ICAR PROFICIENCY TEST - SEPTEMBER Raw cow milk Chemical Reference Methods

Transcription

1 ICAR PROFICIENCY TEST - SEPTEMBER 2017 Raw cow milk Chemical Reference Methods

2 FRAME OF ACTIVITY : ICAR MILK ANALYSES SUB-COMMITTEE (MA SC) ORGANISER: ICAR, VIA SAVOIA 78, I ROME, ITALY pt@icar.org Tel.:

3 Raw cow milk Chemical Reference Methods

4 Table of contents 1. Introduction 2. Your performances analysis 3. Control Charts 4. ICAR Statistical Elaboration Fat (reference-chemical methods) Protein (reference-chemical methods) Lactose (reference-chemical methods) Urea (reference-chemical methods) Somatic Cell (microscopic and fluoro-optoelectronic method) ICAR Proficiency Test (PT) Chemical Reference methods March 2017

5 Introduction Dear Participant, Thank you for participating in the ICAR Proficiency Test (PT) September 2017! In this report you will find sections 2 and 3 which are dedicated to your quality assurance management and section 4 dedicated to the general statistical elaboration for each parameter. The proficiency test is a tool to help evaluate the performance of the laboratory process and to support your laboratory quality assurance system. It s aim is to provide independent data for you to monitor, evaluate and ultimately improve your processes as you see fit. From the analyses of the data received we have identified some aspects that if evaluated and managed may serve to improve some control steps of your quality management ISO When the PT samples arrive to your laboratory they can be viewed as being from a customer that is asking you to provide timely, precise and accurate results. In tables A,B,C,D,E,F,G,H if all the information is reported correctly from the participant, then the cells are filled in green, otherwise they are highlighted in red for your attention, so you can review and verify any causal reasons internally. The control charts H will help you to follow your performance over the time. A) In table A you find your participation codes and the information if all the results from the samples received, have been sent to the PT provider. B) In table B is indicated if the results have been sent on time. C) In table C is indicated if the results have been reported in the correct unit of measurements. D) It is the ranking of your laboratory. The values of table 1 for each parameter are reported. In table D the ranking of your lab will be green if the mean of difference and standard deviation of difference value are in the box of figure 2 of each parameter. Limits are only indicative and so far do not constitute standard values; they indicate what is normally reachable by labs for their self evaluation. According the results obtained the MA SC will decide eventually to revise. During the meeting of Milk Analyses Sub Committee held in Copenhagen in June 2016 the experts decided to update the limit of the box to evaluate the accuracy. E) Here are reported the samples that resulted outlier for your participation code for Grubbs or Cochran test F) The evaluation of repeatability of the results should be one of the first controls before communication of the data. In table F the absolute difference between replicates is compared with the repeatability limit of the relevant reference method indicated. If one or more results have a result out of the limit, the cell is in red. It may be that you have deployed a chemical method that is different from the reference method indicated. If the repeatability is bigger it will be evaluated internally with the precision of the specific method used. You can ICAR Proficiency Test (PT) Chemical Reference methods March 2017

6 find all the detailed information of your data in Table II in the section Statistical elaboration for each parameter. G) In table G the results of your Z-Score PT (standard deviation calculated on this proficiency test) and the Z-Score FIX (standard deviation of the reference method) are summarized. If you have obtained all the -2<Z-Score results<+2 the cell will be filled in green. If you have obtained one or more results in the moderate or poor performance range the cells will be filled in yellow or red respectively. H) Your ZS Control Charts have been updated with data of the previous ICAR PT if you have participated. On the control charts the samples are ordered by concentration. The sample preparation and statistical elaboration have been done by ICAR Sub- contractor Actalia, accreditated for ISO In the second part of the report the statistical elaboration followed the template approved by ICAR s Milk Analyses Sub Committee chaired by Dr. Gavin Scott (NZ). You find the statistical elaboration for all the ICAR interested parameters, fat, protein, lactose, urea and somatic cell. We think it is important to show you, as ICAR member, the reproducibility of the ICAR laboratories, even if you have not participated in this PT round. For each parameter the SR=standard deviation of reproducibility has been calculated after the outlier elimination. If you have participated, and your results are in the repeatability limits, you can use this value for the calculation of your uncertainty of measurement. ICAR would like to see, in the next years, part 4 of this report, completed with the results, reference and/or routine methods, from all the ICAR countries for the parameters indicated. We are sure with your support and contribution it will grow to benefit all! The list of all ICAR reference laboratories and those participated in ICAR PT in September 2017 with at least one parameter is reported below and also available in ICAR website at: ICAR Proficiency Test (PT) Chemical Reference methods September 2017

7 Name of the laboratory Comité du Lait ASBL Department Valorisation des productions Agricoles ILVO Can West Central Milk Testing Lab Horizon Lab Ltd Pacific Milk Analysis Valacta - Centre d Expertise en Production Laitière du Québec COOPRINSEM Dairy Cattle Research Center of Shandong Academy of Agricultural Sciences Shangai Dairy Breeding Center Co. Ltd Croatian Agricultural Agency, Central Laboratory for Milk Quality Control University of Zagreb Faculty of Agriculture Dept. of Dairy Science Laborator pro rozbor mléka Brno, Ceskomoravská spolecnost chovatelú a.s. Laborator pro rozbor mléka Bustehrad, Ceskomoravská spolecnost chovatelú a.s. Milkom a.s Dairy research institute The National laboratory for raw milk Agrovyzkum Rapotin s.r.o. ChemoMetec A/S Eurofins Steins Laboratory A/S Country Belgium Belgium Belgium Canada Canada Canada Canada Canada Chile China China Croatia Croatia Czech Republic Czech Republic Czech Republic Czech Republic Denmark Denmark ICAR Proficiency Test (PT) Chemical Reference methods September 2017

8 Name of the laboratory Cattle Information Service (CIS) Osuuskunta Satamaito, laboratorio Valio Oy/Seinajoen aluelaboratorio Actalia Milchprüfring Baden-Württemberg e.v. Teagasc Food research Center Central Milk Lab ICBA Laboratorio Standard Latte Japan Dairy Technical Association Pieno Tyrimai Laboratorium Oceny Mleka KCHZ Laboratorium Referecyjne z/s w Parzniewie Alip LRV-Laboratorio Regional de Veterinaria Holstein-Ro Breeders Association Laboratory Laboratorija za ispitivanje kvaliteta mleka, Poljoprivredni fakultet Novi Sad Deltamune Merieux Nutriscience South Africa University of Pretoria, Faculty Vet Sciences, Dept. Production Animal Studies Milk Lab. Onderstepoort Lab Agroalimentario de Santander LIGAL Edificio de Laboratorio Agrarios Eurofins Steins Laboratory A/B Agroscope Institute for food Sciences IFS Suisselab AG Taiwan Livestock research Insitute Qlip B.V., Direction de l' Amelioration Genetique Eastern Lab services Vetlab Agricultural Showgrouds Country England Finland Finland France Germany Ireland Israel Italy Japan Lithuania Poland Portugal Portugal Romania Serbia South Africa South Africa South Africa Spain Spain Sweden Switzerland Switzerland Taiwan The Netherlands Tunisia USA Zambia Attached to this report you find the certificate of your participation in the ICAR PT.- ICAR would like to stay at your side to support you in any way we can to help improve overall quality management systems for milk analyses. Your active participation in the ICAR PTs and in the Milk Analyses meetings is encouraging. We welcome any and all feedback/comments you may have on this activity, as it will help us continuously improve and to ultimately provide you a better service. Kind Regards, ICAR Secretariat ICAR Proficiency Test (PT) Chemical Reference methods September 2017

