6820 GC 氣相層析儀教育訓練

教育訓練內容

• 1.氣相層析原理與6820GC簡介
• 2.注射口(INLET)
• 2-1分流/非分流注射口(split/splitless inlet)
• 2-2填充式注射口(purged packed inlet)
• 3.分析管柱
• 4.偵測器
• 4-1火焰離子偵測器(FID)
• 4-2電子捕捉偵測器(u-ECD)
• 5.儀器操作
• 6.日常維護與保養

1
 1.氣相層析原理與6820GC簡介

The sample determines the instrument configuration, i.e.:

• Type of Carrier Gas
• Type of Sample Inlet
• Type of Column
• Type of Detector
• Type of Data Acquisition

6820 GC 外觀

2
 Applications
Chlorinated Hydrocarbons in Water Aromatic Hydrocarbons in Water
by Headspace Analysis by Headspace Analysis
2 1
3 1. Chloromethane 1. Benzene
2. Dichloromethane 2 2. Toluene
3. Trichloromethane
4. Tetrachloromethane
4
1

15 min 10 min

Column: HP-1 (Cross-Linked Methyl Silicone) Column: HP-1 (Cross-Linked Methyl Silicone)
30 m x 0.53 mm x 2.65 μm film 30 m x 0.53 mm x 2.65 μm film
(Part No. 19095Z-123) (Part No. 19095Z-123)
Carrier: Helium, 5.2 psi Carrier: Helium, 5.2 psi
Oven: 40 C Oven: 60 C
Injection: 1cc, splitless Injection: 1 cc, split 5:1
Detector: FID Detector: FID

Type of Carrier Gas Effect on

Efficiency and Resolution

C at 175 C
17
HETP
k' = 4.95 Helium
(mm) Hydrogen
N WCOT Column Nitrogen (58 cm/sec)
1.2 2
OV-101 0.4 μm (58 cm/sec)
(58 cm/sec)
25 m x 0.25 mm
1.0

.8 He

.6 15 m x 0.25 mm
H2
Glass WCOT
.4
SE - 52
.2 Isothermal, 150 C

10 20 30 40 50 60 70 80 90 R = 1.17 R = 1.37
Average Linear Velocity (cm/sec)

Efficiency curves for a 25 m x 0.25 mm id Effect of carrier gas on the resolution

WCOT column with 0.4 um of OV-101. of n-heptadecane and pristane.

3
 calibration

6820 流量控制系統

Detector
Flow Blocks

Carrier
Chemical
Filters Inlet
Flow/Pressure
Controls

New Split Vent

Trap

L43 Inlet/Detector Pressure

Controls - Standard
2011/5/16
Page 8
Agilent Restricted

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 氣相層析系統組成

Mol-Sieve
Traps

Injection
Regulators Port
檢測器
Detector Electrometer

Flow
PC
Controller

注射器 Column
Hydrogen

Carrier Gas

注射口
Air

管柱

儀器狀態

• 6890 style electronics

• New keypad and display

2011/5/16
Page 10
Agilent Restricted

5
 2. INLET 注射口

• 導入樣品
• sample 控制進樣量
• 保持 sample 原貌,不使降解或反應
• 充分使樣品汽化

6820 Inlets type

9 Inlet Type
– Capillary
Split/Splitless
– Purged
Packed
9 Manual pneumatics
9 6890 style heater/
sensor

16 May 2011 Agilent Restricted

6820 update training

6
 2-1 分流非/分流注射口(Split/Splitless Inlet)

Liner O-Ring
Septum

Liner

Gold Seal

Capillary Column

5/4/00

分流模式
5
“TOTAL”
SEPTUM PURGE
MASS FLOW
CONTROLLER VENT
“C” LINE
“P” LINE 4
>60 PSI
CARRIER
SUPPLY
P P
2- SPLIT VENT
TOTAL FLOW IN
50 ML/MIN
1 53.5 ML/MIN “S” LINE
S

Split Vent 3
Trap PURGE
VALVE
SPLIT
“ON”

5 2

COLUMN
HEAD PRESSURE
BACK-PRESSURE
COLUMN FLOW = .5 ML/MIN REGULATOR/GAUGE

1 2
The split vent flow will now be
4 set to 50 ml/min
3
PRIMARY FLOW PATH

REDUCED FLOW PATH 16 May 2011

Agilent Restricted 6820 update training

7
 6820 Split/Splitless Capillary Inlet Manual Pneumatics
Control Panel
SPLIT

5 Column Head Pressure

Gauge

INCR INCR

1 Inlet Total Flow 2 Column Head Pressure

(Mass Flow Controller) (Back Pressure Regulator)

TOTAL FLOW COLUMN

HEAD PRESSURE

3 Split Vent 4 Septum Purge Vent

INLET VENT VENT
SPLIT/SPLITLESS SEPTUM PURGE
16 May 2011
Agilent Restricted 6820 update training

非分流模式 purge valve is “OFF”.

