Leche Polvo (25114) Enero 2014

FAPAS Report 25114
Nutritional Components in Milk Powder
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December 2013-January 2014
Page 1 of 36
FAPAS Report 25114
PARTICIPANT LABORATORY NUMBER

Participants can log in to FAPAS SecureWeb at any time to obtain their laboratory number
for 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 PDF
documents [1]. The use of Adobe CDS allows the PDF files to certify that the author of the
report is FAPAS and that the document has not been altered in anyway. A blue ribbon and
information bar indicates this validation when the document is opened using Adobe
Reader v7 or later.
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Hard copies of FAPAS reports can never incorporate this level of integrity and consequently
when a FAPAS report is printed a watermark, stating that printed copies are not controlled,
appears on every page.
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End users of FAPAS reports should ensure that either the opened PDF file displays a valid
FAPAS digital signature or that the content of any hard copy exactly matches the content of
a PDF file that displays a valid FAPAS digital signature.
QUALITY SYSTEMS
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FAPAS is accredited by UKAS as complying with

the requirements of ISO/IEC 17043:2010 [2].
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The Food and Environment Research Agency is

an ISO 9001 certified organisation.
0009
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DEFRA hereby excludes all liability for any claim, loss, demands or damages of any kind
whatsoever (whether such claims, loss, demands or damages were foreseeable, known or
otherwise) arising out of or in connection with the preparation of any technical or scientific
report, including without limitation, indirect or consequential loss or damage; loss of actual or
anticipated 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 or
damage to or corruption of data; loss of use of money or otherwise, and whether or not
advised 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 statutory
rights.
Nothing in this disclaimer excludes or limits DEFRAs liability for: (a) death or personal injury
caused by DEFRAs negligence (or that of its employees, agents or directors); or (b) the tort
of deceit; [or (c) any breach of the obligations implied by Sale of Goods Act 1979 or Supply
of Goods and Services Act 1982 (including those relating to the title, fitness for purpose and
satisfactory 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 to
the non-exclusive jurisdiction of the English courts.
Crown Copyright 2014
Page 2 of 36
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 (xa) 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:
number of scores,
total number
g/100g
|z| 2
of scores
moisture
3.34
77
ash
6.08
70
total fat
21.35
78
nitrogen
4.44
titratable acidity
1.09
lactose
39.45
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assigned value, xa
80
88
91
86
81
83
98
34
59
58
53
62
85
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84
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4. Surplus test materials are available for sale, see APPENDIX II.
Page 3 of 36
% |z| 2
92
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analyte
FAPAS Report 25114
CONTENTS
1. INTRODUCTION
1.1. Proficiency Testing
2. TEST MATERIAL
2.1. Preparation
2.2. Homogeneity
2.3. Dispatch
5
5
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3. RESULTS
4. STATISTICAL EVALUATION OF RESULTS
4.1. Calculation of the Assigned Value, xa

4.2. Standard Deviation for Proficiency, p
4.3. Individual z-Scores
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5. INTERPRETATION OF SCORES
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6. REFERENCES
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TABLES
Results and z-Scores
Table 2:
Participants Comments
Table 3:
Assigned Values and Standard Deviations for Proficiency
15
Table 4:
Number and Percentage of z-Scores where |z| 2
15
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Table 1:
FIGURES
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15
z-Scores for moisture
Figure 2:
z-Scores for ash
Figure 3:
z-Scores for total fat
Figure 4:
z-Scores for nitrogen
19
Figure 5:
z-Scores for titratable acidity
20
Figure 6:
z-Scores lactose
21
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Figure 1:
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APPENDIX II:
APPENDIX I:
17
18
APPENDICES
16
Analytical Methods Used by Participants
22
FAPAS SecureWeb, Protocol and Contact Details
36
Page 4 of 36
FAPAS Report 25114
1. INTRODUCTION
1.1. Proficiency Testing
Proficiency testing aims to provide an independent assessment of the competence of
participating laboratories. Together with the use of validated methods, proficiency testing is
an essential element of laboratory quality assurance.
Further details of the FAPAS proficiency testing scheme are available in our
protocols [3, 4].
2. TEST MATERIAL
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2.1. Preparation
IN
Preparation of the samples for this proficiency test was sub-contracted to a laboratory
meeting the quality requirements of the schemes accreditation [2].
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The test material was prepared from a blend of full-fat milk powder and skimmed milk
powder.
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Samples were stored at ambient temperature until dispatch.
2.2. Homogeneity
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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 schemes
accreditation [2].
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These data showed sufficient homogeneity and were not included in the subsequent
calculation of the assigned values.
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2.3. Dispatch
3. RESULTS
The start date was 13 December 2013. Test materials were sent to 110 participants.
The instructions for reporting results were as follows:

Determine the level of moisture, ash, total fat, nitrogen, titratable acidity and lactose
present 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 acid
or 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. The
reported analyte concentrations are given in Table 1.
Participants comments are given in Table 2.
Page 5 of 36
FAPAS Report 25114
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 an
assigned value for each analyte. The assigned values were then used in combination with
the standard deviation for proficiency, p, to calculate a z-score for each result. The
procedure follows that recommended in the IUPAC International Harmonised Protocol for the
Proficiency 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, xa

The assigned value, xa, for each analyte was derived from the consensus of the results
submitted by participants.
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The following results were excluded from the calculation of the assigned value:
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.
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i)
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For moisture, ash, total fat, and nitrogen this procedure was straightforward and the robust
mean was chosen as the assigned value.
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For titratable acidity and lactose the major mode was chosen as the assigned value because
it was evident that there was a clear multi-modal distribution for titratable acidity and a slight
skewing of the distribution for lactose.
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The assigned values for all analytes are shown in Table 3.
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4.2. Standard Deviation for Proficiency, p
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The standard deviation for proficiency, p, was set at a value that reflects best practice for
the 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 criteria
based on expert advice.
The values for p used to calculate z-scores from the reported results of this test are given in
Table 3.
4.3. Individual z-Scores

Participants z-scores were calculated as:
z=
where
and
( x xa )
x
xa
p
= the participants reported result,

