Meg, VAN PHONG CONG NHAN CHAT LUQNG Bureau of Accreditation (BoA) HE THONG CONG NHAN PHONG THE NGHTEM VIET NAM Vietnam Laboratory of Accreditation Scheme (VILAS) HUONG DAN CAC Vi DY UGC LUQNG DQ KHONG DAM BAO DO. TRONG PHAN TICH HOA HOC DINH LUQNG Ma sé: AGL 19 Lan ban hanh: Ngay ban hanh: 04 Bign soan Xem xét Phé duygt Ho tn ‘Hoang Thank Dune | VieXudn Thiy | T8.H6 Tit Thing Kg ten THEO DOI SUA DOI TAI LIEU TT Vis NOi dung siza di Neay sita diHludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg Liimé diu: Huéng din my duge xiy dug dua trén nguyén tie cia cée ti ligu sa 1, EURACHEM: Quantifying Uncertainty in Analytical Measurement, Laboratory of the Government chemist, London, UK, 1995. ISBN 0-948926-08-02. 2. Guide to the Expression of Uncertainty in Measurement, ISO, Geneva, Switzerland 1993, ISBN 92-67-10188-9. 3. Protocol for uncertainty evaluation from validation data, Valid Analytical Measurement, report number LGC/VAM/1998/088, January 2000, 4. 180 5725:86: Accuracy (trueness and precision) of measurement methods and results Part 16. 5. SAC-SINGLAS Technical Guide 2, A guide on measurement uncertainty in chemical analysis, First edition, April 2000 GIGI THIEU CHUNG Hiudng din may dua ra oée vf dy oy thé v8 we lung d> khGng dim bio cho fe chi tigu thi nnghigm, Trong hudng din sé dua ta cée vi dy ey thé cho cée chi tigu phan tich hod he dh lugng. Tit vf dy don gin dén vf dy uéc lugng d6 KDB cho ede chi tigu phan tich phite tap, niu bude tong qué tinh this nghigm. Mue dich cia hudng din A 48 hé tre, cung chp cho cée phong thir nghiém héa hge c6 mgt bite tranh tng quat vé céc bude ude higng d6 KDB cho efe chi tiéu oy thé va 6 thé 6p dung 48 uée lugng 45 KDB cho cée chi tigu oy thé cia PIN, [Noi dung hung din gbm 3 phan ehinh nh sa: [Use lugng d6 khdng dam bio think phin tir nhimg dit H, Uée lugng d6 khong dim bao cho mot s6 bude trong qua tinh phn tich HL, Ube lugng 46 khong dim bao cho mG s6 chi tiéu chit nghiém oy thé AGL Is Tin ban inh 10 Trang?2. Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg UEC LUQNG DO KDB THANH PHAN TY NHONG DU LIBU CO SAN (Qui dink Ky thuft o¥a nha sin xuét cung eép cho binh dinh mie 100mL efp A iat 0.08mL. Tinh d6 khdng dim bio chutin cia thé ti binh? Qui vé Phin bé dang hah i nhat - 46 khdng dim bao chuda la: 0.08//3 = 0.046 mL ‘Qui dinh ky thus eda aha sin xudt cho pipet 2m 1A O,0ImL. Tinh 45 khéng dim bio ich chét long chuyén qua pipet? (Qui wé Phin b dang hinh chi nt - 46 khong dim bao chun li cchudin eta thi 0.01/V3 = 0.0058 mL (Ching chi higu chain cho cin 4 s6 cho bie d6 khdng dim bio do a 0,0004g véi mice 46 tin cy khdng (t hon 95%. Tinh d6 khéng dim bio chudn? phin bé chuén va d} KDB chuin bing d} KDB mé ring Mite tin e@y 95% nén qui chia 2 0,0004/2 = 0.0002 ¢ 16 tinh Khidt cia mot hop chit hof hye duge abit cung cdp dara fi (99.9 £ 0,1) % Xée dinh d khéng dam bao chudn eta d6 tinh khiét cua hop chit? (Qui vé Phin b dang hin chi nt 6 Khéng dim bo chun Bs O.1/V3 =0.058 % Mt qua cin higu chun duge chimg nha 1A 10.00000g # O.04mg véi mie tin céy it nbd 1a 959. Tinh d@ khong dim bao chudn cia qua can? Mite tin cy 959% nén qui v phin bé chun vA 46 KDB chun bing d} KDB mé rng chia 2 0.042 = 0.02 mg 'B6 Igoh chudn cia eée lan edn lap lai cua qua cAa 0,3g 10,0002. Tinh 6 khong dim bio chuén? 'B6 Iéch chudn chfak t khing dim bio chuén nén d KBB chuén I: 0.00021 g ing chi higu chuan cua pipet 25mL cap A 6 ghi dG khong dam bao 1a + 0.03mL. D> ning dim bio nay duge dya vio 46 kh6ng dm bio chudn nhin véi hg sé phi k=2, cho mgt mie d6 tin by xép xi 1 95%. Tinh &6 khong dm bio chuén eta thé tich chit Jong chuyén qua pipet? C6 hg sb phis k=2 nén qui vé phn bé ehudn va.d5 KDB chu 1a 0.032 = 0.015mL AGL Is Tin ban inh 10 Trang? 2GL Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg i khng dim bio cia thé ch dung djch (rong binh djnh mre 1B dung méi hi ca hod tan vio binh dinh mize 100m dén vach dinh mee, Tinh J Ikkéng dim chun eda thé tich ling trong binh dinb mie? Cho cde dit ligu sau: = K&t qué cia 10 tin thye hign (ean va) 46 vao Binh dinh mie edp A 100m 6 &6 lech bud 18 0.01732 = Qui dinh ky thugt cia nba sin xudt cho binh 1a + O.OBmL., Hg s6 nd cia thé tch eda dung méi hitu co hoa tan 1a 1x107°Ct = Sw khée nhaw gitta abigt 46 phng thir nghigm va nbigt d6 higu chuin bink diah mée duye ude lugng 1a £3°C voi mite tin efy 18 95%. Tinh, + BO khong dim bio chuén do sy kde nhau gita ubimng tin dong va edn chinh 1a do Ich chun: 0.017321. + Tir qui dinh ky thufe cia nha sin xudt qui v8 phan bé hinh chit abt va tin ra dO ‘ng dim bio chuda cia thé tich bin 1a +0.08//3 = 0.046mL + DG khng dim bio do sy khée nhaw gidta nhigt dS phdng thi nghigm va nhigt d6 higu chuan binh duge uée Iuong IA £Vx3x1x10"mL véi V 1a thé tich cia binh, 3 1A su bin thign nhige dG o6 thé Va 1x10" a hg s6-né thé tich eta dung dich chét hw ea, Vi 1g cia chit ling Iém how nhidu thé tch gid nd eta bink nén ehi quan, tim dén thé tich gidn nér cia dung dich, Sy kde nhau v8 thé tfc do dn hung higt 445 duge tinh (dya vio mite 45 tn ey 18 95%) a 100 x3x 1x 10° =0.3mL ‘Va duge chuyén thinh d6 lgch chudn bing ede chia cho h s6 phi k=2 ‘DG khéng dam bao do anh hudng cua nhigt 46 1a 0.3/2=0.1SmL Tong hop 3 thank phin dG kbOng dim bio ten sé duge dS khong dim bio cia thé ich dung djch tong binh dinh mite I (0.0179 +0.046" +0.150° =0.16 mL Dj khong dim bio cia thé ich chit ling chuyén qua pipet Mot pipet 2m. cp A due sit dung dé pha dung mdi hi co. Tinh dB khéng dim bio chutin thé teh cht long due ehuyén qua pipet? Cho ede dit ligu saw: = Cie thé ich we 10 Ldn lp lai vige chuy8n chdt 1éng tr pipet 2mL ep A 06 d6 ech chudn 18 0,0016mL. = Qui diah ky thugt oia nba sin x ‘mdi hu co [a 1x107°C* pipet + 0.01mL. Hg s6 né thé tich cia dung = Sw kine nhau gitanhigt 6 phong thir nghifm va nhigtd@ higu chudn binh dah mic duge use lugng la + 3°C voi mize tin cy 1A 95%. 8 Tin ban inh 10 TrangHludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg Tinh + BG khdng dim bio chun do vige dong lip lai dung mdi qua pipet chinh fa d9 Igch chun; 8.0016mL é dang + BO khdng dim bio do higu chun pipét ti nha sin xudt duuge qui theo phi think chit abit. Vay d khing dm bio do bigu chudn pipet la: 0.01/V3= 0.0058mL +B Khdng dim bio do sur Kinde nhau gita nbigt d6 phong thf nghigm va nhigt 46 higu chudn pipet ude lugng Ia Vx 3.x 1 x 10° mL. wéi V 1 thé tich cua pipet, 3 sw thay di nhigt &6 va 1x10 1 hg s6 pin na thé ch 1 1bng Ién hom thé tich gin ng cia pipet néa chi can tinh &6 gin né cia dung mi, Sy bidn ehign vé thé tich do anh hug eta nhigt d6 due tin a iia dung moi hi co. Vid 2x3x1x 10° =0.006 mL ‘Sau dé chuyén think d6 lech chudn bing eéch chia cho 2 nén 4 khdng dim bio do anh hhuéng cia nhi 60 0.00672 = 0.0030 mL. Téng hop 3 thank phn 49 khong dim bio tr s® cho d6 khong dm bao cia thé ich dlung mi chuyén qua pipet Ik 0.0016? +0.0058 +.0.0030 4, 0.0067 mt. 10, BO khong dim bio can Mét pluzong phép yéu clu cin mt chun ni b6 100mg trén cin 4 36, Tinh d@ khng dim bio chun ca vige cin? ~~ Chimg chi higu chuan cua cén e6 néu d} khong dim bao do 1A + 0.0004g vei muse tin cdy king dui 95% = Cn fp Iai qua en 100mg tn cn 4 s6 06 lech chudn 18 0.000041, Tinh + BG khdng dim bio ti vige higu chudn ca duge tinh todn te chime chi higu chudn, 6 khéng dim bio duge wich din 1A £0,0004g véi mic tin cy IA 95%. Bién 461 than dé léch chuén bing céch chia d§ khéng dim béo cho 2. D§ khong dim bio higu hud 0.0004/2= 0.0002g = 0.200mg + BG khong dim bio do sy bién thin cia ee Lan doe edn 18 d6 Ife chun cia efe phép can fp tai 0.000041 = 0.041mg + Téng hyp d6 khong dim bio «én sé cho d6 KhGng dim bio eta ki ngng vat ligu hs ue, = V0.2007 +0041? = 0208 me AGL Is Tin ban inh 10 Trang? 4Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg u. 1D) khong dim bio cia ndng 4 mot dung dich Ding dich chun n6i b9 duge chudn bi bing hod tan khodng 100mg vétligu (edn bing cin 4 s6) trong m6t dung méi hitu ca hoa tan va dB dy vio binh dink me ti vach 100mL . Tinh néng 46 cita dung dich theo mg/L. Tinh d6 khéng dim bio chudn va d6. khdng dim bio mé rng ota nag d6 dung dich ? Dari 100mg v9 gu duge fn. DS Kg dim bio chub ign quan ti vig ea my doge toh dy 10 ven ~ Dé tinh khiét vat ligu duge trich dn tir nha sin xudt 1A (9.9: 0.1)%. 9 ksi dim bio chudn eta thé wh et Lg tong bin dink mae 100m. duge Uh wong vdy.9 wen Tinh C&e ngudn khdng dim bio gop phin vio toan bg 45 khdng dim bio cia ning &6 dung dich } Vige can vie tigu dé chudn bi dung dieh; > Dp nh Ake ua va ig; } ThEuchcubi cdg eta dung dish Ce khdng dim bo ie quan hs Cén vat ligu (u,): 0.208mg. 1 unk ie ca wt hia) 0.1/5 = 0.00058% ‘Thé tich cudi cing: 0.16 mL Nag doi dng dich aC (g/L) dagen co cing thi au Come 1) = 2°? 1000 rong ds 'W. kh hagng eta ve ligu st dyng (mg) P: — d@ tinh sgch cita vét ligu sit dung (% d6 tinh sach chia 100) “Tab woh oud: cong cia dune dh nt) Ning 9 cia dog deh n: “22999? 