Ver.2.22
AUTO-SHOT SAMPLER
MODEL AS-1020E / AS-1020ET
OPERATION MANUAL
www.frontier-lab.com
BEFORE USING THIS DEVICE
Thank you for purchasing Frontier Lab’s Auto-Shot Sampler (AS-1020E/ ET). We advise you to read this
operation manual carefully before attempting to use this device in order to fully exploit its capabilities.
This manual describes installation, operation, maintenance, and troubleshooting. We recommend that you
make handy the operation manuals of your gas chromatograph, GC/MS and Pyrolyzers 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,.
A-2
Ver. 2.22
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.
!
WARNING
This hazard signs indicates that incorrect handling may cause
hazardous conditions, resulting in death or severe personal injury.
This sign indicates that incorrect handling may cause hazardous
!
CAUTIO
conditions resulting in minor or moderate personal injury and physical
damage.
N
!
Note
Other important handling information is placed in a frame like this.
1. When working with this device, be sure to wear a pair of safety
!
WARNING
glasses.
2. While sample cup recovery chute is removed, a safety circuit is
activated and cups cannot be retrieved. If the safety circuit is forced
to be deactivated, a high temperature sample cup is shot up at high
speed, running risk of your body.
3. When this device is operated, do not remove the top cover to avoid
electrical shock and damaging critical parts. Product warranty is void
if the device is operated without the cover in place.
4. Even though the device is protected by a cover, avoid touching the
cover with bare hands since the temperature of the cover can be as
high as 50~70°C while the pyrolyzer is being operated.
5. Before uninstalling this device, make sure that the pyrolyzer is fully
cooled down and that the power cable is unplugged.
6. When the device is operated, make sure you have good ventilation.
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Ver. 2.22
1. When this device is connected to Agilent 6890, 6850, or 7890; or
!
CAUTION
Shimadzu GC-2010, splitless injection cannot be used, because of
the GC carrier gas control of this Auto-Shot Sampler.
If the splitless injection is used with GC or GC/MS described above,
the injector pressure becomes open when the sample is introduced,
resulting in a large flow of carrier gas. This will end up with sample
cup not introduced into pyrolyzer furnace and may lead to failure of
the device. Please never use splitless injection mode with GC or
GC/MS listed above.
2. Sample cups other than Eco-cup LF (80µL), Eco-cup G (50µL), or
Eco-cup GQ (50µL) cannot be used. Also, before using, inspect the
sample cup shape using the supplied cup inspection tool. (refer to
section 6.1 of this manual)
3. Glass sample cups (Eco-Cup G and Eco-Cup GQ) should never be
reused.If reused, the cup may not be introduced to the pyrolyzer
furnace or may not be recovered properly.
4. When analyzing samples with a large amount of resides left in the
sample cup, the volume of the sample should be less than 50% of
the sample cup volume and plug the cup with flamed quartz wool to
prevent the residues from scattering when the sample is retrieved.
5. The path along which the sample cup travels may be contaminated.
In particular, when reactive pyrolysis is performed the path gets
contaminated frequently. In reference to Chapter 6 of this manual,
conduct regular cleaning of the path. Severe contamination may
lead to failure of sample cup retrieval or malfunction of this device.
(Proper maintenance of this device is required for warranty
coverage.)
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Ver. 2.22
The sample cup tray cover is properly secured to the tray only if the
!
CAUTION
cover position guide pin located in the back of the cover (Fig. A) is in
the position guide hole of the carrousel (Fig. B)
In an event where the tray cover is secured while the guide pin is in
one of the depressions (Fig. B), sample cups will not be recovered
and they are piled up in the Pyrolyzer furnace or in the Auto-Shot
Sampler. This can clog the valves of Auto-Shot Sampler and
seriously damage the instrument.
Position guide pin
Fig. A
Cover position guide pin
in the back of tray cover
Depressions for manual rotation
Position guide hole
Carrousel
Fig. B
Top view of Auto-Shot Sampler
(tray cover removed)
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Ver. 2.22
CONTENTS IN THE PACKAGE
A-6
Ver. 2.22
AS-1020E PARTS BOX
＜Agilent GC＞
AS-1020E Installation Kit for Agilent 6890/7890
P/N:AS1-K680, P/N:AS1-K780
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Ver. 2.22
＜Agilent GC＞
AS-1020E Sideways Installation Kit for Agilent 7890
P/N:AS1-K784
①
① AS mounting plate (1ea)
If ordered as PY-1020E-S15D,
these parts are already
attached to the AS-1020E
main unit.
③
②
②AS supporting rod (1ea)
④
M4 fixing screw 1 ea
M4 height adjusting scew 1 ea
M4 lock nut 1 ea
③AS cover for sideway
installation
⑤
④ Auto-Shot Sampler supporting plate set
⑤Stand (60mm) 1 ea
Auto-Shot Sampler fixing plate (with NBR rubber sheet) 1 ea
M6 hexagonal screw 1 ea
M6 washer 2 ea (spare 1 ea)
M6 spring washer 2 ea (spare 1 ea)
M6 spacer 1 ea
＜Shimadzu GC＞
AS-1020E Installation Kit for Shimadzu GC-17A/2010
P/N:AS1-K201
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Ver. 2.22
＜Thermo Fisher GC >
AS-1020E Mounting Kit N for TRACE GC Ultra contents
P/N:AS1-K902
①
③
②
③ Long stand (80mm) (2ea)
① AS mounting plate (1ea)
If ordered as PY-1020E-S15D,
these parts are already attached to
the AS-1020E main unit.
② AS supporting rod (1ea)
(with M4 washer (2ea), M4 spring
washer (1ea), M4 nut (1ea), screw
for fixing the AS (1ea)
AS-1020E Mounting Kit N for TRACE GC 1300/1310 contents
P/N:AS1-K904
①
1
③
②
③ Stand (40mm) (1ea)
① AS mounting plate (1ea)
(If ordered as PY-1020E-S17D,
these parts are already attached to
the AS-1020E main unit.)
