ISO/IEC 17025

1.
2. ISO/IEC 17025
3. ISO/IEC 17025
4.
ISO/IEC 17025
5. ISO/IEC 17025-2005
5.1
5.2
5.3
5.4
5.5
5.6
5.7
5.8
5.9
5.10
5.11
6. ISO/IEC 17025
6.1
6.2
6.3
7.

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5

ISO/IEC 17025-2005

ISO/IEC 17025-2005

5
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ISO/IEC 17025

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1.



.. 2535



ISO/IEC 17025
2546

8
-
2549 2550
ISO/IEC 17025


ISO/IEC
17025
2. ISO/IEC 17025
ISO/IEC 17025

3. ISO/IEC 17025
ISO/IEC
(International Standardization Organization, ISO)
-3-

 (International Electrotechnical Commission, IEC) ISO

Guide 25, 9000, 14000

ISO/IEC 17025
(General Requirements for the Competence of Testing and Calibration
Laboratories) .. 2521 1
ISO Guide 25- 1978: Guideline for Assessing the Technical
Competence of Testing Laboratories (GLP)
ISO/IEC Guide 25- 1982: Guideline Requirement for the
Competence of Testing Laboratories (Quality System)
ISO/IEC Guide 25- 1990: Guideline Requirement for the
Competence of Calibration and Testing Laboratories (Calibration, ISO 9002)
ISO/IEC 17025- 1999: General Requirements for the
Competence of Testing and Calibration Laboratories
ISO/IEC 17025- 2005: General Requirement for the
Competence of Testing and Calibration Laboratories
1 ISO/IEC 17025
ISO/IEC 17025 -1999 .. 2542 (.. 1999)
ISO/IEC
17025-1999

ISO/IEC 17025-1999
28 2543 .
17025-2543 (ISO/IEC 17025 -1999):




ISO/IEC 17025-1999 ISO 9001:1994 ISO
9002:1994 ISO 9001:2000
ISO/IEC 17025-1999 ISO/IEC 17025-2005
-4-


ISO 9001:2000
.17025-2543 . 17025-2548
ISO/IEC 170252005 General Requirement for the
Competence of Testing and Calibration Laboratories ISO/IEC
31 2548

ISO/IEC
17025-2005 2


. 17025-2548 ISO/IEC 17025-2005
4.
ISO/IEC 17025-2005
ISO/IEC 17025-2005
(Management Requirements) 15 (Technical
Requirements) 10 1 4
5

1. ISO/IEC 17025-2005
4.1)
4.2)
4.3)
4.4)
4.5)
4.6)
4.7)
4.8)
4.9)
4.10)
4.11)
4.12)
4.13)
4.14)
4.15)
-5-

5.1)
5.2)
5.3)
5.4)

5.5)
5.6)
5.7)
5.8)
5.9)
5.10)

5. ISO/IEC 17025-2005


5.1
ISO/IEC 17025-2005



ISO/IEC 17025-2005 25

5.2.


1) (Quality Manual, QM)
ISO/IEC 17025-2005 25

-6-

 2
ISO/IEC 17025-2005

4.1
4.1.2
4.1.3
4.1.4
4.1.5()
4.1.5()
4.1.5()
4.1.5()
4.1.5()
4.1.5()
4.1.5()
4.1.5()
4.1.5()

4.1.5()
4.1.5()
4.1.6
4.2
4.2.1

4.2.2
4.2.3
4.2.4
4.2.5
4.2.6

ISO/IEC 17025

ISO/IEC17025

-7-


4.2.7
4.3
4.4
4.4.1
4.5
4.6
4.6.1
4.6.2
4.7
4.7.1
4.7.2
4.8
4.9
4.10
4.11
4.12

4.13
4.13.1
4.13.2
4.14
4.15

5.2
5.2.1
5.2.2
5.2.3
5.2.4
5.2.5

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5.3
5.3.1
5.3.2
5.4
5.4.1
5.4.2
5.4.5
5.4.6
5.4.7
5.5
5.5.1
5.5.2
5.5.3
5.5.5
5.5.6
5.6
5.6.1
5.6.2
5.6.3
5.6.4
5.7
5.8
5.8.1
5.8.2
5.8.3
5.9
5.9.1
5.9.2
5.10

SI

2) (Standard Operating Procedure, SOP)

22
25

3) (Standard Test Method, STM)

