MicroJet Cryo-Trap MODEL MJT-1030Ex OPERATION MANUAL · MicroJet Cryo-Trap MODEL MJT-1030Ex OPERATION MANUAL . ... 4.3 Manual Mode Operation 4-2

Ver. 3.07

MicroJet Cryo-Trap

MODEL MJT-1030Ex

OPERATION MANUAL

www.frontier-lab.com

A-2 Ver. 3.07

BEFORE USING THIS DEVICE

Thank you for purchasing our MicroJet Cryo-Trap (MJT-1030Ex). We advise you to read this operation

manual carefully before attempting to use this device in order to fully exploit the capabilities of this device.

This manual contains descriptions on installation, operation, performance tests, and troubleshooting. We

recommend that you make handy the operation manuals of your gas chromatograph, Pyrolyzer and/or Micro

Reactor, when using this device.

PRODUCT WARRANTY

Frontier Laboratories Ltd. warrants this product against defects or failures in accordance with the warranty

terms and conditions stipulated in a separate sheet. The product warranty can also be downloaded from our

website.

ABOUT PRODUCT SUPPORT PERIOD

We will stock consumable and maintenance parts and will accept inspection and repair orders seven years

from the date of product sales termination. However, in the event where electronic parts supplied from parts

manufacturers are discontinued; thus our stock level becomes too low, we may not be able to provide

support even within seven years from the date of product sales termination,.

FOR YOUR SAFETY

To use this product safely and properly, be sure to read the safety precautions and warnings

before attempting to operate. If this product is used in a manner not instructed in this manual, the

protective functions of this product may not be activated. Frontier Laboratories Ltd. will not be

responsible for losses incurred due to the neglect of these precautions and warnings.

This sign indicates that incorrect handling may cause hazardous

conditions resulting in minor or moderate personal injury and physical

damage.

CAUTION !

Other important handling information is placed in a frame like this. Note

This hazard signs indicates that incorrect handling may cause

hazardous conditions, resulting in death or severe personal injury. ! WARNING

!

A-3 Ver. 3.07

CONTENTS IN THE PACKAGE

H) S

tan

d

Base

Stand Pole

(KD pole with a washer and a screw, 1set)

* a part of Liquid Nitrogen Container Kit

B2) MJ1-1514

C) contents:

A1) MJ1-1303

Liquid Nitrogen Feed Tube Ex(1ea)

E2) MJ1-4201

MJT Control Cable (1ea)

G1) MJ1-1511

D1)

Flow Controller (1unit)

MJT-1030Ex Packing contents check list

This product is including following items. We recommend that you first examine the contents of the package you have received. If the contents differ from the package list below, or some items are missing, contact your dealer immediately.

(bottom layer)

D) F

low

Co

ntro

ller

A) Liquid N2 Feed Tube

※ View from top

(top layer)

A) contents:

B1) MJ1-5501

MS Trap Tube (1ea)

B) contents: D) contents:

G) contents:

E) contents:

AC Power Cable (1ea)

E3) MJ1-4202

MJT Signal Cable (1ea)

E6）

Indicator (1ea)


E5) MJ1-1517

Stand Base (1ea)


H1) MJ1-1513

H) contents:

Liquid N2 Container 2L (1ea)

*a part of Liquid Nitrogen Container Kit

E4) MJ1-1515

Clamp (1ea)


E7）MJ1-1121

LN2 Saver (2ea)MicroJet Tube (2ea)

(Re-order : MJ1-1111, 1ea)

C1) PY1-7052

Operation manual CD

Installation guide

Inspection report

(middle layer)

C)

Operation

Manual

E) Others

F) Others

H) S

tan

d

Base

G) Liquid N2

Container

2L

E1）

100V (Re-order: PY1-7001, 1ea)

A-4 Ver. 3.07

F) contents:

MJ1-1204

MJ1-3502

Tube Hanger (1set)

MJ1-1201MJ1-1202

Support Plate[with sems screw (M4 x 8) 4ea ,

MJT O-ring （P-5） 4ea, 1set]

F1) MJ1-K580: MJT-1030E/Ex Installation Kit for

HP5890 (1set)

MJ1-1208

Tube Hanger (1set)

MJ1-3501


Agilent6890/7890 (1set)

Tube Hanger (1set)

MJ1-3501

Installation Kit [one of these kit(F1)]

F1) MJ1-K380 MJT-1030E/Ex Installation kit for

Varian CP3800GC (1set)

Tube Hanger (1set)

MJ1-3501

MicroJet Tube Union Set (with a hexagon cap nut and

a fixing nut, 1set) (Re-order : MJ1-3101)

Graphite Ferrule (2pcs/pk)(Re-order: MJ1-7941, 5pcs/pk, 1set)

F5) MJ1-K300 MicroJet Tube Securing Kit (1set)F3) MJ1-1512

Container Cap 2L (1ea)

F2) MJ1-4211

Short Plug (1ea)

F4) MJ1-1305

Thermal Exchange

Coil 2L (1ea)


Shimadzu GC-17A/2010 (1set)

MJ1-1209


PerkinElmer Clarus GC (1set)

Tube Hanger (1set)

MJ1-3501





Support Plate[with sems screw (M4 x 8)4ea ,


Support Plate[with sems screw (M4 x 8)4ea ,




MJ1-1207

F1) MJ1-K901: MJT-1030E /Ex Installation kit for

TRACE GC (1set)

Tube Hanger (1set)

MJ1-3501

Support Plate[with sems screw (M4 x 8) 2ea,


MJ1-1218


Thermo TRACE 1300/1310GC (1set)

A-5 Ver. 3.07

MJT-1030Ex & PY-1030Ex-CHG (Change Option of Liq. N2 Container) Packing contents list

A1) MJ1-1303

Liquid Nitrogen Feed Tube (1ea)

E2) MJ1-4201

MJT Control Cable (1ea)

MJT-1030Ex & PY-1030Ex-CHG (Change Option of Liq. N2 Container)

Packing contents check list

This product is including following items. We recommend that you first examine the contents of the package you have received. If the contents differ from the package list below, or some items are missing, contact your dealer immediately.

