HNG DN S DNG MT S THIT B CHNH

D n: PHNG TH NGHIM CP VIN KHOA HC V CNG NGH

VIT NAM, NGHIN CU V: SINH HC - NG LC HC BIN

H thng khi ph cm ngPlasma (ICP-MS)

Model: Agilent 7700 x ICPMS System
Hng sx:Agilent Nht Bn

Hng dn s dng phn mm

H thng khi ph cm ng-Plasma
Model: Agilent 7700 x ICP-MS System
Khi ng:
Khi ng phn mm ca my 7700 series ICP-MS:
- Nhp i chut vo biu tng ICP MS trn mn hnh
, hoc
- Chn ng dn Programs > ICP-MS Mass Hunter Workstation > ICP-MS Top
trong Windows Start menu.
Ca s ICP-MS c m ra:

Toolbar : Cc phm tt sau y c dng trong thanh cng c ca phn mm ICP-MS:

Chun b cho vic phn tch:

Cc ch sau y gip cho bn chun b cc cng c phn tch vi phn mm
my 7700 series ICP-MS.
Nhng iu cn kim tra trc khi phn tch:
H thng ph tr:
-

p sut kh Argon :500 n 700 kPa

Kh cell (Cell kh)(Helium): 90 n 130 kPa
Kh cell (Cell Kh) (Hydrogen): 20 n 60 kPa(options)
Qut ht kh
Nc gii nhit ( B lm lnh hoc b trao i nhit :on)
ng dn v bnh ra (not full) (rng)
ng bm peristaltic (ng bm nhu ng):
Mu, ng dn, v ng ni chun.

Chun b dung dch iu chnh:

Bn s cn cc tiu chun v dung dch cho s hot ng ca ICP/MS:
- iu chnh dung dch chun my (1ppb, Li, Co, Y,Ce, Tl).
- Ni dung tiu chun (dung dch ni chun P/A nu cn)
Pha long h s iu chnh dung dch P/A 75x, sau trn 2 dung dch vi t l 1:1 vi 1
h s iu chnh dung dich P/A cho s dng trong phng th nghim. H s iu chnh
PA c s dng t c s tuyn tnh trn detectors pluse v phng php tng
t. Pulse mode c s dng cho quantitable nng tng i thp (ppb). Phng
php tng t c s dng cho quantitable nng cao (ppm).
Bt ngn la Plasma chun b qu trinh phn tch
1 M Instrument Control panel mt trong cc cch sau y:
- Chn Instrument Control t the Instrument menu, hoc
- Nhp vo biu tng Instrument control

Chng trnh iu khin ICP-MS c m ra:

2 Xc nhn chng trnh ny l ch ch bng cch kim tra thanh tiu ca

bng iu khin chng trnh.
3 t chy trong plasma bng cch nhn vo biu tng Ignite Plasma
trong
thanh cng c.
4 Khi plasma trn ( ch hot ng) v chng trnh chy (chuyn) t ch
ch sang ch phn tch, kim tra hiu chnh nh m t trong phn sau:
Kim tra hiu chnh
Sau y l s cc b phn ca thit b ICP-MS. Bn c th tham kho v cc
thong s iu chnh trong phn ny.

M Tuning panel bng cch chn Turn trong Instrument menu, hoc nhn vo biu
tng Tune

trn thanh cng c ICP-Top.

Toolbar Cc mc sau y (phm tt) c sn trn bng Tuning toolbar:

Mo Xem Tuning 7700 trong tr gip trc tuyn cho () bit thm cc thng tin v cc
thng s hiu chnh.

Plasma Correction (Hiu chnh Plasma)

Thc hin chnh sa cc plasma cn thit l trong cc trng hp sau y:
Khi chng trnh c ci t. (Ci t chng trnh)
Khi my phun sng b thay i.
Khi qu trnh ly mu cone b thay i.
Khi torch c thay.
Khi mng li tolerance (khi dung sai ca ng nn) thay i sau khi chng trnh
s dng t 6 n 12 thng v cc th tc bo tr c tip tc (v cc th tc bo
tr vn c tun theo). Sau khi (mi ln) iu chnh plasma c thc hin, do
khng cn phi tin hnh iu chnh ln na trong cc trng hp khc, cung cp
chng trnh s dng o bnh thng.
Operating Method (phng thc hot ng)
Khi thc hin iu chnh plasma, s dng 1 pbb dung dch iu chnh c cha Ce (s
dng dung dch iu chnh Ce 1 ppb ). Sau y l gii thch cc phng php, tham
kho trong tr gip trc tuyn.

