ion chromatography technologyƒ訪.pdf · 2015-12-19 · semi amc tf2...

SEMI AMC TF2 微污染防治專案為提升國內微污染量測之技術水平，特舉辦離子層析儀之原理教學與儀器參訪活動，邀請 AMC TF2 成員參加，期盼讓 SEMI 會員對於離子層析技術於微汙染防治之儀器功能及未來之應用有進一步的認識。以實作參訪及教學模式，使SEMI會員深刻瞭解離子層析技術之概念與原理，並於活動中結合產業專家，進行研討，提出未來應用與發展方向之建議。

【參訪日期】中華民國103年12月11日(星期四) 下午1:30 ~ 3:30 【報名日期】103年12月4日至 103年12月10日止【主辦單位】SEMI Taiwan 高科技廠房設施委員會奈米微污染控制工作小組【協辦單位】台灣賽默飛世爾科技股份有限公司【報名方式】本參訪活動由郭啟文先生負責報名信箱 : [email protected] / 0988-935-753

Ion Chromatography

Introduction & New Technology

台灣賽默飛世爾科技股份有限公司

3

Eluted slowly

Eluted with middle speed

Eluted quicklyEluent(移動相)

CHROMATOGRAPHY

固定相

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Temporal

course

Mechanism of Ion Exchange Separation

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5 Proprietary & Confidential

Example of Anion Measurement

0 2 4 6 8 10 12 14 16

Retention time(min)

0

8

mS

F-

NO3- SO4

2-Cl-

NO2-

Br- HPO42-

6

Example of Cation Measurement

Retention time (min)

0 2 4 6 8 10 12 14

0

1

2

3

4

Na+NH4

+K+

Mg2+ Ca2+µS

7

Basic Flow diagram of IC

Eluent

Pump

Column

Detector

Pumping Separation Detection Recording

F-

NO3- SO4

2-

Cl-

NO2-

Br-

HPO42-

Sample injection valve

Suppressor

Detection cell

Injection


RFIC- EG

Data

Manageme

nt

* No external eluent

No external regenerant

Conductivity

Detector

High-Pressure

Non-Metallic Pump

Eluent Generator

(OH– or H+)

Waste

Sample Inject

(Autosampler) Recycle

Mode

Suppressor

Detection

H20


Samplingpump

（stop）

AnalysisInjection Position

Samplingpump

（pumping）

ConcentrationLoad Position

Waste

Conc.

column

Samplingpump

（start）

Eluent

To separatepart

EquilibriumInjection Position

Injection Valve

IC – Concentrator design


Superficial Anion Exchanger

CH2

CH

CH CH2

CH2

CH2

CH

CH2

CH2

CH CH2

CH CH2

CH CH3

CHCH2

CH

(CH3)3NCH

2+Cl- (CH

3)3NCH

2+Cl-

(CH3)3NCH

2+Cl- (CH

3)3NCH

2+Cl-

Functional Group

DVB Crosslink


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Ion Exchange Resin (樹脂Latex type）

５μm

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Ion Exchange Resin (接枝Grafted type)


1°Amines

R-NH2

2°Amines

R’

R-N-H

4°Amines

R4N+

Functional Groups Detected with Suppressed Conductivity

3°Amines

R’

R-N-R”

Suppressed Conductivity Detection

InorganicAnions

e.g., F_, CI

_,

NO2

_, NO3

_,

SO42_

,

PO43_

, I_,

Br_, CIO3

_,

SCN_,

S2 O3 2_

InorganicCations

Alkali Metals:

Li+, Na+, K+,

Rb+, Cs+,

Alkaline Earths:

Mg2+, Ca2+

Sr2+, Ba22+ ,

Ammonia:NH4

+

Carboxylic

R-C-OH

PhosphatesO

R-O-P-OH

OH

Sulfates

R-O-S-OHO O

O

Sulfonates

R-S-OH

O

O

Phosphonates

R-P-OH

O

OH


Role of Suppressor

Waste

Back Ground： Na2CO3 / NaHCO3

(700μS)

NaF,NaCl,NaNO3Na2HPO4,Na2SO4

～～

Retention time

Conductivity

NaF NaCl NaNO3

Na2HPO4

Na2SO4

Back Ground： Na2CO3 / NaHCO3

(700μS)～～

Retention time

Conductivity

HF HCl

HNO3H3PO4

H2SO4

Retention time

Back Ground： H2CO3 (15μS)

Conductivity


抑制作用

Increase the conductivity of analytes：

Raise sensitivity

陰離子 Na+/ K+, Cl- H+, Cl-

陽離子 Na+, Cl- /SO42- OH-, Na+

Decrease the conductivity of BG (Eluent) :