= the assigned value
= the standard deviation for proficiency.
Page 6 of 36
FAPAS Report 25114
Participants z-scores for all analytes are given in Table 1 and are shown as histograms in
Figures 16. It is possible for the z-scores published in this report to differ slightly from the
z-score that can be calculated using the formula given above. These differences arise from
the necessary rounding of the actual assigned values and standard deviations for proficiency
prior to their publication in Table 3.
The number and percentage of z-scores in the range -2 z 2 for all analytes are given in
Table 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 <|z| <3 are to be expected, at a rate of 1 in 20. Whether or
not such scores are of importance can only be decided by considering them in the context of
the other scores obtained by that laboratory.
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Scores where |z| >3 are to be expected at a rate of about 1 in 300. Given this rarity, such
z-scores very strongly indicate that the result is not fit-for-purpose and almost certainly
requires investigation.
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The consideration of a set or sequence of z-scores over time provides more useful
information than a single z-score. Examples of suitable methods of comparison are provided
in the IUPAC International Harmonised Protocol for the Proficiency Testing of Analytical
Chemistry Laboratories [5].
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6. REFERENCES
Adobe Certified Document Services,

http://www.adobe.com/misc/pki/cds_cp.html, accessed 08/05/2013.
ISO/IEC 17043:2010, Conformity assessment General requirements for proficiency

testing.
FAPAS, 2012, Protocol for Proficiency Testing Schemes, Part 1 Common Principles,
Version 3, Issued January 2012.
FAPAS, 2012, Protocol for Proficiency Testing Schemes, Part 2 FAPAS, Version 2,
Issued January 2012.
Thompson, M., Ellison, S.L.R. and Wood, R., 2006, The International Harmonised
Protocol for the Proficiency Testing of Analytical Chemistry Laboratories, Pure Appl.
Chem., 78, No. 1, 145196.
Thompson, M., 2000, Recent trends in inter-laboratory precision at ppb and sub-ppb
concentrations in relation to fitness for purpose criteria in proficiency testing, Analyst,
125, 385-386.
Birthe Mortensen, A. and Wallin, H., 1989, Gravimetric Determination of Ash in foods:
Collaborative Study, J AOAC Int., 72, 481-483.
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Page 7 of 36
FAPAS Report 25114
Results and z-Scores
laboratory
number
analyte
total fat
assigned value
21.35 g/100g
result
z-score
result
001
3.32
-0.1
002
3.3
-0.2
6.2
1.5
21.1
003
3.54
1.1
6.13
0.6
21.35
004
3.20
-0.8
005
3.18
-0.9
006
3.52
1.0
007
3.43
0.5
6.05
-0.4
21.24
008
3.23
-0.6
6.13
0.6
009
2.551
-4.3
6.107
0.3
010
3.86
2.8
011
3.48
0.8
012
3.16
-1.0
z-score
result
hydrolysis? z-score
yes
0.0
21.5
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ED
22.06
lactose
assigned value
39.45 g/100g
result
result
z-score
result
z-score
1.16
0.7
z-score
4.528
0.6
4.52
0.5
1.08
-0.1
41.9
2.0
28.93
172.5
0.152
-9.6
40.3
0.7
0.947
-1.5
39.6
0.1
41.316
1.5
0.2
1.1
-0.2
4.41
-0.2
22.58
no
1.9
4.38
-0.4
1.26
1.7
21.866
yes
0.8
4.554
0.8
1.071
-0.2
21.40
0.1
4.506
0.4
1.17
0.8
2.3
-29.7
0.118
-9.9
23.95
-12.4
21.0
-0.5
1.25
1.6
42.42
2.4
41.6
1.7
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titratable acidity
assigned value
1.09 g/100g
nitrogen
assigned value
4.44 g/100g
YES
1.0
yes
6.16
-0.4
EN
ash
assigned value
6.08 g/100g
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moisture
assigned value
3.34 g/100g
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Table 1:
013
014
3.53
1.0
6.1
0.2
21.4
No
0.1
4.53
0.6
0.984
-1.1
41.9
2.0
015
3.43
0.5
6.08
0.0
21.32
No
0.0
4.50
0.4
0.97
-1.2
40.83
1.1
z-scores outside |z| >2 are shown in bold, see Section 5
Page 8 of 36
FAPAS Report 25114
Table 1 (continued): Results and z-Scores

analyte
ash
assigned value
6.08 g/100g
total fat
assigned value
21.35 g/100g
result
z-score
result
z-score
result
016
3.56
1.2
6.04
-0.5
21.10
017
3.27
-0.4
5.95
-1.7
20.38
-1.5
018
3.25
-0.5
5.84
-3.1
21.54
0.3
019
3.2
-0.8
6.1
0.2
21.2
yes
020
3.49
0.8
6.10
0.2
21.75
No
021
3.45
0.6
022
3.5
0.9
023
3.37
0.2
024
3.47
0.7
025
1.92
-7.7
026
3.28
-0.3
6.01
-0.9
027
3.32
-0.1
6.10
028
3.37
0.2
6.12
029
3.39
0.3
030
3.45
0.6
result
z-score
result
z-score
result
z-score
4.58
1.0
1.10
0.1
38.30
-0.9
4.41
-0.2
0.16
-9.5
39.70
0.2
4.41
-0.2
41.5
1.6
-0.2
4.51
0.5
1.19
1.0
39.7
0.2
0.6
4.53
0.6
0.969
-1.2
37.20
-1.8
-0.2
4.44
0.0
38.78
-0.5
YES
-0.1
4.4
-0.3
1.45
3.7
40.46
0.8
4.49
0.3
1.11
0.2
39.21
-0.2
0.64
-4.6
15.7
148.9
41.90
2.0
8.66
77.1
40.29
0.7
LL
2.0
W
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-0.5
21.46
0.2
TR
21.02
Yes
-1.0
21.0
yes
-0.5
4.22
-1.6
0.2
21.98
yes
1.0
4.38
-0.4
0.5
21.17
No
-0.3
4.26
-1.3
6.07
-0.1
21.30
Yes
-0.1
4.41
-0.2
6.27
2.4
21.36
yes
0.0
4.52
0.5
20.72
6.24
-0.4
EN
yes
21.3
lactose
assigned value
39.45 g/100g
hydrolysis? z-score
21.24
0.2
titratable acidity
assigned value
1.09 g/100g
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moisture
assigned value
3.34 g/100g
6.1
nitrogen
assigned value
4.44 g/100g
ED
laboratory
number
Page 9 of 36
FAPAS Report 25114

