Ngi trnh by: TS.

NGUYN TiN DNG

C LNG V CNG B
KHNG M BO O
I. Gii thiu
II. Mt s Khi nim
III. Qui trnh c lng khng m bo o
IV. ng dng ca khng m bo o
V. Thc hnh c lng khng m bo
o theo ISO 19036
VI. Tho lun
NI DUNG
I. GII THIU
1. YU CU CA ISO/IEC 17025 V KB
- i vi Phng th nghim:
C v p dng th tc (5.4.6.2)
Phn tch thch hp (5.4.6.3)
Cng b trong bo co (5.10.3.c) khi:
+ Khch hng yu cu;
+ Xc nhn hiu lc ca kt qu;
+ Gii hn lm c s quyt nh s ph
hp qui nh k thut ;
+ VILAS yu cu.
2. PHNG PHP LUN DIN T V C LNG KB
O
- ISO.GUM.1995 (AGL 17 - 2005) - Hng dn nh gi v
din t khng m bo o.
- EURACHEM/CITAC Guide 2000 - Hng dn nh gi
KB trong phn tch ha hc nh lng
3. MT S TI LIU THAM KHO KHC
- TCVN 6910 (1 - 6) [ ISO 5725 (1 - 6) ]
- ISO/TS 21748:2004: S dng d liu c lng v lp li,
ti lp, ng c lng KB
- ISO/TS 19036: 2006: Hng dn v c lng khng
m bo o nh lng Microbiology of food and animal
feeding stuffs Guidelines for the estimation
ofmeasurement uncertainty for quantitative
determinations

I. GII THIU (tip)
1. NH NGHA V KB O
Thng s gn vi kt qu ca php o,
c trng cho s phn tn ca cc gi tr c
th quy cho i lng o mt cch hp l
VIM :1993 (3.9)
Thng s c trng cho s phn tn ca cc
gi tr ca i lng, c quy cho i lng o
da trn cc thng tin s dng
ISO/IEC Guide 99:2007
II. KHI NIM - KB
- Thc o khng m bo o:
- lch chun (hoc bi ca n) : S
- Na rng ca mt khong c mc tin cy
nh: a
- khng m bo o nh gi bng:
Phn b thng k ca 1 dy cc php o -
lch chun thc nghim nh gi kiu A
Phn b xc sut m phng bng thc
nghim hoc thng tin v lch chun. -
nh gi kiu B
II. KHI NIM - KB (tip)
- khng m bo o gm nhiu thnh
phn:
Ny sinh t nh hng ngu nhin
Ny sinh t nh hng h thng
- khng m bo o cho bit phm vi m
trong gi tr ca i lng xut hin vi
mt xc sut tin cy.
- Kt qu ca mt php o l c lng tt nht
ca gi tr i lng o v tt c cc thnh
phn khng m bo o
II. KHI NIM - KB (tip)
Sai s ca php o/error of measurement: Kt qu
ca php o tr i gi tr thc ca i lng o
[A 5 3.10 VIM draft 2004]
Sai s ngu nhin/Random error: Kt qu ca mt
php o tr i kt qu trung bnh t mt s v hn
cc php o cng mt i lng o trong iu kin lp
li.
[A 7 3.13 VIM draft 2004]
Sai s h thng/Systematic error: Kt qu trung bnh
t mt s v hn cc php o cng mt i lng o
trong iu kin lp li tr i gi tr thc ca i lng
o
[A 8 3.14 VIM draft 2004]
II. KHI NIM - SAI S (tip)
Gi tr trung
bnh ca tp hp
(m)
sai s
ngu nhin
gi tr thc (t)
sai s
Kt qu ca mt
php o (y)
sai s h thng
U
U
II. KHI NIM SO SNH KB V SAI S
Sai s:
+ L mt gi tr n l
+ Gi tr ca sai s c dng lm s hiu
chnh cho kt qu o
khng m bo:
+ Dng ca mt di cha gi tr ca i lng
+ Khng dng hiu chnh kt qu o
II. KHI NIM SO SNH KB V SAI S (tip)
- Cch din t
khng m bo chun u(x
i
)
- Phng php nh gi
nh gi khng m bo chun kiu A u
A
(x
i
)
nh gi khng m bo chun kiu B u
B
(x
i
)
- Phng php tng hp
khng m bo chun tng hp t cn
bc hai ca tng hp cc phng sai u
C
(y)
- Xc nh hp l
khng m bo o m rng U(y)