“TOTAL”
SEPTUM PURGE
MASS FLOW
CONTROLLER “P” LINE
VENT
“C” LINE
>60 PSI
CARRIER
SUPPLY
P P
2- SPLIT VENT
TOTAL FLOW IN
50 ML/MIN
1 53.5 ML/MIN “S” LINE
S

Split Vent 2
Trap PURGE
VALVE
SPLIT
“OFF”

COLUMN
HEAD PRESSURE
BACK-PRESSURE
COLUMN FLOW = .5 ML/MIN REGULATOR/GAUGE

Note: The split vent flow will still

PRIMARY FLOW PATH
remain 50ml/min
REDUCED FLOW PATH 16 May 2011
Agilent Restricted 6820 update training

8
 非分流模式樣品進樣後 purge valve
“ON”, 以流量 (50 ml/min) 吹掃氣化管

“TOTAL”
SEPTUM PURGE
MASS FLOW
CONTROLLER “P” LINE
VENT
“C” LINE
>60 PSI
CARRIER
SUPPLY
P P
2- SPLIT VENT
TOTAL FLOW IN
50 ML/MIN
1 53.5 ML/MIN “S” LINE
S

Split Vent 2
Trap PURGE
VALVE
SPLIT
“ON”

COLUMN
HEAD PRESSURE
BACK-PRESSURE
COLUMN FLOW = .5 ML/MIN REGULATOR/GAUGE

The split vent flow will now be

set to 50 ml/min
PRIMARY FLOW PATH

REDUCED FLOW PATH 16 May 2011

Agilent Restricted 6820 update training

2-2填充式注射口Purged Packed inlet

proportional
valve

flow flow pressure septum purge

frit sensor sensor regulator
septum purge
vent

flow control loop

Flow-controlled mode recommended for packed columns

9
 3分析管柱分離原理
Flow
A

Separation is a Partitioning Process

MOBILE STATIONARY
SAMPLE
PHASE PHASE

10
 Column Types
Open (Capillary)
Packed

Regular

Wall Coated
Open Tube

Conventional Porous Bead Porous Layer

Packed and Layer Column Open Tube
Micro Packed Bead

PACKED SERIES 530 WSCOT (wide) WCOT (narrow)

LENGTH (meters) .5-10 5-100 5-100 5-100
I.D. (mm) 2-4 .530 .3-.75 .1-.25

FLOW RATE (ml/min) 10-60 4-30 1-30 0.3-1.0

PRESSURE DROP (psi) 10-90 1-20 1-40 5-90
SAMPLE CAPACITY 100ng/peak 100 ng/peak 50 ng/peak

Column Separation Characteristics

• Efficiency:
Ability of the column to produce sharp peaks
• Resolution:
Ability of the column to separate two peaks from each other
• Selectivity:
Ability of the column to determine chemical and/or physical difference
in two peaks

GOOD GOOD
POOR POOR

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 4偵測器Detectors

9 偵測器detectors
– FID
– Micro ECD
9 Manual
pneumatics

16 May 2011 Agilent Restricted

6820 update training

Renovate Life with Technology

科技生活化的創意族

4-1火焰離子偵測器 FID
e
en
lu

10
To

ol
an
l
ex
no

8
c

Relative
oi

H
ta
an

Bu
l

Response
no
ex
c

6
ni

ha
H

(by wt.)
io

ol
Et
op

n
id

ha
Pr
ic

4
Ac

et

et
Ac

M
ic
rm

2
Fo

H H H H H H H

H C OH H C C OH H C C C C OH

H H H H H H H

Methanol Ethanol Butanol

Response is proportional to the number of carbon-hydrogen bonds.

12
 6820 FID Flow Diagram
Keyboard FID
main board board
Flex Cable
Detector 1.5 VDC
Vent voltage
applied to
igniter
Air
Air
Vent

H2 + AUX

When FID igniter is pressed:

- Air vents dropping detector flow to 100 ml/min (2/3 flow)
- Micro-switch in FID flow block is closed, pressing a “Key” on the main keypad via Flex Cable
- The “Key-press” is detected by firmware, which activates the ignitor circuit on the FID interface board
- FID ignitor circuit applies 1.5 VDC to the glow-plug
- Flame lights with a faint “pop”
- Button is released, restoring air flow and un-pressing the keypad button which is sensed by firmware,
turning off the ignitor voltage
16 May 2011
Agilent Restricted 6820 update training