5.1000 = 1004,0me / 100 Vi céch tinh ndng d chi gbm phép nin va chia, cdc think phan &6 khong dm bio dye tng hop nhs e4e 45 lich chudn tcong déi (relative standard deviations) h d6 king dim bio ting hop cia ng d6 dung dich chu 2-(5)+ st 208) SEY [EY gn, Vioos | *{-0999-) *{i00 | AGL Is Tin ban inh 10 TrangHludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg Gif tr ci d6 khdng dim bio chun céa ndng.d ching dich chun n6ib§ 18 2.65mg/L. § khdng dm bio mé rng la 8.38mg/L dug tinh toin bing céch six dung hé 36 phi ke2 Néng d6 cita dung dich e6 thé dirge cding bé trong béo céo [8: 1004 5 mg/L va ghi chi Lad khdng dim bdo duge tinh dya vao d6 khong dim bdo chudn nhan véi hg sé phi 2 va cho mgt mite 9 tn ey Ia xp xi 95% AGL Is Tin ban inh 10 Trang 6Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg I, USCLUQNG DO KDB CHO MOT S6 BUGC TRONG QUA TRINH PHAN TiCH 1. CAN LL Myc dich 1.1.1 Cin 500g Cu bing cfe phuong phip 1.12 Che béo fo kb hugng Webioh dyng + Cu,g 32,5829 Wrbink dung ¢ 32,0822 Wee, g 0.5007 Ch thich: We a KhBi ng 12. Xiée dink nguén khang dim béo cia phip phim tik 1.2.1 BB thi nguyén nhin va ké quafinh bung ox tinh khiét Khdi lugng WCu Kh6i lung m (bi) Higu chun Khdilkengm —_Higu chudn “D6 nhay 1.3 Dinh lcong cic dp khong dim bio than phin 1.3.1 Surtnk tinh kbidt cia kim logi ding Cée nha cung cdp dua ra thing béo vé 45 tinh khiét cia Cu trong chimg chi phn tch ki luong Cu 1a 99,99 320,01% ma king dé cp da d9 tin dy cia 06 ‘Viking ai dun ra gi6i npn tin efy cia tinh sach ny, chung ti dua ra 1 phép tinh vé d@ khng dim bao theo phin rc) a lang chit nhét nén d9 khing dim bao chudn w 0,0001 /-/3 = 000088 1.3.2 Qui tinh cin 1.3.21. Higu chun tuyén tin Higu chun bén ngodi cia cin duge sir dung dé tuyén bé ring sr khéc nba gita trong lagng thie én dia cin va s6 (ong higng) dye tren thaée chia dO trong khoing + 0,05img véi 6 tin cay 95%. AGL Is Tin ban inh 10 Trangs7Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg Véi sx phi bé binh thing, d5 tn ey 95% cho mgt hi s6 181,96, Bai vay d khong dam bao lign quan din dat nhu d6 Iéch chudn ta 0052 =0,025mg (Chi: d khong dim bio cia thank phan nay ting len gdp doi boi lien quan dé 2 Fin iin mt ln a rr hi thé kn Yoa Cu v1 Un 1 sa Bhi thém Ci 13.22. B9 lp lat Lap Iai 10 lan phép do cd bi va trong legng Gng sé e6 1 d6 Igch chudn cia cée sai kehéc git cde Hin cin 1a 0,06mg véi khodng trong lugng trong khodng tt 20mg dén 100mg Ching a tinh dB lp lai chi duy nhdt 1 lan boi v1 no dade tinh v2 se khde chi hau cia trong lurgng diea dén mot dé léch chudn etia edc lan cin khée nhaw 1323. D6 nhay 9 ahay cin cin o6 thé khdng duege quaa tim vi ahng trong lung khée nha duge do trén cing 1 ean pham vi rt hep 13.2.4. Tinh 9 khong dim bao chudn tng hop trong quy tinh c&n 14 1s u(mCu) = 2(0,025)’ +0,06" = 0,07mg Ting két céc gid tr] cita dg khng dim bio MB ti Gidtix | oG) uae £86 tinh khiét ctia kim logi Cu, P 0.9999 | 0000058 | 0.000058 We cia kim loai Cu (mg) 50,7 | 007 0.00014 Tink dp khang dim bao ting hop vad khong dim bio marrOng Bai vi dd khdng dam bao téng hyp u (WCu) / WCu = '0,000058 * + 0,00014 * = 0.00015 vay w (wCu) = 0.00015 . $00,7 = 0,07 BG khng dim bio mi rng véi hé s6 phi k =2 18 U(WCu) = 0.07 x2 = 0.14 'Bé kh6i hzgng dag 500-7mg béo efo d khong dim bao Li 500,7 + 0,14 mg véi hé sé phis k=2 [mite d6 tin cy xdp xi 95%] Ghi chit phan bd dé Rhing dim bio cia d6 tinh Rhiét cia ding 1a rdt nhé 06 thé hong inh dé, AGL Is Tin ban inh 10 Trang 8Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg 2. SW CHUAN B] THE TICH 21 Myc dich 2.1.1 Dé chudn bj mét axit dbng hod dung dich chudn nitrat Cu t dinh mite SOOmL 10.7mg Cu pha trong binh 2.1.2 Cie bude tén han 3) Cin S00mg Cu tinh Khiée ong ebe cain b) Dang SmL axit nitrit dge hoa tan Cu ©) Kh phan ding ngling vA Cu di hod tan hodn todn trong dung dich axit, Chuyén dung dich nly vao binh dink mde SOOmL. Thém nude edt én vech dinh mee. 22. Xée dink nguén khong dim bio 2.2.1 So dé nguyén nhan va dn budmg vow Higu chudn thé tich V Anh huong 7? 23° Xde dinh dp khong dim bio think phn 2.3.1 Swkhiag dim bio kk o bg 86 pha th 2 2.3.2 Higu chudn thé téch eta nha san xude Tuyén bé eda nha san xude I binh dinh mite SOOmL c6 sai s6 + 0,1SmL.é nhige a6 20°C. King 06 1 euyén bd vé d§ tn ody ndo, BBi viy cing ta cho ring c6 mt phn bé dang tam gide vi thé tch tht dao dng ga tim hom la khodng gid han xa. Do vay d6 khong dim bio trong higu chun 180,15/-V6 = 0,06mL. 1 yéu 06 hinh thanh dau tign khi cin S00,7mg + 0,14mg voi 2.3.3 Lap Iai cée phan tich thé tich Lap tai 10 tin d6 day va edn binh dinh mée SOOmL eho mot dd khong dim bdo chun duéi dang 49 Igeh chudn TA 0,04mL s6 nay duge ding dé tinh urye tgp két qua cubi ing Anh busing etia nhigt d6 Theo nha sia xudt, bink dink mée duge higu chudn & 208C, boi thé trong phdng th nghigm giéi hen thay d3i trong Khong °C. D§ Khdng dm bio sinh ra te dnb hug iy ¢6 thé duge tinh tr vige usc Iugng khoding nbigt d6 va hé s6 a’ 8 tich. Vid nes AGL Is Tin ban inh 10 Trang 9Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg cia chit ling Id hom dp ni thé tich binh dink mic nén d n6 cia chit long it duge coi trong, hé 88 ni cia nude 18 0,00021°C" 500mL x +4°C x 0, 00021°C' = +0,420mL Tinh d6 khéng dim béo chudn déi véi sy thay di nbigt 6 bing sit dung d5 phin bé theo dang chit nhat: 0,420/3 = 0,25mL. Ah 4G khong dim bio ehudn téng hop 2357 10 phép do thé tieh u (V) u(V) = ¥0,06 +004 +0,25 =0,26 24 Tim tit ede gid tr ctia nhiimg dp khing dim bao trong vige chutin bj thé tch MB ti ciawix [Ua Ux Trong layne Cu,mg | 500.7 007 00014 Thé teh V, mg 500 026 0.0005 25 Tink dp khéng dim bio ting hep va. mé ring ty néng dim bio tong hgp cia vige chudn bj 500,7mg Cu trong 500ml dung dich xem gf 6 khong dims io ia vig cn Wa dong thé teh i u(Cone)/Cone 00052 feovyw f+ vyiv¥F = yfo.078/ S007} + [0.267 500F Ciing nh ndng d6 eta dung djch Cu 14 500,7mg/SO0mL = 1001,4mg/L Uicaw) = 0000052 x1.001,4mg/L = 0,52me/L. D6 khéng dim bao mo rgng cita vige chudn bj 500,7 mg Cu trong 500ml dung dich hay ndng d5 1001.4 mg/L la 0.52 x2 = 1,04mgi/L véi 36 phi k=2 Bai thé, nding 49 cin dung dich Cu I 1001.41 Omg/L wi hi s6 phi k=2 26 Nhgn xét 2.6.1 Véi nhiing diéu tinh bay tén, phn b6 cha dp khdng dim bio khi cin nb hon ahitu so ‘véi vige chuan bj thé tich AGL Is Tin ban inh 10 Trang 10Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg 3. TINH TRONG LUNG PHAN TU CUA DUNG DICH 31 Myc dich DE chuin bj 1 mol hofe dung dich thudng, tong leeng phn tt eta dung dich edn biée va d9 king dim bdo trong dénh gid 6 khdi lugng pha ti. VD, ching ti yéu clu tinh 9 khng dim bio bing céch inh kh6i Iuyng phn tte KMnOs 4.2. Hi ding IUPAC vé kidi legng nguyen viva sye die thie dng vf TUPAC xfy dung m6t danh séch nhiing nguyén t8 véi khdi hong nguyén ti rigng ré va ‘46 khéng dam bao lién két trong bai Pure AppL.chem, vol 69,pp.2471-2473 (1997). Bang danh mye dy di cia tt c& ede nguyen 16 Vid Khong dim bio cia ebving e6 thé ‘am ehdy tong trang web sau: hxtpJhvaw chem mua uiviupac/ACWU 4.4 Tink khdi legng phan tr cita KMnO4 va df khong dim béo 3.3.1 Kh6i twgng nguyén tir va d6 khOng dim bio duge ligt ké (tk IUPAC) déi véi timg (thanh phn) nguyén t6 céu tgo cia KMnO,. Nguyén té | Khéi lngng nguyén tir | DG khong dim | DO khdng dim bio AW (0) bio u (e) chun u (N3 K 19,0983 0.0001 0,000058 Mn 54938049 0.000009 0,0000052 ° 15,9994 0.0003, 0.00017 diwoe sit dung tit bing TUPAC sau khi tink todn dé Khong dam bao trong diinh gid do su tao nén cée lién két bang phan bé dang chit nhat. 3.3.2 Khoi lugng phan te KMnOy I: NWKMn0, = 39,0983 + 54,938049 + 4x15,9994 = 158, 39 gamol {0,000058 +0,0000053 + (4x0,00017} 0007 g.mot 34 Sw phin b6 cia cée nguyén tb KMnO, li sy tip hop don gin nhing sy phin bé cia nguyen td don. Bai vay, d6 khong dim bio thng hyp duge tin 1a binh phuong cha ting binh phuzong eta phn bé cia tig nguyen tt AGL Is Tin ban inh 10 Trang? 11Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg Danh myc mét sé nguyén t6 thong thing Neguyén t6 | Khéitugng nguyén tir [ D9 KDB lién quan a 100794 0100007 c 12.0107 0.0008 N: 14.00674 0.00007 0; 15.9994 0.0003, F 189984032 ‘0.000005 Na 2.989770 0.000002, Mg 24,3050 0.0006 Al 26981538 0.000002, P 30973761 0.000002 s 0.006 ch 0.0009 K 0.0001 Ca 40.078 0.004 cr 51.9961 0.0006 Mn 594,938049 0.000009 Fe 55.845 0.002 Co 58.933200 0.000009 Ni 598.6934 0.0002 cu 63.546 0.003 Zo 65.39 0.02 as 7492160 0.00002 Br 79.904 0.001 Ag 107.8682 0.0002 ca 112411 0.008 Ti 118.710 0.007 Sb 121.760 0.001 I 126,90447 0.00003, Ba 137.327 0.007 Hg 20059 0.02 Pb 207.2 on AGL Is Tin ban inh 10 Trang? 12Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg 4. BUONG CONG HIEU CHUAN 41 Quan hi tuyén tinh ‘M6t phurong phép hode mOt dung cu phan tich thurdmg duge higu chudn bing khdo sét bing xu hung, y, dé dm abig gid aj cia x. Trong phin léa cée treémg hyp quan hg may 18 mbi quan bg euyén tinh v dy y= a+ bx vi ab da bike tht v6 due me dicing cong hig chu, Trong ering hep nly ndng d6 xobs bit tr phn tch 1 mu mA quan sit duge sit td Ibi yobs tr d6 of cong thire: xobs = (yobs -a)/b ‘Trong vii ruéng hop, phuong phép phan tich yéu cbu quan hé tuyén tinh di tO VD: =0, rong tung hop nay quan he tyén tink fa y=bx va xobs = yobs/b Phuong php thong thudng cia quan hg tuyn tinh da tr ting ep higu chun (x, yi) duge si dung phuong phép higu chun binh phuong tuyén tinh nbd nhdt (cing hhode khéng cing anh huéig, téc dong = 0) 42° Neuén khong dim béo C6 4 nguén khdng dim bio chia déng quan tim khi déah gié d6 Khong dim bio cia robs 4. Sy thay di ngiu nhién eda phép do y (gbm yiva yobs) , inh hung nglu nhién qui cho nhiing gié uj cia xi c. Hing sé khOng bide gta xi va yi 4. Gib dinh khong 66 gié wi twyén t6 Trong 4 nguén trén thi mbt agudn e6 ¥ ngha nhée fA (a). Phuong php dénh gid (a) con Iai S, S cd thé SPs E(yi-yeyl(o-2) thing qua 5 thay inh bing cing thie: Trong 6; yi: Ia s6 doe diém higu chuan thé i ye la sé duge tinh try = atbx n: 86 dim higu chun viru (nobsy}= Yar) véi var ()=S%* 43° Vide rong vf dy ny 6 3 chun si-dyng A higuehuin 6 tip rung, xi Thu age 9 5 as so 1197 200 4784 Y= a4 bx thch hop vi higu chudn tr a vb dage tinh nr sa AGL Is Tin ban inh 10 Trang 1Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg E xisyit =i b= Trong vi dy nay 125 5 25 1197 59850 2500 200 ‘| 4754 950800 | 40000 Tong. 255 | 6076 won27s | 42525 ‘Trung binh | 85 2025,333 ‘rong d6: E xiyie = ak 1011275 -3 x85 x 2025,333 b= = 23732 Exi- nx” 42525 -3 x 85" a= y- bx =2025,333 ~ 23,7321343 x 85 = 8,102 vind y= a+ bx= 8,102 + 23,732. ‘Trong vi dy ny cé thé tinh todin thu duge ye tr gid tej d& bigt cla x va bink phyong cia higu (y - ye)? x z 3 durge fn wd 3_ [as [72676259 310672 30 [1197 1194,7086 5.25056 200 [4754 [758.5288 0.27961 S? SE (yi- yoy'M(n-2) 10672 + 5,25036 + 0,27961)/(3 -2) = 8,63669 varix) = Sb 63669 23,7321343 = 0,0153346 uugxobs.y) = Yvar(x) = V0.015334¢=0,124 AGL Is Tin ban inh 10Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg 5 Sr 52 ONG DUNG CUA GC-MS SAC KY KHOIPHO Muc dich Vi dy dudi chi ra d§ khéng dim bio do tong ky khé khdi phd GC- MS (gas chromatographic - mass spectrometric) Thic ye ede bueée dink gid dp khong dim bio lién quan Burbc 1: Céc yeu ci kj thuge Hoos chit siz dung cho kj thugt GC-MS dé phan «ch néng d6 biphenyl tinh Khiét wong benzen, Chit chudn sie dung a2 tring (vd Oup/m, dng 6 (ug/mL) eda biphenyl trong benzen e6 thé duge tinh tos st dyng phuong Dhap higu chusin bai dim (Phurong phép Bracketing/dBng hang) Cspl = Aspl x Cso! (Asa - Ao) cbudin IA SOug/ml dung dich chuan vi dung dich Trong dé Aspl: Ving t Ioidphin tng cin GC-MS cho biphenyl & méu phan t ‘Asa : Ving tIbifphin ting cia GC-MS cho biphenyl eda chudn ‘Aoi Ving tr i/phan img cia GC-MS cho biphenyl & méu ting ‘Coo: Nong 46 biphenyl & dung dich chuan cé ndng 46 SOug/ml biphenyl Burée 2: Xéc dinh nguén khing dém bao D6 chyin Coo Tuyén tinh + Cspl 7 \ / Ao, Asyy Aspl/ ‘D6 chym Dé chum DG chy Bude 3: Xéc djnh dp khong dam bao ting hop Coe Dung dich chun duge chudn bj tr chit rin biphenyl, du tign can va sau 46 hoa tan va pha long trong benzen Véi cdc lin cin khéc nhaw tinh duge dB khong dim béo chudn i 0.000206g d6i vei 0.0528 biphenyl AGL Is Tin ban inh 10 TrangHludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg = BS tinh Khiét cia biphenyl duge nha cung cip tuyén b6 Ia én hon 99.0% . Do d6 se tinh khigt cia nguyén liga duge tinh toén Ia 99.59 vi d6 khng dim bao liga quan (100% -998)2.V3 = 0.289% = Chit rin byphenyl sau d6 due hod tan vA pha losing thinh 1,000mL vio binh dinh mig. Chi tit Ky thuft eta binh dinh mic 1L sir dung tuyén b6 cp chin xée 1a 1000.22 + 0.20mL. Trong truimg hop nay phin b6 inh eh mbit duge st dung nhc mt phn cia kiém tra vige kiém sodt chit lngng (QC) da chi raring trung tim phn 8 phi hop hom cée ving gin pham vi, BG khding dm bio chudn tr ching chi higu chun cd binh gém thuy tinh Ih 0.20/V6 =0,0816mL. Lip Ini viged8 va cin da chi ra duye db king dim bio chun la 0.15mL. ‘V8 anh hung cia nhigt 46 khde naw d5i vi kh hagng benzen sir dung && hod tan Va pha loding khng 6 die ligu cia hg 36 né cin benzen ching ta cho ring hg sb nd cia né fa gdp d6i nhur nude toi nhige dB thug (ma c6 hg s6 né fa 2,1x10“mL/C), ‘Tinh nghigm ching ta bige ring we huyng nay c6 thé day di, Nhige d6 phong dao A+ Bn Ma duge thiét lip tong sir khGng hod tan cba m@t ah chit e6 thé hod tan eta AB, 18 ee de diém bai sin phdm hod tan Ksp=[AN[B]" 19 tép trung [A] va [B] sit dung wong sin phim pha lodng phi thudng duge ign dat he ndng 46 phi tr gam, Céc gid rj Ksp cin mgt vai vit eit quan tong duge dua ra a bing dud AGL Is Tin ban inh 10 Trang? 19Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg (Cie sin phim c6 thé tan cia mt vai hop chit v5 co khng ho’ tan tai nbigt d6 (C) trong ngode () Hyp chat Ksp Tigp chit halogen ‘AgCl 1,56 x 10 Qs) Age 7.7 x10-" 5) Agl 1.5 x10" (25) Tgp chit hydro Fe (OH); 11 x10% (18) AL(OWs 11x10 (18) Zn (OW); 1.6 x 10 (18) Tgp chit sunphat CaSO. 2.45 x 10° (25) BaSO, 1.08 x10" Q5) PbSOs 1.5 x 10°18) Hop chit cacbon CaCOs 0.87 x 10* (28) MgCOs 26 x 10° (12) BaCOs 7.0 x 10° (16) 622 Vidul Bé tinh méi quan hé sai, nguyen nln do hod tan etia ph cia chit ké tha trong qué (cinh ria bing edch gan/chit 0.1g eda AgCl duge rita v6i 250m nude tg 25°C Gdiy— Ksp=[Agh[Ct]= 156 x 10" mol? Néu mt mol ciia AgCl hod tan trong mgt lit nude thi: [Ag] = [Cl] =a Ti d6 vige hod tan cia mt mol AgCl, mot mol ion Ag va m9t mol ion Cl duge sinh ra Thay thé vio sy didn dat cho Ksp ching ta o6: Ksp = a= 1.56 x 10" mofL? va do dé: a= 1,25 x 10° moL.L" Nong d6 cia AgCl p/. 1 dua rabdi cong thie nbin trong lugng gram cla AgCl 1.25 x 10 moLL" x 143.3g.mol" = 1.8 x 10° gL Boi viy chi 4.5 x 10 g ciia AgCl sé hod tan trong 250ml nude rita sit dung Soi sb dikem bs 45x107x 100 — = 045% 01 (Chi thich, Sai sd nay Khing nhé nén Khong thé bo qua duce. Sai sé nay pha dieoe higu Chink trong vige we hiomg dé khong dim bio 62.3 Vidy2 bbé tinh nguyén nha sai sb tong phn th trong lugng cia 0.1g AgCI bing ra che ke tia vi 250m dung dich HCLO.0IM Trong tring hop nay, [CT] = 0.01M bode 107mol.L’ AGL Is Tin ban inh 10 Trang 20Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg Khéng chi ¥ vige so sinh nding d6 ion Cl ma cé thé IA nguyéa nhin bai sy hoa tan AgCl, ching ta thu duge: [Ag] = Ksp (1Ct] = (1.56 x 10 1.56 x 10" mol.L: Twang duong véi 1,56 x 10 mol,L x 143,3g,mol" = 2.24 x 10 g/l. cho sytan ciia AgCl Bai viy 5.6 x 10° cla AgCI tan trong 250 ml eda axit str dung ‘mol’L*) 1x 10%mol.L" ‘Trong trading hop nay sai sé 1a 56x 10° x 100 % = 0.056% on Chi thich: Gi tr nay 06 thd khong tinh ding trong ci phan tich chinh xde. Hom niga 1nd 06 thé céin nhde trong thyc hign, inh v8 ne la Rhdng hoan toan dupe thir lip giika dung dich rita va chat két tia nén sai sé thye té la nho hom nhiéu so véi mét tinh todn. 63 Saisd trong chuin dé cht két tia 63.1 Sin phim tan duge cing duge sir dung dé tinh tosn wong chun a6 chét két tia ma diém can bing 66 thé duge chi ra béi si tao thin cia hod tan tre chit ké tia qua rie chudn &6 va rong su phe tap chun &6 ma me cht ké tia dupe hod tan fi 632 Vidu3 Trong chuiin 4 Mohr duag djch nitrat bge vao dung djch NaCI ma thém cromat kali AgCl két tita hon toan trong Khi chudn 46 nhug rt nhanh chéng ndng 46 Cl tit mot sid tr hign tg, dang clo ge ndu dé chi ra mae efn bing hose diém két thie, Téng ede ion Cl khng duge chun d6 tuong duong tsi ndng d9 ion bac & dang clo bys ‘Tang sy khng chia 46 nay 6 thé duge xée dint sin phém K(AgCr0.) = [Ag"][Cr0."] = 2 x10 mol Bing tinh nbng d@ ion wong dung dich va thay thé gid tr nay vo cOng tht ton, Néa ching ta cin nhc ting hyp ma ImL. cia Sse wiv dung dich clo kali duge thém vio 48 hoa 25mL cia 0.1M dung dich Clo va 0.1 nitrat bac, nbng 49 fon Clo Bi 0.05 1000 [cro] mol. = 5.15 x 10" moLL" 194.250 Khi ndng d6 ion Clo Khéng duge chun d9 Ia twong duong véi ndng 49 ion bye duge dua ra | 2x1 s [2a oc? 22x 10S ot Ae eT VSsa0 Ting clo khOng duge chudn d6 La AGL Is Tin ban inh 10 Trang: 21Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg 50 =x 2.x 10% mol = 10 mol 1000 Niu ing 4 cn 25 . xO.mol Vi thé sai sé kém theo Ii: 1000 C6 thé thy ce tinh tosn tn ong rutmg hyp my sai sb chun d6 phy thuge vio nbng 45 ciia chit ehi thi thém vio; ditu nay duye dim dat sy cén va chuyén vai t cia chit lim két tia, Néu cho qué ahitu clo vio dung dic bi dat duge diém két thc; mae kc néu nag d6 clo ti qua nh, thém nitrat bac thém vio dung dich vugt gus va bai vy mi miu clo bac s® kh6 duge dinh dang trede thdy hon, Vi thé sai s6 6 thé Lam ahd. di bi vige git ditu kign chun d6 (abu téng chit chi thj ndng 46 va dung teh eta dung deh.) gin nw gidng nhau qua sy tidy fin hod ea chudn 46 biing chuén 46 cia clorua nate tinh Khiée dé sir dung sau Khi chudn 46 trong xéc dinh miu. 64° Sai sé ciia phuong phap chiét 6.4.1 Trong mé inh phan tich hoé hoc ce phuong phép chiét 1 thuimg duge sic dung && phn chia cfc chit. Qui tée ctta ee phong phap 1a sy phiin bé m6t chit trong hai dung mdi, Thi tye thye hign bao gdm vige lic dung dich, chutng mot dung dich ma vige léc khdng hod tin duge mi chit 46 duge chiét dé dé hoa tan hom theo sx phiin chia ca hge eta hai gia doen 6.42 Trong phn tich hod he hitu co dung dich - sr chiée dung dich duye sir dung cho thi sian dis trong phin ch hos hge v8 cg, hep chit phe @p (think thosng miu) cia c&e kim logi khée nhau durge chigt trong dung mi phin oye thip. Sw phic tap cia mi 66 thé do duge ngay lip tée bai may do mu, Hoe dung mdi c6 thé due bay hoi sau khi chia, vA thinh phn chit duge dua tr Ini dung dich nude va xée dink duge didn chia 6.4.3 Khd nang tring hop khéc trong vach vi du thyc hign chiét lai vao dung dich nude cha it thinh phin Khe (thimg pH khée nha) te dung djehvhod tan khi sr chiét d& bude du két thc. Trong efe phan tch vét sg chit fh