A) contents:

D1) MJ1-5501

MS Trap Tube (1ea)

D) contents:

C1)

E) contents:

AC Power Cable (1ea)

E3) MJ1-4202

MJT Signal Cable (1ea)

Flow Controller (1unit)

C) contents:

E4）E5）MJ1-1121

LN2 Saver (2ea)MicroJet Tube (2ea)

(Re-order : MJ1-1111, 1ea)

B) contents:

B1) PY1-7052

Operation manual ＣＤ

Installation guide

Inspection report

G) contents:

G1) MJ1-1306

Thermal Exchange Coil for 30L (1ea)*a part of Thermal Exchange Coil Set for 30L

A) Liquid N2 Feed Tube

※ View from top (top layer) (second layer) (bottom layer)

C) F

low

Co

ntro

ller

(third layer)

B)

Operation

Manual

E) Others

F) Others

E1）

100V (Re-order: PY1-7001, 1ea)

A-6 Ver. 3.07

F2) MJ1-4211

Short Plug (1ea)

F4 )MJ1-1522

Container Cap for 30 liters Container

(1ea)

*a part of Thermal Exchange Coil Set for 30L

MicroJet Tube Union Set (with a hexagon cap nut and

a fixing nut, 1set) (Re-order : MJ1-3101)

Graphite Ferrule (2pcs/pk)(Re-order: MJ1-7941, 5pcs/pk, 1set)

F3) MJ1-K300 MicroJet Tube Securing Kit (1set)

F) contents:

MJ1-1204

MJ1-3502

Tube Hanger (1set)

MJ1-1201MJ1-1202




Agilent6890/7890 (1set)

Tube Hanger (1set)

MJ1-3501

Installation Kit [one of these kit(F1)]

F1) MJ1-K380 MJT-1030E/Ex Installation kit for

Varian CP3800GC (1set)

Tube Hanger (1set)

MJ1-3501


Shimadzu GC-17A/2010 (1set)

MJ1-1209


PerkinElmer Clarus GC (1set)

Tube Hanger (1set)

MJ1-3501

A-7 Ver. 3.07

TABLE OF CONTENTS

BEFORE USING THIS DEVICE A-2

PRODUCT WARRANTY TERMS AND CONDITIONS A-2

ABOUT PRODUCT SUPPORT PERIOD A-2

FOR YOUR SAFETY A-2

CONTENTS IN THE PACKAGE A-3

TABLE OF CONTENTS A-7

CHAPTER 1 ABOUT MICROJET CRYO-TRAP 1-1

1.1 Overview of Product 1-1

1.2 Principle 1-1

1.3 Front and Rear Panels of Flow Controller 1-4

CHAPTER 2 SPECIFICATIONS 2-1

CHAPTER 3 INSTALLATION 3-1

3.1 Getting Prepared for Installing MicroJet Cryo-Trap 3-1

3.2 Attaching Liquid Nitrogen Feed Tube Securing Plate 3-2

3.3 Installing Flow Controller 3-7

3.4 Installing Liquid Nitrogen Feed Tube 3-8

3.5 Attaching MicroJet Tube 3-10

3.6 Connecting Tubes and Cables 3-12

3.7 Checking and Calibrating Temperature Display 3-15

3.8 Installing Stand 3-17

3.9 Installing Column 3-18

3.10 Inserting Thermal Exchange Coil to Liquid Nitrogen Container 3-19

3.11 Un-plugging the liquid N2 feed tube from MJT control cable 3-20

CHAPTER 4 OPERATION 4-1

4.1 Handling Thermal Exchange Coil 4-1

4.2 Setting Nitrogen Pressure 4-1

4.3 Manual Mode Operation 4-2

4.4 Control from Temperature Controller of Pyrolyzer 4-2

CHAPTER 5 PERFORMANCE TESTS 5-1

5.1 Testing Flow Rate 5-1

5.2 Testing Cooling Temperature 5-1

5.3 Testing Trapping Performance 5-1

CHAPTER 6 TROUBLESHOOTING 6-1

CHAPTER 7 REPLACEMENT PARTS 7-1

1-1 Ver. 3.07

CHAPTER 1 ABOUT MICROJET CRYO-TRAP

1.1 Overview

In capillary chromatography, when dilute gases such as gases produced from a heated polymer sample

are introduced into a separation column for analysis, the gases are introduced into the capillary column

as an extremely broad band, resulting in poor resolution of peaks. To avoid this problem, gases must be

trapped at the front of the column to narrow the band width to increase the peak separation. To date

several methods have been devised for this purpose; however, they have all experienced problems such

as requirement of a large amount of coolant, inadequate cooling performance, and difficulties evolved in

automated operation. Frontier Lab has addressed these issues and developed the MicroJet Cryo-Trap,

based on an innovative technique not found in the past.

Our MicroJet Cryo-Trap allows trapping of low boiling species such as butane (n-C4) by cooling the front

portion of a capillary column down to near -196ºC. Combining this with our Pyrolyzers or Micro Reactors,

it allows various automated analysis.

