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FAPASReport 25103

Nutrit ional Components in Milk Powder

November-December 2012

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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

Since 2006 all FAPAS reports have been distributed as AdobeCertified Document Services(CDS) AdobePDF documents [1].

The use of AdobeCDS allows the PDF files to certify that the author of the report is FAPASand that the document has not been altered in anyway. A blue ribbon and information barindicates this validation when the document is opened using AdobeReader 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 with the requirements ofISO/IEC 17043:2010 [2].

The Food and Environment Research Agency is an ISO 9001 certified organisation.

0009 PT

Whereas this report has been produced in good faith and in accordance with best industry

practice, neither The Food and Environment Research Agency nor the Secretary of State forEnvironment, Food and Rural Affairs accepts any liability whatsoever as to the application oruse of the information contained therein.

Crown Copyright 2013

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SUMMARY

1. The test material for FAPASproficiency test 25103 was dispatched in November 2012.

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:

analyte assigned value, xa

g/100 g

number of scores,

|z| 2

total number

of scores

% |z| 2

moisture 3.19 67 81 83

ash 5.94 64 73 88

total fat 22.50 63 79 80

nitrogen 4.36 68 81 84

titratable acidity 1.07 31 55 56

lactose 39.49 43 55 78

4. Surplus test materials are available for sale, seeAPPENDIX II.

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CONTENTS

1. INTRODUCTION 51.1. Proficiency Testing 5

2. TEST MATERIAL 52.1. Preparation 52.2. Homogeneity 52.3. Dispatch 5

3. RESULTS 54. STATISTICAL EVALUATION OF RESULTS 6

4.1. Calculation of the Assigned Value, xa 64.2. Standard Deviation for Proficiency, p 64.3. Individual z-Scores 6

5. INTERPRETATION OF SCORES 76. REFERENCES 7TABLES

Table 1: Results and z-Scores 8Table 2: Participants Comments 15Table 3: Assigned Values and Standard Deviations for Proficiency 15Table 4: Number and Percentage of z-Scores where |z| 2 16FIGURES

Figure 1:

z-Scores for Moisture 17

Figure 2: z-Scores for Ash 18Figure 3: z-Scores for Total Fat 19Figure 4: z-Scores for Nitrogen 20Figure 5: z-Scores for Titratable Acidity 21Figure 6: z-Scores for Lactose 22APPENDICES

APPENDIX I: Analytical Methods Used by Participants 23APPENDIX II:

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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 milk was prepared from a blend of full-fat milk powder and skimmed milk powder.

All analytes were present at natural levels.

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 schemes

accreditation [2].These data showed sufficient homogeneity and were not included in the subsequentcalculation of the assigned values.

2.3. Dispatch

The start date was 16 November 2012. Test materials were sent to 107 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 93 participants (87%) before the closing date for this test,28 December 2012.

Each participant was given a laboratory number, assigned in order of receipt of results. Thereported analyte concentrations are given inTable 1.

Participants comments are given inTable 2.

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The analytical methods used by each participant are summarised inAPPENDIX 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, xa

The assigned value, xa, 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 reported as approximately 10, 100 or 1000 greater or smaller than themajority of submitted results (as these were considered to be reporting errors),

ii) results for moisture that appeared to be for total solids,

iii) results for total fat that did not state use of either acid or alkaline hydrolysis,

iv) results for nitrogen that appeared to be for protein,

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

For all analytes, this procedure was straightforward and the robust mean was chosen as theassigned value.

The assigned values for all analytes are shown inTable 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 moisture, ash and nitrogen, pwas derived from collaborative trial data [6, 7, 8].

For total fat, titratable acidity and lactose, pwas calculated using fitness-for-purpose criteriabased on expert advice.

The values for pused 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:

p

axx

z

)( =

where x = the participants reported result,xa = the assigned value

and p = the standard deviation for proficiency.

