trace metal analysis - sigma-aldrich · ic, voltammetry, polarography. reagents and standards for...
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Improving trace metal analysis by dedicated analytical standards, CRMs and reagents
•Dr. Frank Michel, Markus Pfluger
sigma-aldrich.com
1)
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Buchs Site, Switzerland, Core Capabilities
500 employees
Automated milligram filling Chiral separation (SMB) GMP custom synthesis Microreaction synthesis Comprehensive analytical capabilities Production from microgram up to 1‘600 L
4,000 products produced
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Accreditation acc. to ISO/IEC 17025 & ISO Guide 34
GMP
q-NMR Titration ICP-OES Density
Qua
lity
ISO 9001IS
O17
025
Production of certified reference materials(high purity materials, high precision weighing)
TraceCERT© reference materialswww.sial.com/tracecert
TraceSELECT© high purity productswww.sial.com/traceselect
Systems & QC
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Physical data: mp, bp, n, d, viscosity, optical rotation etc. Titration: all kind of titrations, KF Spectroscopy: IR, NIR, UV, NMR (H,C,P,F), X-ray, luminescence Chromatography: GC, GC-MS, GC-HS, HPLC,GPC, TLC Hyphenated techniques: HPLC-MS (Ion Trap), UHPLC-MS (qToF), HPLC-NMR (600 MHz), Elemental analysis: C, H, N, S Biochemical analysis: MALDI-MS, CE, gel electrophoresis (IEF, SDS-PAGE, agarose
gels), enzyme activity, enzymatic content determination, determination of enzyme impurities, protein assay etc.
Trace analysis:AFSAAS (Flame, Graphite furnace with FI) ICP-OES (1x axial, 1x radial)ICP-MS (2x with reaction cell) Polarography, CVIC (2x anion / 1x cation)Wet chemistry
Analytical Expertise
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Releases of Mercury in the environment (man related) 1)
stationary combustion (coal-
fired power plants)
65%
non-ferrous metal production
7%
other5%
caustic soda production
3%waste disposal
3%cement production
6%
gold production 11%
Natural sources: Volcanoes, natural mercury deposits, volatilization from the ocean
1) Wikipedia
Mercury compounds are extremely toxic (heavy metal)Monitoring of Hg regulatory necessary (EPA, WHO, …)Chemicals used for ultra trace analyis must be low of Hg
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The Mercury Cycle
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WHO: Provisional tolerable weekly intake of Hg2µg/kg bodyweight per week (75kg 150µg/week)
WHO: Guideline Values (Total Mercury)< 1 µg/l Water
< 1 µg/m3 Air
< 30 µg/kg Food
< 500 µg/kg Fish
Instrument with lowest detection limits necessary
(specifications of ultra pure chemicals should be « 1 µg/kg)Ultra Pure Chemicals for analyis of Hg necessary
Analytical control of• air • foodstuff • drinking water
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Analytical techniques for determination of Hg
ICP-MS
CV-AAS
HydrEA(CV+GFAAS)
FAAS
CV-AFS
ICP-OES GFAAS
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Analytical techniques for determination of Hg
ICP-MS
CV-AAS
HydrEA(CV+GFAAS)
FAAS
CV-AFS
ICP-OES GFAAS
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Principles of Optical Spectroscopy
1)
1) G. Glomb, Schlemmer, Labatzke, Analytik Jena
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Choice of the right technique at Sigma-AldrichDesign Qualification Part I: Detection Limit [g/l]
ICP-MS
CV-AAS
HydrEA(CV+GFAAS)
FAAS
CV-AFS
ICP-OES GFAAS
150
1
0.005
0.01
0.030.1
0.001
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Choice of the right technique at Sigma-AldrichDesign Qualification Part II: instrument price [k€]
ICP-MS
CV-AAS
HydrEA(CV+GFAAS)
FAAS
CV-AFS
ICP-OES GFAAS
25
6050
30
150
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Choice of the right technique at Sigma-Aldrich Design Qualification Part III: different matrices
ICP-MS
CV-AAS
HydrEA(CV+GFAAS)
FAAS
CV-AFS
ICP-OES GFAAS
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Choice of the right technique at Sigma-AldrichDesign Qualification Part IV: dynamique range
ICP-MS
CV-AAS
HydrEA(CV+GFAAS)
FAAS
CV-AFS
ICP-OES GFAAS
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Choice of the right technique at Sigma-AldrichDesign Qualification Part IV: dynamique range
FAASCV-AAS
HydrEA(CV+GFAAS)
CV-AFS
GFAAS
1)
2)
1) 2) G. Schlemmer, Analytik Jena
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Choice of the right technique at Sigma-AldrichDesign Qualification Part IV: dynamique range
