MAPS. Scheme Description. Malt Analytes Proficiency Testing Scheme

Transcription

1 MAPS Malt Analytes Proficiency Testing Scheme Scheme Description LGC Standards Proficiency Testing Chamberhall Business Park Chamberhall Green Bury Lancashire BL9 0AP United Kingdom Telephone: +44 (0) Fax: +44 (0) ptcustomerservices@lgcgroup.com Website Issue: 9 Page of 7 Issue date: September 08

2 Record of issue status and modifications ISSUE ISSUE DATE DETAILS AUTHORISED BY Sept 03 Details for sample 3 updated. Methods for FAN and EBC reject fraction updated for 04. W.Gaunt Jan 04 Assigned value text updated. Methods updated for various parameters for 04. W.Gaunt 3 Aug 04 Methods updated for various parameters. W.Gaunt 4 Sep 04 SDPA updated for colour in sample 4. Inclusion of subcontracting information in Test Materials section. W.Gaunt 5 Sep 05 6 Sept 06 7 Sept 07 8 Oct 07 Black and crystal malt separated (now 4A and 4B) Removed Hard copy report information. Details updated for TSN (EBC & IOB) and EBC fermentability IOB fermentability (unboiled 0.) and IOB fermentability (boiled) removed for 08. Kjeldahl and Dumas methods for Kolbach index deleted and replaced with Calculation. Total UV digestion added to TSN (EBC Wort) & TSN (IoB wort). SDPA for EBC fermentability reduced to.0. New samples added for high DP (6) and malted wheat (7). Analytes amended for samples 6 and 7. Methods updated for Beta glucan (EBC & IOB) W.Gaunt A.McCarthy W.Gaunt W.Gaunt W.Gaunt 9 Sep 08 Analyte clarification for 0.mm and FAN in malted wheat W.Gaunt Notes: Where this document has been translated, the English version shall remain the definitive version Issue: 9 Page of 7 Issue date: September 08

3 Scheme Aims and Organisation The primary aim of the Malt Analytes Proficiency Testing Scheme (MAPS) is to enable laboratories performing the analysis of malt and barley to monitor their performance and compare it with that of their peers. MAPS also aims to provide information to participants on technical issues and methodologies relating to testing of malt and barley. The MAPS scheme year operates from January to December. Further information about MAPS, including test material availability, round despatch dates and reporting deadlines, are available on the current MAPS application form. Test Materials Details of test materials available in MAPS are given in Appendix A. The test parameters are continually reviewed to ensure they meet the needs of current laboratory testing and regulatory requirements. Test material batches are tested for homogeneity for at least one test parameter where deemed appropriate. Details of homogeneity tests performed and results are given in the MAPS Scheme Reports. Some aspects of the scheme, such as test material production, homogeneity testing and stability assessment, can from time to time be subcontracted. When subcontracting occurs, it is placed with a competent subcontractor and LGC is responsible for this work. The planning of the scheme, the evaluation of performance and the authorisation of the final report will never be subcontracted. Statistical Analysis Information on the statistics used in MAPS can be found in the General Protocol and in the Scheme Report. Methods for determining assigned values and the values for SDPA used for individual samples are given in Appendix A Methods Methods are listed in PORTAL. Please select the most appropriate method from the list. If none of the methods are appropriate, then please report your method as Other and record a brief description in the Comments Section in PORTAL. Results and Reports MAPS results are returned through our electronic reporting software, PORTAL, full instructions for which are provided by . However, participants may request result submission forms on which to report and return results if they are unable to report through electronic means. This will incur an additional charge. MAPS reports will be available on the website within 0 working days of round closure. Participants will be ed a link to the report when it is available. Issue: 9 Page 3 of 7 Issue date: September 08