thumg bao gm quang ph hye hose tre quang shit va phitra nguyen tr 6.4.4 Nang 6 «4 a6) cenie trong dung djch gidm di bdi sr chide tr ndng d9 nguyén Co ti nbng VA C1=Co- DVB+VA Néu D 1 hg sé phin bé va VA, VB IA dung tich cia giai dogn A vA B sir dung tong chi. “Trong hoat d6ng chi ip theo ndng 46 cua chit duge chiétgidm so v6i néng d@ ban di 1a AGL Is Tin ban inh 10 Trang 22Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg VA 2 C2°Ca DVB+VA ‘va sau n Jan thye hign - VA a Ca “Co DVB +VA 645 Te 1g méilign quan nay duge tinh theo: a. Thé ch dung mai sir dung of thé dc én: b. Nhung chigt hodn toin sé dat duge bing trung binh cia chit lp li vi mdi nhé hon véi chiét mt lin wéi thé tich 16 c. Tuy ahién dai luong cl khing bao gid dat duge béi vay ching ta phi thod min wi sy ehigt oan coin the gig boda ton c6 4. Vai td quan tong duge vin binh bing gi tj cia dai lugng phn bé, D néu chu di lim, vige chit boan toda 6 thé dat duge véi sy chigs dam; tuy ahign hg sd may thip vige chit phi duge tap lai mt va dn 646 Vidu4 Khi chiét 0.20g iot tr 100mL eta dung dich nuée véi SOmL phin CCl, (D=85) phin cn Ig sau Ldn chidt du tiga 18 100 c"02 | - = 0.0046 » 85 x50+ 100 ‘va d5 King dim bio chudn gly ra bai sy chide khng hodn toda fin du tia ba 0.0046 x 100 el = 23% (métsai sé ding ké) 02 Sau ln ehiét thir hai edn lai I: 100 2 © “02 00001057 g 85x 50+ 100 vA gly ra dé khOng dim bio Li 0.0001057 x 100 2 008 % (khong duge tinh dén) 02 Do dé khi thye hign chiét CCI 1a da dé chidt hodn toan iot tir dung dich nuée, AGL Is Tin ban inh 10 Trang?Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg 7. CHUAN B] CHUAN HIEU CHUAN i thigu: VF dy nay thio Tusa vé vige chuda bj moe dung dich chudn cho ehigt bi quang phb ap phy nguyén tir (AAS), tir kim logi c6 46 tinh khiét cao (trong vi dy nay 1: 000me/L Ca pha trong HINOs), Da vi dy my khong dai dign cho mgt phép phan tich nbung vige st dung hud higu chudn 1A mge phn eva héw h&t fe phép phin ch vi phép phin ich thdng thang 18 c&e phép do ma c6 lién quan tdi e&e chudn dé cung cp vie lién két chudn t6ih§ don vi SI Bucbec 1: Yeu cia kj thugt “Mue tigu cita bude 1 1a viétra tuyén bé 18 ring IA dai ugng mio duge do. Yéu cd ky thugt & cchudn bj chuén vi dy nay 1a m6 6 vi chudn va phép toda thé hign méilién quan eta dat Iugng do va céc thong s6 ma dai lugng do phy thude, Qui trinhitha tye ‘Chuan bj chudn higu chudn bao gm cée bude sau ‘Chui bj chudn eadmi (Cd) Lam sych bé mje kim ogi —i An kim loa q Hoa tan va pha loing (Cc bude tién hah + BE mat cia kim logi 6 tinh khiecao duge xi If véi hin hyp axit dé logi bo eée oxit ‘kim logi, Phuong phép Lam sach duge ahi cung ep kim logi dua ra va cn dé 6 thé thu dg kim log tinh Khigtnbur da cding b6 trong ching chi = Binh dinh mite (100mL) durge cfin theo 2 céch Ia khéng ¢6 kim logi tinh khiét va c6 kim loai tinh khiét bén trong. Cin sir dung o6 d6 phn gai 0.01mg Imi axitnitrie (HNO) (65%nvim) vA SmL made 4X khi ion duge thém vio Binh dinh mute dé hod tan Ca (twong duong 100mg, duge cin chinh xéc). Sau dé binh dink mie duge dd day nud da kn ion da vach dinh mite va te binh 4€ tra db nt 30 fn, Tinh ron Bai luyng do tong vi dy nay [8 nding d& cia dung dich higu chudn va phy thuge vio KhSi lugng 4 tinh khiét ctia kim logi e6 d6 tinh Khiét cao (Cd), Dung tich cia dung dich duge pha Toing. Nang d6 cia dung dich duge d hign theo cng thice AGL Is Tin ban inh 10 Trang 24Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg Cogn 000 ng Vv Trong d Cog: nding d6 cia chudn higu chun mg/L} 1000; ahéng s6 chuyén ddi tt (mL) sang [L] P 46 tinh khiét cia ciia kim loai V dung sch eva dung djeh chudn higu chun fm] Bucée 2: Xéc dinh cic nquén d KBB trong phan tich ia bute thi 2 1 ligt Ké tt cf fe ngudn gay rad KBB cia wimg thong sb md dah tri cha dai hegng do. 16 tinh khigt cba kim logi (Ca) dye nha cung cép dia ra tong chimg chi 1a 99.99 + 0.01 6. do &6 P 1a 0.9999 4 0.0001. Cac gid tr phu thuGe vio higu qué cia vie Lam sach b mt kim lopi tinh khit.‘Theo thi tue eta nha cung cfp thi khOng c6 4 KBB trong vige nhiém bé m§t kim logi do cée oxit kim logi va do 46 kh6ng c6 49 KDB nio urge ghi trong trong chimg chi. Tuy nhin 6 thé kiém tea lp Ini va théy ring phn b6 4 KDB trong phn nay o6 thé b6 qua Giai doan th hai cia vige chndn bj bao gdm vige ean kim logit khist. Khéi hrong cia Cd duge xée dinh bing vige ein cé bi thu duge m= 0.100285 Tai ligu cin nha cung cdp xée dinh la o6 3 ngudn KDB trong vige cin cd bi: d6 lp las Xi ning doe (46 phin gi s6/ digital resolution) cn cin vA phn bé d KDB trong chi ning higu chudn céa cin, V8 chic ning higu chuén o6 2 nguén KDB duge xée inh 1a d9 ohay va tinh euyén tinh, DG nhdy e6 thé duge bé qua vi ede khéi hung khiée hau duge can trén cing mét cin trong khoding hep. Thé tich (V) Thé tich cita dung dich chiza trong binh dinh mic cé 3 nguén gay ra 46 KDB: ~ D6 KDB eta ching chi cua binh djnh mie + Phuong sai cia cfc Lin cin vi dinh mic t6i vach = Binh vA dung dich tong bink trong mbt did chudn binh vA dung tch Cfo anh hueng khie duge thé hign trong so d3 xuong cf dud dy: ave ahigt d} Khie voi nhigt 46 higu AGL Is Tin ban inh 10 Trang 35Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg Vv ‘DG tinh khiét (P) Nit ag Higu chuds 6 Hip lai PF (Ca) 6 phin giai \popnin mibi) (tng) Tuyén tinh Tuyéa tink 6 nhiy —»/B6 lap lai / BS Ih Iai 6 nhiy Higu chun Higu chuda Burée 3: Bink lcpng cdc thank phin dp KDB ‘Trong bude 3 1 dinh Ivong eée nguda gay ra d KDB cho dai lung do, si dung efe ét qua thy nghigm hoge ti eée phan tich tos hoe dé wée lung i tinh khiét 'B6 tinh khide cia Cd tong ching ebi ciia CA TA 0.9999g £ 0.0001g, Vi kong 06 them moe thdag tin nao khée v8 d KDB nén gid thiét 8 phan b6 hink chi nhgt. BE e6 duge d} KBB ‘u(P) fi chia 0.0001 cho V3 0.0001 9.000058 3 Khéi booms m 1G KBB lién quan véi khéi ung cia Cd duge ude kugng sr dung di igu ti ching chi hig chun cin va Khuyén o4o oi nh sin xuit v8 vige ude lugng &6 KDB I 0.05mg. Vige ude lugng may Ite 3 ngudn KDB di duge néu trong bude 2 Thé tich V CCindn bj thé tch 06 3 nguda anh hung chin higu chudn,d§ tp fi va nbige 86. ~ Higu ehudn: nh& sin xudt cung edp sé ligu eho binh dinh mée 1 100mL + 0.1mL tai digu kign 20°C, Gia td} KDB duge cung cép khdng e6 mic 46 tin cy hode théng tin vé phn 8, do d6 dy don pin bé theo hinh tam giée va dj KBB duge tinh theo cng thc: O.lmt v6 O4mL. = BS lip ln: 4 KBB qua wie hug thyc nghiém tr vige cin va dé ddy 10 Lin téi 100mL cho d6 Igch chun fa 0.02mi. va duge sir dung tue tifpthinh d§ KDB chuén - Nhigt d6: theo nha cung cap binh dinh mée thi binh duge higu chudn & 20°C do nhigt 46 & PIN dao dng trong khoing + 4°C, Dé KDB do anh hudng ny c6 thé duge tinh tir khoang AGL Is Tin ban inh 10 Trang 26Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg thé toh thay di £ (100 x 4.x 2.1 x 10%) == 0,084 mL Gia thie phn bd hinh chit nh nén 46 KBB chudn la: 0.084mL. B = 0.05mL, Ba phin bé d6 KDB tén duye ting hop thinh d} KDB Burke 4: Tinh ton d9 KDB ng hop (Céng thie tinh CCd Sit dng cde gid tj thu duge thé hign trong bing «én tinh due nng d cda chun higu chun CCA ah sau: 100% 100.28 x0.9999 Cos 100.00) = 1002.7mg /L Neudn do KDB, gié tr va gid tr 4} KDB ign quan va 4} KDB twong déi duge thé hign qua bang sau Gidtix | _u® wey 1G tinh Kh 0.9999 | 0.000058 [0.000058 Khoi lugng cia kim logi m 100.28 0.05 mg | 0.0005 Dung tich efia bink dink mie V (mt) [100.00 [0.07 mi. [0.0007 ya vio cing thie tinh d6 KDB cag hop véi tncing hop cding thie tinh dai rong do 1 phép hin va chia ta thu duge 4} KDB tng hgp: +(#2) (82) = Yo1ooa0se" + 00005" + 0.0007" = ooo09 cms J ‘cs X0,0009 = 1002. 7mg/L x 0.0009 = 0.9 mg/L. 9 KDB md rng U(cea) duge tinh bing céch nhin d6 KBB téng hop véi hg s6 phi k= 2: U(Cca) = 2 x 0.9mg/L = 18 mg/L (Qua phan tinh 9 KDB ting hop ching ta nh§n thay 4} KDB chudn do anh hudng cia vige cchudn bj dung tich 6 binh dinh mic IA lén nbét sau dé dén anh hung do cén kim logi. anh hung do ds tinh Khigt cia kim logi g8y ra 8 KDB rit nhé, khong dng Ke AGL Is Tin ban inh 10 Trang 27Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg + Vie tinh tof 45 KDB ting hop c6 thé duge tinh theo cich sir dung bang tinh di a A B c D E i P m v 2 Gui 0.9999 100.00 | BO KDB 0.000058 0.07 4 sp 09999 onsgo8 [0.9999 0.9999 6 [m 100.28 100.28 100.33 100.28 7_\v 100.00 100.00 100.00 100.07 [s_| 9 [aca vo02.69972 | 1002.75788 | 1003.19966 _ | 1001,99852 10_[wyai) 0.05816 [0.49995 07014 11 [uyacyxiy’ [0.74529 0.00338 0.24995 0.49196 12 13 [wee [os Chi thich; Cée gid tej cba cée tham 86 duge dién tr C2 dén E2. BG KDB tuung img duge ign vao dong dudi ti C3 - F3, Copy cée gid tr we C2 — 2 vio oGt thir 2 BS — tioh nbng 46 C(Ca) tinh duge tit fe gid tej trén va dua ra wong B9. C5 chi gid tj cia Pw C2 Ong thém 4 KDB 6 C3. Kée qu tinh C C7 thé hign wong C9 CGD VAE dé tinh CCA) cing theo eéch tn, Cée gid te chi ra 8 ddng 10 (C10 ~ E10) tah biing eich léy e4e git tt dng (C9 — E9) tri di gié tj & B9. Dang 11 (C11 E11) I eée gis tr eda dng 10 (C10 ~ E10) duge binh phong lén va tng eée gid ti may duye thé hign wong B11. C13 dua ra gid trj 46 KDB chuan tong hgp tinh bang céc ét qua Ca) sir dung efe gid wi tir lay can ca BIL AGL Is Tin ban inh 10 Trang 28Tiung dln che vi dy use heyog d§ KDB do trong