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(123doc) Gioi Han Phat Hien Tham Dinh Phuong Phap Phan Tich Hoa Hoc
(123doc) Gioi Han Phat Hien Tham Dinh Phuong Phap Phan Tich Hoa Hoc
HCM
KHOA K THUT HA HC
TIU LUN
MC LC
Trc khi p dng mt phng php phn tch cn c cc chng minh rng
phng php p ng yu cu t ra, tc l phng php gii c thm
nh. Yu cu ny khng ch cho cc phng php th ni b m cn cn cho
cc phng php tiu chun. Vic thm nh phng php tiu chun v phng
php ni b c s khc nhau, do cn ch khi lp k hoch thm nh. C
hai yu cu ch yu ca vic thm nh phng php tiu chun:
Phi c kt qu thm nh ca phng php tiu chun, v kt qu ny phi ph
hp vi yu cu ca phng th nghim.
Phng th nghim cn m bo c th t c cc thng s c m t trong
phng php tiu chun.
Theo yu cu ca ISO 17025, khi cc phng th nghim p dng cc phng
php tiu chun cn c h s nh gi cc iu kin c bn, cc ngun lc theo
yu cu ca phng php th v vic t c kt qu th nghim c chnh
xc nh phng php yu cu hoc nh mong mun ca phng th nghim. i
vi cc phng php th ban hnh m khng c d liu v chnh xc th
phng th nghim phi xc nh d liu chnh xc ca php th da trn d
liu nghin cu th nghim
xy dng cc bc thm nh phng php tiu chun cn kim tra:
1. Phng php c thm nh hay cha, thm nh ton b hay mt phn
2. Nn mu c ging nhau hay khng
3. Khong lm vic ca phng php c ph hp vi yu cu ca phng th
nghim hay khng
4. C cng loi thit b ( hang sn xut, model) hay khng? Phng php tiu
chun c cho s dng cc loi thit b khc khng ?
5. C nhng lu g c bit ca phng php tiu chun m phng th
nghim khng th p ng khng ?
Nu mt trong cc yu t trn khng ph hp, th phng th nghim cn thc
hin cc php th nh gi li phng php. Cc kt qu nh gi ny cn
phi tng ng vi cc kt qu thm nh ca phng php chun, nu khng
cn phi thm nh li ton b phng php.
1.3.Thm nh phng php khng tiu chun
i vi phng php khng tiu chun, vic thm nh phi tri qua nhiu bc
hn, bt u t qu trnh nghin cu kho st phng php, ti u ha phng
php n khi hon thin phng php. Thm nh phng php l mt yu cu
bt buc phi thc hin i km vi vic php trin phng php mi v p dng
cc phng php khng tiu chun vo thc hin thnh thng quy. Cc bc
tin hnh thm nh bao gm:
1. Xy dng SOP d kin ( thoe cc ti liu tham kho hoc theo cc nghin
cu xy dng phng php mi)
2. Xy dng cng thm nh bao gm:
a. Xc nh thi gian v ngi thc hin
b. Cht cn phn tch: tn cht, d on hm lng trong mu
c. Xc nh i tng thm nh: nn mu
d. Xc nh mc ch cn phi t: yu cu v gii hn cho php, cn t
LOD, LOQ, chnh xc
e. Xc nh cc thng s cn thm nh v khong chp nhn
f. Xc nh cc th nghim cn thc hin
3. Kim tra cc iu kin cn cho cng vic n nh
a. Cc yu cu v trang b
b. Ha cht, thuc th
c. Mu th nghim
4. Thc hin thm nh
a. Cc php th thm nh s b
b. Thay i cc thng s ca phng php
c. Thc hin thm nh ton din
5. Hon thin SOP ca phng php
6. Bo co thm nh: cn c cc thng tin sau
a. Tn ngi thm nh, thi gian thm nh
b. Tm tt phng php: nguyn l, thit b, ha cht, quy trnh
c. Cc kt qu thm nh
d. Cc yu cu p ng a phng php vo thc hin thng
xuyn: kim tra tnh tng thch ca h thng mu, mu QC, c
lng khng m bo o ca kt qu
e. Xc nh cc thng s v thi gian cn thm nh li
1.4. Thm nh li
Cng vic thm nh khng ch thc hin mt ln khi pht trin phng php ban
u m cn thc hin trong sut qu trnh p dng. V a s cc iu kin thc hin
phng php c s thay i trong sut qu trnh p dng. V d nh c s thay i
Trong v d trn, vi nng di 100 ppm kt lun dng tnh khng cn chc
chn 100%, gii hn pht hin trong trng hp ny l 100 ppm.
