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第 3 章. 原子发射光谱法. A tomic E mission S pectroscopy For Short : AES. §3.1 概述 §3.2 基本原理 §3.3 原子发射光谱仪器 §3.4 发射光谱分析方法. §3.1 概述. 一、原子发射分析过程. 数据处理与显示. 单色器. 激发源 ( 光源 ). 检测器. 1 、试样蒸发、激发产生特征辐射; 2 、色散分光形成光谱(复合光 →单色光) ; 3 、检测谱线的波长和强度(定性和定量)。. 二、原子发射光谱法的特点.

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3

3

Atomic Emission Spectroscopy

For ShortAES


3

  • 3.1

  • 3.2

  • 3.3

  • 3.4


3

3.1

()

123


3

1. 70PSNFClBr

2

3

40.1~10g/g(g/mL)ICPng/mL

55%~10%ICP1%

6mgmg

71~2ICP4~6


3

1

(2

3


3

E3

E2

E1

hi

E0

3.2

.

(<10-8s)


3

.

1.

( n)

n =1 2 3 4 5 67

KLMNOPQ

(l)

l =01 2 3 4

spd f g

(ml)

ml=01 2 3l

(ms)

ms=1/2

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

(3s)1n =3l =0 m l =0 m s =+1/2


3

(L)

L = l ,

2L = (l1+ l2) (l1+ l2-1) (l1- l2)

2.

(n)

n =1 2 3 4 5 67

(S)

S = 012 3 ms(ms)

S = 1/23/2 5/2 ms(ms)

(M)M=2S+1

(J)

J = L+S L+S-1 L-S(LS)

J = S+L S+L-1 S-L(S >L)


3

.

n2S+1LJorn M LJ

1

  • n--L--

  • S-- M=2S+1,

  • J--

  • Na 5889.96 32S1/2----32P3/2

  • 5895.93 32S1/2----32P1/2

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


3

42F5/2 42F7/2

32D3/2 32D5/2

32P1/232P3/2

32S1/2

2

(1) nn0

(2) LL=1

(3) JJ=01J=0 J=0

(4) SS=0

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


3

3

--,

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


3

E3

E2

E1

E0

.

1.:

2.

3.

4.

()

M * M * (I)

(,) M+* M+ ()M2+* M2+ ()


N i n 0 g i g 0 e e i kt 1

Ei

E0

.

Ni = N0gi/g0 e-Ei/kT (1)

1.

N0NiBoltzmann:

gi g0 g=2J+1

Ei

kBoltzmann 1.3810-23JK-1

T K


3

Ai

i

Ii= Ni Ai hi2

0 i

  • 12 Ni = N0gi/g0 e-Ei/kT (1)

Ii = gi/g0 e-Ei/kTAihiN0

Ii =[A]C

-


3


3

2.

A.

I = I0e-adc

I0 ;

a ;

d

B.

rR

Ii =[A]C b


3

ICP

CID

3.3

.

()


3

.

1.():

2.

3.

4.

A. B. C.

D. ICP(Inductively Coupled Plasma)


3

:


3

A.

3800 K

4000~7000K


3

:

:


3

220V

50Hz

A

B.

6000~8000K

2.5~3KV

10KV


3

();

(6000~8000K)

()


3

C.

10000V

10~25KV


3

1

10000 -50000A/cm210000K

2

3


3

D. ICPInductively coupled plasma


3

0.1%

DCPICPMIP

ICP6070


3

Ar

Ar

Ar

1~2mmAr


3


3

Ar

Ar


3


3

ICP

1

10000K

2

10 -20mm6000 -8000K

3

6000K


3

ICP

ICP


3

  • 104K

  • ,10-3~10-5ppm

  • ICP1%

  • 1%

  • ppm

70


3


3

f

f

2.

1.


3

1.

:

n = A + B/2 + C/4

nABC

1

d/d

dl/d


3

A

N

i

C

B


3


3

  • 6560

  • dn /d

  • 400nm~800nm200nm~ 400nm

    dn /d


3

0.4nmmm0.8nmmm


3

2

R

R = /

bdn /d

R = / = bdn /d

R = / = mbdn /d

mbm


3

  • n

    3

    d/f)2

    d:f

    f dl/d


3

2

1

dsin sin= K

Kd


3

  • K=0=-

  • K0

  • K1 1= K2 2= K3 3=

    1= 600nm2= 300nm 3=200


3

2

:K = d(sinsin)

A

d/d=d/d= K/d cos

d/dK/d

=00~80cos=1~0.99:

200cos 1dKf


3

B. R

N

50.0 mm1200 /mm6000

R=1501200=6104

=/R =6000/60000 = 0.1


3

a

d

3

ad

= =

K=2dSin


3

. ()

d/dl<10/mm ;

d/dl10~20/mm

d/dl20~100/mm


3

1.


3

2.

(AgBr++)


3

i0

i

B. (S)

A(H) (E)

=S/ log H

()

i0

i

C(S)(H)

(S)(H)

0.4~1.8

:---

:Hi---

bc---

Hi---


3

3.

170~340nm

CSP etc

200~900nm


3

8~60


3

CID

SCD

CCD

ICP

CID


3 4 aes

3.4AES

.

1.

2~3

.


3

A

2.

  • (

  • 2~3


3

B.

20

  • 210~660nm4600

  • 65480


3

  • 1~10

  • ()( + 2+ 3+ )

  • 12.32712.347.3 2747.3


3

1~10

  • 1~2

  • 20

  • 2~3


3 aes

3. AES

1

2

35~6A6~20A

45~7m


3

-10.001%

-20.003%

-30.01%

-40.03%

-50.1%

-1

-2

.

1.


3

2.-

Pb %

0.001 2833.069,2614.1782802.00

0.0032833.069,2614.178,2802.00

0.01,2663.172873.32

0.03

0.10,

0.302393.8, 2577.26


3

.

-

I = aC b

1.

b=1 , b1,

a

2.

A.

  • -----


C 0 b 0 1

B.

C0b0=1

:

a1= a0


3

C.


3

2.

:

:

t1= t2

i1=i2, 1=2=

:


3


3

. AES

  • ()

  • :

  • 20m

NaClNaFLiF


3

log I

S

log C

logC

logR

logC

.AES

log I = b log C + log A

S =blogC+ log A

logR=log(I/ I)= blogC+log A


3

2. CL

1. S

.

XL = X B + KBL

XLX BK = 399.6%.,BL.:

CL ( CQ ) = KBL/S

S = (IL/IB)/C

:

C .:

CQ = KBL/S

K = 6

3.CQ


3

4. (RSD%)

5.


3

  • 1

  • 2~x%

  • 30.0x~0.x)

  • 4CrMnCuFeVTippm~x%)

  • 1

  • 2Y2O3

  • 3

400~800


3

  • P53 10111213141516


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