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TRNG I HC TI NGUYN V MI TRNG H NI KHOA MI TRNG
PHM VN HI
N TT NGHIP XC NHN GI TR S DNG CA PHNG PHP XC NH TNG HM LNG ST TRONG NC
BNG PHNG PHP TRC QUANG TI PHNG TH NGHIM MI TRNG, TRNG I HC TI
NGUYN V MI TRNG H NI
H NI, 2014
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TRNG I HC TI NGUYN V MI TRNG H NI KHOA MI TRNG
PHM VN HI
N TT NGHIP XC NHN GI TR S DNG CA PHNG PHP XC NH TNG HM LNG ST TRONG NC
BNG PHNG PHP TRC QUANG TI PHNG TH NGHIM MI TRNG, TRNG I HC TI
NGUYN V MI TRNG H NI
Ngnh: Cng ngh K thut Mi trng M ngnh: 52510406
NGI HNG DN: ThS. Trnh Th Thy
H NI, 2014
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LI CM N Sau gn 2 thng lm n cng vi s lm vic n lc ca bn thn,
n tt nghip ca ti hon thnh ng thi hn, vi tn ti : Xc nhn gi tr s dng ca phng php xc nh tng hm lng st trong nc bng phng php trc quang ti phng th nghim Mi Trng, Trng i Hc Ti Nguyn V Mi Trng H Ni.
hon thnh kha lun tt nghip ny, li u tin ti xin by t lng bit n chn thnh v su sc nht ti ngi hng dn l: Thc s Trnh Th Thy cng tc ti Trng i Hc Ti Nguyn Mi Trng H Ni tn tnh hng dn ti trong sut qu trnh nghin cu v thc hin ti.
Ti cng xin chn thnh ti ban lnh o nh trng, cc phng ban v c bit l thy, c trong phng th nghim Mi Trng to mi iu kin thun li v gip ti hon thnh kha lun tt nghip ny.
Ti xin gi li cm n n cc thy c gio trong khoa Mi Trng Trng i Hc Ti Nguyn Mi Trng H Ni trang b cho ti nhng kin thc v kinh nghim qu gi trong qu trnh hc tp ti trng.
Mc d c nhiu c gng, nhng do thi gian c hn, trnh v k nng ca bn thn cn nhiu hn ch nn chc chn ti tt nghip ny ca ti khng trnh khi nhng thiu st. Rt mong c s ng gp, ch bo, b sung thm ca thy c v cc bn.
Ti xin chn thnh cm n! H Ni, Ngy 09 thng 06 nm 2014
Sinh vin
Phm Vn Hi
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MC LC
M U ....................................................................................................... 1
CHNG 1: TNG QUAN .......................................................................... 3 1.1. Tng quan v xc nhn gi tr s dng ca phng php......................... 3
1.1.1. Khi nim v xc nhn gi tr s dng. ................................................. 3
1.1.2. Quy trnh xc nhn gi tr s dng ca phng php ............................ 3 1.1.3. Khi nim cc thng s cn xc nh .................................................... 5
1.2. Tng quan v tiu chun ISO/IEC 17025:2005 ........................................ 7
1.2.1. Gii thiu v tiu chun ISO/IEC 17025:2005 ...................................... 7
1.2.2. Cu trc ca tiu chun ISO/IEC 17025:2005 ...................................... 8
1.2.3. Mc ch ca tiu chun ISO/IEC 17025:2005 ..................................... 8
1.3. Tng quan v st ..................................................................................... 9
1.3.1. Tng quan v st trong nc ................................................................. 9
1.3.2. nh hng ca st. ............................................................................. 10
1.4. Cc phng php xc nh st ............................................................... 11
1.4.1 Xc nh st bng xphng php trc quang dung thuc th 1-10phenaltrolin theo TCVN 6177-1996 ......................................................... 11
1.4.2. Xc nh st bng phng php ph hp th nguyn t. ..................... 11
CHNG 2: THC NGHIM ................................................................... 12
2.1. i tng nghin cu ............................................................................ 12
2.2. Phng php nghin cu ....................................................................... 12
2.3. Ly mu v x l mu ........................................................................... 12 2.4. Tin hnh xc nhn gi tr s dng ........................................................ 13
2.4.1. La chn phng php (bc 1) ......................................................... 13
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2.4.2. Cc thng s ca phng php cn xc nhn (bc 2). ....................... 17 2.4.3. K hoch xc nhn gi tr s dng (bc 3). ....................................... 17 2.4.4. Thc hin cc php th xc nhn cc gi tr ca phng php (bc 4). ................................................................................................................. 18 CHNG 3: KT QU .............................................................................. 22 3.1. Kt qu xc nh khong tuyn tnhv xy dng ng chun. ............. 22
