Affinerie Group From Anode slime to silver doré From Anode slime to silver-doré Production control by XRF D Michael Steffen Dr. Michael Steffen Norddeutsche Affinerie AG, Hamburg, Germany Aurubis AG, Hamburg, Germany 1 Production 1. Production 2. XRF analysis 3. Basics for XRF

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Page 1: Steffen FULL from anode slime to dore part1.ppt - LBMA · The LBMA Assaying & Refining Seminar, 24-25 March 2009 1 Norddeutsche Affinerie Group From Anode slime to silverFrom Anode

The LBMA Assaying & Refining Seminar, 24-25 March 2009 1

Norddeutsche Affinerie Group

From Anode slime to silver doréFrom Anode slime to silver-doré

Production control by XRF

D Michael SteffenDr. Michael Steffen

Norddeutsche Affinerie AG, Hamburg, Germany

Aurubis AG, Hamburg, Germany

1 Production1. Production

2. XRF analysis

3. Basics for XRF

Page 2: Steffen FULL from anode slime to dore part1.ppt - LBMA · The LBMA Assaying & Refining Seminar, 24-25 March 2009 1 Norddeutsche Affinerie Group From Anode slime to silverFrom Anode

The LBMA Assaying & Refining Seminar, 24-25 March 2009 2

1 Production1. Production

2. XRF analysis

3. Basics for XRF

AurubisOne of the largest copper smelter and refiner produce ca. 1 Mio. t g pp pKupfercathodes from copper concentrates, copper scrap and copper containing residues

Silver (ca. 1000 t) and Gold (ca. 30 t) from PM containing slimes, sweep and fines, computer scrap and PM alloys.

Anode slime (product from electrolytic refining of copper cathodes), is one of the most important source for precious metals production.p

At Aurubis anode slimes are treated in a modern Boliden top blown rotary converter (TBRC) process in two routes and fully controlled by XRF

Page 3: Steffen FULL from anode slime to dore part1.ppt - LBMA · The LBMA Assaying & Refining Seminar, 24-25 March 2009 1 Norddeutsche Affinerie Group From Anode slime to silverFrom Anode

The LBMA Assaying & Refining Seminar, 24-25 March 2009 3

Production line 1 (Detail)

Copper line Roasting, smelting, converting to metal

phase PbO, SeO2, slag

TBRC 1

Raw material

Anode slime, Cu-rich ( ~20 % PM)

PM-dross (~ 2 % PM)Ag-Doré (~ 92 % PM)

PbO

R t i l

silver anode

Ag-Doré (~ 98 % PM)

Raw material

Rich bullion ( ~ 70 % PM)

TBRC 2

Cupellation processTo analyse by XRF

PM = Ag, Au, Pt, Pd, Rh, Ir, Ru

Impurities = Pb, As, Sb, Se, Sn,

Te, Bi, Ni, Cu, Cl

Production line 2 (Detail)

Lead lineZnPbAg-crust

ZnPbAgAlloy (~25 % PM)

Electric furnace

Lead refining

Raw material

Anode slime, Cu-poor (~ 7 % PM)

Cu/Pb-matte ( ~ 0,3 % PM)

Pb-concentrate (~ 0,01 % PM)

Bullion (~ 4 % PM)

Rich bullion (~ 70 % PM)

PbO

Ag-Doré (~ 98 % PM)Silver anode

To analyse by XRF

PM = Ag, Au, Pt, Pd, Rh, Ir, Ru

Impurities = Pb, As, Sb, Se, Sn,

Te, Bi, Ni, Cu, Cl

TBRC 2

Cupellation process

Page 4: Steffen FULL from anode slime to dore part1.ppt - LBMA · The LBMA Assaying & Refining Seminar, 24-25 March 2009 1 Norddeutsche Affinerie Group From Anode slime to silverFrom Anode

The LBMA Assaying & Refining Seminar, 24-25 March 2009 4

Production lines

Copper line

Anode slime Ag-Doré

TBRC 1 TBRS 2Silver anode

Lead line

Electric furnace

Lead refining

Silver tankhouse

Silver ingots

Anode slime

Playground for OES

1 Production1. Production

2. XRF analysis

3. Basics for XRF

Page 5: Steffen FULL from anode slime to dore part1.ppt - LBMA · The LBMA Assaying & Refining Seminar, 24-25 March 2009 1 Norddeutsche Affinerie Group From Anode slime to silverFrom Anode

The LBMA Assaying & Refining Seminar, 24-25 March 2009 5

Sample preparation

Delivering by

pneumatic post

preparation milling sieving

Weighing,

mixing with fluxdecompositionpressingReady for analysis

XRF-Analysis

QS check by monitor sample XRF analysis

Metall sample

decomposed, milled, pressed with binder

Direct pressed

Page 6: Steffen FULL from anode slime to dore part1.ppt - LBMA · The LBMA Assaying & Refining Seminar, 24-25 March 2009 1 Norddeutsche Affinerie Group From Anode slime to silverFrom Anode

The LBMA Assaying & Refining Seminar, 24-25 March 2009 6

1 Production1. Production

2. XRF analysis

3. Basics for XRF

Basics for XRF analysis

XRF mashines are stupid

They look only intensities

Page 7: Steffen FULL from anode slime to dore part1.ppt - LBMA · The LBMA Assaying & Refining Seminar, 24-25 March 2009 1 Norddeutsche Affinerie Group From Anode slime to silverFrom Anode

The LBMA Assaying & Refining Seminar, 24-25 March 2009 7

Basics for XRF analysis

reference essential !!!

Reference samples /

Calibration samples

available on the marked ? calibration calculation of functionally

dependence

create by yourself

or

Collecting from the production

analysing all elements >0,1 %,

influence of the intensities by attenuation

if not sufficient

Example: Determination of Ag in Ag-DoréCalibration ranges

Ag: 0,01 - 100 %

Au: 0,01 - 20,0 %

Pt : 0,002 - 1,0 %

Pd: 0,002 - 2,0 %

Rh: 0,002 - 0,5 %

Ir : 0,001 - 0,4 %

Bi : 0,01 - 5,0 %

Cu: 0,01 - 10,0 %

Pb: 0,01 - 30,0 %

Sb: 0,001 - 0.5 %

Se: 0,001 - 5,0 %

Ru: 0,002 - 0,5 % Te : 0,001 - 6,0 %

Conclusion

Determination of Ag in Ag-Doré will be interact by 12 elements.

Calibration range will be made by 64 calibration samples.

Calculation of α-correction only for Ag will be made by 38 calibration samples.

Page 8: Steffen FULL from anode slime to dore part1.ppt - LBMA · The LBMA Assaying & Refining Seminar, 24-25 March 2009 1 Norddeutsche Affinerie Group From Anode slime to silverFrom Anode

The LBMA Assaying & Refining Seminar, 24-25 March 2009 8

Example: Determination of Ag in Ag-DoréCalibration range without α−correction

Example: Determination of Ag in Ag-DoréCalibration range after α-correction

Page 9: Steffen FULL from anode slime to dore part1.ppt - LBMA · The LBMA Assaying & Refining Seminar, 24-25 March 2009 1 Norddeutsche Affinerie Group From Anode slime to silverFrom Anode

The LBMA Assaying & Refining Seminar, 24-25 March 2009 9

Basic for correct analysis

Only possible with motivated, well skilled employees