PHN III: MT S CH TIU CHT LNG CA DU M

1/ ACID BO T DO
nh ngha: y l phng php xc nh lng acid bo t do c trong mu Phm vi: c p dng cho tt c cc loi du th, tinh ch, du c v m ng vt Dng c, thit b 1/ Bnh ng mu; 115 hoc 230 ml hoc bnh tam gic 250ml Thuc th: 1/ Cn 95%: cn phi c xc nh c im cui vi phenolphthalein r rt. Phi trung ha vi kim n khi xut hin mu hng nht bn ngay trc khi s dng. 2/ Dung dch ch th Phenolphtalein 1% trong cn 95%. 3/ Dung dch NaOH c chun ha chnh xc, chi tit trong AOCS H12-25. Bng 1 cho bit lng NaOH thch hp ph thuc vo lng acid bo t do c trong mu. Tin trnh: 1/ Mu phi c trn u v c chuyn v dng lng trc khi cn, tuy nhin, khng c lm nng mu qu im nng chy 100C. Bng 1:gii hn acid bo t do , s lng cn v nng kim %FFA 0.00-0.2 0.2-1.0 1.0-3.0 30.0-50.0 50.0-100 KL mu (g) 56.4 0.2 28.2 0.2 7.05 0.05 7.05 0.05 3.525 0.001 Cn (ml) 50 50 75 100 100 Nng kim 0.1N 0.1N 0.25N 1N hoc 0.25 1N

2/ S dng bng 1 xc nh khi lng mu khc nhau gii hn cho cc acid bo t do. Cn mt lng mu xc nh cho vo bnh tam gic 3/ Cho mt lng cn nng trung ha v 2 ml ch th 4/ Chun vi dung dch chun NaOH , lc mnh n khi xut hin mu hng c cng mu nh lc trung ha cn trc khi cho vo mu. Mu hng phi bn 30 giy. Cch tnh: % acid bo t do trong tt c cc dng ca cht bo v du c qui v acid oleic. Mc d du da v du ht c thng c biu din nh acid lauric v du c c qui v acid palmitic V kim. N. 28.2 a/ Acid bo t do qui v oleic %= KL mu

V kim. N. 20 b/ Acid bo t do qui v lauric. %= KL mu V kim. N. 25.6 c/ Acid bo t do qui v palmitic. %= KL mu 2/ Acid bo t do thng c din t qui v ch s acid thay v ca % acid bo t do. Ch s acid c xc nh bng s mg KOH cn thit trung ha 1g mu. Chuyn % acid bo t do bng cch nhn ch s acid nhn % acid bo t do bng 1,99 S chnh xc: S liu chnh xc ca du tinh ch, ty mu, kh mi c th hin trong bng 2, s liu chnh xc cho du th c th hin trong bng 3. Bng 2: Mc trung bnh s khc nhau gia cc phng th nghim cho s xc nh cho cc acid bo trong du tinh ch, ty mu v kh mi Ch s FFA(%) SR RSD(CV.%) 2.8SR 0.01-0.05 0.007 33.93 0.02 0.05-0.1 0.010 12.73 0.03 0.1-1.0 0.04 9.90 0.13 1.0-2.0 0.073 4.75 0.20

Bng 3: Mc trung bnh s khc nhau gia cc phng th nghim cho s xc nh acid bo trong du th Ch s FFA(%) SR RSD(CV.%) 2.8SR Ch : 1/ isopropanol 99% c th c s dng nh dung mi thay th cho cn vi du th, du thc vt tinh ch. 2/ y np bnh v lc mnh trong vng mt pht nu kh CO2 vn cn ln trong du. Tham kho See.J.Assoc.off.Anal.Chem.59:658(1976) 0.1-1.0 0.077 14.57 0.22 1.0-2.0 0.156 9.84 0.44

2/CH S PEROXIDE
Phng php acid acetic v chloroform nh ngha: y l phng php xc nh tt c cc cht. l gii hn ca s milligram ng lng ca peroxide/1000g mu . l s oxi ha KI di iu kin th

nghim. Cc cht thong thng c cha peroxidesd hoc ging nh sn phm ca cht bo b oxy ha. Phm vi: p dng cho tt c cc cht bo, du thng thng bao gm c du c. y l phng php thc nghim cao v c vi thay i trong phng thc thc nghim dn n kt qu thay i Dng c- thit b 1/ Pipet 0.5ml hoc nhng dng c c dung tch thch hp khc. pha ch 0.5 ml dung dch KI bo ha. 2/ Bnh tam gic hoc bnh thy tinh c nt 250ml. Thuc th 1/ Dung dch acid acetic-chloroform: V(3:2): pha ch bng cch trn 3V ca dung dch acid acetic vi 2V ca chloroform 2/ Dung dch KI bo ha: c chun b mi mi ngy. Thc hin ha tan mt lng qu mc KI trong nc ct un si. Chc chn rng dung dch to thnh phi bo ha trong sut thi gian s dng. Nhn bit c bi s c mt ca tinh th KI khng b ha tan. trong ti khi cha s dng. Kim tra dung dch KI bo ha bng cch cho 2 git dung dch tinh bt vo 0,5ml dung dch KI trong 30ml dung dch acid acetic v chloroform. Nu mu xanh c to thnh th cn phi cho hn mt git dung dch Na2S2O3 0.1N ty mu th loi b dung dch KI v chun b dung dch mi. 3/ Dung dch Na2S2O3.5 H2O nng 0.1N, c chun ha chnh xc. K2Cr2O7 theo qui trnh sau: a/ Na2S2O3 0.1N c chun b bng cch ha tan 24,9g Na2S2O3 trong nc ct, pha long nh mc n 1l b/ K2Cr2O7 : ch tiu quan trng nht: nn nghin nh, sy kh 0 105 C trong 2 gi v lm ngui trong bnh ht m. cn 0,16-0,22g K2Cr2O7 cho vo bnh cu 500ml hoc nhng bnh tng ng. Ha tan trong 25ml nc v 5ml HCl m c, 20ml dung dch KI v o trn ,cho php yn trong vng 5 pht v thm vo 100ml nc ct. Chun bng dung dch Na2S2O3 0.1N, lc lin tc cho n khi mu vng hu nh b mt. Cho thm 1-2 ml ch th tinh bt v tip tc chun . Thm dung dch Na2S2O3 chm n khi mu xanh va bin mt. Nng ca dung dch Na2S2O3 c biu din trong gii hn tiu chun: 20,394Klca K2Cr2O7 Nng ng lng ca dung dich Na2S2O3 = V ca Na2S2O3 4/ Na2S2O3 0.01N : dung dch ny c th c chun b bng cch ht chnh xc 100ml dung dch Na2S2O3 0.1N vo trong bnh c th tch 1000ml v pha long bng nc ct nng n vach th tch. 5/ Dung dch ch th tinh bt: c kim tra tnh nhy. c chun b bng cch lm h bt vi 1g tinh bt v mt lng nh nc ct lnh, trong lc khuy cho thm nc ct nng n 200 ml v un nng vi giy. Ngay lp tc chuyn t nng v ngui. Acid salycilic 1,25g/l c th thm thuc th bo qun. Nu cn bo qun lu th dung dch phi c trong t lnh 4-100C. Ch th mi phi c chun b khi kt thc qu trnh chun m mu xanh khng mt i mt cch r rt. Nu trong t lnh th dung dch tinh bt c th n nh c khong 2-3 tun. Kim tra nhy: cho 5ml dung dch tinh bt vo 100 ml nc, thm 0,05ml dung dich KI c chun b mi v 1 git dung dch chlorine 50ppm c lm