II. KHI NIM DIN T KB THEO GUM
chm (Precision): Mc gn nhau gia
cc kt qu th nghim c lp nhn c
trong iu kin qui nh
TCVN 6910 1 : 2001
Gm :
lch chun lp li/ repeatability standard
deviation
lch chun ti lp/ reproducibility standard
deviation
II. KHI NIM CHNH XC
lch chun lp li l thc hin th nghim
trn cc mu th ng nht, cng phng php,
trong cng mt phng th nghim, cng ngi
thao tc v s dng cng mt thit b, trong
khong thi gian ngn
lch chun ti lp l thc hin th nghim
trn cc mu th ng nht thc hin cng mt
phng php, trong cc phng th nghim khc
nhau, vi nhng ngi thao tc khc nhau, s
dng thit b khc nhau
II. KHI NIM CHNH XC
chch (Bias) : Mc sai khc gia k vng
ca cc kt qu th nghim v gi tr qui chiu
c chp nhn
Nghin cu chch l nghin cu tng sai
s h thng. S sai khc h thng so vi gi
tr quy chiu c chp nhn cng ln th
chch cng ln
chch gm:
chch phng th nghim
chch phng php
II. KHI NIM CHNH XC
La chn pp thc hin
Xc nh ngun gy ra
khng m bo o
Tnh ton khng m
bo o theo pp chn
Lp H s v khng
m bo o
Bc 1
Bc 2
Bc 3
Bc 4
III. QUI TRNH C LNG KB
D liu ni b t xc nhn hiu lc
phng php
Nghin cu lin phng v c tnh
ca phng php (theo ISO 5725 )
D liu kim sot cht lng trong qu
trnh o hoc th
D liu th nghim thnh tho
D liu nghin cu t trc
Tnh KB da vo d liu ph duyt phng php.
Nghin cu xc nhn hiu lc phng php phn tch
nh lng cn xc nh c trng mt vi hoc tt c cc
thng s sau:
1. chm/Precision: gm
lch chun lp li
lch chun ti lp
chm trung gian/ lch chun ti lp trung gian
2. chch/Bias
3. Tnh tuyn tnh/Linearity
4. Gii hn pht hin/Detection limit
5. Tnh chn lc/Selectivity
Tnh ton khng m bo o da vo d liu c sn
Nguyn tc ca ISO/TS 21748 l:
Tnh KB t cc ngun d liu sn c
v nghin cu chm v ng (
lp li, ti lp, chch)
Tng hp thm cc ngun KB khng bao
gm trong nghin cu chm, ng
v trong chng trnh so snh lin phng.
khng m bo ca php o tnh theo cng thc

=
+
+ + + =
n
i
i i r
R lab method
x u c S u
S u B u B u y u
1
2
2
2
2 2 2 2
) ( ) (
) ( ) ( ) ( ) (
Trong :
) (
) (
) (
R
lab
method
S u
B u
B u
KB lin quan chch phng php
KB lin quan chch PTN
KB lin quan lch chun ti lp
Tng bnh phng cc KB khc do
cc ngun cha nghin cu trong nghin
cu chnh xc ca php th

=
n
i
i i
r
x u c
S u
1
2
2
) (
) (
KB lin quan lch chun lp li
Nghin cu chch ca PTN theo hng dn nghin
cu thu hi.
Nghin cu chch ca phng php t chng trnh
so snh lin phng v tnh lch chun theo cng
thc sau:
Trong :
p: S lng phng th nghim
N: s ln th lp li ca mi phng th nghim
p
S
n
S
B S B u
r R
method method
2 2
)
1
1 (
) ( ) (