② AS supporting rod (1ea)
with screw for fixing the AS (1ea)
＜SCION / Bruker GC＞
AS-1020E Installation Kit for Varian GC3800/ Bruker SCION 430/436/450/456-GC
P/N:AS1-K380
①
②
③
①Stand base （1ea）
②Screw (Ｍ3、1ea)
③Washer （15 mm od、1ea）
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Ver. 2.22
TABLE OF CONTENTS
BEFORE USING THIS DEVICE
A-2
PRODUCT WARRANTY
A-2
ABOUT PRODUCT SUPPORT PERIOD
A-2
FOR YOUR SAFETY
A-3
CONTENTS IN THE PACKAGE
A-7
TABLE OF CONTENTS
A-10
Chapter 1 About Auto-Shot Sampler
1-1
1.1 Functions of Auto-Shot Sampler
1-1
1.2 Principle
1.2.1 Operation of Auto-Shot Sampler
1.2.2 Principle of Sample Cup Movement
1-2
1-2
1-4
1.3 Structure and Parts Names
1-5
Chapter 2 Specifications
2-1
Chapter 3 Installation
3-1
3.1 Preparing for Installation
3-1
3.2 Replacing Interface (ITF) Unions
3-1
3.3 Connecting Tubes and Cables
3.3.1 Connecting Tubes
3.3.2 Connecting Cables
3.4 Installing Auto-Shot Sampler
3-4
3-4
3-5
3-7
3.5 Removing Sample Cup Tray
3-10
Chapter 4 Notes About Pre-treatments of Samples
4-1
4.1 Sample preparation
4-1
4.2 Preventing sample from scattering
4-2
Chapter 5 Setting Auto-Shot Sampler
5-1
5.1 Setting Parameters for Accessory Devices
5.1.1 When using with Multi-Shot Pyrolyzer
5-1
5-1
5.1.2 When using with Double-Shot Pyrolyzer
5-2
5.2 Creating, Saving, Loading and Printing Method File
5-3
5.2.1 Connecting Tubes
5-3
5.2.2 Connecting Cables
5-3
5.3 Creating Sequence Table
5-4
5.4 Operation Procedure and Operation Examples with GC and GC/MS
5.4.1 Connecting Agilent Technologies ChemStation (Example)
5.4.2 Connecting Shimadzu GCMS solution (Example)
5-5
5-6
5-7
Chapter 6 Maintenance
6-1
6.1 Sampler Cups
6-2
6.2 Auto-Shot Sampler
6.2.1 Cleaning Sample Cup Path
6.2.2 Cleaning Carrousel and Sample Cup Tray
6.3 Cleaning Quartz Pyrolysis Tubes
6-3
6-3
6-5
6-6
6.4 Cleaning Interface Needle
6-6
Chapter 7 Troubleshooting
7-1
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Ver. 2.22
CHAPTER 1
ABOUT AUTO-SHOT SAMPLER
1.1 Function of Auto-Shot Sampler
Auto-Shot Sampler AS-1020E/ET has been developed to use with our pyrolyzers. See Fig. 1.1 for
details.
Auto-Shot Sampler AS-1020E/ET allows automatic continuous analysis of up to 48 samples with the
Single-Shot technique. At low temperatures the thermal desorption method can be used, while at
high temperatures pyrolysis technique can be used with this device.
Auto-Shot Sampler AS-1020E/ET can be installed onto EGA/PY-3030D, PY-3030S or PY-2020iD/iS
pyrolyzer
Auto-Shot Sampler
Carrier Gas
(Connects to GC flow controller outlet)
Multi-shot pyrolyzer
Double-shot pyrolyzer
Single-shot pyrolyzer
From He/N2 source
(Carrier gas used for sample cup
recovery)
Gas
reservoir
MS
GC Oven
Temperature controller of Pyrolyzer
PC
PC
Fig. 1.1 Auto-Shot Sampler with Py-GC/MS system
(Shown as an example)
1-1
Ver. 2.22
1.2 Principle
1.2.1 Operation of Auto-Shot Sampler
Fig. 1.2.1 shows the principle of Auto-Shot Sampler.
A: Position of sample
cup introduction
Cup sensor
V1: Shutter for sample cup introduction
Carrousel
V2: Gate valve
V3: Control pin
Purge flow
(2ml/min)
Carrier gas
(GC flow control)
Pyrolyzer
Purge
(2ml/min)
Carrier gas for
purging and recovery
1. Analysis ready
2. Sample cup introduction
Sample cup recovery chute
B : Sample cup standby position
Purge
Purge
(2ml/min)
(2ml/min)
3. Standby
Recovery
4. Sample analysis
5. Sample cup recovery
Fig. 1.2.1 Operation Principle of Auto-Shot Sampler
1-2
Ver. 2.22
A. Sample introduction, standby state and analysis steps
1. A maximum of 48 cups are loaded into the carrousel which rotates after each analysis. Each
sample cup moves sequentially to the sample-cup-introduction position A by action of a stepping
motor.
2. Cup sensor detects the cup and gate valve V2 rotates to open the path.
3. Sample cup introduction shutter slides to allow the sample cup to drop onto the sample cup
standby position B.
4. V1 and V2 close, and the cup stands by during the system is purged with carrier gas. Any
stand-by time can be set using "Instrument Set Up" of the PY-2020iD Control Software.
Refer to
Article 5.1 for further details.
5. V2 then closes and once the system is fully purged with carrier gas, the cup control pin V3 slides
to allow the sample cup to free-fall into the pyrolyzer furnace for analysis.
B. Sample cup recovering steps
1. When analysis is over and GC oven is cooled down to initial temperature, all of cup introduction
shutter V1, gate valve V2, and cup control pin V3 open.
2. Then sample cup recovering carrier gas (300 to 500kPa) is instantly introduced into the system at
the position between pyrolyzer and GC injection port. The sample cup is rapidly blown up to the
cup recovery container through the cup recovery chute.
!
CAUTION
When analyzing a sample that leave a large amount of residues, the
amount of sample added to the sample cup should be no more than
50% of the cup volume. Further, regardless of analysis mode, plug the
sample cup with a small amount of flame heated quartz wool to
prevent scattering of sample residues.
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Ver. 2.22
1.2.2 Principle of Sample Cup Movement
After the thermal desorption program in Double-Shot analysis, as well as after the heating program of
each zone in the heart-cut EGA analysis, the sample cup is transferred back to the sample cup
stand-by position. Fig. 1.2.2 shows how it is done.
V4 : Relief valve for the
cup-recovery carrier gas
V1
V2
V3
Recovery
Purge
(2ml/min)
Recover
y
1. End of the Program
2. Open V3 and V4
(thermal desorption or heating)
3. Close V3
Purge
(2ml/min)
4. Recovery of sample cup
back to the stand-by
position
Fig. 1.2.2 Operation of Auto-Shot Sampler in Double-Shot Analysis or Heart-Cut EGA
1. The thermal desorption program in Double-Shot analysis, or the heating program of each zone in
the heart-cut EGA analysis is over.