bng cch pha long 1ml dung dch NaOCl 5% n 1000ml. V mu xanh m c to ra phi c loi b khi cho 0,05ml dung dch Na2S2O3 0.1N Cch tin hnh cho du v m 1/ Cn 5g 0,05g mu vo trong bnh tam gic 250ml v cho thm 30ml dung dch acid acetic v chloroform theo t l 3:2. Lc ha tan mu. Cho vo 0,5ml dung dch KI bo ha. S dng pipet c dung tch thch hp. 2/ yn dung dch trong 1 pht. Ngay sau cho thm 30ml nc ct. 3/ Chun bng Na2S2O3 0.1N. Cho vo t t v lc lin tc.Tip tc chun cho n khi mu vng iod hu nh bin mt. Cho thm khong 0.5ml dung dch ch th tinh bt. Tip tc chun v lc lin tc, gn n im cui gii phng ton b iod t dung mi. Cho vo tng git Na2S2O3 0.1N n khi mu xanh va bin mt 4/ Chun b 1 mu trng. khng c vt qu 0.1ml dung dch Na2S2O3 Cch tin hnh i vi du c 1/ Lm tan chy mu bng cch un nng trn bp in hoc bng cch un nng trong khng t sy 60-700C. Trnh un qu nng v c bit ko di thi gian un nng ca du khi du t nhit qu 400C. 2/ Khi lm tan chy mu xong, chuyn mu ra khi ch nng hoc lm ngui n khi dung dch phn chia v dng rn y cc. 3/ Gn, chc du trong cc cho thm qua giy lc Whatman s 4 vo mt cc sch khc. Khng lm nng li du lc tr khi cn thit. mu phi trong v sng. 4/Tip tc lm nh cch lm i vi du v m on 1.4 Cch tnh 1/ Ch s peroxide (mili ng lng peroxide/1000g mu) (S-B) N1000 KL mu Trong : B l dung dch tiu tn trong chun mu trng S l dung dch tiu tn trong chun mu N l nng dung dch Na2S2O3 Ch Chloroform c bit l cht gy ung th, n l cht c khi ht vo v l cht c c tnh gy m. Trnh tip xc vi da, n hoc ht vo trong thi gian di c th dn n bnh au gan, h thn, ct v c th nguy him n tnh mng. N khng chy nhng c th t chy khi trn la lu hoc nhit cao.TLV trong khng kh 10ppm. Nn s dng t ht trong sut thi gian s dng chloroform. Acid acetic trng thi tinh khit th tit ra cht c khi n vo bng v k vo. N kch thch mnh n da v m. TLV trong khng kh l 10ppm Mt s ch 1/ Issoctance cj a ra thay th cho chloroform trong phng php ny. Phng php m s dng Issoctance c ph chun bi AOCS nm 1990 2/ Tinh bt khoai ty cho iod. c a chung bi v tinh bt to ra mu xanh m khi c mt ca ion iod. Tinh bt ha tan th khng c a chung bi v mu xanh m c c th khng c hnh thnh khi vi loi tinh bt ha tan tc ng vi ion iod. C mt s loi tinh bt thch hp sau y: tinh bt ha tan cho iod Fisher S516-100, tinh bt khoai ty ha tan Sigma S 2630, tinh bt khoai ty ha tan cho iod: JT Baker 4006-04 3/ Th nghim nn a ra ngoi vng nh sng kch thch hoc nh sng nhn to, che y t hng ca ngun sng. Bng bo co trn mt phng php in lng cho s o c ch s peroxide cho bit phn ng iod -peroxide c phn ng v kt thc 1 pht v s gii phng iod chu nh hng nhiu ca nh sng.

4/ Nu qu trnh chun s dng t hn 0,5 ml Na2S2O3 0.1N th s dng Na2S2O3 0.01N xc nh li. Tham kho 1/ Oil and Soap 9:98(1932) 2/J.Assoc.Off.Anal.Chem.75:507 (1992)

3/CH S IOD CA DU M
PHNG PHP WIJS nh ngha: Ch tiu iod l tiu chun nh gi cc loi du m khng no. V c biu th bng s centigram ca iod b hp th/ khi lng mu. ng dng p dng cho tt c cc loi du m thng thng khng cha lin kt i lin hp. Dng c 1/Bnh cha iod - 500ml 2/ Bnh nh mcdung tch 1000ml chun b dung dch chun. 3/ Pipet 25ml phn phi chnh xc 25 ml dung dch Wijs 4/ Dng c th tch 20ml iu chnh 1ml rt dung dch KI 10% 5/ Dng c th tch 2ml iu chnh 1ml rt dung dch tinh bt 6/Dng c th tch 50ml iu chnh 1ml rt nc ct 7/ Pipet, bnh 20ml cho cyclohexane 8/ Cn phn tch chnh xc 0.0001g 9/ My khuy t 10/Giy lc what man s 41H hoc tng ng 11/ Cc 50ml 12/ L sy 13/ ng h bm thi gian Thuc th 1/ dung dch Wijs 2/ dung dch KI 3/ CCl4. Kim tra s vng mt ca cht oxihoas trong thuc th c kim tra bng cch lc 10ml thuc th vi 1ml dung dch K2Cr2O7 no bo ha v 2ml acid sunfuaric m c, khng c mu xanh xut hin 4/ Ha tan dung dch tinh bt , chun b mi y. Kim tra nhy bng cch lm h bt t 1g tinh bt ha vi mt lng nh nc ct lnh, trong lc khuy cho thm nc nng n 100ml. Kim tra nhy cho 5ml dung dch tinh bt ha tan vo trong 100ml nc, thm vo 0.05ml dung dch KI 0,1N mi c chun b v 1 git dung dch chlorine 50ppm c lm bng cch pha long 1ml NaOCl 5% n 1000ml, mu xanh m to thnh phi c ty bng 0,05ml dung dch Na2S2O3 0.1N 5/ K2Cr2O7 c nghin nh v sy n khi lng khng i khong 110oC trc khi s dng. Ch : tiu chun mu ca K2Cr2O7 vi giy chng nhn phn tch c th t c t b chnh ph ca tiu chun trong Washington. 6/ Na2S2O3.5 H2O

Cc dung dch 1/ Dung dch KI 10%(100g/l): c chun b bng cch ha tan 100g KI trong 1000 ml nc kh ion ha 2/ Dung dch ch th tinh bt: c chun b v kim tra nh ghi ch trong thuc th, acid salicylic(1,25g/l) c th c cho thm lm cht bo qun Nu cn gi lu th yu cu dung dch phi c gi trong t lnh nhit 0 4-10 C (40-500F). Ch th mi phi c chun b ngay khi n im cui chun khi mu xanh khng b mt i mt cch r rt. Nu gi trong t lnh th dung dch tinh bt c th n nh c khong 2 -3 tun. 3/ Na2S2O3.5 H2O 0,1N c chun ha chnh xc bngK2Cr2O7 theo qui trnh sau: a/ Dung dch Na2S2O3 0.1N chun b bng cch ha tan 24,9g Na2S2O3. trong nc ct v pha long n 1l. b/ Cn 0,16 -0,22g K2Cr2O7 khan vo trong bnh 500ml. Ha tan trong 25 ml nc, thm 5ml HCl m c v 20ml KI o trn, yn trong 5 pht. Sau cho 100ml nc ct, chun bng dung dch Na2S2O3, lc mnh n khi mu vng hu nh bin mt. Cho 1-2ml ch th tinh bt v tip tc chun . Cho dung dch Na2S2O3 chm cho n khi mu xanh va bin mt Nng ng lng dung dch Na2S2O3 c tnh theo cng thc n. ng lngNa2S2O3=20,394khi lng K2Cr2O7 4/ Dung dch wijs Tin hnh 1/lm chy tan mu nu n khng dng lng( nhit trong qu trnh lm tan mu khng nn vt qu nhit nng chy ca du 100C), lc qua giy lc v rt ra cn bn v vt hi m cn li. Qu trnh lc c th thc hin trong l nhit 1000C nhng nn hon tt trong vng 5 pht 30 giy. Mu phi hon ton kh Ch : tt c cc thy tinh phi hon ton kh v sch Bng 1: Khi lng mu Ch s iod Khi lng (g) 0.001 <5 3.000 5-20 1.000 21-50 0.400 51-100 0.200 101-150 0.130 151-200 0.100 2/ Sau khi lc, cho mu lc t nhit 68-71oC1 trc khi cn mu 3/ Khi mt mu t c nhit 68-71oC lp tc cn mu trong bnh 500ml, s dng cn v cn chnh x khi lng nh trong bng 1 (xem ghi ch 6) 4/ Cho thm 15ml CCl4 vo mu v xoay n khi m bo mu tan hon ton 5/ Phn tn 25ml Dung dch wijs, s dng pipet( ht chnh xc) vo trong bnh cha mu,y np bnh v xoay n khi m bo dung dch c trn u. Ngay lp tc bm ng h 1 hoc 2 gi ty thuc ch s iod ca mu IV<150,1h, IV150,2h. ngay bnh vo trong bng ti theo yu cu thi gian phn ng nhit 25 5oC 6/ Chuyn bnh ra v cho thm 20ml dung dch KI , cho thm 150ml nc ct

