Division 11 Method performance characteristics (precision)

United Kingdom

Statistical results of the interlaboratory test: the following tables give the values for the following compounds: ethanal, ethyl acetate, acetal, total ethanal, methanol, butan-2-ol, propan-1-ol, butan-1-ol, 2-methyl-propan-1-ol, 2 methyl-butan-1-ol, 3 methyl-butan-1-ol.

The following data were obtained from an international method performance study carried out to internationally agreed procedures.

Year of interlaboratory test	1 997
Number of laboratories	32
Number of samples	5
Analyte	ethanal

Samples	A	B	C	D	E
Sample types
A Brandy; blind duplicates. B Kirsch; blind duplicates. C Grappa; blind duplicates. D Whisky; split levels (). E Rum; split levels ().
Number of laboratories retained after eliminating outliers	28	26	27	27	28
Number of outliers (laboratories)	2	4	3	3	2
Number of accepted results	56	52	54	54	56
Mean value ( $\times^{-}$ ) μg/g	63,4	71,67	130,4	38,4	28,6
Mean value ( $\times^{-}$ ) μg/g				13,8 (*)	52,2 (*)
Repeatability standard deviation (S_r) μg/g	3,3	1,9	6,8	4,1	3,6
Repeatability relative standard deviation (RSD_r) (%)	5,2	2,6	5,2	15,8	8,9
Repeatability limit (r) μg/g	9,3	5,3	19,1	11,6	10,1
Reproducibility standard deviation (S_R) μg/g	12	14	22	6,8	8,9
Reproducibility relative standard deviation (RSD_R) (%)	18,9	19,4	17,1	26,2	22,2
Reproducibility limit (R) μg/g	33,5	38,9	62,4	19,1	25,1

Year of interlaboratory test	1 997
Number of laboratories	32
Number of samples	5
Analyte	ethyl acetate

Samples	A	B	C	D	E
Sample types
A Brandy; blind duplicates. B Kirsch; blind duplicates. C Grappa; blind duplicates. D Whisky; split levels (). E Rum; split levels ().
Number of laboratories retained after eliminating outliers	24	24	25	24	24
Number of outliers (laboratories)	2	2	1	2	2
Number of accepted results	48	48	50	48	48
Mean value ( $\times^{-}$ ) μg/g	96,8	1 046	120,3	112,5	99,1
Mean value ( $\times^{-}$ ) μg/g				91,8 (*)	117,0 (*)
Repeatability standard deviation (S_r) μg/g	2,2	15	2,6	2,1	2,6
Repeatability relative standard deviation (RSD_r) (%)	2,3	1,4	2,1	2,0	2,4
Repeatability limit (r) μg/g	6,2	40,7	7,2	5,8	7,3
Reproducibility standard deviation (S_R) μg/g	6,4	79	8,2	6,2	7,1
Reproducibility relative standard deviation (RSD_R) (%)	6,6	7,6	6,8	6,2	6,6
Reproducibility limit (R) μg/g	17,9	221,9	22,9	17,5	20,0

Year of interlaboratory test	1 997
Number of laboratories	32
Number of samples	5
Analyte	acetal

Samples	A	B	C	D	E
Sample types
A Brandy; blind duplicates. B Kirsch; blind duplicates. C Grappa; blind duplicates. D Whisky; split levels (). E Rum; split levels ().
Number of laboratories retained after eliminating outliers	20	21	22	17	21
Number of outliers (laboratories)	4	3	2	4	3
Number of accepted results	40	42	44	34	42
Mean value ( $\times^{-}$ ) μg/g	35,04	36,46	68,5	20,36	15,1
Mean value ( $\times^{-}$ ) μg/g				6,60 (*)	28,3 (*)
Repeatability standard deviation (S_r) μg/g	0,58	0,84	1,6	0,82	1,9
Repeatability relative standard deviation (RSD_r) (%)	1,7	2,3	2,3	6,1	8,7
Repeatability limit (r) μg/g	1,6	2,4	4,4	2,3	5,3
Reproducibility standard deviation (S_R) μg/g	4,2	4,4	8,9	1,4	3,1
Reproducibility relative standard deviation (RSD_R) (%)	12,1	12,0	13,0	10,7	14,2
Reproducibility limit (R) μg/g	11,8	12,2	25,0	4,0	8,7

Year of interlaboratory test	1 997
Number of laboratories	32
Number of samples	5
Analyte	total ethanal