Participants z-scores for all analytes are given in Table 1 and shown as histograms inFigures 16. It is possible for the z-scores published in this report to differ slightly from the

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z-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 inTable 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: Results and z-Scores

laboratorynumber

analyte

moisture ash total fat nitrogen titratable acidity lactoseassigned value

3.19 g/100gassigned value

5.94 g/100gassigned value22.50 g/100g

assigned value4.36 g/100g



result z-score result z-score result hydrolysis? z-score result z-score result z-score result z-score

001 3.17 -0.1 6.07 1.7 22.92 alkaline 0.6 4.36 0.0 1.35 2.9 40.32 0.7

002 3.00 -1.1 5.86 -1.0 22.72 acid 0.3 4.38 0.2 1.41 3.5

003 3.47 1.6 5.94 0.1 17.6 alkaline -7.3 27.75 297.8 0.94 -1.4 39.0 -0.4

004 3.28 0.5 5.71 -2.9 21.70 alkaline -1.2 4.37 0.1 1.0 -0.8 40.22 0.6

005 3.23 0.2 22.14 alkaline -0.5

006 3.0 -1.1 5.95 0.2 23.47 alkaline 1.4 4.41 0.6 1.35 2.9 39.15 -0.3

007 3.34 0.8 22.28 -0.3 5.7 47.9 42.14 2.1

008 3.17 -0.1 22.67 alkaline 0.2 4.36 0.0 38.59 -0.7

009 2.6 -3.4 6.0 0.8 22.2 acid -0.5 4.448 1.1

010 3.82 3.6

011 3.21 0.1 5.79 -1.9 22.8 alkaline 0.4 4.37 0.1 1.0 -0.8 41.6 1.7

012 3.14 -0.3 5.94 0.1 21.50 acid -1.5 4.37 0.1 1.34 2.8 38.98 -0.4013 22.56 alkaline 0.1

014 2.22 -5.5 5.94 0.1 25.74 alkaline 4.8 4.38 0.2 1.031 -0.4 40.18 0.6

015 3.1 -0.5 6.0 0.8 22.5 acid 0.0 4.33 -0.4 1.30 2.3 42.6 2.5

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








016 3.36 0.9 5.95 0.2 22.42 alkaline -0.1 4.16 -2.6 17.12 166.1 39.52 0.0

017 42.5 2.4

018 3.47 1.6 5.86 -1.0 22.75 no 0.4 4.42 0.7 1.2 1.3 40.70 1.0

019 1.92 -7.3 5.74 -2.5 22.10 alkaline -0.6 4.31 -0.7 0.688 -4.0 37.99 -1.2

020 3.26 0.4 22.57 alkaline 0.1 4.40 0.5

021 3.39 1.1 5.93 -0.1 22.68 acid 0.3 4.34 -0.3 26.8 -10.1

022 3.20 0.0 5.97 0.5 21.99 acid -0.8 4.27 -1.2

023 23.16 alkaline 1.0 4.25 -1.4

024 3.13 -0.4 5.82 -1.5 28.0 acid 8.1 4.60 3.0 42.1 2.1

025 3.08 -0.6 5.74 -2.5 20.74 acid -2.6 4.31 -0.7 39.95 0.4

026 1.83 -7.8 4.39 0.3

027 2.98 -1.2 5.90 -0.5 22.53 alkaline 0.0 4.29 -0.9 1.11 0.4 41.25 1.4028 3.34 0.8 6.07 1.7 22.54 No 0.1 4.39 0.3 1.16 0.9 38.65 -0.7

029 3.30 0.6 6.0 0.8 22.46 -0.1 4.42 0.7 0.98 -1.0 44.44 3.9

030 2.97 -1.3 5.92 -0.2 23 0.7 4.26 -1.3 1.01 -0.7 40.94 1.2


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laboratorynumber

analyte








031 3.45 1.5 5.71 -2.9 22.74 alkaline 0.3 4.39 0.3 0.10 -10.1 38.42 -0.8

032 3.48 1.6 5.95 0.2 22.6 alkaline 0.1 4.48 1.5 0.129 -9.8 40.09 0.5

033 24.25 alkaline 2.6

034 3.3 0.6 5.90 -0.5 22.7 alkaline 0.3 4.39 0.3 1.06 -0.1 38.3 -0.9

035 3.34 0.8 5.91 -0.3 22.69 acid 0.3 4.41 0.6

036 3.3 0.6 5.92 -0.2 22.31 acid -0.3 4.210 -1.9 1.64 5.9 41.37 1.5

037 3.27 0.4 5.84 -1.2 22.55 0.1 4.48 1.5

038 3.22 0.1 6.02 1.1 22.59 alkaline 0.1 4.37 0.1 38.4 -0.9

039 3.21 0.1 5.84 -1.2 22.56 alkaline 0.1 27.0 288.3 0.115 -9.9 36.8 -2.1

040 3.35 0.9 6.1 2.1 21 acid -2.2 4.31 -0.7 0.81 -2.7 41.5 1.6

041 3.27 0.4 5.89 -0.6

042 3.21 0.1 5.82 -1.5 22.24 alkaline -0.4 4.41 0.6 1.12 0.5 39.03 -0.4043 3.25 0.3 5.82 -1.5 22.52 alkaline 0.0 4.32 -0.5 0.114 -9.9 36.8 -2.1

