Leche Polvo (25114) Enero 2014

8/12/2019 Leche Polvo (25114) Enero 2014

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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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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 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



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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FAPAS Report 25114


laboratorynumber

analyte








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


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laboratorynumber

analyte








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


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laboratorynumber

analyte








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


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laboratorynumber

analyte








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


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FAPAS Report 25114


laboratorynumber

analyte








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


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FAPAS Report 25114

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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FAPAS Report 25114

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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FAPAS Report 25114

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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FAPAS Report 25114

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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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



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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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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


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


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



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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


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



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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

Documents

Leche Polvo (25114) Enero 2014