laboratory
number
analyte
ash
assigned value
6.08 g/100g
total fat
assigned value
21.35 g/100g
result
z-score
result
z-score
result
031
3.30
-0.2
032
3.00
-1.9
6.14
0.7
21.43
no
0.1
2.08
no
-30.1
YES
3.19
-0.8
6.04
-0.5
22.24
035
3.46
0.6
6.00
-1.0
21.40
result
z-score
result
z-score
result
z-score
4.515
0.5
0.9959
-1.0
41.89
2.0
1.4
4.37
-0.5
1.06
-0.3
0.1
4.46
0.1
0.112
-10.0
35.08
-3.5
NO
0.2
4.501
0.4
yes
4.43
-0.1
0.144
-9.6
39.00
-0.4
EN
hydrolysis? z-score
3.50
0.9
6.14
0.7
21.0
LL
-0.5
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
38.65
-0.6
4.48
0.3
40.1
0.5
TR
037
21.48
036
lactose
assigned value
39.45 g/100g
W
H
034
titratable acidity
assigned value
1.09 g/100g
ED
033
nitrogen
assigned value
4.44 g/100g
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moisture
assigned value
3.34 g/100g
045
21.68 0.87
Page 10 of 36
0.88
-2.1
FAPAS Report 25114

laboratory
number
analyte
ash
assigned value
6.08 g/100g
total fat
assigned value
21.35 g/100g
nitrogen
assigned value
4.44 g/100g
titratable acidity
assigned value
1.09 g/100g
lactose
assigned value
39.45 g/100g
result
z-score
result
z-score
result
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
1.0
4.429
-0.1
0.106
-10.0
39.01
-0.3
0.2
4.34
-0.7
1.02
-0.7
Yes
-0.5
4.43
-0.1
20.2
no
-1.8
20.94
Yes
-0.6
4.36
-0.6
6.06
-0.3
054
3.10
-1.3
6.10
0.2
6.0
-1.0
21.04
EN
W
H
ED
21.5
TR
-1.7
3.03
3.69
1.9
6.13
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
056
0.1
053
21.39
no
LL
21.99
052
055
hydrolysis? z-score
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moisture
assigned value
3.34 g/100g
Page 11 of 36
FAPAS Report 25114

analyte
moisture
assigned value
3.34 g/100g
ash
assigned value
6.08 g/100g
total fat
assigned value
21.35 g/100g
result
z-score
result
z-score
result
061
2.06
-7.0
6.07
-0.1
22.7
062
2.97
-2.0
6.71
7.9
20.19
-1.8
063
3.73
2.1
6.07
-0.1
22.7
2.1
064
3.21
-0.7
6.02
-0.8
065
3.27
-0.4
6.08
0.0
21.64
066
3.20
-0.8
6.12
0.5
21.57
-4.6
6.14
0.7
069
3.22
-0.7
5.71
-4.7
070
3.35
0.0
071
3.28
-0.3
6.10
0.2
072
3.54
1.1
6.10
0.2
073
3.17
-0.9
5.94
074
3.43
0.5
075
3.21
-0.7
z-score
result
z-score
result
z-score
4.53
0.6
0.9
-1.9
4.58
1.0
1.45
3.7
4.70
1.8
0.87
-2.2
42
2.0
0.5
4.42
-0.2
40.50
0.8
0.4
4.348
-0.7
0.138
-9.7
37.435
-1.6
33.47
-4.8
39.97
0.4
EN
W
H
ED
No
no
2.1
19.8
-2.4
4.28
-1.1
1.30
2.1
22.07
1.1
4.43
-0.1
0.14
-9.7
4.59
1.0
0.6
4.47
0.2
TR
2.50
result
21.71
0.96
-1.3
39.20
-0.2
1.11
0.2
5.31
-27.3
39.4
0.0
068
lactose
assigned value
39.45 g/100g
2.1
yes
LL
22.70
titratable acidity
assigned value
1.09 g/100g
hydrolysis? z-score
067
nitrogen
assigned value
4.44 g/100g
PR
IN
TE
D
laboratory
number
21.17
no
-0.3
4.39
-0.4
6.14
0.7
7.35
no
-21.9
4.42
-0.2
6.13
0.6
21.5
0.2
4.37
-0.5
-1.8
Page 12 of 36
FAPAS Report 25114

analyte
moisture
assigned value
3.34 g/100g
ash
assigned value
6.08 g/100g
total fat
assigned value
21.35 g/100g
result
z-score
result
z-score
result
076
3.58
1.3
6.12
0.5
21.3
077
3.07
-1.5
5.92
-2.0
21.40
078
3.25
-0.5
6.15
0.9
21.54
Yes
21.6
No
21.67
No
0.7
081
082
3.33
-0.1
5.65
-5.5
21
083
3.90
3.0
5.9
-2.3
084
3.32
-0.1
6.05
-0.4
085
3.40
0.3
6.14
0.7
086
2.26
-5.9
6.10
0.2
087
3.52
1.0
6.12
088
2.48
-4.7
5.98
089
2.71
-3.4
090
3.35
0.0
EN
0.3
W
H
6.14
-0.1
0.1
LL
080
No
ED
079
hydrolysis? z-score
titratable acidity
assigned value
1.09 g/100g
lactose
assigned value
39.45 g/100g
result
z-score
result
result
z-score
4.53
0.6
38.9
-0.4
4.51
0.5
40.20
0.6
4.53
0.6
42.91
2.8
4.50
0.4
37.58
-1.5
4.20
-1.7
21.6
0.4
4.29
-1.1
0.77
-3.3
21.37
0.0
4.21
-1.6
1.115
0.3
39.85
0.3
0.4
4.22
-1.6
1.08
-0.1
38.57
-0.7
1.16
0.7
40.60
0.9
1.07
-0.2
39.07
-0.3
1.12
0.3
42.65
2.6
TR
N
1.0
4.52
0.5
0.5
3.00
NO
-28.6
4.42
-0.2
21.6
No
-1.3
20.37
Yes
-1.5
4.30
-1.0
6.11
0.4
18.11
No
-5.1
4.47
0.2
5.93
-1.9
21.46
0.2
4.28
-1.1
2.3
0.5
21.98
1.32
z-score
-0.5
no
0.4
nitrogen
assigned value
4.44 g/100g
PR
IN
TE
D
laboratory
number
Page 13 of 36
FAPAS Report 25114