-9-

4) (Instrumental Operating Manual, IOM)

5) (Work Instruction, WI)


6) (Technical Document, Tech. Doc)

APHA/AWWA/WEF Standard Method for the Examination of Water and
Wastewater
7) (Laboratory Notebook, LNB) (Form)
(Label)
/
//


5.3

/

(Record)



5.4




2 6

- 10 -

5.5

5.6






ISO/IEC 17025 (QM)
(, SOP)



5.7

- -

-
ICP/MS

5.8




- 11 -


ISO/IEC 17025-2005
(Intermediate check)


5.9

/ /
4.4 ( )
(Lab Sample ID)


(Laboratory Information Management System, LIMS)
5.4.7 ()
5.10

/ (
1) (Accuracy) (Precision)
(Limit of Quantitation, LOQ) (
2)

(International System of Units, SI )

(Method blank) (Duplicates)
(Recovery of Known Addition)
(Calibration Check Standard)
(Control Chart)
(Proficiency Testing) ()
( CAEAL, Canadian Association for Environmental Analytical Laboratories
EANET, The Acid Deposition Monitoring Network in East Asia ; NILU,
Norwegian Institute for Air Research )
5.11

1
- 12 -


(Internal Auditor) 2
6





6. ISO/IEC17025
6.1
ISO/IEC17025
(
)
3
3

(R-02)
1)
2)
6
3)

1)

1
2)
12
3)
3
4)

1

4
5)

1)
2)

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(LA-R-03)
1)
2)
6
3)

1)

1
2)
1
3)
3 6
4)

1

4
5)

1)
1
2)
6

(R-02)
3)


3

1
4) 3

5)
1 3

6)

90
7)

1)

...

2)

3)

4)

1)

2)

- 14 -

(LA-R-03)
3)


3

1
4) 3

5)
12
3

6)


30
7)

45

1)

xxxx

2)

3)

4)

1)

2)

(R-02)
3)
/

4)
5)

6)
1) 1,000
2) 5,000
/
3) 10,000 /
1

(LA-R-03)
3)
/

4)
5)

6)
1) 1,000
2) 2,000
//
3) 10,000 /

6.2


1)

2)
3)

4)

5)

6)

7) (Certified Reference Materials/Reference Materials)

8)
9)
ISO/IEC17025
10)
11)
- 15 -




6.3

1
1
6
6

2-3

15

3

1


1
6

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7.


4
4

1) (QM)
2) (SOP)

3)
4)

1)
2)

3)
/ /
/

..
2535

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100,000
5
5

-1
-2

-3
-4

-5

-1

-2

-3

-4

-2

..


.

(

)

( .
)
1)
2)

.

.

1)
.
.
2)

-

.

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-3

-4

-1

-2

-3

-4

-1

-2

1)
.
.
2)

-



.
.
1)
CAEAL

.
2) (invoice) CAEAL
(
)

1)

CAEAL.
2) FedEX
CAEAL
1)

.
2)

-
-
-

- 19 -

-3

.-1
.

.-2

.-3

.-4

.-5

-1

-2

-3

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-5

-
-

-
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.
1)
2)

1)
2)
3)
4)

1)
2)

1)
2)
3)
4)

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1. . 17025-2548 (ISO/IEC 17025-2005) :

(General Requirements for the Competence of testing and Calibration Laboratories)
2.
. 17025-2548 (G-02-2/08-05)
:
(ISO/IEC 17025-2005)
3.
(R-02-4/01-07)
4.
( .17025) (R-08-02/08-01)
5.
(F-AP07-5/01-07)
6.
(LA-R-03)
7.
(LA-F-02-5/06-06)
8. ( 3)
.. 2539
9. 2550

- 21 -

- 22 -


1. (Purpose)

2. (Scope)


3. (Work Instruction)
3.1
Method Validation
Standard Method




3.2 ( tools ) performance characteristic

Accuracy
Precision
Range
Linearity
Limit of Detection
Limit of Quantification
Specificity/Selectivity
Ruggedness /Robustness
Accuracy
(Measure Value) (True
Value) Analyte Accuracy
Bias
Bias

