Báo Cáo TH C Hành TBPTTP

B CNG THNG TRNG I HC CNG NGHIP THC PHM KHOA CNG NGH THC PHM
BO CO THC HNH
Mn GVHD
: :
Thit b phn tch thc phm Nguyn Thanh Nam

Nhm 1
Nhm thc hin :
LP 04CDNKN2 Nin kha: 2011 2014 Tp.H Ch Minh
Trng i hc Cng nghip thc phm TP.HCM Khoa Cng ngh thc phm
Thit b phn tch thc phm
LI M U
Knh cho thy, y l bi bo co ghi li ton b cng vic v kin thc hc c trong mn Thit b phn tch thc phm ca Nhm 1 trong thi gian thc hnh qua. Nhm 1 cm n thy Nguyn Thanh Nam tn tnh ch dy chng em trong qu trnh hc tp v thc hnh, cn nhiu thiu st trong qu trnh hc cng nh trong qu trnh lm bo co nn mong thy b qua v cho chng em li nhn xt cng nh gp hon thin hn v mt kin thc trnh by trong bi bo co ny. Mt ln na xin cm n thy, chc thy nhiu sc khe v thm nhiu thnh cng trong cng vic ging dy.
Danh sch Nhm 1

H v tn Phng Thin Tm (NT) Nguyn Th Ngc Nhung L Th Hng Phng L Th Thu Phng Nguyn Th Kim Tho M s sinh vin 3305110568 3305110468 3305110516 3305110517 3305110616
GVHD Nguyn Thanh Nam 2
Nhm 1
BI 1: Gii thiu v cc thit b trong phng th nghim ---------------------------
Cn k thut
Cn phn tch
Nhm 1
L nung
My UV-Vis
Nhm 1
My AAS
My HPLC
Nhm 1
BI 2: Xc nh hm lng nitrit, nitrat trong mu rau bng phng php UV-Vis ------------2.1 Nguyn tc:
Trong mi trng acid (pH = 2) nitrit s b diazo ho acid sulphanilic, sau kt hp vi alpha naphthylamin cho hp cht naphathylamino azobenzen sulphonic c mu khng bn. Nitrat trong nc, sn phm tht v rau c cadimi kh thnh nitrit. nh gi nitrit trc v sau khi kh nitrat thnh nitrit th chng ta c th tnh ton hm lng nitrat bng php so snh gia nitrit trc v sau khi kh.
2.2 Thit b, dng c, ho cht:

Thit b: - My UV-Vis - Cn phn tch - Cn k thut - Bp in
Nhm 1
Dng c: - Bnh nh mc 50ml, 100ml, 250ml, 500ml, 1000ml - Cc thu tinh 50ml, 100ml, 200ml - ng ong 100ml - Chai l ng thuc th - Pipet 1ml, 2ml, 5ml, 10ml - Qu bp cao su - Bnh tia - Phu thu tinh Ho cht: - Dung dch nitrit chun 1000ppm - Dung dch sulphanilamin 0,2%. Cch pha: ho tan 2g sulphanilamin trong 800ml nc nng, lc, thm 100ml acid hydrochloric c, khuy k v pha long ti 1000ml vi nc ct (thuc th 1). - Dung dch N-1 naphthylethylen diamin dihydrochlorua 0,1%. Cch pha: ho tan 0,25g N-1 naphthylethylen diamin dihydrochlorua trong nc. Pha long ti 250ml vi nc ct. Bo qun trong l nu nt kn v gi trong t lnh (thuc th 2). - Dung dch acid HCL 44,5%. Cch pha: pha long 445ml acid hydrochloric c ti 1000ml vi nc (thuc th 3).
Nhm 1
- Dung dch chun gc natri nitrit nng 10000mg/l. Cch pha: ho tan 1g natri nitrit trong nc v pha long ti 100ml (thuc th 4). - Dung dch lm vic natri nitrit nng 50mg/l. Cch pha: pha long 5ml dung dch gc ti 1000ml vi nc (thuc th 5). - Dung dch dihydrogen dinatri ethylene diamine tetra acetat dihydrat 1%. Cch pha: ho tan 20ml acid hydrochloric c vi 500ml nc ct, thm 10g dihydrogen dinatri ethylene diamine tetra acetat dihydrat v 55ml dung dch aminiac c. Pha long ti 1000ml vi nc. Chnh pH = 9,6 9,7 (thuc th 6). - Cadimi kim loi (thuc th 7). - Giy lc
2.3 Cch tin hnh:

Chun b mu: Chit nitrat v nitrit t mu rau mung, ly 200g mu rau, ng nht mu bng cch dng dao xt nhuyn. Cn chnh xc khong 5g mu cho vo cc 200ml, thm vo 100ml nc ct un nng (>70oC). un trong ni cch thu si khong 30 pht chit nitrit v nitrat trong mu rau mung. ngui, cho vo bnh nh mc v nh mc ti vch bng nc ct. dung dch trong 30 pht sau cht cn thn lp cht lng trn, lc qua giy lc (khng c nitrit v nitrat), thu ly dch lc trong.
Nhm 1
Xy dng ng chun: Dung dch chun gc natri nitrit c nng 1000ppm nn pha long xung 10ppm. Ht 1ml dung dch chun gc natri nitrit c nng 1000ppm cho vo bnh nh mc 100ml v nh mc ti vch bng nc ct. Lc u v s dng dung dch ny xy dng ng chun nh sau. Ht ln lt 0; 1; 2; 3 v 5ml dung dch chun gc natri nitrit nng 10ppm cho vo 5 bnh nh mc 50ml, thm khong 25ml nc ct, 5ml thuc th 1 v 3ml thuc th 2 vo mi bnh. dung dch ny trong ch ti 5 pht. Tip theo thm 1ml thuc th 2 vo v lc u hn hp, vo ch ti 3 pht. Sau 3 pht ly ra v nh mc ti vch bng nc ct, nng nitrit ca cc dung dch ny s l 0; 0,2; 0,4; 0,6 v 1ppm, lc u hn hp v o hp thu bc sng 538nm. i vi mu nh lng nitrit: Ht 10ml dch lc t mu rau cho vo bnh nh mc 50ml. Thm vo khong 25ml nc ct, , 5ml thuc th 1 v 3ml thuc th 2 vo mi bnh. dung dch ny trong ch ti 5 pht. Tip theo thm 1ml thuc th 2 vo v lc u hn hp, vo ch ti 3 pht. Sau 3 pht ly ra v nh mc ti vch bng nc ct, lc u hn hp v o hp thu bc sng 538nm. Cn c vo ng chun dung dch o c c nng Cx (ppm).
Nhm 1
Bm Dd chun (ml) Dch mu (ml) TT1 (ml) TT3 (ml) TT2 (ml) C (ppm) Abs
1 0
2 1
3 2
4 3
5 5
mu 0
0 5 3 1 0 0
0 5 3 1 0,2 0,133
0 5 3 1 0,4 0,278
0 5 3 1 0,6 0,449
0 5 3 1 1 0,670
10 0 3 1 Cx Tb 3 ln o=0,010
i vi mu nh lng nitrat: Ht 5ml mu sau khi lc v khong 1g cadimi t cho vo bnh nh mc 100ml, cho cadimi vo bnh nh mc bng phu nh v s dng mt lng nh nc ct trng phu. Thm 25ml dch lc, y nt v lc u. Pha long ti vch bng nc ct, trn tht k hn hp v yn khong 10 pht cho cadimi lng. Ht 10ml ca dung dch ny ( x l vi cadimi kh nitrat thnh nitrit) cho vo bnh nh mc 50ml v to mu nh xc nh nitrit trn.
Nhm 1
Bm Dd chun (ml) Dch mu (ml) TT1 (ml) TT3 (ml) TT2 (ml) C (ppm) Abs
1 0
2 1
3 2
4 3
5 5
mu 0 10 ( x
l vi cadimi)
5 3 1 0 0
5 3 1 0,2 0,133
5 3 1 0,4 0,278
5 3 1 0,6 0,449
5 3 1 1 0,670
0 3 1 Cx Tb 3 ln o=0,014
V phng trnh hi qui tuyn tnh: T kt qu Abs o c v phng trnh hi qui tuyn tnh th hin mi tng quan gia nng v hp thu (quy trnh phn tch nitrit v nitrat theo nguyn tc phi s dng ring ng chun nhng do hn ch v thi gian v dng c nn s dng chung mt ng chun).
Nhm 1
Nitrit
0.8 0.7 0.6 0.5 Axis Title 0.4 0.3 0.2 0.1 0 0 1 2 3 Axis Title 4 5 6 y = 0.1365x + 0.0057 R = 0.9943
Nitrit Linear (Nitrit)
2.4 Tnh kt qu:

Cn c vo hp thu ca dung dch mu t ng chun, tnh ra nng nitrat v nitrit trong mu. Ta c Abs ca mu nitrit l 0,010 v phng trnh ng chun c dng vi R2 = 0.9943 t ta c th tnh c Cx ca mu bng cch th vo phng trnh ng chun: <=>
Nhm 1
<=> => Hm lng nitrit trong mu tnh theo cng thc sau:

Xnitrit (mg/ml) =
= 0.016 (mg/L)
Vi Cx : nng ca mu (ppm) Vbm : th tch bnh nh mc (ml) Vmu : th tch mu ht (ml) K : h s pha long 1000: n v mg/L nn phi chia 1000 i t ml => L i vi mu nitrit tng, ta c kt qu Abs l 0,014 v phng trnh ng chun c dng vi R2 = 0.9943 t ta c th tnh c Cx ca mu bng cch th vo phng trnh ng chun: <=>
Nhm 1
<=> => Hm lng nitrit tng trong mu sau khi kh nitrat tnh theo cng thc sau:

Xnitrit tng (mg/ml) =
= 0.0305 (mg/L)
Vi Cx : nng ca mu (ppm) Vbm : th tch bnh nh mc (ml) Vmu : th tch mu ht (ml) K : h s pha long 1000: n v mg/l nn phi chia 1000 i t ml => L Hm lng nitrat = nitrit tng nitrit = 0.0305 0.016 = 0.0145 (mg/ml)
2.5 Nhn xt:

R2 ca ng chun ng tin cy Cc kt qu c tin cy khng cao do qu trnh chun b mu v o hp thu c sai s.
Nhm 1
Dy chun nitrit
Nhm 1
BI 3: nh lng Fe bng phng php UV-Vis (mu rau mung) ------------3.1 Nguyn tc:
Fe(II) trong dung dch, kt hp vi 1,10-phenaltroline thnh mt phc cht mu cam bn trong mi trng pH 3-9. Nu mun mu ny khng b nh hng ca thuc th d v c mt ca cc ion khc, phn ng cn tin hnh pH 3,5-4,5. Phc cht ny gm 3 phn t 1,10-phenaltroline kt hp vi 1 ion Fe(II). Phn ng c hiu cho Fe(II) nn phi chuyn ht Fe(III) v Fe(II) bng cch kh vi hydroquinone hay hydroxylamine clohydic. 2NH2OH + 4Fe3+ N2O + 4Fe2+ + 4H+ + H2O