2. After the valves, V3 and V4, open, the carrier gas for cup-recovery with a pressure controlled at 300
to 500kPa is rapidly introduced from the point between furnace and GC injection port, and the
sample cup is blown up to the position between V2 and V3.
3. V3 closes.
4. The carrier gas for cup-recovery stops, and the sample cup is held at the stand-by position.
!
When using Double-Shot or Heart-Cut Analysis mode, place a small
CAUTION
amount of flame heated quartz wool on the top of sample in a sample
cup to prevent scattering of sample
1-4
Ver. 2.22
1.3 Structure and Parts Names
Figs. 1.3~1.8 show construction and parts names of the Auto-Shot Sampler.
Sample cup tray
Sample cup recovery chute
Pilot lamp
Sample cup recovery container
Housing
Fig. 1.3 Front View of Auto-Shot Sampler
AS Teflon sheet G
Sample cup tray cover
Carrousel
Sample cup recovery
chute
Threaded hole for
carrousel securing screw
Sample cup tray fixing screw
Sample cup tray
Fig. 1.4 Parts Names of Auto-Shot Sampler
(Left : with sample cup tray cover; Right : with sample cup tray cover removed.)
1-5
Ver. 2.22
Sample cup recovery chute
Sample cup recovery container
Sample cup path
Cap nut for connecting with Pyrolyzer
Height adjuster
Pyrolyzer
Fig. 1.5 Front View of Auto-Shot Sampler without Cover
RS232C connector
GC fixing plate
I.O. Port
Non-fuse breaker
Power switch
AC cable connector
Connector for sample cup
recovering valve cable
Fig. 1.6 Rear View of Auto-Show Sampler
1-6
Ver. 2.22
Stopcock: OPEN
Stopcock: CLOSE
Pressure gauge
Stopcock
Fig. 1.7 Front View of Gas Reservoir
Carrier gas inlet
Pressure adjuster
Carrier gas outlet
Connector for sample cup
recovering valve cable
Fig. 1.8 Rear View of Gas Reservoir
Stopcock
He IN
Pressure
regulator
Restrictor
Pressure
Gauge
Buffer Tank
Solenoid Valve
He OUT
Fig. 1.9 Flow Scheme inside Gas Reservoir
1-7
Ver. 2.22
CHAPTER 2
FEATURES AND SPECIFICATIONS
Sample Introduction:
Free-fall into vertical furnace
Sample cup recovery:
Blown upward by pressurized carrier gas
Recovery gas:
Pressurized carrier gas (He or N2; if carrier gas line is shared with other
GC units, the gas pressure may fluctuate and cause some undesirables
results. We advise that you use a dedicated gas line for sample cup
recovery.)
Recovery gas press:
300 ~ 500kPa (When using glass cup, 400 ~500kPa)
Analysis mode:
Use with PY-3030S or PY-2020iS: Single-Shot
Use with EGA/PY-3030D or PY-2020iD:
Single-Shot, Double-Shot, Direct EGA, Heart-cut EGA
No. of sample cups:
A maximum of 48 cups
Sample cup:
Deactivated stainless steel cups (id 3.8mm, height 8mm, wall thickness
0.1mm, volume 80µL)
Non quartz coated glass cup (id 3mm, height 8mm, wall thickness 0.5mm,
volume 50µL)
Quartz coated glass cup (id 3mm, height 8mm, wall thickness 0.5mm,
volume 50µL)
P ol ym er c o a te d c up (id 3mm, height 8mm, wall thickness 0.5mm,
volume 50µL)
Control software:
Auto-shot sampler control program is installed in PC that is used to
control your GC or GC/MS. Pyrolyzer
Supported GC, GC/MS:
Agilent (5975, 7890, 6890), Shimadzu (2010, 17A), JEOL, etc. (However
Auto-Shot Sampler is unusable with splitless mode of Agilent GC7890,
6850,6890 and Shimadzu GC-2010)
Appearance and specifications are subject to modifications without notice for improvement.
Auto-Shot Sampler model AS-1020ET must be used to install onto Thermo
!
CAUTION
!
CAUTION
Fisher GCs. If AS-1020E is used, the GC may be shut down due to
uncontrollable injector pressure.
Glass sample cups (Eco-Cup G and Eco-Cup GQ) should never be reused.If
reused, the cup may not be introduced to the pyrolyzer furnace or may not be
recovered properly.
2-1
Ver. 2.22
CHAPTER 3 INSTALLATION
3.1 Preparations
1) Set up a GC with a Split/Splitless injection. If your GC or GC/MS is not a supported model, talk
with one of our dealers or contact us directly.
2) AC110V (>1A) with 3P plug
3) Reserve a space (19cm x 10cm x 28cm) for the gas reservoir in the vicinity of Auto-Shot Sampler
(within 0.5m).
4) Set the carrier gas pressure for sample cup recovery to 300 to 500kPa (when using glass cup, to
400 to 500kPa) at the secondary pressure of the pressure regulator. If carrier gas line is shared
with other instrument, the pressure may fluctuate and cause adverse effects. We advise that you
use a dedicated gas line for the sample cup recovery.
3.2 Replacing Interface (ITF) Unions
Follow the procedure below to replace the ITF union with that attached to Auto-Shot Sampler, so that
pressurized carrier gas can be used for sample cup recovery.
1. Make sure that both pyrolyzer furnace and GC injection port are fully cooled.
2. Turn off GC or GC/MS.
3. Loosening the screws of the injection port, and uninstall the pyrolyzer
4. Remove ITF thermal insulator and stainless steel cover.
5. Replace the ITF union with that for Auto-Shot Sampler as shown in Fig.3.1.1 – Fig.3.1.3. Attaching
the ITF union for Auto-Shot Sampler to the pyrolyzer, using the wrench supplied in the package as
shown in Fig.3.2. If difficulties are encountered in removing Vesper ferrule, see Chapter 6
Maintenance (6.1.2 “Cleaning Quartz Pyrolysis Tube”).
6. Once ITF union has been replaced, attach ITF needle as shown in Fig. 3.3.
7. Attach ITF thermal insulator for Auto-Shot Sampler (Fig. 3.4).
8. Set the pyrolyzer onto the GC injection port.
!
WARNING
Tip of the ITF needle is extremely sharp. Wear safety glasses and
exercise caution when handling these parts.