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10 Chemical Reference Methods Laboratory participation codes and Performance analyses ICAR PT RF0917 Laboratory Name Your participation Codes A B Subscription Fat ref Protein ref Lactose ref Urea ref SCC ref/alt Yes Yes Yes Yes Yes Participation Codes Are all the sample results received? Yes Yes Yes Yes Yes Data results received on time No Have you sent the data with the correct units of measurements? C Fat ref Protein* ref Lactose ref Urea ref SCC ref/alt g/100g nitrogen g/100g g/100g mg/dl SCC*1000/ml Yes Yes Yes Yes Yes * It was requested to report the value in total nitrogen Ranking of your lab Fat ref Protein* ref Lactose ref Urea ref SCC ref/alt g/100g nitrogen g/100g g/100g mg/dl SCC*1000/ml Code % % D d % Sd % D % Method ISO 1211 IDF 1 ISO8968 IDF20 ISO26642 IDF214 ISO14637 IDF195 ISO IDF148-2 Limits d 0,020 0,025 0,10 2,5 10% Sd 0,030 0,020 0,10 1,5 10% Outliers Fat ref Protein* ref Lactose ref Urea ref SCC ref/alt g/100g nitrogen g/100g g/100g mg/dl SCC*1000/ml Sample 1 Cochran Cochran E Sample 2 Sample 3 Sample 4 Sample 5 Sample 6 Sample 7 Sample 8 Sample 9 Sample 10 Cochran Cochran Cochran Cochran

11 F Repeatability Your "r" performance Fat Protein Lactose Urea SCC g/100g nitrogen g/100g g/100g mg/dl SCC*1000/ml Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample If the repeatability in smaller than the limit the cell is in green if there is a sample with a "r" bigger than the limit the cell is in red. Please check table II in correspondence of the parameter and your lab code. Limits Fat Protein Lactose Urea SCC g/100g g/100g g/100g mg/dl SCC*1000/ml ISO 1211 IDF 1D ISO 8968 IDF 20 ISO IDF 198 ISO IDF 195 0,043 0,038 0,06 1,52 Level ISO IDF r Your Z-Score PT Fat Protein Lactose Urea SCC Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Your Z-Score Fix G Fat Protein Lactose Urea SCC Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample If there is a sample with a "z-score" in the yellow or red area please check table VI and VII in correspondence of your lab code. Interpretation Z-Score Z-Score<-3-3<Z-Score<-2-2<Z-Score<2 2<Z-Score<3 Z-Score>3 Poor Moderate Good Moderate Poor

12 ZSCORE-PT - fat_ref ZSCORE-FIX - fat_ref 4 RF RF RF0317 RF RF0317 RF ZSCORE-PT - protein_ref ZSCORE-FIX - protein_ref 4 RF RF RF0317 RF RF0317 RF ZSCORE-PT - lactose_ref ZSCORE-FIX - lactose_ref 4 RF RF RF0317 RF RF0317 RF

13 ZSCORE-PT - urea_ref ZSCORE-FIX - urea_ref 4 RF RF RF0317 RF RF0317 RF ZSCORE-PT - scc_ref ZSCORE-FIX - scc_ref 4 RF RF RF0317 RF RF0317 RF

14 DETERMINATION of FAT in RAW (cow) MILK - page 1/8 ICAR PROFICIENCY TESTING SCHEME September 2017 Raw Milk Determination of FAT CONTENT Röse Gottlieb method Sending date of statistical treatment : 9 th October 2017 Frame of activity : ICAR Milk Analyses Sub Committee (MA SC) Contact : Gavin Scott gavin@milktest.co.nz ICAR Staff Silvia Orlandini pt@icar.org silvia@icar.org Proficiency test accreditated ISO ACCRÉDITATION N PORTÉE DISPONIBLE SUR

15 DETERMINATION of FAT in RAW (cow) MILK - page 2/8 Table I : Ranking of the laboratories Units : g / 100 g Nb % N d Sd D Method The table should be studied in parallel with figure 1 where the ,000 0,004 0,004 A laboratories are located according to an acceptability area (or target) ,001 0,005 0,005 A the limits of which are : ,003 0,004 0,005 A ,002 0,005 0,005 A ,003 0,005 0,006 A _ ,002 0,006 0,006 A +/- 0,020 g / 100 g for d and 0,030 g / 100 g for Sd ,003 0,008 0,009 A ,009 0,004 0,010 A ,002 0,011 0,011 A REF : Assigned values are robust average values per sample according to ,007 0,010 0,012 A algorithm A of standard ISO 13528, of 16 laboratories using the reference ,001 0,019 0,019 A method ISO 1211 IDF 1, after outliers discarging using Grubbs test ,006 0,021 0,022 B at 5% risk level, ,026 0,031 0,041 A ,037 0,023 0,044 A A ISO 1211 IDF 1D Röse Gottlieb Method ,048 0,089 0,101 A B ISO 2446 / IDF 226 Gerber method ,059 0,159 0,170 A (NC : OUT of RANKING because of insufficient data number) (Nb : laboratory rank; % : relative rank) (N : laboratory identification number) (d et Sd : mean and standard deviation of the differences (laboratory -reference)) (D : Euclidian distance to YX-axis origin = SQUARE ROOT.(d² + Sd²)) Note : Limits are only indicative and so far do not constitute standard values; they indicate what is normally reachable by labs for their self evaluation. Repeatability standard deviation of this ICAR proficiency test (after Cochran elimination at 5 %) Sr PT 0,007 Reproducibility standard deviation of this ICAR proficiency test (after Cochran and Grubbs elimination at 5 %) SR PT 0,014

16 DETERMINATION of FAT in RAW (cow) MILK - page 3/8 Table II : REPEATABILITY - Absolute difference between replicates in g / 100 g Sample Lab code Sr NL 1 0,006 0,005 0,002 0,004 1,000 * 0,014 0,006 0,003 0,003 0,002 0, ,012 0,017 0,002 0,002 0,019 0,000 0,001 0,000 0,013 0,020 0, ,002 0,002 0,001 0,003 0,001 0,001 0,000 0,001 0,003 0,001 0, ,003 0,015 0,019 0,002 0,021 0,005 0,006 0,003 0,022 0,004 0, ,010 0,010 0,010 0,010 0,010 0,000 0,010 0,010 0,010 0,020 0, ,030 0,020 0,000 0,020 0,000 0,020 0,010 0,010 0,010 0,000 0, ,025 0,008 0,027 0,007 0,002 0,008 0,014 0,002 0,006 0,014 0, ,003 0,013 0,011 0,003 0,001 0,011 0,007 0,006 0,000 0,003 0, ,000 0,006 0,006 0,004 0,004 0,000 0,011 0,001 0,000 0,001 0, ** ** ** 0,013 0,011 0,009 0,002 0,015 0,012 0,004 0, ,013 0,012 0,018 0,002 0,007 0,010 0,006 0,003 0,013 0,000 0, ,000 0,003 0,001 0,001 0,010 0,016 0,013 0,013 0,006 0,007 0, ,014 0,013 0,006 0,010 0,006 0,014 0,007 0,007 0,000 0,005 0, ,005 0,005 0,006 0,006 0,002 0,003 0,006 0,002 0,002 0,005 0, ,008 ** 0,000 0,008 0,003 0,000 0,011 0,010 0,002 0,013 0, ,046 * 0,021 0,010 0,017 0,007 0,019 0,004 0,003 0,008 0,012 0, Sr 0,012 0,009 0,008 0,006 0,177 0,008 0,006 0,005 0,006 0, NE L 0,033 0,032 0,030 0,024 0,025 0,029 0,022 0,019 0,025 0,026 Sr : repeatability standard deviation of each laboratory limit 0,016 g/100g NL : number of measurements per laboratory L : Limit for difference between duplicates according Cochran test at 5% level. SE : repeatability standard deviation per sample NE : number of measurements per sample *: discarded data using the test of Cochran at 5 % ** : missing data r : limit of repeatability, absolute difference betwen two replicates=0,043 according ISO 1211 IDF 1D 2010