FID Functional Schematic

Collector
Detector electronics

≈ - 220 volts

Flame
Chassis ground

Jet

Column Signal output

13
 FID Response/Selectivity
CHO
Air FID air supply CO2 He
+
H2O
CH4 Methane in sample N2 CHO
+ CHO
N2
+
CO2
CHO+ Methyl cations CHO
+
He
H2O CHO
H2 FID hydrogen
+ N2
Air N2 He Air
He
He Carrier gas
H2O Water N2 He H2
CH
H2 He 4
N2 Makeup gas N2 N2
He
H2 H2
CH4
N2 N2
He
H2 H2
CH4
N2 N2
He
H2 H2
CH4

H2 & Makeup H2 & Makeup

Carrier & Sample

FID Undetectable Compounds

Compounds that yield little or no response from an FID

Rare Gases NH3 CS2
Nitrogen Oxides H2 COS
Silicon Halides CO O2
H2O CO2 N2
Perhalogenated Compounds HCOH HCOOH

14
 4-2電子捕捉偵測器 Electron Capture Detectors
To ship the ECD:

Remove Gang fitting from EPC module

Remove four screws from ECD

Leave Heater/Sensor Installed

Remove ECD and cap the column fitting

ECD Theory

Detector Anode - pulsed

with positive voltage -
Constant Current/Variable Frequency
Secondary Emission
of Electrons
-e
Gas Exit

-e -e
N2 -e -e
-e -e
-e -e -e

Ni63
Source

Makeup Gas -
N2 or ArMe
Column - He, N2 or H2
Carrier

15
 ECD Theory

Detector Anode -
Pulse frequency increases
to maintain constant current
Secondary Emission
of Electrons
-e
Gas Exit

X -e
-e
N2 -e -e As electronegative
-e -e X sample enters cell -
-e -e -e
X free electron population
is depleted...

Ni63
Source

Makeup Gas -
N2 or ArMe
Column - He, N2 or H2
Carrier

6820 Electron Capture Detector - Display

Menus
Front/Back Detector
FRONT/BACK DET (ECD)
Temp
255 300<
Output
157
Output
in hertz

CONFIG FRONT/BACK DET

Setting the electrometer to “OFF”
Electrometer
Turns off the pulser to the anode
Off/On<

16 May 2011
Agilent Restricted 6820 update training

16
 5儀器操作

• 開機步驟:
打開氣體鋼瓶, 層析儀電源開關,電腦(確認儀表壓力是否到達)
儀器連線( Cerity QA/QC, Instrument 1 on-line)
(FID)等偵測器溫度到達設定值!點火
U-ECD 打開偵測器氣體
等訊號穩定,即可分析樣品
• 關機步驟:
OVEN降溫至室溫50℃, 偵測器(FID<100℃)
關閉偵測器氣體,
關閉層析儀電源
關閉氣體鋼瓶

5儀器操作-軟體介面

Main functions
easily accessed by
selecting 1 of 4
Views

Sub-functions
accessible by
selecting a
Page View

16 May 2011
Agilent Restricted 6820 update training

17
 分析樣品

Just enter Test

to be performed

Instrument Status
&
Real Time Plot

Worklist
With
Results

16 May 2011
Agilent Restricted 6820 update training

6.日常維護與保養
6-1注射口保養
6-2分析管柱保樣與維護
6-3偵測器保養與維護

18
 6-1注射口Split/splitless inlet

Replace Septum

Septum nut

Septum

定期更換
避免鎖太緊(hand tight)

19
 更換氣化管 Replace Liner

Purpose:sample evaporated complete in gas phase

Replace :
• peak shape degradation
• poor reproducibility
• sample decomposition
• Ghost peak

Liner 氣化管

去活性低壓降, 870uL 分流 5183-4647

去活性, 900uL 不分流 5181-3316

去活性, 2mm ID, 250uL 直管型 5181-8818

廣泛適用, 870uL 分流/不分流 5183-4711

去活性, 900uL 不分流 5062-3587

去活性, 800uL 不分流 5181-3315

1.5mm ID, 140uL 直管型 18740-80200

2mm ID, 250uL 直管型 18740-80220

4mm ID, 玻璃棉, 990uL 分流 19251-60540

带杯无填充, 800uL 分流，手动 18740-80190

带杯有填充, 800uL 分流，手动 18740-60840

20
 B-4 O-ring
O-ring can become deformed or
“flattened” over time when compressed
between the insert retainer weldment
and the inlet body.

Slide new o-ring over liner about ¼” and

drop liner into inlet. Liner should contact
the Gold Seal. Gently tighten insert
retainer on the inlet weldment.

Normal o-ring Deformed o-ring

Splitless Liner Split Liner

5062-3587 5183-4647

liner

B-3 Seal & Washer

Remove the column and reducing nut.

Clean or replace seal and washer.