4 APPENDIX A - Description of abbreviations used Assigned Value (AV) - The assigned value may be derived in the following ways: From the robust mean (). This is the median of participant results after the removal of test results that are inappropriate for statistical evaluation, e.g. miscalculations, transpositions and other gross errors. Generally, the assigned value will be set using results from all methods, unless the measurement is considered method-dependant, in which case the assigned value will be set by method as illustrated in the report tables. For some analytes, where there is a recognised reference method for that type of measurement, this may be used as the assigned value for a particular analyte i.e. it would be applied to results obtained by any method. Traceability: Assigned values which are derived from the participant results, or a sub-set of the results are not traceable to an international measurement standard. The uncertainty of assigned values derived in this way is estimated from the participant results, according to ISO 358. From a formulation value (Formulation). This denotes the use of an assigned value derived from sample preparation details, where known and exact quantities of analyte have been used to prepare the sample. Traceability: Assigned values calculated from the formulation of the test sample are traceable, via an unbroken metrological traceability chain, to an international measurement standard. The measurement uncertainty of the assigned value is calculated using the contributions from each calibration in the traceability chain. From a qualitative formulation (Qual Form). This applies to qualitative tests where the assigned value is simply based on the presence/absence of the analyte in the test material. Traceability: Assigned values calculated from the qualitative formulation of the test sample are traceable to a certified reference standard or a microbiological reference strain. From expert labs (Expert). The assigned value for the analyte is provided by an expert laboratory. Traceability: Assigned values provided by an expert laboratory may be traceable to an international measurement standard, according to the laboratory and the method used. The uncertainty of measurement for an assigned value produced in this way will be provided by the laboratory undertaking the analysis. Details of traceability and the associated uncertainty will be provided in the report for the scheme/round. Range This indicates the concentration range at which the analyte may be present in the test material. SDPA SDPA represents the standard deviation for proficiency assessment which is used to assess participant performance for the measurement of each analyte. This may be a fixed value (as stated), a percentage (%) of the assigned value or based on the robust standard deviation of the participant measurement results, either across all methods or by method depending on whether the measurement made is method dependent (see assigned value). Issue: 9 Page 4 of 7 Issue date: September 08

5 Units This indicates the units used for the assessment of data. These are the units in which participants should report their results. For some analytes in some schemes participants may have a choice of which units to report their results, however, the units stipulated in this scheme description are the default units to which any results reported using allowable alternative results will be converted to. DP This indicates the number of decimal places to which participants should report their measurement results. Issue: 9 Page 5 of 7 Issue date: September 08

6 Sample : Brewers and Distiller malt for chemical analysis Participants will receive x 000ml pots of malt ) Malt sample - Malt dependent tests Moisture Oven Method 0.5 % w/w DPWK (Diastatic power) Iodometric (reference method) 0 Diastatic Power (DP IoB) Alpha Amylase Segmented flow (e.g. Skalar) Calculated value (from IOB) Fehling s Ferricyanide Segmented flow (e.g. Skalar) Calculated value (from DPWK) International method automated segmented flow (e.g. Skalar) International method manual > >8 60 >60 (Iodometric) Calculated value WK units, dry IoB, as is 0 DU, dry 0 Dumas 0.08 %, dry Total Nitrogen Kjeldahl 0.08 %, dry NIR (Dumas) 0.04 %, dry Friability Friability meter Expert.7 % Homogeneity Friability meter 0.5 % Glassy (Whole) Corns Friability meter 0.4 % Partly Unmodified Grains Friability meter 0.5 % Sieving Test <.0mm Sieving Test.0 to.50mm Sieving Test.50 to.80mm Sieving Test >.80mm Steinecker/Glasblaserei Sortimat Steinecker/Glasblaserei (EBC Fraction III) Sortimat Steinecker/Glasblaserei (EBC Fraction II) Sortimat Steinecker/Glasblaserei (EBC Fraction I) (Steinecker) (Steinecker) (Steinecker) (Steinecker) 0.3 % 0.5 %.5 %.8 % Issue: 9 Page 6 of 7 Issue date: September 08

7 EBC Reject Fraction (EBC Fraction IV plus Analytica EBC 0.5 % foreign matter) EBC Fraction IV (<.mm + damaged corns from all other sieves) Analytica EBC 0.5 % Malt Modification Image analyser Visual (all methods).6 % Malt Mod Homogeneity DMSP (Malt) (Dimethyl Sulfide Precursor) Free DMS (Malt) (Dimethyl Sulfide) Total DMS (Malt) (Dimethyl Sulfide) DMSP EBC Wort (Dimethyl Sulphide Precursor) Residual Sulfur Dioxide Image analyser Visual GC-FPD GC-FID GC-FPD GC-FID GC-FPD GC-FID GC-FPD GC-FID GC, Monier Williams Para Rosaniline, DTNB, Ripper, Enzymatic 8 >8 8 >8 0 >0 0 >0 0 >0 (all methods) 8 % mg/kg, as is mg/kg, as is mg/kg, as is mg/kg, as is mg/kg, as is Cold Water Extract Cold water extract 0.5 % (m/m), as is Hartong VZ45 VZ45.5 %, dry NDMA GC-TEA g/kg, as is (Nitrosodimethylamine) GC-MS >.5.0 Glycosidic Nitrile Distillation 0. g CN/tonne, as is Total Phenols Chromatographic methods mg/kg, as is Colorimetric (all methods) Issue: 9 Page 7 of 7 Issue date: September 08