3.2 LOD ca phng php nh lng
C nhiu cch xc nh LOD khc nhau ty thuc vo phng php p dng l
phng php cng c hay khng cng c. Cc cch tip cn c th chp nhn c
bao gm:
Da trn lch chun
Cch 1: Lm trn mu trng ( mu trng c thnh phn nh mu th nhng khng
c cht phn tch)
Phn tch mu 10 ln song song tnh lch chun. lch chun ny phi khc 0
Tnh LOD:
Trong
Cch 2: Lm trn mu th: Lm 10 ln song song. Nn chn mu th c nng
thp( v d trong khong 5 n 7 ln LOD c lng.)
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Da trn ng chun
Cch tnh tng t nh trong phn LOD nhng theo cng thc sau:
LOQ= (10xSD)/a
Lu : ngoi vic tnh ton nh trn cn quan tm n lp li ti LOQ, ty
theo mi phng php, gi tr RSD % cn phi t c theo mt mc yu cu
no . Xem thm phn chm v yu cu RSD % cho tng nng d c th
2.6.Tnh c hiu/Tnh chn lc
Tnh c hiu:
L kh nng pht hin c cht phn tch khi c mt cc tp cht khc nh
cc tin cht, cc cht chuyn ha, cc cht tng t, tp cht C th trong
php phn tch nh tnh l phi chng minh c kt qu l dng tnh khi
c mt cht phn tch, m tnh khi khng c mt n, ng thi kt qu phi l
m tn khi c mt cc cht khc c cu trc gn ging cht phn tch. Trong
php phn tch nh lng, l kh nng xc nh chnh xc cht phn tch trong
mu khi b nh hng ca tt c cc yu t khc, nhm hng n kt qu
chnh xc.
Tnh c hiu thng lin qun n vic xc nh ch mt cht phn tch
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Tnh chn lc: L khi nim rng hn tnh c hiu, lin quan n vic phn
tch mt s hoc nhiu cht chung mt quy trnh. Nu cht cn xc nh phn
bit r vi cc cht khc th phng php phn tch c tnh chn lc
Nh vy, tnh chn lc c th bao trm c tnh c hiu. Do cc phng php
phn tch thng c nhiu cht cng xut hin nn khi nim tnh chn lc
thng mang tnh khi qut hn
xc nh tnh c hiu/chn lc ca phng php nh tnh, nh lng cn
b tr cc th nghim sau:
Phn tch cc mu trng, lp li ti thiu 6 ln i vi tng loi nn mu. Mu
trng phi khng c cho tn hiu phn tch.Nu mu trng c hn 10%
dng tnh hoc xut hin tn hiu th cn phi thay i phng php loi
tr cc nh hng.
Phn tch mu th hoc mu trng thm chun hm lng cn LOQ, lp li
ti thiu 6 ln. So snh kt qu vi mu trng, phi cho tn hiu cht cn phn
tch.
S dng phng php thm chun sau chun b mu, cch ny thng p dng
i vi phng php sc k. Sau khi chun b mu v phn tch mu trn thit
b sc k thu c cc pic sc k, ta thm chun vo mu chit xut v phn
tch mu ny. So snh sc k ca hai mu nh gi c hiu/chn lc.
Phn tch mu khng c cht phn tch nhng c cht cu trc tng t cht
phn tch. Phi cho kt qu m tnh ( i vi phng php nh tnh) v khng
c nh hng n kt qu nh lng ca cht phn tch( i vi phng
php nh lng)
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