Samples	A	B	C	D	E
Sample types
A Brandy; blind duplicates. B Kirsch; blind duplicates. C Grappa; blind duplicates. D Whisky; split levels (). E Rum; split levels ().
Number of laboratories retained after eliminating outliers	23	19	22	21	22
Number of outliers (laboratories)	1	5	2	3	2
Number of accepted results	46	38	44	42	44
Mean value ( $\times^{-}$ ) μg/g	76,5	85,3	156,5	45,4	32,7
Mean value ( $\times^{-}$ ) μg/g				15,8 (*)	61,8 (*)
Repeatability standard deviation (S_r) μg/g	3,5	1,3	6,5	4,4	3,6
Repeatability relative standard deviation (RSD_r) (%)	4,6	1,5	4,2	14,2	7,6
Repeatability limit (r) μg/g	9,8	3,5	18,3	12,2	10,0
Reproducibility standard deviation (S_R) μg/g	13	15	24,1	7,3	9,0
Reproducibility relative standard deviation (RSD_R) (%)	16,4	17,5	15,4	23,7	19,1
Reproducibility limit (R) μg/g	35,2	41,8	67,4	20,3	25,2

Year of interlaboratory test	1 997
Number of laboratories	32
Number of samples	5
Analyte	Methanol

Samples	A	B	C	D	E
Sample types
A Brandy; blind duplicates. B Kirsch; blind duplicates. C Grappa; blind duplicates. D Whisky; split levels (). E Rum; split levels ().
Number of laboratories retained after eliminating outliers	26	27	27	28	25
Number of outliers (laboratories)	4	3	3	1	4
Number of accepted results	52	54	54	56	50
Mean value ( $\times^{-}$ ) μg/g	319,8	2 245	1 326	83,0	18,6
Mean value ( $\times^{-}$ ) μg/g				61,5 (*)	28,9 (*)
Repeatability standard deviation (S_r) μg/g	4,4	27	22	1,5	1,3
Repeatability relative standard deviation (RSD_r) (%)	1,4	1,2	1,7	2,1	5,6
Repeatability limit (r) μg/g	12,3	74,4	62,5	4,3	3,8
Reproducibility standard deviation (S_R) μg/g	13	99	60	4,5	2,8
Reproducibility relative standard deviation (RSD_R) (%)	3,9	4,4	4,6	6,2	11,8
Reproducibility limit (R) μg/g	35,2	278,3	169,1	12,5	7,9

Year of interlaboratory test	1 997
Number of laboratories	32
Number of samples	4
Analyte	butan-2-ol

Samples	A	B	C	E
Sample types
A Brandy; blind duplicates. B Kirsch; blind duplicates. C Grappa; blind duplicates. E Rum; split levels (*).
Number of laboratories retained after eliminating outliers	21	27	29	22
Number of outliers (laboratories)	4	3	1	3
Number of accepted results	42	54	58	44
Mean value ( $\times^{-}$ ) μg/g	5,88	250,2	27,57	5,83
Mean value ( $\times^{-}$ ) μg/g				14,12 (*)
Repeatability standard deviation (S_r) μg/g	0,4	2,2	0,87	0,64
Repeatability relative standard deviation (RSD_r) (%)	6,8	0,9	3,2	6,4
Repeatability limit (r) μg/g	1,1	6,1	2,5	1,8
Reproducibility standard deviation (S_R) μg/g	0,89	13	3,2	0,87
Reproducibility relative standard deviation (RSD_R) (%)	15,2	5,1	11,5	8,7
Reproducibility limit (R) μg/g	2,5	35,5	8,9	2,4

Year of interlaboratory test	1 997
Number of laboratories	32
Number of samples	5
Analyte	propan-1-ol

Samples	A	B	C	D	E
Sample types
A Brandy; blind duplicates. B Kirsch; blind duplicates. C Grappa; blind duplicates. D Whisky; split levels (). E Rum; split levels ().
Number of laboratories retained after eliminating outliers	29	27	27	29	29
Number of outliers (laboratories)	2	4	3	2	2
Number of accepted results	58	54	54	58	58
Mean value ( $\times^{-}$ ) μg/g	86,4	3 541	159,1	272,1	177,1
Mean value ( $\times^{-}$ ) μg/g				229,3 (*)	222,1 (*)
Repeatability standard deviation (S_r) μg/g	3,0	24	3,6	2,3	3,3
Repeatability relative standard deviation (RSD_r) (%)	3,4	0,7	2,3	0,9	1,6
Repeatability limit (r) μg/g	8,3	68,5	10,0	6,4	9,1
Reproducibility standard deviation (S_R) μg/g	5,3	150	6,5	9,0	8,1
Reproducibility relative standard deviation (RSD_R) (%)	6,1	4,1	4,1	3,6	4,1
Reproducibility limit (R) μg/g	14,8	407,2	18,2	25,2	22,7

Year of interlaboratory test	1 997
Number of laboratories	32
Number of samples	5
Analyte	propan-1-ol