8 ) Malt sample - EBC wort dependent tests Extract:.0mm Paddle stirrer /Density Meter, Magnetic stirrer/density Meter 0.4 %, dry Extract: 0.mm Paddle stirrer /Density Meter, Magnetic stirrer/density Meter 0.4 %, dry EBC Extract Difference (0.-.0) Calculation 0.3 %, dry ph (EBC Wort) ph meter 0.05 Units Visual deg EBC Colour (EBC Wort) Boiled Wort Colour (EBC Wort) TSN (EBC Wort) (Total Soluble Nitrogen) Kolbach Index FAN (Free Alpha Amino Nitrogen) Viscosity (EBC Wort) EBC Fermentability (Boiled) Spectrophotometric Visual heating plate Visual oil bath >6 6 >6 0.4 Issue: 9 Page 8 of 7 Issue date: September 08 9 >9 0.8 deg EBC deg EBC Spectrophotometer heating plate Spectrophotometer oil bath >9 deg EBC Dumas 0.05 % (m/m), dry Kjeldahl 0.05 % (m/m), dry Spectrophotometric (Kjeldahl) 0.05 % (m/m), dry Total UV digestion 0.05 % (m/m), dry Calculation.4 % Manual Ninhydrin method Automated Ninhydrin method (e.g. Skalar) Automated other (e.g. Beermaster) Falling Ball Viscometer, Rotary Viscometer, Glass Capillary Viscometer Dried yeast/density meter Fresh (brewers/distillers) Yeast/ Density meter Fresh (bakers) Yeast/ Density meter 9 mg/l mpas (Fresh brewers/distille rs yeast).0 % Beta Glucan (EBC Wort) Spectrophotometric automated 0 mg/l 0

9 analyser (e.g. beermaster) Spectrophotometric manual test kit Fluorimetric automated analyser (e.g. Skalar) 0 mg/l 0 Fluorimetric manual injection Enzymatic 0 mg/l 0 3) Malt sample - IoB wort dependent tests IoB Extract 0.7mm Paddle stirrer /Density Meter, Magnetic stirrer/density Meter.5 L deg/kg, dry Manual stir/density Meter IoB Extract 0.mm Paddle stirrer /Density Meter, Magnetic stirrer/density Meter.5 L deg/kg, dry Manual stir/density Meter IoB Extract Difference (0.-0.7) Calculation L deg/kg, dry IoB Soluble Extract.0mm Calculation 0.3 % sol ext, as is IoB Soluble Extract 0.7mm Calculation 0.3 % sol ext, as is IoB Soluble Extract 0.mm Calculation 0.3 % sol ext, as is IoB Sol Extract Difference (0.-0.7) Calculation 0.3 % sol ext, as is IoB Sol Extract Difference (0.-.0) Calculation 0.35 % sol ext, as is ph (IoB Wort) ph meter 0.05 ph units Colour (IoB Wort) Visual >6 deg EBC Spectrophotometric >6 deg EBC Dumas 0.05 % (m/m), dry Kjeldahl 0.05 % (m/m), dry TSN (IoB Wort) (Total Soluble Nitrogen) Spectrophotometric 0.05 % (m/m), dry (Kjeldahl) Total UV digestion 0.05 % (m/m), dry SNR Dumas.5 % Issue: 9 Page 9 of 7 Issue date: September 08

10 (Soluble Nitrogen Ratio) Kjeldahl.5 % FAN (IoB Wort) (Free Alpha Amino Nitrogen) Manual Ninhydrin method Automated Ninhydrin method (e.g. Skalar) Automated other (e.g. Beermaster) 8 mg/l 0 Viscosity (IoB Wort) IoB Fermentability (Unboiled 0.7mm) Predicted Spirit Yield (as is) Beta Glucan (IoB Wort) Falling Ball Viscometer, Rotary Viscometer, Glass Capillary Viscometer Dried yeast/density meter Fresh (brewers/distillers) Yeast/ Density meter Fresh (bakers) Yeast/ Density meter NIR Calculation from fermentability Spectrophotometric automated analyser (e.g. beermaster) Spectrophotometric manual test kit Fluorimetric automated analyser (e.g. Skalar) Fluorimetric manual injection 0.03 mpas 0.5 % 3 L alcohol/tonne, as is 0 mg/l 0 0 mg/l 0 Enzymatic 0 mg/l 0 0 Issue: 9 Page 0 of 7 Issue date: September 08

