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FAPAS Report 25114
Nutrit ional Components in Milk Powder
December 2013-January 2014
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FAPAS Report 25114
PARTICIPANT LABORATORY NUMBER
Participants can log in to FAPAS SecureWeb at any time to obtain their laboratory numberfor this proficiency test.
Laboratory numbers are displayed in SecureWeb next to the download link for this report.
REPORT INTEGRITY
FAPAS reports are distributed as Adobe Certified Document Services (CDS) Adobe PDFdocuments [ 1]. The use of Adobe CDS allows the PDF files to certify that the author of thereport is FAPAS and that the document has not been altered in anyway. A blue ribbon andinformation bar indicates this validation when the document is opened using Adobe Reader v7 or later.
Hard copies of FAPAS reports can never incorporate this level of integrity and consequentlywhen a FAPAS report is printed a watermark, stating that printed copies are not controlled,appears on every page.End users of FAPAS reports should ensure that either the opened PDF file displays a validFAPAS digital signature or that the content of any hard copy exactly matches the content ofa PDF file that displays a valid FAPAS digital signature.
QUALITY SYSTEMS
FAPAS is accredited by UKAS as complying withthe requirements of ISO/IEC 17043:2010 [ 2].
The Food and Environment Research Agency isan ISO 9001 certified organisation.
0009
DEFRA hereby excludes all liability for any claim, loss, demands or damages of any kindwhatsoever (whether such claims, loss, demands or damages were foreseeable, known orotherwise) arising out of or in connection with the preparation of any technical or scientificreport, including without limitation, indirect or consequential loss or damage; loss of actual oranticipated profits (including loss of profits on contracts); loss of revenue; loss of business;loss of opportunity; loss of anticipated savings; loss of goodwill; loss of reputation; loss ordamage to or corruption of data; loss of use of money or otherwise, and whether or notadvised of the possibility of such claim, loss demand or damages and whether arising in tort
(including negligence), contract or otherwise. This statement does not affect your statutoryrights.
Nothing in this disclaimer excludes or limits DEFRAs liability for: (a) death or personal injurycaused by DEFRAs negligence (or that of its employees, agents or directors); or (b) the tortof deceit; [or (c) any breach of the obligations implied by Sale of Goods Act 1979 or Supplyof Goods and Services Act 1982 (including those relating to the title, fitness for purpose andsatisfactory quality of goods);] or (d) any liability which may not be limited or excluded by law(e) fraud or fraudulent misrepresentation.
The parties agree that any matters are governed by English law and irrevocably submit tothe non-exclusive jurisdiction of the English courts.
Crown Copyright 2014
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FAPAS Report 25114
SUMMARY
1. The test material for FAPAS proficiency test 25114 was dispatched in December 2013.
Each participant received a milk powder test material to be analysed for moisture, ash,
total fat, nitrogen, titratable acidity and lactose.
2. An assigned value ( x a ) was determined for each analyte and in conjunction with the
standard deviation for proficiency ( p ) was used to calculate a z-score for each result .
3. Results for this proficiency test are summarised as follows:
analyte assigned value, x a g/100g
number of scores,|z| 2
total numberof scores
% |z| 2
moisture 3.34 77 92 84
ash 6.08 70 80 88
total fat 21.35 78 91 86
nitrogen 4.44 81 83 98
titratable acidity 1.09 34 59 58
lactose 39.45 53 62 85
4. Surplus test materials are available for sale, see APPENDIX II.
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FAPAS Report 25114
CONTENTS
1. INTRODUCTION 5
1.1. Proficiency Testing 5
2. TEST MATERIAL 5 2.1. Preparation 5 2.2. Homogeneity 5 2.3. Dispatch 5
3. RESULTS 5
4. STATISTICAL EVALUATION OF RESULTS 6
4.1. Calculation of the Assigned Value, x a 6 4.2. Standard Deviation for Proficiency, p 6 4.3. Individual z-Scores 6
5. INTERPRETATION OF SCORES 7
6. REFERENCES 7
TABLES
Table 1: Results and z-Scores 8
Table 2: Participants Comments 15
Table 3: Assigned Values and Standard Deviations for Proficiency 15
Table 4: Number and Percentage of z-Scores where |z| 2 15
FIGURES
Figure 1:
z-Scores for moisture 16
Figure 2: z-Scores for ash 17
Figure 3: z-Scores for total fat 18
Figure 4: z-Scores for nitrogen 19
Figure 5: z-Scores for titratable acidity 20
Figure 6: z-Scores lactose 21
APPENDICES
APPENDIX I: Analytical Methods Used by Participants 22
APPENDIX II:
FAPAS SecureWeb, Protocol and Contact Details 36
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FAPAS Report 25114
1. INTRODUCTION
1.1. Proficiency Testing
Proficiency testing aims to provide an independent assessment of the competence ofparticipating laboratories. Together with the use of validated methods, proficiency testing isan essential element of laboratory quality assurance.