phin ich hos bye din heyog IIL UGC LUQNG BQ KBB CHO MOT SO CHI TIEU THU NGHIEM Cy THE 1, CHUAN DQ AXIT/ BAZO: XAC DIN AXIT CLOHIDRIC (HCL) 1 Phuong php. + Xée dinh dung dich NaOH 0,1 M bing chuén d6 uén co sé dung dich KHP 0,1 M (potassium hydrogen phthalate); + Sau 46 xéc dinh ndng d6 ciia 0,1M HCI bing chudn 46 trén co sé dung dich 0,1M NaOH. 12 Thit tue. (ONG DQ CUA DUNG DICH Cin Sg KHP Hoa tan KHP trong nude va dinh mic ti 250 ml thé tich e 3: Tin ton ndng d§ phn tir gam ciia KHP Ho’ tan 2 g NaOH hat trong nude va dinh mite ti $00 ml thé tich ‘Bua 25 mil dung dich NaOH vio 1 binb tam gide ‘Chuan &9 dung dich NaOH bing KHP tie mgt Burette 50 ml ‘Tinks toan nding d@ cia dung dich NaOH. ‘Bua 25 ml dung dich NaOH vio binh tam gide + Bude 9: Chuan d§ dung dich NaOH da duge chuin hos bing dung dich HCI tir mot Burette 50 ml = Bude 10: Tinh todn ndng dé eila dung dich HCI 1.3 Sordi nguyén nhin va kés qué dé xéc dink ning dj dung dich NaOH 6 tinh khiét (KHP) i lung (KHP) ~\ — — Thé tich (KHP) ‘Trong lugng phan ti (MW - KHP) ing di (NaOH) 14. inh gid cdc thinh phn dp khong dim bao Bue 1: Cin KHP Cong vige Hop dung +KHP [33,5895 @ Hop ring 28,5130 8 Khdi hugng KHP 5,0765 g AGL Is Tin ban inh 10 Trang 29Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg Che ngudn khdng dim bdo Tg HP) Vitucnadn Higcchuln Qnty 6 lap ta De ys tinh 6 nhay 8 nh khist (HP) 96 TR (89 tyéhn tin Kuang (th = 0) Ko 8 aera rnb _ enema ie 2) Kit hop wi vigehigu chudn cin duge sir dung. Giy chimg nhs higu chudn chi ra ring tai d5 tin cdy 95%, mbt lin cin dat dege bing (aon) sy khée nhau trong cing m6t pham vi IA + 0,1 mg ciia gid tri duge hién thi, Thanh phin d® khdng dim bo dé c6 thé duge biéu dién akar 6 Igch chuin bing céch chia 0.1/2 ta 66 0005 mg ) BS lgch chmdn cia nhing in cin Kp Ii (1-50 g) theo béo céo QA eta PIN chi ra gt d9 léch chun 0,09 mg ‘Nhiing d6 khdng dm bao phéi hgp Khi cn u (Wk) u (Wk) = (0,05 +009") = + 0,103 mg ‘Bude 2: Chun bi dung dich KPH chuén (Cong vige; Hoa tan § g KPH va diah mie t6i 250 ml wong binh din mée Cae ngudn d§ king dim bio ame eae aR, hast pe osinin Can (bi) - 7 oust) sesame AGL Is Tin ban inh 10 Trang 30Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg &._D§ khéng dim bio ea thé ich déi véi binh dinh mie duge sie dung: Catalog eta nbd sin xuit nding binh dinh mée 250 ml cé 46 khéng dim bio + 0,15 ml khong dB cép {6i dG tin ey, Do 46, mgt phn bé hinh cht nhit eta sai s6 duge ehdp nha véi 3. DG Igch chudn eda dung tich khi dé 1a 0,15/V3 = 0,087 mL. b. DG Khéng dim bio do wong vige dinh mize dén thé tol thiée KE: DG Tgeh chun d6i wi hing thé tch khée nhau cba binh din mie duge tah tosn sau mét logteée tin din mite Ip Tei (10 lin) va cn nude én vach dinh mize duge dua ra 10,014 mL. Gist 46 S€ duge sir dng trong lin tinh tos cudi cing vé d6 khong dim bio do trong phép do thé ch, ©. Sykbée nhaw gita nhigt dG dung dich va nbigt 6 higu chuén cia binh diab mec Coi hw chi hg s6 gin nd thé tich tia dung dich bdi vi né TA con sé dng ké Ion hon dung tch gin né cia bink dink mie thu tinh, cho mye dich thye hign Ly hg sé gitn nd di véi nude 12.1 * 10% wea mpedp C va ndu syrkbse hau ve nhige 46 gia dung dich va nhigt 46 higu chudn 1S d.. Dbi wi dung tich 250 ml duge sit dng s8 da a mgt khodng tin ey 95% et 250x5x 2.1.x 10% mL= 0.263 Do dé sy khdc nhau dé Igch chuan cha nhiét 46 1a: 0263/2 =0.132 ml op cia thé tch chun KHP u (VI BG khéng dim bao do phi w(vy = {0087 +0014 40,132" Buée 3: Tinh toén nbng d6 phn ut gam KHP ng d9 ca dung dich KHP, Mk duge tinh todn theo cBng thc: Mk= (Wkx Px 1000)/(Viex MW) Cong vige: N ‘Trong ds Wk: Khbi eng iia KHP duge sie ung (5,0765 g) P: DG tinh khiét ciia KHP (99,8 + 0,2%) Vii Thé tich cia dung dich duge din mac (250 mL) MW: Khii legng phan tr eda KHP theo cding thie CHOXK Bé sung cho dp khing dim bio cia Wk va Vieduge kigm tra sém hom, 06 hai d@ khong dim bio duge xe dinh, a. DO khéng dim bio déi véi dé tinh khiét cia KAP D6 tinh khiét cia KHP do nha cung cap dua ra 18 99.8% + 2%, 6 nghia P 1a 0.998 + 0.002. Khi d6 d6 tin c@y da khong duge cOng bé cho d6 khOng dim béo, Chiing ta phai diva ra mtphin b6 hinh cht nh vé sai s6 dig vit V3, vata 6. u(P)=0,002/ ¥! b. DO khGng dim bio cia khdi lugng phin ti KHP AGL Is Tin ban inh 10 Trang 3)Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg Cg thc phin cin KHP 1 CoHSO.K . Xeo bing tong lcong nguyén rca efenguyén 15, C,H, 0, K bao gm ofe ude hrymg d6 King dim bio duge ban hinh bai TUPAC tap ch Hoa ge tinh khigt ving dung, 9 66 Neuyént® | Khdilugngnguyéa te | DSKDB | D9 KDB chun c 12011 =o001 [000058 it 1.00794 = 000007 [000008 0 159994 = 00003 [0.00017 K 39.0988 00001 [0.000058 ‘Chi $; Ce d9 khong dim bio chun duge tinh bing eéch chia d6 Khong dim béo cho VF Su tép hop d khong dam bio cia mdi nguyén t6 déi véi khéi lugng phan tir cua KHP duge tinh bing cfch ting cutmg timg d6 khong dim bdo chun bing 36 Iugng c4e nguyén te cia bi nguyén 66 trong cOng thie phan Wi, va két qua duge lip bang nw dudi day: 84 nguyén tir | Trong lung dugc | Két quaduge | Dé KDB duce wong céng thie | tink tofn ‘ah tap hop G 8x 12011 96.088 (0.0046 Hs Sx 1.00794 5.0397 0.00020 04 4x 15.9994 0.00068 K 1 x39.0983 39.0983 0.000058 204.2236 Do &6 kh6i lagng phan tr cia KHP Ia 204,2236 va d6 khong dim bio téng hop cia w(MW) Ta cin bie 2 cia tng binh phuong cia cbc ving dim boring bet, Vi di u(MW) = ¥(0,0046" +0,0002" +0,00068" +0,000058") = 0,0047 ‘Tit ca nhiing tp hop do kh6ng dim bao do, ching ta o6 thé tm tat chting nhu duéi diy: Nhint8 KDB | Gidtriduge st | B§ KDB | D6 Igch chuan lién dung, V quan Wk 50765 g 00104 [2.05 * 10% P 0.998 0.0012 1,202 * 10 Ver 250 ml 0.16 64 * 107 MW 204.2236 (0.0087 23105 Do 46 6 khong dim bio chudn eta néng 46 (Mk) trong dung dich chudn KHP duge biéu din nb sa: u(Mky/ Mk = (0,0000205" + 0,001202* + 0,00064" + 0,000025") = 0,0014 mot I? Néng d6 dung dich KHP, Mk, duge tinh theo efing thie (1) nhur sau: ‘Mk = (5,0765 * 0,998 * 1000) / (250 * 204,236) = 0,0992 mol L” AGL Is Tin ban inh 10 Trang 32Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg Do dé ta ¢6-d6 kinong dim bdo chun u (Mk) trong dung dich KHP 1. (MK) = 0,0014 *0,0992 = 0,00014 Tr d6 a 6 nding 49 dung dich KHP 10.0992 mol 1 wi dd Khdng dim bao chun 0,00014 mol L”. Bde 4: Chun bj dung dich NaOH Dung dich NaOH da duye chun bj duge chuén hoé bing phn tich hos tc tgp biti dung dich chuén KHP, d6 king dim bio lin quan Gi vige chun bi dung dich NaOH khing duge uu ¥ mic dit d6 tinh khiét cia dung dich NaOH va thé tich dung dich da duge chun bj c6 43 khong dim bio, Buéc §: Cho 25 ml dung dich NaOH (bing Pipet) vio binh dinh mice Nhu trong bude 2, cfc phn dui diy duge hau ki chuyéa 25 mL. NaOH dé chudn d6 a, DO Khdng dim bio trong thé tich dinh mie pipet duge st dung Nha sin xuét pipet tyén bé ring pipet dugc st: dung o6 d5 khng dim bio £0.03 ml. Gin ng vdi pin b6 hinh chit nh bai vt d9 tn cy khong duge bid, dO Tech ehudn cba thé tfeh pipet duge tinh 1A 0,03/ V3 hog 0,017 mL. b. Dé khdng dim bao trong dinh mic pipet dén 25 mL (Che phép do can Ip li cia thé ich 25 ml. vi pipet d6 dua ra mgt 46 Igeh chun 0,001 mi, dhuage sit yng trye tip wong vige tinh tofn cubi cdng cia dp khong dim bio chun, ©. 9 khdng dim bio trong thay dBi thé tich do tée dng cia mhig 46 (Nhigt d6 cua phép phn tich Vs nhigt d6 higu chudi Udy sr thay di nhigt 6 6 thE cn 5 "C va hi s6 gid né thé toh ea thu tin 182.1 x 104, do 46 v6i d6 tin edy eta phép phn tich thé tich 18.9596 tht nba v6 nbige &6 1 25 x5 x2,1 x 10% = 0,0263 mL in cia piped) “Tied6, d6 Igch chun di wise thay di nhigt dS 8 0,0263/2 = +0,013mL. Ph6i hop tét cd 3 ngudn khong dim bio trén, ching ta €6 dp Khng dim bio u (Vs) trong vige chuyén déi dung dich NaOH nhw cin be 2 ting binh phuong 3 43 chuan tén, ¢6 ket qua sau u(Vs) = ((0.017" +0,001° +0,013°) oo21 Bue 6: Chun d dung dich NaOH trén ca so dung dich KHP chun (Va) 25 dung dich NaOH duge chudn d6 trén co sd dung dich chudn KHP tr mge burette $0 mL. Mit ki, ching ta cin Kru ede ngudn khdng dim bio tr quan diém cia cfc 3 yéu 16 wrong ducong di dye thio fuga & tr a, BQ khdng dim bio trong thé tich duge céng bio cila Buretter Ih 50 mL. AGL Is Tin ban inh 10 Trang 33Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg Nba sin xu cing bS ring buret duge sit dung e6 dB khéng dim bio £0.05 mL. Gin ding vi phn b hin chit nt bai vi d6 tin cay khong duge bid, 6 lech chun thé ich cin pipet dug tinh 18 0,05/¥% = 0,029 mi b. B) khong dm bio tong thé tch dung dich chun KHP duge sr dung dé chan d Khi mong muén siedung khong 25 ml dung dich chudn tong vige chudn 49, vige ein va dye lap Tai eta thé tic 25 mi tt buret due Kiém tra va data mt dO ech chudn 0,012 mL. Ching ta pha sit dung con s6 nay nhur dp khong dm bio chun cia thé ich duge sr dung, c. BG khdng dm bao cla anh hudng ahigt d6 gitta nhigt dé chuan dé tai nhigt d6 phong VA nhigt d6 higu chudn eta buret Ly su thay ddi ahigt dp 06 thé 6 5 °C nha rude vag 86 gid x 10°C, Véi dé tin ody 95% eita phép do thé tich thi yéu 05 nit 49 lk ng thé tich eta thuy tinb Ia 2,1 25. x5x 21 x107 ml= 0.0263 mL Do d6,d6 léch chun d6i véi sy thay di nit dé 1a 0,0263/2 = 40.013 ml ‘Trong vige chuén d$ my, 25,20 ml dung dich KHP-duge dung 48 ste dyng trong vige dat duge