CN PHN TCH Trung Tm o To V Pht Trin Sc K 9/25/2014 EDC - HCM 2
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I. GII THIU V CN 1) Cn : l phng tin o dng xc nh khi lng ca vt th thng qua tc ng ca trng trng ln vt th . Da theo cch thc hot ng, cn c phn thnh hai loi : a) Cn khng t ng l loi cn cn n s can thip ca ngi thao tc trong qu trnh cn. b) Cn t ng, v d : cn bng chuyn, cn ng gi sn phm.
2. Cc thng s k thut ca cn: Mc cn ln nht (Max. capacity) : l mc cn ln nht c th cn c khng tnh n kh nng b b ca cn. Mc cn nh nht (Min. capacity) : l gi tr ca ti m nu cn nh hn gi tr ny th kt qu cn c th mc sai s ln hn sai s cho php. Phm vi cn : l phm vi gia mc cn nh nht v mc cn ln nht. Mc ti an ton ln nht (Limit) : l mc ti c th cn m khng lm thay i cht lng v mt o lng ca cn. Gi tr chia nh nht (d) l : - Hiu s gia hai gi tr tng ng hai vch chia lin tip cn c c c cu ch th tng t - Hiu s gia hai gi tr ch th lin tc ch th hin s.
Gi tr chia kim (e) l gi tr th hin bng n v khi lng c dng phn cp v kim nh cn. S lng chia kim (n) l t s Mc cn ln nht / e . ng l kh nng phn ng ca cn i vi nhng bin ng nh ca ti trng. lp li l lch gia cc kt qu ca nhiu ln cn cng mt ti trng, khng c vt qu gi tr tuyt i ca sai s cho php ln nht ca cn ti mc ti . lch tm Khi ti trng c t ti cc v tr khc nhau trn bn cn th s ch th gia cc ln cn khng c sai bit vt qu sai s cho php ln nht ti mc ti .
3. Cp chnh xc ca cn: Theo T chc o lng hp php quc t OIML R76-1, cn khng t ng c phn lm 4 cp chnh xc : - Cp chnh xc c bit ( special accuracy ) I - Cp chnh xc cao ( high accuracy ) II - Cp chnh xc trung bnh ( medium accuracy ) III - Cp chnh xc thng ( ordinary accuracy ) IIII - Gi tr chia kim e, s lng chia kim n v gii hn cn nh nht (min) ca cc cp chnh xc nu trn c cho trong bng :
Cp chnh xc Gi tr phn chia kim e S lng chia kim n Gi tr cn nh nht Cp chnh xc I 0.001g e 50.000 khng hn ch 100d Cp chnh xc II 0,001 g e 0,05 g 0,1 g e 100 100 000 5 000 100 000 20 d 50 d Cp chnh xc III 0,1 g e 2 g 5 g e 100 10 000 500 10 000 20 d 20 d Cp chnh xc IIII
5 g e 100 1 000 10 d Cch xc nh gi tr chia kim e : Cn c thang chia c c cu ch th ph tr nh : con m, c cu c xen vo, c cu ch th ph, c cu ch th vi chia vi phn ( hin s v c s l sau u chm) th gi tr chia kim e c xc nh bi biu thc : d < e 10d e = 10 k kg vi k = 0, 1, 2 Yu cu ny khng p dng cho cc cn cp chnh xc I c d < 1 mg th e = 1 mg. Ngoi ra, nh sn xut c th chn e ph hp v ghi ln nhn cn.