7/ Chun bng dung dch Na2S2O3 0,1N, cho t t v lc lin tc v mnh, tip tc chun cho n khi mu vng hu nh bin mt, cho thm 1-2ml dung dch ch th tinh bt v tip tc chun n khi va mt mu xanh 9/ Chun b v lm ti thiu 1 mu trng. xc nh i vi mi nhm mu, lm ng thi v song song vi mu nhng khng cha mu. Cch tnh (B-S)N12,69 Ch s iod = KL mu B: lng dung dch tiu tn trong qu trnh chun mu trng S: lng dung dch tiu tn trong qu trnh chun mu N: nng ca dung dch Na2S2O3 Ch Dung dch wijs gy ra chy d di v hi ca n c th gy tn hi cho phi v mt. Nn s dng t ht khi s dng Dung dch wijs, dung dch wijs khng c cha CCl4 c bn trn th trng CCl4 c bit l cht gy ung th. N l c t khi n vo bng, ht phi hoc tip xc vi da. N l mt cht gy m. N c th s dng dp tt la. N phn hy to thnh kh COCl2 rt c nhit cao. TLD trong khng kh l 5ppm. Nn s dng t ht khi s dng CCl4 HCl l mt acid mnh v s gy ra bng d di, cn phi bo v qun o khi b n mn khi lm vic vi acid ny. N l mt cht c khi n phi v ht vo, n gy kch thch mnh n mt v da, s dng t ht khi lm vic vi HCl. Khi pha long acid lun lun cho acid vo nc, khng bao gi c lm ngc li Chlorine l kh c, TLV trong khng kh l 1ppm, n l tc nhn oxi ha mnh v khng c tip xc vi cc hp cht hu c. Phi s dng t ht khi s dng chlorine. H2SO4 l mt acid mnh c kh nng gy chy. Bo v qun o khi mn khi lm vic vi acid ny. N l mt tc nhn oxi ha v khng c gn hoc tip xc vi cc hp cht hu c. Ht sc ch khi trn vi nc. V ta nhit v c th gy n hoc bn tung te, lun cho acid vo nc , khng bao gi c lm iu ngc li Acid acetic trng thi tinh khit l mt cht c nh khi n phi hoc ht vo. N kch thch mnh n da v m. TLV trong khng kh l 10ppm Dn d Dung dch cyclohexan + acid cetic 1:1l cht c th thay th tt cho CCl4 (xem AOCS cd 1b-87) v c tm quan trng i vi mi trng. 1,1,2 trichloro-1,2,2 trifluoroethance th khng c a chung. Acid acetic ring hoc hn hp acid acetic v cyclohexan (4:1 v/v) khng thch hp thay th cho CCl4 Mt s ch Khi ch s iod xc nh trn cc cht c cha ni i lin hp th kt qu khng o c tng lng ni i nhng vn tt hn ch tiu thc nghim biu th tng s lng ni i c mt. Kt qu t c c kh nng so snh tng lng ni i. Khi ch s iod c yu cu cho cc acid bo. S chun b v s phn ly c trnh by nh trong phng php AOCS Bi v s chun b dung dch wijs cn phi s dng ha cht mang hai c tnh va c hi va nguy him. Dung dch ny c th kim c t cc nh cung cp ha cht. Dung dch ny c sn CCl4 khng no. Dung dch wijs rt nhy vi nh

sng, nhit v m. Cn bo qun ni thong mt v ti, khng bao gi c nhit cao hn 25-30oC. Phng th nghim chun b dung dch wijs c ch cho mc ch yu cu Thuc th a/ Acidacetic/: Kim tra MnO4 chc chn n s dng c Kim tra MnO4: pha long 2ml acid vi 10ml nc ct v 0,1ml KMnO4 0,1N. Mu hng khng phi hon ton mt i trong 2 gi Kim tra xen k s vng mt ca cc cht oxi ha trong thuc th c th kim tra bng cch lc 10ml thuc th vi 1ml dung dch K2Cr2O7 no v 2ml H2SO4 m c khng c mu xanh xut hin. b/ Chlorine 99,8%: c lm kh bng cch cho qua hi H2SO4 trc khi cho vo dung dch iod c/ iod d/HCl m c 1,19g e/ H2SO4 m c 1,84g f/ ICl s chun b trong phng th nghim a/ Ha tan 13g iod trong 1l acid acetic, un nng nh c th cn thit cho qu trnh hot ha dung dch, chuyn mt lng nh (100-200ml) v vo ni lnh s dng sau. Cho qua hi Clorine trong dung dch iod n khi s chun gc khng kt hp ton b hai phn c tnh chuyn mu c gi li trong dung dch wijs khi lng chlorine thch hp c a vo , c th c s dng xc nh im cui Cho mt t chlorine v ngay lp tc mang i chun bng cch cho mt t dung dch iod gc l dung dch c rt ra phn u. c hai dung dch gc v hon ton dung dch wijs c chun vi dung dch Na2S2O3 nh cch lm phn 6 v 7 b/ Dung dch wijs c th c chun b t ICl s dng trong cng nghip nh sau: Dung dch d tr: cho 317 0,1g ICl vo 1l acid acetic v lc qua giy lc vo trong bnh sch v kh. Lc nhanh trnh nhim m. Ct ni mt m. Phi loi b dung dch nu n b ngng t nc. Dung dch wijs: s dng cc chia , rt 117 0,1ml dung dch d tr trong bnh chun 5.1b ca acid acetic v trn u bng cch lc c/ T s ca dung dch I/Cl ca dung dich wijs c gii hn trong phm vi 1/10 0,1. Cch xc nh t s nh sau: Lng iod: 150ml nc bo ha Cl trong bnh tam gic 500ml v cho thm 5ml dung dch wijs trong bnh cu c cha nc chlorine bo ha, lc v un nng nhanh trong khong 10 pht, ngui v cho 30ml H2SO4 2% v 15 ml dung dch KI 15%, trn u v lp tc chun bng dung dch Na2S2O3 0,1 N, c cho tinh bt im cui. Tng lng halogen: 150ml nc ct un si trong bnh tam gic sch v kh 500ml, cho 15 ml dung dch KI 15% ri cho 20ml dung dch wijs vo trong bnh ri trn u. chun bng dung dch Na2S2O3 0,1 N, c cho tinh bt im cui. Cch tnh t l halogen 2A T l halogen = 3B-2A A: lng Na2S2O3 chun

B: tng lng halogen chun vi Na2S2O3 3/ Dung dch tinh bt 1% c th mua t nh cung cp ha cht 4/ Tinh bt khoai ty cho iod. c a chung bi v tinh bt to ra mu xanh m khi c mt ca ion iod. Tinh bt ha tan th khng c a chung bi v mu xanh m c c th khng c hnh thnh khi vi loi tinh bt ha tan tc ng vi ion iod. C mt s loi tinh bt thch hp sau y: tinh bt ha tan cho iod Fisher S516-100, tinh bt khoai ty ha tan Sigma S 2630, tinh bt khoai ty ha tan cho iod: JT Baker 4006-04 5/ Dung dch Na2S2O3 c th mua t nh cung cp ha cht. Tuy nhin phi c chun ha li trong phng th nghim 6/ Vi khi lng nh vy s vt qu khi lng gii hn ca dung dch wijs 50-60% tng lng thm vo 100-150% tng lng hp th. Trng hp ca du c khi lng mu l 0,1-0,2 g s dng thm 55 3% dung dch wijs. Trong trng hp du hydrat ha v hydrat ha acid bo t do khi lng 0,1-0,13 7/ Thi gian phn ng ca ch th c ch r trong IUPAC. Phng php tiu chun iod 2205 v thi gian phn ng s dng trong IUPAC /ISO mt cch c hiu lc ca cyclohexan v acid acetic phng php (AOCS Cd-92). Trc li din ta AOCS ca ch s iod ch r thi gian phn ng 0,5 gi, nhng ch rng thi gian phn ng c th cn thit cho cc loi du c ch s iod cao, thi gian phn ng di, xut hin khi xyclohexan c thay th cho CCl4 8/ Nu phn ng khng xy ra hon ton trong vng 3 pht sau mu phi b 9/ Mu phi c chun trong vng 30 pht. Phn ng sau thi gian s phn tch khng c hiu lc 10/ my trn c s dng cho s rung ng trong sut qu trnh cho thiosunphat vo Ti liu tham kho 1/standard Method for a Analysic of Oils, Fats and Oil Derivatives, Internaional union of Prue and Applied Chemistry