17 DETERMINATION of FAT in RAW (cow) MILK - page 4/8 Table III : Means of the replicates in g / 100 g Sample Lab code ,742 4,123 3,480 2,750 2,640 * 4,459 3,752 3,091 1,501 2, ,757 4,113 3,466 2,737 2,137 4,465 3,737 3,080 1,473 2, ,760 4,120 3,477 2,746 2,138 4,471 3,746 3,091 1,486 2, ,739 4,080 3,467 2,724 2,120 4,356 * 3,720 3,053 1,471 2, ,755 4,145 3,465 2,735 2,125 4,480 3,705 3,075 1,465 2, ,725 * 4,090 3,480 2,710 2,120 4,460 3,775 3,095 1,455 2, ,038 * 4,218 * 3,500 * 2,745 2,151 4,463 3,738 3,083 1,473 2, ,761 4,099 3,458 2,751 2,142 4,487 3,745 3,092 1,484 2, ,762 4,106 3,470 2,740 2,124 4,463 3,730 3,080 1,464 2, ,733 2,121 4,451 3,752 3,069 1,471 2, ,761 4,115 3,466 2,739 2,129 4,458 3,736 3,079 1,469 2, ,762 4,105 3,463 2,737 2,128 4,460 3,740 3,078 1,479 2, ,758 4,104 3,471 2,721 2,119 4,477 3,745 3,068 1,469 2, ,753 4,098 3,460 2,734 2,119 4,468 3,739 3,089 1,476 2, ,763 3,471 2,744 2,137 4,462 3,744 3,085 1,479 2, ,682 * 4,048 3,426 * 2,681 * 2,091 * 4,424 * 3,727 3,070 1,468 2,407 M 4,756 4,103 3,469 2,736 2,129 4,466 3,739 3,080 1,474 2,442 REF. 4,757 4,105 3,469 2,737 2,128 4,465 3,739 3,080 1,473 2,444 SD 0,008 0,023 0,007 0,011 0,010 0,010 0,015 0,011 0,010 0,017 M = mean per sample REF. = reference values SD = standard deviation per sample *: discarded data using the test of Grubbs at 5 % REF : Assigned values are robust average values per sample according to algorithm A of standard ISO 13528, of 16 laboratories using the reference method ISO 1211 IDF 1, after outliers discarging using Grubbs test at 5 % risk level. Table IV : Outlier identification Sample Outliers Cochran 16 1 Outlier 6; 7; Grubbs ; 16 7; ; 16 sr 0,006 0,009 0,006 0,006 0,007 0,007 0,006 0,005 0,006 0,007 SR 0,009 0,024 0,008 0,012 0,011 0,011 0,016 0,012 0,011 0,018

18 DETERMINATION of FAT in RAW (cow) MILK - page 5/8 Table V : ACCURACY - differences (laboratory - reference) in g / 100 g Sample Lab code d Sd lab t 1-0, , , , ,512-0, , , , , ,059 0,159 1,18 2-0, ,008-0, , ,008-0,000-0,003-0,000-0, , ,002 0,005 1, , , , , , , , , , , ,009 0,004 7,64 4-0,019-0,025-0,002-0,013-0,009-0,110-0,019-0,028-0,002-0,037-0,026 0,031 2,66 5-0, ,040-0,004-0,002-0, ,015-0,034-0,005-0,008-0,004-0,001 0,019 0,13 6-0,032-0, ,011-0,027-0,008-0, , ,015-0,018-0,014-0,006 0,021 0, , , , , ,023-0,002-0, ,003-0, , ,048 0,089 1, ,003-0,006-0, , , , , , , , ,007 0,010 2, , , , ,003-0,004-0,002-0,010-0,001-0,009-0,009-0,003 0,005 1, ,004-0,008-0, ,013-0,012-0, ,013-0,002 0,011 0, , ,010-0, , ,000-0,007-0,003-0,002-0,005-0,005-0,001 0,005 0, , ,001-0, ,000-0,001-0, ,000-0, , ,003-0,000 0,004 0, ,001-0, ,002-0,016-0, , ,005-0,013-0,004-0,006-0,003 0,008 1, ,005-0,007-0,009-0,003-0, ,002-0, , , ,004-0,002 0,006 0, , , , ,008-0, , , ,006-0, ,003 0,004 2, ,076-0,056-0,043-0,056-0,038-0,041-0,012-0,011-0,005-0,036-0,037 0,023 5,24 d - 0,001-0,001-0,000-0, , , ,000-0, ,001-0, ,003 0,051 Sd 0,008 0,023 0,007 0,011 0,010 0,010 0,015 0,011 0,010 0,017 0,013 d = mean of differences Sd = standard deviation of differences t = Student test - comparison to 0 _ Upper limits : d = +/- 0,02 g / 100 g Sd = 0,03 g / 100g ISO 1211 IDF 1 : Precision of the method : Sr = g / 100 g SR = g / 100 g

19 Z score PT DETERMINATION of FAT in RAW (cow) MILK - page 6/8 Table VI : Zscore of the different laboratories for each sample. ZS calculated on the PT standard deviation Sample Lab code ,93 +0,77 +1,61 +1,17 +50,93-0,66 +0,83 +0,90 +2,61 +0,74 2-0,04 +0,34-0,37 +0,00 +0,80-0,04-0,18-0,03-0,07 +0, ,33 +0,67 +1,11 +0,77 +0,90 +0,52 +0,44 +0,90 +1,18 +0,71 4-2,37-1,08-0,30-1,17-0,90-11,35-1,25-2,49-0,21-2,17 5-0,29 +1,74-0,52-0,18-0,35 +1,51-2,23-0,48-0,79-0,21 6-4,07-0,63 +1,61-2,43-0,85-0,56 +2,33 +1,31-1,74-0, ,25 +4,89 +4,38 +0,68 +2,24-0,25-0,08 +0,24-0,02 +1, ,40-0,26-1,58 +1,22 +1,30 +2,18 +0,34 +1,04 +1,03 +0, ,59 +0,06 +0,19 +0,27-0,45-0,25-0,63-0,08-0,88-0, ,41-0,80-1,54 +0,83-1,06-0,21 +0, ,40 +0,45-0,37 +0,18 +0,00-0,77-0,21-0,17-0,45-0, ,56 +0,03-0,82 +0,01-0,08-0,55 +0,02-0,21 +0,51 +0, ,08-0,05 +0,33-1,44-0,94 +1,20 +0,34-1,15-0,40-0, ,61-0,30-1,23-0,27-0,94 +0,21-0,01 +0,77 +0,27 +0, ,71 +0,33 +0,63 +0,80-0,35 +0,28 +0,41 +0,55-0, ,51-2,43-6,04-5,03-3,74-4,26-0,80-0,95-0,50-2,15 In yellow the values bigger or smaller than 2/-2 In red the values bigger or smaller than 3/-3 Figure 2 : Zscore of the different laboratories for each sample. ZS calculated on the PT standard deviation sample1 sample2 sample 3 sample sample 5 sample 6 sample 7 sample sample 9 sample 10-5 Laboratory code