4. Sai s cho php khi kim nh, hiu chun cn ban u:
Sai s cho php Ti trng m c th hin theo gi tr chia kim e Cp chnh xc I Cp chnh xc II Cp chnh xc III Cp chnh xc IIII 0.5e 0 m 50000 0 m 5000 0 m 500 0 m 50 1e 50000<m 200000 5000<m 20000 500<m 2000 50<m 200 1.5e 200000 < m 20000<m 100000 2000<m 10000 200<m 1000 Bi tp: 1) Mt cn phn tch 4 s l c d = 0.1mg, max = 220g. - Xc nh cp chnh xc ca cn. - Tnh gi tr cn nh nht ca cn - Tnh sai s cho php ln nht ca cn khi s dng mc cn 10g. - Tnh sai s tng i khi cn mc cn 0.1g, 5g, 20g. 2) Mt cn k thut, d = 0.001g, Max = 120g - Xc nh cp chnh xc ca cn - Xc nh gi tr cn nh nht - Tnh sai s ln nht ca cn khi s dng mc cn 50g. - Tnh sai s tng i khi cn mc cn 5g, 20g, 70g. II. HNG DN LP T, S DNG CN 1. V tr t cn: - Lung gi : Phi t cn v tr trnh ca s, ca va vo, ngi qua li v gn cc thit b cng tc khc nh qut, my iu ho... - Rung ng : Tt c cc loi cn, k c cn in t u chu nh hng ca rung ng. php o t n 0,01 g hoc nh hn th cn t cn trn bn cch ly rung ng - Loi bn vng chi ny thng c mt bn lm bng b tng hoc c chiu dy ti thiu 400 mm t c lp, tch bit khi tng nh v nhng thit b khc - Khng nn t bn cn trn nn g hoc treo di trn; cng khng nn t cn trn nn vi bn chng rung c n hi cao, v c th khi cn dn n nghing bn cn.
- Niv thng bng : Mt bn t cn phi c niv thng bng v chn cn cn phi iu chnh c n khi bt nc niv nm trong vng trn gii hn. - Bi : Cn phi c t ni sch s, khng c bi, nc v nhng ho cht, cht n mn, xng du, cht hu c khc. - Nhit : iu kin l tng l c c mi tr- ng n nh nhit trong phm vi 3 o C. - m : m cao dn n ngng t hi nc lm nh hng n hot ng ca cc chi tit c bit ca cc mch in t, dn n cn hot ng km tin cy - Can nhiu in t trng : Cn in t l i lng chu can nhiu ca in t trng
2. Kim tra cn: - Kim tra im 0: Hng ngy, hoc trc mi ln cn. - Kim tra mt im nht nh: thng kim tra im thng s dng (dng vt chun bit trc khi lng, hoc qu cn chun): kim tra hng ngy. - Kim tra lp li ti di o thng s dng: 6 thng/ln. - Hiu chun chu k: 1 nm hoc 3 nm/ln, ty chu k kim tra 3. S dng cn: - S dng ng gii o ca cn - Gi sch cn, lau bi, vt bm sau mi ln cn. - t nht mi ngy, sau khi s dng phi lau chi, v sinh cn. - Khng c cn khi lng gn bng max. - Trc khi cn phi kim tra Niv thng bng. III. Quy trnh hiu chun cn - Kim tra bn ngoi. - Kim tra o lng 1. PHNG TIN HIU CHUN : - Vic s dng qu cn chun phi tha mn nguyn tc chung sau y : cc qu cn chun dng hiu chun cn phi c sai s khng ln hn 1/3 sai s cho php ln nht ca cn ti mc cn kim tra. - S dng cc qu cn chun cp chnh xc E 2 hoc cp chnh xc F 1 kim nh cn cp chnh xc 1, cc qu cn chun cp chnh xc F 1 hoc cp chnh xc F 2 kim nh cc cn cp chnh xc 2.
2. IU KIN HIU CHUN : Khi tin hnh hiu chun phi m bo cc iu kin sau : - Phng hiu chun phi kh ro, sch s, khng b rung ng v gi la. Nhit nm trong khong gii hn nhit lm vic c nh sn xut qui nh. S thay i nhit trong phng (trong thi gian hiu chun) khng c vt qu gii hn 0,5 o C/h (i vi cn cp chnh xc 1) v 1 o C/h (i vi cn cp chnh xc 2). - nh hng ca tc ng bn ngoi (rung ng, in t trng, in p li, ) khng lm sai lch kt qu hiu chun. - Bn t cn phi vng chc, m bo cn khng b nh hng bi cc ngun rung ng. - Ni t cn phi sng, xa cc ngun sinh nhit v in t trng (l nung, t sy, bp, ), xa cc ngun sinh gi v rung ng (ca ra vo, ca s, my iu ha nhit , my ht m ).
