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Reference Materials and

Analytical Quality Assurance -
a current view

Prof. Hendrik Emons
Unit for Reference Materials

RM Unit/HE/16 September 2003

conservation analytical sample preparation Matrix RM analyte identification quantitative measurement evaluation assessment RM Unit/HE/16 September 2003 . Total Analytical Process Problem Definition Quality Assurance sampling processing.

. . .. . .comparability of a defined method between laboratories x x x xx x x xxxxx xx x PRECISION RM Unit/HE/16 September 2003 . .. . . . . .lab-internal reproducibility (‘method stability’) . . . . . Reference Materials needed for (I) • assessment of an analytical (measurement) method . .

the assessment of a measurement method. ISO Guide 30 (1992) RM Unit/HE/16 September 2003 . or for assigning values to materials. Reference Material (RM) Material or substance one or more of whose property values are sufficiently homogeneous and well established to be used for the calibration of an apparatus.

g.material stable for the purpose .‘property value’ well established (e..material sufficiently homogeneous . RM Classification (I) Reference Materials Quality Control Materials (QCMs) Proficiency Testing Materials (PTMs) Prerequisites: . analyte concentration known) RM Unit/HE/16 September 2003 .

characterisation) selection Homogeneity Storage Processing Interim transport Material study and storage collection Stability study Characterisation Value Assignment RM Use (and Distribution) Follow-up stability monitoring of RM RM Unit/HE/16 September 2003 . processing. Procedure for RM Production Material Feasibility study Planning (collection.

Reference Materials needed for (II) • assessment of an analytical (measurement) method xxxxx xx xxxxxxx x TRUENESS with CRMs RM Unit/HE/16 September 2003 .

2 µg/g with uncertainty • stated traceability RM Unit/HE/16 September 2003 .3 ± 0. RM Classification (II) Reference Materials QCMs Certified Reference Materials (CRMs) (PTMs) additional features: • certificate Pb in mussel tissue • certified value 8.

and for which each certified value is accompanied by an uncertainty at a stated level of confidence. accompanied by a certificate. one or more of whose property values are certified by a procedure which establishes its traceability to an accurate realization of the unit in which the property values are expressed. ISO Guide 30 (1992) RM Unit/HE/16 September 2003 . Certified Reference Material (CRM) Reference material.

Reference Materials from IRMM Environmental. ‘Industrial’ CRMs RM Unit/HE/16 September 2003 . Clinical. Food. Feed.

processing. characterisation) selection Homogeneity Storage Processing Interim transport Material study and storage collection Short-term Long-term Interlaboratory Value Assignment stability study stability study Characterisation (Certification) Follow-up stability Assessment Documentation monitoring of CRM by experts CRM Distribution and Sales RM Unit/HE/16 September 2003 . Procedure for CRM Production Material Feasibility study Planning (collection.

characterisation) selection Homogeneity Storage Processing Interim transport Material study and storage collection Short-term Long-term Interlaboratory Value Assignment stability study stability study Characterisation (Certification) Follow-up stability Assessment Documentation monitoring of CRM by experts CRM Distribution and Sales uncertainty contributions RM Unit/HE/16 September 2003 . processing. Procedure for CRM Production Material Feasibility study Planning (collection.

Chemical Characterisation Strategies: • multi-method approaches in interlaboratory study (with truly independent methods.but non-existing for matrix materials) • single method in interlaboratory study (for chemically non-defined measurands) • single method in one laboratory (not for certification) RM Unit/HE/16 September 2003 . “expert” labs) • multi-method approach in one lab (including a “primary” method .

Types of Measurands Elements (atoms) Molecules/chemical species method-specific parameters: such as N (Kjeldahl). dietary fibre. moisture & volatiles in rapeseed metals by sequential extraction Dynamic Parameters mobility reactivity extractability enzyme activity (of Pb species from soil A) immunological activity RM Unit/HE/16 September 2003 .

comparable analyte Material concentration digestion analyt.Control Materials in Element Analysis deep-frozen homogenized subsamples (internal) QCM: Quality Control Material . determination RM Unit/HE/16 September 2003 .identical processing Certified Reference .identical matrix freeze- drying .

conservation analytical sample preparation Matrix RM analyte identification brant Cali- quantitative measurement evaluation assessment RM Unit/HE/16 September 2003 . Total Analytical Process Problem Definition Quality Assurance sampling processing.

Reference Materials needed for (III) • calibration of an apparatus pure calibrants: 6000 As(V) A for methods AB 5000 DMA ‘without’ 4000 matrix influence Intensität / cps AC 3000 Tetra TMAO 2000 1000 0 0 100 200 300 400 500 600 700 800 900 matrix CRMs: Retentionszeit / min for methods with signal analytical value matrix influence (XRF.…) RM Unit/HE/16 September 2003 . SS-ET-AAS.

Global comparability. Quality and traceability of analytical results SI units Analytical International (field) Reference materials Measuring internat. PTMs) (Metrology) standards System Local comparability. accepted laboratories (CRMs. accepted everywhere” Traceability RM Unit/HE/16 September 2003 . Intergovernmental Mutual Precision Trueness Recognition Arrangement “once measured.