3-1
Ver. 2.22
ITF union
ITF union
Bottom
Pyrolyzer
Replac
e
ITF union for
Auto-Shot Sampler
Top
Fig. 3.1.2 Replacing ITF unions
Fig. 3.1.1 Location of ITF union
ITF union for
Auto-Shot Sampler
ITF union body
ITF nut
Needle nut
Fig. 3.1.3 Composition of ITF union for Auto-Shot Sampler
ITF union for Auto-Shot Sampler
1/16 inch stainless steel tube
6mm wrench
Back
12mm wrench
Front
Tighten
Fig. 3.2 Attaching ITF Union for Auto-Shot Sampler
3-2
Ver. 2.22
6mm wrench
ITF needle
8mm wrench
(5/16 inch)
Front
Back
Fig. 3.3 Attaching ITF Needle
1. Insert the heat sink from the bottom
2.
Minimize the clearance between
interface block and the heat sing adapter
Interface block
Heat sink adapter
Fix with scew
AS Interface (ITF) union
1.6mm tube from
the interface union
accommodate to the
Auto-Shot Sampler
The slit should face to
back of the furnace
Minimize the
clearance here.
AS Interface (ITF)
union
Fig. 3.4 Heat sink adpter installation
3-3
Ver. 2.22
3.3 Connecting Tubes and Cables
3.3.1 Connecting Tubes
Carrier gas used for sample cup recovery should be fed from a dedicated gas source. Adjust
pressure to be between 300 and 500kPa. (When using glass cup, adjust pressure to be between 400
and 500kPa.)
1) Using 1/8 inch copper tube contained in tubing kit, connect a carrier gas source to carrier gas inlet
located at the back of the gas reservoir (Fig. 3.5)
Carrier gas inlet
Pressure adjuster
Carrier gas outlet
Connector for sample cup recovering valve cable
Fig. 3.5 Rear View of Gas Reservoir
2) Using a 1/8 inch copper tube and a union, connect 1/16 inch stainless steel tube from ITF
union attached to the pyrolyzer (Fig. 3.2) to the carrier gas outlet of the gas reservoir shown in
Fig. 3.5 (Fig. 3.6).
Pyrolyzer
Back ferrule
1/8 inch union
Front
From carrier gas outlet of
the gas reservoir. See
Fig. 3.5.
Rubber seal
1/8 inch nut
1/8 inch copper tube
1/16 inch stainless steel tube
Fig. 3.6 Connecting ITF Union and Gas Reservoir
3-4
Ver. 2.22
3.3.2 Connecting Cables
Fig. 3.7a and b show how Auto-Shot Sampler is hooked up to other devices with cables.
3.3.2a Using with Multi-Shot Pyrolyzer (EGA/PY-3030D)
Auto-Shot Sampler is connected to EGA/PY-3030D temperature controller via RS-232 cable. Sample
cup recovery valve cable needs to be connected to recover used sample cups by pressurized carrier
gas by activating EM valve placed in the gas reservoir.
Auto-Shot Sampler
RS-232C cable
Gas reservoir for Auto-Shot Sampler
Pyrolyzer
Sample cup recovering valve cable
EGA/PY-3030D temperature Controller
GC
PC
Pyrolyzer temperature
control cable
USB cable
GC remote cable
Fig. 3.7a Auto-Shot Sampler and Cable Connections to Other Devices
(with Multi-Shot Pyrolyzer; EGA/PY-3030D)
3-5
Ver. 2.22
3.3.2b Using with Double-Shot Pyrolyzer (PY-2020iD)
Auto-Shot Sampler is connected to PC via RS-232 cable. Sample cup recovery valve cable needs to
be connected to recover used sample cups by pressurized carrier gas by activating EM valve placed
in the gas reservoir.
Auto-Shot Sampler
RS-232C cable
Gas reservoir
Pyrolyzer
Cup recovery valve cable
PY-2020iD temperature controller
GC
PC
Temperature control
cable
RS232C cable
GC remote cable
Fig. 3.7b Cable connections other instrument (In this example, Pyrolyzer PY-2020iD is used)
3-6
Ver. 2.22
3.4 Installing Auto-Shot Sampler
1.
Remove double-shot sampler or liquid sampler if any of them is attached to the pyrolyzer.
2.
When installing the Auto-Shot Sampler to Shimadzu GC (GC 17A ver. 2, GC 17A ver. 3, and
GC2010), attach the Auto-Shot Sampler supporting bracket (supporting stand) using the
threaded holes located at upper left side cover of GC (Fig. 3.8). For GC 17A, use the holes 1
of the bracket, and with GC 2010, use the holes 2.
Securing the bracket using these threaded holes
(Making threaded holes on the side-cover is required
for the case of GC 17A ver. 2.).
Fig. 3.8 Attaching the supporting bracket (stand)
3.
When installing the Auto-Shot Sampler to Thermo Fisher TRACE 1300/1310 GC, replace the
stand (length:30mm) with the supplied stand (length:40mm). A height adjuster (flat head
screw) and a lock nut (nut) shall be reused.
4.
Place the Auto-Shot Sampler on the pyrolyzer and secure them using pyrolyzer connecting
cap nut (Fig. 3.9.1). Because a rubber O-ring is used for joint sealing, gently hand tighten it.
Do not over tighten.
Pyrolyzer connecting cap nut
Pyrolyzer furnace
Fig. 3.9.1 Connecting Auto-Shot Sample and Pyrolyzer
5.
Adjust two height adjusting screws located at the bottom left of the Auto-Shot Sampler, so that
the top surface of the Auto-Shot Sampler is completely leveled. See Fig. 1.5.
3-7
Ver. 2.22
6.
When installing to Agilent GC, attach the supporting rod to the back-side of the Auto-Shot
Sampler using the fixing screws (See Fig.3.9.2.).
7.
When installing to Shimadzu GC, secure the Auto-Shot Sampler to the supporting plate using
the fixing screws (See Fig.3.9.3).
8.
When installing to Thermo Fisher TRACE GC Ultra, attach the supporting rod to the GC top
cover as shown in Fig 3.9.4 and then fix the supporting rod to the back side of the Auto-Shot
Sampler using the fixing screws (See Fig.3.9.5)
9.
When installing to Thermo Fisher TRACE 1300/1310 GC, attach the supporting rod to the
back of the stand (Fig. 3.9.5). Then secure the back of the Auto-Shot Sampler to the
supporting rod using fixing screws (Fig. 3.9.5)
Fig. 3.9.2 Supporting rod (Agilent6890)
Fig. 3.9.3 Supporting plate (Shimadzu GC)
40mm stand
is used here
Fig. 3.9.4 Attaching supporting rod
(Thermo Fisher TRACE GC Ultra)
Fig. 3.9.5 Supporting rod
(Thermo Fisher Trace 1300/1310GC)
3-8
Ver. 2.22
10.