20 score Fix Z score Fix DETERMINATION of FAT in RAW (cow) MILK - page 7/8 Table VII : Zscore of the different laboratories for each sample. ZS calculated on the standard deviation of reproducibility of the method Sample Lab code ,77 +0,90 +0,57 +0,65 +25,58-0,32 +0,64 +0,51 +1,36 +0,62 2-0,02 +0,40-0,13 +0,00 +0,40-0,02-0,14-0,02-0,04 +0, ,13 +0,77 +0,39 +0,43 +0,45 +0,25 +0,34 +0,51 +0,61 +0,60 4-0,94-1,25-0,11-0,65-0,45-5,50-0,96-1,39-0,11-1,83 5-0,12 +2,02-0,18-0,10-0,17 +0,73-1,71-0,27-0,41-0,18 6-1,62-0,73 +0,57-1,35-0,42-0,27 +1,79 +0,73-0,91-0, ,01 +5,67 +1,54 +0,38 +1,13-0,12-0,06 +0,13-0,01 +1, ,16-0,30-0,56 +0,68 +0,65 +1,05 +0,26 +0,58 +0,54 +0, ,23 +0,07 +0,07 +0,15-0,22-0,12-0,49-0,04-0,46-0, ,22-0,40-0,75 +0,64-0,59-0,11 +0, ,16 +0,52-0,13 +0,10 +0,00-0,37-0,16-0,09-0,24-0, ,22 +0,03-0,29 +0,00-0,04-0,27 +0,02-0,12 +0,26 +0, ,03-0,05 +0,12-0,80-0,47 +0,58 +0,26-0,64-0,21-0, ,24-0,35-0,43-0,15-0,47 +0,10-0,01 +0,43 +0,14 +0, ,28 +0,12 +0,35 +0,40-0,17 +0,21 +0,23 +0,29-0, ,78-2,81-2,13-2,79-1,88-2,06-0,62-0,53-0,26-1,81 This table will allows to compare your ZSCORE from one PT to an other because the standard deviation has always the value of SR of the method SR=0,02 In yellow the values bigger or smaller than 2/-2 In red the values bigger or smaller than 3/-3 Figure 3 : Zscore of the different laboratories for each sample. ZS calculated on the standard deviation of reproducibility of the method sample 16 6 Laboratory Laboratory code code sample1 sample1 sample2 sample2 sample 3 sample 3 sample 4 sample 4 sample 5 sample 5 sample 6 sample 7 sample 7 sample 8 sample 8 sample 9 sample 9 sample 10 sample 10

21 DETERMINATION of FAT in RAW (cow) MILK - page 8/8 ICAR Interlaboratory Proficiency Study - - September Trial of : 04/09/2017 Sd Sd 0, laboratories samples 4 Labs 4 Labs OUT OUT OF OF THE THE TARGET TARGET ( 25 %( 25 ) % ) ,100 0,100 Student Student 5 5 % % Student Student 5 % 5 % 0,050 0,050 0,000 0,000-0,100-0,050 0,000 0,050 0,100-0,100-0,050 0,000 0,050 0,100 _ d _ d Figure 1 : ACCURACY - Evaluation of the individual performances (to see table I). LIST OF THE PARTICIPANTS ICAR ICAR PROFICIENCY TEST RAW MILK FAT CONTENT Röse Göttlieb September 2017 Name City Country Actalia Poligny France Agroscope 3003 Bern-Liebefeld Switzerland Central Milk Lab ICBA Caesarea IL Department Valorisation des productions Agricoles Gembloux Belgium Eastern Lab services Medina USA ILVO Melle Belgium Japan Dairy Technical Association Tokyo Japan Lab Agroalimentario de Santander Santander Cantabria Spain Laboratorio Standard Latte Maccarese Italy Laboratorium Oceny Mleka KCHZ Parzniewie Pruszkow Poland Milchprüfring Baden-Württemberg e.v. Kirchheim unter Teck Germany Pieno Tyrimai Kaunas Lithuania Qlip B.V., Zutphen NL Teagasc Food research Center Cork IR Nat. Lab. for raw milk Agrovyzkum Rapotin s.r.o. Vikyrovice Czech Republic Valacta - Quebec Canada

22 DETERMINATION of CRUDE PROTEINin RAW (cow) MILK - page 1/8 ICAR PROFICIENCY TESTING SCHEME September 2017 Raw Milk Determination of CRUDE PROTEIN CONTENT KJELDAHL Method Sending date of statistical treatment : 9 th October 2017 Frame of activity : ICAR Milk Analyses Sub Committee (MA SC) Contact : Gavin Scott gavin@milktest.co.nz ICAR Staff Silvia Orlandini pt@icar.org silvia@icar.org Proficiency test accreditated ISO ACCRÉDITATION N PORTÉE DISPONIBLE SUR

23 DETERMINATION of CRUDE PROTEINin RAW (cow) MILK - page 2/8 Table I : Ranking of the laboratories Units : g / 100 g Nb % N d Sd D The table should be studied in parallel with figure 1 where the ,002 0,005 0,006 laboratories are located according to an acceptability area (or target) ,004 0,008 0,008 the limits of which are : ,007 0,006 0, ,008 0,007 0, ,011 0,008 0,014 _ ,010 0,013 0,016 +/- 0,025 g / 100 g for d and 0,020 g / 100 g for Sd ,017 0,008 0, ,019 0,008 0, ,002 0,022 0,022 REF : Assigned values are robust average values per sample according to ,017 0,014 0,022 algorithm A of standard ISO 13528, of 15 laboratories using the reference ,012 0,020 0,023 method (ISO IDF 20-1), after outlier discarging using Grubbs test at ,008 0,022 0,024 5% risk level ,023 0,012 0, ,011 0,026 0, ,050 0,031 0, ,054 0,201 0,208 (NC : OUT of RANKING because of insufficient data number) (Nb : laboratory rank; % : relative rank) (N : laboratory identification number) (d et Sd : mean and standard deviation of the differences (laboratory -reference)) (D : Euclidian distance to YX-axis origin = SQUARE ROOT.(d² + Sd²)) Note : Limits are only indicative and so far do not constitute standard values; they indicate what is normally reachable by labs for their self evaluation. Repeatability standard deviation of this ICAR proficiency test (after Cochran elimination at 5 %) Sr PT 0,007 Reproducibility standard deviation of this ICAR proficiency test (after Cochran and Grubbs elimination at 5 %) SR PT 0,021