Samples	A	B	C
Sample types
A Brandy; blind duplicates. B Kirsch; blind duplicates. C Grappa; blind duplicates. (*).
Number of laboratories retained after eliminating outliers	20	22	22
Number of outliers (laboratories)	4	4	6
Number of accepted results	40	44	44
Mean value ( $\times^{-}$ ) μg/g	3,79	5,57	7,54
Repeatability standard deviation (S_r) μg/g	0,43	0,2	0,43
Repeatability relative standard deviation (RSD_r) (%)	11,2	3,6	5,6
Repeatability limit (r) μg/g	1,1	0,6	1,2
Reproducibility standard deviation (S_R) μg/g	0,59	0,55	0,82
Reproducibility relative standard deviation (RSD_R) (%)	15,7	9,8	10,8
Reproducibility limit (R) μg/g	1,7	1,5	2,3

Year of interlaboratory test	1 997
Number of laboratories	32
Number of samples	5
Analyte	2-methylpropan-1-ol

Samples	A	B	C	D	E
Sample types
A Brandy; blind duplicates. B Kirsch; blind duplicates. C Grappa; blind duplicates. D Whisky; split levels (). E Rum; split levels ().
Number of laboratories retained after eliminating outliers	28	31	30	26	25
Number of outliers (laboratories)	3	0	1	5	6
Number of accepted results	56	62	60	52	50
Mean value ( $\times^{-}$ ) μg/g	174,2	111,7	185,0	291,0	115,99
Mean value ( $\times^{-}$ ) μg/g				246,8 (*)	133,87 (*)
Repeatability standard deviation (S_r) μg/g	2,3	1,6	2,5	1,8	0,74
Repeatability relative standard deviation (RSD_r) (%)	1,3	1,4	1,3	0,7	0,6
Repeatability limit (r) μg/g	6,4	4,5	6,9	5,0	2,1
Reproducibility standard deviation (S_R) μg/g	8,9	8,9	9,7	6,0	6,2
Reproducibility relative standard deviation (RSD_R) (%)	5,1	8,0	5,2	2,2	5,0
Reproducibility limit (R) μg/g	24,9	24,9	27,2	16,9	17,4

Year of interlaboratory test	1 997
Number of laboratories	32
Number of samples	5
Analyte	2-methyl-butan-1-ol

Samples	A	B	C	D	E
Sample types
A Brandy; blind duplicates. B Kirsch; blind duplicates. C Grappa; blind duplicates. D Whisky; split levels (). E Rum; split levels ().
Number of laboratories retained after eliminating outliers	25	26	25	27	25
Number of outliers (laboratories)	3	2	3	1	2
Number of accepted results	50	52	50	54	50
Mean value ( $\times^{-}$ ) μg/g	113,0	48,3	91,6	72,1	39,5
Mean value ( $\times^{-}$ ) μg/g				45,2 (*)	61,5 (*)
Repeatability standard deviation (S_r) μg/g	2,1	1,5	1,7	2,3	2,3
Repeatability relative standard deviation (RSD_r) (%)	1,9	3,1	1,8	3,9	4,5
Repeatability limit (r) μg/g	6,0	4,2	4,7	6,4	6,3
Reproducibility standard deviation (S_R) μg/g	7,4	3,8	6,6	4,7	4,5
Reproducibility relative standard deviation (RSD_R) (%)	6,6	7,9	7,2	8,1	8,8
Reproducibility limit (R) μg/g	20,8	10,7	18,4	13,3	12,5

Year of interlaboratory test	1 997
Number of laboratories	32
Number of samples	5
Analyte	3-methyl-butan-1-ol

Samples	A	B	C	D	E
Sample types
A Brandy; blind duplicates. B Kirsch; blind duplicates. C Grappa; blind duplicates. D Whisky; split levels (). E Rum; split levels ().
Number of laboratories retained after eliminating outliers	23	23	24	27	21
Number of outliers (laboratories)	5	5	4	1	6
Number of accepted results	46	46	48	54	42
Mean value ( $\times^{-}$ ) μg/g	459,4	242,7	288,4	142,2	212,3
Mean value ( $\times^{-}$ ) μg/g				120,4 (*)	245,6 (*)
Repeatability standard deviation (S_r) μg/g	5,0	2,4	3,4	2,4	3,2
Repeatability relative standard deviation (RSD_r) (%)	1,1	1,0	1,2	1,8	1,4
Repeatability limit (r) μg/g	13,9	6,6	9,6	6,6	9,1
Reproducibility standard deviation (S_R) μg/g	29,8	13	21	8,5	6,7
Reproducibility relative standard deviation (RSD_R) (%)	6,5	5,2	7,3	6,5	2,9
Reproducibility limit (R) μg/g	83,4	35,4	58,8	23,8	18,7