11 Sample : Barley Participants will receive Barley for chemical analysis x 000ml pot of barley Oven (ISO Method) 0. Moisture Moisture meter (ISO oven) 0.3 % w/w NIR (Near Infrared) 0. Dumas 0.03 %, dry Total Nitrogen Kjeldahl 0.03 %, dry NIR (Near Infrared) (Dumas) 0.03 %, dry Steinecker/Glasblaserei Sieving Test <.0mm Sortimat Other (Steinecker) 0.3 % Steinecker/Glasblaseri Sieving Test <.5mm Sortimat Other (Steinecker) 0.3 % Steinecker/Glasblaserei Sieving Test.0 to (EBC Fraction III).50mm Sortimat (Steinecker) % Other Steinecker/Glasblaserei Sieving Test.5 to Sortimat.50mm Other (Steinecker) % Steinecker/Glasblaserei Sieving Test >.50mm Sortimat Other (Steinecker).5 % Steinecker/Glasblaserei Sieving Test.50 to (EBC Fraction II).80mm Sortimat (Steinecker) 3 % Other Steinecker/Glasblaserei Sieving Test >.80mm (EBC Fraction I) Sortimat (Steinecker) 3.5 % Other EBC Reject Fraction (EBC Fraction IV plus Foreign Matter) Analytica EBC 0.5 % Issue: 9 Page of 7 Issue date: September 08

12 EBC Fraction IV (<.mm + damaged corns from all other sieves) Thousand Corn Weight Germinative capacity Germinative energy BRF 8ml Test Hectolitre Weight Analytica EBC 0.5 % EBC 3.4 (Automatic corn counter) EBC 3.4 (Manual corn counter) 0.6 g, dry Rapid (TET M ) staining.5 % 0 Peroxide.5 % 0 Aubry 5 day test % 0 Schonfeld 5 day test % 0 BRF 4ml Test (7hrs).5 % 0 7hrs Chrondrometer NIR 90 > % Kg/hectolitre Sample 3: Mycotoxin Participants will receive Malt flour for mycotoxin analysis x 00g pots of malt flour (sample and blank*) Ochratoxin A ELISA Lateral flow (e.g. Charm, Neogen) 5% of AV µg/kg HPLC Deoxynivalenol (DON) ELISA Lateral flow (e.g. Charm, Neogen) HPLC 5% of AV µg/kg 0 *Blank material supplied as a quality control material only (results are not required to be returned for this material). Issue: 9 Page of 7 Issue date: September 08

13 Sample 4A: Black malt Participants will receive Specialised malt for chemical analysis x 300ml pot Moisture Oven Moisture meter 0.5 % w/w Colour EBC 5.6, Vis Col, 450g mixed mash EBC 5.0 / IoB 3.6, Vis Col, 450g boiled mash IoB 3..4, Vis Col, 55ml boiled mash EBC 5.6, 430nm Spec Col, 450g mixed mash EBC 5.0 / IoB 3.6, 430nm Spec Col, 450g boiled mash IoB 3..4, 430nm Spec Col, 55ml boiled mash deg EBC Sample 4B: Crystal malt Participants will receive Specialised malt for chemical analysis x 300ml pot Moisture Oven Moisture meter 0.5 % w/w Colour 55ml Spec Wort Colour, (IoB 3.3, hour 65 C, 50/50 mixed mash) 55ml Visual Wort Colour (IoB 3.3, hour 65 C, 50/50 mixed mash) 450g Spec Wort Colour (IoB 3.3 / EBC 5.7, hour 65 C, 50/50 mixed mash) 450g Visual Wort Colour (IoB 3.3 / EBC 5.7, deg EBC hour 65 C, 50/50 mixed mash) 450g Spec Wort Colour (EBC 5.5, C extraction, 50/50 mixed mash) 450g Visual Wort Colour (EBC 5.5, C extraction, 50/50 mixed mash) Degrees of crystallisation Visual % Issue: 9 Page 3 of 7 Issue date: September 08

14 Sample 5: NDMA Participants will receive Malt flour for NDMA analysis x 00g flour based matrix NDMA GC-TEA g/kg, as is (Nitrosodimethylamine) GC-MS >.5.0 Text written in italics is for reference purposes only and will not feature in the published report. Sample 6: Participants will receive High diastatic power malt for chemical analysis x 000ml pot of high DP malt ) Malt sample - High diastatic power malt dependent tests Moisture Oven Method 0.5 % w/w Iodometric (reference method) DPWK Segmented flow (e.g. Skalar) WK units, dry (Diastatic power) Calculated value (Iodometric) > (from IOB) 0 Diastatic Power (DP IoB) Alpha Amylase IoB Soluble Extract 0.7mm TSN (IoB Wort) (Total Soluble Nitrogen) FAN (IoB Wort) (Free Alpha Amino Fehling s Ferricyanide Segmented flow (e.g. Skalar) Calculated value (from DPWK) International method automated segmented flow (e.g. Skalar) International method manual >8 Calculated value Issue: 9 Page 4 of 7 Issue date: September > IoB, as is 0 DU, dry 0 Calculation 0.3 % sol ext, as is Dumas Kjeldahl Spectrophotometric Total UV digestion Manual Ninhydrin method Automated Ninhydrin method (e.g % (m/m), dry 8 mg/l 0