24 DETERMINATION of CRUDE PROTEINin RAW (cow) MILK - page 3/8 Table II : REPEATABILITY - Absolute difference between replicates in g / 100 g Sample Lab code Sr NL 1 0,001 0,001 0,001 0,000 0,001 0,008 0,008 0,002 0,003 0,002 0, ,010 0,006 0,001 0,001 0,000 0,001 0,001 0,000 0,008 0,003 0, ,006 0,006 0,006 0,006 0,006 0,000 0,006 0,000 0,006 0,000 0, ,012 0,009 0,011 0,002 0,008 0,009 0,000 0,006 0,015 0,002 0, ,070 * 0,007 0,049 * 0,085 * 0,073 * 0,021 0,002 0,031 0,021 0,004 0, ,002 0,048 * 0,018 0,057 * 0,005 0,093 * 0,004 0,009 0,004 0,053 * 0, ,006 0,007 0,004 0,003 0,013 0,009 0,027 0,001 0,010 0,020 0, ,003 0,002 0,021 0,017 0,008 0,006 0,016 0,007 0,000 0,001 0, ,004 0,006 0,003 0,002 0,008 0,004 0,005 0,006 0,005 0,003 0, ,015 0,006 0,002 0,003 0,009 0,012 0,000 0,003 0,007 0,005 0, ,008 0,006 0,001 0,006 0,006 0,006 0,015 0,001 0,003 0,000 0, ,003 0,013 0,002 0,010 0,004 0,001 0,011 0,008 0,026 0,008 0, ,033 * 0,008 0,017 0,014 0,000 0,013 0,006 0,011 0,002 0,005 0, ,002 0,001 0,005 0,008 0,004 0,002 0,004 0,006 0,008 0,003 0, ,006 0,006 0,024 0,010 0,012 0,011 0,001 0,034 0,003 0,017 0, ,010 0,014 0,065 * 0,005 0,006 0,102 * 0,027 0,003 0,002 0,030 * 0, Sr 0,014 0,010 0,016 0,019 0,014 0,025 0,008 0,009 0,007 0, NE L 0,020 0,020 0,030 0,021 0,019 0,024 0,032 0,034 0,028 0,021 Sr : repeatability standard deviation of each laboratory limit 0,014 g /100g NL : number of measurements per laboratory L : Limit for difference between duplicates according Cochran test at 5% level. SE : repeatability standard deviation per sample NE : number of measurements per sample *: discarded data using the test of Cochran at 5 % ** : missing data r : limit of repeatability, absolute difference betwen two replicates=0,040 according ISO 8968 / IDF 20

25 DETERMINATION of CRUDE PROTEINin RAW (cow) MILK - page 4/8 Table III : Means of the replicates in g / 100 g (*) : Data have been modified in right units. Sample Lab code (*) 1 3,817 3,593 3,316 2,973 2,792 3,717 3,518 3,161 3,294 2, ,798 3,611 3,322 2,951 2,766 3,720 3,536 3,150 3,347 2, ,825 3,627 3,327 2,964 2,772 3,720 3,531 3,152 2,715 * 2, ,774 3,589 3,319 2,926 2,745 3,700 3,508 3,131 3,336 2, ,800 3,583 3,372 2,979 2,801 3,719 3,531 3,150 3,338 2, ,806 3,629 3,343 2,924 2,784 3,689 3,530 3,214 3,356 2, ,800 3,625 3,325 2,954 2,764 3,711 3,526 3,149 3,355 2, ,795 3,602 3,306 2,943 2,745 3,700 3,505 3,141 3,333 2, ,792 3,612 3,320 2,946 2,758 3,699 3,514 3,136 3,337 2, ,778 3,606 3,323 2,949 2,761 3,690 3,514 3,138 3,340 2, ,803 3,620 3,326 2,955 2,766 3,719 3,542 3,151 3,355 2, ,783 3,596 3,318 2,935 2,755 3,703 3,515 3,135 3,283 2, ,758 3,578 3,287 2,947 2,762 3,695 3,543 3,159 3,366 2, ,823 3,639 3,348 2,966 2,778 3,733 3,548 3,165 3,364 2, ,798 3,620 3,344 2,982 2,788 3,750 3,556 3,188 3,373 2, ,747 3,576 3,311 2,879 * 2,700 * 3,723 3,438 * 3,081 3,268 2,828 M 3,793 3,607 3,325 2,953 2,769 3,712 3,528 3,150 3,336 2,876 REF. 3,795 3,607 3,325 2,953 2,769 3,711 3,528 3,150 3,340 2,877 SD 0,022 0,019 0,019 0,018 0,017 0,016 0,015 0,028 0,031 0,020 M = mean per sample REF. = reference values SD = standard deviation per sample *: discarded data using the test of Grubbs 5 % REF : Assigned values are robust average values per sample according to algorithm A of standard ISO 13528, of 15 laboratories using the reference method ISO IDF 20-1, after outliers discarging using Grubbs test at 5 % risk level. Table IV : Outlier identification Sample Outliers Cochran Outlier Grubbs 5; ; 16 5; 6 5 6; 16 6; sr 0,005 0,005 0,008 0,006 0,005 0,007 0,007 0,009 0,007 0,006 SR 0,021 0,020 0,017 0,016 0,015 0,017 0,016 0,029 0,032 0,017

26 DETERMINATION of CRUDE PROTEINin RAW (cow) MILK - page 5/8 Table V : ACCURACY - differences (laboratory - reference) in g / 100 g Sample Lab code d Sd lab t 1 + 0,023-0,013-0, , , ,006-0, ,011-0, , ,002 0,022 0, , ,004-0,003-0,002-0, , , , ,007-0, ,002 0,005 1, , , , , , , , ,002-0, ,001-0,054 0,201 0,86 4-0,021-0,018-0,006-0,027-0,024-0,010-0,020-0,019-0,003-0,024-0,017 0,008 6, ,005-0, , , , , , ,001-0, , ,012 0,020 1, , , ,018-0, ,015-0, , , , , ,011 0,026 1, , ,019-0, ,001-0,005-0,000-0,002-0, , , ,004 0,008 1, ,001-0,005-0,018-0,009-0,024-0,011-0,023-0,008-0,007-0,010-0,011 0,008 4,60 9-0, ,006-0,004-0,007-0,011-0,012-0,013-0,013-0,002-0,007-0,007 0,006 3, ,017-0,001-0,002-0,004-0,008-0,021-0,013-0,012-0,000-0,005-0,008 0,007 3, , , , ,002-0, , , , , , ,010 0,013 2, ,011-0,010-0,007-0,018-0,014-0,008-0,012-0,014-0,056-0,020-0,017 0,014 3, ,037-0,029-0,038-0,006-0,007-0, , , , ,006-0,008 0,022 1, , , , , , , , , , , ,019 0,008 7, , , , , , , , , , , ,023 0,012 5, ,048-0,030-0,014-0,074-0, ,012-0,089-0,069-0,072-0,049-0,050 0,031 5,06 d - 0,001-0, ,001-0, , , , ,001-0,003-0,001-0,006 0,054 Sd 0,022 0,019 0,019 0,018 0,017 0,016 0,015 0,028 0,031 0,020 0,021 d = mean of differences Sd = standard deviation of differences t = Student test - comparison to 0 _ Upper limits : d = +/- 0,025 g / 100 g Sd = 0,020 g / 100 g ISO IDF 20-1 : Precision of the method : Sr = g / 100 g SR = g / 100 g