044 2.8 -2.2 6.0 0.8 22.3 acid -0.3 4.4 0.5 0.90 -1.8 34 -4.4

045 2.79 -2.3 6.00 0.8 22.84 alkaline 0.5 24.68 258.7 1.33 2.7 38.75 -0.6


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laboratorynumber

analyte








046 3.35 0.9 5.94 0.1 22.17 -0.5 4.39 0.3

047 3.24 0.3 5.98 0.6 22.43 alkaline -0.1 4.390 0.3 0.86 -2.2 39.63 0.1

048 3.2 0.0 5.9 -0.5 22.4 alkaline -0.2 4.2 -2.1 0.97 -1.1

049 3.22 0.1 5.87 -0.8 22.25 alkaline -0.4 4.41 0.6 38.57 -0.7

050 3.20 0.0 6.03 1.2 22.49 alkaline 0.0 4.35 -0.2 0.88 -2.0 38.75 -0.6

051 2.91 -1.6 5.9 -0.5 23.13 0.9 4.36 0.0 1.01 -0.7

052 3.0 -1.1 39.95 0.4

053 38.35 -0.9

054 2.50 -3.9 5.93 -0.1 22.41 -0.1 4.38 0.2 0.9525 -1.3 41.26 1.4

055 3.023 -1.0 24.00 acid 2.2 4.156 -2.6 0.74 -3.5

056 3.3 0.6 5.92 -0.2 22.67 acid 0.2 4.38 0.2 1.03 -0.4

057 3.34 0.8 5.92 -0.2 22.7 alkaline 0.3 4.4 0.5 0.113 -9.9 39.55 0.0058 3.5 1.7 6.06 1.6 23.02 alkaline 0.8 4.4 0.5 0.11 -10.0 40.9 1.1

059 3.31 0.7 5.88 -0.7 24.00 acid 2.2 4.23 -1.7 6.20 53.1

060 3.31 0.7 5.95 0.2 22.86 alkaline 0.5 4.42 0.7 0.89 -1.9 39.06 -0.3


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laboratorynumber

analyte








061 3.44 1.4 5.73 -2.7 4.42 0.7 1.08 0.1

062 3.19 0.0 5.96 0.3 22.59 0.1 4.29 -0.9 1.03 -0.4

063 3.11 -0.5 6.01 1.0 4.28 -1.1 0.93 -1.5

064 3.13 -0.4 5.92 -0.2 4.06 alkaline -27.3 27.63 296.3 39.92 0.3

065 3.1 -0.5 6.4 6.0 21 acid -2.2 4.6 3.0 0.13 -9.8 39.1 -0.3

066 4.169 -2.5

067 88.21 484.0 2.7 -29.3 0.51 -49.1 7.0 61.3

068 3.10 -0.5 6.18 3.2 21.72 acid -1.2 4.32 -0.5

069 4.42 0.7

070 5.87 -0.8 22.4 acid -0.2 4.43 0.9 0.94 -1.4 38.4 -0.9

071 5.87 -0.8 22.4 acid -0.2 4.43 0.9 0.94 -1.4 35.4 -3.3

072 2.56 -3.6 6.09 2.0 22.71 alkaline 0.3 4.40 0.5073 3.22 0.1 5.97 0.5 22.0 alkaline -0.7 4.44 1.0 0.945 -1.3 41.6 1.7