When installing to SCION/Bruker 4 3 0 / 4 3 6 / 4 5 0 / 4 5 6 GC, attach the Auto-Shot Sampler
fixing plate to the stand base with supplied screw and washer (Fig. 3.9.6). Then engage the
screws of the Auto-Shot sampler support rod into the slots at both ends of the fixing plate and
secure the plate by finger-tightening the screw.
Fixing screw
（M3）
Washer
Fixing plate
Stand base
Fig. 3.9.6 Stand base
(Scion/Bruker 430/436/450/456 GC)
11.
Put the pyrolyzer housing cover in place.
12.
Then put the Auto-Shot Sampler housing cover back in place by sliding it from the front to the
back of the sampler. Secure the housing cover using 2 screws on the right side and 2 screws
on back left side of the device.
When the above is over, check again to see if ITF union, gas reservoir, and carrier gas source are
all properly connected. Also, make sure that power cable, RS232C cable, and sample cup recovery
valve cable are properly connected.
13.
Start your GC or GC/MS.
3-9
Ver. 2.22
3.5 Removing Sample Cup Tray
Sample cup tray can be easily removed from the Auto-Shot Sampler. When a large number of
sample cups are used, removing the sample cup tray from the Auto-Shot Sampler will make it easy
to load the cup tray with sample cups.
1.
Remove sample cup tray cover and sample cup recovery chute. See Figs. 3.10 and 3.11. The
sample cup recovery chute is magnetically attached to the sensor cover. Auto-Shot Sampler
will not work without the sample cup recovery chute in place for safety reasons. A magnetic
sensor located inside the sensor cover detects whether the sample cup recovery chute is put
in place or not.
AS Teflon sheet G
Sample cup recovery chute
Sample cup tray cover
Sample cup tray
Sensor cover
Fig.3.10 Top View of Auto-Shot Sampler
2. Remove the sample cup securing screw and put it in the threaded hole to fix the sample cup
tray and carrousel. See Fig. 3.11.
3. Pull the sample cup tray straight upward and place it on your work table.
Sample cup tray securing screw
Magnetic sensor
Threaded hole for fixing carrousel
(Be sure to move the securing screw here)
Fig. 3.11 Sample Cup Tray Securing Screw and Carrousel Securing Screw
3-10
Ver. 2.22
4. Fig. 3.12 shows sample cups placed on the sample cup tray. When handling sample cups, use
contamination-free tweezers that have been baked with a burner flame. The sample cup stand
may be used.
It can hold up to 10 sample cups at a time.
Sample cup t
Fix carrousel to tray
Carrousel
Sample cup tray
Sample cup stand
Fig. 3.12 Placing Sample Cups in Sample Cup Tray
1.
!
Note
Sample cups will fall off if the carrousel alone is removed. Be sure to fix
the carrousel to the sample cup tray by moving the sample cup tray
securing screw to the threaded hole before attempting to remove the
carrousel.
2.
Make sure that the sample cups are cooled down to room temperature
before placing them in the carrousel. Putting hot sample cups in the
carrousel may damage the tray sheet located between the sample cup
tray and the carrousel.
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Ver. 2.22
The sample cup tray cover is properly secured to the tray only if the
!
CAUTION
cover position guide pin located in the back of the cover (Fig. 1) is in
the position guide hole of the carrousel (Fig. 2)
In an event where the tray cover is secured while the guide pin is in
one of the depressions (Fig. 2), sample cups will not be recovered
and they are piled up in the Pyrolyzer furnace or in the Auto-Shot
Sampler.
This can clog the valves of Auto-Shot Sampler and
seriously damage the instrument.
Position guide pin
Fig. 1 Cover position guide pin in the back of tray cover
Depressions for manual rotation
Position guide hole
Carrousel
Fig. 2
Top view of Auto-Shot Sampler (tray cover removed)
3-12
Ver. 2.22
CHAPTER 4 NOTES ON PRETREATMENT OF SAMPLES
4.1 Sample preparation
When pretreating samples, note the following;
1. There is no need to clean disposable Eco-cups with solvent before placing sample in the cup. It
is recommended that the sample cup should not be reused.
2. When handling sample cups, other tools such as tweezers, cutter knives, etc. must be baked
beforehand to remove any contaminations.
3. If the sample material is not too hard, samples can be prepared by cutting the material on a
clean glass plate using a cutter knife. Use only contamination-free knives and tweezers for
sample preparations. Such tools must be baked with a micro burner (torch) flame in advance.
4. When placing sample in a sample cup, we recommend you use Eco-Stand, which comes with
Pyrolyzer. It not only allows hot sample cup to cool down, but also makes it easy to weigh the
sample.
Eco-Stand AL
Sample Cup Stand 10
Fig. 4.1 Cup Stands
4-1
Ver. 2.22
4.2 Preventing sample from scattering
In an analysis using the Auto-Shot Sampler (AS-1020E/ET), the sample or sample residues in the
sample cup (Eco-cup) may scatter during the operation. In situations like this, clean quartz wool
needs to be used to plug the sample cup to prevent the sample from scattering.
Described below is an example：
1． A small but appropriate amount of quartz wool is taken out from container using a pair of
tweezers.
2. Form the quartz wool into a tangled ball with a diameter of 6~8 mm using fingers (Fig. 4.2). Take
an extra care not to make the ball too small for the sample cup.
6～8 mm
Fig. 4.2 Quartz wool formed into a tangled
ball
3. If you touch the quartz wool ball with bare hand, hold the ball with a pair of tweezers and heat it
with a butane torch to burn off organics (Fig. 4.3).
Fig. 4.3 Cleaning quartz wool ball by torch
flame
4. Place the cleaned quartz wool in the Eco-cup. If difficulties are encountered, use two pairs of
tweezers as shown in the figure below. (Fig. 4.4)
Fig. 4.4 Placing quartz wool ball in sample cup
5. Make sure that the wool ball does not run off the Eco-cup.
This completes the anti-scattering protection using quartz wool.
The anti-scattering protection is not always needed depending on the nature of samples or analysis
mode. The anti-scattering protection is not needed in situations where a sample is dissolved in a
solvent or sample has a high viscosity; and when analyzing residue free samples in single-shot or
evolved gas analysis (EGA) mode in which returning the sample cup to the standby position is not
required.
4-2
Ver. 2.22
!