3.2. Kt qu kho st th tch dung dch K2S2O8 nh hng ti kh nng x l mu trong qu trnh th nghim xc nh nng tng hm lng st. ......... 23
3.3. Xc nh LOD, LOQ. ............................................................................ 24 3.4. lp li ............................................................................................... 25
3.5. thu hi. ............................................................................................. 27
3.5.1. i vi mu nc thi v nc mt .................................................... 27
3.5.2. i vi mu nc ngm. .................................................................... 28
KT LUN, KIN NGH ............................................................................ 29
TI LIU THAM KHO ............................................................................ 30
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DANH MC CC CH VIT TT
AOAC KB
IEC
XNGTSD LOD LOQ PTN
QA QC RSD SD TCVN VILAS WTO
Hip hi cng ng phn tch Chu u khng m bo o y Ban K Thut in Quc T (International Electrotechnical Commission ) Xc nhn gi tr s dng Gii hn pht hin ( Limit of Detection) Gii hn nh lng (Limit of Quantity) Phng th nghim Bo m cht lng
Kim sot cht lng lch chun tng i
lch chun
Tiu chun Vit Nam
H thng cng nhn phng th nghim, hiu chun T chc thng mi th gii
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DANH MC CC BNG
Bng 1.1. Cc thng s cn xc nh khi tin hnh XNGTSD ...................... 4
Bng 2.1. nh gi iu kin c bn ca phng php trc quang .............. 16
Bng 2.2. K hoch XNGTSD ca phng php xc nh st ...................... 18
Bng 3.1. Kt qu o Abs xc nh khong tuyn tnh. ................................ 22
Bng 3.2. Kt qu kho st nh hng ca th tch K2S2O8 .......................... 23
Bng 3.3. Kt qu xc nh LOD, LOQ ca phng php. ........................... 24 Bng 3.4. Kt qu xc nh lp li ca phng php. .............................. 25
Bng 3.5. lp ti a chp nhn ti cc nng khc nhau theo AOAC ... 26
Bng 3.6. thu hi i vi mu nc mt v nc thi nng 0.2 mg/l27
Bng 3.7. thu hi i vi mu nc ngm nng 0.15 mg/l, 0.3 mg/l, 0.6 mg/l ........................................................................................................ 28
DANH MC HNH
Hnh 3.1. th biu din mi quan h gia Abs v C. ................................ 23
Hnh 3.2. Kt qu xc nh khong tuyn tnh. ............................................. 23
Hnh 3.3. S bin thin nng Fe khi thm cht chun khc nhau ............. 26
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1
M U
pht trin v kin ton h thng quan trc v phn tch mi trng
cho vic pht hin, nh gi nhim, gim st cht lng mi trng phc v cng tc ging dy v nghin cu khoa hc, hin nay phng th nghim Mi Trng, Trng i hc Ti Nguyn V Mi Trng H Ni ang tin hnh xy dng h thng PTN t chun ISO/IEC 17025:2005, xc nhn nng lc ca PTN, m bo kt qu th nghim/o lng t kt qu ng tin cy nht, c gi tr v mt k thut.
Xc nhn gi tr s dng ca phng php l mt trong nhng yu cu v mt k thut trong tiu chun ISO/IEC 17025: 2005, cung cp bng chng khch quan rng cc yu cu xc nh cho vic la chn v s dng phng php th c p ng.
Nhiu quyt nh quan trng da vo kt qu phn tch. Trong khi , mi php o u c sai s, xc nh cc gi tr sai s ny rt phc tp, i hi nhiu n lc, sng to, v c trc gic. V vy, kt qu phn tch hon
thnh vi gi tr tin cy cao th phng php phn tch phi m bo. Xc nh gi tr ca phng php l mt phn khng th thiu nu mun c kt qu phn tch ng tin cy.
V vy, ti chn ti Xc nhn gi tr s dng ca phng php xc nh tng hm lng st trong nc bng phng php trc quang ti Phng th nghim Mi trng, Trng i hc Ti nguyn v Mi trng H Ni.
Mc tiu nghin cu ca ti
Xc nhn gi tr s dng ca quy trnh phn tch chn theo TCVN 6177: 1996.
Ni dung nghin cu:
- Nghin cu ti liu ISO 17025:2005.
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2
- Nghin cu kho st cc iu kin ca PTN phc v cho phng php th.
- Lp k hoch xc nhn gi tr s dng ca phng php bao gm: xc nh thi gian, ngi thc hin, ch tiu th, mu cn phn tch...
- Xc nh gi tr s dng ca quy trnh phn tch chn bng phng php tiu chun:
+ Xc nh khong tuyn.
+ Xc nh lp vi quy trnh phn tch chn.
+ Xc nh gii hn pht hin (LOD) v gii hn nh lng (LOQ).
+ Xc nh thu hi.