MicroJet Cryo-Trap: United States Patent 6190613

1.2 Principle

Fig 1.2.1 shows the flow diagram of the MicroJet Cryo-Trap. Flow controlled dry nitrogen (by Flow

Controller) is liquefied by passing through a thermal exchange coil immersed in liquid nitrogen. The

liquefied dry nitrogen is allowed to blow against the front of the column in the GC oven to cool only the

front portion of the column. Gases introduced into the column are captured at the trap.

The flow diagram of the Flow Controller is shown in Fig. 1.2.2. Nitrogen gas flowed into the Flow

Controller passes through the stopcock and its flow rate is then controlled by restrictor and mass flow

controllers. Restrictor supplies 10mL/min of nitrogen gas all times, regardless of the state of the solenoid

valve in order to prevent the liquid nitrogen feed tube from icing. The solenoid valve performs

OPEN/CLOSE control of nitrogen from mass flow controller. With the valve OPEN, the column in the

oven is chilled by the liquid nitrogen passing through the thermal exchanger. The mass controller

controls the nitrogen flow rate to obtain a required cooling temperature. A safety valve located at the exit

of the Flow Controller prevents sudden rise of pressure in the vent of clogged liquid nitrogen feed tube.

Drawings in Fig. 1.2.3 illustrate how the trap works when the column is cooled and when trapped species

are thermally desorbed. Employing our newly designed MicroJet tube and LN2 saver configuration

prevents the inside of the tube from contacting moisture in the air while cooling with liquid nitrogen jet.

Therefore, it can be used even in moist atmosphere without icing of the column (Fig. 1.2.3A). Once the

solenoid valve is closed, heated air (e.g. 40ºC) in the oven passes through the trap, as shown in Fig.

1.2.3B, to rapidly heat the trap tube at a rate of ca. 10ºC/sec to desorb the trapped species.

1-2 Ver. 3.07

Fig. 1.2.1 Flow Scheme of MJT-1030EX

Column

Pyrolyzer or other attachment

Liq. N2 Container

MicroJet Tube MS Trap

Liq. N2 Feed Tube

Column Holder

Flow Controller

Thermal Exchange Coil

N2 C

ylin

der

Fig. 1.2.2 Flow Scheme inside Flow Controller

Safety Valve

Stopcock

GAS OUT 1

Pressure Gauge

N2 GAS IN

Mass Flow Controller (7L/min)

Solenoid Valve

Restrictor (10ml/min)

1-3 Ver. 3.07

A. Trapping

H2O in Air

N2 N2

MicroJet Liq N2 Flow

Column

Column Holder

Temperature Sensor

LN2 Saver

B. Desorbing

Heated Air N2 OFF

Fig. 1.2.3 Trapping by Liquid N2 and Thermal Desorption by Heated Air

1-4 Ver. 3.07

1.3 Front and Rear Panels of Flow Controller

Fig.1.3.2 Rear Panel of Flow Controller

Power Switch

Control Cable connector AC Power Code Socket

N2 Gas Inlet

N2 Gas Outlet

Circuit Breaker

Fig.1.3.1 Front Panel of Flow Controller

Control Mode Switch

Pressure Gauge

Stopcock

Power Lamp

Cooling Lamp

N2 Flow Adjust Knob

2-1 Ver. 3.07

CHAPTER 2 SPECIFICATIONS *

Cooling Temperature : -180ºC (with 7L/min N2 gas flow and 40°C of GC oven temperature)

Safety Device : Excessive pressure protection valve (Max 600kPa)

Required Pyrolyzers : EGA/PY-3030D, PY-3030S, PY-2020iD, PY-2020iS

Temperature Display : Available through EGA/PY-3030D or PY-2020iD

Column Size : id 0.25mm or less for metal capillary columns or id 0.5mm or less for fused silica capillary columns

Power Requirement : AC 100V/110V, 0.5A

Operating Environment : Less than 30°C recommended

Required GC System

: Agilent 7890, 6890

Shimadzu GC-17A, 2010

Thermo TRACE 1300/1310, TRACE GC Ultra

Perkin Elmer Clarus GC

No additional attachments must be installed on and over GC oven.

* Subject to modifications for improvement.

3-1 Ver. 3.07

CHAPTER 3 INSTALLATION

3.1 Getting Prepared for Installing MicroJet Cryo-Trap

1) Nitrogen - When this device is being operated, 7L of nitrogen is consumed every minute. If a nitrogen

cylinder is used, a dedicated nitrogen cylinder should be used. Sharing nitrogen cylinder with other

instrument may end up with pressure fluctuations. Nitrogen used must contain no greater than 5ppm

of oxygen, with dew point of less than -65ºC.

2) Pressure Regulator - If nitrogen cylinder is used, the maximum use pressure of the secondary

pressure should be greater than 1MPa, and the maximum flow rate should be greater than 20L/min

when the pressure difference is 400KPa. Inadequate flow rate will result in poor cooling performance.

3) Power Source - 3-pin AC 100V/110V (max 0.5A) power source with a grounding wire. The length of

the supplied power code is 2 m.

4) Butane gas - Butane gas of a cigarette lighter. Used for performance inspection.

Suffocation hazard - This device uses a large amount of nitrogen gas.

Be sure to install this device in a well-ventilated area. ! WARNING

Suffocation hazard - If sufficient liquid nitrogen is vaporized so as to

develop low oxygen atmospheres, you are at risk of oxygen deprivation.