= =
Ghi ch
KB ch l c lng, nu d liu c lng
khng c sn th phi chp nhn nhng d liu
c sn v c th c lng c v nu l do.
Thng KB khng c qu nh.
i khi ch c th c c lng th v KB.
C c lng c phn no cn hn l khng c g
c bng cch s dng cc d liu c sn.
Nu khng c thng tin g th phi xem li phng
php th nghim l phng php g?.
Tnh ton KB o tng hp
khng m bo o tng hp:
y = f(x
1
, x
2
,...,x
n
)
Trong :
u
c
: khng m bo o tng hp
u(x
i
): khng m bo thnh phn th i
n: s thnh phn khng m bo
c
i
: h s nhy ca thnh phn th i

=
=
n
i
i i c
x u c y u
1
2 2
) ( ) (
Mt s quy tc tnh khng m bo tng hp
Cng v tr:
V
y
= V
a
+ V
b
Nhn v chia:
C = W/V
q = Bx
Khi B l hng s:

Ly tha: q= X
n
(
(

|
.
|

\
|
+
|
.
|

\
|
=
2 2
v
u
w
u
c
u
v w c
x
nu
q
u
x
q
=
b a
v v
y
u u u
2 2
+ =
x q
Bu u =
V d tnh khng m bo tng hp
Gi s : y = p +q + r
Bit : p = 5,02 ; q = -6,45 ; r = 9,04
v : u(p) = 0,13 ; u(q) = 0,05 ; u(r) = 0,22
Tnh y v khng m bo chun ca n
p dng quy tc 1:
y = 5,02 - 6,45 +9,04 = 7,61

26 , 0
22 , 0 05 , 0 13 , 0
) (
2 2 2
= + + = y u
V d tnh khng m bo tng hp

Gi s : y =(o. p / q . r )
Bit : o = 2,46 ; p = 4,32 ; q = 6,38 ; r = 2,99
v : u(o) = 0,22; u(p) = 0,13 ; u(q) = 0,11; u(r) = 0,07
Tnh y v khng m bo chun ca n
ap dng quy tc 2:
y = (2,46. 4,32) / ( 6,38 2,99) = 0,56

024 , 0 56 , 0 ) (
99 , 2
07 , 0
2
38 , 6
11 , 0
2
32 , 4
13 , 0
2
46 , 2
02 , 0
2
= + + + = |
.
|

\
|
|
.
|

\
|
|
.
|

\
|
|
.
|

\
|
y u
khng m bo o m rng
U = k.u
c
(y)
Trong :
U: KB o m rng
k: h s ph
u
c
(y): KB tng hp ca i lng o y
S dng h s ph k = 2 vi mc tin cy xp x 95%
Theo:
- qui nh ca VILAS
- qui nh ca APLAC-MRA
- khuyn co ca GUM v EURACHEM
H s c lng KB o
Hon thnh mt bo co phn tch nn lu h s
bao gm nhng iu sau:
- phng php s dng tnh ton kt qu v
khng m bo;
- Cc gi tr v ngun v phn tch khng
m bo;
- Danh mc tt c cc thnh phn ca khng
m bo v s liu tnh ton ca mi thnh
phn;
- D liu v phn tch cn din t theo mt
cch r rng c th tnh li nu cn thit.
Bo co kt qu KB o
Phn tch: Kt qu x (n v) kxU (n v)
Y = y (n v) kxU (n v)
Bo co KB c tnh ton bng cch s
dng h s ph k bng 2 [xp x vi mc
tin cy l 95%]
C s khoa hc nh gi s ph hp ca
sn phm hoc qu trnh;
Biu th cht lng ca kt qu hiu
chun v th nghim to s tin cy cho
ngi s dng trong vic so snh cc kt
qu ca cng mt i tng o cc PTN
khc nhau. S tin cy l iu quan trng
tin ti xo b hng ro thng mi quc
t;
IV. NG DNG CA KB O
Gip cho vic xc nhn hiu lc phng
php ;
L mt phn khng th thiu trong tnh
lin kt chun ca mt kt qu o;
p ng yu cu ca tiu chun ISO/IEC
17025 : 2005
IV. NG DNG CA KB O (tip)
S dng gi tr UM
nh gi s ph hp v so
snh gia cc kt qu
V. THC HNH C LNG KHNG
M BO O THEO ISO 19036
Phm vi p dng theo ISO 19036
Hng dn c lng khng m bo o cho cc
phng php nh lng vi sinh vt trong thc phm bng k
thut m khun lc.
Cc dng thc phm cho ngi, thc n gia sc, cc mu
mi trng
Cch tip cn tnh UM da trn standard deviation of
reproducibility of the final result of the measurement /
lch chun ti lp ca kt qu o cui cng.
Khng p dng trong cc trng hp:
- nh lng bng k thut MPN