Bias = ( x - )
x

Accuracy 3
1

- 23 -

 1 (Standard Reference Materials (SRM))/(Certified

Reference Materials (CRM)
2
3 Analyte (Spiked Sample/
Fortified Sample)
1 (Standard Reference Materials (SRM)/
Certified Reference Materials (CRM))
1. Reagent Blank Standard Reference Materials (SRM)/Certified Reference
Materials (CRM) 7
2. Blank
3. (Certified Value) CRM/SRM
Accuracy
3.1 % Recovery Standard Reference Materials (SRM)/Certified
Reference Material (CRM)
% Recovery
% Recovery = ( 100) /
90- 110%

3.2 Certified Value Standard Reference Materials

(SRM)/(Certified Reference Materials (CRM)
Certified Value Uncertainty
3.3 t-test 10

1) Reagent Blank Standard Reference Materials (SRM)/

Certified Reference Materials (CRM) 10
2) Blank
3). CRM/SRM (Certified Value) t-test

(SD/ n )
t -test = ( X - )
df
= n-1
X =
SD =
= Reference Value
df = degree of freedom
n =
t - Critical (tc) t tc
tc degree of freedom (df)
- 24 -

 2
1. Reagent Blank Standard Reference Material (SRM)/ Certifild Reference
Material (CRM) 10
2. Blank
3. 2 t-test

t = (X1 X 2 ) /[(SD1 2 / n 1 ) + (SD 2 2 / n 2 ]1 2

df = ( n1- 1) +(n2 1 )
df = ( n1+n2 2 )
X 1
X 2
SD1
SD2
n1
n2
df degree of freedom
t- Critical (tc) tc degree of
freedom t tc
3. Analyte

reagent blank, unspiked spiked sample
3 7
% Recovery
% Recovery =
( C sp C s 100) / Ca
Csp spiked sample
Cs unspiked sample
Ca
80-120%

Precision

% RSD %CV

%CV = % RSD =

SD
100
X

Precision
- Repeatability ( r ) Precision
- 25 -


- Reproducibility (R) Precision

precision
1. RM (Reference Materials) fortified sample blank
3 10
2. Mean () (Standard Deviation (SD))

3. % RSD (Relative Standard Deviation) % CV

% RSD
= (SD x 100)
= %CV
X
3
1. Horwitz equation
2. F-test 2
3. % RSD Reference AOAC (AOAC Peer-Verified
Method, Nov. 1993)

% RSD

100 %
1.3
10 %
2.8
1 %
2.7
0.1 %
3.7
100 ppm
5.3
10 ppm
7.3
1 ppm
11
100 ppb
15
10 ppb
21

Range
(
) precision, accuracy
Range
1. blank ( precision
accuracy )

2. (Accuracy)
(Precision) %Recovery %RSD (Relative Standard Deviation)
3. %Recovery 85-110% % RSD 10 %
Range Linearity
- 26 -

Linearity
(linearity)

Correlation Coefficient( r ) 0.995
Linearity
1. Blank ( Fortified Sample Blank (
6 blank)
2. (Concentration)
(Response) (Concentration) X (Response)
Y
3. Correlation Coefficient (r)
r 0.995

Limit of Detection (LOD)

LOD (Quantitative Analysis) 3

1. APHA/AWWA/WEF
1.1 Inject ( 5 IDL)
( 20 )
1.2 SD (Standard Deviation)
1.3 LOD LOD = 2(1.645)SD
2. EURACHEM
LOD (Limit of detection) 2
1 Sample Blank 10
LOD LOD = mean+3SD
2 Fortified Sample 10
LOD LOD = mean + 4.65SD
3. TAYLOR
3.1 blank spike sample 3 ( )
7
3.2 ( SD )
3.3 plot curve concentration ( x) standard deviation (y)
- y So
- LOD LOD = 3So

- 27 -

Limit of quantification (LOQ)

Accuracy Precision

LOQ 3
1. APHA/AWWA/WEF
LOQ (Limit of Quantification )
1. reagent blank 20
2. (SD)
3. LOQ = 10 SD
2. EURACHEM
LOQ (Limit of Quantification) 2
1
1. sample blank 10 SD
a. LOQ = mean + 10 SD
b. fortified sample LOQ
c. Accuracy precision
2
1. fortified sample aliquots of a sample blank LOD
10 LOQ Accuracy Precision

3. TAYLOR
LOD Taylor LOQ = 10 S0
SPECIFICITY / SELECTIVITY
(Sample Matrix)

Specificity/Selectivity
()
()

Robustness / Ruggedness
pH accuracy precision.
Ruggedness
1.
2. (Youden)
3.
4. Accuracy Precision.