Exposure to low oxygen atmospheres can quickly bring about

unconsciousness without warning. Use this product in a well-ventilated

area and avoid spilling liquid nitrogen.

.

! WARNING

When immersing the thermal exchange coil in liq. N2, allow nitrogen gas

to flow through the coil for at least one minute to purge moisture in the

liq. N2 feed tube, then while streaming nitrogen gas through it, lower it

slowly down into the liq. N2.

While immersing the thermal exchange coil in liq. N2, leave the nitrogen

gas cylinder valve and the stopcock of the Flow Controller

(MJT-1030Ex) open (See Fig. 1.3.1).

CAUTION !

CAUTION !

3-2 Ver. 3.07

Fig. 3.2.2 Making a Through Hole at the Top Wall of GC Oven

Make a hole of 1cm in diameter.

Make a hole over here.

3.2 Attaching Liquid Nitrogen Feed Tube Securing Plate

3.2.1 Installing onto Agilent 7890, 6890GC

1. Remove aluminum sheet located on the top of the GC oven by cutting off parts of the sheet shown in

Fig. 3.2.1 using nippers.

2. Push a screw driver or a similar object into the thermal insulator at the opening of the upper wall inside

the GC oven, and force it to make a through hole with 1cm in diameter (see picture below). The picture

shows the top wall of GC oven with SS adaptor of our Selective Sampler installed.

Cut off at these points

Fig. 3.2.1 Aluminum Sheet on GC Oven (Agilent Technologies 6890)

3-3 Ver. 3.07

3. Push down the tube guide of the liquid nitrogen feed tube securing plate into the hole made in step 2 so

that the plate is seated on the GC oven (Fig. 3.2.3).

4. Secure the plate with two screws supplied (M4 x 8mm) as shown below.

5. Attach two guide posts on the plate as shown in Fig. 3.2.4.

Fig. 3.2.3 Attaching Liquid Nitrogen Feed Tube Securing Plate

Secure the plate on top of GC oven using screws. The screw holes may differ by version. Two screws are used to secure the plate

Tube guide

Fig. 3.2.4 Attaching Guide Posts

Install guide posts at threaded holes.

Attach two O-rings (P5) to each guide posts

3-4 Ver. 3.07

Fig. 3.2.5 Making a through hole on the top of GC oven

a. Installing on to GC-17A b. Installing onto GC-2010

3.2.2 Installing onto Shimadzu GC-17A/ GC-2010

1. The installation position differs depending on the GC models. In reference to the descriptions below,

make a hole at the proper position.

[GC-17A]

Drive a screwdriver or a similar object all the way into the thermal insulator at the top cover of GC

oven shown in Fig. 3.2.5(a) and make a through hole with a diameter of 1 cm. Also, remove the cover

supporting rod (Fig. 3.2.5(a)).

[GC-2010]

The MicroJet Cryo-Trap is installed at the location where a detector is installed. Make a through hole

with a diameter of 1 cm from inside the GC oven (Fig.3.2.5(b)). Ensure the opening of the column

holder faces the right direction. See section 3.4 for details.

2. Insert the tube guide, located at the bottom of the liquid nitrogen feed tube securing plate, into the

hole made in step 1 and secure the plate on the top of GC oven with two screws (M4x8) (Figs. 3.2.5

and 3.2.6).

Installation position

Make a hole in thermal

insulator

Tube Guide

(In GC Oven)

Screw Hole of Securing Plate

Guide Post

Fig. 3.2.6 Liquid Nitrogen Feed Tube Securing Plate

Attach O-rings to the guide posts. (Two O-rings (P5) for each)

3-5 Ver. 3.07

3.2.3 Installing onto Perkin Elmer Clarus GC

1. At the position indicated in Fig. 3.2.7 drive a screwdriver or a similar object all the way into the GC

oven through the thermal insulator and make a through hole with 1 cm in diameter.

2. Insert the tube guide of the liquid nitrogen feed tube securing plate into the hole made previously

(section 1) and secure the plate to the top of the GC oven with supplied screws.

Position to make a hole

Fig.3.2.7 Making a through hole at the top of GC oven (Clarus GC)

Fig. 3.2.8 Liquid nitrogen feed tube securing plate

Tube guide (Inserted into GC oven)

Guide posts

Attach two O-rings (P-5) to each of guide posts

3-6 Ver. 3.07

Fix the plate using two screws.

Fig. 3.2.11 Attaching liquid nitrogen feed tube securing plate.

3.2.4 Installing onto Thermo TRACE 1300/1310GC

1. At the position indicated in Fig. 3.2.9 take out the detector module and install a thermal insulator at

the detector position.

2. Insert the tube guide of the liquid nitrogen feed tube securing plate into the hole made previously

(section 1) and secure the plate to the top of the GC oven with supplied screws.

Thermal insulator

Fig. 3.2.9 Installing a thermal insulator at the detector position of GC oven

Tube guide (Inserted into GC oven)

Guide posts

Attach two O-rings (P-5) to each of guide posts

Fig. 3.2.10 Liquid nitrogen feed tube securing plate

3-7 Ver. 3.07

3.3 Installing Flow Controller

Set Flow Controller and liquid nitrogen container in secured place. An example is shown in Fig. 3.3.1

An optional 10 L nitrogen container or your own container of 20 L or more should be placed on the floor

right in front of your GC. The length of the liquid nitrogen feed tube is fixed.