analyte
total fat
assigned value
21.35 g/100g
result
z-score
result
z-score
result
091
3.17
-0.9
6.05
-0.4
21.12
092
3.35
0.0
6.15
0.9
21.4
093
3.21
-0.7
6.04
-0.5
21.10
hydrolysis? z-score
-0.4
Yes
-0.4
094
-0.3
6.30
2.8
21.80
096
3.34
0.0
6.07
-0.1
21.64
097
3.63
1.6
5.94
-1.8
21.80
098
3.53
1.0
099
3.80
2.5
6.05
-0.4
100
3.56
1.2
6.04
-0.5
101
3.63
1.6
5.97
-1.4
102
3.75
2.2
6.05
-0.4
103
4.05
3.9
5.89
result
z-score
result
z-score
result
z-score
4.71
1.9
1.34
2.5
41.83
1.9
4.50
0.4
38.7
-0.6
4.503
0.4
38.99
-0.4
38.55
-0.7
0.5
1.09
0.0
37.06
-1.9
yes
0.5
4.47
0.2
1.61
5.3
36.98
-2.0
4.39
-0.4
1.09
0.0
40.03
0.5
20.59
YES
-1.2
4.53
0.6
1.0164
-0.8
21.35
yes
0.0
4.39
-0.4
1.01
-0.8
21.76
no
0.6
4.30
-1.0
38.99
-0.4
22.24
No
1.4
4.23
-1.5
41.2
1.4
21.17
no
-0.3
4.543
0.7
0.58
-5.2
43.26
3.0
4.38
-0.4
1.12
0.3
TR
0.7
lactose
assigned value
39.45 g/100g
4.51
titratable acidity
assigned value
1.09 g/100g
0.7
ED
3.28
nitrogen
assigned value
4.44 g/100g
LL
095
0.1
EN
ash
assigned value
6.08 g/100g
W
H
moisture
assigned value
3.34 g/100g
PR
IN
TE
D
laboratory
number
-2.4
Page 14 of 36
FAPAS Report 25114
Table 2:
Participants Comments
participant number
comments
088
Titratable acidity is reported on dry basis of sample & Lactose is reported as

anhydrous 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
moisture
92
3.34
0.0270
ash
80
6.08
total fat
74
21.35
nitrogen
81
4.44
titratable acidity
57
1.09
lactose
61
39.45
standard deviation for

proficiency, p, g/100g
TE
D
assigned value,
xa, g/100g
uncertainty,
0.184
0.0100
Coll. Trial [7]
0.0791
0.0601
ffp
0.640
0.0109
Horwitz [6]
0.142
0.0254
ffp
0.0981
0.328
ffp
1.25
PR
IN
Coll. Trial [7]
EN
H
W
data points,
ED
analyte
Number and Percentage of z-Scores where |z| 2
O
N
Table 4:
TR
O
LL
ffp = fitness-for-purpose criteria
number of scores where

|z| 2
total number
of scores
% |z| 2
77
92
84
70
80
88
total fat
78
91
86
nitrogen
81
83
98
titratable acidity
34
59
58
lactose
53
62
85
ash
moisture
analyte
Page 15 of 36
48
103
83
10
99
102
63
56
41
44
101
97
38
60
76
100
16
72
3
98
14
87
6
37
22
42
20
11
24
57
35
59
30
21
74
50
15
7
85
49
51
29
28
23
92
90
70
96
82
84
27
1
31
2
95
71
26
65
17
78
18
8
69
93
75
64
66
19
4
34
5
91
73
12
43
54
77
46
53
39
58
47
32
62
40
89
9
68
88
86
61
25
ED
LL
O
TR
-6.0
-8.0
Laboratory Number
O
-4.0
Figure 1: z-Scores for moisture
Page 16 of 36
W
H
EN
PR
IN
TE
D
3.71 g/100g
2.0
2.97 g/100g
-2.0
3.34 g/100g
0.0
z-score
FAPAS Report 25114
6.0
4.0
48
62
95
50
30
24
49
40
44
2
42
5
92
78
85
80
74
68
37
32
75
56
8
3
87
76
66
38
28
89
46
9
86
72
71
54
27
22
20
19
14
65
15
96
63
61
57
29
53
43
102
99
91
84
60
47
7
100
93
58
34
16
64
59
26
55
35
88
101
39
17
97
73
90
77
83
103
18
69
82
ED
LL
O
TR
-4.0
-6.0
Page 17 of 36
6.08 g/100g
W
H
EN
PR
IN
TE
D
4.0
0.0
5.92 g/100g
-2.0
Laboratory Number
6.0
6.24 g/100g
2.0
z-score
Figure 2: z-Scores for ash
FAPAS Report 25114
10.0
8.0
58
67
63
61
8
101
34
69
5
51
86
27
9
97
95
100
20
71
80
96
65
85
83
79
66
78
18
75
53
4
49
36
90
24
44
32
57
92
77
60
35
14
10
52
84
30
99
3
15
39
76
48
29
22
38
21
7
42
19
102
73
28
91
93
16
2
54
23
82
40
37
26
12
56
50
43
25
98
17
88
55
62
47
46
68
59
89
74
87
11
33
ED
LL
O
TR
-6.0
-8.0
Laboratory Number
W
H
EN
-4.0
Page 18 of 36
21.35 g/100g
PR
IN
TE
D
22.63 g/100g
2.0
0.0
20.06 g/100g
-2.0
z-score
Figure 3: z-Scores for total fat
FAPAS Report 25114
4.0
5
50
91
63
70
62
16
9
102
98
78
76
61
39
20
14
2
86
57
44
30
3
32
95
77
19
10
93
36
92
79
58
15
59
48
24
45
96
89
71
49
35
47
21
69
54
40
37
51
46
87
74
65
29
18
17
7
43
22
99
97
73
103
27
8
75
34
56
38
66
53
100
88
83
90
68
42
28
101
85
26
84
82
T
-3.0
4.16 g/100g
W
H
EN
PR
IN
TE
D
3.0
-2.0
Figure 4: z-Scores for nitrogen
Page 19 of 36
4.44 g/100g
ED
LL
O
TR
-1.0
Laboratory Number
1.0
0.0
4.73 g/100g
2.0
z-score
FAPAS Report 25114
6.0
5.0
4.0
FAPAS Report 25114