3. CHUN B HIU CHUN : - Lm sch v tr t cn, bn trong v bn ngoi bung cn. - Lm sch bi bm trn cc c cu v cc chi tit ca cn. - Kim tra li ni-v, nu cn thit iu chnh li cho cn ngay ngn, cn bng. - Kim tra li nhit k t trong phng hiu chun. - M np cc hp qu cn chun. Qu cn chun phi cn trong thi hn hiu lc hiu chun. M cc bung cn ( lm ng u nhit gia khng gian bn ngoi v bn trong bung cn, gia cc qu cn chun dng hiu chun v cc chi tit ca cn). - Ty thuc vo tng loi cn c th, cn tun th cc cng vic chun b theo ng ch dn trong ti liu Hng dn s dng trc khi tin hnh hiu chun (v thi gian sy cn, v trnh t v phng php tin hnh hiu chun 4. TIN HNH HIU CHUN : 1. - Kim tra bn ngoi : phi kim tra theo cc yu cu sau y : - Kim tra tnh y ca cc c cu, cc cm chi tit trn cn. - Kim tra yu cu trn nhn hiu phi ghi ti thiu nhng t trng sau : + K hiu cn hoc c s sn xut (nh sn xut hoc nc sn xut). + Cp chnh xc. + Mc cn ln nht Max. + Gi tr chia nh nht d. + Gi tr chia kim e. + S cn. - Cc k hiu, s hiu trn nhn hiu cn phi r rng, khng c ty xa. 2. - Kim tra o lng : 2.1- Kim tra lp li : Vic kim tra lp li ca cn c thc hin bng cch tin hnh hai lot php cn tng ng vi hai mc cn bng 50% Max v Max (hoc gn vi Max). Mi lot bao gm 6 php cn, thc hin theo trnh t sau : - Quan st ch th ca cn lc khng ti. Nhn Tare tr v zero. - t mt qu cn chun hoc mt nhm cn chun c khi lng danh nh bng 50% Max ln gia a cn, ghi li gi tr ca cn lc c ti. Ly qu cn ra. - Ln lt tin hnh cc php cn lin tip nhau cho n khi hon thnh 6 ln cn. - Tip tc thc hin lot cn th hai mc cn Max (hoc gn Max) theo trnh t nh trn . - X l s liu : ly gi tr ca cn lc c ti ln nht tr gi tr nh nht ta c sai s gia cc ln cn lp li. So snh sai s vi sai s cho php. Tnh khng m bo o.
2.2- Kim tra ti trng lch tm : Vic kim tra sai s ca cn khi t cng mt ti trng ln cc v tr (cc gc) khc nhau ca a cn c thc hin mc cn bng (hoc gn bng) Max/3 theo trnh t sau : - Quan st ch th lc khng ti. Nhn Tare tr v zero. - t mt qu cn chun hoc mt nhm qu cn chun) c khi lng danh nh bng (hoc gn bng) Max/3 ln gia a cn. Ghi li gi tr ch th. - Tip tc thc hin chuyn tun t qu cn chun (hoc nhm qu cn chun) sang v tr (cc gc) khc nhau ca a cn theo chiu kim ng h. Ghi li cc gi tr ch th tng ng. - X l s liu : ly gi tr c c ti tng v tr tr i khi lng thc ca qu cn chun ta c sai s ca tng v tr cn. So snh vi sai s cho php.
2.3- Kim tra cc mc ti : Thc hin kim tra ti thiu 5 mc cn khc nhau, k c mc cn khng (trong phi c cc gi tr Max v cc gi tr ngay ti (hoc gn) im nhy bc ca sai s cho php theo c hai chiu : tng v gim ti. - Quan st ch th lc khng ti. Nhn Tare tr v zero. - Thc hin kim tra tng ti : t tng qu c khi lng t nh n ln c trong b qu cho n khi tng cc qu trn a cn bng (hoc gn bng) Max. Ghi li cc gi tr ch th. - Thc hin kim tra gim ti : ly tng qu c gi tr t ln ti nh (ngc li qu trnh tng ti) cho n khi khng cn qu cn no trn a cn. Ghi li cc gi tr khi gim ti (k c im zero). - X l s liu : ly gi tr ch th tr i gi tr ca cc qu cn chun ta c sai s ca hai qu trnh tng v gim ti. So snh vi sai s cho php.