Fig. 3.3.1 Setting Flow Controller and Liquid Nitrogen Container

Flow controller

Liquid nitrogen

container

PY temperature controller

Liquid nitrogen feed tube can be damaged, if the moving parts of

sample introduction device hit the feed tube. Provide extra care for the

tube not being damaged.

CAUTION !

3-8 Ver. 3.07

Fig. 3.4.2(a) Installing Liquid Nitrogen Feed Tube

Insert the end of the liquid nitrogen feed tube to the hole (tube guide) of the securing plate.

Insert guide posts into guide post holes

3.4 Installing Liquid Nitrogen Feed Tube

1. Carefully insert the end of liquid nitrogen feed tube into the hole of the liquid nitrogen feed tube

securing plate, and secure the tube holder by inserting tube guide posts into guide post holes (see

Figs. 3.4.1 and 3.4.2).

Fig. 3.4.2(b) Column Holder Opening Facing GC Oven Door (for GC-2010)

For Shimadzu GC-2010, orient the liquid nitrogen feed tube so that the opening of the column holder is parallel to the GC oven door (Fig. 3.4.2 (b)).

For other GC models, orient the tube so that the opening of the column holder is perpendicular to the GC oven door.

Utmost care must be exercised in handling liquid nitrogen feed tube

to avoid damaging the column holder (made of pure gold).

Column holder opening

Tube guide

Fig. 3.4.1 End of Liquid Nitrogen Feed Tube

Column holder Tube holder

Tube holder securing screws

Guide post holes

The opening of the column holder is

parallel to that of the MicroJet tube. This

can be misaligned when in use. If this is

the case, loosen the tube holder fixing

screw and rotate the tube holder to adjust

alignment.

CAUTION !

3-9 Ver. 3.07

2. When the liquid nitrogen feed tube has been fixed, affix the supplied arrow seal to the front of the tube

to indicate the direction of column holder opening. (See Fig.3.4.3)

Fig.3.4.3 Arrow indication of the liquid nitrogen feed tube insertion direction.

3. Pass the thermal exchange coil pipes through the liquid nitrogen container lid, and connect the liquid

nitrogen feed tube with thermal exchange coil (Fig. 3.4.4). Join two sets of pipes together by

hand-tightening the cap nuts. Next, gently tighten them using a wrench (1/4 turn or less)

4. Pass the liquid level indicator through the small hole of the liquid nitrogen container lid, and attach a

stopper at the end (Fig. 3.4.4).

Fig. 3.4.4 Connecting thermal exchange coil and attaching liquid level indicator.

Thermal exchange coil

Liquid level indicator stopper

Connect these pipes

Liquid level indicator

Liquid nitrogen connector

Temperature sensor connector

3-10 Ver. 3.07

3.5 Attaching MicroJet Tube

1. MicroJet tube securing kit is attached to the quartz MicroJet tube. First, insert a cap nut and graphite

ferrule into the MicroJet tube and join it with MicroJet tube union. Hand-tighten the cap nut, followed

by turning 1/3 turn more with a wrench. See Fig. 3.5.1. Be careful not to tighten it too hard or the

MicroJet tube may be broken.

2. Attach freeze protection jigs to the MicroJet tube (Fig.3.5.2)

Fig.3.5.1 Attaching MicroJet Tube Securing Kit

Hand tightening, followed by turning 1/3 turn more with a wrench.

MicroJet tube nut

MicroJet tube union A

Graphite ferrule

Fig. 3.5.2 Attaching freeze protection jigs to MicroJet tube

Hand-tighten plus 1/3 turn more Micro Jet tube union A

LN2 Saver

3-11 Ver. 3.07

Fig. 3.5.3 Connecting tube guide to MicroJet tube

3. First, screw the nut of MicroJet tube securing kit into the tube guide of the liquid nitrogen feed tube

securing plate. This is followed by attaching the MicroJet tube with a union previously attached (Fig.

3.5.3).

4. By turning the MicroJet tube, adjust the position of the column holder, so that it is positioned at the

center of the horizontal tube of the MicroJet tube. Then securely fix the MicroJet tube by tightening

the nut (Fig. 3.5.4).

Tube holder

Guide post

Tube guide

Column holder

Nut

MicroJet tube

GC oven top panel

Liquid nitrogen feed tube securing plate

Position the column holder at the center of the MicroJet tube.

Fix the position of the MicroJet tube with this nut.

Fig. 3.5.4 Positioning and fixing MicroJet tube

3-12 Ver. 3.07

3.6 Connecting Tubes and Cables 1. Using MJT control cable, connect the Flow Controller and liquid nitrogen feed tube (see Fig. 3.6.1),

making sure to match the color of the cables.

2. Using PY signal cable, the Flow Controller and Temperature Controller of Pyrolyzer are connected.

Plug the valve connector of the PY signal cable into socket labeled PY at the rear panel of the flow

controller (see Fig.3.6.2), and connect the sensor connector to MJT control cable.

3. Referring to Fig. 3.6.3, connect cables to VALVE and SENSOR sockets at the rear panel of the

pyrolyzer temperature controller.

Fig.3.6.1 Connecting Flow Controller and Liquid Nitrogen Feed Tube

Connect these together

MJT control cable

Liquid nitrogen feed tube

Before connecting any cables, turn off power of all devices and unplug

the power codes. !