Adaptive kernel density plot - titratable acidity
2.0
10.0
6.0
4.0
1.0
0.5
PR
IN
TE
D
8.0
Density
1.5
0.0
0.0
0.5
1.0
1.5
A nalytical result (g/100g)
2.0
2.0
EN
W
H
z-score
0.0
2.5
ED
-2.0
LL
-4.0
TR
-6.0
-8.0
Laboratory Number
26
28
96
62
22
40
47
91
78
68
8
50
12
46
42
57
19
10
86
1
103
90
84
74
24
16
97
95
85
49
3
9
88
34
53
98
99
32
14
15
20
71
6
61
44
63
83
25
102
17
5
37
69
66
58
11
35
48
51
-10.0
Figure 5: z-Scores for titratable acidity
Page 20 of 36
1.29 g/100g
1.09 g/100g
0.89 g/100g
FAPAS Report 25114
4.0
2.0
PR
IN
TE
D
41.95 g/100g
0.0
Adaptive kernel density plot - lactose
EN
z-score
-2.0
0.20
W
H
-4.0
ED
0.10
LL
-6.0
Density
0.15
0.05
0.00
32
34
36
38
40
42
Analytical result (g/100g)
44
46
48
Figure 6: z-Scores lactose
Laboratory Number
102
78
90
12
63
26
14
3
32
91
13
42
18
9
101
15
86
65
22
50
60
5
28
77
58
45
99
70
84
19
17
6
75
24
71
88
51
37
100
93
76
48
21
92
44
85
94
59
57
43
16
47
80
66
20
95
96
35
69
11
74
40
30
-10.0
TR
-8.0
Page 21 of 36
39.45 g/100g
36.94 g/100g
FAPAS Report 25114
APPENDIX I: Analytical Methods Used by Participants

Methods are tabulated according to the information supplied by participants, but some
responses may have been combined or edited for clarity.
Moisture
laboratory number
yes
003 004 006 008 009 010 012 014 016 019
021 023 024 025 026 030 031 032 034 035
037 039 043 047 048 049 053 056 057 059
063 066 070 074 075 076 078 082 083 084
088 089 090 091 093 095 097 098 099
no
001 005 007 017 018 028 038 040 050 051
062 065 068 071
Method Based On
laboratory number
International Standard
001 003 004 006 008 009 010 012 016 024
031 047 049 051 057 063 065 068 071 076
078 088 093
National Standard
007 014 017 021 023 026 028 035 037 038
040 043 050 059 062 066 070 074 082 083
084 090 091 095 098 099
Manufacturer/Kit Instructions/Technical
Note
005
TR
O
Sample Weight (g)
O
N
1 - <2
2 - <5
5 - <10
ED
018 019 025 032 075 089 097
LL
In house method
EN
PR
IN
TE
D
Method Used Accredited
laboratory number
001 008 009 017 025 047 065 068 071 078
084 088 090 091
003 004 005 010 012 014 016 018 019 021
023 024 026 030 031 034 035 037 038 039
048 049 057 059 062 063 066 070 075 076
082 083 089 093 097 098 099
006 007 028 032 040 043 050 051 056 074
095
25 - <50
053
Moisture Determination Procedure
laboratory number
to constant weight
001 004 006 007 008 009 010 012 014 016
017 018 019 021 023 024 025 026 028 031
032 035 037 038 040 043 047 049 050 051
056 057 059 062 063 065 068 070 071 074
075 076 078 082 083 084 088 089 091 093
095 097 098 099
4 h at 102C
003
Page 22 of 36
FAPAS Report 25114
laboratory number
Drying furnace
005
IS16072:2012
090
Apparatus used for constant weight
laboratory number
conventional oven
001 004 005 007 009 010 012 014 016 017
018 019 021 023 024 025 028 031 035 038
040 043 049 050 056 059 062 063 065 066
068 070 071 074 075 078 082 083 084 089
091 093 095 097 098 099
heated in beaker
026 037
vacuum oven
008 032 047 057 088
convection oven
076
Hot Air Oven
090
oven with dryed air
006
Reference Drier RD-8 Funke Gerber
051
Oven Temperature (C) for moisture

determination
laboratory number
<100
006 021 030 032 040 051 066
EN
PR
IN
TE
D
Moisture Determination Procedure

(continued)
ED
100 - <105
TR
O
LL
001 003 004 005 007 008 009 010 012 016
018 023 024 025 026 028 034 037 038 039
043 047 048 049 050 053 056 057 059 062
063 065 068 070 071 074 075 076 078 083
084 088 089 090 091 093 095 097 098
O
N
105 - <110
031 082
110 - <150
014 017 035 099
laboratory number
<1
Time Heated for Moisture Determination

(hours)
082
1 - <5
003 004 005 006 007 008 009 012 014 016
017 021 023 024 025 026 031 032 035 038
040 043 047 050 057 059 062 063 065 066
068 070 075 078 084 089 090 091 093 095
099
5 - <10
001 018 028 034 037 039 051 071 083 088
097 098
10 - <24
010 030 049 053 056 074 076
Page 23 of 36
FAPAS Report 25114
Dessicator Used To Cool The Sample
laboratory number
yes
001 003 004 005 006 007 008 009 010 012
014 016 017 018 019 021 023 024 025 026
028 030 031 032 034 035 037 038 039 040
043 047 048 049 050 051 053 056 057 059
062 063 065 066 068 070 071 074 075 076
078 082 083 084 088 089 090 091 093 095
097 098 099
Ash
laboratory number
yes
003 007 008 009 014 016 019 024 026 030
032 034 035 037 039 043 047 048 049 055
056 057 059 062 063 065 066 074 075 076
078 080 082 083 084 088 089 090 091 093
095 097 099
no
005 017 018 028 038 040 050 053 068 071
Method Based On
laboratory number
003 008 009 016 047 057 063 065 068 071
076 078 084 088 093
National Standard
007 014 017 026 028 035 038 040 043 049
055 059 062 066 074 082 083 090 091 095
099
O
N
In house method
T
O
N
2 - <5
Sample Weight (g)

1 - <2
037
TR
O
Note
LL
ED
EN
PR
IN
TE
D
005 018 019 024 032 056 075 080 089 097
laboratory number
003 009 016 018 038 047 048 057 065 071
074 078 083 088 099
005 008 014 017 019 024 028 030 032 035
039 040 043 049 053 055 059 062 066 068
075 076 080 082 084 089 090 091 093 095
097
5 - <10
007 026 034 037 050 056 063
Steps Taken To Avoid Spattering
laboratory number
charred on hotplate before ashing
009 014 017 024 026 028 030 032 035 037
039 040 043 047 048 053 056 059 062 063
068 071 074 076 082 083 084 088 089 090
091 093 095
crucible with lid
005 008 014 032 035 088
Page 24 of 36
FAPAS Report 25114
laboratory number
pre-dried in oven
005 007 016 019 034 035 037 038 095 097
099
slow temperature ramp
014 040 049 057 065 075 078 080 088
Control sample kept
018
pre-burned with Bunsen
050
TGA (Leco)
003
Ash Furnace Temperature (C)
laboratory number
<500
024
500 - <550
003 005 009 016 018 030 034 037 038 040
047 048 049 050 055 059 062 063 065 076
084 089 091 093
550 - <600
007 008 014 017 019 026 028 032 035 039
053 057 066 068 071 075 078 080 083 088
090 095 097 099
600 - <650
043 074
900 - <950
082
550 25
056
Time In Ash Furnace (hours)
laboratory number
ED
EN
PR
IN
TE
D
Steps Taken To Avoid Spattering