27 Z score PT DETERMINATION of CRUDE PROTEINin RAW (cow) MILK - page 6/8 Table VI : Zscore of the different laboratories for each sample. ZS calculated on the PT standard deviation Sample Lab code ,04-0,69-0,44 +1,14 +1,40 +0,35-0,66 +0,41-1,46 +0, ,15 +0,23-0,13-0,09-0,18 +0,54 +0,58 +0,01 +0,23-0, ,39 +1,05 +0,12 +0,60 +0,20 +0,54 +0,24 +0,08-20,08 +0,04 4-0,96-0,92-0,33-1,52-1,43-0,63-1,30-0,66-0,10-1, ,22-1,23 +2,41 +1,47 +1,94 +0,48 +0,22 +0,02-0,04 +1, ,52 +1,15 +0,94-1,66 +0,89-1,34 +0,18 +2,31 +0,53 +0, ,22 +0,97-0,02 +0,08-0,28-0,01-0,11-0,01 +0,50 +0, ,03-0,25-0,95-0,54-1,43-0,65-1,48-0,30-0,22-0,50 9-0,12 +0,29-0,23-0,39-0,64-0,70-0,88-0,47-0,07-0, ,80-0,04-0,10-0,25-0,49-1,27-0,88-0,42-0,00-0, ,39 +0,70 +0,03 +0,11-0,17 +0,52 +0,91 +0,04 +0,49 +2, ,53-0,54-0,38-1,04-0,85-0,46-0,81-0,51-1,82-0, ,73-1,48-1,98-0,34-0,41-0,98 +0,99 +0,35 +0,84 +0, ,29 +1,64 +1,20 +0,75 +0,58 +1,37 +1,33 +0,55 +0,78 +0, ,13 +0,70 +1,01 +1,67 +1,17 +2,36 +1,85 +1,39 +1,07 +0, ,23-1,57-0,72-4,19-4,13 +0,74-5,84-2,44-2,32-2,42 In yellow the values bigger or smaller than 2/-2 In red the values bigger or smaller than 3/-3 Figure 2 : Zscore of the different laboratories for each sample. ZS calculated on the PT standard deviation sample1 sample2 sample 3 sample sample 5 sample 6 sample 7 sample sample 9 sample 10-5 Laboratory code

28 Z score Fix DETERMINATION of CRUDE PROTEINin RAW (cow) MILK - page 7/8 Table VII : Zscore of the different laboratories for each sample. ZS calculated on the standard deviation of reproducibility of the method Sample Lab code ,25-0,75-0,47 +1,11 +1,30 +0,32-0,56 +0,64-2,53 +0, ,18 +0,24-0,14-0,08-0,17 +0,49 +0,49 +0,02 +0,40-0, ,67 +1,13 +0,12 +0,59 +0,18 +0,49 +0,21 +0,12-34,72 +0,04 4-1,15-1,00-0,35-1,48-1,32-0,57-1,10-1,03-0,18-1, ,27-1,33 +2,59 +1,44 +1,80 +0,44 +0,19 +0,03-0,07 +1, ,62 +1,24 +1,01-1,63 +0,82-1,23 +0,15 +3,60 +0,92 +0, ,27 +1,04-0,02 +0,08-0,26-0,01-0,09-0,02 +0,87 +0, ,04-0,27-1,03-0,53-1,32-0,59-1,26-0,46-0,38-0,56 9-0,14 +0,32-0,25-0,39-0,60-0,64-0,75-0,73-0,13-0, ,96-0,04-0,11-0,24-0,45-1,16-0,75-0,66-0,00-0, ,46 +0,76 +0,04 +0,11-0,15 +0,47 +0,78 +0,07 +0,85 +2, ,63-0,58-0,41-1,01-0,78-0,42-0,69-0,79-3,14-1, ,07-1,60-2,13-0,33-0,38-0,89 +0,85 +0,55 +1,45 +0, ,54 +1,77 +1,29 +0,73 +0,54 +1,25 +1,13 +0,85 +1,34 +0, ,16 +0,76 +1,08 +1,64 +1,09 +2,16 +1,57 +2,16 +1,86 +0, ,67-1,69-0,78-4,10-3,83 +0,68-4,97-3,81-4,01-2,73 This table will allows to compare your ZSCORE from one PT to an other because the standard deviation has always the value of SR of the method SR=0,018 In yellow the values bigger or smaller than 2/-2 In red the values bigger or smaller than 3/-3 Figure 3 : Zscore of the different laboratories for each sample. ZS calculated on the standard deviation of reproducibility of the method sample1 sample2 sample 3 sample sample 5 sample 6 sample 7 sample sample 9 sample 10-5 Laboratory code

29 DETERMINATION of CRUDE PROTEINin RAW (cow) MILK - page 8/8 ICAR Interlaboratory Proficiency Study - September 2017 Trial of : 04/09/2017 0, laboratories 10 samples Sd 6 Labs OUT OF THE TARGET ( 38 % ) ,100 Student 5 % Student 5 % 0,050 0,000-0,100 _ -0,050 0,000 0,050 0,100 Target limits : d = +/ g / 100 g of milk Sd = g / 100 g of milk _ d Figure 1 : ACCURACY - Evaluation of the individual performances (to see table I). LIST OF THE PARTICIPANTS ICAR ICAR PROFICIENCY TEST RAW MILK NITROGEN CONTENT September 2017 Name City Country Actalia Poligny France Agroscope Bern-Liebefeld Switzerland Central Milk Lab ICBA Caesarea IL Department Valorisation des productions Agricoles Gembloux Belgium Eastern Lab services Medina USA ILVO Melle Belgium Japan Dairy Technical Association Tokyo Japan Lab Agroalimentario de Santander Santander Cantabria Spain Laboratorio Standard Latte Maccarese Italy Laboratorium Oceny Mleka KCHZ Laboratorium Referecyjne z/s w Parzniewie Pruszkow Poland Milchprüfring Baden-Württemberg e.v. Kirchheim unter Teck Germany Pieno Tyrimai Kaunas Lithuania Qlip B.V., Zutphen NL Teagasc Food research Center Cork IR The National laboratory for raw milk Agrovyzkum Rapotin s.r.o. Vikyrovice Czech Republic Valacta - Centre d Expertise en Production Laitière du Québec Quebec Canada

30 DETERMINATION of LACTOSE in RAW (cow) MILK - page 1/8 ICAR PROFICIENCY TESTING SCHEME September 2017 Raw Milk Determination of LACTOSE CONTENT Sending date of statistical treatment : 9 th October 2017 Frame of activity : ICAR Milk Analyses Sub Committee (MA SC) Contact : Gavin Scott gavin@milktest.co.nz ICAR Staff Silvia Orlandini pt@icar.org silvia@icar.org ACCRÉDITATION N PORTÉE DISPONIBLE SUR