Further details of the FAPAS proficiency testing scheme are available in ourprotocols [ 3, 4].
2. TEST MATERIAL
2.1. Preparation
Preparation of the samples for this proficiency test was sub-contracted to a laboratorymeeting the quality requirements of the schemes accreditation [2].
The test material was prepared from a blend of full-fat milk powder and skimmed milkpowder.
Samples were stored at ambient temperature until dispatch.
2.2. Homogeneity
To test for homogeneity, randomly selected test materials were analysed in duplicate.Testing was sub-contracted to a laboratory meeting the quality requirements of the schemesaccreditation [2].
These data showed sufficient homogeneity and were not included in the subsequentcalculation of the assigned values.
2.3. Dispatch
The start date was 13 December 2013. Test materials were sent to 110 participants.
3. RESULTS
The instructions for reporting results were as follows:
Determine the level of moisture, ash, total fat, nitrogen, titratable acidity and lactosepresent in the test material, in g/100g, as received.
If you analyse for total fat, it is essential that you tell us whether you have used an acidor alkaline hydrolysis method.
For titratable acidity, express results as lactic acid and report as g/100g of dry sample. Lactose is to be reported as anhydrous lactose.
Results were submitted by 103 participants (94%) before the closing date for this test,24 January 2014.
Each participant was given a laboratory number, assigned in order of receipt of results. Thereported analyte concentrations are given in Table 1.
Participants comments are given in Table 2.
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The analytical methods used by each participant are summarised in APPENDIX I.
4. STATISTICAL EVALUATION OF RESULTS
The results submitted by participants were statistically analysed in order to provide anassigned value for each analyte. The assigned values were then used in combination withthe standard deviation for proficiency, p , to calculate a z-score for each result. Theprocedure follows that recommended in the IUPAC International Harmonised Protocol for theProficiency Testing of Analytical Chemistry Laboratories [ 5].
Further details on the procedure followed can be found in the relevant protocols [3, 4].
4.1. Calculation of the Assigned Value, x a
The assigned value, x a , for each analyte was derived from the consensus of the resultssubmitted by participants.
The following results were excluded from the calculation of the assigned value:
i) results for total fat that did not state use of either acid or alkaline hydrolysis,
ii) results for nitrogen that appeared to be for protein,
iii) results for titratable acidity that were considered to be reporting errors.
For moisture, ash, total fat, and nitrogen this procedure was straightforward and the robustmean was chosen as the assigned value.
For titratable acidity and lactose the major mode was chosen as the assigned value becauseit was evident that there was a clear multi-modal distribution for titratable acidity and a slightskewing of the distribution for lactose.
The assigned values for all analytes are shown in Table 3.
4.2. Standard Deviation for Proficiency, p
The standard deviation for proficiency, p , was set at a value that reflects best practice forthe analyses in question.
For nitrogen, p was derived from the appropriate form of the Horwitz equation [ 6].
For moisture and ash, p was derived from collaborative trial data [ 7].
For total fat, titratable acidity and lactose, p was calculated using fitness-for-purpose criteriabased on expert advice.
The values for p used to calculate z-scores from the reported results of this test are given inTable 3.
4.3. Individual z-Scores
Participants z-scores were calculated as:
p
a x x z
)( =
where x = the participants reported result,
x a = the assigned value
and p = the standard deviation for proficiency.
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FAPAS Report 25114
Participants z-scores for all analytes are given in Table 1 and are shown as histograms inFigures 16. It is possible for the z-scores published in this report to differ slightly from thez-score that can be calculated using the formula given above. These differences arise fromthe necessary rounding of the actual assigned values and standard deviations for proficiencyprior to their publication in Table 3.
The number and percentage of z-scores in the range -2 z 2 for all analytes are given inTable 4.