(continued)
TR
O
O
N
5 - <10
10 - <15
T
O
N
48
15 - <24
24 - <48
003 005 007 009 014 026 030 032 034 035
043 048 050 055 057 059 062 063 066 068
071 074 078 080 082 084 090 091 093 095
099
LL
1 - <5
008 016 038 039 040 065 083 088 097

019 024 028 047 075 076
018 049 053 056 089
017
037
Total Fat
laboratory number
yes
003 004 008 009 010 012 014 016 021 024
025 026 030 032 033 034 035 036 037 039
043 045 048 049 050 052 055 056 057 059
062 065 066 067 071 075 076 079 080 082
083 084 088 090 091 093 095 097 098 099
no
005 007 017 018 019 023 028 038 040 047
051 053 063 068 074 078 089
Page 25 of 36
FAPAS Report 25114
laboratory number
003 004 008 009 010 012 016 021 036 045
047 051 052 057 063 065 067 068 071 076
078 080 093 095
National Standard
007 014 017 023 026 028 035 037 038 040
043 048 049 055 062 066 074 079 082 083
084 088 090 091 098 099
Note
005 025 033 059
In house method
018 019 024 032 034 056 075 089 097
Sample Weight (g)
laboratory number
<1
009 045
1 - <2
003 008 010 012 014 016 017 018 021 023
024 028 032 035 036 049 050 051 053 055
057 062 063 065 066 068 071 076 078 079
080 084 090 091 095 097 098
2 - <5
004 007 030 034 038 040 052 056 059 075
083 088 089 093 099
5 - <10
005 025 026 037 039 043 047 067 082
10 - <25
074
50
033
ED
EN
PR
IN
TE
D
Method Based On
laboratory number
LL
Acid/Alkaline Hydrolysis Used
TR
O
acid
O
N
alkaline
003 008 010 014 017 018 021 023 024 028
032 035 049 051 055 062 065 068 071 076
078 079 080 083 084 089 090 091 093 095
097
005 012 033 036 057 074 075
none
004 007 009 016 025 026 030 034 037 038
039 040 043 045 047 050 053 056 059 063
067 082 088 098 099
Total Fat Extraction Method
laboratory number
Buchi
007 043
Mojonnier
008 009 010 018 024 028 032 062 067 076
079 080 091
Rse-Gottlieb
003 012 017 021 023 033 036 049 051 057
065 066 068 071 083 084 089 090 095 097
Soxhlet
019 034 038 039 047 048 074
Soxtherm
025 099
Tecator/Soxtec
016 056 075 098
Werner Schmidt
063 088
Alkaline Hydrolysis
078
Page 26 of 36
FAPAS Report 25114
laboratory number
ASE (accelerated solvent extraction)
093
Butirometric Method
050
Butyrometer
059
Gerber 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
088 089 095 099
no
004 007 009 012 016 017 018 021 024 026
028 030 033 034 037 038 039 040 043 045
047 049 050 051 053 056 057 059 063 065
066 067 068 071 074 075 076 078 079 080
082 084 090 091 093 097 098
Pre-extraction Time (hours)
laboratory number
<1
005 007 008 014 019 021 023 032 036 051
052 062 063 079 083 088 089 095 099
ED
EN
PR
IN
TE
D
Total Fat Extraction Method (continued)
1 - <2
LL
025 098
TR
O
5 - <6
O
N
Extraction Solvent Components
ethyl acetate
diethyl ether
038 074
laboratory number
007 009 010 012 014 017 018 021 024 028
032 036 048 049 050 052 053 057 062 063
065 066 067 068 071 075 076 078 079 080
084 088 089 091 095 097 098
035
hexane
093
petroleum ether/spirit
012 014 016 017 018 019 021 023 024 025
028 030 032 034 035 036 038 039 043 047
049 050 051 052 053 056 057 062 063 065
066 067 068 071 074 076 078 079 080 083
084 088 089 091 095 097 099
sodium chloride
088
water
012 088
ammonium hydroxide
012
ethanol
008 012 014 051 063 089
Page 27 of 36
FAPAS Report 25114
laboratory number
Ethyl alcohol
095
no solvent extraction - only separation of

fat 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
<1
005 008 009 010 012 018 024 040 049 057
063 068 071 079 080 093
1 - <2
007 014 016 021 032 036 037 043 050 053
062 065 075 076 078 083 091
2 - <5
017 023 025 028 030 035 052 056 059 066
067 084 088 089 095 098 099
5 - <10
019 034 038 039 074
>10
047
EN
PR
IN
TE
D
Extraction Solvent Components

(continued)
ED
Nitrogen
laboratory number
LL
O
N
TR
O
yes
005 007 017 018 028 038 040 050 051 053
068
no
003 008 009 010 014 016 019 021 024 026
030 032 034 035 036 037 039 043 045 047
048 049 056 057 059 062 063 065 066 070
071 074 075 076 078 079 082 083 084 088
089 090 091 093 095 097 098 099
Method Based On
laboratory number
003 008 009 010 016 021 024 036 045 057
065 068 070 071 076 078 084 088 095
National Standard
007 014 017 026 028 035 037 040 043 048
050 062 066 074 079 082 083 090 091 098
099
Paper Published In An International