074 7.72 25.8 5.93 -0.1 21.4 alkaline -1.6 4.75 4.9 1.20 1.3 35.17 -3.4

075 3.01 -1.0 5.89 -0.6 24.2 alkaline 2.5 4.28 -1.1 0.91 -1.7 40.8 1.0


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laboratorynumber

analyte








076 3.23 0.2 3.52 -31.3 24.70 3.3

077 3.07 -0.7

078 2.44 -4.3 5.99 0.7 21.16 acid -2.0 4.203 -2.0 0.12 -9.9

079 2.57 -3.6 6.03 1.2 25.19 alkaline 4.0 4.24 -1.6 1.15 0.8

080 3.36 0.9 6.02 1.1 23.15 acid 1.0 4.32 -0.5

081 3.0 -1.1

082 3.26 0.4 5.90 -0.5 23.50 alkaline 1.5 4.35 -0.2 1.03 -0.4 38.70 -0.6

083 3.16 -0.2 6.06 1.6 22.11 alkaline -0.6 4.32 -0.5 39.39 -0.1

084 3.25 0.3 6.00 0.8 21.07 -2.1 3.96 -5.1 1.26 1.9

085 22.5 alkaline 0.0 4.4 0.5

086 3.23 0.2 5.85 -1.1 22.64 acid 0.2 4.51 1.9 1.16 0.9 40.84 1.1

087 3.55 2.0 6.07 1.7 22.60 alkaline 0.1 4.29 -0.9 37.01 -2.0088 3.31 0.7 5.9 -0.5 4.29 -0.9 0.09 -10.2 37.46 -1.6

089 3.294 0.6 6.033 1.3 22.69 acid 0.3 4.52 2.0

090 3.06 -0.8 6.01 1.0 14.43 acid -12.0 4.34 -0.3 1.02 -0.6 20.5 -15.1


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laboratorynumber

analyte








091 4.12 5.3 5.87 -0.8 22.32 acid -0.3 4.49 1.6

092 4.34 -0.3

093 5.95 0.2 22.31 No -0.3 4.517 2.0 41.80 1.8


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Table 2: Participants Comments

participant number comments

016 For the determination of moisture use temperature of 102 C. All methodsused to follow IN # 68 12/12/2006 MAPA.

055 Used methods: Total Fat: AOAC 2000 18 acid hydroysis detection (Gerbermethod); Moisture: AOAC 920.20; Nitroen: AOAC 991.20;Titratable acidity:AOAC 947.05

058 Lactose GC = 36 g/100g

067 titratable acidity is measured like Soxhlet Henkel degree

070 Ash:Ref. AOAC 945.46; Total fat: TCVN 6688-1:2007; Nitrogen: TCVN8100:2009; Titratable Acidity: 5448:1991; Lactose: CASE.SK.0001

071 Ash: Ref. AOAC 945.46; Total fat: TCVN 6688-1:2007; Nitrogen: TCVN8100:2009; Titratable Acidity: 5448:1991; Lactose: HPLC-Merck KGaA

082 titratable acidity as lactic acid in g/100g sample as it is: 1.00 g/100g

comments are as submitted by participants

Table 3: Assigned Values and Standard Deviations for Proficiency

analyte data points,

n

assigned value,

xa, g/100 g

uncertainty,

u

standard deviation for

proficiency, p, g/100 g

moisture 80 3.19 0.0233 Coll. Trial [6] 0.176

ash 73 5.94 0.0111 Coll. Trial [7] 0.0772

total fat 65 22.50 0.0853 ffp 0.675

nitrogen 76 4.36 0.0100 Coll. Trial [8] 0.0785

titratable acidity 44 1.07 0.0307 ffp 0.097

lactose 55 39.49 0.264 ffp 1.257

ffp = fitness-for-purpose criteria

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Table 4: Number and Percentage of z-Scores where |z| 2

analyte number of scores where

|z|2

total number

of scores

% |z| 2

moisture 67 81 83

ash 64 73 88

total fat 63 79 80

nitrogen 68 81 84

titratable acidity 31 55 56

lactose 43 55 78

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Figure 1: z-Scores for Moisture

26

19

14

78

54

72

79

9 45

44

51

30

27

2 6 52

81

75

55

90

77

25

15

65

68

63

24

64

12

83

1 8 62

22

48

50

11

39

42

38

49

73

5 76

86

47

43

84

20

82

37

41

4 89

29

34

36

56

59

60

88

7 28

35

57

40

46

16

80

21

61

31

3 18

32

58

87

10

91

74

67

3.55 g/100g

3.19 g/100g

2.84 g/100g

-8.0

-7.0

-6.0

-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

6.0

7.0

8.0

9.0

10.0

z-score

Laboratory Number

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Figure 2: z-Scores for Ash

76

431

61

19

25

11

24

42

43

37

39

86

218

49

70

71

91

59

41

75

27

34

48

51

82

88

35

30

36

56

57

64

21

54

74

312

14

46

616

32

60

93

62

22

73

47

78

915

29

44

45

84

63

90

38

80

50

79

89

58

83

128

87

72

40

68

65

6.09 g/100g

5.94 g/100g

5.78 g/100g

-10.0

-9.0

-8.0

-7.0

-6.0

-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

6.0

z-score

Laboratory Number

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Figure 3: z-Scores for Total Fat