Settings for preset mode (ci t cho ch thit lp sn)

Chn loi my phun sng (nebulizer) v iu chnh, ci t ch thit lp sn.
Di ch thit lp sn, thng s nh RF power, v tr ly mu, tc dng kh mang, tc
dng kh b tr v tc bm nebulizer c c nh vi cc gi tr nh sn.
1. Trong ca s Tuning, chn Preset Plasma >> Select Plasma. Hp th thoi Plasma select
xut hin.
4

2. Kim tra hp Preset Mode.

3. Chn type of nebulizer s c s dng drop-down menu (cho 7700x).
4. Chn Robust hoc mt trong 3 mc ca Ultra Robust (cho 7700x). Chn Plasma (cho
7700s). Nu nng matrix vt qu 1%, chn Ultra Robust-Level : High (nu nhy
mong mun khng t c, chn mc Medium hoc Low).
5. Nhn OK.
Ca s Tuning s c kch hot.
Checking the tuning (kim tra s iu chnh)

Kim tra s iu chnh nh sau:

1. Kim tra mi thng s:
M tp tin cui cng c s dng ( thng l nogas.u, h2.u hoc he.u).
Chn Acquisition Parameters t Acd.Params menu. t s khi lng cn o nh 7(Li),
89(Y), 205(Tl) v 156/140 ( T l hnh thnh Ce oxid) v nhn OK.
Kim tra cc gi tr hin th sau trn ca s Tuning:

2. nhy mong mun khng t c, chon Autoturn t Tume menu. Tham kho
trong phn Help v thc hin Autotune.
3. Sau khi hon thnh autoturn, kim tra cc thng s nhy trn ca s v ICP-MS
Tuning-Sensitivity.
4. Lu tp tin iu chnh li bng cch chn Save t menu file. Ni chung, bn s
mun ghi ln file iu chnh m, n c gi tr cp nhp.
5. (Ty chn) To mt bo co iu chnh bng cch chn Generate Report t file
menu. Nhp kin ty chn nu mun v nhn OK. Mt bo co hin th cc thng
tin sau y c gi n my in:
- Sensitivity data (d liu v nhy)
- Resolution/Axis data (d kiu v s phn gii )
- Lens parmeter settings (ci t thng s thu knh)
Ty thuc vo cch ch ca bn c nh hnh, kt qu iu chnh cng s c
ghi li trong nht k bo tr.
Tip Bn cng c th c c mt bn in cc thng s iu chnh hin ti bng cch
nhp vo np Stop v chn Print t file menu.
Reference : vi 7700x
Cc ngh iu chnh gi tr tham s cho 7700x c hin th di y:

Reference : vi 7700s
Cc ngh iu chnh gi tr tham s cho 7700x c hin th di y:

Setting Quantitative Method parameters (Thit lp thng s phng php nh lng)

Cc ch sau y s gip bn to mt phng php thu thp phn tch dnh lng vi
Agilent 7700 Series ICP-MS MassHunter Workstation.
Set up a quantitative method (Thit lp phng php nh lng)
To mt phng php nh lng phn tch mi trng (cho mi trng phn tch) nh
m t di y:
1. Chn Edit Entire Method t Methods menu. iu ny bt u mt lot cc hp thoi
bn c th thit lp cc thng s cho phng php ca bn. Xem s gip trc tuyn
cho mt m t y cc mc trn cc hp thoi.
2. Trn hp thoi Edit method, nh du ty chn sau y, sau nhn OK.

3. Trn hp thoi Method information:

a. Nhp li bnh lun.
b. nh du hp kim tra d liu phn tch chy cc phn tch d liu t ng sau khi
thu thp d liu. c hng dn thit lp mt phng php phn tch d liu, xem
Open an existing batch for data analysis.
c. Nhn OK.
4. Trn loi mu chn ( hoc chn QC items, nu intelligent sequence phn mm c ci
dt) hp thoi:
7

a. nh hnh cc danh sch la chn QC items bn phi c CalStd v Sample duy nht.
b. Ty thuc vo phng php bn bt u, bn c th phi s dng Add > v <Remove
to cc danh sch mong mun.
c. Nhn OK.
5. Trn hp thoi interference equations:
a. Hin th can thip sa cha equations (phng trnh hiu chnh cn nhiu) mt trong cc
cch sau y:
- Chn Show All Masses hin th tt c cc phng trnh hiu chnh nhiu,
- T pull-down menu goc di bn phi mn hnh, chn th vin Interference equation,
hin th cc phng trnh sa cha can thit (hiu chnh cn nhiu)vo cc th vin
chn.
b. chnh sa phng trnh can thit cho mt khi lng:
- Nhn vo s khi lng mong mun trong danh sch.
- Nhn vo nt Edit m hp thoi Edit Equation.
- Chnh sa cc phng trnh nh m t trong tr gip trc tuyn v nhn OK ng
hp thoi Edit Equation.
c. Lp li bc 5b cho tt c khi lng m bn mong mun.
d. (optional) nhn vo nt Save trn hp thoi phng trnh can thit lu li phng
trnh chnh sa s dng vi cc phng php khc.
e. Khi hon thnh, nhn OK.
6. Trn hp thoi Acquisition Mode:
a. Kim tra ty chn Spectrum (Multi Tune).
b. Nhn OK. Multi Tune cho php bn s dng cc ch iu chnh khc nhau (ch
Hydrogen v Helium) cho cc yu t khc nhau trong mt ln chy n.
7. Xc nh khi lng v yu t phn tch nh sau:
a. Trn Spectrum (Multi Tune) thng s hp thoi thu nhn, nhn vo bng tun hon nh
hnh di y:

Sau s m hp thoi khi lng nh sau:

b. S dng bng 4 trang 18 nh hng dn, nhp chut chn khi

lng iu
chnh khi lng cho mi nguyn t. Khi lng c chn s xut hin trong hp thoi.
Nhp p vo mt nguyn t m hp thoi chn ng v. Nhn vo nt cho cc ng v
bn mun theo di. Kim tra bng cch nh du ng v c chn. xa mt ng
v, nhp chut phi. Nhn OK khi bn kt thc la chn ng v cho khi lng.
c. Lp li bc 7b thit lp cho mi khi lng nh th hin trong bng 4.
d. Khi bn hon tt, nhn vo np Mass Table. Hp thoi Mass Table m ra hin th
cho mi khi lng c iu chnh cho mi nguyn t. Kim tra xem chng c lit
k trong bng hp thoi khi lng ph hp vi nhng th hin trong bng 4 v iu
chnh nu cn thit. y l danh sch ca khi lng s c iu chnh trong phng
php.
e. Khi ci t xong cc yu t cn thit v khi lng, nhn OK trn bng khi lng v
hp thoi khi lng.
8. Thit lp Tune File v Stabilization time cho mi bc trong ch pha trn bn phi ca
Spectrum (Multi Tune) thu nhn thng s hp thoi.

9. Thit lp Integration time per Point cho mi khi lng:

a. Nhn vo hng cho khi lng trong ct cho cc bc thch hp (v d bc 1 cho ch
Hydrogen, bc 2 cho ch Helium) nh quy nh trong ct kh phn ng trong
bng 4 trang 18. Bn c th chn nhiu khi lng bng <Ctrl> + clicking trn chng.
b. Nhp Integration time per Point nh bng 4. Cc thi gian kt hp trong bng ni chung
l tng i ngn, v c th m rng khi cn thit.
c. Nhn nt Enter. Per point thi gian kt hp v tnh per Mass thi gian kt hp s c
cp nhp trong bng.
9

d. Lp li cho tng khi lng trong bng. i vi khi lng nh 71 m c iu

chnh hai bc, nh nhp thi gian kt hp cho c hai.
10. Thc hin cc lu chn b sung sau y trn Spectrum (Multi Tune) thu nhn thng s
hp thoi.
a. Chn Full Quant (3) cho Peak Pattern.
b. Ci t Repetition n 3.

c. nh du ty chn Return to First Tune Step di cng mn hnh, v nhn OK.

11. Trn hp thoi chng trnh bm peridtaltic, thit lp cc thng s sau y, sau nhn
OK. Xem tr gip trc tuyn cho bit thm thng tin v cc thng s ny va v cc tnh
ty chn: intelligent rinse v execute pre-emptive rinse.
- Before Acquisition
- After Acquisition (Rinse Port)
- After Acquisition (Rinse Vial)
12. (ty chn) thit lp pre-emptive rinsing nh sau:
a. Chn Set PeriPump Program t PeriPump menu trong ca s Acquistion.
b. Trn hp thoi chng trnh Peristaltic Pump, nh du ty chn Execute Pre-emptive
Rinse di cng mn hnh.
c. Nhp mt thi gian ban u l 15 giy, sau nhn OK.
d. iu chnh thi gian phn tch l 5 giy hon thnh trc khi dng dung dch ra n
nebulizer.
13. Lu phng php:
a. Trn hp thoi ty chn Method Save< nh du tt c im, v nhn OK.
b. Trn hp thoi Save Method As, nhp tn method, v nhn OK.
10

Access Method parameters directly

Bn c th truy cp mt s bng phng php trc tip, s dng mt trong cc menu items
sau:

11

Use the method wizard to create a method

Bng cch ny to ra mt phng php d dng to ra phng php phn tch mi
trng, v n cung cp rt nhiu thng s thch hp cho cc loi mu khc nhau v quy nh.
1. Chn Run Method Wizard t Methods menu trong ICP-MS top.
2. Nhp tn ca phng php v nhn nt Next >.
3. Chn mu nh sau:
a. Chn Environmental nh Application Type.
b. Chn Sampe, nh l Drinking Water hoc High TDS. M t v cc la chn hin
ti c hin th phn di ca s.
c. Chn Regulation, nh l EPA200.8 hoc EPA6020. Cc hng dn ch c p
dng cho cc mu c chn s c hin th.
d. Nhn nt Next>.
4. Danh sch ca khi lng v cc nguyn ts c theo di v hin th. Cc
thng tin trong danh sch ny da trn cc mu v cc quy nh chn trn.
Xem li thng tin nguyn t v thc hin bt c hiu chnh nh sau:
a. Nhp chut phi chn cc nguyn t quan tm trong danh sch thng tin nguyn
t.
b. Chn mt trong cc ty chn sau t bng phm tt:
- Add - xem bc 4c bn di
- Delete - tho ty chn khi lng t danh sch
- Edit - xem bc 4c bn di
c. Nu bn thm hoc chnh sa mt nguyn t, nhp cc thng tin sau y trn Add
(hay Edit) hp thoi Elements, sau dod nhn OK.
- Mass
- Element Name
- Integration time (see/point)
- Tune step number
d. (ty chn) nhn nt Edit/View Equation xem hoc chnh sa mt interference
correction equation. Xem tr gip trc tip bit thm thng tin.
e. Nhn nt Next.
5. Xem li thng tin phng php, sau nhn nt Finsh.
12

Bn c th hiu chnh phng php sau khi chn Edit Entire Method t Methods
menu v nh du cc phn ca phng php ny chnh sa, hoc t cc mc
menu c hin th trong phn trc.
Running the Samples
Nhng ch sau s gip bn chun b mt sequence, v chy mu vi my Agilents
7700 series ICP-MS MassHunter Workstation.
Set up the Sequence
Thit lp mt sequence phn tch nh sau:
1. Chn Edit Sample Log Table t Sequence menu trong phn
trn ca s ICP-MS. Mu m bn mun nhp vo s c tim theo th t lit k
trong bng.
2. Nhp cc thng tin sau y cho mu u tin ( hang 1) ca
bng:
a. Method: Nhp i chut trong ct Method ca dng 1 m
hp thoi chn phng php mong mun v nhp OK.
b. Type: Nhn vo ct Type ca hng 1 m danh sch cc
loi.
- Chn Calblk cho calibration.
- Chn CalStd cho calibration standards.
- Chn Sample cho unknown samples.
c. Vial: nhn vo trong ct vial ca dng 1 nhp s l ca
mu u tin hoc mu chun.
- Cc l ln ra c t 1, 2, v 3.
- Cc l nh c t ti 1001, 1002, 1003
d. Data file: li trng ny ch nh mt tn tp tin t
ng trong thi gian chy.
e. Sample: nhp tn ca mu trong ct Sample.
f. Comment: nhp li bnh cho mu trong ct Comment.
g. Dil/Lvl: Ch nh mt h s pha long hoc mc .
- For standard solutions: nhn vo ct Dil/Lvl ca hng 1 v
chn mc mong mun t danh sch.
- For samples: nhn vo ct Dil/Lvl ca hng 1 v nhp vo
cc h s pha long ( 1 cho khng pha loaanx), hoc nhp p m hp thoi tnh
ton h s pha long. Xem tr gip trc tuyn cho bit thm thng tin.
h. ISTD Cone: nhp p vo ct ISTD Cone ca hng 1 m
hp thoi thit lp ISTD Cone. Chn mc hiu chun mong mun, hoc thit lp
mt gi tr ISTD Cone, sau nhn OK.
3. in vo gi tr cc phn cn li ca mu nh sau:
a. Chn hng u tin v cc hng tip theo bng cch ko chut.
b. Kch chut phi vo trong nh du cc ng v chon Fill Down t phm tt
menu.
c. Cc gi tr ca Method, Type, Dil/Lvl v ISTD Cone c sao chp t hng 1 ti
cc hng trng. Dy s Vial c quy nh.
4. Sa cc thng tin cho cc hng Sample c thm vo trong bc 3 ph
hp vi phn tch ca bn.
5. (ty chn) tt plasma t ng cui dy, gn vo cc dng sau vo cui dy:
- Type: Keyword
- Data File: Standby
- Cc khc cn li trng.
6. ( ty chn) chn Import DA Method from Existing Batch kim tra hp nhp
mt phng php phn tch d liu hin c t hng lot th mc c th. Bn c th
13

nhp DA Method Only hoc DA method and Std Data. Bn cng c th p dng mt
phng php phn tch d liu sau khi thu thp d liu.
7. Nhn OK ng hp thoi Edit Sample Log Table.
8. Nu li c tm thy trong bng, tin nhn xut hin.
a. Nhn OK v cc phn vi phm s c nh du trong bng Fix.
b. Sa cc vn trong nh du.
9. Lp li bc 7 v 8 cho n khi khng cn li b pht hin.
10. (ty chn) chn Save t Sequence menu trong phn u ca s ICP-MS. Nhp
tn cho sequence m bn to ra, v nhn OK. Bn khng cn lu li sequence
chy n, nhng lm vy cho php bn m n sau ny v s dng n nh mt im
bt u cho php to mt senquence mi nhanh hn.
Analyze the samples (phn tch cc mu)
1. Chun b cc tiu chun sau y, cc mu, v mi dung mi
s dng phn tch. Cc dung mi bao gm HCl 0,5% cng nh acid nitric.
- B tr cc iu chnh tiu chun sau y bng cch pha long SPEX XSTC -760A
vi acid nitric xp x .1%. Nng cc dung dch khng b pha long l 100x l
tiu chun cht lng nc ung.