ICP-MS
CV-AAS
HydrEA(CV+GFAAS)
FAAS
CV-AFS
ICP-OES GFAAS
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Method of Choice for Sigma-Aldrich
CV-AFS
• budget not more than 25 k€ (additional capacity)
• low maintenance costs
• complex and varying matrices
• lowest detection limits necessary
• wide range of linearity
Existing methods (pharma customers)
CV-AAS
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Method of Choice for Sigma-Aldrich
CV-AFS
• budget not more than 25 k€ (additional capacity)
• low maintenance costs
• complex and varying matrices
• lowest detection limits necessary
• wide range of linearity
Existing methods (pharma customers)
CV-AAS
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Design Qualification: Assessment
Vendor Assessment:
• general tests (ease of operation, Software, …)
• Parameter tests (detection limit, drift, baseline)
• instrument tests with matrix (HNO3 65%, H2O230%, H2SO4 96%, H3PO4 85%, NaOH 30%, 1ppb solution in HNO3, NaBH4 with MSA)
•Financial aspects
•Service
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Decision after Assessment
Mercur DUO Plus® (Analytik Jena):
• Atomic fluorescence and atomic absorption
• Good results for instrument demonstration
• MSA available for NaBH4 application
• Low cost of purchase and maintainance
• Good service availability
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MERCUR DUO PLUS ®
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Mercur DUO Plus® and corresponding reagents
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TraceSELECT®Ultra <0.1 µg/kg (<0.1 ppb)
Metal Contaminations
TraceSELECT® <10 µg/kg (<10 ppb)
Hig
h P
urity
Rea
gent
s
puriss. p.a. <500 µg/kg (<500 ppb)
Highest Purity for successful analysis
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What TraceSELECT means for Trace Analysis
Accurate, fast and cost-effective analyses
Highest Purity and long term stability over 60 cation traces specified in the low ppt
(TraceSELECT Ultra) or ppb range (TraceSELECT) long shelf life with consistent purity due to high quality
fluoropolymer bottles
Comprehensive product range AAS (graphite furnace AAS, flame AAS, hydride AAS) ICP-OES, ICP-MS, LC-ICP-MS IC, Voltammetry, Polarography
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Reagents and Standards for the whole Analytical Process
Digestion reagents (acids, bases, salts)...for trace analysis (TraceSELECT®)...for ultra-trace analysis (TraceSELECT®Ultra)
Matrix modifiers, buffers, reducing agents for AASSolvents for LC-ICP-MS applicationsEluent concentrates for ICUltra pure reagents for Polarography
TraceCERT®
Certified Reference Materials
SamplePreparation
Calibration
Analysis
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Digestion reagents withultra-low blank values
purified by subboiling destillation
stored in high-quality fluoropolymer bottles
(...)
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...recommended products for Hg analysis
Brand Product Name Description Pack size
Fluka 44355 Tin(II) chloride TraceSELECT®, 99.999 % metals basis 250g, 2.5kg
Fluka 84415 Hydrochloric acid 37 %, TraceSELECT®, for trace analysis, fuming 100mL, 500mL
Fluka 84385 Nitric acid 69.0 %, TraceSELECT®, for trace analysis 250mL, 1 L
Fluka 95305 Water TraceSELECT®, for trace analysis 500mL, 1L, 2.5L, 10L
Fluka 90737 Potassium bromide TraceSELECT ®, >= 99.9995 % metals basis 50g
Fluka 60085 Potassium bromate puriss. p.a., ACS reagent, >= 99.8 % RT dried material 50g, 250g
Fluka 11514 Hydroxylamine hydrochloride TraceSELECT®, >= 99.9995 % metals basis 100g
Please find the complete product list at www.sigmaaldrich.com/traceselect
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...recommended products for Hg analysise.g. Nitric Acid
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...recommended products for Hg analysis calibration curve
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...selected TraceCERT products for calibration
Brand Product Name Description Pack size
Fluka 16482 Mercury Standard for AAS TraceCERT™, Hg 1000mg/L nitric acid 100mL
Fluka 28941 Mercury Standard for ICP Trace CERT™, Hg 1000mg/L nitric acid 100mL
If you can‘t find the right standard, visit our custom standard platform and design your own:www.sial.com/csp
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Brochures for Spectroscopy
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Dziękuję za uwagę!
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