Bo co xc nh UM
Xc nh cc ngun ca UM:
Qui trnh thc nghim:
nn mu; cch ly mu phn tch;
vi sinh vt ch/nhm VSV ch trn nn mu; s mu/1 nn
mu/qui trnh TN>= 10samples of the same matrix.
Chn nn mux mang tnh i din
TN cc ngy khc nhau (bao hm ton b cc k thc hin TN
khc nhau)
Thc hin dy Pha long trong di nng TN hng ngy
Tt nht l cc mu nhim t nhin, h VSV t nhin-
> Gn nht vi cc iu kin th nghim hng ngy
La chn cng thc tnh ton v cng b kt qa UM: U = log10 (c)
k RSD RC (k = 2) ( lch chun ti lp)
Lu : i vi pp nh tnh ch xc nh ngun gy nn UM v cng
b gii hn pht hin ca pp. PP nh lng gm tt c cc bc
trn
Bo co kt qu UM

ISO/TS 19036:2006

8,0 log 0,14 log

8,0 log [7,9; 8,1]

10
8
CFU/ml [7,910
7
; 1,310
8
]

(10
8
CFU/ml [10
8
- 79%; 10
8
+
130%])






S khun lc di 30
U=uk (U=2S
R
) h s k= 2, vi tin cy 95%; s
khun lc nh lng t 10 30 CFU.





30
0,18862
C
0,18862
S 2 U
2
R
+ + =

C : tng s khun lc m
c

ISO/TS 19036: 2009 (amd)
V d tnh ton UM
CFU/ml 100.000
0,0022
220
0,0001 0,0001 0,001 0,001
10 6 104 100
(C) Result = =
+ + +
+ + +
=
log 0,15
2,30259
0,35
2,30259
RS
SR Us
R
= = = =
log 5,0 (C) Log =
log 0,3 2S U usikkerhet Utvidet
R
= = =

5,0 log 0,3 log
5,0 log [4,7; 5,3]
100.000 CFU/ml [50.000; 200.000]
10
5
CFU/ml [510
4
; 210
5
]
(100.000 CFU/ml [100.000 - 50%; 100.000 + 100%])
(10
5
CFU/ml [10
5
- 50%; 10
5
+ 100%])


CFU/ml 100
0,22
22
0,01 0,01 0,1 0,1
3 1 7 11
Resultat = =
+ + +
+ + +
=
log 0,11 S U Usikkerhet
R
= = =
log 2,0 Resultat =
0,30
30
0,18862
22
0.18862
0,11 2
30
0,18862
C
0,18862
S 2 2U
2
2
R
= + + = + + =

2U 2S usikkerhet Utvidet
R
= =

2,0 log 0,3 log
2,0 log [1,7; 2,3]
100 CFU/ml [50; 200]
10
2
CFU/ml [510
1
; 210
2
]
(100 CFU/ml [100 - 50%; 100 + 100%])
(10
2
CFU/ml [10
2
- 50%; 10
2
+ 100%])

k=2 (vi mc tin cy 95%)
Ti liu tham kho
ISO/TS 19036:2006
www.pronorm.no
International Accreditation New Zealand, Technical guide:
Uncertainty of Measurement Precision and Limit of
Detection in Chemical and Microbiological Testing
Laboratories (2004)
www.ianz.govt.nz

Standard Unit, Evaluations & Standards Laboratory,
Center for Infections
Uncertainty in Measurement in Testing (QSOP 4: 2005)
www.evaluations-standards.org.uk

Verden gr videre!!