15 Nitrogen) Skalar) Automated other (e.g. Beermaster) Glycosidic Nitrile Distillation 0. g CN/tonne, as is Sample 7: Participants will receive Malted wheat for chemical analysis* x 000ml pot of malted wheat ) Malt sample - Malted wheat dependent tests Moisture Oven Method 0.5 % w/w Iodometric (reference method) DPWK Segmented flow (e.g. Skalar) WK units, dry (Diastatic power) Calculated value (Iodometric) > (from IOB) 0 Diastatic Power (DP IoB) Alpha Amylase Protein Fehling s Ferricyanide Segmented flow (e.g. Skalar) Calculated value (from DPWK) International method automated segmented flow (e.g. Skalar) International method manual > Issue: 9 Page 5 of 7 Issue date: September > IoB, as is 0 DU, dry 0 Dumas 0.6 %, dry ** Kjeldahl 0.6 %, dry ** NIR (Dumas) 0.3 %, dry ** Extract: 0.mm (EBC) Paddle stirrer /Density Meter, Magnetic stirrer/density Meter 0.4 %, dry ph (EBC Wort) ph meter 0.05 ph units Colour (EBC Wort) Visual >6 deg EBC Spectrophotometric >6 deg EBC Boiled Wort Colour Visual heating plate (EBC Wort) Visual oil bath >9 deg EBC

16 Spectrophotometer heating plate Spectrophotometer oil bath >9 deg EBC Dumas 0.05 % (m/m), dry TSN (EBC Wort) % (m/m), dry Kjeldahl 0.05 (Total Soluble Nitrogen) Spectrophotometric % (m/m), dry 0.05 (Kjeldahl) Kolbach Index Dumas.4 % Kjeldahl.4 % Manual Ninhydrin method FAN (EBC wort) Automated Ninhydrin method (e.g. (Free Alpha Amino Skalar) Nitrogen) Automated other (e.g. Beermaster) 9 mg/l 0 Falling Ball Viscometer, Rotary Viscosity (EBC Wort) Viscometer, Glass Capillary 0.0 mpas EBC Fermentability (Boiled) Beta Glucan (EBC Wort) IoB Extract 0.7mm Viscometer Dried yeast/density meter Fresh (brewers/distillers) Yeast/ Density meter Fresh (bakers) Yeast/ Density meter Spectrophotometric automated analyser (e.g. beermaster) Spectrophotometric manual test kit Fluorimetric automated analyser (e.g. Skalar) Fluorimetric manual injection (Fresh brewers/distille rs yeast).4 % 0 mg/l 0 0 mg/l 0 Enzymatic 0 mg/l 0 Paddle stirrer /Density Meter, L deg/kg, dry Magnetic stirrer/density Meter.5 Manual stir/density Meter ph (IoB Wort) ph meter 0.05 ph units Visual deg EBC Colour (IoB Wort) >6 Spectrophotometric deg EBC Issue: 9 Page 6 of 7 Issue date: September 08

17 >6 Dumas 0.05 % (m/m), dry % (m/m), dry Kjeldahl 0.05 TSN (IoB Wort) (Total Soluble Nitrogen) % (m/m), dry Spectrophotometric 0.05 (Kjeldahl) Total UV digestion 0.05 % (m/m), dry SNR Dumas.5 % (Soluble Nitrogen Ratio) Kjeldahl.5 % Manual Ninhydrin method FAN (IoB Wort) Automated Ninhydrin method (e.g. (Free Alpha Amino Skalar) Nitrogen) Automated other (e.g. Beermaster) 8 mg/l 0 Falling Ball Viscometer, Rotary Viscosity (IoB Wort) Viscometer, Glass Capillary 0.03 mpas Viscometer Spectrophotometric automated analyser (e.g. beermaster) Spectrophotometric manual test 0 mg/l 0 Beta Glucan (IoB Wort) kit Fluorimetric automated analyser (e.g. Skalar) 0 mg/l 0 Fluorimetric manual injection Enzymatic 0 mg/l 0 * Not currently included in LGC s UKAS Scope of Accreditation ** Results may also be reported expressed as Nitrogen. These values will be converted to protein using the factor 5.7 Issue: 9 Page 7 of 7 Issue date: September 08