5. INTERPRETATION OF SCORES
In normal circumstances, over time, about 95% of z-scores will lie in the range -2 z 2.Occasional scores in the range 2
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Table 1 (continued): Results and z-Scores
laboratorynumber
analyte
moisture ash total fat nitrogen titratable acidity lactoseassigned value
3.34 g/100gassigned value
6.08 g/100gassigned value21.35 g/100g
assigned value4.44 g/100g
assigned value1.09 g/100g
assigned value39.45 g/100g
result z-score result z-score result hydrolysis? z-score result z-score result z-score result z-score
016 3.56 1.2 6.04 -0.5 21.10 yes -0.4 4.58 1.0 1.10 0.1 38.30 -0.9
017 3.27 -0.4 5.95 -1.7 20.38 -1.5 4.41 -0.2 0.16 -9.5 39.70 0.2
018 3.25 -0.5 5.84 -3.1 21.54 0.3 4.41 -0.2 41.5 1.6
019 3.2 -0.8 6.1 0.2 21.2 yes -0.2 4.51 0.5 1.19 1.0 39.7 0.2
020 3.49 0.8 6.10 0.2 21.75 No 0.6 4.53 0.6 0.969 -1.2 37.20 -1.8
021 3.45 0.6 21.24 -0.2 4.44 0.0 38.78 -0.5
022 3.5 0.9 6.1 0.2 21.3 YES -0.1 4.4 -0.3 1.45 3.7 40.46 0.8
023 3.37 0.2 21.02 -0.5
024 3.47 0.7 6.24 2.0 21.46 0.2 4.49 0.3 1.11 0.2 39.21 -0.2
025 1.92 -7.7 20.72 Yes -1.0 0.64 -4.6
026 3.28 -0.3 6.01 -0.9 21.0 yes -0.5 4.22 -1.6 15.7 148.9 41.90 2.0
027 3.32 -0.1 6.10 0.2 21.98 yes 1.0 4.38 -0.4
028 3.37 0.2 6.12 0.5 21.17 No -0.3 4.26 -1.3 8.66 77.1 40.29 0.7
029 3.39 0.3 6.07 -0.1 21.30 Yes -0.1 4.41 -0.2
030 3.45 0.6 6.27 2.4 21.36 yes 0.0 4.52 0.5
z-scores outside |z| >2 are shown in bold, see Section 5
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Table 1 (continued): Results and z-Scores
laboratorynumber
analyte
moisture ash total fat nitrogen titratable acidity lactoseassigned value
3.34 g/100gassigned value
6.08 g/100gassigned value21.35 g/100g
assigned value4.44 g/100g
assigned value1.09 g/100g
assigned value39.45 g/100g
result z-score result z-score result hydrolysis? z-score result z-score result z-score result z-score
031 3.30 -0.2
032 3.00 -1.9 6.14 0.7 21.43 no 0.1 4.515 0.5 0.9959 -1.0 41.89 2.0
033 2.08 no -30.1
034 3.19 -0.8 6.04 -0.5 22.24 YES 1.4 4.37 -0.5 1.06 -0.3
035 3.46 0.6 6.00 -1.0 21.40 0.1 4.46 0.1 0.112 -10.0 35.08 -3.5
036 21.48 NO 0.2 4.501 0.4
037 3.50 0.9 6.14 0.7 21.0 yes -0.5 4.43 -0.1 0.144 -9.6 39.00 -0.4
038 3.61 1.5 6.12 0.5 21.28 yes -0.1 4.36 -0.6
039 3.03 -1.7 5.97 -1.4 21.31 yes -0.1 4.53 0.6
040 2.76 -3.2 6.21 1.6 21.0 yes -0.5 4.43 -0.1 1.42 3.4 3.71 -28.5
041 3.67 1.8
042 3.49 0.8 6.16 1.0 21.20 Yes -0.2 4.27 -1.2 1.22 1.3 41.57 1.7
043 3.15 -1.0 6.06 -0.3 20.9 yes -0.7 4.40 -0.3 38.3 -0.9
044 3.65 1.7 6.20 1.5 21.45 yes 0.2 4.52 0.5 0.88 -2.1 38.65 -0.6
045 21.68 0.87 4.48 0.3 40.1 0.5
z-scores outside |z| >2 are shown in bold, see Section 5
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Table 1 (continued): Results and z-Scores
laboratorynumber
analyte
moisture ash total fat nitrogen titratable acidity lactoseassigned value
3.34 g/100gassigned value