- Pha long mu vi acid nitric xp x .1%.

- Pha long dung dich ni chun (P/N 5188-6525) 200 ln ( i vi cc ng ni
chun).
- S dng acid nitric (1 n 5%) c khuyn khch cho cc dung dch lm sch, v
n s lm sch h thng a vo tt hn so vi nc tinh khit. Nu nc tinh khit
c s dng, b nh cn li c th c ra ra trong khi a mu c tnh acid, nh
hng n vic nh lng.
2. Chn Run t Sequence menu hoc nhn vo biu tng
trn thanh cng c
m hp thoi Start Sequence.
3. Thit lp thng s cc gi tr mong mun.
4. Data Batch Directory c thit lp tn duy nht da trn ngy hin ti v thi
gian. nh dang nm, ngy, thng, ngy, gi, v s th t. V d, 08H14K01.b l th
mc th hai to ra 10:00 11:00 ngy 14 thng 8 nm 2008. Cc phn trn c ngun
gc nh sau:
08 = 2008
H= thng 8 (thng- t A n L tng ng vi 12 thng, A= thng ging)
14 = cc ngy ca thng
K = cc gi trong ngy (A-X tng ng vi 0-23)
01 = mt s tun t cho cc trnh t chy trong cng mt gi, tc l 00, 01 ,02.
14

.B = phn m rng tp tin cho mt tp tin thc thi.

Nu bn mun, bn c th g th mc khc thay th. Tn c th n 8 k t. Cc th
mc s c to ra trong
C: \ICPMH\1\DATA\.
5. (ty chn) chn Import DA Method from Existing Batch kim tra hp nhp
mt phng php phn tch d liu hin c t hng lot thu mc d liu c th. Bn
c th nhp DA Method Only hoc DA method and Std Dt.
6. Nhn vo nt Edit DA Method pha di bn tri hp thoi, sau to ra mt
phng php phn tch d liu nh m t trang 28.
7. Nhn nt Run Sequence bt u chy. Hp thoi Run Sequence status xut
hin.

8. Nu mun, bn c th theo di vic thu nhn nh m t trong tr gip trc tuyn.

9. Khi sequence hon thnh, phn tch cc d liu nh m t sau y.
Quantitative Data Analysis (d liu phn tch nh lng)
Cc ch di y s gip bn thc hin phn tch d liu trn mu ca bn vi
Agilent 7700 Series ICP-MS MassHunter Workstation.
Typical scenarios for data analysis

Open an existing Batch for data analysis (m hng lot d liu phn tch)
15

Nu ca s cha c m, m ca s ICP-MS Data Analysis bng mt trong cac

cch sau y:
- Chn Main Panel t DataAnalysis menu trong phn u ca s ICP-MS hoc
- Nhn vo nt

trn thanh cng c ICP-MS.

Tip m mt lot hin hnh

a. Chn Open Analysis File t File menu m hp thoi hin hnh.
b. Chn tp tin quan tm v nhn Open. iu ny s m mt tp tin phn tch d
liu c lu trc .
c. Sau tin hnh Create the Data Analysis (DA) method for Quantitative data
analysis trn trang 28 to ra mt phn tch d liu (DA) phng php (nu
mt phng php DA khng c p dng ti thi im thu thp d liu)
hoc sa i cc phng thc, nu cn thit (nu cc phng php c p
dng DA).
Creating a new batch for data acquisition (to mt nhm mi cho thu thp d liu)
1. To mt lot th mc mi, s c s dng cha cc kt qu phn tch d liu
ca bn:
a. M hng lot hp thoi New Folder bng mt trong cc cch sau:
hoc
- Nhn vo nt thanh cng c New Batch Folder
- Chn New Batch Folder t File menu.
b. G tn cho th mc mi ( bn c th chn mt v tr khc nu mun).
c. Nhn vo nt Create.
2. Nhp cc mu nh sau:
a. Chn Import Samles t File menu.
b. Di chuyn n th mc tp tin d liu m cc tp tin d liu quan tm c t v
nhn vo nt Open. Cc tp tin d liu trong th mc c hin th trn hp thoi
Import Samples.
c. nhp mu khc t th mc, nhn nt Browse.
d. Lp li cc bc b v c cho n khi tt c cc mu quan tm c hin th trn
hp thoi Import Samples.
e. Chn cc mu nhp:
- <Ctrl>+click chn nhiu mu t danh sch lit k.
- Nhp vo nt Select All chn tt c cc mu trong danh sch.
f. Nhn OK.
Create the Data Anylasis (DA) method for quantitative dt analysis
1. M ca s Method Editor bng mt trong cc cch sau:
- Nhn vo nt thanh cng c Edit method
, hoc
- Chn Edit t Method menu.
Tip nhp phng php DA hin hnh, nhn Import Method only hoc Import
Method and Standard Dt v chn mt tp tin phn tch nhp.
2. Chn Dt Analysis Method t Method Task section 2 ( pha bn tri ca mn
hnh) hin th ca s phng php phn tch d liu.
3. Thit lp ty chn nh sau:
a. nh du vo kim tra FullQuantAnalysis.
b. Thit lp Analysis Mode Spectrum.
c. Chn phng php iu chnh t danh sch Interference Corection.
16