4/MU SC
PHNG PHP S DNG THY TINH MU CHUN VI THANG O MU SC K Khi nim: Phng php xc nh mu tng xng ca nh sng truyn qua b dy ca du hoc m lng n nh sng gc t ngun ging nhau c truyn qua thy tinh mu chun Tiu chun CIE ca thy tinh mu chun Lovibond c lit kt trong bng 1 ng dng :

p dng cho tt c cc loi du, m ng thc vt, c chun b khng c cc cht c trong mu. y l phng php c cn c vo tiu chun Anh BSI , phng php BS684. y l phng php c tha nhn cc quc gia o mu trong du m ng thc vt Dng c: 1/Cc dng c th nghim thng thng 2/My so mu: s c bo qun trong iu kin tt, sch 3/ Bung sng gm c 2 n 60 oat, hot ng in p chnh, v mi mu chiu sng trong phm vi 45 , nhng ci n s cng v tr vi ng quan st Ch : 2 ci n ko c hot ng lu hn 100 gi. H thng thch hp s lm cho n sng, 2 n s sng ng thi V tr t mt v khong cch b lc t i din vi ng cha mu v phm vi ca ng ng mu v tm knh trng thng c t 1 gc 90 . Bung chiu sng thng xuyn c kim tra loi b nhng vt do bn v khi sn b trc, bung s sn li vi 1 mu sng khi mu tr nn ti hn 4/ Nhng thanh mu chun bao gm: , vng ,xanh v mu trung tnh vi s ghi nh sau: :0,1-0,9 ,1.0-9.0,10.0-20.0 Vng : 0,1-0,9 ,1.0-9.0, 10.0-70.0 Xanh: 0,1-0,9 ,1.0-9.0 Trung tnh: 0,1-0,9 ,1..0-3.0 Nhng knh mu chun ng vi tng gi tr CIE lit k trong bng 1 5/ Khay cha mu 6/ Cuvet: c lm t knh quang hc vi chiu dy nh sau: 1,6mm(1/16in) ,3,2mm(1,8in),6,4mm(1/4in) 12,77mm(1/2in),25,4mm(1in),133,4(5.1/4in) 7/V bao kim loi ti S la chn ca ngi so mu 1/Tt c nhng ngi so mu s phi p ng c mi yu cu v kim tra kh nng nhn mu v s c kim tra khong 5 ln/1 nm 2/ Khng c eo nhng knh c mu v knh nhy sng khi quan st Mu 1/mu s c lm ph hp vi mu th c chp nhn Chun b mu Chun b mu th nghim ph hp vi tiu chun Anh, phng php BS 684. iu cn thit l mu du hoc m phi hon ton dng lng, sch v sng khi tin hnh xc nh. Nu mu khng dng lng nhit phng th cn un nng chng n khong nhit ln hn nhit nng chy 100C Cch tin hnh 1/ iu cn thit cho s xc nh l mu phi c thc hin trong iu kin nh sng du ngha l khng c mt ca ca s hoc nm trong hng ca nh sng mt tri 2/ Rt mu chun b vo cuvet, lm y cuvet c kt qu theo nhng thang mu c ghi trong bng 1. m bo cuvet sch v kh hon ton, nu cn thit chng phi c ra sch loi b cht rn bm vo 3/ Ni cuvet l bn trong bao kim loi ti, tng phn vi bung sng . Cm nhng thanh mu lp tc xc nh mu ca mu bng cch s dng thanh mu theo t s 10 vng,1 . Chnh sa cho n khi t c chnh xc mu tng xng.

Khng cn thit phi duy tr t s 10 vng 1 . V s dng mt t mu xanh hoc mu trung tnh n v n khi t c s cn xng, nhng khng nhiu qu 9 xanh hoc 3 trung tnh Ch : m bo cho s trn b mt thy tinh mu trong c mu v b lc ging nhau 4/ V mt rt d b mi nn ngi th my s ngh ngi mt sau 30 giy vn hnh my. Th nghim c lm t 2 ngi vn hnh tr ln. 5/ Nu lm li khng tha mn yu cu trong phn lp li v trong bng 2 th mt ngi th ba c li, ly cng vi kt qu trung bnh ca 2 ngi o mu gn xc nhau 6/Ghi li kch c ca hp thy tinh s dng . c mu : , vng, xanh .v mu trung tnh o c tng xng Din t kt qu 1/Ly khong gia kt qu t c t hai ngi o. Nu yu cu ca ngi lm li khng chun xc th c khong gia ca hai ngi m c khong cch gn nhau nht 2/din t kt qu trong gii hn sau a/ c s ca mu , vng, xanh v trung tnh t c tng xng b/ B dy ca hp thy tinh 3/Mu o c trong mt kch thc hp thy tinh s khng c s dng tnh ton mu cho hp thy tinh c kch thc khc lp li: Mt s khc nhau gia kt qu t c t hai ngi o c din t trong qui trnh, s dng dng c ging nhau ng thi trong phng th nghim hoc l k tip nhau s khng vt qu gi tr bng 2 Bng 2: S chp nhn c trong cch c mu c n 0.9 T 1,0 n 2.9 T 3.0 m 4.0 T 4,1 n 1,2 S khc nhau chp nhn c 0,2 0,4 0.5 1.0

Bng bo co 1/bng bo co th nghim s biu din phng php s dng, kt qu t c, n s ni n nhng ngi o khng ch r trong phng php ny hoc ty . c xem nh l nhng trng hp c th nh hng n kt qu 2/ Bng bo co bao gm tt c cc chi tit yu cu cho s hon thnh ng nht ca mu Ch :\ 1/ My so mu lovinbond ph bin kiu AF 900/684 ( Hoc sm hn, hocc tng ng) t c t mi ci o mu Ltd Wilshire vng quc Anh hoc khoa hc HF Ine. Fort Myer FL USA c tm thy mt cch thch hp cho vic s dng trong phng php ny 2/ Trong thc hnh k c mu dch quc t, nhng n v trong h o lng c s dng hin ti cho n nay

3/ Hp thy tinh ng mu s c lm bng thy tinh tt vi tiu chun cao 4/ Ti cc hip hi quc t FOSFA bn v s hi ha trong cc phng php phn tch vo thng 12 nm 1991 ra nn chn v kim loi en s dng cho phng php ny. Nu v ny c s dng th ghi ch v bo co 5/ Kt qu tt nht l ngi tin hnh t nh gi 6/ Nhng ngi mang knh trng hoc thu knh c th tip tc mang chng.