- 28 -

3.3 /

performance characteristic tools
3.4 /

3.5 /

3.6 /
/
3.7 Method Validation

Method Validation Method
Validation Reference Method Validation

4. (Tools)

Blank :
- solvent blank /reagent blank blank
/solvent
- Sample blank, matrix blank, solution blank blank
matrix (Analyte)

Fortified sample

% recovery
Spiked sample

% recovery spiked
spiked

Sample of known analyte content

reference material
Reference standard


Certified reference material (CRM)
- 29 -

Replication

Interlaboratory comparison proficiency testing

5.
- mean : ( data )
population mean : (True mean)
N

Xi

= i=1
N
N =
Sample Mean : X
n

Xi

X = i=1
n
n =
- Variance XI Mean

2
2 (X i )
1.Population Variance: =
N =
N
(X i X )
S=
n

2.Sample

Variance :

n =

- Standard Deviation (SD)

mean
1. Population SD: =

(X i ) 2

- 30 -

N =

2. Sample SD :

S=

(X i X ) 2
n 1

n =

- Standard Deviation of Mean /Standard Error

Xi
SD
N =
1. Population n =
N
SD
2. Sample
n =
Sn =
n
- Significant Level/Confidence Level P
P =0.05 ( CL=95%) 0.05
5%
- t-test/F-test 2
1 accuracy mean
Reference value( )
(X )
t=
( SD / n )
df = n-1
t-critical ( tc )
tc degree of freedom(df)
t < tc 2
t < tc 2
2 mean 2
(X 1 X 2 )
t=
SD1 2 SD 2 2
+

n
n

1
2

df = (n1-1)+(n2-1) = n1+n2-2
t-critical (Tc)

- Coefficient of Variation (CV) Relative Standard Deviation (RSD)

precision
SD
%CV = % RSD = 100
X
- F-test precision
variance (S)2 2

- 31 -

S2
F = 12
S2

S12> S22

df = n-1
F-critical (Fc)
Fc degree of freedom(df)
F<Fc 2
F>Fc 2
- Correlation Coefficient (r) (linearity) ( y =
a+bx )

r=

n X i Yi X i Yi
n X i 2 ( X I )2 n Yi 2 ( Yi )2

][

r +1 +1
r = +1 X Y

r = -1
X Y
r = 0.0
- Horwitz equation precision
1. predicted RSD (RSDp) % RSD
2.
Horwitz ratio = experimental RSD < 1
Predicted RSD
3. Horwitz predicted RSD (RSDP)
1. Reproducibility Horwitz predicted RSD (RSDR) = 2(1-0.5logc )
2. Repeatability Horwitz predicted RSD (RSDr) = 0.66 x 2(1-0.5logc)
i.e. 1% C = 10-2
1 ppm , C = 10-6
C = faction concentration
6. (Reference)
6.1 APHA/AWWA/WEF, Standard Methods for the Examination of Water and Wastewater

21st edition,2005, part 1010 C., 1030 C.

6.2
6.3
6.4

EURACHEM GUIDE, The Fitness for Purpose of Analytical Method; A Laboratory Guide to
Method Validation and Related Topics, December 1998 ( WWW.vtt.fi/Ket/euracherm )
Taylor, John Keenan Quality Assurance of Chemical Measurements, Lewis Publishers,
Michigan, 1987
/

- 32 -

- 33 -


1.

2.
2.1
(Uncertainty of Measurement ; U)

1.
1.1 (random uncertainty, UR)

1.2 (systematic uncertainty; Us)

2.
2.1 Type A
Type A

Type A
n
n
X = 1 Xk -------------------- (1.1)
n k=1
Xk k X


(Standard deviation) n
n 200
n
SD = { (Xi - X)2 }1/2 ----------------- (1.2)
i=1 n
X =


n
SD = { (Xi X)2 }1/2
- 34 -

-------------------- (1.3)

i=1 n-1
X =

= SD
-------------------- (1.4)
n
(1.4)
Type A
U (Xi) =
--------------------- (1.5)


n=1
(1.4)
10 4
2.2 Type B

Type B
Type B

-
-
-
-
Type B

(Standard uncertainty; Ux)

x
Type A Type B
Ux = a
k
a =
k = (confidential factor)
(a)
1. (repeatability)
- 35 -