Journal
093
Note
049 059
In house method
005 018 019 038 047 056 063 089 097
Page 28 of 36
FAPAS Report 25114
laboratory number
<1
003 007 009 010 014 017 018 019 021 024
028 030 032 035 036 037 038 040 043 045
047 048 049 050 056 057 059 062 068 070
076 078 079 082 084 089 090 093 095 097
1 - <2
016 026 034 039 051 053 065 071 074 075
083 088 091 098 099
2 - <5
008 066
5 - <10
005
10 - <25
063
Determination Method (Nitrogen)
laboratory number
Dumas
003
Kjeldahl
007 008 009 010 014 016 017 024 026 028
030 032 034 035 036 037 038 039 040 043
045 047 048 050 051 053 056 057 062 066
068 071 074 075 076 078 082 084 088 089
090 091 093 095 097
Kjeltec-Tecator System
018 019 021 049 059 065 070 079 083 098
099
FT-NIR SPECTROMETER
063
Milkoscan FT120
005
ED
laboratory number
LL
Digestion Acid
018 024 040 066 089 098
TR
O
hydrogen peroxide
O
N
sulphuric acid
Hydrochloric acid
EN
PR
IN
TE
D
Sample Weight (g)
007 008 009 010 014 016 017 018 019 021
024 026 028 030 032 034 036 037 038 039
040 043 045 047 048 049 050 051 053 056
057 059 062 065 068 070 071 074 075 076
078 079 082 083 084 088 089 090 091 093
095 098 099
035
phosphosulphuric acid
097
Catalyst
laboratory number
copper (Cu)
008 009 010 014 016 018 019 021 024 028
030 034 036 037 038 039 040 043 045 048
049 050 051 053 056 057 062 065 068 071
074 075 076 079 082 083 084 088 089 091
093 095 098 099
potassium (K)
008 010 018 019 021 024 036 037 038 039
040 043 045 049 053 056 062 068 071 075
076 079 082 083 090 095
selenium (Se)
007 017 066 070
sodium (Na)
028 040 050 084 088
Page 29 of 36
FAPAS Report 25114
Catalyst (continued)
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
TE
D
Titratable Acidity
laboratory number
yes
001 006 008 009 010 012 014 016 026 034
035 037 047 049 053 062 063 066 083 084
088 090 091 095 097 099
no
003 005 017 019 024 025 028 032 040 048
050 051 057 068 071 074 078
Method Based On
laboratory number
ED
EN
PR
IN
001 006 009 010 024 047 048 051 057 063
068 074
LL
TR
O
National Standard
014 017 026 028 035 037 040 050 062 066
083 084 088 090 091 095 099
025
In house method
005 019 097
O
N
Paper Published In An International

Journal
<1
Sample Weight (g)
laboratory number
074 083 095
1 - <2
005 008 009 019 032 047 063 090 091
2 - <5
014 016 026 028 035 037 050 062 066 071
099
5 - <10
001 003 010 012 025 040 049 084 088
10 - <25
006 017 024 051 068 097
Titration Reagents (Acidity)
laboratory number
ethanol
019 090
phenolphthalein
008 009 012 028 049 051 057 062 068 074
084 088 091 095 097 099
Page 30 of 36
FAPAS Report 25114
laboratory number
sodium hydroxide
001 005 006 008 010 012 017 024 025 028
032 034 035 037 040 047 049 050 051 057
062 063 066 068 071 078 083 084 088 091
095 099
pH meter
014
Titration Method (Peroxide and Acidity)
laboratory number
add water
001 003 010 014 026 028 035 040 062 066
071 074 083 084 090 091 095 097
mix sample and reagents
010 017 028 035 037 040 084 091 095
Titration of Free Fatty Acids
laboratory number
phenolphthalein
001 003 008 024 028 037 040 062 066 071
090 095
sodium hydroxide
008 010 014 017 024 026 028 035 040 062
074 095
Other Method
laboratory number
IS:1165:2002
090
ISO6091:2010
001
ED
EN
PR
IN
TE
D
Titration Reagents (Acidity) (continued)
TR
O
LL
Lactose
O
N
yes
003 006 012 013 014 021 024 026 035 037
043 045 047 048 059 063 065 070 071 075
076 078 084 088 090 091 093 095 099
005 009 016 017 018 019 028 032 040 050
051 057 066 074 080
Reference
no
laboratory number
laboratory number
1991
026
1995
095
1999
032
AOAC Official Methods
048
AOAC Official Methods 1993 18
047
AOAC Official Methods 1996 33.2.31

Chapter 33 Page 22
045
AOAC Official Methods 2005 - -
080
AOAC Official Methods 2005 18th Edition

Ch 33, P.17
071
Page 31 of 36
FAPAS Report 25114
laboratory number
AOAC Official Methods 2011 Fructose,

Glucose, Lactose, Maltose and Sucrose
in Milk Chocolate 31.5.04
065
DGHS Lab Manual No. 1 2005 85
028
FIL-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-2:1961
Page no-25
090
ISO
003 006
J. AOAC Int. 1979 62 1292
024
ED
EN
PR
IN
TE
D
Reference (continued)
J. AOAC Int. 1992 Vol.75 No.3 443-464
070
LMBG Method 1983

Manufacturer's Instructions
TR
O
LL
Lane Eynon
078
043
076 099
016
Manufacturer's Instructions 2003 15GB
005
MAPA 2009
040
O
N
Manufacturer's Instructions 1980
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
<1
003 012 021 024 035 065 066 074 076 099
1 - <2
006 014 016 028 047 059 063 080
2 - <5
017 018 019 043 051 070 071 078 093 095
Page 32 of 36
FAPAS Report 25114
laboratory number
5 - <10
005 026 032 037 040 045 050 075 088 090
10 - <25
084 091
Sample Preparation (Lactose)
laboratory number
Carrez I & II
003 006 012 016 017 019 040 043 051 057
070 075 076 078 084 088 091 093 095 099
centrifuge
014 065 095
dilution with water
012 013 014 018 021 024 028 032 037 050
051 057 059 063 065 066 071 074 078 080
084 088 090 091 095
filtration
012 013 014 018 021 028 035 037 040 050
051 057 059 065 066 071 075 076 078 084
088 091 095
precipitation
012 018 026 028 050 051 065 071 078 084
088 091 095
dill.-pre.-fil.
047
IR (AOAC 972.16)
045
milkoscanFT120
005
NIN (By Difference)
009
ED
EN
PR
IN
TE
D
Sample Weight (g) (continued)
Method
laboratory number
016 057 074
LL
colorimetric method
TR
O
enzymatic method
Ion Chromatography (IC)
O
N
HPLC
titration
003 006 040 043 057 076 099