6.08 g/100gassigned value21.35 g/100g
assigned value4.44 g/100g
assigned value1.09 g/100g
assigned value39.45 g/100g
result z-score result z-score result hydrolysis? z-score result z-score result z-score result z-score
046 3.04 -1.6 6.11 0.4 19.95 Yes -2.2 4.424 -0.1 1.23 1.4
047 3.01 -1.8 6.05 -0.4 20.01 yes -2.1 4.44 0.0 1.36 2.7 37.84 -1.3
048 5.97 14.3 28.7 286.1 21.3 no -0.1 4.49 0.3 0.11 -10.0 38.9 -0.4
049 3.40 0.3 6.21 1.6 21.49 no 0.2 4.46 0.1 1.08 -0.1
050 3.43 0.5 6.28 2.5 20.92 yes -0.7 28.12 166.8 1.25 1.6 40.42 0.8
051 3.39 0.3 21.99 no 1.0 4.429 -0.1 0.106 -10.0 39.01 -0.3
052 21.39 0.1
053 3.03 -1.7 6.06 -0.3 21.5 0.2 4.34 -0.7 1.02 -0.7
054 3.10 -1.3 6.10 0.2 21.04 Yes -0.5 4.43 -0.1
055 6.0 -1.0 20.2 no -1.8
056 3.69 1.9 6.13 0.6 20.94 Yes -0.6 4.36 -0.6
057 3.46 0.6 6.07 -0.1 21.41 No 0.1 4.52 0.5 1.20 1.1 38.37 -0.9
058 3.02 -1.8 6.04 -0.5 23.61 yes 3.5 4.50 0.4 0.122 -9.9 40.11 0.5
059 3.45 0.6 6.01 -0.9 19.0 yes -3.7 4.49 0.3 38.5 -0.8
060 3.60 1.4 6.05 -0.4 21.4 yes 0.1 40.4 0.8
z-scores outside |z| >2 are shown in bold, see Section 5
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Table 1 (continued): Results and z-Scores
laboratorynumber
analyte
moisture ash total fat nitrogen titratable acidity lactoseassigned value
3.34 g/100gassigned value
6.08 g/100gassigned value21.35 g/100g
assigned value4.44 g/100g
assigned value1.09 g/100g
assigned value39.45 g/100g
result z-score result z-score result hydrolysis? z-score result z-score result z-score result z-score
061 2.06 -7.0 6.07 -0.1 22.7 yes 2.1 4.53 0.6 0.9 -1.9
062 2.97 -2.0 6.71 7.9 20.19 -1.8 4.58 1.0 1.45 3.7
063 3.73 2.1 6.07 -0.1 22.7 2.1 4.70 1.8 0.87 -2.2 42 2.0
064 3.21 -0.7 6.02 -0.8
065 3.27 -0.4 6.08 0.0 21.64 No 0.5 4.42 -0.2 40.50 0.8
066 3.20 -0.8 6.12 0.5 21.57 no 0.4 4.348 -0.7 0.138 -9.7 37.435 -1.6
067 22.70 2.1
068 2.50 -4.6 6.14 0.7 19.8 -2.4 4.28 -1.1 1.30 2.1
069 3.22 -0.7 5.71 -4.7 22.07 1.1 4.43 -0.1 0.14 -9.7 33.47 -4.8
070 3.35 0.0 4.59 1.0 39.97 0.4
071 3.28 -0.3 6.10 0.2 21.71 0.6 4.47 0.2 0.96 -1.3 39.20 -0.2
072 3.54 1.1 6.10 0.2
073 3.17 -0.9 5.94 -1.8 21.17 no -0.3 4.39 -0.4
074 3.43 0.5 6.14 0.7 7.35 no -21.9 4.42 -0.2 1.11 0.2 5.31 -27.3
075 3.21 -0.7 6.13 0.6 21.5 0.2 4.37 -0.5 39.4 0.0
z-scores outside |z| >2 are shown in bold, see Section 5
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Table 1 (continued): Results and z-Scores
laboratorynumber
analyte
moisture ash total fat nitrogen titratable acidity lactoseassigned value
3.34 g/100gassigned value
6.08 g/100gassigned value21.35 g/100g
assigned value4.44 g/100g
assigned value1.09 g/100g
assigned value39.45 g/100g
result z-score result z-score result hydrolysis? z-score result z-score result z-score result z-score
076 3.58 1.3 6.12 0.5 21.3 No -0.1 4.53 0.6 38.9 -0.4
077 3.07 -1.5 5.92 -2.0 21.40 0.1 4.51 0.5 40.20 0.6
078 3.25 -0.5 6.15 0.9 21.54 Yes 0.3 4.53 0.6 1.32 2.3 42.91 2.8