Note
1. Sample cups other than Eco-cup LF (80µL), Eco-cup G (50µL), or
Eco-cup GQ (50µL) cannot be used. Eco-cup S and platinum sample
cups must not be used. Use of these voids warranty.
2.
Do not use deformed sample cups. Sample cups can be inspected using
the sample cup inspection tool.
3.
When in Double-Shot or Heart-Cut EGA mode analysis, add a small
amount of quartz wool to the sample cup (on the top of sample) to
prevent scattering of sample.
4.
When analyzing a sample that leave a large amount of residues, the
amount of sample added to the sample cup should be no more than 50%
of the cup volume. Further, regardless of analysis mode, plug the sample
cup with a small amount of flame heated quartz wool to prevent
scattering of sample residues.
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Ver. 2.22
CHAPTER 5 SETTING AUTO-SHOT SAMPLER
5.1 Setting Parameters for Accessory Devices
Regarding the software for devices other than that for Auto-Shot Sampler, read the operation manual
of each device.
5.1.1 When using with Multi-Shot Pyrolyzer
1. Start the software program by double clicking the icon of control program for pyrolyzer. If the
program detects the connection to the Auto-Shot Sampler, a screen shown in Fig. 5.1 is displayed.
If the sample cup tray on the upper right is not displayed, follow the steps below (2 through 4) to
correct the problem.
Sample cup tray
Fig. 5.1 Main Control Screen for EGA / PY-3030D
From the main screen, select “Settings”. A window showing a list of accessory devices is displayed
(Fig. 5.2)
2. Check the box for “Auto-Shot Sampler” and select “OK”.
3. If the communication with the Auto-Shot Sampler is not established, a dialog box shown in Fig. 5.3
is displayed. Ensure that the cable is properly connected and the power is tuned on, then hit “OK”
button.
Fig. 5.2 Setting Screen for Accessory Devices
Fig. 5.3 Error massage of connection
5-1
Ver2.22
5.1.2 When using with Double-Shot Pyrolyzer
1. Start the software program by double clicking the icon of control program for pyrolyzer. If the
program automatically detects the connection to the Auto-Shot Sampler, a screen shown in Fig.
5.4 is displayed. If the sample cup tray on the upper right is not displayed, follow the steps below
(2 through 4) to correct the problem.
Sample cup tray
Fig. 5.4 Main Control Screen for PY-2020iD
2.
From the menu bar, select “Tools” – “Instrument Set Up”. A window showing a list of accessory
devices is displayed (Fig. 5.5)
3.
Check the box for “Auto-Shot Sampler” and select “OK”.
4.
If the communication is not established, a dialog box shown in Fig. 5.6 is displayed. Select the
proper Com port number and click “OK” button.
Fig.5.5 Setting Screen for Accessory Devices
Fig.5.6 Error massage of connection
5-2
Ver2.22
5.2 Creating, Saving, Loading, and Printing Method Files
Method files must be created, because all parameters such as pyrolyzer temperature settings, etc.,
required to run the Auto-Shot Sampler are saved in the method files. A method file can be printed by
selecting “Print” from “File” menu (Fig. 5.7).
5.2.1 Creating and Saving a Method File
All files related to the operation of the Auto-Shot Sampler are stored in “EGA_PY-3030D”,
“PY-2020iD Control” or “PY-2020iS Control” directory under “Program Files”.
1.
At first, analytical parameters for pyrolyzer should be entered. In the main control screen of
pyrolyzer, enter pyrolyzer furnace temperature and interface temperature, followed by selecting
accessory devices connected to the Auto-Shot Sampler.
2.
From “File” menu, selecting “Save as” will display a dialog box shown in Fig. 5.7 Type in a new
filename, then click “OK” button to save a method file just created.
Fig. 5.7 Saving a Method File
5.2.2 Loading a Method File
1. From the menu bar, select “File” – “Open” to display a directory in which method files are listed
(Fig. 5.8).
2. Select a method file of your choice with the mouse pointer and hit “OK” button to load the file.
Fig. 5.8 Loading a Method File
5-3
Ver2.22
5.3 Editing a Sequence Table
In a sequence table, positions of sample cups, method filenames, and analytical modes are entered.
1. From the menu bar, select “Tools” – “Sequence Table”. Alternatively, in the main control screen
clicking the sample cup tray icon (Fig. 5.1) will display the Sequence Table.
2. Saving a Sequence Table
-
Cup Nos. can be entered into the sample cup # column using the
PC keyboard, or alternatively, clicking any position of the carrousel and moving the mouse pointer
to a different position will turn the color of the sample cups between the two positions to green.
Clicking again at a sample will turn the color of the selected sample cups to gray. And at the same
time, the selected sample cup numbers are automatically entered in the sequence table (Fig. 5.9).
To delete unwanted rows of the table, click at a desired row then click “Delete Entry” button at the
bottom of the screen.
3. Fig. 5.10 shows entry items in a sequence table. A and C must be entered, while B and E are
optionally entered. When entering method filenames in column C, “Pick up from Directory”
button at the bottom of the screen should be useful. Column D is automatically entered depending
on analysis mode selected.
4. Once the sequence table is completed, save the sequence table by selecting “File” – “Save” or
“File” – “Save as” from the menu bar.
5. Now set the start and end sample cup position Nos. Enter the start cup position No. in G, and the
end cup position No. in H. These are defaulted to the first and last position Nos. of the table.
A: Sample cup
C: Method filename
position No.
D: Analysis mode
B: Sample name
E:: Comment
F: Carrousel
G: Start No.
H: End No.
Fig. 5.9 An example of sequence table screen
5-4
Ver2.22
5.4 Analysis Procedure and an Example of Working with GC and GC/MS
Procedure from setting Auto-Shot Sampler to actual analysis:
1. Place samples in sample cups. Then load the carrousel with the sample cups.
2. Attach the sample cup tray onto the Auto-Shot Sampler.
3. Put the sample cup chute, sample cup recovery container, and tray cover in place on the
Auto-Shot Sampler.
4. Setting parameters for pyrolysis: Load a method file into the system or create a new one.
5. Creating a sequence table: Load a sequence table into the system or create a new one.
Settings for GC and GC/MS:
Files required for automated continuous analysis need to be created according to the operation
manual of each instrument that is connected to the Auto-Shot Sampler.
1. Create the same number of data files as the number of samples to be analyzed by Auto-Shot
Sampler.
2.
Allow GC to be in “Ready” state
When all of the above steps are completed, click “Minimize” button at the upper right corner of the
sequence table window to return to the main control screen of the Auto-Shot Sampler. Pressing
“START” button located at the upper right will initiate analysis. During the analysis, sample cup
number that is being analyzed is displayed on the right to “Cup” in Monitor area of the main control
screen.