diém cudi voi dung dich NaOH. Tir day, sit dung nhiing s6 da 06 duge d tén, DG khong 4m bio chun phi hop u (Va) due tinh tosin nh sa: (vay = (0.025 F0.012" 0.013) hoke 0.034 mt Bue 7: Tinh toin ning dp dung dich NaOH. co thie duge sir dung trong vige tinh toan ctia dung dich NaOH Ii Ms = (Mk x Va)/Vs_ Ms: Ning d6 dung dich NaOH Mk; Nong d6 dung dich KAP ebuin dude sir dng Vs: Thé ich dung dich NaOH duge chuin 46 ‘Lam § to’n b6 ning tép hop d6 khOng dim bio trong bué 3 dén buée 6, chting ta 06 thé tom tit chiing nhu dudi day: hint khong ] Gidwiduge sir | DO Khong dim | DO Iéch chudn’ dam bio dung, V bao ign quan, Mk (0.0992 mot" | 0.00014 141 x10 Vk 25.2 ml 0.034 135 x10" Va 25.0 ml 0.021 8,40 x 10% ‘DG khOng dim bao chudn trong ndng d6 dung dich NaOH (Ms) duge tinh nbur sau: (Ms Ms = (0.00141 + 0.00135" +0,00084 ) = 0,0021 mol L* AGL Is Tin ban inh 10 TrangHludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg Ning dein dung dich NaOH, Ms, duge in theo cOng thie (2) nh sa Ms= = 0.100 mol L"* 5.20 x 0.992)/ 25. Ti 46, dj khdng dm bio chuin u (Ms) tong nbng db dung dich NaOH Bi 1u (Ms) = 0.0021 x 0,1000 = 0.00021 mol L” Ly 25 ml dung dich NaOH dé chun d6 HCL (Vb) ch dung dich NaOH chuin duge sit dung cho chué 49, nhiing leu ¥ teomg ty 6 thé duge ap dung nhu trong bude 5, 25 ml dung dich voi dé khdng dam bao chudn 1.u (Vb) 40.021 ml Bude 9: Chain d} NaOH trén c@ dung dich HCL (Ve) Nh teong bude 6, dung dich HCL chudn &§ 25 ml NaOH er buret 50 ml, Do d6 d6 Khing y= 122.6528926x. Vi thé xx x y Tinh ye (y= ye)" 0 0 0 1 122652893 | 107.06265 2 245.305785 | 1068.9117 4 9061157 [541.2005 10 122652893 __|1192.2467 AGL Is Tin ban inh 10Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg Do dé, S$? = Lyi - yey'n-2) = (107.06263 + 1068,9117 + 45412005 +1192,2467)/ (5-2) = 2303.14 vvar(x)= S'/b? = 2303.14/122.65289267 = 0.1531 1531 =0.391 Kéequi 8 (Cm) = 0.391 mg/L. Vs Binh dung tich sic dung dé d6 diy dung dich cubi cing dén 25m. o6 ching chi gi tr 25.040 + 0.015 mi. tai 20°C thu duege tr ti ligu KY thu§t eta nha cung ep. Trong nghién etna niy phn bé dang hinh 0.01543 = 0.00866mL. nhgt duge Iya chon. Bai viy dO khOng dim bio higu chun 1h Binh thn tinh duge sie dung trong mi tncing ma nhiged@ thay déi 4.0% (mic d9 tin fy ‘9506, néu khdng néu mite 46 tin ey thi phan bé inh chi nt durge thira nln) He sb né cia heptan theo sy thay d6i nbigt a} [A KhOng duge biét dén, ci thita nha né Ihodng gip hai nh hg s6 ng cla nage 2.1x10% mLAC, Trong tradng hop ny he s6 nd cia heptan duge thia nhin IA 4.2x10* mLAC. Tit kinh nghigm cia ching ta ching ta biét ring sy thta nhgn [A wong e& 16m hon dé pham vi mhigt 49 cia PTI noi ma tién hanh phan teh, DO khdng dam bao theo sy thay di nhigt 46 cho mét dung tich 25.04mL Ia dat t6i diém lin nhat ctta 25.04x(4.0/2)x4.2x10" = 0.0210m1. Bai vay, u(V) = = 0.0227 Fla; nh vi dy truge trong Ingng phn ti (NW) cia axit linoleic (CisHs202) va dG khdng dim bo cia né duge tinh nbu sau: c H oO Gis ui 0107 [1.00794 15,9994, BEKDB [0.00046 | 0.00004 0.00017 c 12.0107 016 | 12.0107 12.0107, H 1.00794 1.00794 | 1.00798 1.00794 oO 15,9994 15.9994 | 15.9994 15.9957 Fla 280.4548 [280454 | 280.447 280.446 0.00832 [0.00128 (0.00035 zosik-05 [698-05 | 1.68.06 126-07 uF) [0.008421 AGL Is Tin ban inh 10 Trang 39Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg Fil: Tuong ty, NW ciia mehtyl linoleic (CiyHs40) va dG khdng dm bio li c H ° Gia wi 120107 [1.00794 | 15.9994 DEKDB [0.00046 [0.00004 | 0.00017 c i0107 [1201116 [12.0107 _| 12.0107 H 1.00794 [1.00794 [1.00798 | 1.00794 oO 159994 [159994 [15.9994 | 15.9957 Fmt 29447206 [294.481 [294.473 | 294.472 0.00878 [0.00136 | 0.00035 7902k-05 [776-05 [185-06 | 125-07 w(Fmi) [0.088895 Wopl: khdi rong cia mau fi 10,0232g véi abitu in ca khde nba. Béo ofo higu chun chi Fda neu chun dua ra 1a 0.4/J3 = 0.231mg cita rad Koh lon nhit 18 04mg ti ae 49 khéng am bao chun cho méi lan cn, Nhur can cia mau bao gdm ca trong lrng ca mau ‘va bao bi d6 khdng dim bdo tinh ti dg Igch duge nbn hai wQWspl) = (0.231 +0.231") 327 mg —> 0.000327g ‘Thu héi (R): theo cdc bude nghién ciru trude trén mét miu tuong ty thir thu hdi Hip di duge thy hign én me mu don va im chéy o6 trung binh thu hai 18 91.3% véi dO tech chun Ta 5.49%, Vi thé d6 Kc chudn lién quan Ii §.494/91.34% = 0.0591. Dei vi miu higm tn sy thu hdi 18 0.950 (95%), Vithé d6 khong dim béo chudn theo thu hdi IA 959%x0.0591 = 5.615%. DG chinh xée(r): trade, mot miu da duge thir lip lai, Qua dé ma nghién ciru tinh chink xéc ndng d axit linoleic di duge tim thy trung bink 1 S.65mg/g véi d6 Igeh chudn 1a 0.96mg/g, ‘Vi thé d9 khéng dim bio chuda lién quan Ia 0.96/5.65 = 0.170 24 Tinh ton dg khing dim bio tong ‘Che 46 khdng dim bao chudn theo Cml, V, Fla, R, Fml va Wspl duge téng hop dau tién boi phuong phap chia bang sau: AGL Is Tin ban inh 10 Trang 40Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg v Fa R Fini Wel Gis wi 25.04 | 280.4458 [90% | 294.47206 [10.0232 poKps [0391 [0.0227 [0008421 [561% [0.00889 [0.00033 mi [7as ws [7s [745 718 715 TAS Vv 25.04 25.04 [25.0627 | 25.04 2504 | 25.04 25.04 Fla__| 28044548 | 280.445 | 280.445 | 280.4539 [280.445 | 280.4548 [280.445 R 95.0% [eso% [950% [95.0% 10.61% [950% [95.0% Fmi__ [29447206 | 294.472 | 204.472 [29447206 [294.472 _[294.48005 [204.472 Wspt__[ 10.0232 [10.0232 [10.0232 | 100232 [100232 | 10.0232 _ [10.0235 Cop 906665 17.9229 |17.907203 [169082 | 17.906125 [17.9061 097923 | 0.01623 | 0.005376 |-0.9985 _|-0.000541_|-0.00058 1,9561078 [0.95889 [0.00026 |2.896-07 [099695 | 2.9228-07 [345-07 uiCspl) | 1.3986092 DG khong dm bio chudn tén thu duge [a ting hop ma tir 46 sy inh xe duge dua ra cho tng d9 king dim bio think phan. Sy chin xe thu duge tn la M6 Kgch chun lign quan, vi thé ‘u(Csply/Csp ‘u(Cspl) = 0.187xCsp! 187 x 17.9067 y{(1.3986/17.9067" +0.170- Vi thé, tng d6 khong dim bao thanh phiin 1 3.35mgig 0.87 DG khong dim bio mé rng U(Cspl) voi mite d9 tin edy 95% da thu duge tie dG khGng dim. bao ting hyp véi hg s6 phi ‘UCspl) ‘dng U6 ciia axit linoleic trong thitn Te 1796.7 mg/g Bio cfo d§ khong dim bao [a 49 khOng dim bio mé rng duge tinh bing efch sit dung phi k=2 véi mite d9 tin ey twomg duong 1A 95% 25 thgn xét inh gi ede thank phin quan tong ‘Theo qui lugt nhan Ién cia sai s6 sy thém vio va bét di lién quan, vi dy x 6.70me/g 4 + x2 d6 khOng am bao téng hyp 1 cin cia binh phwong ciia tong céc d6 khdng dim bao think phn. vi dy Tin ban inh 10 a AGL IsHludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg )}.-Vithé sy tp trang cia tig thinh phan t6i d6 khong dam bao tng ua) = helm) sue hop 06 the 30 sinh ay tfp gia u(x) va vim) ‘Tuy nhién tong trudng hyp Khi méi ign quan Id nhl vihoge chia. vf dy x= xu 6 KhOng dim bio chudn tg hop dug tinh uooix= Vd xP Hide /eF Bai véy trinh te dé so sinh phn bS cia moi thinh phan ti d6 Khong dm béo tng mée I d& so sinh mi ign quan cia &@ khdng dim béo chin cia cée thin pha vi dy: u6x)hxi Va U(K2)/K Bi vi vé dy thio Iuga trén méi lign quan [A nbn vA chia. Vi thé sy s0 séah phiin b6 méi think phan , mdi dhinh phn d6 khong dim bo phi duge thé hign mdi lign hé v6i dp Khong «tim chun Gis wi KBB chuin [KDB lién quan Cm 7.15mele, 0.391 mele 0.0547 v 25.041. (0.0227 mL. 0,009) Fla 280.44548z/mo!_| 0.00842 ymol | 0.00003 Fil 294.47206g/mol_|0.00889 g/mol | 0.00003 ‘Wspl 10.0232 (0.000327 g 0.00003, R 95.0 % 5.61% 0.0591 r 0.170 Cpl 17.90667me/g [3.35 mele 0.192 Ti bing tn 16 rang sy g6p phn chinh 18 te Ci, R va r, Thye t& mot e6 thé tinh bay 4 king dim bio tng hop chit ba ngudn bing eéch ly di khée ngudn nhs khéc. Trong tung bgp nay, w(Cml)(Cat = (0.0547 +0.059) D 3.37mplg, Vi vay 16 ring A 46 khong dm bio chi duge tinh wt efe ngubn ‘nga Khe nhau tr sy thu duge sau khi ea nie tt e8 e&e nguda, 0.188. Vi thé u(Cml) = 0.188x17:90667 = nh TA Khdng 66 AGL Is Tin ban inh 10 Trang 4Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg 3. XAC DINH HAM LUQNG AXITS TRONG DAU 3.1 Phuong php Use sé cia miu du duge hod tan trong sy trung hod TPA va chudn d6 dya vio chit chun 18 lung deh KOH 0.. moVL véi chit bi tj phenolphtbalein 42° Sordé nguyen nhan va két qué Cron W (abu) MW (KOH) Gis trj cia axit 4.3 Xd dinh cdc dp khing dim bio 3.3.1 Dung dich cbuin KOH 0.1M véi HCLO.SM A. Chuin bj HCIO.5M V8 plnuomg dign thong mai chun bj dung dich HCI chia 18.230 g HCL (mFICD duge sit dung dé chun bj Cst HCI 0.5M dung tch1000nL Binh diah mic sir dung dé chudn bi dung diel 6 dung teh Bs 1000mL # 0.4m. tei 20°C. BG Igeh chun thich hgp eda sy higu chuin dung th siz dyng phn b6 hinh chit bgt la 0.4/3 hoje 0.23mL “Tye nhigtd@ thye va nhigt 6 higu chudn binh djnh mek s6-né dung tich cin nude Ia 2.1 x 10°C, sr biéa di thé tich 06 thé 1000 x 3 x 2.1 x 10% bode 0.63mL. 