079 21.6 No 0.4 4.50 0.4
080 6.14 0.7 21.67 No 0.5 37.58 -1.5
081 - - - - - -
082 3.33 -0.1 5.65 -5.5 21 no -0.5 4.20 -1.7
083 3.90 3.0 5.9 -2.3 21.6 0.4 4.29 -1.1 0.77 -3.3
084 3.32 -0.1 6.05 -0.4 21.37 0.0 4.21 -1.6 1.115 0.3 39.85 0.3
085 3.40 0.3 6.14 0.7 21.6 0.4 4.22 -1.6 1.08 -0.1 38.57 -0.7
086 2.26 -5.9 6.10 0.2 21.98 No 1.0 4.52 0.5 1.16 0.7 40.60 0.9
087 3.52 1.0 6.12 0.5 3.00 NO -28.6 4.42 -0.2
088 2.48 -4.7 5.98 -1.3 20.37 Yes -1.5 4.30 -1.0 1.07 -0.2 39.07 -0.3
089 2.71 -3.4 6.11 0.4 18.11 No -5.1 4.47 0.2
090 3.35 0.0 5.93 -1.9 21.46 0.2 4.28 -1.1 1.12 0.3 42.65 2.6
z-scores outside |z| >2 are shown in bold, see Section 5
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Table 1 (continued): Results and z-Scores
laboratorynumber
analyte
moisture ash total fat nitrogen titratable acidity lactoseassigned value
3.34 g/100gassigned value
6.08 g/100gassigned value21.35 g/100g
assigned value4.44 g/100g
assigned value1.09 g/100g
assigned value39.45 g/100g
result z-score result z-score result hydrolysis? z-score result z-score result z-score result z-score
091 3.17 -0.9 6.05 -0.4 21.12 -0.4 4.71 1.9 1.34 2.5 41.83 1.9
092 3.35 0.0 6.15 0.9 21.4 Yes 0.1 4.50 0.4 38.7 -0.6
093 3.21 -0.7 6.04 -0.5 21.10 -0.4 4.503 0.4 38.99 -0.4
094 38.55 -0.7
095 3.28 -0.3 6.30 2.8 21.80 0.7 4.51 0.5 1.09 0.0 37.06 -1.9
096 3.34 0.0 6.07 -0.1 21.64 yes 0.5 4.47 0.2 1.61 5.3 36.98 -2.0
097 3.63 1.6 5.94 -1.8 21.80 0.7 4.39 -0.4 1.09 0.0
098 3.53 1.0 20.59 YES -1.2 4.53 0.6 1.0164 -0.8
099 3.80 2.5 6.05 -0.4 21.35 yes 0.0 4.39 -0.4 1.01 -0.8 40.03 0.5
100 3.56 1.2 6.04 -0.5 21.76 no 0.6 4.30 -1.0 38.99 -0.4
101 3.63 1.6 5.97 -1.4 22.24 No 1.4 4.23 -1.5 41.2 1.4
102 3.75 2.2 6.05 -0.4 21.17 no -0.3 4.543 0.7 0.58 -5.2 43.26 3.0
103 4.05 3.9 5.89 -2.4 4.38 -0.4 1.12 0.3
z-scores outside |z| >2 are shown in bold, see Section 5
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Table 2: Participants Comments
participant number comments
088 Titratable acidity is reported on dry basis of sample & Lactose is reported asanhydrous Lactose
097 titratable acidity as lactic acid in sample as it is: 1.05 g/100g
comments are as submitted by participants
Table 3: Assigned Values and Standard Deviations for Proficiency
analyte data points,
n
assigned value,
x a , g/100g
uncertainty,
u
standard deviation for
proficiency,
p , g/100g
moisture 92 3.34 0.0270 Coll. Trial [7] 0.184
ash 80 6.08 0.0100 Coll. Trial [7] 0.0791
total fat 74 21.35 0.0601 ffp 0.640
nitrogen 81 4.44 0.0109 Horwitz [6] 0.142
titratable acidity 57 1.09 0.0254 ffp 0.0981
lactose 61 39.45 0.328 ffp 1.25
ffp = fitness-for-purpose criteria
Table 4: Number and Percentage of z-Scores where |z| 2
analyte number of scores where|z| 2
total numberof scores
% |z| 2
moisture 77 92 84
ash 70 80 88
total fat 78 91 86
nitrogen 81 83 98titratable acidity 34 59 58
lactose 53 62 85
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FAPAS Report 25114