!
1.
Note
Do not remove the sample cup chute during analysis. If it is removed, the
safety circuit becomes activated and analysis is forced to be terminated.
If this is the case, follow the steps 1 thought 4 below to restore.
1)
Put the sample cup chute back in place.
2)
Turn the power switch located at the back of the Auto-Shot Sampler
OFF, then turn it back ON to reset the system.
3)
Go to the sequence table and move the mouse pointer over the
sample cup number of which analysis has been done then click
“Delete Entry” button to delete the entry from the sequence table.
Then save the file.
4)
2.
Click “START” button in the main control screen to restart analysis.
While automated analysis is in progress, do not hit “STOP” button of the
main control screen, or a dialog box will be displayed. Hitting “OK” will
terminate
automated
analysis
sequence
and
sample
cups
are
immediately ejected.
5-5
Ver2.22
5.4.1 Connecting Agilent Technologies ChemStation (Example)
1. Click ChemStation icon. From the menu bar, select “Sequence” and click “Edit Sample Log
Table” to display a window shown in Fig. 5.10.
Fig. 5.10 Creating a Sequence Table
2. Click “Repeat” to create the same number of data files as the number of samples to analyze.
Methods available for analysis can be displayed by entering “?” in the “Method” space. The
completed sequence can be stored in computer memory by clicking “OK” button and becomes
available for use. To save the sequence file created, select “Sequence” – “Save” from the menu
bar.
3. A dialog box shown in Fig. 5.11 is displayed by selecting “Sequence” – “Run” from the menu bar.
To avoid overwriting old data files, keep “Overwirte Existing Data Files” unchecked.
4. Click “Run Sequence” button to bring the system in standby state (Fig. 5.12).
Fig. 5.11 Checking Settings for Analysis
Fig. 5.12 Standby Dialog Box
5-6
Ver2.22
5.4.2 Connecting Shimadzu GCMS solution (Example)
Creation of a batch file required for continuous analysis is described below as an example.
1.
Double-click “GC Analysis” icon to start the application (Fig. 5.13).
2.
Clicking “Batch Processing” icon (circled) in the Assistant bar will display a screen for batch
process.
Menu bar
Batch
processing
Assistant bar
Fig.5.13 Main Screen of GCMS solution (Left) and Screen of Batch Processing (right)
3.
Click “Setting” in the Assistant bar to display a setting screen (Fig. 5.14). Here, enter folder
name for storing analysis data and data filename.
Fig. 5.14 Setting Screen
<Example>
Start line: Select “Start the line next to the previously aborted line”
Folder: Specify a folder to store analytical data.
Data filename (for automatic naming):
Put a checkmark on “Automatically generate a data filename”
5-7
Ver2.22
4.
Clicking “Wizard” in the assistant bar
will display a screen of “Batch Table
Wizard”. Complete
the wizard in reference to Fig. 5.18. Enter a method filename that is used for analysis. Click
“NEXT (N)” to proceed.
Fig. 5.15 Batch Table Wizard
5.
In “Batch Table Wizard – Unknown sample (1)”, enter the number of samples, sample name, and
sample ID. When completed, click “NEXT (N)” to proceed (Fig. 5.16).
Fig. 5.16 Batch Table Wizard with Unknown Sample (1)
6.
Type in a data filename of your choice. Checking “Auto numbering” will generate filenames with
suffixes of successive numbers at the end. Do not check “Report output” (Fig. 5.18).
Fig.5.17 Batch Table Wizard with Unknown Sample (2)
7.
Click “FINISH” button. A batch table is automatically created (Fig. 5.19). Enter sample names if
desired. To save the batch file, select “File” – “Save as” from the menu bar.
8.
Clicking “START” button will bring the system in standby state.
5-8
Ver2.22
Fig. 5.18 An Example of Batch Table
5-9
Ver2.22
CHAPTER 6
MAINTENANCE
In order for trouble-free operation of Auto-Shot Sampler, daily and periodical maintenance is required.
Frequency of required maintenance is proportional to the number of samples analyzed.
In daily routine work, items that need maintenance are mainly sample cups, quartz pyrolysis tube,
and interface needle. We advise you to keep an operation log in which date of operation, the number
of samples analyzed, etc. are recorded to learn when maintenance needs to be done. For
maintenance of GC injection port (septum, insert, column, etc.), refer to the Operation Manual of
Double-Shot Pyrolyzer. (Chapter 5. Maintenance)
This device is composed of various precision parts in order to effectively introduce
!
Note
sample cups to the pyrolyzer and to recover them after analysis. Disassembling,
adjustment or modification of this device can result in malfunction and voids product
warranty.
6-1
Ver2.22
6.1 Maintenance of Sample Cups
1.
Inspecting sample cups
Once analysis is over, the sample cup is blown upward for recovery at a high speed from the
pyrolysis furnace by action of high pressure carrier gas. This may cause the sample cups to
be damaged. Use of distorted sample cups is a source of malfunction of the system and cup
recovery may not be properly done. Used sample cups should be inspected using the
sample cup inspection jig (Fig. 6.1). Use only such cups that pass through the jig freely.
Put a sample cup from flat one
TOP
Sample cup:
Disposable Eco-cup LF
Sample cup inspection jig
(P/N: AS1-1531)
BOTTOM
Fig.6.1 Using Sample Cup Inspection jig
2.
Cleaning Sample Cups
The attached disposable Eco-cup LF is produced for single-round usage. It is highly recommended to
use a new cup at every analysis. If there is a concern of the contamination of the previous sample,
wipe the inner surface of the cup with cotton swab, soaked with solvent. Then stir the cups with just
enough solvent to cover them. Ultrasonic cleaner should not be used to clean the cups. Make sure
the cups are well-dried before use.
6-2
Ver2.22
6.2 Maintenance of Auto-Shot Sampler
6.2.1 Cleaning Sample Cup Path
Contamination occurs in places of the Auto-Shot Sampler and accessory devices as analyses are
performed. If the amount of sample is large, in particular, high boiling point components from
pyrolysis often deposit at the upper portion of the quartz pyrolysis tube, and inside and vicinity of the
joint cap nut between the Auto-Shot Sampler and pyrolysis furnace. These should be cleaned with a
cotton swab dampened with a solvent such as acetone. Note that this operation must be performed
when pyrolysis furnace is fully cooled down to room temperature and after separating the Auto-Shot
Sampler from the Pyrolyzer (Figs. 6.2 and 6.3).