'C v6i mite tin ey 95% hg 6 fh ehud wong ng I 0.63.96 bof 032m ‘Téng hop hai phan bé 46 khdng dm bio u(V), ching ta c6 yyy = (0.23" + 0.32*)7i000 =0.00039 Nong d9 cis HCL 1a mHCL/ MHCL. V noi MHCT 18 khdi leong phin te ba HCL in 0.02% cho °C. Lay mt sy Khe nhau o6 thé trong PTN cia aha sin xudt - 2°C (vei d6 tin ey 95%), d@ khdng dam bdo chuén cia m HCL li Nha sin xuét dung dich HCL chi dn mot d@ Igch €6 thé cita d6 eh ‘u(mHCL) = 18.230 x 0,02 x 2/ (100 x 1.96) = 0.004 g ‘u(mHCL)/m yc, = 0.00022 AGL Is Tin ban inh 10 Trang 3Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg 1p khong dim bio chuén cia trong lugng phan ti HCL, theo khbiIuong nguyen tr TUPAC va phin bé hinh chit ab, I ‘u(mHCL) = 0.000043, Cin hou ¥ ring WMHCLY MHCL 1a khing dng ké khi so. sinh vi u(V)V va u(mHCL)/ mHCL , 46 khéng dam bao chuan lién quan 1a; wcCso/ Cxt= yf 0.00045, B. Xécdjah CKOH NBng d@ chinh xe oia dung dich KOH duge thiét kip ade Khi si dung bi trén co si dung dich HCL chun Do 6, CKOH = Cst * Vst! VKOH. Noi, Vst 18 thé VKOH (ml) Niu di duge ti ch (ml) dung dich HCL chudn duge sit dung cho chun d6 thé tich dung dich KOH, h bay & trén, u(Cst)/ Cst= 0.00045 Déi voi vige chuyén dung dich KOH dén binh tam gic, m6t pipet thuy tinh dung tich 5 4001 ml duge st dng. Lay sr bin di nbigt dG 6 th IA. SOC wi dd tin cay 95%, va d6 lip Ipi ca pipet (46 Igch chudn) 0.0033 mL, né c6 thé tinh u(VKOH)/VKOH = 01s Vige chun &6 duge hon thinh si dyng me buret vi lagmg S mil e6 vach chia d6 0.01 ml (46 chinh x4c higu chun ciia nha sin xudt 1A + 0.01 ml) Sirsai Khe nbiGt dG o6 thé 8 tuong ty nh df néu tn, 6 Ifeh chun ct vi 0.0033 mL vad lech cl (0.017m1) 140.0098%n dong chi cubi cang tung duong vi of cia buret Vi thé gid tj lim mbit eta u(Vst/Vst = 0.013 néu CKOH = 0.1 moV/L va tuong ting Vst =I mL D6 khong dim bio u(Cst/Cst va U(VKOH)/VKOH 18 khong déng ké trong so sin (6 u(Vst)/Vst Vi viy u(CKOHYCKOH = u(Vst)Vst= 0.013, 33.2 Xée dink gid uj cia axit Gis tj ota ait AV= MKOHVKOHCKOH/ mn Luu § phuong phép thir sir dung vé khdi lugng phan t KOH 1A 56.1 thay thé hoan toan gid tr) MKOH = 56,1056; bai thé wong wumg bop aay ‘u(MKON)/MKOI = 0,00564/(56.1 x ¥3) = 0.00006 é chigt axit béo ty do bing dung dich KOH ching ta sir dung buret SmL néi trade uCVst)/Vst = u(CatyiCst = u(VstyVst = 0.013 AGL Is Tin ban inh 10 TrangHludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg § khong dim bio cia miu du ong hegng 2.5g 18 w(m)/m = 0.0023 ‘Thit 5 ring d} khéng dim bio cia tong lcong phn ti KOH vA ca méu dif khong ding iké, vi thé u(Av)/ Av= VlulVou)/Veoul+belCeon)/ Cou) = 0018 ‘DG khGng dim bio md rng voi he s6 phi k 218 U(AVVAV =2x 0.018 hode 0.04 Ghi chai: sé chi cita diém két thiic cua chudn d6 Ia nguén anh hudng khong dam bao Ion, Néu bret vay 0 1 0.85mi 49 King dm bio mG rong oth tng dén 0.07 Hon na mbu cia db va sy thay 481 06 hé rong chit chi thi chay ti gdn didm két tue trong dung dich di hod tan 1 King duge tinh ti, Tang ye mai ién quan tinh fume ia CO khdng khé wong Cro AGL Is Tin ban inh 10 TrangHludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg UGC LUQNG DO KpB TU DC LIGU PHE DUYET PHUONG PHAP. XAC BINH THUOC TRU SAU PHOSPHO HUU COTRONG BANH MY 4.1 Tom tit 4.11 Myc dich Xe dinh dvs lugng thude tris su phospho hitu co trong bénh my ding phwong php chiét va she ky khi (GC) 4.1.2 Qué trink do (Qua trinh xée dinh due Iugng thube writ hinh 4a phospho hi eg trong bah my dee thé Hinh 4.. Phan tich thudc trir sau phospho hiru co Dang alt Tach chide Lam sch 1 ‘Chuan bj chun Ch dic ‘higu chudn Xée dinh GC Higu chuin GC Két qua 4.1.3 gi hegng do Dir lugng thuée tri su phospho hiru co trong binh mj duge tinh theo cB tit su Laan p08 mpeg! Rec Tig 10 me ke Veg rae Trong d6: Poy am lugng thude et si 66 trong mu (mg ke") op: Cudmg d t6i da cua phn chide cba mu Cec: Nong d6 kb Irgng ota chit Voy: ThE tich cudi cing cia dich chide 10": chuyén we g.g" sang mg kg Jer: Curing 46 tdi da cita chdt chud in (jig) AGL Is Tin ban inh 10 Trang 46Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg Rec : phn tha hdd tha hi ‘Mnple | khdi Leong mau Fon: hé s6 higu chink cho méu khng dBag nit 4.1.4 Xéc dink cac nguén gay ra do khong dém bao do Che ngubn gc cia d6 khdng dim bio do e6 efe nguyén ahin due thé hign & inh 4b Minh 4.b Phan tich ngudn géc cita 49 khong dim bao do Nguchule tayén ay 0th 06) ‘ih toe op ao) A shi g) eu ctala 9 tp sigias —\ wot = Ptop) | xt icin a /) th ao ween ti ro ren ale 4.1.5 Dinh lucong céc thimh phan cia d khéng dim bao do Daa trén dt liga phé duyét phuong php thir ni bg, 06 3 yéu tb t90 nén d§ KBB do. Cie yéu 16 nay duge ligt ké trong bing 4.c va thé hign trén so dé 4.d (céc gid tri duge suy ra tir bing 4c) Bang 4.c : Dj khdng dim bio do trong phan tich thude trir stu 3 eKDB | 05) KDB chuin 5 Moticéengwin | Gitti | eee | eee hi hs , Dya trén 2 lin tht cia 2 6 lap lai 10 027 27 | Penn? be DG chgeh 09 0.083 0.048 | miu them ‘Cie agudn gbe Khe Binh gid wen co st (4 déng ahi.) io 02 02 | phuomg phip stt dung U(P apap - - 034 | KDB chudn wrong d6i AGL Is Tin ban inh 10 Trang 47Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg inh 4.4 D§ khong dim bao do trong phan tich thude trir sau uGy.xi) (mek) Déng nhit BG chéeh BG ip lai Poop) ° on 02 03 oa Cie gif tr ctia u(y, 5) = (8y/%x)).u(x) bby tr bing 4. 4.2 Hudng din chi tiét 42.1 Gisi thigu ‘Vi dy nay minh hga mt me phuomg php tish 4} KBB bing eéch sit dung cée dt liu phé dluyét pong phap thir ndi b}. Mye dich cla phép do Ia xdc dinh téng du lugng thude rit sau phospho hi co trong bin mj. Qui rink phé duyét va céc lign kit thiét lip aghién et thie nghigm bing céch tién hank trén cfc miu thém. Gia dinh d} KDB do sy khée nha trong két «qui dot sy thém va phan eh trong miu [nh so v6i db KBB do tong. 4.2.2 Bucbe 1. Bie diém kj thugt Die ume cits phép do ddi vei ce phuong phip phn ich duge mé ring sé wt hon néu duge in ta ede bute khde nau eta qué tin phin tich vi md ta edng thie todn hye tinh kt qua dont Qui trinh: Qua trinh do dage m6 ti trong so dB inh 4.2 Qué tinh my duge ebia thinh efe gini dosn 3) Bling nble: Mu duge chia thinh nhiing phn nh6 (khodng 2em), ty ng nbién 15 phin tong sé niy vi dég hoé ching, Név e6 phin nio d6 aghi ng khong duge dng hod té phi duge ly ti ude hi tin du ii) Cin ong hugng ota khbi mu ndy c6 Khbi lugng 1h mane ii) Chidt: lupng dich chit cia miu phan ich véi dung m6i htu co, dem gan va sy gua ct NaySOy vi ob dae dich chit bing céch siz dung thie bi Kuderna-Danish iv) Moa tong ¥)Axcton nitri/erane long, ria axeton nitril bing hexane, sly hexane qua cét natri sulphate vi) C6 dic dich rca bing ga véi ngon ka ahi cho dén khi dich chigt gin nhs kh hon toin ovis Tin ban inh 10 Trang 48Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg vii) Pha losing dén thé ic tu chun V5p(Khosing 2m) wong dag nghigm chia vych 10m viii) Do : Tiém Syl djch chide vA do GC dé c6 duge exmg d6 mii (Peak) Ip ix) Chudin bj dung dieh chudn Sp ant (ndng d6 ki lung Cr) x) Higu chudn GC sir dung Spl dung dich chudn, tiém va do GC dé 6 eutmg 46 mii etm Ip Hinh 4.2. Phan tich thude trirsdu phospho hitu co Ding nie —+ Téch chi Lim spch Ciné bi ebudn Bulkup higu chuén Xée dink GC Higu chun GC Tinh todn ki qua Nang 49 kh6i kugng Cy, cia miu cudi cing duge tinh nk sau gant" va dink gié Pp cia him hayng thude tsi trong miu c6 (mg.kg") dave tinh bat oVn 105 mek" Recmanyie we Hoe, thay Cy vio cing thi M106 pe Tg RECManyie ene Trong a6; yi Mite d§ thude isu trong mu (mgkg") Top: Curtmg 46 mii cia mau chiét Coe Ning d6 Kh legng cia miu chun (gn) AGL Is Tin ban inh 10 Trang a9Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg Vor: Thé tic oubi cng ota dich chit (rl) 10%: Bbi tie (g.g") ra (mg.kg") Ing: Cutimg.d pick eta mu chun Rec: Dé thu hd Amante: Ki tugng cba chia ( Pham vi Phuong php phin tich nly o6 kh nang ép dung cho ede thude tnt stu o6 ban chit hod ge ‘twong ty véi ning d6 tir 0.01 dén 2 mg.kg’' véi céc logi mau bénh my khée nhau, 42.3 Bucie 2: Xée dink cdc nguan dp KDB do ‘Xée dinh vA phfn tich cfc nguyén nhiin gly ra d khGng dim bio do [A mt qué winh phan ‘ich ting hop, e&ch tt nhét 18 phn tch theo so db nguyéa nhin va két qua. Cée thing sb trong biéu thite toan hye cua phép thir duge thé hign béi cée nhénh chinh wén so d6, Céc thong s6 méi duge thém vio so dB theo ting bude tong qué tin plhin tich (hinh 4.b) cho {dn Khi cde thing s6 duzge ligt Ké day di. Su khong dng abit cia miu khong pha mgt ehong sé trong cdng thie ton hye tinh ket ‘qué cha phép thir nhung né Iai inh hug ding ké dén gua tinh pha eh, Vi thé mot nbn hah mdi cho thong s6 F(bom), dai dign cho sy kiGng ding abit cia mu duge them vio wong so dé nguyéa nhin va két qua (hin 4.