Figure 1: z-Scores for moisture
2 5
6 1
8 6
8 8
6 8
9 8 9
4 0
6 2
3 2
4 7
5 8
3 9
5 3
4 6
7 7
5 4
4 3
1 2
7 3
9 1
5 3 4
4 1 9
6 6
6 4
7 5
9 3
6 9
8 1 8
7 8
1 7
6 5
2 6
7 1
9 5
2 3 1
1 2 7
8 4
8 2
9 6
7 0
9 0
9 2
2 3
2 8
2 9
5 1
4 9
8 5
7 1 5
5 0
7 4
2 1
3 0
5 9
3 5
5 7
2 4
1 1
2 0
4 2
2 2
3 7
6 8 7
1 4
9 8
3 7 2
1 6
1 0 0
7 6
6 0
3 8
9 7
1 0 1
4 4
4 1
5 6
6 3
1 0 2
9 9
1 0
8 3
1 0 3
4 8
3.71 g/100g
3.34 g/100g
2.97 g/100g
-8.0
-6.0
-4.0
-2.0
0.0
2.0
4.0
6.0
z - s c or e
Laboratory Number
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Figure 2: z-Scores for ash
8 2
6 9
1 8
1 0 3
8 3
7 7
9 0
7 3
9 7
1 7
3 9
1 0 1
8 8
3 5
5 5
2 6
5 9
6 4
1 6
3 4
5 8
9 3
1 0 0
7 4 7
6 0
8 4
9 1
9 9
1 0 2
4 3
5 3
2 9
5 7
6 1
6 3
9 6
1 5
6 5
1 4
1 9
2 0
2 2
2 7
5 4
7 1
7 2
8 6
9 4 6
8 9
2 8
3 8
6 6
7 6
8 7
3 8 5 6
7 5
3 2
3 7
6 8
7 4
8 0
8 5
7 8
9 2
5 4 2
2 4 4
4 0
4 9
2 4
3 0
5 0
9 5
6 2
4 8
6.24 g/100g
6.08 g/100g
5.92 g/100g
-6.0
-4.0
-2.0
0.0
2.0
4.0
6.0
8.0
10.0
z - s c or e
Laboratory Number
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Figure 3: z-Scores for total fat
3 3
1 1
8 7
7 4
8 9
5 9
6 8
4 6
4 7
6 2
5 5
8 8
1 7
9 8
2 5
4 3
5 0
5 6
1 2
2 6
3 7
4 0
8 2
2 3
5 4
2 1 6
9 3
9 1
2 8
7 3
1 0 2
1 9
4 2
7 2 1
3 8
2 2
2 9
4 8
7 6
3 9
1 5
3 9 9
3 0
8 4
5 2
1 0
1 4
3 5
6 0
7 7
9 2
5 7
3 2
4 4
2 4
9 0
3 6
4 9
4 5 3
7 5
1 8
7 8
6 6
7 9
8 3
8 5
6 5
9 6
8 0
7 1
2 0
1 0 0
9 5
9 7
9 2 7
8 6
5 1
5 6 9
3 4
1 0 1
8 6 1
6 3
6 7
5 8
22.63 g/100g
21.35 g/100g
20.06 g/100g
-8.0
-6.0
-4.0
-2.0
0.0
2.0
4.0
z - s c or e
Laboratory Number
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Figure 4: z-Scores for nitrogen
8 2
8 4
2 6
8 5
1 0 1
2 8
4 2
6 8
9 0
8 3
8 8
1 0 0
5 3
6 6
3 8
5 6
3 4
7 5
8 2 7
1 0 3
7 3
9 7
9 9
2 2
4 3
7 1 7
1 8
2 9
6 5
7 4
8 7
4 6
5 1
3 7
4 0
5 4
6 9
2 1
4 7
3 5
4 9
7 1
8 9
9 6
4 5
2 4
4 8
5 9
1 5
5 8
7 9
9 2
3 6
9 3
1 0
1 9
7 7
9 5
3 2
3 3 0
4 4
5 7
8 6
2 1 4
2 0
3 9
6 1
7 6
7 8
9 8
1 0 2
9 1 6
6 2
7 0
6 3
9 1
5 0
5
4.73 g/100g
4.44 g/100g
4.16 g/100g
-3.0
-2.0
-1.0
0.0
1.0
2.0
3.0
4.0
5.0
6.0
z - s c or e
Laboratory Number
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Figure 5: z-Scores for titratable acidity
5 1
4 8
3 5
1 1
5 8
6 6
6 9
3 7
5 1 7
1 0 2
2 5
8 3
6 3
4 4
6 1
6 7 1
2 0
1 5
1 4
3 2
9 9
9 8
5 3
3 4
8 8
9 3 4 9
8 5
9 5
9 7
1 6
2 4
7 4
8 4
9 0
1 0 3
1 8 6
1 0
1 9
5 7
4 2
4 6
1 2
5 0
8 6 8
7 8
9 1
4 7
4 0
2 2
6 2
9 6
2 8
2 6
1.29 g/100g
1.09 g/100g
0.89 g/100g
-10.0
-8.0
-6.0
-4.0
-2.0
0.0
2.0
4.0
6.0
8.0
10.0
z - s c or e
Laboratory Number
2.52.01.51.00.50.0
2.0
1.5
1.0
0.5
0.0
Analytical result (g/100g)
D e n s i t y
Adaptive kernel density plot - titratable acidity
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APPENDIX I: Analyt ical Methods Used by Participant s
Methods are tabulated according to the information supplied by participants, but someresponses may have been combined or edited for clarity.