WARNING

3-13 Ver. 3.07

Fig. 3.6.2 Signal Cable Connection to Flow Controller

Fig. 3.6.3 Signal Cable Connection to Pyrolyzers

A. Connection to Double-Shot Pyrolyzer (PY-2020iD)

1st from top: red

2nd

from top: white

3rd

and 4th from top

(non-polarized)

SENSER

R

VALVE

E

B. Connection to Multi-Shot Pyrolyzer (EGA/PY-3030D)

VALVE

E

SENSOR

R

Sensor Cable

Valve Cable

3-14 Ver. 3.07

4. Connect outlet labeled “OUT” of the MS trap tube to port labeled “N2 GAS IN” at the back of the Flow

Controller. Then connect inlet labeled “IN” of the MS trap tube to a nitrogen cylinder.

5. Fig. 3.6.5 is the overall picture showing how nitrogen tube, valve control cable and sensor cable are

connected. Make sure that these are properly connected.

Fig. 3.6.4 Connecting MS Trap Tube

N2

IN MS trap tube

OUT

Fig. 3.6.5 MicroJet Cryo-Trap Connection Scheme

Controller GC MJT-1030Ex

MJT control cable

MJT signal cable

MS trap tube Liquid nitrogen feed tube

N2 Gas Signal

3-15 Ver. 3.07

A. Click on the checkbox.

B. Temperature reading for MicroJet Cryo-Trap

3.7 Checking and Calibrating Temperature Display

Depending on the combination of the liquid nitrogen feed tube and the temperature controller of Pyrolyzer, liquid nitrogen temperature (-196ºC) may not be correctly displayed. Follow the procedure described below to check and calibrate temperature readings.

1) [EGA/PY-3030D]

After starting the pyrolyzer control Software program, and click “Settings”, then click on the

checkbox for “MicroJet Cryo-Trap(MJT)” (Fig.3.7.1(1),A). The current temperature of MicroJet

Cryo-Trap will be displayed at he lower right corner of the window (Fig. 3.7.1(1),B).

[PY-2020iD]

After starting the pyrolyzer control Software program, go under “Tools” menu, under “Instrument

Set up”, and click on the checkbox for “MicroJet Cryo-Trap”(Fig.3.7.1(2),A). The current temperature

of MicroJet Cryo-Trap will be displayed at he lower right corner of the window (Fig. 3.7.1(2),B)

Fig. 3.7.1(1) Cooling temperature display (EGA / PY-3030D)

B. Temperature reading for MicroJet Cryo-Trap

A. Click on the checkbox..

Fig. 3.7.1(2) Cooling temperature display (PY-2020iD)

3-16 Ver. 3.07

2) Pull the liquid nitrogen feed tube out from the top of the GC, and immerse the tip of the tube in the

liquid nitrogen.

3) Check to see if the temperature reading for cryo-Trap in Fig. 3.7.1 is -196±1°C. If the temperature

does not fall into this range, proceed to 4 for temperature calibration.

4) Go under “Tools” menu, and select “Maintenance”. Then type the pass word of each instrument to

display a screen shown in Fig. 3.7.3.

5) While the temperature sensor is immersed in the liquid nitrogen, enter the temperature reading

(step C), then click “Save” (step D). Check to see if the temperature reading now is -196±1ºC.

Fig. 3.7.2 Immersing Temperature Sensor in Liquid Nitrogen

Liquid nitrogen feed tube

Liquid nitrogen

Fig. 3.7.3(1) Calibrating temperature display (EGA/PY-3030D)

B. Current temperature reading

for MicroJet Cryo-Trap

C. Enter current Cryo-Trap temperature

reading B, then click “Save”

-170

-170

3-17 Ver. 3.07

3.8 Installing Stand

Attach the stand support rod on the stand base then attach the clamp to the rod (Fig. 3.8.1).

Fig. 3.7.3(2) Calibrating temperature display (PY-2020iD)

C. Enter current Cryo-Trap temperature

reading B, then click “Save”

B. Current temperature reading

for MicroJet Cryo-Trap

-170

-170

Fig.3.8.1 Installing Stand

Clamp with holder

Stand support rod

Stand base

3-18 Ver. 3.07

3.9 Installing Column

1. Place a column on the column hanger inside GC oven.

2. Put the front of the column through the column holder, then connect the end to the GC injection port

(see Fig. 3.9.1).

Fig. 3.9.1 Putting Column through Column Holder

Column MicroJet tube LN2 Saver

Column

Run column through column holder (gold tube)

Fig. 3.9.2 An Example of Column and MicroJet Cryo-Trap Installed

Column connected to injection port Column connected to detector

3-19 Ver. 3.07

Fig. 3.10.1 Inserting Thermal Exchange Coil into Liq. N2 Container

3.10 Inserting thermal exchange coil to liquid nitrogen container

1. Open the main valve of nitrogen cylinder, followed by opening its stopcock. Then turn control mode

switch of Flow Controller to ON. While allowing nitrogen to flow through the thermal exchange coil,

immerse thermal exchange coil into a liquid nitrogen container (Fig. 3.10.1).

When handling liquid nitrogen, be sure to wear cryogenic gloves such

as leather gloves for protection against liquid nitrogen splashes. Never

use gloves made of cloth.

! WARNING

When immersing the thermal exchange coil into liquid nitrogen,

exercise extra care to work slowly and carefully to avoid liquid nitrogen

splashes. !

WARNING

Be sure to immerse the thermal exchange coil into liquid nitrogen, while

streaming nitrogen gas through the coil. Otherwise, moisture in air

becomes frozen and clogs the coil.

CAUTION !

Even while no cooling is performed, a small amount of liquid nitrogen is

consumed. Therefore, remove the thermal exchange coil from the

liquid nitrogen container when not in use for a long period of time.

CAUTION !