Trim and reinstall column.

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 新的分流平板(密封金墊)

• 改進的生產技術，保證更加光滑
的表面，從面進一步提升密封性
• 專有的電鍍技術保證更惰性的金
屬表面
• 新的包裝裡含有墊圈 價格不變
• 更好的包裝確保分流平板的清潔
度

•新的分流平板部件號 (5188-5367)
• (推薦用於分流\不分流進樣口)

B-5 Ferrule

Why replace ?
oxygen
sample loss
poor retention time reproducibility
increase of noise

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 Ferrule Installation

GC安裝位置 6890 GC管柱安裝位置 5890GC管柱安裝位置

Split/splitless Inlet 管柱凸出ferrul 4~6 mm 管柱凸出ferrul 4~6 mm

Inlet
Purged packed Inlet 管柱凸出ferrul 1~2 mm 管柱凸出ferrul 2 mm

FID/NPD 伸到底後往下拉1 mm 伸到底後往下拉1 mm

TCD 伸到底後往下拉1 mm 伸到底後往下拉1 mm

Det.

ECD/uECD 管柱頂端至Nut約70±1 mm 管柱頂端至Nut約75 mm

FPD 管柱頂端至Ferrul約153 mm 管柱頂端至Nut約162 mm

(NEW FPD 145 mm)

6-2分析管柱維護-Condition column

1. 首先使所有加熱部位（如進樣口和偵測器）降温
2. 關閉載氣，將原色譜柱拆下，用no-hold ferrule(5181-3308)封住偵
測器端
3. 將管柱接在進樣口上，開通載氣流量(依色譜柱管徑選擇適當流量)
4. 切割毛细管柱出口，將出口端插入盛有甲醇的燒杯，正常情况下 應
能够觀察有氣泡產生，否則應即時檢查漏氣、色譜柱斷裂、或 進樣
口參數設置
5. 保持烘箱開放，用載氣流量跑 15-30min，以排除O2 (色譜柱壓力選
擇如後)
6. 關閉烘箱，提升進樣口温度，缓慢升温至分析方法的最高温度
7. 温度升至方法最高温度+20度 (請勿超過色譜柱恆常耐受最高溫度)
後繼續烘烤2小时（或参考色譜柱出廠建議的烘烤時间），降低爐温
，將色譜柱出口端接到偵測器
• 觀察blank baseline 是否穩定（不進樣的空针，2~3次）
• 不要使用H2做載氣烘烤色譜柱，以免引起爆炸。

23
 A-2 Common Causes of Column Performance
Degradation

1.Physical damage to the polyimide coating

2.Thermal damage
3.Oxidation (O2 damage)
4.Chemical damage by samples
5.Contamination

A-2-1 Physical damage to the polyimide

coating

24
A-2-2/3 Thermal /oxidation damage

Gas purifiers

25
 A-2-4 Chemical damage by
samples

6-3偵測器維護與保養 -FID Parts Explosion

Insulators Igniter

Collector

Interconnect
Insulators
Detector boards
(upper/lower)
Detector palette

Plumbing block Interconnect cable

Jet
Adapter
Detector base

Heater/sensor Insulation

26
 噴嘴的識別區分

FID 頂端
用於填充柱和毛細管柱的
FID 噴嘴很難從噴嘴頂端
的外觀和長度上加以區分
，

把FID 噴嘴安裝到檢測器上

噴嘴入口端
用於填充柱的 FID 噴嘴,其管內
徑小於毛細管柱噴嘴的管內徑.
可從噴嘴的入口端觀察到
左邊是用於填充柱的FID噴
嘴，部件號 18710-20119

* 注: 用於NPD 和 FPD 檢測器的噴嘴是一樣的

FID Typical Problems

• Flame blowing out or not lighting

• Spiking
• Low sensitivity
• Noise
• Drift

27
 Electron Capture Detectors (ECD)

Electron Capture Precautions

CARRIER GAS ............................................ dry and pure - 99.9995 %

SEPTUM ..................................................... low bleed (precondition)

SOLVENTS ..... clean, preferably hydrocarbon NEVER halogenated

QUANTITATION ......................................................... check linearity

汙染 –熱烤u-ECD
將u-ECD端管柱拆下用盲封封住偵測器端(確認沒有漏氣)!設
定OVEN 250℃,u-ECD 350 ℃ ,烘烤overnight,觀察基線

uElectron Capture Detectors

Micro Electron Capture Column Installation - using Mixing Liner

(Compatible with 5890/6890 ECD)

Indent

uECD
Mixing Liner
P/N G2397-20540

Insert Column to Indent and

withdraw 1-2 mm -

If column ID < .20 mm,

Install as shown below:
Final MUG
Adapter
Installation

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