5/IM NNG CHY Theo phng php AOCS nh ngha im trt l mt ch s ca nhit m ti lm mm m v tr thnh dng lng trt trong ng mao dn. ng dng: y l phng php c s dng trong cc c tnh ca du c trong mu dch quc t. y l phng php c ng dng cho du c v cc loi m th bao gm du ht c, du da, sterin, du hydrogenatet v m heo th, n khng ph hp cho m ln, m mm, m ng vt. N khng ph hp cho m ln pha, trn gia m th, m mm v nh tng. Dng c: 1/ ng o nng chy: ng mao dn thy tinh, ng knh trong khong 1mm, ng knh ngoi 2 mm l ti a, chiu di thch hp l 50-80mm c cung cp t Kontes Vineland,NJ USA 2/ nhit k loi 2-68C hoc -2-80C trong ti liu AOCS H6-40 hoc H7-45. n s (NIST) 3/ Cc thy tinh 600ml 4/ Ngun nhit: bp in vi h thng bin tr Tin hnh 1/ Lm mu tan chy v lc qua giy lc loi b cht bn v nhng hi m dng vt trong du. iu cn thit i vi mu l tuyt i kh 2/ Nhng t nht ba ng mao dn trong mu lng hon ton, a mu dng ln khong 10mm chiu cao trong ng, lm lnh u cui ca ng mao dn cha mu trn mt khi lnh cho n khi du m tr nn c v rn 3/ ng trong cc v cho vo trong t lnh 4-10C trong 16 gi c th qua m 4/Chuyn ng t trong t lnh v gn vi dy cao su hoc bng phng tin thch hp sao cho im di cng ca ng mao qun ngang bng vi nhit k thy ngn. 5/ Treo l lng nhit k trong cc 600ml, nc ct sch. Ci y ca nhit k c nhn chm trong nc ngm 6/ iu chnh nhit ban u ca cc nc n di im nng chy ca mu 8-100C. Khuy cc nc vi lung kh nh hoc phng tin thch hp. V nng

nhit cc nc ln theo t l 10C/ pht. n gn im nng chy th chm hn 0.5C/phut. 7/ Tip tc un nng n khi ct m dng ln trong mi ng. Quan st nhit m ti cht bo dng ln mi ct v tnh ton nhit trung bnh ca mi ng. vit bo co im trt Bng 1: Nhng nghin cu ca cc phng th nghim c hon thnh bi Porim 1980 vi s tham gia ca 13 phng th nghim ring bit. C hai ln kim tra s thu c kt qu cho mi mu phn tch ring bit v c thng k kt qu tm tt trong bng sau Thng s im trt C S.C lp li CV ca lp li % Ch s lp li,r=2,8.Sr SR.C lp li CV ca lp li % Ch s lp li,r=2,8.SR Ch 1/ B nc v b iu khin nhit c th c s dng cho h thng kim sot nhit chnh xc hn 2/ Du c v cc sn phm du c s c lm nng 10oC 1 trong 16h 3/ phng php c nhanh chng trong vic kim tra cht lng mu, 16 gi c th gim xung 2 gi hoc 1 gi, kt qu c bo co ti im trt 1 gi hoc 2 gi. Thp hn khong 0,2oC so vi im trt chun 10 gi. i vi du c th ln hn khong 1,2 oC Tham kho J.Am. Oil.Chem.Soc.59(5):244(1982) A 35,3 0,30 0,8 0,8 0,87 2,5 2,4 B 20,2 0,17 0,8 0,5 0,68 3,4 1,9 C 52,2 0,20 0,4 0,5 0,59 1,1 1,6

XC NH HM LNG CC CHT BAY HI V M (M) AOCS Ca 2c-25

in 1995, 1983 Ph chun li 1973, 1993 S dng t 6/92 n 5/01 theo 1973 S dng t 6/01 theo 1993 I/ Nguyn tc: Du hoc cht bo c gia nhit ti 130oC1oC va trng lng mt i c xc nh. Cht bay hi bao gm nc c tnh theo phn trm lng mu phn tch. II/ Chun b mu: Lm mm mu du c 45-50oC v khuy trn u III/ Phng php 1/ Ra sch a v sy kh trong t sy 1301oC t nht 30 pht 2/ Lm ngui a trong bnh ht m 3/ Cn a ghi gi tr (mo)

4/ Thm 11ml du c chy mm bng pipet (khong 101 mu du) 5/ t a vo bnh lm ngui 6/ Cn a c du chnh xc 0.1mg (m1) 7/ Sy a du trong t sy 130 1oC trong 30 pht 8/ Ly a du ra trong bnh ht m, lm ngui n nhit phng. 9/ Cn li chnh xc 0,1mg 10/ Sy li mu thm 30 pht na 11/ Lm ngui trong bnh ht m 12/ Cn li mu (m2) 13/ Lm li cho n khi trng lng sai s khng qu 0,05% so vi mu sy trc 30 pht. IV/ Kt qu tnh. M M2 % m 1 x100 M1 M 0 V/ Dng c: 1/ T sy nhit 130oC1oC 2/ a thy tinh ng knh 5 cm 3/ Bnh ht m. 4/ Cn phn tch chnh xc n 0.1 mg 5/ Pipet chia

XC NH TP CHT KHNG TAN TRONG DU C (I)

Ca 3a- 46

AOCS

Thay th Ca 3 25 v Ca 3 -46 in 1987 Ph chun li 1973, 1993 S dng t 6/92 n 5/01 theo 1973 S dng t 6/01 theo 1993 I/ Mu: Vic phn tch c thc hin i vi du c nng chy nhit 45-50oC v trn u. II/ Phng php. 1/ t giy lc vo phu lc Gooch 2/ Ra giy lc bng petroleum ether ( khong 10ml) 3/ Sy kh giy lc v phu 101 1oC trong t sy khong 30 pht. 4/ Lm ngui trong bnh ht m. 5/ Cn phu c giy lc chnh xc 0,1mg (M2) 6/ Cn 20g 1g du cn phn tch, chnh xc 0,01g vo cc thy tinh sch kh (Mo) 7/ Lm nng du nng chy hon ton. 8/ Thm 50ml dung mi v lc u cho tan du trong dung mi, lm nng nu cn. 9/ lng cho n khi cc cht khng tan lng xung y cc ( khong 5 pht) 10/ Rt t t dung mi vo phu lc v ht nh bng my ht chn khng 11/ Dng dung mi sch hon ton cht khng tan t cc vo phu. 12/ Ra phu lc nhiu ln ( khong 50ml dung mi ) cho n khi cc vt du c khng cn dnh trn phu lc v giy lc.

13/ Ht nh, u sau ly phu lc ra, lau sch bn ngoi bng vi sch hoc giy tissue. 14/ Sy kh phu lc 101 1oC trong t sy khong 30 pht. 15/ Lm ngui trong bnh ht m v cn chnh xc 0,1mg (M1) III/ Kt qu tnh: M M2 % Tp cht 1 x100 M0 IV/ Dng c: 1/ Phu lc Gooch, ng knh trong 2.1 hay 2.4 cm 2/ Giy lc va kht vi phu lc. 3/ T sy 101 1oC 4/ Bnh ht m Silicagel 5/ Cn phn tch. 6/ Cc thy tinh 7/ Bm chn khng. V/ Ha cht. Petroleum ether nhit si 60-80oC

XC NH IM C (C.P)
Cloud test = cloud point test

AOCS Chai chun 6- 25 Ph chun li 1973, 1993 S dng t 6/92 n 5/01 theo 1973 S dng t 6/01 theo 1993

I/ nh ngha: im c l nhit m ti c s c du c hnh thnh do bc u ca s kt tinh. p dng: p dng cho tt c cc loi du ng vt v thc vt. II/ Dng c 1/ Cc thy tinh. 2/ Nhit k. 3/ Ni cch thy c nhit khng i, khng t hn 2oC hoc ln hn 50C di im c. III/ Qu trnh th 1/ Mu phi c sy kh hon ton trc khi tin hnh. Gia nhit khong 75ml mu trong cc thy tinh 100ml ti 130oC v lm ngui ti nhit phng. 2/ Khi mu t 10oC trn im c dng nhit k khuy trn u mu ngn s kt ta thnh cc. 3/ T khng c ly nhit k ra khi cc mu. Cc c nhng trong chu nc v tr sao cho mt du ngang vi mt nc. 4/ Ly cc ra v kim tra thng xuyn. im c l nhit ti khng th thy c bu thy ngn ca nhit k trong cc khi nhn ngang qua mu. ( Nhit k t gia cc thy tinh.) Ch xc nh im nng chy: - du v cc sn phm ca du c nn gi nhit 10 1oC trong 16h - i vi phng php nhanh cho mc ch kim tra cht lng, 16h c th gim cn 2h hay 1h

XC NH HM LNG SAVON TRONG DU ( phng php chun )