3-20 Ver. 3.07

MJT control cable Short plug Connect these

Fig. 3.11.1 Connection of the short plug

Clamp with holder

Liq. N2 feed tube

Stand support rod

2. Secure liquid N2 feed tube by the cramp as shown in Fig.3.10.2.

Fig. 3.10.2 Fixing liquid nitrogen feed tube

3.11 Unplugging the liquid N2 feed tube from MJT control cable

When the liquid N2 feed tube is disconnected from MJT control cable, the sensor connector of the MJT

control cable should be shorted with the supplied short plug as shown in Fig.3.11.1. With this connector is

open, actual temperature of Pyrolyzer (PY and ITF) may shift from their target temperature.

The liquid N2 feed tube must be secured by stand to prevent falling

down the liquid N2 container. ! WARNING

4-1 Ver. 3.07

CHAPTER 4 OPERATION

4.1 Handling Thermal Exchange Coil

1. When adding liquid nitrogen to the liquid nitrogen container, be sure to remove the thermal exchange

coil from the liquid nitrogen container.

2. Allow dry nitrogen to flow through the thermal exchange coil for at least 1 min to purge the coil to

remove any residual moisture prior to inserting it into the liquid nitrogen container (see Fig. 3.10.1). It

should be immersed as slowly as possible.

3. While the thermal exchange coil remains immersed in the liquid nitrogen container, a small amount of

liquid nitrogen is consumed, even if it is not actually used. If it is not used for a long period of time,

remove it out of the liquid nitrogen container.

4.2 Setting Nitrogen Pressure

Set the nitrogen pressure to 600kPa. The Flow Controller has been so configured at the time of shipping

that, with this setting, it can provide adequate flow rate to the system. Inadequate pressure will deteriorate

the cooling performance.

When the thermal exchange coil is being immersed in the liquid

nitrogen container, make sure that the stopcocks of nitrogen cylinder

and MJT-1030Ex Flow Controller be open (Fig. 1.3.1) to allow nitrogen

to flow through the system, otherwise, the liquid nitrogen feed tube may

be clogged with frozen moisture.

! WARNING

4-2 Ver. 3.07

4.3 Manual Mode Operation

(Manually turning ON/OFF of COOLING)

1. Open the stopcock of the nitrogen cylinder, then open the stopcock of the Flow Controller.

2. Flip the POWER switch located at the back of the Flow Controller (Fig. 1.3.1) to ON position, and make sure that the POWER lamp in the front panel comes on.

3. Setting the control mode switch to ON position will light the COOLING lamp and initiate cooling. Cooling can be stopped by flipping the switch to OFF. The cooling temperature is displayed on the PY-2020iD control screen.

4. The head of the separation column is cooled down to near liquid nitrogen temperature in 2 min as shown in Fig. 4.3.1. When desired temperature is reached, inject a sample into the system.

5. When sample has been injected, turn the control mode switch to OFF and start your GC.

4.4 When operating with Pyrolyzer or µ-Reactor

When this device is used in conjunction with Pyrolyzer or µ-Reactor, set “Control mode switch” on the

front panel of temperature controller to “AUTO”.

Analytical conditions are set through their each control software. Refer to their each operation manual for

the operation of the software.

Fig. 4.3.1 Cooling Temperature Profile GC oven: 40 ºC

4 min 1 2 3 0

-50

-100

0

-200

Cooling start

ºC

40

N2 gas flow

3.5 L/min

5 L/min

7 L/min

5-1 Ver. 3.07

CHAPTER 5 PERFORMANCE TESTS

5.1 Testing Flow Rate

1. Set the secondary pressure of nitrogen cylinder connected to the Flow Controller to 600kPa.

2. Turn on POWER switch located at the rear panel of the Flow Controller (Fig.1.3.2).

3. Open the stopcock on the front panel (Fig. 1.3.1).

4. While keeping the thermal exchange coil at room temperature, turn ON the control mode switch of the

Flow Controller. At this point, make sure that the pressure gauge of the Flow Controller reads 340kPa.

Within this pressure range, required flow of nitrogen stream can be obtained.

5.2 Testing Cooling Temperature

1. While allowing nitrogen to flow through the thermal exchange coil, slowly insert it into the liquid

nitrogen container.

2. Make sure that the temperature drops to -180°C or below in less than 3 min.

5.3 Testing Trapping Performance

1. Turn the control mode switch to COOLING OFF.

2. Install a column into a GC, and set the GC oven temperature to 40°C. Use normal GC settings for

others such as injection port and detector temperatures, etc.

3. Inject 2µL of butane gas from a cigarette lighter into GC using a regular 10µL syringe.

4. Make sure that a peak due to butane is observed (see Fig. 5.3.1A).

5. Turn ON the control mode switch of the Flow Controller to initiate cooling.

6. Once the temperature reaches -180°C (normally in 2~3min), inject 2µL of butane gas into GC as

mentioned above.

7. Make sure that peak due to butane is not observed at the retention time for butane upon the operation

described above (section 3).

8. After 3 min, turn OFF the control mode switch to terminate cooling.

Then make sure that butane trapped is again observed on the GC chart (see Fig. 5.3.1B).

Prior to inserting the thermal exchange coil into the liquid nitrogen

container, purge the liquid nitrogen feed tube for at least 1 min by

flowing nitrogen through it, then slowly immerse the coil into liquid

nitrogen.

! WARNING

5-2 Ver. 3.07

This concludes all the performance tests. If there are any problems, refer to CHAPTER 6

TROUBLESHOOTING.