1.1 (repeatability)
standard deviation of mean (Sn) standard deviation (SD)
SD = a / n

SD = a
1.2 (RSD) coefficient of variation
(CV) (%RSD) / X = SD x 100 = %CV

%RSD x X = SD = a
100

2.
2.1
1000 + 0.08
a = + 0.08 ml
2.2 (purity) C+U
a = +U
2.3 C+U
a = +U
3.
volumetric flask 100 ml + 4 oC
= 2.1 x 10-4 ml/ oC
= 2.1 x 10-4 x 4 x 100 = 0.084 ml = a
(Confidential factor, K)
1. (normal distribution)
1.1 type A (repeatability) K = 1
1.2 type B 95 % K = 1.96 K = 2
2. (rectangular distribution)
K = 3
3. (triangular distribution)
K = 6
4. U (U-shape distribution)
K = 2

- 36 -

Table 1 Source of Uncertainty

Divisor
Distribution
6
Triangle

Source
Temperature

Repeatability
Electricity, Energy, Frequency
Calibration Certificate
Reference Standard (Type B)
Drift
Resolution
Internal calibrate glasses
External calibrate glasses
Accuracy

1
2
2

Normal
U-shape
Normal

3
3
6
3
3

Rectangular
Rectangular
Triangle
Rectangular
Rectangular

2.2
()

U1

U2

U3
Result

U4

U5

U6

U1-6 =
2.2.1 (Purity)
Standard Certificate 99.99 + 0.01%
Value = 0.9999 + 0.0001
Ux = a/ 3 = 0.0001/ 3
= 0.000058
2.2.2 Volumetric flask / pipette
- Calibration
volumetric flask 100 + 0.1 ml
a) + 95%
Ux = a/2 = 0.1/2 = 0.05 ml
b) Triangular distribution

- 37 -

Ux = a/ 6 = 0.1/ 6 = 0.04 ml
- Repeatability / Precision
10 standard
deviation volumetric flask 100 ml SD = 0.02 ml
Ux = SD = 0.02 ml
- Temperature
= 2.1 x 10-4 ml/ oC
volumetric flask 100 ml + 4 oC
volumetric variation = 2.1 x 10-4 x 4 x 100 = + 0.084 ml
rectangular distribution
Ux = a/3 = 0.084/3 = 0.05 ml
2.2.3 (Weight / Balance)
- Repeatability / Precision mass/balance
mass 50-200 g standard deviation = 0.04 mg
Ux = S = 0.04 mg
tare gross precision
- Linearity / Uncertainty Calibrate
0-10 g Linearity + 0.03 mg
Ux = a/ 3 = 0.03/ 3
= 0.017 mg
tare gross standard uncertainty 2 ( tare 1 )
2.2.4

-
=+a
- (Standard deviation) = SD
- Relative Standard Deviation
= %RSD
- Coefficient of Variance
= %CV
- Reproducibility Repeatability
=+a
- Linearity Sensitivity
=+a
-
=+a
- Recovery
=+a

= + a
1.1 95 %
Ux = a/2
1.2
Ux = a/ 3

- 38 -

SD
Repeatability/Reproducibility
Ux = SD
Peak area / Peak height / Intensity / Absorbance
- Repeatability / Precision Standard Sample
n
- replicate sample standard deviation, SD
Ux = SD/ n ( Ux )
UX = SD ()
- Instrument Calibration / Validation / Performance / Reproducibility

uncertainty reproducibility Standard deviation, SD
Ux = SD

2.2.5 Recovery
%Recovery n Standard deviation
Ux = SD/ n
recovery 42 recovery 90 %
Standard deviation 28 %
Ux = 28/ 42
= 4.32 %
= 0.0432 (g/g)
2.2.6 Correction factor - replicate
- correction factor

- / clean up
- (Replicate)
Ux = SD
2.2.7 Proficiency test
Inter Comparison Laboratory
Ux = SD

2.4

2.4.1
Uc = U2x1 + U2x2 + + U2xn
2.4.2
Uc = C RSD1 2 + RSD2 2 + + RSDn 2
C

- 39 -

 RSD = Ux
V
V parameter
RSD 1/3 RSD

2.5
UE = kpUc
95% (kp = 2) UE = 2Uc
2.6
C+U
C
U
3.
3.1 EURACHEM/CITAC Guide Quantifying Uncertainty in Analytical Measurement., Second Edition.
2000

- 40 -