4. Chn Sample Template t danh sch

5. Chn Analyte List t Method Tasks section 3 hin th danh sch phn tch

17

 m analyte list t d liu c sn:

- Nhn nt
, hoc
- Nhp chut phi vo trong khung v chn Load lt from acquired data.
Tip Bn c th to analyte lt bng mt trong cc cch sau y:
- ti mt danh sch phn tch t mt phng php quan tm c trnh by,
nhn vo nt

- thm dng analyte mi, nhn nt

, sau ch nh bc Tune, Mass, Name
va Analyte/ISTD cho mi dng mi nh m t trong bc 6.
6. Nhp thng tin di ay cho mi analyte:
a. Nhn nt

cui bn phi ca ct Tune Step, v chn mt s bc iu chnh.

b. Nhn nt cui bn phi ca ct Analyte/ISTD v chn analyte hoc ISTD.

7. Chn Full Quant t Method Task mc 4 biu din bng Fullquant method table

18

8. Thit lp nhng thng s ca ng cong hiu chnh

Phng php ng cong hiu chnh (Hiu chnh ngoi chun/ hou chnh thm chun).
Phn loi nhng hiu chnh VIS cho nhng nguyn t ISTD.
Phn loi ng cong ph hp (tuyn tnh / phng trnh bc 2 / loi tr)
Cch th hin ca ngun gc (b qua / bt buc / b tr mu trng)
Tc ng ca ng hiu chnh
Nhng nguyn t ISTD c dng lm hiu chnh.
Nng ca mc ng cong hiu chnh (nng thp nht). Trong hu ht ng dng, nhp vo l
0.
n v nng
Nng ca mu trng
9. Nhng Advanced Info di trong method tasks c miu t thng qua h tr trc tuyn:
FullQuant outlier
Edit Report Templates
10. Chn Validate t mc 5 ca Method tasks. Sa cha nhng li ca phng php trc khi tin
hnh.
11. Chn Return to Batch at a Glance trong mc 5 ca Method tasks. Nhn YES lu phng
php.
QU TRNH VN HNH
1. Bc u chun b vn hnh, thc hin mt trong nhng thao tc sau:
Nhp chn biu tng Process Batch trn thanh cng c, hay
Vo menu Process chon mc Process Batch.
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Php phn tch mu c cho vo qu trnh vn hnh trong ti trc, dng thng s c
ci t trong DA method (d liu phn tch). Xem ti To d liu phn tch trong phn tch
nh lng Trang 28
2. Xem li kt qu phn tch c th hin trong bng Batch Table v nhng Calibration
Curve, nh v d sau y:

Ch : Nt Process Batch s hin th di mu en trong qu trnh vn hnh.

XEM KT QU PHN TCH
Bng Batch Table
1. Xem nng cng nh cch tnh tan cho mi nguyn t trong mu c trong bng
Batch Table.
Nng cng nh nhng cch tnh tan cho nhng s liu phc tp s c th hin mt
mu nn khc nhau trong nhng ct trong bng Batch Table
Xem nhng h tr trc tuyn c thm thng tin nu mun thay i cch th hin trnh
by d liu phn loi cc ct trong bng theo yu cu
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Ngoi ra xem h tr trc tuyn c thng tin nu mun thay i cch b tr hay lm vic
t ng.
Ph
2. Xem khi ph trong bng Spectrum pane. C th phng to xc nh nguyn t bng
cch nhp chut phi v ko chon tr chut quanh s ch khi lng mong mun. Xem h tr trc
tuyn c thm thng tin v cch khc biu din v x l s liu trong Spectrum pane nh:
ng tt cch biu din s liu theo ng log hay theo ng tuyn tnh
ng tt gia mt chui hay 3 chui
Thm li ch thch
Xc nh nhng ph khc vi d liu nguyn t
Loi tr ph nn
Che chn ph phc tp
Lp bng thng tin ca ph
Bng Calibration Curve
3. Xem ng hiu chnh i vi mi nguyn t trong mu bng Calibration Curve
Khi xy ra vn vi ng hiu chnh phong nn trong bng s hin mu hng.
Xem h tr trc tuyn c thm thng tin v nhng thay i i vi ng hiu chnh nh loi tr
cp ca ng hiu chnh, thay i nng ca ng hiu chnh, thay i loi ng hiu
chnh, thay i ch trnh by thuc tnh, thay i nhng yu t ph ca ng hiu chnh
Bng th n nh cho ISTD
4. Xem phn trm thu hi ca mi nguyn t ISTDtrong bng th n nh ISTD. Xem h tr trc
tuyn c thm thng tin
LU KT QU PHN TCH
Phi chc chn rng lun lu kt qu phn tch bng mt trong nhng cch sau:
i vi mt tp tin mi: chn Save Analysis File As trong mc File
Chp ln mt tp tin c sn vi cng tn:
Nhp vo nt Save trn thanh cng c, hay
Chn Save trong mc File
A RA BO CO
1. Chn Generate t trong mc Report trong ca s MassHunter ICP-MS Analysis
2. Ty chn nhng bo co mong mun v nhn OK (xem v d bn di)
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3. Nhn Ok a ra bo co.