012 013 014 018 021 024 051 059 063 065
066 075 078 093
032 080
017 019 026 028 037 047 050 084 088 090
091 095
071
HPLC DRID
035
Gravimetric method, Munson - Walker
IR Spectrophotometry
045
MilkoscanFT120
005
Sample Hydrolysed
laboratory number
yes
005 016 026 035 076
no
012 013 014 018 019 021 024 028 032 037
040 043 045 050 051 059 063 065 066 071
074 075 078 080 084 088 091 093 095 099
Page 33 of 36
FAPAS Report 25114
laboratory number
acidify
021 037
blend / homogenise with solvent
037 075
centrifuge
014 016 065
clarify
016 051
de-proteinise
018 021 051 075 078 093
dilute
018 032 065 078
dissolve in water
013 014 021 032 035 051 059 078 093
filter
012 013 014 018 021 032 051 059 063 065
078 093
hot water extraction
016 032 035 075 078 093
internal standard addition
021 051
Precipitation with Acetonitrile
024
Internal Standard Added
laboratory number
yes
012 021 032 051
no
005 006 013 014 016 018 024 035 037 043
045 050 059 063 065 066 071 075 076 078
080 091 093 095 099
Actual Internal Standard Added
laboratory number
021
LL
D(+)-Melezitose
ED
EN
PR
IN
TE
D
Sample Treatment Prior to HPLC
TR
O
D-glucoheptose
glycerine
O
N
Pentaerythritol
032
012
051
laboratory number
5 - <10
012 035 051 059 075
25 - <50
O
N
10 - <25
HPLC Injection Volume (L)
013 014 021 032 063 065 066 078 093

016 018
100 - <150
024
HPLC Column Packing
laboratory number
Ion Exchange
013 021 032
NH2
016 018 024 035 059 063 065 066 075 078
093
Amide
051
Carbohydrate
014
hypersil
012
Page 34 of 36
FAPAS Report 25114
laboratory number
ambient
016 032 059 066 075
>ambient - <50
012 014 018 024 035 051 063 065 078 093
50
013 021
Isocratic Mobile Phase
laboratory number
yes
013 014 016 018 021 024 032 035 051 059
063 065 066 075 078
no (gradient)
012 076 093
Organic Component
laboratory number
acetonitrile
012 014 016 018 024 035 051 063 065 066
075 078 093
methanol
059
Aqueous Component
laboratory number
sodium hydroxide
032
water
012 013 014 016 018 021 024 035 051 059
063 065 066 075 078 093
HPLC Detector Type
laboratory number
ED
EN
PR
IN
TE
D
HPLC Column Temperature (C)
032
LL
PAD
TR
O
RI
O
N
DRID
Other Method
Correc Result: 39,7 g/100g
iodometry
Enzymatic spectrophotometric
012 013 014 016 018 021 024 051 059 063
065 066 075 078 093
035
laboratory number
019
076
037
It's based on absorption of IR energy at

045
specific wave nuber by CH groups in fatty acid
chains of fat molecles by carbonyl groups in
ester linkages of fat molecules by peptide
linkages between amino acids of protein
molecules and by OH groups lactose
Page 35 of 36
FAPAS Report 25114
APPENDIX II: FAPAS SecureWeb, Protocol and Contact Details

1. FAPAS SECUREWEB
Access to the secure area of our website is only available to participants in our proficiency
tests. Please contact us if you require a UserID and Password. FAPAS SecureWeb allows
participants to:
Obtain their laboratory numbers for the proficiency tests in which they have
participated.
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 have
participated.
View charts of their z-scores obtained in previous FAPAS proficiency tests.
PR
IN
TE
D
EN
2. PROTOCOL
ED
The Protocols [3, 4] set out how FAPAS is organised. Copies can be downloaded from our
website.
TR
O
LL
3. CONTACT DETAILS
O
N
This report was prepared and authorised on behalf of FAPAS by Jennifer Leak (Round
Coordinator). Participants with any comments or concerns about this proficiency test should
contact:
FAPAS
The Food and Environment Research Agency

Sand Hutton
York
YO41 1LZ
UK
Tel: +44 (0)1904 462100
Fax: +44 (0)1904 500440
info@fapas.com
testmaterials@fapas.com
www.fapas.com
Page 36 of 36

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FAPAS Report 25114

Nutritional Components in Milk Powder

December 2013-January 2014

FAPAS Report 25114

PARTICIPANT LABORATORY NUMBER

FAPAS is accredited by UKAS as complying with

The Food and Environment Research Agency is

FAPAS Report 25114

FAPAS Report 25114

1.1. Proficiency Testing

4. STATISTICAL EVALUATION OF RESULTS

4.1. Calculation of the Assigned Value, xa

Assigned Values and Standard Deviations for Proficiency

Number and Percentage of z-Scores where |z| 2

z-Scores for moisture

z-Scores for ash

z-Scores for total fat

z-Scores for nitrogen

z-Scores for titratable acidity

Analytical Methods Used by Participants

FAPAS SecureWeb, Protocol and Contact Details

FAPAS Report 25114

Samples were stored at ambient temperature until dispatch.

The instructions for reporting results were as follows:

FAPAS Report 25114

The analytical methods used by each participant are summarised in APPENDIX I.

4. STATISTICAL EVALUATION OF RESULTS

4.1. Calculation of the Assigned Value, xa

results for nitrogen that appeared to be for protein,

results for titratable acidity that were considered to be reporting errors.

The assigned values for all analytes are shown in Table 3.

4.2. Standard Deviation for Proficiency, p

4.3. Individual z-Scores

= the participants reported result,

FAPAS Report 25114

Adobe Certified Document Services,

ISO/IEC 17043:2010, Conformity assessment General requirements for proficiency

FAPAS Report 25114

Results and z-Scores

z-scores outside |z| >2 are shown in bold, see Section 5

FAPAS Report 25114

Table 1 (continued): Results and z-Scores

z-scores outside |z| >2 are shown in bold, see Section 5

FAPAS Report 25114

Table 1 (continued): Results and z-Scores

z-scores outside |z| >2 are shown in bold, see Section 5

FAPAS Report 25114

Table 1 (continued): Results and z-Scores

z-scores outside |z| >2 are shown in bold, see Section 5

FAPAS Report 25114

Table 1 (continued): Results and z-Scores

z-scores outside |z| >2 are shown in bold, see Section 5

FAPAS Report 25114

Table 1 (continued): Results and z-Scores

z-scores outside |z| >2 are shown in bold, see Section 5

FAPAS Report 25114

Table 1 (continued): Results and z-Scores

z-scores outside |z| >2 are shown in bold, see Section 5

FAPAS Report 25114

Titratable acidity is reported on dry basis of sample & Lactose is reported as

titratable acidity as lactic acid in sample as it is: 1.05 g/100g

comments are as submitted by participants

Assigned Values and Standard Deviations for Proficiency