I/ nh ngha: y l phng php xc nh kim ca mu quy v sodium oleate II/p dng: Ch p dng i vi du thc vt tinh luyn III/ Thit b: 1/ ng nghim c np, quy cch 150*40mm hoc bnh tam gic 250ml 2/ Buret vi lng (Microburet 5ml), vch chia 0.02ml 3/ Bp cch thy ( B hi hay b nc nng). IV/Thuc th: 1/ Acetone cha 2% nc: thm 20ml nc ct vo 980 ml acetone. 2/ HCl 0.01N, dung dch chun ( pha t ng chun). 3/ Dung dch ch th Bromophenol xanh 1% trong nc. 4/ Dung dch NaOH 0.01N, phi hiu chnh li trc khi s dng. V/ Quy trnh: 1/ Ch trc khi phn tch mu, chun b dung dch th bng cch thm 0.5ml ch th Bromophenol xanh vo mi 100ml dung dch Acetone 2% v chun vi HCl 0.01N hay NaOH 0.01N n khi dung dch th va chuyn sang mu vng. 2/ Cn 40g mu du, xem ghi ch, cn xc nh vo ng nghim 1 (bnh tam gic) v phi ra ng nghim (bnh tam gic) bng dung dch th ( bc 1 ca qui trnh) 3/ Thm 1ml nc vo mu th, un nng v lc mnh. Sau khi un nng, thm 50ml dung dch th (bc 1) vo v lc k ng nghim (bnh tam gic), yn ch tch thnh 2 lp hon ton. Ghi ch: nu c x phng trong du, lp bn trn s c mu xanh l m cho n mu xanh dng 4/ Thm t t HCl 0.01N t microburet cho n khi mu va chuyn t xanh l m /xanh dng sang mu vng. Lp li vic un nng ng nghim (bnh tam gic), lc v thm HCl 0.01N cho n khi mu vng lp bn trn vn cn r. Ghi li tng th tch HCl 0.01N dng mls (ml) 5/ Lm ngui mu trng (du khng c x phng) c thc hin theo cc bc trong quy trnh t 1-4. Ghi li th tch HCl 0.01N dng mlb(ml) Tnh ton: Hm lng x phng (ppm) quy v sodium oleate (mls mlb ) xNx30400 Ppm quy v sodium oleate W (g) Trong : - W: khi lng mu (g) - Mls: th tch HCl dng, bc 4. ml - Mlb: th tch HCl dng, bc 5.ml - N: nng ng lng HCl. Ghi ch: Acetone rt d chy. Dng peroxide hnh thnh s n khi gp tc nhn oxi ha. Nn s dng t ht. Khng nn trn vi chloroform (CHCl3). S ghi ch: 1/ Phng php ny ph hp i vi mu du c hm lng x phng ti a 0.05%. Nu mu c hm lng x phng cao hn, nn cn 4g mu v s dng HCl 0.01N.

XC NH HM LNG DU MT TRONG T TY
in 1992 S dng t 6/92- 12/01:1992 Sa li T1/02(JOMALINA),mc 2 p.p phn tch, trl 3-14/24:21/04/95 S dng t T1/02: JOMALINA/95

Mt du trong ty mu:
I/Phng php: 1/ Cn chnh xc khong 5g t thi vo a petri v t trong t sy 103oC trong 2 gi. 2/ Lm ngui a petri trong bnh ht m v cn 3/ Sy li trong t sy 0.5 gi, lm ngui, cn li. 4/ Lp li trnh t 3 cho n khi cc ln cn k tip chnh lch t hn 0.001g. 5/ Tnh % m trong cht thi l: W tks Wt sks x100 % Moistre t M t tks 6/ Cn chnh xc khong 3g mu t thi sy vo giy lc, gi giy lc v ct cht. 7/ t gi giy lc vo b soxhlet v trch ly bng 200ml n-hexan trong bnh cu y bng 250ml ( cn trng lng trc) 8/ Trch ly ton b soxhlet v hi lu trong 4 gi. 9/ Lm ngui v tho bnh cu, chng ct thu hi n- hexan n khi hu nh khng cn dung mi. 10/ Sy trong t sy 1 gi. Lm ngui v cn. 11/ Sy li trong na gi. Lm ngui v cn. 12/ Lp li trnh t 11 cho n khi chnh lch cc ln cn tip theo l 0.001g. 13/ Hm lng % du trong t thi l: Lng du thu c % du trong t thi (kh) l = Khi lng t thi kh 14/ Hm lng du trong t thi t l: Lng du trong t thi kh % Oil (SE) UD = 100 + M (SE) II/ Cch tnh du hp thu bi t lc: C mi 100kg t lc c a vo, n s hp thu: Oil (SE) UD (100 M (FE) ) = kg 100 M (SE) Oil (SE) UD Trong : - Oil (SE) UD = du trong t thi t - M (FE) = m trong t lc sch. 100 100

XC NH CH S X PHNG HA

AOCS Cd 3 - 25 in 1992 S dng 1992-12/01: 1992

Sa li 1995 Ph chun li 1993 S dng t 1/02:93 I/ nh ngha: Ch s x phng ha l s lng kim cn thit x phng ha cc thnh phn c trong cht bo. N c tnh theo s mg KOH dng x phng ha 1g cht bo. Phm vi p dng: Tiu chun ny dng xc nh ch s x phng ha cho du m ng vt v thc vt. II/Thit b: 1/ Bnh tam gic, dung tch 250 hoc 350, c lm bng thy tinh bn kim, c mi c quy cch 24/29 ( hoc 24/40). 2/ B sinh hn khng kh c chiu cao ti thiu 65 cm v c ch ni va kht vi bnh tam gic 1. 3/ Bp cch thy hay bp in c th iu chnh nhit . 4/ Bnh chng ct 2 lt, c mi c quy cch 24/29 ( hoc 24/40), dng hi lu v chng ct ethanol 95% nh ghi trong phn thuc th 2. III/ Thuc th: 1/ HCl 0.5N dung dch chun , phi pha tht chnh xc. 2/Alcoholic potassium hydroxide (KOH) c chun b nh sau: cho 5 -10 g KOH vin vo bnh chng ct 2 lt, k cho thm 1- 1.5 lt ethanol 95% vo bnh 2 lt v hi lu trong bp cch thy t 30 60 pht. Chng ct v thu hi ethanol cho vo bnh mu sch, c np y. Ha tan 40g KOH vi 1l ethanol va ct c v gi dung dch ny nhit 15oC. Dung dch phi trong. 3/ Phenolphtalein, dung dch 1.0% trong ethanol 95% Cch lm: 1/ Lm nng chy du nu du c v lc qua giy lc loi b tp cht v m, mu phi tht kh. 2/ Cn chnh xc khong 4 5g du vo bnh tam gic. Thm chnh xc 50ml alcoholic KOH (dng pipet) vo bnh tam gic). 3/ Lm nh vy i vi mu trng ( Mu khng c du). 4/ y bnh nn bng b sinh hn khng kh, ri t vo ni cch thy, hi lu lin tc khong 1 gi i vi mu thng thng. (c bit i vi mt vi mu kh x phng ha c th hi lu hn mt gi, iu ny ch xc nh cho cc th nghim). Phi chc chn rng vng hi trong b sinh hn khng dng cao n nh ca n, hoc khng xy ra vic mt hi. 5/ Sau bnh nn v ng sinh hn ngui nhng khng dng keo, ra bn trong b sinh hn bng mt lng nh nc ct. K , tho ng lm lnh ra , thm khong 1ml ch th Phenolphtalein v chun ngay vi HCl 0.5N cho n khi mu hng ca ch th bin mt. Ghi th tch ca dung dch chun HCl s dng. IV/ Cch tnh: (B S) N Ch s x phng ha = 56.1 W Trong : - B: th tch HCl 0.5N dng chun mu trng, ml - S: th tch HCl 0.5N dng chun mu du, ml - N: nng ng lng ca dung dch HCl - W: Khi lng ca mu du, g.