Reduce noise

Na+, HCO3- H2CO3 (Carbonate系統)

(Hydroxide系統)Na+, OH- H2O

MSA-, H+ H2O陽離子

陰離子


Microbore 2-mm - Ammonium

10 mL preconcentration volume,

CS12A


Microbore 2-mm - Anion

0.0 2.0 4.0 6.0 8.0 10.0 12.0 14.0 16.0 18.0

-0.050

0.100

0.200

0.300

1 - Autoprep AS17,2mm #1 1 ppt ECD_1

2 - Autoprep AS17,2mm #2 5 ppt ECD_1

3 - Autoprep AS17,2mm #3 10 ppt ECD_1¥ìS

min

321

20 mL preconcentration volume, AS17 with

CRD

Produced by: Dionex Korea Application Lab

Fluoride

Chloirde

Nitrite

Bromide

Nitrate

Sulfate

Phosphate


18

New Technology - Capillary HPIC

Dedicated High Pressure IC

The benefits of speed

without compromising resolution;

24/7 uptime of Capillary IC

and detection choices

in a compact, integrated system


Sensitivity

Column ID Flow rate Sensitivity

1.0 mL/min S/N = 1

0.4 mm 10 µL/min S/N = 100

S/N = 1 S/N = 100

4.0 mm


Sensitivity

-2.0

16.01

LithiumSodium

Ammonia

PotassiumMagnesium

Calcium

-2.0

16.0

0.0 2.0 4.0 6.0 8.0 10.0 12.0 15.0

-2.0

16.0

Capillary IC with 0.4 µL Injection

Volume

Co

nd

uctivity [µ

S]

Retention Time [min]

Microbore IC with 0.4 µL

Injection Volume

Standard bore IC with 0.4 µL

Injection Volume

LithiumSodium

Ammonia

PotassiumMagnesium

Calcium

LithiumSodium

Ammonia

PotassiumMagnesium

Calcium

0.4 mm

2 mm

4 mm

All with same injection volume


I o n C h r o m a t o g r a p h y R e a g e n t - F r e e I C C a p i l l a r y I C C h r o m e l e o n D a t a S y s t e m

SEM Image of 4 µm Supermacroporous Bead

High Resolution using the

Dionex IonPac AS11-HC-4µm

High Resolution using the

Dionex IonPac CS19-4µm

Fast Run using the

Dionex IonPac AS18-4µm

0 401

10

Minutes

µS

0 3-0.5

5.5

µS

Minutes 0 400

5

µS

Minutes

New High Efficiency Dionex IonPac 4µm Capillary IC Columns

Improved Resolution Provides Faster Runs and Better Results

Ion-exchange columns with 4 µm particle-size

Benefits• Smaller particles provide better performance

• Faster run times with higher flow rates using 150 mm columns

• Better resolution with standard flow rates using250 mm columns

Applications• Anions in environmental waters

• Organic acids in foodsand beverages

• Amines in chemical process solutions


Separation of Inorganic Anions using the Dionex IonPac AS18-4µm Column at Different Flow Rates

Column: Dionex IonPac AG18-4µm/AS18-

4µm, (0.4 x 150 mm)

Eluent Source: Dionex KOH Capillary Cartridge

Eluent: 30 mM

Col. Temp.: 30 °C

Inj. Volume: 0.4 µL

Detection: Suppressed Conductivity, Dionex

ACES 300

Peaks: 1. Fluoride 0.2 mg/L

2. Chloride 1

3. Nitrite 1

4. Sulfate 1

5. Bromide 1

6. Nitrate 1

7. Phosphate 2

10

µS

-15

20

Minutes

5

10 µL/min, 1508 psi



2

1

43

5 6

7


Speed

Column: Thermo Scientific Dionex

IonPac AS18-4 µm, 0.4 × 150 mm

Eluent Source: Dionex EGC-KOH (Capillary)

Eluent: 30 mM KOH

Col. Temp.: 30 °C

Inj. Volume: 0.4 µL

Detection: Suppressed Conductivity, Thermo

Scientific Dionex ACES 300

Sample: Anion Standard Solution

mg/L

Peaks: 1. Fluoride 0.2

2. Chloride 1

3. Nitrite 1

4. Sulfate 1

5. Bromide 1

6. Nitrate 1

7. Phosphate 2


10

µS

-15

20

Minutes5





Separation of inorganic anions using a 4 µm column at different flow rates.

Faster run times without sacrificing resolution

ion chromatography technologyƒ訪.pdf · 2015-12-19 · semi amc tf2...

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