KIM TRA HIU CHUN DNG C O TH TCH Trung Tm o To V Pht Trin Sc K I. c im ca dng c o th tch - Dung tch - Loi ra (Ex) hay vo (In). - chia: vch khc trn dng c o tng ng vi cc th tch c th. - Thi gian c (thi gian chuyn th tch), thi gian ch. - Cp chnh xc A/AS, B.
VI. Sai s phng tin o:
Dung sai (mL) Tn ph- ng tin o Gi tr thtch (mL) Cp chnh xc A Cp chnh xc B 1 0,008 0.015 2 0,01 0,02 5 0,015 0,03 10 0,02 0,04 20 0,03 0,06 25 0,03 0,06 50 0,05 0,1 Pipet bu 100 0,08 0,15
Dung sai (mL) Tn ph- ng tin o Gi tr thtch (mL) Cp chnh xc A Cp chnh xc B 1 0,006 0,01 2 0,01 0,02 5 0,03 0,05 10 0,05 0,10 Pipet chia 25 0,10 0,20
Dung sai (mL) Tn ph- ng tin o Gi tr thtch (mL) Cp chnh xc A Cp chnh xc B 1 0,01 0,02 2 0,01 0,02 5 0,01 0,02 10 0,02 0,05 25 0,03 0,05 50 0,05 0,1 Buret 100 0,1 0,2
Dung sai (mL) Tn ph- ng tin o Gi tr thtch (mL) Cp chnh xc A Cp chnh xc B 10 0,025 0,050 20 0,040 0,080 25 0,040 0,080 50 0,060 0,120 100 0,100 0,200 250 0,150 0,300 Bnh nh mc 1000 0,400 0,800
25 September 2014 28 SAI S PHNG TIN O TH TCH
Th tch ca 1 g nc Nhit (C) Th tch ca 1g nc (mL) Nhit (C) Th tch ca 1g nc (mL) 10 1,0013 21 1,0030 11 1,0014 22 1,0033 12 1,0015 23 1,0035 13 1,0016 24 1,0037 14 1,0018 25 1,0040 15 1,0019 26 1,0043 16 1,0021 27 1,0045 17 1,0022 28 1,0048 18 1,0024 29 1,0051 19 1,0026 30 1,0054 20 1,0028 II. Kim tra dng c th tch: Phng tin chun : - Cn phn tch cp chnh xc I - Nhit k thy tinh cht lng vch chia 0,5 o C - Nc ct
25 September 2014 30 HIU CHUN PHNG TIN O TH TCH
Cc bc hiu chun : 1. Chun b dng c o th tch 2. o nhit nc ct 3. Cn lng nc ct ly t dng c o th tch 4. Tnh th tch tng ng 5. Qui v th tch nhit chun 20 o C 6. Tnh sai lch so vi dung tch danh ngha 7. So snh vi sai s cho php LVN 68:2001 8. Kt lun v cp chnh xc A hay B Tnh th tch 20oC: Tnh th tch V ToC = Khi lng x th tch1g nc nhit Th tch 20 o C = V T (1 0.00002(T o C -20 o C)) = 0.00002/ o C: h s gin n nhit ca bnh thy tinh. So snh sai s vi sai s cho php theo o lng Vit Nam 68:2001 My o pH - Thit b quan trng o pH ca dung dch. - Dng nh phn acid, kim, chua trong nhng mu c mu sm khng th pht hin im tng ng bng ch th in cc pH - N l mt loi in cc thy tinh, gi l in cc mng chn lc ion H + - Thnh phn mng thy tinh ch yu l: + 72% SiO 2 22% Na 2 O 6% CaO Hoc + 80% SiO 2 10% Li 2 O 10% CaO - Loi thy tinh ny ch chn lc vi ION H +
in cc pH (cu to) - Bu thy tinh chn lc Ion H+ rt mng. - 2 in cc so snh Ag/AgCl, mt in cc so snh bn trong v mt in cc so snh bn ngoi - Dung dch KCl 3M - Trong bu thy tinh l HCl c nng c nh Nguyn tc hot ng ca my - o s chnh lch th gia trong v ngoi in cc. E do = a + bpH, a, b: l nhng hng s c xc nh bng thc nghim (Calib my). - T th o c, my chuyn v b phn x l s liu v tnh pH dung dch - Trng hp l tng: E do = a + 0.0592pH - 0.0592: h s l thuyt c tnh t phng trnh Nest. - Tuy nhin thc t: pH my o ph thuc vo nhit v nhiu yu t khc dn n h s b khng phi l hng s. - H s b c gi l h s gc (hay Slope) pH ph thuc vo nhit - Nhit thay i lm thay i slope. - pH mu v m cng s thay i. - S khng n nh c th xy ra do nhit bn trong v ngoi in cc kh cn bng. - Nhiu my hin ny c chc nay b nhit ATC, hiu chnh li slope khi nhit mu thay i lm gim sai s khi o mu. - im ng th l g???