31 DETERMINATION of LACTOSE in RAW (cow) MILK - page 2/8 Table I : Ranking of the laboratories Units : g / 100 g Nb % N d Sd D Method ,010 0,020 0,023 IDF ,011 0,021 0,024 N.C ,026 0,018 0,032 IDF ,038 0,018 0,042 Own method ,016 0,043 0,046 Enzymatic method ,049 0,018 0,052 IDF ,025 0,048 0,054 IDF 79B: ,056 0,023 0,061 Polarimeter ,059 0,019 0,062 IDF ,066 0,028 0,072 IDF ,025 0,080 0,084 IDF ,059 0,098 0,115 IDF ,091 0,079 0,121 Lane-Eynon ,021 0,205 0,206 Polarimeter ,315 0,078 0,324 analyse à flux continu The table should be studied in parallel with figure 1 where the laboratories are located according to an acceptability area (or target) the limits of which are : _ +/ g / 100 g for d and g / 100g for Sd REF : Assigned values are robust average values per sample according to algorithm A of standard ISO 13528, of 15 laboratories, after outliers discarging using Grubbs test at 5 % risk level. (NC : OUT of RANKING because of insufficient data number) (Nb : laboratory rank; % : relative rank) (N : laboratory identification number) (d et Sd : mean and standard deviation of the differences (laboratory -reference)) (D : Euclidian distance to YX-axis origin = SQUARE ROOT.(d² + Sd²)) Note : Limits are only indicative and so far do not constitute standard values; they indicate what is normally reachable by labs for their self evaluation. Repeatability standard deviation of this ICAR proficiency test (after Cochran elimination at 5 %) Sr PT 0,014 Reproducibility standard deviation of this ICAR proficiency test (after Cochran and Grubbs elimination at 5 %) SR PT 0,091

32 DETERMINATION of LACTOSE in RAW (cow) MILK - page 3/8 Table II : REPEATABILITY - Absolute difference between replicates in g / 100 g Sample Lab code Sr NL 1 0,006 0,014 0,006 0,004 0,005 0,004 0,001 0,008 0,001 0,002 0, ,000 0,000 0,010 0,000 0,010 0,010 0,010 0,010 0,010 0,000 0, ,018 0,019 0,018 0,037 0,000 0,019 0,038 0,037 0,019 0,001 0, ,077 * 0,056 * 0,003 0,016 0,021 0,012 0,023 0,025 0,038 0,013 0, ,020 0,010 0,000 0,000 0,010 0,010 0,010 0,000 0,010 0,000 0, ,001 0,005 0,001 0,023 0,026 0,034 0,014 0,007 0,013 0,005 0, ,003 0,014 0,004 0,010 0,008 0,000 0,006 0,006 0,001 0,006 0, ,033 0,080 * 0,035 0,009 0,063 * 0,018 0,005 0,068 0,006 0,015 0, ,000 0,000 0,005 0,008 0,004 0,003 0,001 0,021 0,027 0,012 0, ,003 0,012 0,010 0,012 0,004 0,027 0,006 0,001 0,020 0,013 0, ,019 0,165 * 0,010 0,000 0,039 0,039 0,117 * 0,010 0,117 * 0,087 * 0, ,005 0,008 0,002 0,007 0,000 0,011 0,039 0,036 0,033 0,001 0, ,004 0,008 0,004 0,021 0,006 0,063 0,004 0,064 0,010 0,002 0, ,003 0,028 0,030 0,018 0,008 0,020 0,031 0,024 0,020 0,013 0, ,015 0,015 0,029 0,059 * 0,029 0,044 0,015 0,017 0,060 0,017 0, Sr 0,017 0,036 0,011 0,015 0,016 0,019 0,025 0,021 0,027 0, NE L 0,035 0,034 0,042 0,041 0,044 0,072 0,051 0,080 0,065 0,024 Sr : repeatability standard deviation of each laboratory limit 0,022 g/100g NL : number of measurements per laboratory L : Limit for difference between duplicates according Cochran test at 5% level. SE : repeatability standard deviation per sample NE : number of measurements per sample *: discarded data using the test of Cochran at 5 % ** : missing data r : limit of repeatability, absolute difference betwen two replicates=0,061 according ISO / IDF 198

33 DETERMINATION of LACTOSE in RAW (cow) MILK - page 4/8 Table III : Means of the replicates in g / 100 g (*) : Data have been modified in the right units. Sample Lab code ,109 5,043 4,960 4,861 4,742 4,676 4,610 4,553 4,486 4, ,230 5,170 5,075 4,970 4,835 4,765 4,695 4,625 4,555 4, ,163 4,995 5,010 4,904 4,757 4,749 4,608 4,519 4,530 4, ,072 4,914 5,075 4,982 4,882 4,830 4,764 4,714 4,635 4, ,180 5,115 5,010 4,910 4,795 4,725 4,655 4,590 4,515 4, ,082 5,026 5,005 4,834 4,719 4,628 4,583 4,521 4,468 4, ,102 5,031 4,945 4,852 4,730 4,668 4,599 4,545 4,474 4,623 (*) 8 5,192 5,147 5,125 4,939 4,696 4,627 4,577 4,481 4,430 4, ,159 5,116 5,024 4,941 4,811 4,729 4,672 4,618 4,538 4, ,141 5,097 5,007 5,012 4,979 4,836 4,798 4,770 4,672 4, ,534 * 5,451 5,248 5,252 * 5,117 5,117 * 5,010 * 4,879 4,718 4,879 * 12 5,116 5,008 4,917 4,826 4,705 4,641 4,596 4,530 4,464 4, ,117 5,063 5,000 4,886 4,759 4,731 4,631 4,591 4,512 4, ,048 5,011 4,960 4,868 4,739 4,715 4,666 4,647 4,505 4, ,327 * 5,403 5,265 4,982 4,940 4,566 4,572 4,259 4,375 4,576 M 5,131 5,106 5,042 4,912 4,814 4,706 4,645 4,589 4,525 4,654 REF. 5,130 5,081 5,028 4,912 4,802 4,707 4,637 4,591 4,520 4,650 SD 0,052 0,146 0,102 0,060 0,119 0,077 0,069 0,140 0,091 0,055 M = mean per sample REF. = reference values SD = standard deviation per sample *: discarded data using the test of Grubbs 5 % REF : Assigned values are robust average values per sample according to algorithm A of standard ISO 13528, of 15 laboratories, after outliers discarging using Grubbs test at 5 % risk level. Table IV : Outlier identification Sample Outliers 4; 8; Cochran 11 Outlier Grubbs 11; sr 0,009 0,009 0,011 0,011 0,012 0,018 0,014 0,021 0,017 0,007 SR 0,051 0,112 0,103 0,060 0,119 0,078 0,070 0,141 0,077 0,

34 DETERMINATION of LACTOSE in RAW (cow) MILK - page 5/8 Table V : ACCURACY - differences (laboratory - reference) in g / 100 g Sample Lab code d Sd lab t 1-0,021-0,038-0,068-0,051-0,060-0,031-0,028-0,038-0,035-0,007-0,038 0,018 6, , , , , , , , , , , ,056 0,023 7, ,033-0,086-0,018-0,008-0, ,042-0,029-0, , ,020-0,016 0,043 1,14 4-0,059-0, , , , , , , , , ,059 0,098 1, , ,034-0,018-0,002-0, , ,018-0,001-0, , ,011 0,021 1,62 6-0,049-0,055-0,023-0,078-0,083-0,079-0,054-0,071-0,053-0,041-0,059 0,019 9,77 7-0,029-0,050-0,083-0,060-0,072-0,039-0,038-0,046-0,047-0,027-0,049 0,018 8, , , , ,028-0,106-0,080-0,060-0,111-0,090-0,060-0,025 0,080 1, , ,035-0, , , , , , , , ,026 0,018 4, , ,016-0, , , , , , , , ,091 0,079 3, , , , , , , , , , , ,315 0,078 12, ,015-0,073-0,111-0,086-0,097-0,066-0,042-0,061-0,057-0,056-0,066 0,028 7, ,013-0,018-0,028-0,026-0, ,024-0,006-0,000-0, ,017-0,010 0,020 1, ,083-0,070-0,068-0,044-0, , , ,056-0, ,005-0,025 0,048 1, , , , , ,138-0,141-0,065-0,332-0,145-0, ,021 0,205 0,32 d + 0, , , , ,012-0, ,007-0, , , ,019 0,114 Sd 0,052 0,146 0,102 0,060 0,119 0,077 0,069 0,140 0,091 0,055 0,097 d = mean of differences Sd = standard deviation of differences t = Student test - comparison to 0 _ Upper limits : d = +/ g / 100g Sd = g / 100g ISO IDF 198 : Precision of the method : Sr = g / 100 g SR = g / 100 g