XC NH CHT KHNG X PHNG HA.AOCS Ca 6a-40

sa li 1971, 1972 Ph chun li 1989 Sa li :1992 Ph chun li 1993 S dng t T1/02:1993 I/ nh ngha: Cht khng x phng ha l tng hp cc cht c mt trong du hoc trong cht bo m khng b x phng ha bi kim nhng ha tan trong cc dung mi dng ha tan du hoc m. Cc cht khng x phng ha bao gm: cc alcohol bo, cn bo ha, cc cht mu v cc hydrocacbon c mch di. Phm vi p dng Dng cho tt c cc loi du m ng vt v thc vt thng thng. Phng php ny khng thch hp cho cc loi du m cha mt lng qu ln cht khng x phng ha nh i vi cc loi m c chit t cc loi ng vt bin. Phng php ny khng p dng cho cc loi feed grade fats. II/Thit b: 1/ Bnh chit tr c vch, vi np y thy tinh, dung tch 200ml, c th thay bng phu tch 500ml. 2/ Bnh tam gic hay bnh soxhlet ( bnh cu y bng), dung tch 100 200ml. 3/ Phu tch 500ml c np y. 4/ ng siphon thy tinh. III/Thuc th: 1/ Ethanol 95% 2/ KOH 60% v khi lng, c chun b nh sau: Ha tan 60g KOH trong 40ml nc ct v lm ngui. Lu : Lun lun cho vin KOH vo trong nc v khng c lm iu ngc li. 3/ Petrolerum erther (rt d chy) hoc n- hexan 4/ Dung dch NaOH 0.02 N, phi hiu chnh. 5/ Dung dch ch th phenolphtalein 1.0% phi hiu chun. IV/ Qui trnh thc hin 1/ Cn chnh xc khong 5g 0.1g du trn u cho vo bnh tam gic. Thm 30ml ethanol 95% v 5ml dung dch KOH 60%. un si nh nhng n nh trong h thng hi lu trong 1 gi trn bp cch thy n khi x phng ha hon ton. Vic x phng ha kt thc. 2/ Chuyn ton b hn hp vo phu chit hnh tr (hoc phu tch) v ra bnh nn n mc 40ml bng ethanol 95%. Sau ra tip bng nc ct m v k l nc ct ngui n khi tng dung tch 80ml. Ra bnh tam gic vi 5ml petroleum ether v chuyn vo phu tch. Lm lnh dung dch n nhit phng (20-25oC ) v sau thm 50 ml petroleum ether. 3/ y np, lc mnh t nht 1 pht v yn n khi tch r hai lp ( s dng ng siphon thy tinh ly phn pha trn hon ton nu c th v khng ln vo phn bn di, xem lu 1). 4/ Phn petroleum ether tch c tng hp vo trong phu tch 500ml. 5/ Lp li s chit trn ti thiu 6 ln, mi ln dng 50ml petroleum ether v phi lc mnh bnh chit.

6/ Ra li nhng phn chit trong phu tch 3 ln, mi ln dng 25ml ethanol 10% trong nc ct, lc mnh, loi b lp ethanol trong nc sau mi ln chit. Trnh loi b bt c phn no ca lp petroleum ether. Tip tc ra bng dung dch ehtanol 10% cho n khi dung dch ra khng cn mu hng i vi 1 git dung dch phenolphtalein 1% (xem lu 3). 7/ Chuyn phn petroleum ether thu c vo cc sch ( cn trc khi lng cc) v lm bay hi n kh trong t ht. Sau khi ton b dung mi bay hi ht, lm kh trong t sy nhit 75-80oC n khi lng khng i v p sut bn trong khng ln hn 200 mmHg. Lm lnh trong bnh ht m v cn. Kt qu l gi tr A trong cng thc tnh ton. 8/ Sau khi cn, cho thm 50ml ethanol 95% m (50oC) c ch th phenolphtalein v trung ha n im cui ca ch th phenolphtalein vo phn cn li. Chun vi NaOH 0.02N n khi mu im cui nh trn, phi hiu chun chnh xc nng NaOH 0.02N (xem lu 3) xc nh hm lng acid bo t do trong khi lng A, dng mi lin h sau: 1ml NaOH 0.02N th tng ng vi 0.0056g acid oleic. S gam acid bo xc nh bi s chun ny l B trong cng thc xc nh % cht khng x phng ha (xem lu 3). Phi lm mt mu trng tng t. 9/ Xc nh mu trng bng cch mu khng cho du hoc m, thc hin theo quy trnh nh trn. Kt qu mu trng l gi tr C trong cng thc. Tnh ton: A (B C) Cht khng x phng ha, % = x 100 W (g) A: khi lng phn cn li B: Khi lng acid bo, theo acid oleic,g C: Khi lng mu trng W: Khi lng mu, g S chnh xc: Khng c s liu thng k da trn nhng nghin cu hp tc vi phng php AOCS Ca 6a-40. Nhng gi tr sau y ch ra lch chun (SR) v phn trm lch chun tng i (RSD %) v lp li (R) thu c t 1985-1986. Cc kt qu ca chng trnh kim s nh mu xc nh cht khng x phng ha theo phng php AOCS Mu S ln phn S nm ngoi Gi tr cht lch Phn trm tch Outliers khng x chun SR lch chun phng ha RSD % % 1 49 2 0.37 0.128 34.23 2 51 3 0.36 0.097 27.25 3 47 0 0.38 0.108 29.13 4 47 2 0.40 0.088 22.06 5 47 2 0.39 0.075 19.48 Ghi ch: cn thn - Ethanol rt d chy, s dng t ht khi un nng hoc lm bay hi dung mi ny. - KOH ging nh tt c cc cht kim: d gy bng da, mt v h h hp, mang gng tay cao su v mt n che mt bo v khi lm vic vi dung

lp li R

0.36 0.28 0.31 0.25 0.21

dch kim m c. S dng thit b loi hi v khi bo v h h hp, trnh khi bi v hi kim. Khi lm vic vi kim mnh (KOH) lun lun cho KOH dng ht vo nc v khng lm ngc li. Cht kim ta nhit mnh khi ha tan vo nc. Do phi dng bnh cha chu nhit khi pha KOH trnh b b bnh cha. - Petroleum ether cc k d chy. Cn trnh gii hn n trong khng kh l 1-6%. Nn s dng t ht khi lm vic vi Petroleum ether Nhng im lu : 1/ C th s dng phu tch 500ml thay cho phu chit hnh tr, khi khng cn dng ng xiphong thy tnh. Nu s dng phu tch, tho lp nc bn di vo mt phu tch khc, gi li Petroleum ether trong phu th nht. Lp li s chit Petroleum ether trong pha nc nh bc th nm trong qui trnh. Tng hp Petroleum ether chit c vo phu tch th nht. 2/ C mt vi trng hp, s chit lp i lp li 7 ln vn cha . iu ny c xt on tt nht bng cch chit thm 1 ln na v lm bay hi ring phn ny nh bc 7 trong qui trnh. Phi khng c cht khng x phng ha trong phn chit ny. Nu c, ha tan phn ny bng mt lng nh Petroleum ether v cho vo phu chit th nht. Tip tc s chit n khi khng cn cht khng x phng ha trong phn chit sau cng. 3/ S chun chnh xc i vi cc cht acid bo t do c th chit c v nhng tp cht khng x phng ha c th chit c (c hai u qui v acid oleic) s c khuynh hng gia tng tnh th ca bn cht mu du.