Moisture
Method Used Accredited laboratory number
yes 003 004 006 008 009 010 012 014 016 019021 023 024 025 026 030 031 032 034 035037 039 043 047 048 049 053 056 057 059063 066 070 074 075 076 078 082 083 084088 089 090 091 093 095 097 098 099
no 001 005 007 017 018 028 038 040 050 051062 065 068 071
Method Based On laboratory number
International Standard 001 003 004 006 008 009 010 012 016 024031 047 049 051 057 063 065 068 071 076078 088 093
National Standard 007 014 017 021 023 026 028 035 037 038040 043 050 059 062 066 070 074 082 083084 090 091 095 098 099
Manufacturer/Kit Instructions/TechnicalNote
005
In house method 018 019 025 032 075 089 097
Sample Weight (g) laboratory number
1 -
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Moisture Determination Procedure(continued)
laboratory number
Drying furnace 005
IS16072:2012 090
Appar atu s u sed for c on stant weigh t laborato ry numb er
conventional oven 001 004 005 007 009 010 012 014 016 017018 019 021 023 024 025 028 031 035 038040 043 049 050 056 059 062 063 065 066068 070 071 074 075 078 082 083 084 089091 093 095 097 098 099
heated in beaker 026 037
vacuum oven 008 032 047 057 088
convection oven 076Hot Air Oven 090
oven with dryed air 006
Reference Drier RD-8 Funke Gerber 051
Oven Temperature (C) for moist uredetermination
laboratory number
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Steps Taken To Avoid Spattering(continued)
laboratory number
pre-dried in oven 005 007 016 019 034 035 037 038 095 097099
slow temperature ramp 014 040 049 057 065 075 078 080 088Control sample kept 018
pre-burned with Bunsen 050
TGA (Leco) 003
Ash Furnac e Temp eratur e (C) laborato ry numb er
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Method Based On laboratory number
International Standard 003 004 008 009 010 012 016 021 036 045047 051 052 057 063 065 067 068 071 076078 080 093 095
National Standard 007 014 017 023 026 028 035 037 038 040043 048 049 055 062 066 074 079 082 083084 088 090 091 098 099
Manufacturer/Kit Instructions/TechnicalNote
005 025 033 059
In house method 018 019 024 032 034 056 075 089 097
Sample Weight (g) laboratory number
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Total Fat Extraction Method (continu ed) laboratory number
ASE (accelerated solvent extraction) 093
Butirometric Method 050
Butyrometer 059Gerber method 004 037 040
IR (AOAC 972.16) 045
Liposuction bottle 035
Milkoscan FT120 005
simple extraction (seperatory funnels) 053
Pre-extraction Stage laboratory number
yes 005 008 014 019 023 025 032 036 062 083
088 089 095 099no 004 007 009 012 016 017 018 021 024 026
028 030 033 034 037 038 039 040 043 045047 049 050 051 053 056 057 059 063 065066 067 068 071 074 075 076 078 079 080082 084 090 091 093 097 098
Pre-extraction Time (hours) laboratory number
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Extraction Solvent Components(continued)
laboratory number
Ethyl alcohol 095
no solvent extraction - only separation offat and measure in a butyrometer
037
petroleum benzine 010
Methyl tert-butyl ether 051
sulfuric acid 059
amyl alcohol 059
Total Extraction Time (Hours) laboratory number
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Sample Weight (g) laboratory number
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Catalyst (contin ued) laboratory number
titanium (Ti) 021 037 043 049
Catalyst Kjeltabs(3.5 g K2SO4 + 3.5 mg Se)
078
CuSO4 KSO4 035
HgO 047
K , Cu 026
kjeltab 032
Potassium sulphate and Copper sulphate 008
selenium (Se) + potassium sulphate 097
Titratable Acidity
Method Used Accredited laboratory number
yes 001 006 008 009 010 012 014 016 026 034035 037 047 049 053 062 063 066 083 084088 090 091 095 097 099
no 003 005 017 019 024 025 028 032 040 048050 051 057 068 071 074 078
Method Based On laboratory number
International Standard 001 006 009 010 024 047 048 051 057 063