To open all valves, select “Tools” from the menu bar on the screen and then select “Troubleshooting”.
Click “Valve Open” button on the screen shown in Fig.6.4.
For your safety, turn off the AS-1020E/ET power switch (valves 1 and 2 are kept open).
Pyrolyzer joint cap nut
Most frequently
contaminated
Furnace
Fig. 6.3 Cleaning Upper Part of Pyrolyzer
Fig. 6.2 Cleaning Sample Cup Path
Click “Valve Open”
Fig. 6.4 Opening valves
6-3
Ver2.22
Also, maintenance should be similarly performed at sample cup shut and sample cup hole located at
the top of the Auto-Shot Sampler. Right of Fig. 6.5 shows the position of sample cup shut and
enlarged view. Remove sample cup tray and housing cover of the Auto-Shot Sampler. Press the
metal plate attached to the solenoid valve by finger to open the shut (left of Fig. 6.5).
Cleaning operations are shown in Fig. 6.6. A cotton swab dampened with a solvent may be used to
clean the shut.
Sample cup shut
Sample cup hole
Close
Open
Fig. 6.5 The top of the Auto-Shot Sampler (there is no sample cup tray) and enlarged picture.
Cotton swab
Fig. 6.6 Cleaning Sample Cup Shut
6-4
Ver2.22
6.2.2 Cleaning Carrousel and Sample Cup Tray
1.
Remove cup chute and sample cup tray cover.
2.
Remove sample cup tray securing screw from the sample cup tray (Fig. 6.7). Be sure not to lose
the screw
3
Carefully examine each part for dirt. Clean the surface of each part with methanol.
Sample cup tray
cover securing screw
Threaded hole for
securing carrousel
Sample cup tray
securing screw
Sample cup tray
securing screw
Sample cup tray N
Carrousel securing
screw
Sample cup
carrousel N
F ig. 6.7 Sample Cup Tray and Names of the Parts
4.
Clean the inner wall of each hole of carrousel with a cotton swab dampened with a solvent.
This cleaning is very important as the sample cup is very light in weight, small particles derive from dirt
or sample may not allow the sample cup to drop into the furnace and may result in malfunction.
Frequent cleaning is recommended.
Cotton swab
Fig. 6.8 Cleaning Carrousel
6-5
Ver2.22
6.3 Cleaning Quartz Pyrolysis Tube
If quartz pyrolysis tube is heavily contaminated, bake it with a burner flame to clean it (see NOTE
below). While baking the tube, blowing air in from one of the ends of the pyrolysis tube may help burn
off the contaminants. If above does not work, rub the tube with a cotton swab dampened with 0.1N
nitric acid. Never use hydrochloric acid, because it will heavily damage the surface of the quartz
pyrolysis tube, leading to absorption of pyrolyzates on the surface.
When removing quartz pyrolysis tube, difficulties may be experienced in removing the
!
Note
vesper ferrule from interface union and quartz pyrolysis tube. If this is the case, heating
the ferrule with a burner flame will help loosen it. The removed ferrule can not be
reused.
(See Operation manual for Pyrolyzer, Section 6.1.2 Replacing and cleaning quartz
pyrolysis tube)
6.4 Cleaning Interface Needle
Major contaminants of the interface needle are deposited tars of tars and carbons. If the needle is
clogged, drive a thin metal wire through it, followed by immersing it in a solvent and apply ultrasonic
cleaning. If this does not seem to work, replace it with a new needle. In daily routine work, keep the
temperature of the interface (ITF TEMP) and GC injection port between 250°C and 320°C so that the
interface temperature does not drop too low.
6-6
Ver2.22
CHAPTER 7
TROUBLESHOOTING
Symptom, causes, and solutions are summarized below. For problems associated with pyrolyzer
furnace, See the operation manual of your pyrolyzer. If your problems are not found here, please
contact our service personnel
SYMPTOM
Auto-Shot Sampler
not recognized by PC
Auto-Shot Sampler
not operable
Sequence aborts or
not completed.
CAUSE
SOLUTION
Communication error
Check the power supply of each device and connection of the cable.
See Fig. 3.7 for cable connection.
Wrong communication
port number is selected
Select correct port number of which communication cable (RS-232C
cable) of PY-2020iD and/or AS-1020E/ET is connected. See
CHAPTER 5 “Starting Auto-Shot Sampler”.
Sample cup recovery
chute
not
properly
placed and the safety
circuit activated
Check to see if sample cup recovery chute is properly set in place
and correct the problem. See 3.5 “Removing Sample cup Tray”.
Communication error
Check and correct RS-232C connection problem. See Fig. 3.7 for
cable connection.
Sample cup detection
error
Make sure sample cups are Eco-cup L. See Chapter 4 “Notes on
Sample Pretreatment”.
Sample cup recovery
error
Incomplete sequence
table
See below item “Sample cups not recovered”.
Check and correct sequence table. See “5.3 Creating Sequence
Table”.
Perform leakage check of pyrolyzer furnace joint nut and tighten it if
required. See Fig.3.9.1 “Connecting Auto-Shot Sampler and
Pyrolyzer Furnace”.
No peaks
Gas leakage
Check leakage at the ITF joint. Tighten the nut if needed. See Fig.
3.2 “Attaching ITF Union for Auto-Shot Sampler”.
Perform leakage check of entire system and correct the problem.
Contact your dealer, if needed.
Make sure regulator secondary pressure is 500~600kPa.
Recovery gas pressure
too low
Distorted sample cups
Sample cups
recovered
not
Open the stopcock of gas reservoir for Auto-Shot Sampler, if closed,
and check pressure and set it to 300kPa. See Fig. 1.7 “Front View of
Gas Reservoir for Auto-Shot Sampler”.
Check sample cups with sample cup inspection jig and replace cups
with new ones if out of shape. See Fig. 6.1 “Using Sample Cup
Inspection jig”.
Recovery valve cable
connection is error
Check recovery valve cable connection and correct the problem. See
Fig. 3.7 “Connecting Cables”.
Incomplete installation
of Sample cup tray
cover
Check alignment of the hole of the sample cup recovering and the
hole of the sample cup carrousel at the home position (Cup No. “0”).
If misalignment is seen, loosen screws located at the clasp of the tray
cover then adjust or fix the alignment.
Contaminated Sample
cup pass
Sample cups may not recovered due to the contamination or
adherent of foreign objects in the sample cup pass. Cleaning is
needed for these cases.
7-1
Ver.2.22