Thit b: - My UV-Vis - Cn phn tch - Cn k thut
Nhm 1
- Bp in - L nung - Chn nung Dng c: - Bnh nh mc 50ml, 100ml, 250ml, 500ml, 1000ml - Cc thu tinh 50ml, 100ml, 200ml - ng ong 100ml - Chai l ng thuc th - Pipet 1ml, 2ml, 5ml, 10ml - Qu bp cao su - Bnh tia - Phu thu tinh Ho cht: - Dung dch hydroxylamine clohydric 1% - Dung dch m pH 4,0 - Dung dch 1,10-phenalthroline 0,1% - Dung dch HCl tinh khit - Dung dch HCl 20% - Giy lc
Nhm 1
- Dung dch Fe2+ chun. Cch pha: pha long t dung dch Fe2+ 1000ppm xung 10ppm. Ht 1ml Fe2+ 1000pm cho vo bnh nh mc 100ml v nh mc ti vch.
3.3 Cch tin hnh

Chun b mu: ng nht mu v cn chnh xc 3g mu cn phn tch (cn 3,0208g rau mung x l bng dao nha), sau tin hnh v c ho trn bp in n khi than ho en, nung thnh tro trng nhit 500oC trong khong 2g gi. Ho tan tro bng nc ct, un cch thu mu bm trong chn nung c ly ra ht. Lm li ln th 2 v th 3 nh trn. Lc trn giy lc, ra nhiu ln cn, giy lc, chn nung v phu bng nc ct nng thu c ht lng mu. Dch lc v nc ra cho tt c vo bnh nh mc 100ml, thm nc ct ti vch v lc u. Xy dng ng chun: Dung dch Fe chun c nng 1000ppm nn pha long xung nng 10ppm d dng phn tch. Ht 1ml dung dch Fe chun 1000ppm cho vo bnh nh mc 100ml, nh mc ti vch sau lc u, ta c dung dch st chun 10ppm xy dng ng chun. Ht ln lt 0; 1; 2; 3 v 4ml dung dch Fe chun 10ppm vo cc bnh nh mc chun b sn. thm vo mi bnh 1ml hydroxylamine 10% v lc u, tip theo thm vo
Nhm 1
5ml m pH 5, 1ml 1,10-phenontroline 0.1% vo tng bnh, lc nh v yn trong 5 pht, sau dng nc ct nh mc ti vch ta c nng tng ng mi bnh l 0; 0.2; 0.4; 0.6 v 0.8ppm. Mang cc bnh nh mc o hp thu = 510nm. Bnh nh mc Fe(II) 10ppm Mu Hydroxylamin 10% m pH 5 1,10phenantroline 0,1% Nc ct C(ppm) Lc nh, sau 5 pht dng nc ct nh mc ti vch 0 0,2 0,4 0,6 0,8 Cx 1 1 1 1 1 1 mu 0 10 1 (lc 1 pht) 5
1 0 0 1 5
2 1 0 1 5
3 2 0 1 5
4 3 0 1 5
5 4 0 1 5
Sau 15 pht em o = 510nm Khng Abs 0 0,039 0,056 0,110 0,152 pht hin
Nhm 1
V phng trnh hi qui tuyn tnh: T kt qu Abs o c v phng trnh hi qui tuyn tnh th hin mi tng quan gia nng v hp thu.
3.4 Tnh kt qu:
Fe(II)
0.16 0.14 0.12 0.1 Axis Title 0.08 Fe(II) 0.06 0.04 0.02 0 0 -0.02 0.5 1 1.5 2 2.5 3 3.5 4 4.5 Axis Title Linear (Fe(II)) y = 0.0375x - 0.0036 R = 0.9785
Da vo Abs v phng trnh ng chun ta tnh c CFe(II) tuy nhin trong qu trnh o vi mu khng pht hin Fe(II) nn khng c kt qu c th. Nu c kt qu th tnh ton CFe(II) v sau tnh hm lng Fe(II) c trong mu.
Nhm 1
3.5 Nhn xt:

R2 khng ng tin cy Khng pht hin c Fe(II) c th l do li trong qu trnh chun b v x l mu.
Dy chun Fe(II)
Nhm 1
BI 4: nh lng Fe bng phng php UV-Vis (mu sa) ------------4.1 Nguyn tc:
Fe(II) trong dung dch, kt hp vi 1,10-phenaltroline thnh mt phc cht mu cam bn trong mi trng pH 3-9. Nu mun mu ny khng b nh hng ca thuc th d v c mt ca cc ion khc, phn ng cn tin hnh pH 3,5-4,5. Phc cht ny gm 3 phn t 1,10-phenaltroline kt hp vi 1 ion Fe(II). Phn ng c hiu cho Fe(II) nn phi chuyn ht Fe(III) v Fe(II) bng cch kh vi hydroquinone hay hydroxylamine clohydic. 2NH2OH + 4Fe3+ N2O + 4Fe2+ + 4H+ + H2O
Phm vi p dng: cho tt c cc loi thc phm.

Thit b: - My UV-Vis - Cn phn tch
Nhm 1
- Cn k thut - Bp in - L nung - Chn nung Dng c: - Bnh nh mc 50ml, 100ml, 250ml, 500ml, 1000ml - Cc thu tinh 50ml, 100ml, 200ml - ng ong 100ml - Chai l ng thuc th - Pipet 1ml, 2ml, 5ml, 10ml - Qu bp cao su - Bnh tia - Phu thu tinh Ho cht: - Dung dch hydroxylamine clohydric 1% - Dung dch m pH 4,0 - Dung dch 1,10-phenalthroline 0,1% - Dung dch HCl tinh khit - Dung dch HCl 20% - Giy lc
Nhm 1
- Dung dch Fe2+ chun. Cch pha: pha long t dung dch Fe2+ 1000ppm xung 10ppm. Ht 1ml Fe2+ 1000pm cho vo bnh nh mc 100ml v nh mc ti vch.
4.3 Cch tin hnh

Chun b mu: Cn mu sa c cn phn tch (cn 3.5020g sa c), sau tin hnh v c ho trn bp in n khi than ho en, nung thnh tro trng nhit 500oC trong khong 2g gi. Ho tan tro bng nc ct, un cch thu mu bm trong chn nung c ly ra ht. Lm li ln th 2 v th 3 nh trn. Lc trn giy lc, ra nhiu ln cn, giy lc, chn nung v phu bng nc ct nng thu c ht lng mu. Dch lc v nc ra cho tt c vo bnh nh mc 100ml, thm nc ct ti vch v lc u. Xy dng ng chun: Dung dch Fe chun c nng 1000ppm nn pha long xung nng 10ppm d dng phn tch. Ht 1ml dung dch Fe chun 1000ppm cho vo bnh nh mc 100ml, nh mc ti vch sau lc u, ta c dung dch st chun 10ppm xy dng ng chun. Ht ln lt 0; 1; 2; 3 v 4ml dung dch Fe chun 10ppm vo cc bnh nh mc chun b sn. thm vo mi bnh 1ml hydroxylamine 10% v lc u, tip theo thm vo 5ml m pH 5, 1ml 1,10-phenontroline 0.1% vo tng bnh, lc nh v
Nhm 1
yn trong 5 pht, sau dng nc ct nh mc ti vch ta c nng tng ng mi bnh l 0; 0.2; 0.4; 0.6 v 0.8ppm. Mang cc bnh nh mc o hp thu = 510nm. Bnh nh mc Fe(II) 10ppm Mu Hydroxylamin 10% m pH 5 1,10phenantroline 0,1% Nc ct C(ppm) Lc nh, sau 5 pht dng nc ct nh mc ti vch 0 0,2 0,4 0,6 0,8 Cx 1 1 1 1 1 1 mu 0 10 1 (lc 1 pht) 5
1 0 0 1 5
2 1 0 1 5
3 2 0 1 5
4 3 0 1 5
5 4 0 1 5
Sau 15 pht em o = 510nm Abs 0 0.029 0.061 0.087 0.124 Tb 3 ln o=0.018
Nhm 1
0.14 0.12 0.1 0.08 0.06 0.04 0.029 0.02 0 0 0 0.2 0.4 0.6 0.8 1 0.061 0.087 Fe(II) Linear (Fe(II)) Linear (Fe(II))
Fe(II)
y = 0.153x - 0.001 R = 0.9975 0.124
4.4 Tnh kt qu:

Cn c vo hp thu ca dung dch mu t ng chun, tnh ra nng Fe(II). Ta c Abs ca mu l 0,018 v phng trnh ng chun c dng vi R2 = 0.9975 t ta c th tnh c Cx ca mu bng cch th vo phng trnh ng chun: <=>
Nhm 1
<=> => Hm lng Fe(II) trong mu tnh theo cng thc sau:

XFe (mg/ml) =
= 0.0171 (mg/L)
Vi Cx : nng ca mu (ppm) Vbm : th tch bnh nh mc (ml) Vmu : th tch mu ht (ml) M : khi lng mu dng phn tch (g) K : h s pha long 1000: n v mg/l nn phi chia 1000 i t ml => L
4.5 Nhn xt:

R2 ng tin cy Cc kt qu c tin cy khng cao do qu trnh chun b mu v o hp thu c sai s.
Nhm 1
BI 5: Xc nh hm lng Fe bng phng php AAS (mu sa) -----------------5.1 Nguyn tc:
Hm lng Fe trong mu c xc nh bng k thut quang ph hp thu nguyn t ngn la.

Thit b: - My AAS Dng c: - Bnh nh mc 25ml. 50ml, 100ml - Cc thu tinh 50ml, 100ml, 200ml - Pipet vch 1ml, 2ml, 5ml, 10ml - Pipet bu 1ml, 2ml, 5ml, 10ml - Qu bp cao su - Bnh tia Ho cht:
Nhm 1
- Dung dch Fe chun 1000ppm - Nc ct 1 ln, 2 ln
5.3 Cch tin hnh:

Chun b mu: Cn mu sa c cn phn tch (cn 3.5020g sa c), sau tin hnh v c ho trn bp in n khi than ho en (khng cn khi), nung thnh tro trng nhit 500oC trong khong 2g gi. Ho tan tro bng nc ct, un cch thu mu bm trong chn nung c ly ra ht. Lm li ln th 2 v th 3 nh trn. Lc trn giy lc, ra nhiu ln cn, giy lc, chn nung v phu cng trng bng nc ct m thu c ht lng mu. Dch lc v nc ra cho tt c vo bnh nh mc 100ml, thm nc ct ti vch v lc u. Xy dng ng chun: T dung dch Fe chun 1000ppm pha dy chun c nng nh sau: 0; 0.2; 0.5; 1; 2; 5ppm. Nng 5ppm: - Ht 0.5ml (1000ppm) => bnh nh mc 50ml => 10ppm - Ht 25ml (10ppm) => bnh nh mc 50ml => 5ppm
Nhm 1
Nng 2ppm: - Ht 10ml (10ppm) => bnh nh mc 50ml => 2ppm Nng 1ppm: - Ht 5ml (10ppm) => bnh nh mc 50ml => 1ppm Nng 0.5ppm: - Ht 2.5ml (10ppm) => bnh nh mc 50ml => 0.5 ppm Nng 0.2ppm: - Ht 1ml (10ppm) => bnh nh mc 50ml => 0.2ppm Nng 0ppm: - Khng cn ht dung dch chun, nh mc ti vch bng nc ct. Sau khi pha xong dy chun c nng 0; 0.2; 0.5; 1; 2; 5ppm, chun b nc ct 2 ln v mang i o hp thu bng my AAS.
Nhm 1
Bnh nh mc (50ml) CFe (ppm) Ppm/ml
0 0 0
1 0.2 0.176
2 0.5
3 1
4 2
5 5
Mu Cx Khng pht hin Khng pht hin 62.6
0.514 1.061 2.077 4.853
Abs RSD (%)
0 0.13
0.007 4.2
0.021 0.044 0.085 0.197 1.9 1.37 0.17 0.05
Fe
0.25 y = 0.0395x + 0.0018 R = 0.9985
0.2
0.197
0.15 Fe 0.1 0.085 0.05 0.021 0.007 1 2 3 4 5 6 0.044 0 0 Linear (Fe)
Nhm 1
5.4 Tnh kt qu:

Da vo Abs v phng trnh ng chun ta tnh c Cx tuy nhin trong qu trnh o vi mu khng pht hin Fe nn khng c kt qu c th. Nu c kt qu th tnh ton Cx v sau tnh hm lng Fe c trong mu.
5.5 Nhn xt:

R2 ca ng chun ng tin cy. Khng pht hin c Fe(II) c th l do li trong qu trnh chun b, x l mu hoc pha long mu.
Dy chun Fe trong phng php AAS
Nhm 1
BI 6: Xc nh hm lng Acid benzoic bng phng php HPLC -----------------6.1 Nguyn tc:
Acid benzoic trong thc phm c chit v pha long bng nc ct, trong trng hp cn thit mu s c lm sch vi dung dch Carrezz. Acid Benzoic sau c xc nh bng phng php sc k lng hiu nng cao vi detector UV bc sng 226 nm.

Thit b: - My HPCL Dng c: - Bnh nh mc 25ml. 50ml, 100ml - Cc thu tinh 50ml, 100ml, 200ml - Pipet vch 1ml, 2ml, 5ml, 10ml - Pipet bu 1ml, 2ml, 5ml, 10ml - Qu bp cao su
Nhm 1
- Bnh tia Ho cht: - Acetonitile: loi dng cho HPLC. - H3PO4 0.05%: loi dng cho HPLC - Methanol: loi dng cho HPLC. - Dung dch Acid benzoic chun 1000ppm. - Nc ct 1 ln, 2 ln.
6.3 Cch tin hnh:

Chun b mu: Do hn ch v thi gian nn khng th chun b mu thc hnh phng php HPLC, gio vin hng dn cho thao tc bng dung dch chun vi mc ch lm quen v gii thiu v nguyn l hot ng cng nh cu to ca my HPLC. Xy dng ng chun: T dung dch Acid benzoic chun 1000ppm pha dy chun c nng nh sau: 0; 0.2; 0.5; 1; 2; 5ppm. Nng 5ppm: - Ht 0.5ml (1000ppm) => bnh nh mc 50ml => 10ppm
Nhm 1
- Ht 25ml (10ppm) => bnh nh mc 50ml => 5ppm Nng 2ppm: - Ht 10ml (10ppm) => bnh nh mc 50ml => 2ppm Nng 1ppm: - Ht 5ml (10ppm) => bnh nh mc 50ml => 1ppm Nng 0.5ppm: - Ht 2.5ml (10ppm) => bnh nh mc 50ml => 0.5 ppm Nng 0.2ppm: - Ht 1ml (10ppm) => bnh nh mc 50ml => 0.2ppm Nng 0ppm: - Khng cn ht dung dch chun, nh mc ti vch bng nc ct. Sau khi pha xong dy chun c nng 0; 0.2; 0.5; 1; 2; 5ppm, tim mu vo cc vial chun b sn chun b nc ct 2 ln v cc ha cht chuyn dng cho HPCL mang i phn tch = 226nm. iu kin chy my: - Ct: C18 (150mm 4,6mm 5m)
Nhm 1
- Pha ng: H3PO4 0.05% v Acetonitile (60:40) - Detector (u d PDA) = 226nm cho Acid benzoic - Tc dng: 1ml/pht (tc dng cao th dung dch s i nhanh v c th lm h ct) - Nhit ct: ~30oC - Th tch tim mu: 20l. - Thi gian chy mu: 6 pht Bnh nh mc 50ml Cbenzoic (ppm) mAbs Din tch peak % din tch peak 0 43.4170 62.3405 80.1054 87.7340 94.7879 0 178.73540 421.15576 790.15509 1709.01038 4067.13184 0 0 0.2 5.069 0.5 5.016 1 4.976 2 4.924 5 4.862 0 1 2 3 4 5
Nhm 1
V phng trnh hi qui tuyn tnh: T kt qu mAbs v din tch peak chy mu c, v phng trnh hi qui tuyn tnh th hin mi tng quan gia nng v din tch peak.
Acid benzoic
4500 4000 3500 3000 2500 2000 1500 1000 500 0 0 0 790.15509 421.15576 178.73540 1 2 3 4 5 6 1709.01038 Acid benzoic Linear (Acid benzoic) y = 814.66x + 13.102 R = 0.9995 4067.13184
6.4 Nguyn tc hot ng ca HPCL:

Tim mu vo cc vial sau t vo b phn ly mu t ng (auto simple), ci t cc thng s m h thng yu cu nh pha ng (H3PO4 0.05% v Acetonitile t l 60:40), Detector ( = 226nm cho Acid benzoic), tc dng (1ml/pht), nhit ct (~30oC), th tch tim mu (20l), thi gian chy mu (6 pht). Khi bt u chy mu, h thng t tim mu s gp vial n v tr ly mu, dng kim tim ht ly ng lng mu ci t v
Nhm 1
a sang pha ng, pha ng chun b sn H3PO4 0.05% v Acetonitile t l 60:40 c lc qua ray 0.25m, sau qua b loi kh chn khng v cui cng c bm cng vi mu qua ct v bt u qu trnh ra gii. Kt thc qu trnh phn tch dng nc ct v dung mi ra ct.
6.5 Nhn xt:

R2 ca mu ng tin cy. mAbstb mu 4 = 4.998 RSDmu 4 = 100%
Cc vial c tim mu
Nhm 1

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B CNG THNG TRNG I HC CNG NGHIP THC PHM KHOA CNG NGH THC PHM

Thit b phn tch thc phm Nguyn Thanh Nam

Nhm thc hin :

LP 04CDNKN2 Nin kha: 2011 2014 Tp.H Ch Minh

Thit b phn tch thc phm

Danh sch Nhm 1

GVHD Nguyn Thanh Nam 2

Thit b phn tch thc phm

BI 1: Gii thiu v cc thit b trong phng th nghim ---------------------------

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Thit b phn tch thc phm

Thit b phn tch thc phm

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Thit b phn tch thc phm

2.2 Thit b, dng c, ho cht:

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Thit b phn tch thc phm

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Thit b phn tch thc phm

2.3 Cch tin hnh:

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Thit b phn tch thc phm

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Thit b phn tch thc phm

Thit b phn tch thc phm

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Thit b phn tch thc phm

Nitrit Linear (Nitrit)

2.4 Tnh kt qu:

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Thit b phn tch thc phm

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Thit b phn tch thc phm

Xnitrit tng (mg/ml) =

2.5 Nhn xt:

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Thit b phn tch thc phm

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Thit b phn tch thc phm

3.2 Thit b, dng c, ho cht:

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Thit b phn tch thc phm

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Thit b phn tch thc phm

3.3 Cch tin hnh

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Thit b phn tch thc phm

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Thit b phn tch thc phm

3.4 Tnh kt qu:

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Thit b phn tch thc phm

3.5 Nhn xt:

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Thit b phn tch thc phm

Phm vi p dng: cho tt c cc loi thc phm.

4.2 Thit b, dng c, ho cht:

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Thit b phn tch thc phm

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Thit b phn tch thc phm

4.3 Cch tin hnh

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