PHN TCH BN NH LNG

Phn tch bn nh lng cho php qut v c c thng tin mt cch nhanh chng v nng cc
nguyn t c trong mt mu bt k. Voc ny rt c ch kh mun c thng tin v nng ca mt
lng cc nguyn t (>70 mu) m khng c s hiu chnh bn ngoi, nh khi chy u tin phn
tch cc nguyn t yu cu. c th ca php phn tch c chnh1 xc trong khang +/- 30% hay
c th tt hn trn nhng mu han ton khng c bit.
CHUN B CHO PHN TCH BN NH LNG
Chun b mu v cc dung dch sau y:
Mu phn tch (c pha long vi acid nitric 1%)
Dung dch iu chnh (Li, Co, Y, Ce, Tl c nng 1ppb, pha trong dung dch acid nitric 1%)
Dung dch lm sch (dung dch acid nitric 1-5%)
Create a semi Quant acquisition method:
1.

Chn Edit Entire Method t Method menu. iu ny bt u mt loi cc hp th,

bn c th thit lp cc thng s cho phng php ca bn. Xem tr gip trc tuyn
cho mt m t y cc mc trn cc hp thoi.

2.

Trn hp thoi Edit Method, nh du cc ty chn sau, sau nhn OK.

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3. Trn hp thoai thng tin phng php, thit lp cc thng s sau, sau nhn OK:
a. Nhp li bnh.
b. Chc rng hp Data Analysis c kim tra, y l iu cn thit chy chy t ng
d liu phn tch sau khi thu thp d liu.
4. Trn hp thoi mu cn chn ( hoc chn QC items, nu nh phn mm chy Sequence
c ci t), ci t cc thng s di y, sau nhn OK:
a. nh hnh danh sch Selected QC Items bn phi cha ng Sample, SQStd, SQBlk, v
SQISTD.
b. Ty thuc phng php m bn chy vi, bn phi s dng nt Add-> v Remove ci
t danh sch mun c.
5. Thit lp thng s phng php d liu thu thp c:
a. Trn hp thoi Acquisition Mode, nh du ty chn Spectrum v nhn OK.
b. Trn hp thoi Spectrum Acquisition Parameters, nhn nt Mass Scale.
c. Trn hp thoi Masses:
- Nhn nt Clear All.
- Chn ton b s khi lng bng cch nhp i chut trn, gia v cui hng, sau
nhn OK.
d. Chun b cc la chn b sung sau y trn hp thoi Spectrum Acquisition Parameters,
sau nhn OK:
- Chn Seml Quant (6) cho Peak Pattern.
- Dn dp ty chn Set every Mass, sau thit lp per Point Integration time t 0,05 hoc
0,1 giy.
- Thit lp Repetition m n 1.
e. Trn hp thoi Peristaltic Pump Program, ci t cc thng s sau, sau nhn OK.
- Before Acquisition: tc uptake: 0 rps, thi gian uptake: 0 giy, thi gian n nh: 70
giy.
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- After Acquisition ( Rinse Port): thi gian ra: 30 giy.