67

64

90

3 25

40

65

84

78

74

12

4 68

22

73

19

83

5 46

9 42

49

7 44

36

93

91

48

70

71

54

16

47

29

50

15

85

43

27

28

37

13

39

20

38

62

32

87

86

8 56

21

35

89

34

57

72

2 31

18

11

45

60

1 30

58

51

80

23

6 82

55

59

75

33

76

79

14

24

23.86 g/100g

22.50 g/100g

21.15 g/100g

-10.0

-9.0

-8.0

-7.0

-6.0

-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

6.0

7.0

8.0

9.0

10.0

z-score

Laboratory Number

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Figure 4: z-Scores for Nitrogen

67

84

55

16

66

48

78

36

59

79

23

30

22

63

75

27

62

87

88

19

25

40

43

68

80

83

15

21

90

92

50

82

1 8 51

4 11

12

38

2 14

54

56

26

28

31

34

46

47

20

44

57

58

72

85

6 35

42

49

18

29

60

61

69

70

71

73

9 32

37

91

86

93

89

24

65

74

45

39

64

3

4.52 g/100g

4.36 g/100g

4.21 g/100g

-10.0

-9.0

-8.0

-7.0

-6.0

-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

6.0

7.0

8.0

9.0

10.0

z-score

Laboratory Number

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Figure 5: z-Scores for Titratable Acidity

88

31

58

57

43

39

78

32

65

19

55

40

47

50

60

44

75

63

3 70

71

73

54

48

29

4 11

30

51

90

56

62

82

14

34

61

27

42

79

28

86

18

74

84

15

45

12

1 6 2 36

7 59

67

16

1.27 g/100g

1.07 g/100g

0.88 g/100g

-10.0

-9.0

-8.0

-7.0

-6.0

-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

6.0

7.0

8.0

9.0

10.0

z-score

Laboratory Number

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Figure 6: z-Scores for Lactose

90

21

44

74

71

39

43

87

88

19

34

53

38

70

31

49

8 28

82

45

50

12

3 42

60

65

6 83

16

57

47

64

25

52

32

14

4 1 18

75

86

58

30

27

54

36

40

11

73

93

24

7 17

15

29

42.00 g/100g

39.49 g/100g

36.97 g/100g

-10.0

-9.0

-8.0

-7.0

-6.0

-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

z-score

Laboratory Number

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APPENDIX I: Analytical Methods Used by Participants

Methods are tabulated according to the information supplied by participants, but someresponses may have been combined or edited for clarity.

Moisture

Accredi ted Method Used laboratory number

yes 001 002 004 005 007 008 010 014 018 019020 021 022 024 028 032 034 036 038 039040 042 044 045 046 048 049 050 052 054057 058 059 063 065 067 072 073 075 076077 079 080 082 083 084 087 088 089 090

no 003 012 015 016 026 027 035 037 041 051055 060 064 068 074 086

Method Basis laboratory number

international standard 001 003 004 007 010 014 016 020 028 034036 037 049 051 055 060 072 075 076 079083 084 087 089 090

national standard 005 008 012 015 018 024 032 035 039 042044 045 048 057 059 065 067 073 077 088

In house method 022 026 040 041 054 064 068 082

Sample Weight (g) laboratory number

1 -

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Apparatus Used for Constant Weight laboratory number

conventional oven 001 003 004 005 007 008 010 012 014 015019 022 024 026 032 035 036 037 039 040041 042 044 045 046 048 049 051 057 059

060 064 067 068 072 073 074 075 077 080082 084 087 088 089 090

air circulation oven 016

drying oven specified in ISO 5537 / IDF 26 020

forced air 018

heated in beaker 065

microwave oven 076

vacuum oven 028 054 079 083

Oven Temperature (C) laboratory number

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Ash


yes 001 002 004 014 018 019 021 022 028 032034 035 036 038 039 040 042 044 045 046049 050 051 054 057 058 059 063 064 065072 073 075 076 079 080 082 083 084 087088 089 090 093

no 003 012 015 016 024 027 037 041 048 060068 074 086


international standard 003 004 014 028 034 036 037 048 049 051

060 064 072 074 075 076 079 083 084 087089 090

national standard 001 012 015 016 018 024 032 035 039 042044 045 057 059 065 073 088

