The Quadrupole Ion Trap

Top endcap

Bottom Endcap

Ring Electrode

GC column inlet

Filament assembly

Ion Multiplier Detector

Quartz spacer

1

Phorate MW:260 diazinonMW:304 methyl parathionMW:263 fenitrothionMW:277phenthoate MW:320 ethion MW:384

chlorpyrifos MW:350 (EI) 2

13900GC

22000MS

38410I :II:1 2

1

2Ci/CsAi/As

g/Lg/L1400400260040031000400400

49

Nuclear Magnetic ResonanceFor ShortNMR

NMRNMRNMRNMRNMR

NMR--:, ,,1H, 13C, 19F

NMR--:I1/2

NMR--: Planck,

Spin State Energy Differencesvs. Magnetic Field Strength04.79.4EnergyMagnetic field strength, B0 (Tesla) E 200 MHzfor 1Ha spinstate E 400 MHzfor 1HHigh Field NMR increased sensitivity increased resolutionrandomlyoriented nuclei(no magnetic field)

NMR

1 :Chemical Shift Blocala bare nucleus (H+)feels the full effect ofthe external field (B0)electron density partiallyshields the nucleus fromB0 so it feels Blocal electrons generate aninduced field (Bi)which opposes B0 Bi

1 :Chemical Shift .

1H

2 I1/2n1I1/2nI1/2n1

ethylisopropylsinglet doublet triplet quartet pentet 1:1 1:2:1 1:3:3:1 1:4:6:4:1ethyl signature: quartet / tripletwith integration ratio of 2 / 3septet / doublet & 1 / 6 ratio

3 NMREthyl formate 1HNMRCH3CH2CH321321

NMR

400 MHz NMR Spectrometer400 MHz Avance System

400 MHz Superconducting Magnet magnetic field strength 9.4 Tesla (94,000 gauss)

400 MHz is the frequency usedfor proton detection in this fieldNMR sample tube and holderdescend into center of magnetKeep metal (ferromagnetic)objects, pacemakers, and credit cards several feet away!

NMR Sample Position(prior to release into probe)Liquid Helium-269C (4.2 K)Liquid Nitrogen-196C (77.4 K)NMR samplepositioned at top of probeSuperconducting magnetsrequire continuous cooling.

1 NMR,,,.

1 NMR,,.

1 NMR ro offej ij

2 NMRSample preparationPredefine parametersetsLockturn/marchshimAcquireProcessPrint

13

Atomic Emission SpectroscopyFor ShortAES

. (10-8s) 4.()M* M (I); (,) M* + M + () M*2+ M2+ ()

--, Na (1s)2(2s)2(2p)6(3s)1

.gi g0 Ei K Boltzmann T KAi K C 1. Ii =[ gi/g0 e-Ei/kTAihi (1-)k/ ] C: Ii =[ A] C

2. A. I = I0e-ad I0 ; a ; d B. rR Ii =[ A] C b

()

A. 2.5~3KV10KV4000~7000K ()B. ICPInductively coupled plasma

()A.

(AgBr++) 2AgX+2h Ag()+X2A. AgBr +Na2S2O3 NaAgS2O3 Na3Ag(S2O3)2 Na5Ag3(S2O3)4

A(H) (E)B. (S) i0 i C(S)(H) (S)(H) =S/ log H()

Hi---0.4~1.8:--- :Hi---

B. 170~340nm CSP etc200~900nmCICP-OES

AES1.()2~3

A2~32.()

(%)CSe1~10-1AsGeIrOsSmTeThUW10-1~ 10-2AuBBiCoDyErEuHgGdHoLaMnMoNb PPbPrPtRbRnRuSSbSnSiTaTbTiTlVZnZr10-2~ 10-3AlCdCrCsFFeGaGeInMgNiPbScYYb 10-3~ 10-4AgBeCuBaSrCa10-4~ 10-5CsKLiNaRb10-5~ 10-6

1~10()( + 2+ 3+ )12.32712.347.3 2747.3B.2300~3500/1580/68480

D. C. 1~101~28W-202~3

12345678910 %1010~33~11~0.30.3~0.10.1~0.030.03~0.010.01~0.0030.003~0.0010.001

3. I = AC bH = I t 2.

b=1 , b1, I = AC b () log I = b log C + log AA: gi/g0 e-Ei/kT(1-)k/ AihiA4.

B. ICPInductively coupled plasma2outer tube5. Plasma6atomization zone7atomic line emission8ionic line emission1: induction coil 3intermediate tube4sample injectorICP-OESInductively Coupled Plasma Optical Emission Spectroscopy

,10-3~10-5ppmICP1%1%ppm 104K70

B.

ICP-OESICP-OESInductively Coupled Plasma Optical Emission Spectroscopy ICPCIDSCDCCDCID3.5 3.5 cm2512 512