Fig. 5.3.1 Testing Trapping Performance Using Butane

Column: Ultra ALLOY-5+

(5% diphenylpolysiloxane, 30m, 0.25mm i.d., 0.25µm film)

GC oven temp.: 40°C, Injector temp: 250°C, Detector: FID or MS Column gas flow rate: 1mL/min, Split ratio: 1/50~100

Cooling stopped after 3 min

A) Trap disabled

B) Trapped for 3 min

No butane observed

n-C4

iso-C4

C3

n-C4

iso-C4

C3

0 1 2 5 min 3 4

6-1 Ver. 3.07

CHAPTER 6 TROUBLESHOOTING

Symptom, causes, and solutions are summarized below.

SYMPTOM CAUSE SOLUTION

1. System completely dead.

Power code not plugged. Plug power code in power outlet.

Inadequate N2 flow rate. Turn POWER switch to ON, and make sure power lamp comes on. If it does not come on, check circuit breaker. Press reset button, if circuit breaker has been activated.

2. Trap not cooled to -180°C

Inadequate N2 flow rate.

a. In normal operation at cooling, the N2 pressure reading should be 250~300kPa. If thermal exchange coil is left immersed in liq. N2, it is clogged with ice from air moisture, and pressure gauge of Flow Controller may read over 500kPa. Remove the thermal exchange coil from the liq. N2 and allow N2 to flow through it for 5min.

b. Pressure regulator of N2 cylinder not capable to provide 10L/min of flow may cause this problem. If this is the case, replace the pressure regulator.

N2 leaking. Make sure all connections are made securely.

Liquid N2 too low. For best performance, at least bottom 5cm (2 in) of thermal exchange coil must be submerged in liq. N2. Standard 2L container requires at least 300mL of liq. N2. Add more liq. N2, if needed.

Oven temp too high. Set the initial oven temperature to below 70°C.

Room temperature too high.

This device operates 30°C or below.

3. Pressure reading of Flow Controller too high (over 500kPa).

Thermal exchange coil or liquid nitrogen feed tube clogged.

Refer to 2a above.

4. 4. Not controllable from pyrolyzer.

Pyrolyzer signal cable not connected.

Connect pyrolyzer signal cable. See section 3.6 of this manual for details.

Control mode switch of Flow Controller not set to “AUTO”

Turn control mode switch to “AUTO” position.

Cryo Trap setting of pyrolyzer temp controller not set to auto control.

Enter”1” in “Cryo Trap” field of “FUNCTION” screen. See section 4.3 of this manual for details.

5. Peaks too broad or peaks split. Inadequate cooling.

Increase flow rate of N2 or add more liq. N2. See 2. above.

Column in trap covered with ice.

Increase flow rate of N2. See 2. above.

6. Butane not trapped. Inadequate cooling.

If trapping temperature is above -180°C, resolve the problem according to 2. above.

7-1 Ver. 3.07

CHAPTER 7 REPLACEMENT PARTS

See your dealer to place an order for replacement parts listed in table below.

PART NAME PART No. QTY DESCRIPTION

Liquid nitrogen feed tube securing plate (for Agilent6890/7890, with screws)

MJ1-1201 1 Used for Agilent6890/7890

Liquid nitrogen feed tube securing plate (for HP5890, with screws)

MJ1-1202 1 Used for HP5890.

Liquid nitrogen feed tube securing plate (for Shimadzu GC-17A/2010, with screws)

MJ1-1204 1 Used for Shimadzu GC-17A/2010

Liquid nitrogen feed tube securing plate (for Thermo TRACE GC Ultra, with screws)

MJ1-1207 1 Used for Thermo TRACE GC Ultra

Liquid nitrogen feed tube securing plate (for Thermo TRACE 1300/1310 GC, with screws)

MJ1-1218 1 Used for Thermo TRACE 1300/1310 GC

Liquid nitrogen feed tube securing plate (for Varian CP3800 GC, with screws)

MJ1-1208 1 Used for Varian CP3800 GC

Liquid nitrogen feed tube securing plate (for PerkinElmer Clarus GC, with screws)

MJ1-1209 1 Used for PerkinElmer Clarus GC

Liquid nitrogen feed tube Ex MJ1-1303 1 Column holder attached

Guide post MJ1-1251 1 A set of 2 posts required

Thermal Exchange Coil 2L MJ1-1305 1 Thermal exchange coil for 2 liters container

(see Fig.3.4.4)



MicroJet tube MJ1-1111 1 Tube made of quartz (see Fig. 3.5.1).

LN2 Saver MJ1-1121 2 Used with MicroJet tube. (see Fig. 3.5.2).

MicroJet tube securing kit MJ1-K300 1 Used to install MicroJet tube on GC (see Fig. 3.5.1).

MJT control cable MJ1-4201 1 Cable for N2 and sensor signal.

MJT signal cable (for PY-2020D) MJ1-4202 1 Used for valve control.

Tube Hanger for HP5890, Shimadzu GC-17A/2010, TRACE GC, CP3800

MJ1-3501 1 Liquid nitrogen feed tube hanger (for HP5890, Shimadzu GC-17A/2010, TRACE GC and Varian CP3800)

Tube Hanger for Agilent6890 MJ1-3502 1 Liquid nitrogen feed tube hanger (for Agilent6890)

Documents

MicroJet Cryo-Trap MODEL MJT-1030Ex OPERATION MANUAL · MicroJet Cryo-Trap MODEL MJT-1030Ex OPERATION MANUAL . ... 4.3 Manual Mode Operation 4-2