¢) inh de: So dé phan tich céc ngudn gic 49 KDB do trong trudng hyp miu khéng ding nhat cn aye (op) cay ton fi eo \ x Dochym Ps cee \ wet wo SW big etn me ruinng pica > Plop) ning) Bo chum Hy fz— mw culo p— v3 ey Finen) otal hy tackle aie AGL Is Tin ban inh 10 Trang 50Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg “Tém Iai so & thé hia oe nguyén niin da dén 46 khng dim bio doth sx khong dng ita mu da bao gm trong sy tinh toén cia phép th Dé chi ra ede kt qua cia d6 khng dm bao do mét céch 16 rang, tt nhat nén viét cing thite: Lay Vey P. ont Voy 10" me ke Reem, Tag RECM aie “Trong 46 F(hom) 18 mbt s6 higu chinh gi thigecho vi thing mbit trong phép tinh be, Didu 44 chi 0 ring d5 king dim bio do trong chinh pha dure bao gbm trong su dah sid &6 king dim bio do tng. Cong thie tén cing chi ta d6 king dim bio do s8 duge fp sé hi dung. Chi thick: Clic hg 6 higu chink: edi tidp em may kh a hd quat va e6 thé rdt 6 gid ri. VE ma nguyen I, mos phép thie dé phi c5 cdc hés6 hid chink thng nha, Vidu: Bg khing dim bio do Cup ce thd deg dtm det bing ds Khong din bite do chucin dé vi Cay hoie db Khing dim bit do chain ia dim cho King dim b 5 king di ito do Cyd dim dat i db ch i chudin tome i do trong cho had higu chink. Tromg tring hap sau, gid tr-xi din 42.4 Bube 3 : Bin ieong ede thank phin cia dp khong dim béo do BE dinh luyng cfc thinh phin khée nhau cia 4} KBB do tir di ligu nghiés thir ngibG va nghién ctu phé duyét phuong phép: = Sy ude Iegng tét ahdt ca phuong sai téng cba toan bG qué tinh phiin tich qua nhigu «qué tri thie nghigm (this nghigm lap lai, ti Kip) = Sy ude lugng tét nhit eta ting dé chéch (Rec)va d6 king dim do cba n6 - Sy dinh hrgng cia bat cit 46 khéng dim bio do nio lién quan dén két qua tinh tosn khong day di d8i véi todn b6 qui tin. phwong php IMG vai sy sip xép li cfe nguyén nhin vi bigu d3 higu qua rit e6 gif ti two thinh méi ign hg va dua ra nhiing thing tinr0 rang hon, (hinh 4.) ‘Hin 4.f: So’ dé nguyén nhan ya két qua sau khi phan bé Ii dé c6 céc dir ligu nghién cia bccn) én cpap Ath 0p) ta eo wor) ne) A 09) —\ mee ag) 6 smi 9) won Pop) ct sia sn an i hdc) tb teed) Femem) each AGL Is Tin ban inh 10 Trang STHludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg Chi thick: Thang thane mau die chay time 16 ma nh, mai 16 ma chay déu phi higu chudin tid bi, mau kiém tra thu hd dé kém sot 6 chéch va mu tip nein mhién dé kiém tra df chum. SE pha ‘th hign hank dng Ride ph néu trong tring hop cdc Wn tit nay 6 du hi cho ede ket qué lech nhau ding kd Kiém sost chat gmg co bin may dip img dave cée yeu cd chink ea vige dink gi dg KDB ti di ligu phé duyét phinomg phép. Vige chen them mot yéu t6 anh hudng “dp lap Iai” wong se dB cho ta cOng thie tinh Pup ne v. — Foog 10° Foes mg kg! ‘Ong thite * oT Reem, iu ds ehi ra d6 1p tai gidng nhs 86 dng nhdt. Céch sinh ton theo dang nay thug tign hon va duge trinh bay duéi day. Cie déoh gid eta cée inh hudng Khée nhau s€ duge cin nhc Nien ci d@ chum ‘Toda b@ phuong sai cia qué tinh phn ch qua nhitu Hin phan tich duge thys higa 461 véi ce mau thr dp (cong mgt mu dBng nhit, ich chide va qua tinh xe dint) di v6i du tugng thud trit siu phospho hitu co duzgc tim thiy trong céc miu bénh my khée nhau, Két qua duge ‘tinh bay trong bang 4.¢ Bang 4.g: K&t qui nghién citu thir nghigm lip thude trir stu DI D2 | Trung binb Di-Da Detwme | tmeds") | tmese") | tele) | 2? | ounetinn Malathion 1:30 130 [130 0.00) (0.000 Malathion 1:30 009 [110 0.40) 0364 Malathion 057 053 [055 0.04 0073 Malathion 016) 026 [021 “010 | 0476 Malathion 065; ose [062 007, oa Pirimiphos Methyl 0.04 004 [00s 0.00) 0.000 ‘Chlorpyrifos Methyl (0.08 009 [008s 0.01 018 Pirimiphos Methyl 0.02, 002 [002 0.00) 0.000 Chlorpyrifos Methyl 0.01 002 [ois oor | -0667 Périmiphos Methyl 0.02 oor [ois O01 0.667 ‘Chlorpyrifos Methyl 0.03 002 [0.025 001 0.400 ‘Chlorpyrifos Methyl 0.04 006 [005 “002 [0400 Pirimiphos Methyl 0.07 008 [075 “010 | 0133, ‘Chlorpyrifos Methyl 0.01 oor [0.10 0.00) 0.000 Pirimiphos Methyl 0.06) 003 [0.045 0.03) 0.667 AGL Is Tin ban inh 10 Trang 52Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg Ci aig tha dye Khe nha (kc 30 vi rang bink) cing cp mgt kkk qu cho phuang sa tng ci qué tinh tit nghigm lip la. DE da ras ude higng d@ KBB chun tzong déi cho ‘img thir nghigm don Ie, dQ Igeh chudn phai chia cho V2 dé thinh dS léch chuén cho 4 KDB chudn cho céc gié tri don. Tir 46 suy ra gid tri cia 46 KDB chudn tir phuong sai cia qué tinh thir nghigm gp Iai tuan theo toin b9 eée bude tong gud tinh phin tich nhumg logi tri: nh hudng ddng nhét 0.382/ ¥2 = 0.27. Cut thich: Bam dé 5 thé ede phép this dip miy king dia ra dis bde tw do, Nhumg né king od mu ick bs da ra ad home chink xc div dB crm cia guc tri phn ick Ad win mdr log thud tre su dic bigt tome mét log Bains mj Ac Bit mo i. Did quan trong hom tromg qui trink phn tick ‘pep thie La mghiém eu thie mghigm diye ten mhidu logi mau dit wd mite 6 nding do de Laome trome ima Aé cea ra se ea chon de din cia cde lol thuée trie sau phospha hu co: Cc thie higu qua hd la thie nghiém lap lai trin cc loai mdu bank Kée nhaw dé nghién cit bée tr do cho méi log ndu nghién ctw Nehign ci v3 dé chéch BG chch ola phuong phép phan tich duge nghién ete n6i bG trong phdng th nghigm bing fel nghién edu ese miu thém (dng nbét méu va chia miu thinh ede mau ohi va thém mot shim Iugng vio méi miu nbd) bing 4.h dua ra cfc két qua cia mt qué tinh nghiga ctu cée su thém trong mg tht gian di tren efe dang khde nba, ‘Bang 4h. Két qua nghién citu 49 thu hdi thudc trir sau cot | Rae [ek | [RE | ee ‘Dau thai PCB 10.0 8 84 9 Thite an gia sic tonghgp1| _OC 0325 100 90. 9 Diu thye vit vi dng vit oc. 033 M 102 2 DS wong oC. 0325 3 a 9 (1): 6 nghién cia thye nghigm (2): Trang binh va d9 Teh chudn miu svn % 46 thu hi AGL Is Tin ban inh 10 Trang 53Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg During suyén tinh duge suy ra khi lam thi nghigm tén cée mau binh my (uge inh déu bang miu ghi) di chi ra rang Hé sb thu hbi trang binh tir 42 miu La 90% vai 49 Ich chun (s) 18 28%. Dé KDB chudn duge tinh tir d6 Igch chudn cia trung binh Rec) = 0.28/42 = 0.0432 (Mt ¢nghia eta phep thi duge sir dng dB xée din cho h 36 tha hai trung binh ti so sinh sit kde ahau dng ke s0 v6i 1.0. Theo thirnghigm thing ké¢ duge tinh toda theo ong thie sa: 09) 0.0852 2318 Gil tj may dae so sinh vit gi te ti han 2, wi be tv do 9-1 wd tin Ay 18 95% bu t>=t tl Reo ft kde dang huang ket qua ding &8 ue Keong Rec) 31 Bterity = 2.021 ‘rong vi du niy, hg sé higu chinh (1/Rec) doe si dung via do viy 18 ring trong ofc k&t qua tinh toin Rec duge thé hign (wong d6.n 8 so véi 1 ngudn géc khéc cita dé khong dim bi Trong so 48 4.i chira ede ngudn g6c khée cia 49 khOng dim bio do bao gm cée ir ligu ve 446 chy (1), die tigu vé hg s6 thu hi (2) hoge ede ngudn gbe Khe (3) da duge kiém wa va tinh toan trong &9 khong dim bao do Tt eden va dung oy do thé thch quan trong ph dye kiém sot nghiém agit. 86 hymn 5 tha hi phi due tin da trong ayn bing cin vig hig chun cfe dung oy dng 4 do thé tch bai vi trong sudt qué trink thir nghifm déu phi dng cfe dung ow do thé tich pippet. Nghién cima cée phuong sai mé rong tong gin nia nim cho thiy c6 inh hung cia hig &6 moi teeing Ie Mort s6 ege ngun ding g6p khée vio d KDB 1 6 tinh Ki cia mau chun, sy khng tuySa tin ca thigt bi GC kh tr lt ht qua (dai dign bai vige higu cihudn cho cée thing 88 fay vig) va vige miu dng nbét cing 1a moe dhinh phan thém vio it qua, trong yéu cu eda vige nghién ecu, Hinh 4.i Danh gia cae ngudn gic khac cia d§ khéng dim bio do tect) ay eh Dp lpi) op) ryincen 60 SE veep) it) vos) —=\ hig 642) bee vw ev chin Plop) inom) 3) peony et nada AGL Is Tin ban inh 10 Trang 5Hludag din cée vi dy wie heyg 46 KDB do trong ph tich hod hoe diab heyg (1) Dé t4i Kip duge tinh dén trong qué trinh nghién ctu phuong sai cia thi tue phi tich (2) Dé tinh dén trong qué tinh nghién cizu dé chéch cia thi tye nghién ctu 2) BA due tinh dén rong sy dénh gid efe ngudn gée khfe cia d6 khGng dim bio do 'B6 tinh Khige cia chudn ma nba sin xuft cung ep IA 99.55% 4 0.069%, BO tinh Kniée cng 1A nde ngudn gbe eta 49 KDB do ¥5i di KDB do chudn 18 0,0006/ 3 = 0.00085 (phn b6 hin cli nh). Nhung gif tj ny qué nbé so véi nghign ctu d} KDB wi nghign ci d9 chym nén £6 thé D6 qua. 'B6 tuydn tinh cia két qua thude wt su photpho hu ea trong pham vi giét han ning d6 durge {hit lip tong sudt qué tink nghién eu, Hon niia véi efe chi sé trong bing 4.g va 4h o> ng tuyén tin cing d6ng g6p vio phn bé d6 chum. DO ding abit cia miu bénh my 1 nguyén nhin cubi cing gly ra dO Khong dim bio do. Khdng o6 di igu vé phn bé du lugng think phn hitu co trong eée sin phim bénh mj. (46 pt didu ngae nhign vi pha th d6i véi da s6 thye phim dBng nhlt higm hon déi vi eée amu khing dng nhdt), Bing thi thye té hing thy hign efc phép do trvc tgp 46 dBng nha. Boi viy, su dénh gié 46 khong dim bio do dya trén co si cia phurong phip lay méu, Mét sé phan bé dw lung thade tir siu d& duge céng bé va mét vai phép théng ké don gién da duge sir dung dé tinh toén 43 KDB do chudn cho todn thé n lién quan dén d khng dim bao do tigu chudn trong ein thude trt sit 66 tong mi cudi cing fa Dur lugng phiin bé phia trén cting bé mat chi c6: 0.58. Dur lugng phn bé phi déu én b& mgt chi 6: 0.20 Da lugng phan bé du trong miu nbumg bj gidm ndng d@ do bay hoi hoge bi phn bu ti 0.05 ~0.10 (phy thuge vad day hé ma phin tich va vige tinh tosin bbén trong len bi ‘Trumg hop (a) Bh dic bigt cung ep véi ty 1g iy miu hoge dng nhit hod todn :n6 58 xay ra trong tudng hyp thém chat phy gia fen b8 mit. Tradng hgp (b) béi viy duge coi nhu 12 traéng hop xiu nhét, Trung hop (c) duge xem nhs 6 kha ning abit nhumg khOng thé phan bigt dé dang véi (b), ten co st d6 gid tr 0.20 duge chon. 4.2.5, Butéc 4 : Tinh todn dj khing dam bao do ting hgp ‘Trong qué tinh nghién cia phuong php ngi b6 cua thao tée phan tich, dé ti Kip, 46 chgeh va tat cf cde ngudn goe khiée cita 46 khér nay duge ghi trong bang 4.c dim bio do da duge nghién eu kj lung. Cée gid tr Che gid tj ong déi duge két hop bei cong thie: (Pag) [Pap = (0.27° +008 = (Pop) = 0.34 Pry Bang tinh déi véi wrutmg hyp nly duge chi ra trong bang 4.k Ch y (0.373) d6i v6i kéc qui higu clin dan nga lA 1.1111, wed6 06 gid tr 03 Jing d6 KBB do tuy$t déi 3/111 = 0.34 AGL Is Tin ban inh 10 Trang 55