In house method 022 041 054 068 082 093


1 -

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Ash Furnace Temperature (C) laboratory number

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Pre-extraction Stage laboratory number

yes 005 013 019 023 054 064 073 079 089

no 001 002 003 004 007 008 012 014 016 018020 021 022 024 027 028 032 033 035 036

037 040 044 045 046 049 050 051 057 059060 065 067 068 072 074 075 076 080 082083 084 086 087 090 093

Pre-extraction Time (hours) laboratory number

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Nitrogen


yes 001 002 004 008 014 018 019 020 021 022023 028 032 034 036 038 039 040 042 044045 046 048 049 050 051 054 057 058 059060 063 064 065 066 072 073 075 079 080082 083 084 087 088 089 090 092 093

no 003 012 015 016 024 026 027 035 037 055067 068 069 074 086


international standard 003 004 008 014 016 020 028 034 036 042

049 051 055 060 064 066 067 072 074 075079 084 087 088 089 090

national standard 012 015 018 023 032 035 039 045 048 057059 065 073

manufacturer/kit instructions/technical note 001 024

In house method 022 026 044 068 082


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Digestion Acid laboratory number

sulphuric acid 001 002 003 004 008 012 014 015 016 018019 020 021 022 023 024 027 028 032 035036 037 038 040 042 045 046 048 049 050

051 054 057 058 059 060 063 064 065 066067 068 069 072 073 074 075 079 080 083084 086 087 088 089 090 092

phosphosulphuric acid 082

Catalyst laboratory number

copper (Cu) 001 002 004 008 014 015 016 018 019 020022 023 027 028 032 036 037 038 040 042048 049 050 051 057 058 059 060 063 064065 066 072 073 074 075 079 080 083 084

086 087 088 089 090 092 093potassium (K) 001 002 008 012 014 018 020 027 032 036

038 040 048 051 057 058 059 060 065 068073 079 080 082 087 088 089

selenium (Se) 003 021 035 045 069 075 082 086

sodium (Na) 012 016 022 046 075

titanium (Ti) 001 008 019

kjeltab 054

Titratable Acidity


yes 001 004 007 018 019 032 039 040 042 044050 057 059 063 065 067 073 075 079 084

no 003 012 014 015 016 028 034 036 045 048051 054 055 058 060 074 086 088 090


international standard 004 034 045 048 055 060 063 067 073 074075 079 084 090

international book/journal 001 036 075

national standard 012 015 016 018 019 028 032 042 044 050051 057 059 065 088

manufacturer/kit instructions/technical note 003

In house method 014 054

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1 -

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international standard 004 008 017 018 028 034 053 060 064 083087 090

international book/journal 032 036 044 073 074 082 086

national standard 012 015 016 019 042 045 050 057 065 088

manufacturer/kit instructions/technical note 001 003

In house method 014 024 040 049 052 054 075


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Sample Hydrolysed laboratory number

yes 036 065

no 001 003 004 007 008 012 014 015 016 017018 021 024 032 040 042 044 045 049 050

052 053 054 057 060 064 073 074 075 082083 086 088 090 093

Sample Treatment Prior to HPLC laboratory number

acidify 008

blend/homogenise with solvent 001 032 040 049

centrifuge 032 036 064

degas 083

de-proteinise 008 040derivatisation 058

dilute 032 054 064

dissolve in water 008 024 032 052 054

filter 007 008 014 017 018 024 032 044 053 054057 064 075

hot water extraction 040 054

internal standard addition 008

Internal Standard Added laboratory number

yes 007 008 053 054 082 093

no 001 003 004 012 014 016 017 018 024 032036 040 044 045 049 050 052 057 060 064073 075 083 086 087 088 090

Internal Standard Used laboratory number

D(+)-melezitose 008

D-glucoheptose 054glycerine 007

melezitose 053

melibiose 093

trealose 082

none 017 032 049 057 083

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HPLC Injection Volume (L) laboratory number

5 -

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HPLC Detector Type laboratory number

conductivity 093

PAD 001 014 054

RI 007 008 017 024 040 049 052 053 064 075083 087

ELSD 032 044 057

Other Method laboratory number

Lane-Eynon 012 086

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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 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.

2. PROTOCOL

The Protocols [3, 4]set out how FAPASis organised. Copies can be downloaded from ourwebsite.

3. CONTACT DETAILS

This report was prepared and authorised on behalf of FAPAS by Michael Knaggs (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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