XC NH HM LNG PHOTPHO

AOCS Cd 3 - 25 Thay th Ca12 -53 Xot xt 1988 Ph chun li 1993 S dng t 09/01

1/ nh ngha : Phng php ny xc nh hm lng photpho hay hm lng photphatit tng ng bng vic tro ha mu vi s c mt ca oxyt km (ZnO). Sau dng my quang ph o cng mu ca phc xanh Phosphomolybdic acid xc nh hm lng photpho 2/ Phm vi p dng: S dng i vi cc loi du th, du kh gum v du thc vt tinh ch. A/ THIT B: 1/ Chn nung hay tng ng, c kh nng chu ng c nhit trong l nung mc ti thiu 600oC, 50ml 2/ a petri, ng knh 75mm 3/ Bp in, c bin tr. 4/ L nung, c ha k v c kh nng iu chnh dung tr nhit trong khong 550- 600oC 5/ Phu lc thy tinh, cung ngn, ng knh 50mm 6/ Giy lc khng tn, ng knh 90mm Whatman No 42 hay tng ng 7/ Bnh tia 1 lt, s dng vi nc nng. 8/ Cc bnh nh mc 50, 100, 250 v 500ml c np y 9/ Cc pipet chuyn: 2, 5, 10 v 25 ml 10/ Pipet loi Mohr, 10ml vi vch chia 0.1ml

11/ My quang ph c cp theo AOCS 13-50, ti thiu c kh nng o hp th bc sng 650nm vi lp li 0.5%. 12/ Cell 1 0.005cm, s dng trong vng thy c ca dy quang ph. B/ CC THUC TH: 1/ Hydrochloric acid HCl m c, t trng 1.19 (xem cc ghi ch v khuyn co) 2/ Zino oxyt ZnO: thng mi hoc tinh khit. 3/ Potassium hydroxide KOH vin, loi tinh khit. 4/ Sulfuric acid H2SO4 m c, t trng 7.84 (xem cc ghi ch v khuyn co). 5/ Sodium molybdate Na2MoO4.2H2O loi tinh khit. 6/ NH2H2N.H2SO4 loi tinh khit 7/ Potassium dihydrogen phosphate KH2PO4 loi tinh khit, sy kh nhit o 101 C trong 2 gi trc khi s dng. C/ CC DUNG DCH. 1/ Sodium molybdrate: thm cn thn 14 ml H2SO4 vo 300ml nc ct. Lm ngui n nhit phng v thm 12.5g Na2MoO4. Pha long n 500ml vi nc ct, trn u v n nh dung dch t nht 24 gi trc kh s dng. 2/ Hydrazine sulphat 0.015%: Ha tan 0.150g NH2NH2H2SO4 trong mt lt nc ct. 3/ Potasslum hydroxide, dung dch 50%: Ha tan 50g KOH trong 50ml nc ct v lm ngui. 4/ Dung dch photphate chun: a) Dung dch tr chun : Chun b bng cch ha tan 1,0967g KH2PO4 c sy kh trong nc ct v pha long n vch ca bnh nh mc 2502ml. Dung dch ny cha 1mg photpho trn 1ml. b) Dung dch chun gc: Chun b bng cch dng pipet ly 5ml dung dch tr chun cho vo bnh nh mc 500ml v pha long n vch mc bng nc ct. Dung dch ny cha 0.01mg photpho trn 1ml. D/ QUI TRNH. 1/ Cn 3.0-3.2g mu chnh xc 0.001g vo chn nung. Thm 0.5g ZnO. 2/ Gia nhit t t trn bp in n khi mu tr nn sn st, k tng dn vic gia nhit cho n khi mu ha thnh tro hon ton. 3/ t chn nung vo l nung nhit 550-600oC v gi trong 2 gi. Ly ra v lm ngui n nhit phng. 4/ Thm 5ml nc ct v 5ml HCl m c vo tro trn. 5/ y chn nung bng a petri v gia nhit cho si nh trong 5 pht. 6/ Lc dung dch vo bnh nh mc 100ml. Ra bn trong a petri v cc mt ca chn nung vi khong 5ml nc ct nng, dng bnh tia c tia nc mn.Ra chn nung v giy lc thm 4 ln na, mi ln 5ml nc ct nng. 7/ Lm ngui dung dch n nhit phng v thm tng git dung dch KOH 50% trung ha dung dch n khi c nh. Thm tng git HCl m c cho n khi kt ta ZnO c ha tan, k thm d 2 git na. Pha long n vch mc bnh nh mc bng nc ct v trn u. 8/ Dng pipet ly 10ml dung dch ny cho vo bnh nh mc 50ml sch v kh. 9/ Thm 8ml dung dch Hydrazine sulfate ri thm 2ml dung dch Sodium molybdate

10/ y np v o ngc 3-4 ln. Ly np ra v gia nhit vi thi gian 10 0.5 pht trong b cch thy si mnh 11/ Ly ra khi b cch thy v lm ngui ti vch mc v trn u 12/ Chuyn dung dch vo cell sch v kh. o hp th 650 nm vi dng c iu chnh c hp th 0% ( truyn sut 100%) i vi cell cha nc ct. 13/ Chun b mu trng, khng c thm du, theo qui trnh c m t t 1-12 14/ o hm lng photpho ca mu v mu trng bng cch so sch vi ng cong chun , thu c nh sau: Chun b ng cong chun a) Dng pipet ht 0.0,1.0, 2.0, 4.0, 6.0 ,8.0 v 10.0ml dung dch chun gc vo cc bnh nh mc 50ml. Pha long mi bnh ti 10ml vi nc ct bng pipet khc vch. Tip tc nh qui trnh 9-12. Cc ch s tng ng ca cc dung dch l 0.0, 0.01, 0.02, 0.04, 0.06, 0.08 va 0.10 mg P b) V th biu din s hp th ca cc im chun theo hm lng photphp ca chng tnh theo mg trn giy k th. E/ TNH TON: 1 10( A B) %P

WxV

Trong : A: Hm lng photpho ca c s mu du tnh theo mg B: Hm lng photpho ca c s mu trng tnh theo mg W: Khi lng mu, tnh theo g V: Th tch ca dung dch ly trong mc 8 ca qui trnh. 2 % Photphatide tng ng = Px 30 F/ GHI CH: Khuyn co: 1/ HCl l mt acid rt mnh v c th gy chy d di. Phi mc o bo h khi lm vic vi acid ny. N c khi n hoc ht phi v gy kch thch mnh i vi mt v da. ngh khi lm th nghim vi HCl phi tin hnh trong t ht c. Khi pha long acid lun lun cho acid vo nc, khng bao gi c lm iu ngc li. 2/ KOH vin, nh tt c cc cc cht kim n da, c th gy phng da, mt v nh hng nghim trng n b my h hp. Mang bao tay cao su v mt n che mt bo v khi lm vic vi kim lng. S dng t ht c v mt n phng c bo v h thng h hp chng li tc dng ca hi v bi kim. Khi lm vic vi cc cht kim mnh nh KOH lun lun thm vin KOH vo nc v khng c lm iu ngc li. Cc cht kim thng ta nhit rt nhiu khi ha trn vi nc. Cn u phng i vi dng c cha dung dch kim v s ta nhit mnh c th gy b v dng c cha. 3/ H2SO4 m c l acid mnh v c th gy chy d di. Khi lm vic vi n cn phi mc qun o bo h. N l mt tc nhn gy oxi ha v khng c tn tr gn cc hp cht hu c. Cn ht sc cn thn khi ha trn vi nc v vic ta nhit tng nhanh bin thnh hi c th gy ra vic bn tung te acid ln. Lun lun cho acid vo nc, khng bao gi lm iu ngc li. 4/ NH2NH2H2SO4 c th gy kch thch mt, da v gy nguy him i vi gan, thn. Cht ny c bit l cht gy ung th i vi ng vt th nghim nh khi u trong phi v gan ca chut. N b nghi ng l gy ung th cho ngi. phng khi s dng cht ny ta phi dng gng tay, knh v khu trang bo v. Trnh ht

phi bt hay bi cht ny. Khi i cc cht thi hay dung dch thi c cha cht ny phi tun theo phng php thch hp v an ton. S ghi ch 1/ Nu hp th mu ca dung dch c o trong mc 12 ca quy trnh qu cao (> 0.9), ly c ca dung dch nh hn nh ghi trong mc 8 ca qui trnh, pha long ti 10ml bng nc ct, dng pipet v tip tc theo hng dn trong mc 9-12 ca qui trnh. 2/ Cc mu c hm lng phot pho cao c th vn thng cho hp thu > 0.9. i vi trng hp ny, dng pipet ly 10ml dung dch mu c chun b nh mc 7 ca qui trnh cho vo bnh nh mc 100ml v pha long n vch mc bng nc ct. Thc hin trnh t xut hin mu theo nh mc 8 - 12, dng mt kch c thch hp c pha long n 10 ml vi nc ct. Nhn hm lng photpho thu c, dng phng trnh trong mc tnh ton vi h s pha long (10 nu tun th qui trnh c m t trong on ny). 3/ Khng c s khc bit no gia vic m rng s so mu ca vic o hp ph trong mc 8 v mc 14 ca qui trnh. 4/ iu ny gn ng bin i % ca P sang % Photphotide trong du u nnh