35 Z score PT DETERMINATION of LACTOSE in RAW (cow) MILK - page 6/8 Table VI : Zscore of the different laboratories for each sample. ZS calculated on the PT standard deviation Sample Lab code ,41-0,26-0,66-0,84-0,51-0,40-0,40-0,27-0,38-0, ,91 +0,61 +0,46 +0,96 +0,28 +0,75 +0,83 +0,24 +0,38 +0, ,63-0,59-0,17-0,14-0,38 +0,54-0,42-0,52 +0,10 +0,36 4-1,13-1,14 +0,46 +1,16 +0,67 +1,60 +1,82 +0,87 +1,26 +2, ,95 +0,24-0,17-0,03-0,06 +0,24 +0,26-0,01-0,06 +0,37 6-0,94-0,38-0,23-1,30-0,69-1,02-0,78-0,51-0,58-0,75 7-0,55-0,34-0,81-0,99-0,60-0,50-0,55-0,33-0,51-0, ,19 +0,45 +0,95 +0,46-0,89-1,03-0,87-0,79-0,99-1, ,55 +0,24-0,04 +0,48 +0,08 +0,28 +0,49 +0,19 +0,19 +1, ,20 +0,11-0,20 +1,66 +1,49 +1,67 +2,32 +1,27 +1,67 +0, ,75 +2,54 +2,15 +5,64 +2,64 +5,31 +5,38 +2,05 +2,18 +4, ,28-0,50-1,08-1,43-0,81-0,86-0,60-0,44-0,62-1, ,25-0,12-0,27-0,44-0,36 +0,31-0,09-0,00-0,09 +0, ,59-0,48-0,66-0,73-0,53 +0,11 +0,41 +0,40-0,17 +0, ,78 +2,21 +2,32 +1,17 +1,16-1,82-0,94-2,37-1,60-1,33 In yellow the values bigger or smaller than 2/-2 In red the values bigger or smaller than 3/-3 Figure 2 : Zscore of the different laboratories for each sample. ZS calculated on the PT standard deviation sample1 sample2 sample 3 sample sample 5 sample 6 sample 7 sample sample 9 sample 10-5 Laboratory code

36 Z score Fix DETERMINATION of LACTOSE in RAW (cow) MILK - page 7/8 Table VII : Zscore of the different laboratories for each sample. ZS calculated on the standard deviation of reproducibility of the method Sample Lab code ,45-0,80-1,44-1,08-1,28-0,66-0,59-0,82-0,74-0, ,12 +1,90 +1,00 +1,24 +0,71 +1,24 +1,23 +0,72 +0,74 +1, ,70-1,83-0,38-0,18-0,95 +0,89-0,62-1,55 +0,20 +0,42 4-1,25-3,54 +0,99 +1,49 +1,69 +2,62 +2,69 +2,60 +2,44 +2, ,06 +0,73-0,38-0,04-0,15 +0,39 +0,38-0,03-0,11 +0,43 6-1,04-1,17-0,50-1,67-1,76-1,68-1,15-1,51-1,12-0,88 7-0,61-1,06-1,76-1,27-1,53-0,83-0,81-0,99-0,99-0, ,32 +1,40 +2,07 +0,59-2,26-1,70-1,28-2,36-1,92-1, ,61 +0,75-0,09 +0,62 +0,19 +0,46 +0,73 +0,56 +0,37 +1, ,22 +0,35-0,44 +2,13 +3,77 +2,74 +3,42 +3,79 +3,23 +0, ,59 +7,89 +4,67 +7,25 +6,69 +8,72 +7,92 +6,11 +4,22 +4, ,31-1,54-2,36-1,84-2,06-1,41-0,89-1,30-1,20-1, ,28-0,37-0,59-0,56-0,91 +0,50-0,13-0,01-0,17 +0, ,76-1,48-1,44-0,93-1,34 +0,17 +0,60 +1,18-0,32 +0, ,19 +6,86 +5,05 +1,50 +2,94-2,99-1,38-7,06-3,09-1,56 This table will allows to compare your ZSCORE from one PT to an other because the standard deviation has always the value of SR of the method SR=0,047 In yellow the values bigger or smaller than 2/-2 In red the values bigger or smaller than 3/-3 Figure 3 : Zscore of the different laboratories for each sample. ZS calculated on the standard deviation of reproducibility of the method sample1 sample2 1 sample 3 sample sample 5 sample 6 sample 7 sample 8-3 sample 9 sample Laboratory code

37 DETERMINATION of LACTOSE in RAW (cow) MILK - page 8/8 ICAR Interlaboratory Proficiency Study - September 2017 Trial of : 04/09/2017 0, laboratories 10 samples Sd 2 Labs OUT OF THE TARGET ( 13 % ) ,300 Student 5 % Student 5 % 0,150 0,000-0,300-0,150 0,000 0,150 0,300 _ d Figure 1 : ACCURACY - Evaluation of the individual performances (to see table I). LIST OF THE PARTICIPANTS ICAR ICAR PROFICIENCY TEST RAW MILK LACTOSE CONTENT September 2017 Name City Country Agroscope Bern-Liebefeld Switzerland Central Milk Lab ICBA Caesarea IL Department Valorisation des productions Agricoles Gembloux Belgium ILVO Melle Belgium Japan Dairy Technical Association Tokyo Japan Lab Agroalimentario de Santander Santander Cantabria Spain Laboratorio Standard Latte Maccarese Italy Laboratorium Oceny Mleka KCHZ Laboratorium Referecyjne z/s w Parzniewie Pruszkow Poland Milchprüfring Baden-Württemberg e.v. Kirchheim unter Teck Germany Milkom a.s Dairy research institute Praha Czech Republic Pieno Tyrimai Kaunas Lithuania Qlip B.V., Zutphen NL Teagasc Food research Center Cork IR The National laboratory for raw milk Agrovyzkum Rapotin s.r.o. Vikyrovice Czech Republic Valacta - Centre d Expertise en Production Laitière du Québec Quebec Canada

38 DETERMINATION of UREA in RAW (cow) MILK - page 1/8 ICAR PROFICIENCY TESTING SCHEME September 2017 Raw Milk Determination of UREA CONTENT Sending date of statistical treatment : 9 th October 2017 Frame of activity : ICAR Milk Analyses Sub Committee (MA SC) Contact : Gavin Scott gavin@milktest.co.nz ICAR Staff Silvia Orlandini pt@icar.org silvia@icar.org ACCRÉDITATION N PORTÉE DISPONIBLE SUR