068 074National Standard 014 017 026 028 035 037 040 050 062 066
083 084 088 090 091 095 099
Paper Published In An InternationalJournal
025
In house method 005 019 097
Sample Weight (g) laboratory number
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Titration Reagents (Acidit y) (continu ed) laboratory number
sodium hydroxide 001 005 006 008 010 012 017 024 025 028032 034 035 037 040 047 049 050 051 057062 063 066 068 071 078 083 084 088 091
095 099pH meter 014
Titration Method (Peroxide and Acidit y) laboratory number
add water 001 003 010 014 026 028 035 040 062 066071 074 083 084 090 091 095 097
mix sample and reagents 010 017 028 035 037 040 084 091 095
Titration of Free Fatty Acids laboratory number
phenolphthalein 001 003 008 024 028 037 040 062 066 071090 095
sodium hydroxide 008 010 014 017 024 026 028 035 040 062074 095
Other Method laboratory number
IS:1165:2002 090
ISO6091:2010 001
Lactose
Method Used Accredited laboratory number
yes 003 006 012 013 014 021 024 026 035 037043 045 047 048 059 063 065 070 071 075076 078 084 088 090 091 093 095 099
no 005 009 016 017 018 019 028 032 040 050051 057 066 074 080
Reference laboratory number
1991 026
1995 095
1999 032
AOAC Official Methods 048
AOAC Official Methods 1993 18 047
AOAC Official Methods 1996 33.2.31Chapter 33 Page 22
045
AOAC Official Methods 2005 - - 080
AOAC Official Methods 2005 18th EditionCh 33, P.17
071
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Reference (continu ed) laboratory number
AOAC Official Methods 2011 Fructose,Glucose, Lactose, Maltose and Sucrosein Milk Chocolate 31.5.04
065
DGHS Lab Manual No. 1 2005 85 028FIL-IDF 1989 IDF 79A 057
GB 2008 GB/T 22221-2008 014
GB 5413.5-2010 035
IDF Standard 2007 198 First edition 021
In house 018 059 063 075
Indian Standards - 4079 -1967 1995 095
in house 1985 L40.00-7 093
in house method 1999 032
internal method 074
IS 1479 Part 2:1961 2003 25 091
IS -1479-P2,1961 2003 - 25 084
IS:1479:Part-2:1961 IS:1479:Part-2:1961Page no-25
090
ISO 003 006
J. AOAC Int. 1979 62 1292 024
J. AOAC Int. 1992 Vol.75 No.3 443-464 078
Lane Eynon 070LMBG Method 1983 043
Manufacturer's Instructions 076 099
Manufacturer's Instructions 1980 016
Manufacturer's Instructions 2003 15GB 005
MAPA 2009 040
National Standard 1991 026
NIN (By Difference) 009
OICCC 1989 Analytical Method 34 051
R-Biopharm 099
SLMB 017
29248-91 1991 Vol 5 Page 4 037
Sample Weight (g) laboratory number
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Sample Weight (g) (continu ed) laboratory number
5 -
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APPENDIX II: FAPAS SecureWeb, Protocol and Contact Detail s
1. FAPAS SECUREWEB
Access to the secure area of our website is only available to participants in our proficiencytests. Please contact us if you require a UserID and Password. FAPAS SecureWeb allowsparticipants to:
Obtain their laboratory numbers for the proficiency tests in which they haveparticipated.
View the results they submitted in past and current proficiency tests. Submit their results and methods for current tests. Review future tests they have ordered. Order proficiency tests and quality control materials.
Freely download copies of reports (PDF file), of proficiency tests in which they haveparticipated. View charts of their z-scores obtained in previous FAPAS proficiency tests.
2. PROTOCOL
The Protocols [3, 4] set out how FAPAS is organised. Copies can be downloaded from ourwebsite.
3. CONTACT DETAILS
This report was prepared and authorised on behalf of FAPAS by Jennifer Leak (RoundCoordinator). Participants with any comments or concerns about this proficiency test shouldcontact:
FAPAS
The Food and Environment Research AgencySand Hutton
YorkYO41 1LZ
UK
Tel: +44 (0)1904 462100Fax: +44 (0)1904 500440
[email protected]@fapas.com
www.fapas.com
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