Thao tc trn my pH khi o dung dch nc - Ly in cc ra khi dung dch bo qun. - Ra in cc bng nc ct, dng giy lau kh quanh in cc (khng lau bu thy tinh). - Calib my (pH 7, 4) hoc (7, 10) ty vo mi trng ca dung dch cn o. - Ra sch in cc bng nc ct, - Nhng in cc vo dung dch cn o sao cho bu thy tinh chm su trong dung dch, ch n nh v c kt qu pH. Nhng iu cn lu khi thao tc - Thao tc nh nhng, trnh va chm mnh in cc vo thnh cc o. - Khng c t bu thy tinh chm y cc - Khng khuy trn khi o - Khng dng giy lau kh bu thy tinh ca in cc. - Khng o nhng dung dch c tnh n mn thy tinh (HF, st m c) - Lun lun calib my trc khi o - Khong pH ti u 2 12. - c kt qu pH cng vi nhit .
Nhng iu cn lu vi in cc pH - Khi khng s dng phi ngm in cc trong dung dch bo qun (nu khng in cc b kh, lp hidrat ha (10nm) b hng). - Nu dung dch in li bn trong in cc b kh, phi ra sch in cc v np li dung dch in li. - Khi thy mng in cc b d nn lm sch bng cch: + Ngm in cc trrong dung dch thioure 7% trong HCl 0.1mol/L
+ Ngm vi gi trong pepsin 1% trong HCl 0.1mol/L. - Nu nhim bn cht hu c, nn ngm trong dung mi IsoPropanol. - Sau ra li bng nc ct - Ra phn bn trong bng dung dch in li, v thay dung dch in li mi. Khi o trong dung mi khc nc - Dung mi khc nc: oil, ethanol, methanol, acetonenhng dung mi ny lm cho kh nng p ng ca in cc thp v gy sai s khi o: + nhng dch ny c in tr ln dn thp nn chn in cc m bu thy tinh c in tr thp, hoc cho thm mt loi mui tr (nh mui amonium bc 4) tng dn ca dung dch
Khi o trong dung mi khc nc - Lm cho lp hydrat ha b hp th mnh bi nhng ion H+, dn n s trao i ion kh khn , H+ thm vo trong bu thy tinh lm pH khng n nh, v l nguyn nhn lm nhim cho mu nn ra in cc bng dung mi ha tan c mu, sau ra li bng dung mi d bay hi nh acetone, sau ngm vo mt dung dch m.
Khi o trong dung mi khc nc Khi do trong dung mi khc nc, th ni ln l nguyn nhn dn n kt qu c khng n nh, ngoi ra c th to huyn ph, nh gia dung dch in li v mu. - Thay dung dch in li bng: + methanol bo ha nc v KCl + Acid acetic bo ha KI + Acetone bo ha KI + Methanol bo ha LiCl - Sai khi thay th dung dch in li, nn cn bng qua m. - S thay i ny ch dng cho nhng loi in cc cho php thay i nh ROSS ULTRA cua Thermo. - pH trong dung mi v trong dung dch m khc nhau do khc nhau h s F, do o pH trong dung mi hu c ch c tnh tng i.