- After Acquisition ( Rinse Vial).
Xem tr gip trc tuyn bit thm thng tin cc thng s v trn ty chn c trng:
Intelligent Rinse v Execute Pre- Emptive Rinse.
6. lu phng php:
a.Trn hp thoi ty chn Method Save, nh du ton b cc mc, sau nhn OK.
b. Trn hp thoi ty chn Save Method As, nhp tn cho phng php, v nhn OK.
Phn tch mu
1. Trong bng sequence, thit lp sequence cho mu trong ch dn sau:
a. iu chnh dung dch ( 1 ppb Li, Co, Y, Ce, Tl)- Kiu mu SQStd
b. Mu trng ( nh l acid nitric) Kiu mu SQBlk
c. Mu 1 ->Mu 2 -> Mu 3 - Kiu mu Sample
2. Chy sequence:
a. Chn Run t bng Sequence hoc nhp biu tng

trn thanh cng c m hp

thoai Start Sequence.

b. Nhn nt Run Sequence bt u chy. Hp thoi ch tnh trng Run Sequence xut
hin.
c. Nu mun, bn c th theo di vic thu nhn d liu nh m t trong tr gip trc tuyn.
To mt l mi hoc m mt t mi cho d liu phn tch SQ.
To d liu phn tch (DA) phng php cho d liu phn tch Semiquant.
1. M ca s Method Editor bng mt trong cc cch sau:
- Nhn nt Edit Method trn thanh cng c

, hoc

- Nhn Edit t bng method.

Mo: nhp phng php DA hin ti, nhn Import Method only hoc Import Method and
Standard Data v chn mt tp tin phn tch nhp.
2. Chn Data Analysis Method t phn 2 Method Task ( pha bn tri ca mn hnh)
hin th ca s Data Analysis Method.
3. Thit lp cc ty chn nh hnh di y:
a. nh du vo hp kim tra cho SemiQuant Analysis.
b. Thit lp Analysis Mode cho Spectrum.
c. Chn iu chnh phng php t danh sch Interference Correction

24

4. chn Sample Template t danh sch

5. chn SemiQuant t phn 3 Method Tasks n hin th ca s SemiQuant.

Mo: Bn c th chn nguyn t hin th trong ca s bng cch nhn vo Add/Remove
Standard Element.

6. Trn ca s bng SemiQuant Method:

a. nh du hp kim tra cho Advanced Parameters.
b. Thit lp nng ca cc nguyn t c trong cc mu chun c s dng cho cc hiu
chnh h s SemiQuant.
c. Lu chn phng php hiu chnh ISTD.
i vi cc thit lp chi tit, tham kho SemiQuant Pane trong Commands Reference
ca tr gip trc tuyn.
25

7. Chn Validate t phn 5 Method Tasks. Sa li bt k phng php no trc khi tip
tc.
8.Chn Return to Batch-at-a-Glance t phn 5 Method Tasks. Nhn Yes lu d liu
phng php phn tch.
Nhm quy trnh:
1. Bt u x l bng mt trong cc cch sau y:
- Nhn nt Process Batch

trn thanh cng c, hoc

- Chn Process Batch t bng Process.

2. Xem/kim tra kt qu phn tch nh sau:
a. Batch Table pane: Hin th nng v tnh cho mi nguyn t trong cc mu.
b. Spectrum pane: Hin th khi ph. Bn c th phng to xc nh cc yu t bng cch
kch chut v ko con tr chut ln s khi lng mong mun.
c. Semiquant Factor pane: Hin th cc h s SemiQuant th cho mi mu. t con tr
gn mt im trn mt th hin th cc tn nguyn t v cc h s chi tit SemiQuant
chnh. S dng cc phm mi tn di chuyn gia cc mu. Nu cn thit, cc yu t c
th c thay i nh m t trong "Change the SemiQuant Factors". Nu cc h s khung
SemiQuant hin khng hin th, chn Calibration Curve t menu View.
d. ISTD Stability Graph pane: Hin th phn trm recovery ca tng nguyn t ISTD trong
cc mu. Xem tr gip trc tuyn bit thm chi tit.
3. Lu kt qu s dng Save Analysis As hoc Save t File menu.
4. Chn Generate t Report menu, chn report options, v nhn OK.
iu chnh cc h s Semiquant
1. Chn v o mu chun c cha ba hoc bn nguyn t m nng c bit n. Hy
chc chn rng cc nng ca cc nguyn t trong mu tiu chun tri ra t thp, trung
bnh, v cao ca khi ph, hoc s dng cc dung dch iu chnh c cha Li, Co, Y, Ce v
TI l mu chun.
2. Trong ca s ICM-MS Data Analysis, ti cc d liu cho cc mu chun vo cc th mc.
3. t kiu mu ca mu chun np SQStd nh trong v d di y:

4. Bt u x l bng mt trong cc cch sau y:

- Nhn nt Process Batch

trn thanh cng c, hoc

- Chn Process Batch t bng Process.

26

Cc h s SemiQuant cho tt c cc nguyn t s c iu chnh da trn cc nguyn t

c bit nng trong cc mu chun ( SQStd).
Thay i cc h s SemiQuant:
1. Chn SemiQuant Basic Parameters t Global drop-down menu trong ca s ICPAnalysis:

Cc thng s c bn hp thoai SemiQuant m ra:

2. Hy thay i bng cch:

- Kch chut phi trong bng v chn context menu, hoc
- Chn mt cell v trc tip chnh sa ni dung ca n.

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